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Sample records for green microwave-assisted conversion

  1. Microwave-assisted water extraction of green tea polyphenols.

    Science.gov (United States)

    Nkhili, Ezzohra; Tomao, Valerie; El Hajji, Hakima; El Boustani, Es-Seddik; Chemat, Farid; Dangles, Olivier

    2009-01-01

    Green tea, a popular drink with beneficial health properties, is a rich source of specific flavanols (polyphenols). There is a special interest in the water extraction of green tea polyphenols since the composition of the corresponding extracts is expected to reflect the one of green tea infusions consumed worldwide. To develop a microwave-assisted water extraction (MWE) of green tea polyphenols. MWE of green tea polyphenols has been investigated as an alternative to water extraction under conventional heating (CWE). The experimental conditions were selected after consideration of both temperature and extraction time. The efficiency and selectivity of the process were determined in terms of extraction time, total phenolic content, chemical composition (HPLC-MS analysis) and antioxidant activity of the extracts. By MWE (80 degrees C, 30 min), the flavanol content of the extract reached 97.46 (+/- 0.08) mg of catechin equivalent/g of green tea extract, vs. only 83.06 (+/- 0.08) by CWE (80 degrees C, 45 min). In particular, the concentration of the most bioactive flavanol EGCG was 77.14 (+/- 0.26) mg of catechin equivalent/g of green tea extract obtained by MWE, vs 64.18 (+/- 0.26) mg/g by CWE. MWE appears more efficient than CWE at both 80 and 100 degrees C, particularly for the extraction of flavanols and hydroxycinnamic acids. Although MWE at 100 degrees C typically affords higher yields in total phenols, MWE at 80 degrees C appears more convenient for the extraction of the green tea-specific and chemically sensitive flavanols.

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

    Science.gov (United States)

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

    2014-12-01

    The microwave-assisted extraction (MAE) of 13 different green coffee beans (Coffea arabica L.) was compared to Soxhlet extraction for oil obtention. The full factorial design applied to the microwave-assisted extraction (MAE), related to time and temperature parameters, allowed to develop a powerful fast and smooth methodology (10 min at 45°C) compared to a 4h Soxhlet extraction. The quantification of cafestol and kahweol diterpenes present in the coffee oil was monitored by HPLC/UV and showed satisfactory linearity (R(2)=0.9979), precision (CV 3.7%), recovery (Soxhlet method. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. 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...

  4. The Microwave-Assisted Green Synthesis of TiC Powders.

    Science.gov (United States)

    Wang, Hui; Zhu, Wencheng; Liu, Yanchun; Zeng, Lingke; Sun, Luyi

    2016-11-08

    Titanium carbide (TiC) is an important engineering material and has found widespread applications. Currently, TiC is typically synthesized through carbothermal reduction, requiring a high temperature (ca. 1700-2300 °C) and long reaction time (ca. 10-20 h), which is not eco-friendly. During a conventional reaction path, anatase TiO₂ (A-TiO₂) was first converted to rutile TiO₂ (R-TiO₂), which was subsequently reduced to TiC. Herein, we explored the synthesis of TiC powders with the assistance of microwave heating. In particular, we achieved the conversion of A-TiO₂, which was more reactive than R-TiO₂ for the carbothermal reduction, to TiC, which was directly due to quick microwave heating. As such, the carbothermal reduction started at a much lower temperature of ca. 1200 °C and finished within 30 min when reacting at 1400 °C, leading to significant energy saving. This study shows that microwave-assisted synthesis can be an effective and green process for preparing TiC powders, which is promising for future large-scale production. The influence of the reaction temperature, the reaction duration, and the carbon content on the synthesis of TiC powders was investigated.

  5. Microwave-assisted facile green synthesis of silver nanoparticles ...

    Indian Academy of Sciences (India)

    Silver nanoparticles have been successfully synthesized in aqueous medium by a green, rapid and costefficient synthetic approach based on microwave irradiation. In this study, iota-carrageenan (I-carrageenan) is used both as reducing and stabilizing agent. The formation of nanoparticles is determined using UV–vis, ...

  6. Microwave-assisted facile green synthesis of silver nanoparticles ...

    Indian Academy of Sciences (India)

    2016-08-26

    Aug 26, 2016 ... Silver nanoparticles have been successfully synthesized in aqueous medium by a green, rapid and costefficient synthetic approach based on microwave irradiation. In this study, iota-carrageenan (I-carrageenan) is used both as reducing and stabilizing agent. The formation of nanoparticles is determined ...

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

  8. Selective conversion of cellulose to levulinic acid via microwave-assisted synthesis in ionic liquids.

    Science.gov (United States)

    Ren, Huifang; Zhou, Yonggui; Liu, Li

    2013-02-01

    A highly selective approach to produce levulinic acid from cellulose was developed via microwave-assisted synthesis in SO3H-functionalized ionic liquids (SFILs). The effects of reaction conditions and ionic liquid structures on the yield of levulinic acid have been investigated, where the highest yield of 55.0% was obtained. The catalytic activities of SFILs depend on the anions and decrease in the order: HSO4->CH3SO3->H2PO4-, which is in good agreement with their acidity order. The SFILs are efficient catalysts for cellulose conversion into levulinic acid and the subsequent esterification, which facilitates the separation of product and reuse of ionic liquids. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. 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. 

  10. Pd/C-catalyzed aerobic oxidative esterification of alcohols and aldehydes: a highly efficient microwave-assisted green protocol

    Directory of Open Access Journals (Sweden)

    Marina Caporaso

    2014-06-01

    Full Text Available We herein describe an environmentally friendly microwave-assisted oxidative esterification of alcohols and aldehydes in the presence of molecular oxygen and a heterogeneous catalysis (Pd/C, 5 mol %. This efficient and ligandless conversion procedure does not require the addition of an organic hydrogen acceptor. The reaction rate is strongly enhanced by mild dielectric heating. Furthermore, it is a versatile green procedure which generally enables the isolation of esters to be carried out by simple filtration in almost quantitative yields.

  11. Efficient and 'green' microwave-assisted synthesis of haloalkylphosphonates via the Michaelis-Arbuzov reaction

    Czech Academy of Sciences Publication Activity Database

    Jansa, Petr; Holý, Antonín; Dračínský, Martin; Baszczyňski, Ondřej; Česnek, Michal; Janeba, Zlatko

    2011-01-01

    Roč. 13, č. 4 (2011), s. 882-888 ISSN 1463-9262 R&D Projects: GA AV ČR KJB400550903; GA MŠk 1M0508 Institutional research plan: CEZ:AV0Z40550506 Keywords : microwave-assisted synthesis * haloalkylphosphonates * Michaelis-Arbuzov reaction Subject RIV: CC - Organic Chemistry Impact factor: 6.320, year: 2011

  12. Green synthesis of tetrahydrobenzo[b]Pyrans by microwave assisted multi-component one-pot reactions in PEG-400.

    Science.gov (United States)

    Feng, Chun; Wang, Qiuyan; Lu, Cuifen; Yang, Guichun; Chen, Zuxing

    2012-01-01

    Polyethylene glycol is found to be a nontoxic and recyclable reaction medium for the microwave-assisted, multi-component one-pot reactions of aromatic aldehydes with ethyl-2-cyanoacetate and 1,3-cyclohexanedione or 5,5- dimethyl-1,3-cyclohexanedione in the presence of piperidine. This environmentally friendly microwave protocol offers ease of operation and enables recyclability of reaction medium and synthesis of a variety of substituted tetrahydrobenzo[b]pyran derivatives. It is an efficient, promising, and green synthetic strategy to construct tetrahydrobenzo[b]pyran skeleton.

  13. Facile microwave-assisted synthesis of Zn2GeO4:Mn2+, Yb3+ uniform nanorods and near-infrared down-conversion properties

    Science.gov (United States)

    Yang, Min; Deng, Guowei; Hou, Tianwu; Jia, Xiaopeng; Wang, Ying; Wang, Qihui; Li, Bingke; Liu, Jialei; Liu, Xiaoyang

    2017-02-01

    Germanates have potential applications in electroluminescent fields. Herein, we report a simple strategy for the rapid synthesis of near-infrared (NIR) down-conversion Zn1.96-xGeO4+1/2x:Mn0.04Ybx phosphors using the microwave-assisted hydrothermal method. This method is facile, rapid, surfactant-free and environmentally friendly. In the Zn2GeO4 lattice, intrinsic defect transitions and Mn2+ ions act as broadband spectral sensitizers by absorbing UV-Vis (280-500 nm) photons and transferring the absorbed energy to Yb3+ centers in a cooperative down-conversion process. Efficient energy transfer is reflected by a sharp decrease in the excited state lifetime and green photoluminescence (PL) from tetrahedrally coordinated Mn2+ with increasing Yb3+ concentration. The possible formation mechanism for Zn1.96-xGeO4+1/2x:Mn0.04Ybx nanorods has been presented. PL spectroscopic characterizations show that pure Zn2GeO4 sample shows a blue emission due to defects, while Zn2GeO4:Mn2+ phosphors exhibit a green emission corresponding to the characteristic transition of Mn2+ (4T1 → 6A1) under the excitation of UV. The Yb3+ acceptor is then the source of NIR emission at a wavelength of ∼1000 nm. These phosphors are promising for applications in solar spectral down-conversion.

  14. Microwave-assisted polyol synthesis of gadolinium-doped green luminescent carbon dots as a bimodal nanoprobe.

    Science.gov (United States)

    Gong, Ningqiang; Wang, Hao; Li, Shuai; Deng, Yunlong; Chen, Xiao'ai; Ye, Ling; Gu, Wei

    2014-09-16

    The development of multimodal nanoprobes is highly desired in medical imaging because it integrates the advantages of multiple imaging modes. In this study, the gadolinium-doped green luminescent carbon dots (Gd-CDs) were prepared by the simple one-step microwave-assisted polyol method. The obtained Gd-CDs emitted a unique green photoluminescence with a quantum yield of 5.4%. The Gd-CDs exhibited a low cytotoxicity and could optically label the C6 glioma cells. Meanwhile, the r1 relaxivity of Gd-CDs was measured to be 11.356 mM(-1) s(-1). This high r1 value together with the r2/r1 ratio close to 1 nominates Gd-CDs as an excellent T1 contrast agent for magnetic resonance imaging. These Gd-CDs combining two complementary imaging modalities are therefore a promising bimodal nanoprobe in medical imaging for a better diagnosis.

  15. Antibacterial Activities of Green Basil (Ocimum Violaceum Essential Oil and Derivatives By MAOS (Microwave Assisted Organic Synthesis Against Staphyllococus Aureus and Escherichia Coli

    Directory of Open Access Journals (Sweden)

    Dwiarso Rubiyanto

    2014-07-01

    Full Text Available Green basil (Ocimum violaceum , Linn. plantis part of the varieties of basil (Ocimum basilicum, Linn.. Green basil essential oil (GBEO contain chemical compounds that have an anti- bacterial activities . Methyl eugenol and methyl chavikol are in green basil oil has the potential to be used as a material which is biologically active. Conversion reaction of the compounds in GBEO with MAOS methods (microwave assisted organic synthesis aims to obtain properties of the main chemical component in a wider sweet basil oil, and are also useful in an attempt to gain more valuable compounds for commercial and higher. The results showed that the optimum reaction conditions on the conversion reaction of compounds in GBEO with MAOS method with ethylene glycol as a solvent is 10 % KF/Al2O3as catalyst and reaction time 3 minutes , while the solvent is glycerol 10 % KF/Al2O3as catalyst and reaction time 2 minutes . Comparison of anti-bacterial activity resulting from this research are : the inhibitory activity to the growth of S. aureus bacteria have the following order : GBEO > green basilEG10-3 > green basil G10-2> amoxicillin with each inhibition zone diameter amounted to 30.7 mm, 21.1 mm, 18.2 mm and 13.4 mm. While the inhibitory activity to the growth of E.coli bacteria are : GBEO> green basil G10-2 >green basil EG10-3 > amoxicillin with each inhibition zone diameter of 21.1 mm, 15.6 mm , 15.2 mm and 7.9 mm . GBEO and its derivatives have minimal inhibitory concentrations below 1.25 %. From the results of the study found that the main derivates obtained are p-methoxy anisaldehyde , caryophyllene oxide , 3-methoxy cinnamaldehyde , humulena oxide and delta cadinol

  16. Microwave Assisted Expeditious and Green Cu(II-Clay Catalyzed Domino One-Pot Three Component Synthesis of 2H-indazoles

    Directory of Open Access Journals (Sweden)

    Bashir Ahmad Dar

    2018-01-01

    How to Cite: Dar, B.A., Safvi, S.W., Rizvi, M.A. (2018. Microwave Assisted Expeditious and Green Cu(II-Clay Catalyzed Domino One-Pot Three Component Synthesis of 2H-indazoles. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (1: 82-88 (doi:10.9767/bcrec.13.1.963.82-88

  17. Overcoming the Recalcitrance for the Conversion of Kenaf Pulp to Glucose via Microwave-Assisted Pre-Treatment Processes

    Directory of Open Access Journals (Sweden)

    Miguel A. Hurtado

    2011-02-01

    Full Text Available This study evaluates the pre-treatment of cellulose from kenaf plant to yield sugar precursors for the production of ethanol or butanol for use as biofuel additives. In order to convert the crystalline cellulosic form to the amorphous form that can undergo enzymatic hydrolysis of the glycosidic bond to yield sugars, kenaf pulp samples were subjected to two different pre-treatment processes. In the acid pre-treatment, the pulp samples were treated with 37.5% hydrochloric acid in the presence of FeCl3 at 50 °C or 90 °C whereas in the alkaline method, the pulp samples were treated with 25% sodium hydroxide at room temperature and with 2% or 5% sodium hydroxide at 50 °C. Microwave-assisted NaOH-treatment of the cellulose was also investigated and demonstrated to be capable of producing high glucose yield without adverse environmental impact by circumventing the use of large amounts of concentrated acids i.e., 83–85% phosphoric acid employed in most digestion processes. The treated samples were digested with the cellulase enzyme from Trichoderma reesei. The amount of glucose produced was quantified using the QuantichromTM glucose bioassay for assessing the efficiency of glucose production for each of the treatment processes. The microwave-assisted alkaline pre-treatment processes conducted at 50 °C were found to be the most effective in the conversion of the crystalline cellulose to the amorphous form based on the significantly higher yields of sugar produced by enzymatic hydrolysis compared to the untreated sample.

  18. Microwave assisted facile green synthesis of silver and gold nanocatalysts using the leaf extract of Aerva lanata.

    Science.gov (United States)

    Joseph, Siby; Mathew, Beena

    2015-02-05

    Herein, we report a simple microwave assisted method for the green synthesis of silver and gold nanoparticles by the reduction of aqueous metal salt solutions using leaf extract of the medicinal plant Aerva lanata. UV-vis., FTIR, XRD, and HR-TEM studies were conducted to assure the formation of nanoparticles. XRD studies clearly confirmed the crystalline nature of the synthesized nanoparticles. From the HR-TEM images, the silver nanoparticles (AgNPs) were found to be more or less spherical and gold nanoparticles (AuNPs) were observed to be of different morphology with an average diameter of 18.62nm for silver and 17.97nm for gold nanoparticles. In order to evaluate the effect of microwave heating upon rate of formation, the synthesis was also conducted under ambient condition without the assistance of microwave radiation and the former method was found to be much faster than the later. The synthesized nanoparticles were used as nanocatalysts in the reduction of 4-nitrophenol to 4-aminophenol by NaBH4. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Microwave assisted facile green synthesis of silver and gold nanocatalysts using the leaf extract of Aerva lanata

    Science.gov (United States)

    Joseph, Siby; Mathew, Beena

    2015-02-01

    Herein, we report a simple microwave assisted method for the green synthesis of silver and gold nanoparticles by the reduction of aqueous metal salt solutions using leaf extract of the medicinal plant Aerva lanata. UV-vis., FTIR, XRD, and HR-TEM studies were conducted to assure the formation of nanoparticles. XRD studies clearly confirmed the crystalline nature of the synthesized nanoparticles. From the HR-TEM images, the silver nanoparticles (AgNPs) were found to be more or less spherical and gold nanoparticles (AuNPs) were observed to be of different morphology with an average diameter of 18.62 nm for silver and 17.97 nm for gold nanoparticles. In order to evaluate the effect of microwave heating upon rate of formation, the synthesis was also conducted under ambient condition without the assistance of microwave radiation and the former method was found to be much faster than the later. The synthesized nanoparticles were used as nanocatalysts in the reduction of 4-nitrophenol to 4-aminophenol by NaBH4.

  20. Microwave-Assisted Conversion of Levulinic Acid to γ-Valerolactone Using Low-Loaded Supported Iron Oxide Nanoparticles on Porous Silicates

    Directory of Open Access Journals (Sweden)

    Alfonso Yepez

    2015-09-01

    Full Text Available The microwave-assisted conversion of levulinic acid (LA has been studied using low-loaded supported Fe-based catalysts on porous silicates. A very simple, productive, and highly reproducible continuous flow method has been used for the homogeneous deposition of metal oxide nanoparticles on the silicate supports. Formic acid was used as a hydrogen donating agent for the hydrogenation of LA to effectively replace high pressure H2 mostly reported for LA conversion. Moderate LA conversion was achieved in the case of non-noble metal-based iron oxide catalysts, with a significant potential for further improvements to compete with noble metal-based catalysts.

  1. 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...

  2. A facile and green microwave-assisted synthesis of new functionalized picolinium-based ionic liquids

    Directory of Open Access Journals (Sweden)

    Mouslim Messali

    2016-09-01

    Full Text Available A facile preparation of a series of 17 new functionalized picolinium-based ionic liquids under “green chemistry” conditions is described. For the first time, target ionic liquids were prepared using standard methodology and under microwave irradiation in short duration of time with quantitative yields. Their structures were characterized by FT-IR, 1H NMR, 13C NMR, 11B, 19F, 31P and mass spectra.

  3. A facile and green microwave-assisted synthesis of new functionalized picolinium-based ionic liquids

    OpenAIRE

    Messali, Mouslim

    2016-01-01

    A facile preparation of a series of 17 new functionalized picolinium-based ionic liquids under “green chemistry” conditions is described. For the first time, target ionic liquids were prepared using standard methodology and under microwave irradiation in short duration of time with quantitative yields. Their structures were characterized by FT-IR, 1H NMR, 13C NMR, 11B, 19F, 31P and mass spectra.

  4. Microwave-Assisted Selective Hydrogenation of Furfural to Furfuryl Alcohol Employing a Green and Noble Metal-Free Copper Catalyst.

    Science.gov (United States)

    Romano, Pedro N; de Almeida, João M A R; Carvalho, Yuri; Priecel, Peter; Falabella Sousa-Aguiar, Eduardo; Lopez-Sanchez, Jose A

    2016-12-20

    Green, inexpensive, and robust copper-based heterogeneous catalysts achieve 100 % conversion and 99 % selectivity in the conversion of furfural to furfuryl alcohol when using cyclopentyl-methyl ether as green solvent and microwave reactors at low H 2 pressures and mild temperatures. The utilization of pressurized microwave reactors produces a 3-4 fold increase in conversion and an unexpected enhancement in selectivity as compared to the reaction carried out at the same conditions using conventional autoclave reactors. The enhancement in catalytic rate produced by microwave irradiation is temperature dependent. This work highlights that using microwave irradiation in the catalytic hydrogenation of biomass-derived compounds is a very strong tool for biomass upgrade that offers immense potential in a large number of transformations where it could be a determining factor for commercial exploitation. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. A Green Protocol for Microwave-Assisted Extraction of Volatile Oil Terpenes from Pterodon emarginatus Vogel. (Fabaceae).

    Science.gov (United States)

    Vila Verde, Giuliana M; Barros, Diogo A; Oliveira, Marilene Silva; Aquino, Gilberto L B; Santos, Danilo M; de Paula, José Realino; Dias, Lucas D; Piñeiro, Marta; Pereira, Mariette M

    2018-03-13

    Microwave-assisted extraction of volatile oils (MAE) potentially offers a more efficient and bio-sustainable method than conventional extraction by Clevenger apparatus (CE). This study aimed to optimise the MAE of the volatile oil from Pterodon emarginatus fruits and characterise the volatile compounds. A 2³ full-factorial central composite design and response surface methodology were used to evaluate the effects of time (min), moisture (%) and microwave power (W) on the extraction yield. The process optimisation was based on the desirability function approach. The reaction time and moisture conditions were standardised in these analyses. The volatile oil composition was analysed by Gas Chromatography/Mass Spectrometry (GC/MS) in order to compare techniques extractions influences. Microwave irradiation showed excellent performance for extraction of the volatile oil from Pterodon emarginatus and there were some advantages in compare to conventional method with respect to the time (14 times), energy (6 times), reagents amounts and waste formation. About chemical composition presents significant differences with the type of extraction. Caryophyllene (25.65%) and trans -α-bisabolol (6.24%) were identified as major components in MAE sample while caryophyllene (6.75%) and γ-elemene (7.02%) are the components with higher relative percentage in CE samples. The microwaves assisted process shown an increase of economic interested compounds present in volatile oil.

  6. A Green Protocol for Microwave-Assisted Extraction of Volatile Oil Terpenes from Pterodon emarginatus Vogel. (Fabaceae

    Directory of Open Access Journals (Sweden)

    Giuliana M. Vila Verde

    2018-03-01

    Full Text Available Microwave-assisted extraction of volatile oils (MAE potentially offers a more efficient and bio-sustainable method than conventional extraction by Clevenger apparatus (CE. This study aimed to optimise the MAE of the volatile oil from Pterodon emarginatus fruits and characterise the volatile compounds. A 23 full-factorial central composite design and response surface methodology were used to evaluate the effects of time (min, moisture (% and microwave power (W on the extraction yield. The process optimisation was based on the desirability function approach. The reaction time and moisture conditions were standardised in these analyses. The volatile oil composition was analysed by Gas Chromatography/Mass Spectrometry (GC/MS in order to compare techniques extractions influences. Microwave irradiation showed excellent performance for extraction of the volatile oil from Pterodon emarginatus and there were some advantages in compare to conventional method with respect to the time (14 times, energy (6 times, reagents amounts and waste formation. About chemical composition presents significant differences with the type of extraction. Caryophyllene (25.65% and trans-α-bisabolol (6.24% were identified as major components in MAE sample while caryophyllene (6.75% and γ-elemene (7.02% are the components with higher relative percentage in CE samples. The microwaves assisted process shown an increase of economic interested compounds present in volatile oil.

  7. Microwave-assisted green synthesis of silver nanoparticles from Fraxinus excelsior leaf extract and its antioxidant assay

    Science.gov (United States)

    Parveen, Mehtab; Ahmad, Faheem; Malla, Ali Mohammed; Azaz, Shaista

    2016-02-01

    The biosynthesis of nanoparticles has been proposed as a cost effective and environmentally benevolent alternative to chemical and physical methods. In the present study, microwave assisted synthesis of silver nanoparticles (AgNPs) has been demonstrated using leaf extract of Fraxinus excelsior reducing aqueous AgNO3 solution. The synthesized nanoparticles have been characterized on the basis of fourier transform infrared spectroscopy (FT-IR), UV-Vis spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray (EDX) analysis. The presence of a characteristic surface plasmon resonance (SPR) absorption band at 425 nm in UV-Vis reveals the reduction of silver metal ions into silver nanoparticles. FT-IR analysis was carried out to probe the possible functional group involved in the synthesis of AgNPs. Further leaf extracts and AgNPs were evaluated for antiradical scavenging activity by 1,1-diphenyl-2-picryl-hydrazyl (DPPH) assay.

  8. A fast, simple and green method for the extraction of carbamate pesticides from rice by microwave assisted steam extraction coupled with solid phase extraction.

    Science.gov (United States)

    Song, Weitao; Zhang, Yiqun; Li, Guijie; Chen, Haiyan; Wang, Hui; Zhao, Qi; He, Dong; Zhao, Chun; Ding, Lan

    2014-01-15

    This paper presented a fast, simple and green sample pretreatment method for the extraction of 8 carbamate pesticides in rice. The carbamate pesticides were extracted by microwave assisted water steam extraction method, and the extract obtained was immediately applied on a C18 solid phase extraction cartridge for clean-up and concentration. The eluate containing target compounds was finally analysed by high performance liquid chromatography with mass spectrometry. The parameters affecting extraction efficiency were investigated and optimised. The limits of detection ranging from 1.1 to 4.2ngg(-1) were obtained. The recoveries of 8 carbamate pesticides ranged from 66% to 117% at three spiked levels, and the inter- and intra-day relative standard deviation values were less than 9.1%. Compared with traditional methods, the proposed method cost less extraction time and organic solvent. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Microwave assisted template synthesis of silver nanoparticles

    Indian Academy of Sciences (India)

    Administrator

    Abstract. 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 as- sisted process, controlled reaction at elevated temperatures, and microwave assisted process have been evalu ...

  10. Microwave Assisted Rapid and Green Synthesis of Silver Nanoparticles Using a Pigment Produced by Streptomyces coelicolor klmp33

    OpenAIRE

    Manikprabhu, Deene; Lingappa, K.

    2013-01-01

    Traditional synthesis of silver nanoparticles using chemical methods produces toxic substances. In contrast biological synthesis is regarded as a safe and nontoxic process but the major drawback of biological synthesis is, this process is slow. In the present investigation, we developed a rapid and green synthesis of silver nanoparticles employing a pigment produced by Streptomyces coelicolor klmp33 in just 90?s. The silver nanoparticles were characterized by UV-visible spectroscopy, transmis...

  11. Microwave assisted one-step green synthesis of fluorescent carbon nanoparticles from ionic liquids and their application as novel fluorescence probe for quercetin determination

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Deli; Yuan, Danhua [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing 210009 (China); He, Hua, E-mail: dochehua@163.com [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing 210009 (China); Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, China Pharmaceutical University, Nanjing 210009 (China); Gao, Mengmeng [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing 210009 (China)

    2013-08-15

    In this study, a new sensitive and convenient method for the determination of quercetin based on the fluorescence quenching of fluorescent carbon nanoparticles (CNPs) was developed. The CNPs derived from ionic liquids were prepared using a green and rapid microwave-assisted synthetic approach for the first time. The one-step green preparation process is simple and effective, neither a strong acid solvent nor surface modification reagent is needed, which makes this approach very suitable for large-scale production. The prepared CNPs were characterized by high-resolution transmission electron microscopy, Fourier transform infrared spectrometry, elemental analysis and spectrofluorometry. In NH{sub 3}–NH{sub 4}Cl buffer solution (pH 9.47), the fluorescence signals of CNPs decreased obviously with increase of the quercetin concentration. The effect of other coexisting foreign substances on the intensity of CNPs showed a low interference response. Under the optimum conditions, the fluorescence intensity presented a linear response versus quercetin concentration according to the Stern–Volmer equation with an excellent 0.9989 correlation coefficient. The linearity ranged from 2.87×10{sup −6} to 31.57×10{sup −6} mol L{sup −1} with the detection limit (3σ) of 9.88×10{sup −8} mol L{sup −1}. The recovery of this method was in the range of 93.3–105.1%. Therefore, the CNPs could to be a promising candidate as a fluorescence probe for the detection of trace levels of quercetin due to their advantages in low-cost production, low cytotoxicity, strong fluorescence and excellent biocompatibility. -- Highlights: ► Fluorescent CNPs were synthesized with microwave pyrolysis approach. ► Ionic liquids were used as sources of carbon and nitrogen for the first time. ► The formation and functionalization of CNPs were accomplished simultaneously. ► CNPs were used as fluorescent probes for the determination of quercetin. ► A sensitive and convenient method based

  12. Microwave-Assisted Synthesis of a Natural Insecticide on Basic Montmorillonite K10 Clay. Green Chemistry in the Undergraduate Organic Laboratory

    Science.gov (United States)

    Dintzner, Matthew R.; Wucka, Paul R.; Lyons, Thomas W.

    2006-01-01

    A detailed investigation of the clay-catalyzed condensation of sesamol and other phenols with 3-methyl-2-butenal to give methylenedioxyprecocene (MDP) and other chromenes is presented. The clay-catalyzed microwave-assisted condensation of sesamol with 3-methyl-2-butenal is appropriate for incorporation into undergraduate organic laboratory…

  13. A facile green synthesis of Sm2O3 nanoparticles via microwave-assisted urea precipitation route and their optical properties

    Science.gov (United States)

    Xue, Hansong; Zhang, Weina; Li, Xinyu; You, Xiaochang; Rao, Jinsong; Pan, FuSheng

    2017-05-01

    Samarium oxide (Sm2O3) nanoparticles with a narrow size distribution were successfully synthesized by microwave-assisted using urea as precipitant without surfactant or template. The Sm2O3 particles were characterized using X-ray diffraction analysis, field-emission scanning electron microscopy, field-emission transmission electron microscopy and ultraviolet-visible-near-infrared spectrophotometer. The results showed that the samples prepared with different concentration of urea had different particle sizes. When the concentration of urea was 1.2 mol/L, the sample had the smallest particle size. A possible mechanism for the formation of the nanoparticles was proposed. Optical properties of Sm2O3 nanoparticles showed that the nanoparticles had a strong absorption property in the deep ultraviolet region between 200 nm and 270 nm. [Figure not available: see fulltext.

  14. Microwave-assisted ADMET polymerization

    OpenAIRE

    Rojas Jiménez, Giovanni

    2015-01-01

    Microwave-assisted ADMET polymerization is reported on a series of α,ω-diene monomers, both polar and non-polar. Investigations indicate that of the multiple microwave modes possible, constant power is the most advantageous, providing polymers up to M‾w=31,000g/mol. Molecular weight values are nearly triple in comparison with conventional oil bath heating. Polymers are characterized by NMR, GPC, TGA, and DSC. Microwave irradiation provides a highly controllable and energy efficient ADMET poly...

  15. Mechanochemical Synthesis of 3d Transition-Metal-1,2,4-Triazole Complexes as Precursors for Microwave-Assisted and Thermal Conversion to Coordination Polymers with a High Influence on the Dielectric Properties.

    Science.gov (United States)

    Brede, Franziska A; Heine, Johanna; Sextl, Gerhard; Müller-Buschbaum, Klaus

    2016-02-18

    The complexes [MCl2 (TzH)4] (M=Mn (1), Fe (2); TzH=1,2,4-1H-triazole) and [ZnCl2 (TzH)2] (3) have been obtained by mechanochemical reactions of the corresponding divalent metal chloride and 1,2,4-1H-triazole. They were successfully used as precursors for the formation of coordination polymers either by a microwave-assisted reaction or by thermal conversion. For manganese, the conversion directly yielded 1∞ [MnCl2 TzH] (4), whereas for the iron-containing precursor, 1∞ [FeCl2 TzH] (6), was formed via the intermediate coordination polymer 1∞ [FeCl(TzH)2]Cl (5). For cobalt, the isotypic polymer 1∞ [CoCl(TzH)2]Cl (7) was obtained, but exclusively by a microwave-induced reaction directly from CoCl2 . The crystal structures were resolved from single crystals and powders. The dielectric properties were determined and revealed large differences in permittivity between the precursor complexes and the rigid chain-like coordination polymers. Whereas the monomeric complexes exhibit very different dielectric behaviour, depending on the transition metal, from "low-k" to "high-k" with the permittivity ranging from 4.3 to >100 for frequencies of up to 1000 Hz, the coordination polymers and complexes with strong intermolecular interactions are all close to "low-k" materials with very low dielectric constants up to 50 °C. Therefore, the conversion procedures can be used to deliberately influence the dielectric properties from complex to polymer and for different 3d transition-metal ions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. 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.

  17. Microwave-assisted green synthesis of superparamagnetic nanoparticles using fruit peel extracts: surface engineering, T2 relaxometry, and photodynamic treatment potential

    Directory of Open Access Journals (Sweden)

    Bano S

    2016-08-01

    Full Text Available Shazia Bano,1–3 Samina Nazir,2 Alia Nazir,1 Saeeda Munir,3 Tariq Mahmood,2 Muhammad Afzal,1 Farzana Latif Ansari,4 Kehkashan Mazhar3 1Department of Physics, The Islamia University of Bahawalpur, Bahawalpur, 2Nanosciences and Technology Department, National Centre for Physics, 3Institute of Biomedical and Genetic Engineering (IBGE, 4Pakistan Council for Science and Technology, Islamabad, Pakistan Abstract: Superparamagnetic iron oxide nanoparticles (SPIONs have the potential to be used as multimodal imaging and cancer therapy agents due to their excellent magnetism and ability to generate reactive oxygen species when exposed to light. We report the synthesis of highly biocompatible SPIONs through a facile green approach using fruit peel extracts as the biogenic reductant. This green synthesis protocol involves the stabilization of SPIONs through coordination of different phytochemicals. The SPIONs were functionalized with polyethylene glycol (PEG-6000 and succinic acid and were extensively characterized by X-ray diffraction analysis, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, Rutherford backscattering spectrometry, diffused reflectance spectroscopy, fluorescence emission, Fourier-transform infrared spectroscopy, ultraviolet-visible spectroscopy, and magnetization analysis. The developed SPIONs were found to be stable, almost spherical with a size range of 17–25 nm. They exhibited excellent water dispersibility, colloidal stability, and relatively high R2 relaxivity (225 mM-1 s-1. Cell viability assay data revealed that PEGylation or carboxylation appears to significantly shield the surface of the particles but does not lead to improved cytocompatibility. A highly significant increase of reactive oxygen species in light-exposed samples was found to play an important role in the photokilling of human cervical epithelial malignant carcinoma (HeLa cells. The bio-SPIONs developed

  18. Microwave-assisted green synthesis of superparamagnetic nanoparticles using fruit peel extracts: surface engineering, T 2 relaxometry, and photodynamic treatment potential.

    Science.gov (United States)

    Bano, Shazia; Nazir, Samina; Nazir, Alia; Munir, Saeeda; Mahmood, Tariq; Afzal, Muhammad; Ansari, Farzana Latif; Mazhar, Kehkashan

    2016-01-01

    Superparamagnetic iron oxide nanoparticles (SPIONs) have the potential to be used as multimodal imaging and cancer therapy agents due to their excellent magnetism and ability to generate reactive oxygen species when exposed to light. We report the synthesis of highly biocompatible SPIONs through a facile green approach using fruit peel extracts as the biogenic reductant. This green synthesis protocol involves the stabilization of SPIONs through coordination of different phytochemicals. The SPIONs were functionalized with polyethylene glycol (PEG)-6000 and succinic acid and were extensively characterized by X-ray diffraction analysis, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, Rutherford backscattering spectrometry, diffused reflectance spectroscopy, fluorescence emission, Fourier-transform infrared spectroscopy, ultraviolet-visible spectroscopy, and magnetization analysis. The developed SPIONs were found to be stable, almost spherical with a size range of 17-25 nm. They exhibited excellent water dispersibility, colloidal stability, and relatively high R 2 relaxivity (225 mM(-1) s(-1)). Cell viability assay data revealed that PEGylation or carboxylation appears to significantly shield the surface of the particles but does not lead to improved cytocompatibility. A highly significant increase of reactive oxygen species in light-exposed samples was found to play an important role in the photokilling of human cervical epithelial malignant carcinoma (HeLa) cells. The bio-SPIONs developed are highly favorable for various biomedical applications without risking interference from potentially toxic reagents.

  19. 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.

  20. 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.

  1. Microwave-Assisted Combustion Synthesis of ZnO:Eu Nanoparticles: Effect of Fuel Types.

    Science.gov (United States)

    Rasouli, Sousan; Arabi, Amir-Masoud; Naeimi, Alireza; Hashemi, Seyed-Masoud

    2018-01-01

    Nanoparticles of Europium oxide doped with Zinc oxide were synthesized via microwave-assisted combustion method. Citric acid as a simultaneous fuel and chelating agent and glycine as a fuel and mixture of these fuels were sleeted. X-Ray diffraction patterns (XRD) indicated the formation of ZnO structure with a few amount of Eu 2 O 3 phase. Fourier transformation infra red (FTIR) spectra reveal the increase of ZnO 4 bonds with glycine content of fuels mixture. Scanning electron microscope (SEM) images showed the conversion of nanosphere to spongy-like structure with respect to change of fuel mixtures from citric to glycine. From transmission electron microscopy (TEM) nanoparticles of a mean size 30 nm are observed Green fluorescence emission of different samples was due to activation of self activated center of ZnO structure through transition of electron from Eu 3+ to V zn sites.

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

    Science.gov (United States)

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

    2016-01-01

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

  3. Ceramic matrix composites by microwave assisted CVI

    International Nuclear Information System (INIS)

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

    1993-01-01

    Chemical vapor infiltration (CVI) processes for producing continuously reinforced ceramic composites are reviewed. Potential advantages of microwave assisted CVI are noted and numerical studies of microwave assisted CVI are reviewed. The models predict inverted thermal gradients in fibrous ceramic preforms subjected to microwave radiation and suggest processing strategies for achieving uniformly dense composites. Comparisons are made to experimental results on silicon-based composite systems. The role played by the relative ability of fiber and matrix to dissipate microwave energy is noted. Results suggest that microwave induced inverted gradients can be exploited to promote inside-out densification. 10 refs., 2 figs

  4. Microwave assisted template synthesis of silver nanoparticles

    Indian Academy of Sciences (India)

    Administrator

    Various methods for synthesis, such as conventional temperature as- sisted process, controlled reaction at elevated temperatures, and microwave assisted process have been evalu- ated for the kind of silver nanoparticles synthesized. Starch has been employed as a template and reducing agent. Electron microscopy ...

  5. Microwave Assisted Synthesis and Photoluminescence Properties of ...

    Indian Academy of Sciences (India)

    46

    Microwave Assisted Synthesis and Photoluminescence Properties of. ZnS:Pb2+ Nanophosphor for Solid State Lighting. D.N.Game1*, C.B. Palan3, N.B.Ingale2 and S.K.Omanwar3. 1Cusrow Wadia Institute of Technology, Pune, India. 2 Prof. Ram Meghe Institute of Technology and Research, Badnera, Amravati, India.

  6. MICROWAVE-ASSISTED SYNTHESIS OF SOME NITRO ...

    African Journals Online (AJOL)

    Chem. Life Sci. 2014, 347, 387-397. 32. Menteşe, E. Efficient microwave assisted synthesis of some new benzimidazoles containing the mebendazole nucleus. J. Chem. Res. 2013, 37, 168-170. 33. Menteşe, E.; Yılmaz, F.; Mutlu, F.; Kahveci, B. Synthesis of new coumarin containing benzimidazole derivatives. J. Chem. Res.

  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. 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 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. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. Fast and Green Microwave-Assisted Conversion of Essential Oil Allylbenzenes into the Corresponding Aldehydes via Alkene Isomerization and Subsequent Potassium Permanganate Promoted Oxidative Alkene Group Cleavage

    DEFF Research Database (Denmark)

    Luu, Thi Xuan Thi; Lam, Trinh To; Le, Thach Ngoc

    2009-01-01

    oxidation of the latter to the corresponding benzaldehyde by KMnO4/CuSO4 center dot 5H(2)O. The assistance by microwave irradiation results in very short reaction times (eugenol (4-allyl-2-methoxyphenol) into vanillin (4-hydroxy-3-methoxybenzaldehyde) has been carried...

  11. 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.

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

    Science.gov (United States)

    Singh, Inderbir; Rani, Priya; Kumar, Pradeep

    2017-01-01

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

  13. 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. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Microwave-assisted nonionic surfactant extraction of aliphatic hydrocarbons from petroleum source rock

    Energy Technology Data Exchange (ETDEWEB)

    Akinlua, A., E-mail: geochemresearch@yahoo.com [Fossil Fuels and Environmental Geochemistry Group, Department of Chemistry, Obafemi Awolowo University, Ile-Ife (Nigeria); Jochmann, M.A.; Laaks, J.; Ewert, A.; Schmidt, T.C. [Instrumental Analytical Chemistry, University Duisburg-Essen, Universitaetsstr, 5, 45141 Essen (Germany)

    2011-04-08

    The extraction of aliphatic hydrocarbons from petroleum source rock using nonionic surfactants with the assistance of microwave was investigated and the conditions for maximum yield were determined. The results showed that the extraction temperatures and kinetic rates have significant effects on extraction yields of aliphatic hydrocarbons. The optimum temperature for microwave-assisted nonionic surfactant extraction of aliphatic hydrocarbons from petroleum source rock was 105 deg. C. The optimum extraction time for the aliphatic hydrocarbons was at 50 min. Concentration of the nonionic surfactant solution and irradiation power had significant effect on the yields of aliphatic hydrocarbons. The yields of the analytes were much higher using microwave assisted nonionic surfactant extraction than with Soxhlet extraction. The recoveries of the n-alkanes and acyclic isoprenoid hydrocarbons for GC-MS analysis from the extractant nonionic surfactant solution by in-tube extraction (ITEX 2) with a TENAX TA adsorbent were found to be efficient. The results show that microwave-assisted nonionic surfactant extraction (MANSE) is a good and efficient green analytical preparatory technique for geochemical evaluation of petroleum source rock.

  15. Microwave-assisted nonionic surfactant extraction of aliphatic hydrocarbons from petroleum source rock.

    Science.gov (United States)

    Akinlua, A; Jochmann, M A; Laaks, J; Ewert, A; Schmidt, T C

    2011-04-08

    The extraction of aliphatic hydrocarbons from petroleum source rock using nonionic surfactants with the assistance of microwave was investigated and the conditions for maximum yield were determined. The results showed that the extraction temperatures and kinetic rates have significant effects on extraction yields of aliphatic hydrocarbons. The optimum temperature for microwave-assisted nonionic surfactant extraction of aliphatic hydrocarbons from petroleum source rock was 105°C. The optimum extraction time for the aliphatic hydrocarbons was at 50 min. Concentration of the nonionic surfactant solution and irradiation power had significant effect on the yields of aliphatic hydrocarbons. The yields of the analytes were much higher using microwave assisted nonionic surfactant extraction than with Soxhlet extraction. The recoveries of the n-alkanes and acyclic isoprenoid hydrocarbons for GC-MS analysis from the extractant nonionic surfactant solution by in-tube extraction (ITEX 2) with a TENAX TA adsorbent were found to be efficient. The results show that microwave-assisted nonionic surfactant extraction (MANSE) is a good and efficient green analytical preparatory technique for geochemical evaluation of petroleum source rock. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. 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. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. 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.

  18. Application of microwave assisted digestion in industrial hygiene

    International Nuclear Information System (INIS)

    Paudyn, A.M.; Smith, R.G.; Gawlowski, E.

    1990-01-01

    Microwave assisted digestion plays an important role in speeding up acquisition of analytical data for industrial hygiene purposes. This paper will compare hot plate and microwave assisted digestion for the determination of elements in industrial samples (air sampling filters, dusts, ashes, paints) by the ICPAES technique. Also, the determination of radionuclides in environmental samples (soils, sediments, rocks) by alpha, beta and gamma spectroscopy after the dissolution in a microwave oven will be presented. The results on the determination of elements in NIST standard reference materials and radionuclides in IAEA standards will be included. QC/QA protocols used in an occupational health laboratory setting will be discussed. Sample preparation using microwave assisted digestion proved not only to speed-up extraction of acid soluble elements, but also to achieve better recovery of some elements (Pb in paints) and give better reproducibility of determinations

  19. Microwave-assisted low temperature synthesis of sodium zirconium ...

    Indian Academy of Sciences (India)

    Administrator

    Abstract. Microwave-assisted procedure for low temperature solid state synthesis of sodium zirconium phosphate (NZP), a material with the potential for immobilization and disposal of high level nuclear waste, was developed. Three selected fission products, namely, Cesium, Strontium and Tellurium were introduced ...

  20. 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

  1. Microwave-assisted low temperature synthesis of sodium zirconium ...

    Indian Academy of Sciences (India)

    Microwave-assisted procedure for low temperature solid state synthesis of sodium zirconium phosphate (NZP), a material with the potential for immobilization and disposal of high level nuclear waste, was developed. Three selected fission products, namely, Cesium, Strontium and Tellurium were introduced (substituted) in ...

  2. Flexible composite via rapid titania coating by microwave-assisted ...

    Indian Academy of Sciences (India)

    2017-06-09

    fine titanium oxide (TiO2) growth on carbon fibre via microwave-assisted hydrothermal synthesis (MHS) and to evaluate its photocatalytic properties. The TiO2 nanoparticles were directly grown on the carbon fibre (CF). Thus ...

  3. Microwave-assisted extraction and antihyperlipidemic effect of total ...

    African Journals Online (AJOL)

    The process of microwave-assisted extraction (MAE) of total flavonoids from corn silk and the hypolipidemia in animal models were studied. Influence of solvent concentration, microwave power, extraction time and dose of solvent were investigated and then, the orthogonal experiments were performed. Animal models of ...

  4. Microwave-assisted rapid synthesis of Si-MCM-41

    Indian Academy of Sciences (India)

    Administrator

    Microwave-assisted rapid synthesis of Si-MCM-41. HARESH M MODY 1, PRITI PANDYA 1, PRASHANT BHATT 2 and. RAKSH VIR JASRA 1. 1Silicates and Catalysis Discipline, Central Salt and Marine Chemicals. Research Institute, Bhavnagar 364 002, India. 2Department of Chemistry, Bhavnagar University, Bhavnagar ...

  5. Microwave assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Dr.P.T.P

    Microwave assisted one-pot synthesis of benzothiazole and benzoxazole libraries as analgesic agents. C PRAVEEN a. , A NANDAKUMAR a. , P DHEENKUMAR b. , D MURALIDHARAN a and P T. PERUMAL a,. * a. Organic Chemistry Division, Central Leather Research Institute, Adyar, Chennai 600020,. Tamilnadu, India.

  6. Microwave-assisted low temperature synthesis of sodium zirconium

    Indian Academy of Sciences (India)

    Microwave-assisted procedure for low temperature solid state synthesis of sodium zirconium phosphate (NZP), a material with the potential for immobilization and disposal of high level nuclear waste, was developed. Three selected fission products, namely, Cesium, Strontium and Tellurium were introduced (substituted) in ...

  7. Microwave-assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    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 ...

  8. Microwave-assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 124; Issue 3 ... Abstract. 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 ...

  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 hydrolysis of aluminium metal and preparation ...

    Indian Academy of Sciences (India)

    whereas in the microwave assisted process, the boehmite dehydration took place by a single reaction. 2 AlOOH ! Al2O3 ю H2O. The peaks observed at ~780°C in the microwave processed particle probably represent the transformation to other phases of alumina (Levin and Brandon 1998; Gasik 2003). XRD patterns of the ...

  11. Microwave-assisted brazing of alumina ceramics for electron tube ...

    Indian Academy of Sciences (India)

    2, April 2016, pp. 587–591. c Indian Academy of Sciences. Microwave-assisted brazing of alumina ceramics for electron tube applications. MAYUR SHUKLA1,2 ... 1Academy of Scientific and Innovative Research (AcSIR), CSIR—-Central Glass and Ceramic Research Institute, ... element is the most popular method [2].

  12. Microwave assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Dr.P.T.P

    1. Microwave assisted one-pot synthesis of benzothiazole and benzoxazole libraries as analgesic agents. C PRAVEEN a. , A NANDAKUMAR a. , P DHEENKUMAR b. , D MURALIDHARAN a and P T. PERUMAL a,. * a. Organic Chemistry Division, Central Leather Research Institute, Adyar, Chennai 600020,. Tamilnadu ...

  13. Microwave assisted hydrolysis of aluminium metal and preparation ...

    Indian Academy of Sciences (India)

    Centre for Materials for Electronics Technology (C-MET), Department of Information Technology, Government of India, Athani PO, Thrissur 680 581, India. MS received 30 June 2009; revised 27 July 2009. Abstract. Phase pure boehmite particles were prepared by microwave assisted hydrolysis of aluminium sheets.

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

    Energy Technology Data Exchange (ETDEWEB)

    Raghunandan, Deshpande [H.K.E.S' s College of Pharmacy (India); Mahesh, Bedre D. [Gulbarga University, Materials Chemistry Laboratory, Department of Material Science (India); Basavaraja, S. [Jawaharlal Nehru Centre for Advanced Scientific Research, Veeco-India Nanotechnology Laboratory (India); Balaji, S. D. [Gulbarga University, Materials Chemistry Laboratory, Department of Material Science (India); Manjunath, S. Y. [Sri Krupa, Institute of Pharmaceutical Science (India); Venkataraman, A., E-mail: raman_chem@rediffmail.com [Gulbarga University, Materials Chemistry Laboratory, Department of Material Science (India)

    2011-05-15

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

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

    Science.gov (United States)

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

    2011-05-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  17. Microwave-assisted green synthesis and antimicrobial activity of ...

    African Journals Online (AJOL)

    The AgNPs were characterized by the Ultraviolet-visible (UV-vis) spectral analysis, Dynamic Light Scattering (DLS) zetasizer analysis, Transmission electron microscopy (TEM), X-ray diffraction (XRD) analysis and Fourier transform infrared (FT-IR) spectroscopy. The antimicrobial assays of AgNPs were carried out against ...

  18. Microwave-assisted green synthesis and antimicrobial activity of ...

    African Journals Online (AJOL)

    Purpose: To synthesize and evaluate the antimicrobial activity of silver nanoparticles (AgNPs) derived from a supercritical carbon dioxide extract of the fresh aerial parts of Phyllanthus niruri. Methods: The synthesis of AgNPs of a P. niruri extract was carried out in a microwave oven. The extraction was carried out using a ...

  19. Microwave-assisted facile green synthesis of silver nanoparticles ...

    Indian Academy of Sciences (India)

    I-carrageenan has two sulphates per disaccharide. The presence of hydroxyl and sulphate groups in carrageenan structure makes them likely to be hydrophilic. Hydrogels produced from. I-carrageenan are soft, flexible and fast setting. They have been extensively used in the food industry as a thickening and gelling agent.

  20. Microwave-assisted facile green synthesis of silver nanoparticles ...

    Indian Academy of Sciences (India)

    and spectroscopic investigation of the catalytic activity ... efficient synthetic approach based on microwave irradiation. In this study .... 2.2 Methods. 2.2a Synthesis of AgNP-carrageenan: In a typical synthe- sis, 0.1 g of carrageenan was dissolved in 90 ml of hot water in a beaker. To this, 10 ml of 0.05 M AgNO3 solution was.

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

    Science.gov (United States)

    Majithia, Ravish Yogesh

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

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

    Science.gov (United States)

    DeFilippo, Anthony Cesar

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

  3. 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.

  4. 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.

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

    Science.gov (United States)

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

    2018-07-01

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

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

    Science.gov (United States)

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

    2004-10-20

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

  8. 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.

  9. Evaluation of vacuum microwave-assisted extraction technique for the extraction of antioxidants from plant samples.

    Science.gov (United States)

    Xiao, Xiao-Hua; Wang, Jun-Xia; Wang, Gang; Wang, Jia-Yue; Li, Gong-Ke

    2009-12-18

    In the present work, vacuum microwave-assisted extraction (VMAE) was to perform microwave-assisted extraction in vacuum. Two well-known antioxidants, vitamin C from guava and green pepper, and vitamin E (alpha-tocopherol and gamma-tocopherol) from soybean and tea leaves, which were easy to be oxidized, were chosen as representative target compounds for the evaluation of VMAE. The extraction yields of vitamin C, alpha-tocopherol and gamma-tocopherol in VMAE and those in MAE performed in atmosphere (air-MAE) were compared and the effects of extraction time, extraction temperature and sample matrix were studied. Moreover, the effects of the oxygen and subpressure invacuo were also discussed via performed MAE in N(2) atmosphere (N(2)-MAE). The extraction yields of vitamin C, alpha-tocopherol and gamma-tocopherol in VMAE were higher than that in air-MAE, 35% increments of vitamin C from green pepper, 22% increments of alpha-tocopherol and 47% increments of gamma-tocopherol from tea leaves were obtained, respectively. The comparable increased extraction yields of vitamin C, alpha-tocopherol and gamma-tocopherol in N(2)-MAE to that in air-MAE confirmed that oxygen in system was the crucial factor for the oxidation of vitamin C and vitamin E, VMAE was beneficial for the extraction of these oxygen-sensitive compounds. In addition, the subpressure invacuo in the VMAE system also showed positive affect on the extraction yields. On the basis of preventing oxidation and improving extraction efficiency of target compounds because of less oxygen and subpressure invacuo in the extraction system, VMAE has good potential for the extraction of oxygen-sensitive and thermosensitive compounds from plant samples.

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

    Directory of Open Access Journals (Sweden)

    Tong Wen

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

  11. Detoxification of hazardous waste streams using microwave-assisted fluid-bed oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Varma, R.; Nandi, S.P. (Argonne National Lab., IL (USA)); Katz, J.D. (Los Alamos National Lab., NM (USA))

    1990-01-01

    Microwave-assisted oxidation of trichloroethane (TCE) performed at 500-580{degree}C has been found to be significantly more efficient than conventional oxidation methods. Experiments were conducted using a 6 kilowatt, 2.45 gigohertz power supply and a 6 inch bed of silicon carbide granules in a 1 inch diameter quartz reactor tube which in turn was placed in a microwave cavity. After heating the reactor to a given temperature a TCE-air stream was passed through the silicon carbide bed. TCE was almost completely detoxified (98--99%) in a single pass through the silicon carbide bed at 500--580{degree}C. The oxidation products are HCl, CO{sub 2} and CO. By comparison the corresponding single-pass detoxification using conventional thermal methods results in only partial conversion. The principal products being dichloroethylene (C{sub 2}H{sub 2}Cl{sub 2}) and HCl. 5 refs., 1 tab.

  12. 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.

  13. 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.

  14. Microwave assisted combustion synthesis and characterization of nickel ferrite nanoplatelets

    Directory of Open Access Journals (Sweden)

    M. Venkatesh

    2016-09-01

    Full Text Available Nickel ferrite nanoplatelets have been successfully synthesized by a simple microwave assisted combustion method using trisodium citrate as a fuel. The prepared sample was chemically and structurally characterized by different techniques and the magnetic behaviour was studied by field dependent magnetization measurement. The obtained results indicate that the prepared sample is phase pure nickel ferrite nanoplatelets having size in the range of 40–50 nm and it exhibits a soft ferromagnetic nature with saturation magnetization of 49 emu/g and coercivity of 167 G. Hence proposed method is a facile approach to obtain nickel ferrite nanoplatelets for broad spectrum of applications.

  15. Microwave-assisted route for synthesis of nanosized metal oxides

    Directory of Open Access Journals (Sweden)

    Arunkumar Lagashetty et al

    2007-01-01

    Full Text Available Microwave-assisted route for the synthesis of nanomaterials has gained importance in the field of synthetic technology because of its faster, cleaner and cost effectiveness than the other conventional and wet chemical methods for the preparation of metal oxide nanoparticles. In the present work, synthesis of metal oxide nanoparticles viz., γ-Fe2O3, NiO, ZnO, CuO and Co-γ-Fe2O3 were carried out by microwave-assisted route through the thermal decomposition of their respective metal oxalate precursors employing polyvinyl alcohol as a fuel. The metal oxide nanoparticles are then characterized for their size and γ to α (in γ-Fe2O3 transition and structure by employing powder X-ray diffraction (XRD pattern, high-temperature X-ray diffraction (HTXRD pattern and Fourier transform infrared (FT-IR spectral studies. The morphology of the samples ranged from nanorods to irregular-shaped particles for different metal oxide samples on the basis of scanning electron microscopy and transmission electron microscopy images. Frequency-dependent dielectric study of the ferrite samples (γ-Fe2O3 and Co-Fe2O3 showed a similar behaviour, where the dielectric constant decreased rapidly with increase in frequency. Possible explanation for this behaviour is given.

  16. 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.

  17. Microwave-assisted extraction of pectin from cocoa peel

    Science.gov (United States)

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

    2018-02-01

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

  18. Microwave assisted pyrolysis of halogenated plastics recovered from waste computers.

    Science.gov (United States)

    Rosi, Luca; Bartoli, Mattia; Frediani, Marco

    2018-03-01

    Microwave Assisted Pyrolysis (MAP) of the plastic fraction of Waste from Electric and Electronic Equipment (WEEE) from end-life computers was run with different absorbers and set-ups in a multimode batch reactor. A large amount of various different liquid fractions (up to 76.6wt%) were formed together with a remarkable reduction of the solid residue (up to 14.2wt%). The liquid fractions were characterized using the following different techniques: FT-IR ATR, 1 H NMR and a quantitative GC-MS analysis. The liquid fractions showed low density and viscosity, together with a high concentration of useful chemicals such as styrene (up to 117.7mg/mL), xylenes (up to 25.6mg/mL for p-xylene) whereas halogenated compounds were absent or present in a very low amounts. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. 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.

  20. Focused-microwave-assisted sample preparation (M8)

    International Nuclear Information System (INIS)

    Nobrega, J.A.; Santos, D.M.; Trevizan, L.C.; Costa, L.M.; Nogueira, A.R.A.

    2002-01-01

    Full text: Focused-microwave-assisted sample preparation is a suitable strategy when dealing with high masses of organic samples. However, the final acid concentration of the digestate can difficult routine analytical measurements using spectroscopic techniques. Acids could be evaporated, but this step could be slow even when using microwave-assisted heating and requires a scrubber system for acid vapor collection and neutralization. We are investigating two procedures to decrease the acid concentration of digestates. The first one is based on acid vapor phase digestion of samples contained in PTFE devices' inserted into the microwave flask. The acid solution is heated by absorption of microwave radiation, then the acid vapor partially condenses in the upper part of the reaction flask and it is partially collected in each sample container. Calcium, Fe, Mg, Mn, and Zn were quantitatively recovered in samples of animal and vegetable tissues. Better recoveries were attained when adding a small volume of sodium hypochlorite to the sample. This effect is probably related to the generation of chlorine in the sample container after collecting condensed acid. The second procedure developed is based on the gradual addition of liquid samples to a previously heated acid digestion mixture. This procedure was successfully applied for digestion of milk, fruit juices, and red wine. The main advantage is the possibility of digesting up to four-fold more sample using up to ten-fold lower amounts of concentrated acids. Results obtained using both digestion procedures and measurements by ICP-OES with axial view will be presented. (author)

  1. Synthesis of metal nanoparticles by microwave-assisted solvothermal technique

    Science.gov (United States)

    Li, Dongsheng

    Metal nanoparticles of Ag, Ni, Pd, and Pt were synthesized in this research work by microwave-assisted solvothermal technique. The microwave-assisted solvothermol technique was found to be faster than the conventional solvothermal process in the synthesis of all the metal nanoparticles investigated here. Ethylene glycol, methanol, and ethanol were used as both reducing agents and solvents. The particle size and morphology were observed using a transmission electron miroscope (TEM). Particle size and size distribution were calculated by Image J(TM) software. Optical properties of synthesized metal nanoparticles were characterized by UV-Visible (UV-Vis) Spectrophotometer. Silver nanoparticles of about 10 to 50 nm were synthesized with ethylene glycol as reducing agent. The morphology and particle size of Ag nanoparticle were controlled by varying the concentration of Ag metal source (AgNO 3), polyvinyl pyrrolidone (PVP) molecular weight, and the type of ligands. Furthermore, the growth rate was increased by adding NaOH in the system. Well-dispersed Ni nanoparticles were synthesized with ethylene glycol as reducing agent in a binary protecting agent system of PVP and dodecylamine (DDA) with or without Pt seeding. By neutralizing the H+ formed from the reductive reaction and coordinating with Ni particles, DDA added in the reaction system contributed to the morphology and size control and also led to the formation of Ni nanoparticles without Pt seeding. Palladium and platinum nanoparticles were synthesized with methanol and ethanol as reducing agents. The morphology and particle size were controlled by the concentration of metal precursors, the PVP to metal ions ratio, and the type of reducing agents.

  2. Microwave-assisted catalytic pyrolysis of moso bamboo for high syngas production.

    Science.gov (United States)

    Dong, Qing; Niu, Miaomiao; Bi, Dongmei; Liu, Weiyu; Gu, Xuexin; Lu, Chen

    2018-02-06

    Microwave-assisted pyrolysis of moso bamboo with the activated carbon-supported iron(III) ion catalyst was carried out with the aim of obtaining high quality and quantity syngas(H 2  + CO). The effect of the catalyst on moso bomboo pyrolysis involving the temperature-rising characteristics, product distribution, tar conversion and gas compositions were investigated. The results indicated that the catalyst improved the microwave-absorption capability and increased the maximum reaction temperatures. The formation of gases was promoted by the catalyst mainly at the expense of the tar, indicating the catalyst had an excellent activity for the tar conversion .The catalyst had the positive influence on the formation of syngas with the maximum content reaching up to 81.14 vol% with H 2 /CO being 1.04 and inhibited the production of CH 4 and CO 2 . The loading of iron(III) ion into activated carbon exerted a significant influence on bamboo pyrolysis. The addition of the catalyst increased the thermal efficiency of the reaction system. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Saifuddin Nomanbhay

    2017-06-01

    Full Text Available 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.

  4. Simultaneous microwave-assisted synthesis, characterization, thermal stability, and antimicrobial activity of cellulose/AgCl nanocomposites

    International Nuclear Information System (INIS)

    Li, Shu-Ming; Fu, Lian-Hua; Ma, Ming-Guo; Zhu, Jie-Fang; Sun, Run-Cang; Xu, Feng

    2012-01-01

    By means of a simultaneous microwave-assisted method and a simple chemical reaction, cellulose/AgCl nanocomposites have been successfully synthesized using cellulose solution and AgNO 3 in N,N-dimethylacetamide (DMAc) solvent. The cellulose solution was firstly prepared by the dissolution of the microcrystalline cellulose and lithium chloride (LiCl) in DMAc. DMAc acts as both a solvent and a microwave absorber. LiCl was used as the reactant to fabricate AgCl crystals. The effects of the heating time and heating temperature on the products were studied. This method is based on the simultaneous formation of AgCl nanoparticles and precipitation of the cellulose, leading to a homogeneous distribution of AgCl nanoparticles in the cellulose matrix. The experimental results confirmed the formation of cellulose/AgCl nanocomposites with high-purity, good thermal stability and antimicrobial activity. This rapid, green and environmentally friendly microwave-assisted method opens a new window to the high value-added applications of biomass. -- Highlights: ► Cellulose/AgCl nanocomposites have been synthesized by microwave method. ► Effect of heating temperature on the nanocomposites was researched. ► Thermal stability of the nanocomposites was investigated. ► Cellulose/AgCl nanocomposites had good antimicrobial activity. ► This method is based on the simultaneous formation of AgCl and cellulose.

  5. Microwave-assisted combustion synthesis of NiAl intermetallics in a single mode applicator: Modeling and optimisation

    International Nuclear Information System (INIS)

    Poli, G.; Sola, R.; Veronesi, P.

    2006-01-01

    The microwave-assisted combustion synthesis of NiAl intermetallics in a single mode applicator has been simulated numerically and performed with the aim of achieving the highest yields, energy efficiency and process reproducibility. The electromagnetic field modeling of the microwave system allowed to chose the proper experimental set-up and the materials more suitable for the application, minimising the reflected power and the risks of arcing. In all the experimental conditions tested, conversions of 3-5 g 1:1 atomic ratio Ni and Al powder compacts into NiAl ranged from 98.7% to 100%, requiring from 30 to 180 s with power from 500 to 1500 W. The optimisation procedure allowed to determine and quantify the effects of the main process variables on the ignition time, the NiAl yields and the specific energy consumption, leading to a fast, reproducible and cost-effective process of microwave-assisted combustion synthesis of NiAl intermetallics

  6. The microwave-assisted ionic liquid nanocomposite synthesis: platinum nanoparticles on graphene and the application on hydrogenation of styrene

    Science.gov (United States)

    Lee, Jer-Yeu; Yung, Tung-Yuan; Liu, Ling-Kang

    2013-10-01

    The microwave-assisted nanocomposite synthesis of metal nanoparticles on graphene or graphite oxide was introduced in this research. With microwave assistance, the Pt nanoparticles on graphene/graphite oxide were successfully produced in the ionic liquid of 2-hydroxyethanaminium formate [HOCH2CH2NH3][HCO2]. On graphene/graphite oxide, the sizes of Pt nanoparticles were about 5 to 30 nm from transmitted electron microscopy (TEM) results. The crystalline Pt structures were examined by X-ray diffraction (XRD). Since hydrogenation of styrene is one of the important well-known chemical reactions, herein, we demonstrated then the catalytic hydrogenation capability of the Pt nanoparticles on graphene/graphite oxide for the nanocomposite to compare with that of the commercial catalysts (Pt/C and Pd/C, 10 wt.% metal catalysts on activated carbon from Strem chemicals, Inc.). The conversions with the Pt nanoparticles on graphene are >99% from styrene to ethyl benzene at 100°C and under 140 psi H2 atmosphere. However, ethyl cyclohexane could be found as a side product at 100°C and under 1,520 psi H2 atmosphere utilizing the same nanocomposite catalyst.

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

    CSIR Research Space (South Africa)

    Motshekga, SC

    2011-11-01

    Full Text Available Tin oxide (SnO2) - decorated carbon nanotube (CNT) heterostructures were synthesized by microwave assisted wet impregnation method. CNTs of three different aspect ratios were compared. The hybrid samples were characterized by powder X...

  8. 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.

  9. Microwave-assisted extraction of lipid from fish waste

    Science.gov (United States)

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

    2017-06-01

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

  10. 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.

  11. Novel microwave assisted synthesis of ZnS nanomaterials.

    Science.gov (United States)

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

    2013-02-01

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

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

    Directory of Open Access Journals (Sweden)

    Rahul Vijay Kapoore

    2018-02-01

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

  13. Application of ionic liquids in the microwave-assisted extraction of polyphenolic compounds from medicinal plants.

    Science.gov (United States)

    Du, Fu-You; Xiao, Xiao-Hua; Luo, Xue-Jun; Li, Gong-Ke

    2009-05-15

    Ionic liquids (ILs) solutions as solvents were successfully applied in the microwave-assisted extraction (MAE) of polyphenolic compounds from medicinal plants. ILs, its concentration and MAE conditions were investigated in order to extract polyphenolic compounds effectively from Psidium guajava Linn. (P. guajava) leaves and Smilax china (S. china) tubers. The results obtained indicated that the anions and cations of ILs had influences on the extraction of polyphenolic compounds as well as the ILs with electron-rich aromatic pi-system enhanced extraction ability. Under the optimized conditions, the extraction yields of the polyphenolic compounds were in the range of 79.5-93.8% with one-step extraction, and meanwhile the recoveries were in the range of 85.2-103% with relative standard deviations (R.S.D.s) lower than 5.6%. Compared to conventional extraction procedures, the results suggested that the proposed method was effective and alternative for the extraction of polyphenolic compounds from medicinal plants. In addition, the extraction mechanisms and the structures of samples before and after extraction were also investigated. ILs solutions as green solvents in the MAE of polyphenolic compounds from medicinal plant samples showed a great promising prospect.

  14. 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

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

    Science.gov (United States)

    Czarnecki, Sezin; Duering, Rolf-Alexander

    2013-04-01

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

  16. 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.

  17. 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.

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

    International Nuclear Information System (INIS)

    Ning, Rong; Chen, Ding; Zhang, Qianxia; Bian, Zhibing; Dai, Haixiong; Zhang, Chi

    2014-01-01

    Highlights: • TiH 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 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

  19. Low cost guinea fowl bone derived recyclable heterogeneous catalyst for microwave assisted transesterification of Annona squamosa L. seed oil

    International Nuclear Information System (INIS)

    Singh, Veena; Sharma, Yogesh Chandra

    2017-01-01

    Highlights: • Discarded guinea fowl bone used to derive catalyst for biodiesel production. • High conversion of 95.82 ± 0.2% achieved in 20 min by microwave assisted transesterification of Annona Squamosa L. seed oil. • Catalyst was stable and can be reused up to five times by activation with >80% conversion. • Complete process is cheap, eco-friendly and fulfils ASTM standard limits. - Abstract: Guinea fowl bone derived heterogeneous catalyst was utilized for biodiesel production for the first time on microwave heating system from Annona squamosa (custard apple seed) oil. Synthesized catalyst was characterized by TGA, XRD, FTIR, SEM, EDS, BET surface area and basicity. Optimization for various reaction conditions on FAME conversion was explored. Maximum conversion of 95.82 ± 0.2% FAME was attained at 1:18 M ratio of oil: methanol, 4 wt% of catalyst at 800 W microwave power and 65 °C reaction temperatures for 20 min. Custard apple seed oil was studied by GCMS, whereas synthesized FAME was analysed by 1 H FTNMR spectroscopy. Catalyst was reused up to five times with maximum conversion of >80%. Physicochemical properties of synthesized FAME were studied as per ASTM standards. Results displayed that catalyst derived from guinea fowl bone showed better reusability and has enormous potential to be used for biodiesel production under microwave irradiated transesterification of Annona squamosa L. (custard apple seed) oil within a short reaction time.

  20. Green conversion of municipal solid wastes into fuels and chemicals

    Directory of Open Access Journals (Sweden)

    Leonidas Matsakas

    2017-03-01

    Full Text Available Presently, the society is facing a serious challenge for the effective management of the increasing amount of produced municipal solid wastes. The accumulated waste has caused a series of environmental problems such as uncontrolled release of greenhouse gases. Moreover, the increasing amount of wastes has resulted in a shortage of areas available for waste disposal, resulting in a nonsustainable waste management. These problems led to serious public concerns, which in turn resulted in political actions aiming to reduce the amount of wastes reaching the environment. These actions aim to promote sustainable waste management solutions. The main objective of these policies is to promote the recycling of municipal solid waste and the conversion of waste to energy and valuable chemicals. These conversions can be performed using either biological (e.g., anaerobic digestion or thermochemical processes (e.g., pyrolysis. Research efforts during the last years have been fruitful, and many publications demonstrated the effective conversation of municipal solid waste to energy and chemicals. These processes are discussed in the current review article together with the change of the waste policy that was implemented in the EU during the last years.

  1. 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.

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

    Science.gov (United States)

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

    2011-01-01

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

  3. 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.

  4. 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.

  5. Green chemicals : A Kinetic Study on the Conversion of Glucose to Levulinic Acid

    NARCIS (Netherlands)

    Girisuta, B.; Janssen, L.P.B.M.; Heeres, H.J.

    2006-01-01

    Levulinic acid has been identified as a promising green, biomass derived platform chemical. A kinetic study on one of the key steps in the conversion of biomass to levulinic acid, i.e., the acid catalysed decomposition of glucose to levulinic acid has been performed. The experiments were performed

  6. Pd(OAc)2/DPPF-catalysed microwave-assisted cyanide-free ...

    Indian Academy of Sciences (India)

    Pd(OAc)2/DPPF-catalysed microwave-assisted cyanide-free synthesis of aryl nitriles. DINESH N SAWANT and BHALCHANDRA M BHANAGE. ∗. Department of Chemistry, Institute of Chemical Technology, Matunga, Mumbai 400 019, India e-mail: bhalchandra_bhanage@yahoo.com. MS received 13 April 2013; revised 27 ...

  7. 2/DPPF-catalysed microwave-assisted cyanide-free synthesis of aryl ...

    Indian Academy of Sciences (India)

    This study reports microwave-assisted cyanide-free synthesis of aryl nitriles from aryl halides using palladium ... protocol for cyanation of aryl halides using potas- .... eReaction by conventional heating. Figure 2. Structure of ligands from L1–L5. Table 2. Influence of Lewis acids.a. No. Lewis acids (mmol). Yield 3a (%)b. 1.

  8. A facile, solvent and catalyst free, microwave assisted one pot synthesis of hydrazinyl thiazole derivatives

    Directory of Open Access Journals (Sweden)

    D. Chinnaraja

    2015-03-01

    Full Text Available A rapid synthesis of hydrazinyl thiazoles under solvent and catalyst free condition is reported within 30 s. A series of aryl ketones/4-benzoyl pyridine thiosemicarbazone, thiosemicarbazide and α-haloketones were used. This is an environmentally benign microwave assisted and efficient method for rapid synthesis of hydrazinyl thiazoles.

  9. Microwave-assisted polyol synthesis of copper nanocrystals without using additional protective agents

    OpenAIRE

    KAWASAKI, Hideya; KOSAKA, Yuka; MYOUJIN, Yuki; NARUSHIMA, Takashi; YONEZAWA, Tetsu; ARAKAWA, Ryuichi

    2011-01-01

    We report the synthesis of 2 nm copper nanocrystals (Cu NCs)via a microwave-assisted polyol method without using additional protective and reducing agents. The Cu NCs are oxidation resistant and exhibit photoluminescence and highly stableproperties in a colloidal dispersion.

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

    Science.gov (United States)

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

  11. 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...

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

    Science.gov (United States)

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

  13. Microwave-assisted silica-promoted solvent-free synthesis of ...

    Indian Academy of Sciences (India)

    Vol. 125, No. 4, July 2013, pp. 807–811. c Indian Academy of Sciences. Microwave-assisted silica-promoted solvent-free synthesis of triazoloquinazolinone and benzimidazoquinazolinones. G KRISHNAMURTHY. ∗ and K V JAGANNATH. Department of Studies in Chemistry, Central College Campus, Bangalore University,.

  14. 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...

  15. Microwave-assisted synthesis and biological evaluation of novel uracil derivatives inhibiting human thymidine phosphorylase.

    Science.gov (United States)

    Corelli, Federico; Botta, Maurizio; Lossani, Andrea; Pasquini, Serena; Spadari, Silvio; Focher, Federico

    2004-12-01

    New 5-chloro-6-substituted-uracil derivatives have been prepared by microwave assisted-synthesis and tested in vitro as thymidine phosphorylase inhibitors. One of these compounds showed potent inhibitory activity, with an IC50 value in the submicromolar range. The biological activity of the new compounds is discussed in terms of structure-activity relationship.

  16. 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.

  17. Microwave-assisted synthesis and photoluminescence properties of ...

    Indian Academy of Sciences (India)

    ... at 500 nm, under excitation wavelength of 357 nm, exhibiting luminescence propertiestypically observed for Pb 2 + . Effect of concentration of Pb 2 + ions on emission intensity was studied. The colour co-ordinates of prepared phosphor were calculated and found to lie in the green region of Commission Internationale de ...

  18. Rapid tea catechins and caffeine determination by HPLC using microwave-assisted extraction and silica monolithic column.

    Science.gov (United States)

    Rahim, A A; Nofrizal, S; Saad, Bahruddin

    2014-03-15

    A rapid reversed-phase high performance liquid chromatographic method using a monolithic column for the determination of eight catechin monomers and caffeine was developed. Using a mobile phase of water:acetonitrile:methanol (83:6:11) at a flow rate of 1.4 mL min(-1), the catechins and caffeine were isocratically separated in about 7 min. The limits of detection and quantification were in the range of 0.11-0.29 and 0.33-0.87 mg L(-1), respectively. Satisfactory recoveries were obtained (94.2-105.2 ± 1.8%) for all samples when spiked at three concentrations (5, 40 and 70 mg L(-1)). In combination with microwave-assisted extraction (MAE), the method was applied to the determination of the catechins and caffeine in eleven tea samples (6 green, 3 black and 2 oolong teas). Relatively high levels of caffeine were found in black tea, but higher levels of the catechins, especially epigallocatechin gallate (EGCG) were found in green teas. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. 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 produc...

  20. Microwave-assisted nitroxide-mediated miniemulsion polymerization of styrene

    International Nuclear Information System (INIS)

    Li Jieai; Zhu Xiulin; Zhu Jian; Cheng Zhenping

    2007-01-01

    Nitroxide-mediated free-radical miniemulsion polymerizations (NMRPs) of styrene were successfully performed under microwave irradiation at 135 o C. The polymerizations proceeded in a controlled manner, yielding polymers that showed an incremental increase in molecular weight with conversion and had narrow molecular weight distributions. The resulting latexes were colloidally stable. The polymerization behavior, molecular weights of polymers and Z-average size of latex particles were also investigated under two different heating methods, microwave irradiation and conventional heating

  1. Facile synthesis of brownmillerite-type oxides Ba2In2-xMnxO5+x through a microwave-assisted process

    Science.gov (United States)

    Jiang, Peng; Xiao, Ting; Zhou, Yuncheng; Kuang, Jianlei; Wang, Qi; Cao, Wenbin

    2017-03-01

    Brownmillerite-type oxides Ba2In2-xMnxO5+x (0 ≤x ≤ 0.6) samples showing intense turquoise to green color were synthesized through a novel microwave assisted rapid sintering method. The properties of as-synthesized samples were compared with samples prepared by previously reported solid state reaction by X-ray diffraction, scanning electronic microscopy, UV-visible absorbance spectra and X-ray photoelectron spectroscopy. The X-ray diffraction patterns showed that the structure symmetry converts from orthorhombic to cubic with the increase in Mn content. And UV-visible absorbance spectra revealed that the color is tuned from turquoise to green color by manganese doping. In the as-synthesized samples, manganese is showing Mn5+ according to the X-ray photoelectron spectroscopy results.

  2. Microwave-assisted synthesis of chromenes: biological and chemical importance.

    Science.gov (United States)

    Patil, Shivaputra A; Patil, Siddappa A; Patil, Renukadevi

    2015-01-01

    Chromenes constitute chemically important class of heterocyclic compounds having diverse biological and chemical importance. Development of environmentally benign, efficient and economical methods for the synthesis of chromenes remains a significant challenge in synthetic chemistry. The synthesis of chromenes, therefore, has attracted enormous attention from medicinal and organic chemists. Researchers have embraced the concepts of microwave (high speed) synthesis to produce biologically and chemically important chromenes in a time sensitive manner. This review will summarize the recent biological applications such as anticancer, antimicrobial, neurodegenerative and insecticidal activity of new chromenes prepared via microwave irradiation. The development of new methodologies for the synthesis of chromenes including green chemistry processes has also been discussed.

  3. 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

    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...

  4. Novel microwave-assisted solvothermal synthesis of NaYF4:Yb,Er upconversion nanoparticles and their application in cancer cell imaging.

    Science.gov (United States)

    Mi, Congcong; Tian, Zhenhuang; Cao, Can; Wang, Zhijia; Mao, Chuanbin; Xu, Shukun

    2011-12-06

    This work reports the novel microwave-assisted solvothermal synthesis and structural, topographic, spectroscopic characterization of NaYF(4):Yb,Er upconversion nanoparticles (UCNPs) as well as their application in the labeling of HeLa cells. The nanoparticles were prepared in ethylene glycol, with rare earth acetates as precursor and NH(4)F and NaCl as the fluorine and sodium sources. X-ray diffraction, transmission electron microscopy, and luminescence spectroscopy were applied to characterize the nanoparticles. Experimental results showed that the microwave-assisted solvothermal method is an effective approach to create highly crystalline, strongly luminescent UCNPs at a lower temperature (160 °C) and within a significantly shortened reaction time (only 1 h) compared to the traditional methods. The effect of fluorine source on the optical properties of UCNPs was investigated by using NH(4)F, NH(4)HF(2), NaF, and 1-butyl-3-methylimidazolium tetrafluoroborate (BmimBF(4)) as different fluorine sources; NH(4)F proved to be the best one, making the luminescent intensity increase at least 2 orders of magnitude. The UCNPs with four different colors (green, yellow, orange, and cyan) were successfully obtained. After being modified with amino groups and coupled with CEA-8 antibody, the obtained nanoparticles were successfully applied in the specific fluorescent immunolabeling and imaging of HeLa cells to further verify their function as a marker in immunolabeling. © 2011 American Chemical Society

  5. Rapid and Energy-Saving Microwave-Assisted Solid-State Synthesis of Pr(3+)-, Eu(3+)-, or Tb(3+)-Doped Lu2O3 Persistent Luminescence Materials.

    Science.gov (United States)

    Pedroso, Cássio C S; Carvalho, José M; Rodrigues, Lucas C V; Hölsä, Jorma; Brito, Hermi F

    2016-08-03

    Persistent luminescence materials Lu2O3:R(3+),M (Pr,Hf(IV); Eu; or Tb,Ca(2+)) were successfully and rapidly (22 min) prepared by microwave-assisted solid-state synthesis (MASS) using a carbon microwave susceptor and H3BO3 as flux. Reaction times are reduced by up to 93% over previous synthetic methods, without special gases application and using a domestic microwave oven. All materials prepared with H3BO3 flux exhibit LuBO3 impurities that were quantified by Rietveld refinement from synchrotron radiation X-ray powder diffraction patterns. The flux does not considerably affect the crystalline structure of the C-Lu2O3, however. Scanning electron micrographs suggest low surface area when H3BO3 flux is used in the materials' synthesis, decreasing the amount of surface hydroxyl groups in Lu2O3 and improving the luminescence intensity of the phosphors. The carbon used as the susceptor generates CO gas, leading to complete reduction of Tb(IV) to Tb(3+) and partial conversion of Pr(IV) to Pr(3+) present in the Tb4O7 and Pr6O11 precursors, as indicated by X-ray absorption near-edge structure data. Persistent luminescence spectra of the materials show the red/near-IR, reddish orange, and green emission colors assigned to the 4f(n) → 4f(n) transitions characteristics of Pr(3+), Eu(3+), and Tb(3+) ions, respectively. Differences between the UV-excited and persistent luminescence spectra can be explained by the preferential persistent luminescence emission of R(3+) ion in the S6 site rather than R(3+) in the C2 site. In addition, inclusion of Hf(IV) and Ca(2+) codopants in the Lu2O3 host increases the emission intensity and duration of persistent luminescence due to generation of traps caused by charge compensation in the lattice. Photonic materials prepared by MASS with H3BO3 flux show higher persistent luminescence performance than those prepared by the ceramic method or MASS without flux. Color tuning of persistent luminescence in Lu2O3:R(3+),M provides potential

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

    Science.gov (United States)

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

    2016-02-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

  8. 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.

  9. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

    International Nuclear Information System (INIS)

    Cao, Wenqian; Chen, Zhi; Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng; Zhu, Yuxiang; Qin, Laishun; Wang, Jiangying; Huang, Yuexiang

    2016-01-01

    This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO 3 could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO 3 by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

  11. 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). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

    2016-01-01

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

  13. Fast and versatile microwave-assisted intramolecular Heck reaction in peptide macrocyclization using microwave energy.

    Science.gov (United States)

    Byk, Gerardo; Cohen-Ohana, Mirit; Raichman, Daniel

    2006-01-01

    We have revisited the intramolecular Heck reaction and investigated the microwave-assisted macrocyclization on preformed peptides using a model series of ring-varying peptides acryloyl-Gly-[Gly](n)-Phe(4-I)NHR; n = 0-4. The method was applied to both solution and solid supported cyclizations. We demonstrate that the intramolecular Heck reaction can be performed in peptides both in solution and solid support using a modified domestic microwave within 1 to 30 minutes in DMF under reflux with moderate yields ranging from 15 to 25% for a scale between 2-45 mg of linear precursors. The approach was applied to the synthesis of a constrained biologically relevant peptidomimetic bearing an Arg-Gly-Asp (RGD) sequence. These results make the microwave-assisted Heck reaction an attractive renovated approach for peptidomimetics. Copyright 2006 Wiley Periodicals, Inc.

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

    Science.gov (United States)

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

    2017-06-01

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

  15. Microwave-assisted three-component domino reaction: Synthesis of indolodiazepinotriazoles

    Directory of Open Access Journals (Sweden)

    Rajesh K. Arigela

    2013-02-01

    Full Text Available A microwave-assisted three-component protocol involving N-1 alkylation of 2-alkynylindoles with epichlorohydrin, ring opening of the epoxide with sodium azide, and an intramolecular Huisgen azide–internal alkyne 1,3-dipolar cycloaddition domino sequence has been described. The efficacy of the methodology has been demonstrated by treating various 2-alkynylindoles (aromatic/aliphatic with epichlorohydrin and sodium azide furnishing annulated tetracyclic indolodiazepinotriazoles in satisfactory yields.

  16. Microwave-assisted pyrolysis of HDPE using an activated carbon bed

    OpenAIRE

    Russell, Alan Donald

    2013-01-01

    Plastics play an enormous role in modern manufacturing, but the extraction and refining of raw materials, followed by the synthesis of plastics themselves, represents an enormous energy investment into a product that is all too often simply “thrown away” into a landfill after a single use. Microwave-assisted pyrolysis is a recycling technique that allows the recovery of chemical value from plastic waste by breaking down polymers into useful smaller hydrocarbons using microwave heat in the abs...

  17. Microwave-Assisted Extraction of Essential Oil from Eucalyptus: Study of the Effects of Operating Conditions

    OpenAIRE

    A.A. Saoud; R.M. Yunus; R.A. Aziz

    2006-01-01

    Classical extraction of essential oil such as Soxhlet and steam distillation is still a formidable and time-solvent consuming. Microwave assisted process (MAP) is used to accelerate the extraction process of target compounds. It can be used for the extraction of compounds from various plants and animal tissues, or the extraction of undesirable components from raw materials. The investigation of microwave extraction of eucalyptus (globules ) essential oil using ethanol as solvent was carried o...

  18. 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... 1CSIR Materials Science and Manufacturing, PO Box, 395, Pretoria 0001, South Africa boboiriencsir.co.za 2Tshwane University of Technology, Department of Polymer Technology, Pretoria South Africa Abstract Fluidised bed gasification (FBG...

  19. Microwave-Assisted Alkylation of [CB11H12]- and Related Anions

    Czech Academy of Sciences Publication Activity Database

    Valášek, Michal; Štursa, Jan; Pohl, Radek; Michl, Josef

    2010-01-01

    Roč. 49, č. 22 (2010), s. 10247-10254 ISSN 0020-1669 R&D Projects: GA AV ČR IAA400550708; GA ČR GC203/09/J058 Grant - others:AV ČR(CZ) M200550906 Institutional research plan: CEZ:AV0Z40550506 Keywords : carboranes * organometallics * microwave assisted synthesis Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.326, year: 2010

  20. Microwave assisted polyol synthesis of CuGaSe2 nanoparticles for solar cell application

    Science.gov (United States)

    Grevtsev, A. S.; Levin, O. V.; Tverjanovich, A. S.

    Chalcopyrite CuGaSe2 nanocrystals with average size about 90 nm were synthesized by quick and cheap microwave assisted polyol method without special dissolving of Se in organic solvents. Composition, structure and optical properties of the obtained particles correspond to pure bulk CuGaSe2. CuGaSe2/PCBM composite films produced from the synthesized nanoparticles possess reproducible photovoltaic response.

  1. [Determination of trace heavy metal elements in cortex Phellodendron chinense by ICP-MS after microwave-assisted digestion].

    Science.gov (United States)

    Kou, Xing-Ming; Xu, Min; Gu, Yong-Zuo

    2007-06-01

    An inductively coupled plasma mass spectrometry (ICP-MS) for determination of the contents of 8 trace heavy metal elements in cortex Phellodendron chinense after microwave-assisted digestion of the sample has been developed. The accuracy of the method was evaluated by the analysis of corresponding trace heavy metal elements in standard reference materials (GBW 07604 and GBW 07605). By applying the proposed method, the contents of 8 trace heavy metal elements in cortex Phellodendron chinense cultivated in different areas (in Bazhong, Yibin and Yingjing, respectively) of Sichuan and different growth period (6, 8 and 10 years of samples from Yingjing) were determined. The relative standard deviation (RSD) is in the range of 3.2%-17.8% and the recoveries of standard addition are in the range of 70%-120%. The results of the study indicate that the proposed method has the advantages of simplicity, speediness and sensitivity. It is suitable for the determination of the contents of 8 trace heavy metal elements in cortex Phellodendron chinense. The results also show that the concentrations of 4 harmful trace heavy metal elements As, Cd, Hg and Pb in cortex Phellodendron chinense are all lower than the limits of Chinese Pharmacopoeia and Green Trade Standard for Importing and Exporting Medicinal Plant and Preparation. Therefore, the cortex Phellodendron chinense is fit for use as medicine and export.

  2. Optimization of the recovery of high-value compounds from pitaya fruit by-products using microwave-assisted extraction.

    Science.gov (United States)

    Ferreres, Federico; Grosso, Clara; Gil-Izquierdo, Angel; Valentão, Patrícia; Mota, Ana T; Andrade, Paula B

    2017-09-01

    A green microwave-assisted extraction of high value-added compounds from exotic fruits' peels was optimized by Box-Behnken design using 3 factors: solid/solvent ratio, X 1 , temperature, X 2 , and extraction time, X 3 . By using Derringer's desirability function, optimum extraction yields are obtained with X 1 =1/149.95g/mL, X 2 =72.27°C and X 3 =39.39min (white-fleshed red pitaya) and X 1 =1/148.96g/mL, X 2 =72.56°C and X 3 =5.02min (yellow pitaya) and a maximum betacyanin content is achieved with X 1 =1/150g/mL, X 2 =49.33°C and X 3 =5min. None of the factors influenced the extraction of phenolic compounds. Eighteen cinnamoyl derivatives, 17 flavonoid derivatives and 4 betacyanins were identified by HPLC-DAD-ESI/MS n , 23 and 15 new compounds being described in yellow and white-fleshed red pitayas, respectively. These results indicate that it is possible to reuse these by-products to recover compounds for food and pharmaceutical industries. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Microwave assisted one-pot catalyst free green synthesis of new methyl-7-amino-4-oxo-5-phenyl-2-thioxo-2,3,4,5-tetrahydro-1H-pyrano[2,3-d]pyrimidine-6-carboxylates as potent in vitro antibacterial and antifungal activity

    Directory of Open Access Journals (Sweden)

    Ajmal R. Bhat

    2015-11-01

    Full Text Available An efficiently simple protocol for the synthesis of methyl 7 amino-4-oxo-5-phenyl-2-thioxo-2, 3, 4,5-tetrahydro-1H-pyrano[2,3-d]pyrimidine-6-carboxylates via one-pot three component condensation pathway is established via microwave irradiation using varied benzaldehyde derivatives, methylcyanoacetate and thio-barbituric acid in water as a green solvent. A variety of functionalized substrates were found to react under this methodology due to its easy operability and offers several advantages like, high yields (78–94%, short reaction time (3–6 min, safety and environment friendly without used any catalyst. The synthesized compounds (4a–4k showed comparatively good in vitro antimicrobial and antifungal activities against different strains. The Compounds 4a, 4b, 4c, 4d 4e and 4f showed maximum antimicrobial activity against Staphylococcus aureus, Bacillus cereus (gram-positive bacteria, Escherichia coli, Klebshiella pneumonia, Pseudomonas aeruginosa (gram-negative bacteria. The synthesized compound 4f showed maximum antifungal activity against Aspergillus Niger and Penicillium chrysogenum strains. Streptomycin is used as standard for bacterial studies and Mycostatin as standards for fungal studies. Structure of all newly synthesized products was characterized on the basis of IR, 1H NMR, 13C NMR and mass spectral analysis.

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

    Science.gov (United States)

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

    2017-01-01

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

  5. Preparation of silica nanoparticles through microwave-assisted acid-catalysis.

    Science.gov (United States)

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

    2013-12-16

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

  6. 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.

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

    Directory of Open Access Journals (Sweden)

    Magdalena Montowska

    2016-01-01

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

  8. Determination of 90Sr in environmental samples by microwave assisted digestion - chromatographic separation

    International Nuclear Information System (INIS)

    Torres, J.M.; Llaurado, M.; Rauret, G.

    1998-01-01

    The stages involved in the determination of 90 Sr in environmental samples are: sample attack, radiochemical separation (of both 90 Sr and its progeny 90 Y) and measurement. For the determination of 90 Sr, the introduction of microwave-assisted digestion methods has improved acid attack by drastically decreasing both digestion time and the volume of acidic reagents. Recent studies describe many applications of microwave-assisted methods for the determination of inorganic and organometallic compounds in several matrices. We have recently studied the microwave-assisted digestion of soils for the 90 Sr determination. The presented work extends the application of microwaves for the 90 Sr determination to other environmental samples such as sediments, vegetation and milk. An open-focused microwave system, which accepts large samples intakes usually required for radioanalytical chemistry due to the low level content of radionuclides in environmental samples, was used. This system can handle up to 10 g of sample intake which, in many cases, is enough to have acceptable limits of detection. Different digestion procedures are optimised for each matrix studied, paying special attention to the microwave power, the time of digestion and the volume of acidic reagents. Once the sample is in solution a new separation procedure using a specific resin -Sr.Spec- is applied and the measurement is performed by liquid scintillation. The results obtained are compared with a previously optimised method based on liquid-liquid extraction of 90 Y and Cerenkov radiation measurement

  9. Simulation of energetic- and exergetic performance of microwave-assisted fluidized bed drying of soybeans

    International Nuclear Information System (INIS)

    Ranjbaran, M.; Zare, D.

    2013-01-01

    The performance of microwave-assisted fluidized bed drying of soybeans was simulated (using a previously validated mathematical model) and analyzed based on the first- and second law of thermodynamics. The energy and exergy analysis were carried out for several drying conditions. The effects of inlet air temperature, microwave power density, bed thickness and inlet air velocity on the efficiencies and inefficiencies of drying process have been simulated and discussed. Generally, application of microwave energy during fluidized bed drying enhanced the exergy efficiency of drying process. However, the results showed that it was more efficient not to apply microwave energy at the first stage of fluidized bed drying process. The application of higher levels of drying air temperature led in higher exergy efficiencies. The values of mean relative deviations for the predictions of efficiencies and inefficiencies of drying process were less than 14%, compared with those calculated using experimental data. - Highlights: • Introducing a mathematical model to predict the efficiency of microwave-assisted fluidized bed dryers. • Energy and exergy analysis in microwave-assisted fluidized bed drying of grains. • Providing practical recommendations for efficient use of microwave power during drying

  10. Conversing about Citrus Greening: Extension's Role in Educating about Genetic Modification Science as a Solution

    Science.gov (United States)

    Ruth, Taylor K.; Lamm, Alexa J.; Rumble, Joy N.; Ellis, Jason D.

    2017-01-01

    Extension agents across the nation will need to facilitate difficult conversations with the public if genetic modification (GM) science is used to combat citrus greening disease. This study used the innovation characteristics described by Rogers to explore if using GM science as a solution to citrus greening had diffused amongst US residents. An…

  11. 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

  12. EDITORIAL: Non-thermal plasma-assisted fuel conversion for green chemistry Non-thermal plasma-assisted fuel conversion for green chemistry

    Science.gov (United States)

    Nozaki, Tomohiro; Gutsol, Alexander

    2011-07-01

    This special issue is based on the symposium on Non-thermal Plasma Assisted Fuel Conversion for Green Chemistry, a part of the 240th ACS National Meeting & Exposition held in Boston, MA, USA, 22-26 August 2010. Historically, the Division of Fuel Chemistry of the American Chemical Society (ACS) has featured three plasma-related symposia since 2000, and has launched special issues in Catalysis Today on three occasions: 'Catalyst Preparation using Plasma Technologies', Fall Meeting, Washington DC, USA, 2000. Special issue in Catalysis Today 72 (3-4) with 12 peer-reviewed articles. 'Plasma Technology and Catalysis', Spring Meeting, New Orleans, LA, USA, 2003. Special issue in Catalysis Today 89 (1-2) with more than 30 peer-reviewed articles. 'Utilization of Greenhouse Gases II' (partly focused on plasma-related technologies), Spring Meeting, Anaheim, CA, USA, 2004. Special issue in Catalysis Today 98 (4) with 25 peer-reviewed articles. This time, selected presentations are published in this Journal of Physics D: Applied Physics special issue. An industrial material and energy conversion technology platform is established on thermochemical processes including various catalytic reactions. Existing industry-scale technology is already well established; nevertheless, further improvement in energy efficiency and material saving has been continuously demanded. Drastic reduction of CO2 emission is also drawing keen attention with increasing recognition of energy and environmental issues. Green chemistry is a rapidly growing research field, and frequently highlights renewable bioenergy, bioprocesses, solar photocatalysis of water splitting, and regeneration of CO2 into useful chemicals. We would also like to emphasize 'plasma catalysis' of hydrocarbon resources as an important part of the innovative next-generation green technologies. The peculiarity of non-thermal plasma is that it can generate reactive species almost independently of reaction temperature. Plasma

  13. Structural and optical characterization of CuInS2 quantum dots synthesized by microwave-assisted continuous flow methods

    International Nuclear Information System (INIS)

    Fitzmorris, Robert C.; Oleksak, Richard P.; Zhou, Zheng; Mangum, Benjamin D.; Kurtin, Juanita N.; Herman, Gregory S.

    2015-01-01

    Semiconductor quantum dots (QDs) have recently been incorporated into consumer displays and lighting technologies. Now that these materials are being produced on industrial scales, it is important to investigate scalable synthetic methods and less toxic materials and chemistries. To achieve these goals, we have synthesized cadmium-free, visible light-emitting QDs using a microwave-assisted continuous flow reactor. After synthesis, the CuInS 2 QD cores underwent a near-complete Zn cation exchange reaction in a batch reactor, followed by the growth of a ZnS shell. Analysis of X-ray diffraction, transmission electron microscopy, and Raman spectroscopy data indicate that the crystal structure changes from CuInS 2 (chalcopyrite) to ZnS (zincblende) during the cation exchange reaction. Compositional analysis indicated that the core/shell QDs were ∼98 % ZnS, with Cu and In present at much lower concentrations. The photoluminescence (PL) peak position was blue shifted for longer cation exchange reactions, and it was found that the ZnS shell was necessary for improved PL stability. The synthesized QDs have a PL down conversion efficiency of ∼65 % when using a blue LED source

  14. Green chemicals: A Kinetic Study on the Conversion of Glucose to Levulinic Acid

    OpenAIRE

    Girisuta, B.; Janssen, L.P.B.M.; Heeres, H.J.

    2006-01-01

    Levulinic acid has been identified as a promising green, biomass derived platform chemical. A kinetic study on one of the key steps in the conversion of biomass to levulinic acid, i.e., the acid catalysed decomposition of glucose to levulinic acid has been performed. The experiments were performed in a broad temperature window (140–200°C), using sulphuric acid as the catalyst (0.05–1 M) and a initial glucose concentration between 0.1 and 1 M. A kinetic model of the reaction sequence was devel...

  15. 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.

  16. Photocatalytic perfermance of sandwich-like BiVO{sub 4} sheets by microwave assisted synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Suqin, E-mail: liusuqin888@126.com [Department of Chemical engineering and Food Science, Hubei University of arts and science, Xiangyang 441053 (China); Hubei Key Laboratory of Low Dimensional Optoelectronic Materials and Devices, Xiangyang 441053 (China); Tang, Huiling; Zhou, Huan [Department of Chemical engineering and Food Science, Hubei University of arts and science, Xiangyang 441053 (China); Dai, Gaopeng, E-mail: dgp2000@126.com [Department of Chemical engineering and Food Science, Hubei University of arts and science, Xiangyang 441053 (China); Wang, Wanqiang [Department of Chemical engineering and Food Science, Hubei University of arts and science, Xiangyang 441053 (China)

    2017-01-01

    Graphical abstract: Sandwich-like BiVO{sub 4} sheets were successfully synthesized via a facile microwave-assisted method. The as-prepared samples exhibit a high activity for the degradation of methyl orange under visible light irradiation. - Highlights: • Sandwich-like BiVO{sub 4} sheets were synthesized by a facile microwave-assisted method. • The presence of PEG-10000 plays a critical role in the formation of BiVO{sub 4} sheets. • Ostwald ripening is the primary driving force for the formation of sandwich-like BiVO{sub 4}. • The sandwich-like BiVO{sub 4} sheets exhibit a high visible-light photocatalytic activity. - Abstract: Sandwich-like BiVO{sub 4} 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, N{sub 2} 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 BiVO{sub 4} sheets, and Ostwald ripening is the primary driving force for the formation of sandwich-like structures. The sandwich-like BiVO{sub 4} 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 BiVO{sub 4} sheets can be attributed to its large surface area over the irregular BiVO{sub 4} particles.

  17. 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.

  18. Carbohydrate conjugation through microwave-assisted functionalization of single-walled carbon nanotubes using perfluorophenyl azides.

    Science.gov (United States)

    Kong, Na; Shimpi, Manishkumar R; Ramström, Olof; Yan, Mingdi

    2015-03-20

    Carbohydrate-functionalized single-walled carbon nanotubes (SWNTs) were synthesized using microwave-assisted reaction of perfluorophenyl azide with the nanotubes. The results showed that microwave radiation provides a rapid and effective means to covalently attach carbohydrates to SWNTs, producing carbohydrate-SWNT conjugates for biorecognition. The carbohydrate-functionalized SWNTs were furthermore shown to interact specifically with cognate carbohydrate-specific proteins (lectins), resulting in predicted recognition patterns. The carbohydrate-presenting SWNTs constitute a new platform for sensitive protein- or cell recognition, which pave the way for glycoconjugated carbon nanomaterials in biorecognition applications. Copyright © 2014 Elsevier Ltd. All rights reserved.

  19. 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.

  20. Microwave-Assisted Extraction of Essential Oil from Eucalyptus: Study of the Effects of Operating Conditions

    Directory of Open Access Journals (Sweden)

    A.A. Saoud

    2006-12-01

    Full Text Available Classical extraction of essential oil such as Soxhlet and steam distillation is still a formidable and time-solvent consuming. Microwave assisted process (MAP is used to accelerate the extraction process of target compounds. It can be used for the extraction of compounds from various plants and animal tissues, or the extraction of undesirable components from raw materials. The investigation of microwave extraction of eucalyptus (globules essential oil using ethanol as solvent was carried out. The influence of material (eucalyptus/solvent (ethanol ratio, required doses of microwave, and time of microwave exposure on extraction efficiency, was studied.

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

    International Nuclear Information System (INIS)

    Ndiege, Nicholas; Subramanian, Vaidyanathan; Shannon, Mark A.; Masel, Richard I.

    2008-01-01

    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 μm 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 2 H 5 ) 5 ) vapor on the deposition surface

  2. 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...... amines and both ortho- and para-substituted arylo-backbones. By utilizing this optimized protocol a complex nonameric arylopeptoid was synthesized in less than 11 h, featuring a novel alternating ortho-, meta-, and para-substituted backbone pattern and a variety of chemically diverse and challenging side...

  3. Room temperature microwave-assisted recording on 500-Gbpsi-class perpendicular medium

    Science.gov (United States)

    Nozaki, Y.; Ishida, N.; Soeno, Y.; Sekiguchi, K.

    2012-10-01

    Microwave-assisted recording on a 500-Gbpsi-class perpendicular medium was experimentally demonstrated at room temperature. Magnetization reversal under a radio-frequency magnetic field was measured by an electrically shorted coplanar waveguide, which enabled us to evaluate the change in the medium's ferromagnetic resonance spectrum. A frequency-dependent reduction in the switching field was clearly observed in response to a microwave impulse 50 ns in duration. A significant reduction of up to 30% in the coercive field was achieved by applying a microwave impulse with an amplitude of 25 dBm and a frequency of 15 GHz.

  4. 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.

  5. Green and solvent-free procedure for microwave-assisted synthesis ...

    Indian Academy of Sciences (India)

    istry. The pyridyl heterocyclic nucleus is a building block in molecules of natural products, pharmaceuti- cals such as vasodilator, anticonvulsant, antiepileptic, anaesthetic and agrochemicals such as pesticides and herbicidals.6–9 Owing to their π-stacking ability, direc- tional H-bonding and coordination, triarylpyridines are.

  6. Microwave-Assisted Synthesis of 5-Phenyl-2-Hydroxyacetophenone Derivatives by a Green Suzuki Coupling Reaction

    Science.gov (United States)

    Soares, Pedro; Fernandes, Carlos; Chavarria, Daniel; Borges, Fernanda

    2015-01-01

    In recent years, the use of boron-containing reagents in palladium-assisted C-C coupling reactions (the Suzuki reaction) has gained prominence due to the vast array of reagents commercially available. Consequently, the generation of carbon-carbon bonds, namely of functionalized biphenyl systems, is at present considered the backbone of organic…

  7. Green and solvent-free procedure for microwave-assisted synthesis ...

    Indian Academy of Sciences (India)

    Design and development of a heterogeneous nanocatalyst for condensation reaction of acetophenone derivatives, aromatic aldehydes, and ammonium acetate to yield 2,4,6-triarylpyridines followed by microwave irradiation is described. Nanocrystalline MgAl2O4 as a novel heterogeneous recyclable catalyst shows high ...

  8. Microwave assisted green synthesis and characterization of silver/montmorillonite heterostructures with improved antimicrobial properties

    CSIR Research Space (South Africa)

    Kesavan Pillai, Sreejarani

    2013-10-01

    Full Text Available and environmentally friendly. The MW process yielded Mt surfaces with uniformdistribution of Ag nanoparticleswith an average size of 8–10 nm. The presence of reducing agents was found to inhibit the formation of Ag nanoparticles inMWsynthesis. The method was also...

  9. Enhanced visible-light-responsive photodegradation of bisphenol A by Cu, N-codoped titanate nanotubes prepared by microwave-assisted hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Doong, Ruey-an, E-mail: radoong@nctu.edu.tw [Institute of Environmental Engineering, National Chiao Tung University, Hsinchu 30010, Taiwan (China); Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Liao, Chun-Yi [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

    2017-01-15

    Highlights: • The Cu, N-codoped TNTs were prepared by microwave assisted hydrothermal method. • The Cu(0) in codoped TNTs can serve as electron donors as well as electron meditors. • The surface normalized rate constants for BPA removal by Cu, N-TNT were 1.5–4.3 times higher than that of P25 TiO{sub 2}. • The Cu, N-codoped TNTs prolonged the generation of radicals for at least 5 min. - Abstract: In this study, a rapid and effective microwave-assisted hydrothermal method was developed for the synthesis of Cu, N-codoped titanate nanotubes (Cu, N-TNTs) to enhance the photocatalytic degradation efficiency and rate of bisphenol A (BPA) under UV and visible light irradiations. The TNTs were first synthesized at 150 °C for 3 h under microwave heating conditions followed by the calcination at 450 °C in the presence of 6 wt% Cu ions and N{sub 2}/NH{sub 3} to fabricate Cu, N-TNTs composites. The Cu, N-TNTs exhibited excellent photocatalytic activity toward BPA degradation under UV and visible light irradiations. The X-ray photoelectron spectra indicated that Cu species in Cu, N-TNTs were mainly in zerovalent form and could serve as the electron donors as well as shuttling species to accelerate the photodegradation of BPA. In addition, the nitrogen atoms were incorporated into the anatase lattices to increase the visible-light-responsive capability. The surface normalized reaction rate constants for BPA degradation were 4.3 and 1.5 times higher than those of Degussa P25 TiO{sub 2} under UV and visible light irradiations, respectively. The electron spin resonance spectra showed that Cu, N-codoped TNTs prolonged the generation of oxygen-containing radicals for at least 5 min, resulting in the significant enhancement of photodegradation efficiency and rate of BPA. Results obtained in this study open a new avenue by using simple and effective microwave-assisted hydrothermal method to fabricate low dimensional codoped TNTs which can be potentially applied in a wide

  10. Recent advances in heterogeneous catalytic conversion of glucose to 5-hydroxymethylfurfural via green routes

    KAUST Repository

    Wang, Jianjian

    2017-05-12

    With concerns of diminishing fossil fuel reserves and environmental deterioration, great efforts have been made to explore novel approaches of efficiently utilizing bio-renewable feedstocks to produce chemicals and fuels. 5-Hydroxymethylfurfural (HMF), generated from dehydration of six-carbon ketose, is regarded as a primary and versatile renewable building block to realize the goal of production of these high valued products from renewable biomass resources transformation. In this review, we summarize the recent advances via green routes in the heterogeneous reaction system for the catalytic production of HMF from glucose conversion, and emphasize reaction pathways of these reaction approaches based on the fundamental mechanistic chemistry as well as highlight the challenges (such as separation and purification of products, reusing and regeneration of catalyst, recycling solvent) in this field.

  11. Nanotechnology Based Green Energy Conversion Devices with Multifunctional Materials at Low Temperatures.

    Science.gov (United States)

    Lu, Yuzheng; Afzal, Muhammad; Zhu, Bin; Wang, Baoyuan; Wang, Jun; Xia, Chen

    2017-07-10

    Nanocomposites (integrating the nano and composite technologies) for advanced fuel cells (NANOCOFC) demonstrate the great potential to reduce the operational temperature of solid oxide fuel cell (SOFC) significantly in the low temperature (LT) range 300-600ºC. NANOCOFC has offered the development of multi-functional materials composed of semiconductor and ionic materials to meet the requirements of low temperature solid oxide fuel cell (LTSOFC) and green energy conversion devices with their unique mechanisms. This work reviews the recent developments relevant to the devices and the patents in LTSOFCs from nanotechnology perspectives that reports advances including fabrication methods, material compositions, characterization techniques and cell performances. Finally, the future scope of LTSOFC with nanotechnology and the practical applications are also discussed. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

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

    Science.gov (United States)

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

    2014-11-01

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

  13. Improved hydrogen production via thermophilic fermentation of corn stover by microwave-assisted acid pretreatment

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Chun-zhao; Cheng, Xi-yu [National Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100093 (China)

    2010-09-15

    A microwave-assisted acid pretreatment (MAP) strategy has been developed to enhance hydrogen production via thermophilic fermentation of corn stover. Pretreatment of corn stover by combining microwave irradiation and acidification resulted in the increased release of soluble substances and made the corn stover more accessible to microorganisms when compared to thermal acid pretreatment (TAP). MAP showed obvious advantages in short duration and high efficiency of lignocellulosic hydrolysis. Analysis of the particle size and specific surface area of corn stover as well as observation of its cellular microstructure were used to elucidate the enhancement mechanism of the hydrolysis process by microwave assistance. The cumulative hydrogen volume reached 182.2 ml when corn stover was pretreated by MAP with 0.3 N H{sub 2}SO{sub 4} for 45 min, and the corresponding hydrogen yield reached 1.53 mol H{sub 2}/mol-glucose equivalents converted to organic end products. The present work demonstrates that MAP has potential to enhance the bioconversion efficiency of lignocellulosic waste to renewable biofuel. (author)

  14. 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.

  15. 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.

  16. 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.

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

  18. Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

    Directory of Open Access Journals (Sweden)

    E. Aivazoglou

    2018-04-01

    Full Text Available The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG or PEG and β-cyclodextrin (β-CD/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD, Transition Electron Microscopy (TEM, Fourier-transform Infrared Spectroscopy (FTIR, Raman Spectroscopy, Vibrating Sample Magnetometer (VSM, X-Ray Photoelectron Spectroscopy (XPS and Thermal analysis (TG/DSC. The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

  19. Microwave-assisted Olefin Metathesis as Pivotal Step in the Synthesis of Bioactive Compounds.

    Science.gov (United States)

    Etse, Koffi Senam; Ngendera, Alice; Ntumba, Nelly Tshibalonza; Demonceau, Albert; Delaude, Lionel; Dragutan, Ileana; Dragutan, Valerian

    2017-01-01

    Over the last two decades, olefin metathesis has emerged as a new avenue in the design of new routes for the synthesis of natural products and active pharmaceutical ingredients. In many cases, syntheses based on olefin metathesis strategies provide significant routes in terms of increasing the overall yields, improving the synthesis scope, and decreasing the number of steps. On the other hand, over the last decade, microwave-assisted chemistry has experienced an incredible development, which rapidly opened new areas in organic synthesis and in homogeneous catalysis. In this review article, we highlight applications of microwaveheated olefin metathesis reactions as pivotal steps in the total synthesis of biologically active compounds. By drawing selected examples from the recent literature, we aim to illustrate the great synthetic power and variety of metathesis reactions, as well as the beneficial effects of microwave irradiation over conventional heating sources. The majority of the selected applications of microwave-assisted olefin metathesis cover the synthesis of medium-ring cycles, macrocycles, and peptidomimetics by means of ring-closing metathesis (RCM) and crossmetathesis (CM) routes. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  20. 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.

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

    Science.gov (United States)

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

    2015-06-01

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

  2. Microwave-assisted surface modification of metallocene polyethylene for improving blood compatibility.

    Science.gov (United States)

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

    2013-01-01

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

  3. 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.

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

    Directory of Open Access Journals (Sweden)

    Bai-Liang Xue

    2015-02-01

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

  5. Morphological evolution of Bi2Se3 nanocrystalline materials synthesized by microwave assisted solvothermal method

    Science.gov (United States)

    Bera, Sumit; Behera, P.; Mishra, A. K.; Krishnan, M.; Patidar, M. M.; Singh, D.; Gangrade, M.; Venkatesh, R.; Deshpande, U. P.; Phase, D. M.; Ganesan, V.

    2018-04-01

    Structural, morphological and spectroscopic properties of Bi2Se3 nanoparticles synthesized by microwave assisted solvothermal method were investigated systematically. A controlled synthesis of different morphologies by a small variation in synthesis procedure is demonstrated. Powder X-ray diffraction (XRD) confirmed the formation of single phase. Crystallite and particle size reductions were studied with XRD and AFM (Atomic Force Microscopy). Different morphologies such as hexagonal nanoflakes with cross section of around˜6µm, nanoflower and octahedral agglomerated crystals of nearly ˜60 nm size have been observed in scanning electron microscope while varying the microwave assisted synthesis procedures. A significant blue shift observed in diffuse reflectance spectroscopy evidences the energy gap tuning as a result of morphological evolution. The difference in morphology observed in this three fast, facile and scalable synthesis is advantageous for tuning the thermoelectric figure of merit and for probing the surface states of these topological insulators. Low temperature resistivity remains similar for all three variants depicting a 2D character as evidenced by a -lnT term of localization.

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

    Science.gov (United States)

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

    2007-02-28

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

    Kusuma, Heri Septya; Mahfud, Mahfud

    2015-12-01

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

  9. Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

    Science.gov (United States)

    Aivazoglou, E.; Metaxa, E.; Hristoforou, E.

    2018-04-01

    The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG) or PEG and β-cyclodextrin (β-CD)/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD), Transition Electron Microscopy (TEM), Fourier-transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Vibrating Sample Magnetometer (VSM), X-Ray Photoelectron Spectroscopy (XPS) and Thermal analysis (TG/DSC). The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

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

    International Nuclear Information System (INIS)

    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 CO 2 atmosphere under conventional and microwave-assisted heating is investigated to achieve CO 2 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.

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

    Science.gov (United States)

    Quoc, Le Pham Tan; Muoi, Nguyen Van

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Shahid, Robina, E-mail: rkhan@kth.se [Division of Functional Materials, Royal Institute of Technology (KTH), 16440, Kista, Stockholm (Sweden); Toprak, Muhammet S., E-mail: toprak@kth.se [Division of Functional Materials, Royal Institute of Technology (KTH), 16440, Kista, Stockholm (Sweden); Muhammed, Mamoun [Division of Functional Materials, Royal Institute of Technology (KTH), 16440, Kista, Stockholm (Sweden)

    2012-03-15

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

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

    Science.gov (United States)

    Mittal, Vineet; Nanda, Arun

    2017-12-01

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

  14. Shape-control by microwave-assisted hydrothermal method for the synthesis of magnetite nanoparticles using organic additives

    Energy Technology Data Exchange (ETDEWEB)

    Rizzuti, Antonino [Politecnico di Bari, Dipartimento di Ingegneria Civile, Ambientale, del Territorio, Edile e di Chimica (Italy); Dassisti, Michele [Politecnico di Bari, Dipartimento di Meccanica, Management e Matematica (Italy); Mastrorilli, Piero, E-mail: p.mastrorilli@poliba.it [Politecnico di Bari, Dipartimento di Ingegneria Civile, Ambientale, del Territorio, Edile e di Chimica (Italy); Sportelli, Maria C.; Cioffi, Nicola; Picca, Rosaria A. [Università di Bari, Dipartimento di Chimica (Italy); Agostinelli, Elisabetta; Varvaro, Gaspare [Consiglio Nazionale delle Ricerche, Istituto di Struttura della Materia (Italy); Caliandro, Rocco [Consiglio Nazionale delle Ricerche, Istituto di Cristallografia (Italy)

    2015-10-15

    A simple and fast microwave-assisted hydrothermal method is proposed for the synthesis of magnetite nanoparticles. The addition of different surfactants (polyvinylpyrrolidone, oleic acid, or trisodium citrate) was studied to investigate the effect on size distribution, morphology, and functionalization of the magnetite nanoparticles. Microwave irradiation at 150 °C for 2 h of aqueous ferrous chloride and hydrazine without additives resulted in hexagonal magnetite nanoplatelets with a facet-to-facet distance of 116 nm and a thickness of 40 nm having a saturation magnetization of ∼65 Am{sup 2} kg{sup −1}. The use of polyvinylpyrrolidone led to hexagonal nanoparticles with a facet-to-facet distance of 120 nm and a thickness of 53 nm with a saturation magnetization of ∼54 Am{sup 2} kg{sup −1}. Additives such as oleic acid and trisodium citrate yielded quasi-spherical nanoparticles of 25 nm in size with a saturation magnetization of ∼70 Am{sup 2} kg{sup −1} and spheroidal nanoparticles of 60 nm in size with a saturation magnetization up to ∼82 Am{sup 2} kg{sup −1}, respectively. A kinetic control of the crystal growth is believed to be responsible for the hexagonal habit of the nanoparticles obtained without additive. Conversely, a thermodynamic control of the crystal growth, leading to spheroidal nanoparticles, seems to occur when additives which strongly interact with the nanoparticle surface are used. A thorough characterization of the materials was performed. Magnetic properties were investigated by Superconducting Quantum Interference Device and Vibrating Sample magnetometers. Based on the observed magnetic properties, the magnetite obtained using citrate appears to be a promising support for magnetically transportable catalysts.

  15. Shape-control by microwave-assisted hydrothermal method for the synthesis of magnetite nanoparticles using organic additives

    Science.gov (United States)

    Rizzuti, Antonino; Dassisti, Michele; Mastrorilli, Piero; Sportelli, Maria C.; Cioffi, Nicola; Picca, Rosaria A.; Agostinelli, Elisabetta; Varvaro, Gaspare; Caliandro, Rocco

    2015-10-01

    A simple and fast microwave-assisted hydrothermal method is proposed for the synthesis of magnetite nanoparticles. The addition of different surfactants (polyvinylpyrrolidone, oleic acid, or trisodium citrate) was studied to investigate the effect on size distribution, morphology, and functionalization of the magnetite nanoparticles. Microwave irradiation at 150 °C for 2 h of aqueous ferrous chloride and hydrazine without additives resulted in hexagonal magnetite nanoplatelets with a facet-to-facet distance of 116 nm and a thickness of 40 nm having a saturation magnetization of 65 Am2 kg-1. The use of polyvinylpyrrolidone led to hexagonal nanoparticles with a facet-to-facet distance of 120 nm and a thickness of 53 nm with a saturation magnetization of 54 Am2 kg-1. Additives such as oleic acid and trisodium citrate yielded quasi-spherical nanoparticles of 25 nm in size with a saturation magnetization of 70 Am2 kg-1 and spheroidal nanoparticles of 60 nm in size with a saturation magnetization up to 82 Am2 kg-1, respectively. A kinetic control of the crystal growth is believed to be responsible for the hexagonal habit of the nanoparticles obtained without additive. Conversely, a thermodynamic control of the crystal growth, leading to spheroidal nanoparticles, seems to occur when additives which strongly interact with the nanoparticle surface are used. A thorough characterization of the materials was performed. Magnetic properties were investigated by Superconducting Quantum Interference Device and Vibrating Sample magnetometers. Based on the observed magnetic properties, the magnetite obtained using citrate appears to be a promising support for magnetically transportable catalysts.

  16. Microwave assisted in situ synthesis of Ag–NaCMC films and their reproducible surface-enhanced Raman scattering signals

    International Nuclear Information System (INIS)

    Jiang, Tao; Li, Junpeng; Zhang, Li; Wang, Binbing; Zhou, Jun

    2014-01-01

    Graphical abstract: Two kinds of Ag–NaCMC films for surface-enhanced Raman scattering (SERS) were prepared by conventional heating and microwave assisted in situ reduction methods without any additional capping or reducing agents. A relatively narrow and symmetric surface plasmon resonance band was observed in the absorption spectra of the films fabricated by the microwave assisted in situ reduction method. More uniform silver nanoparticles (NPs) implied by the symmetric absorption spectrum were further confirmed by the scanning electron microscopy images. After the simulation of the E-field intensity distribution around the silver NPs in NaCMC film, the Raman scattering enhancement factors (EFs) of these films were then investigated with 4-mercaptobenzoic acid molecule as a SERS reporter. Improved reproducibility of SERS signal was obtained in the microwave assisted synthesized Ag–NaCMC film, although it maintained an EF as only 1.11 × 10 8 . The reproducible SERS signal of the Ag–NaCMC film is particularly attractive and this microwave assisted in situ reduction method is suitable for the production of excellent substrate for biosensor application. - Highlights: • The synthesis of Ag–NaCMC films was successfully fulfilled by a low-cost microwave method. • More uniform silver nanoparticles were observed in Ag–NaCMC film synthesized by microwave. • Improved reproducibility of SERS signal was obtained in microwave synthesized Ag–NaCMC film. - Abstract: Two kinds of Ag–NaCMC films for surface-enhanced Raman scattering (SERS) were prepared by conventional heating and microwave assisted in situ reduction methods without any additional capping or reducing agents. A relatively narrow and symmetric surface plasmon resonance band was observed in the absorption spectra of the films fabricated by the microwave assisted in situ reduction method. More uniform silver nanoparticles (NPs) implied by the symmetric absorption spectrum were further confirmed by

  17. Microwave-assisted synthesis, molecular docking and antitubercular activity of 1,2,3,4-tetrahydropyrimidine-5-carbonitrile derivatives

    Czech Academy of Sciences Publication Activity Database

    Mohan, S. B.; Kumar, B. V. V. R.; Dinda, S. C.; Naik, D.; Seenivasan, S. P.; Kumar, V.; Rana, D. N.; Brahmkshatriya, Pathik

    2012-01-01

    Roč. 22, č. 24 (2012), s. 7539-7542 ISSN 0960-894X Institutional research plan: CEZ:AV0Z40550506 Keywords : antitubercular * binding interactions * luciferase reporter phage (LRP) assay * microwave-assisted * molecular docking Subject RIV: CC - Organic Chemistry Impact factor: 2.338, year: 2012

  18. 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...

  19. 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...

  20. Room Temperature Magnetic Behavior In Nanocrystalline Ni-Doped Zro2 By Microwave-Assisted Polyol Synthesis

    Science.gov (United States)

    Parimita Rath, Pragyan; Parhi, Pankaj Kumar; Ranjan Panda, Sirish; Priyadarshini, Barsharani; Ranjan Sahoo, Tapas

    2017-08-01

    This article, deals with a microwave-assisted polyol method to demonstrate a low temperature route polyol precursors decompose exothermically below 300°C. IR data confirms the reduction of Zr(OH)4 precipitates to ZrO2, in agreement with the conclusions drawn from the TGA analysis.

  1. 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…

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

    Science.gov (United States)

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

    2012-01-27

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

  3. The optimized microwave-assisted decomposition of formamides and its synthetic utility in the amination reactions of purines

    Czech Academy of Sciences Publication Activity Database

    Čechová, Lucie; Jansa, Petr; Šála, Michal; Dračínský, Martin; Holý, Antonín; Janeba, Zlatko

    2011-01-01

    Roč. 67, č. 5 (2011), s. 866-871 ISSN 0040-4020 R&D Projects: GA MŠk 1M0508; GA AV ČR KJB400550903 Institutional research plan: CEZ:AV0Z40550506 Keywords : microwave-assisted synthesis * DMF * formamides * dehalogenative amination * purines Subject RIV: CC - Organic Chemistry Impact factor: 3.025, year: 2011

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

    Science.gov (United States)

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

    2016-01-15

    A spectrophotometric method was developed based on the microwave assisted synthesis of Maillard product. Various conditions of the reaction were optimized by varying the relative concentration of the reagents, operating temperature and volume of solutions used in the reaction in the microwave synthesizer. The absorbance of the microwave synthesized Maillard product was measured in the range of 360-740 nm using UV-Visible spectrophotometer. Based on the maximum absorbance, 370 nm was selected as the optimum wave length for further studies. The LOD and LOQ of glucose was found 3.08 μg mL(-1) and 9.33 μg mL(-1) with standard deviation of ±0.05. The developed method was also applicable to urine sample. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2010-11-02

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

  6. 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.

  7. 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

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Science.gov (United States)

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

    2003-08-01

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

  10. Comparison of soxhlet and microwave-assisted extractions for the determination of fenitrothion residues in beans.

    Science.gov (United States)

    Diagne, Rokhaya G; Foster, Gregory D; Khan, Shahamat U

    2002-05-22

    White and black "niebe" beans [Vigna unguiculata (L.) Walp] from Senegal were treated with fenitrothion (O,O-dimethyl O-4-nitro-m-tolyl phosphorothioate), and the residues were determined by high-performance liquid chromatography (HPLC) and electron capture gas chromatography (EC-GC). Fenitrothion residues from the beans were extracted by Soxhlet extraction (SE) and microwave-assisted extraction (MAE). A column cleanup procedure was used to remove the coextractives in the extract before HPLC and EC-GC analyses. The overall mean recoveries of fenitrothion residues in the 0.19-1.90 microg/kg fortification range determined from extracts obtained by SE and MAE were 88.4 and 89.8%, respectively, with respective relative standard deviations of <4%. The results show that MAE is a viable alternative to the commonly used SE for the determination of fenitrothion residues in beans.

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

    Science.gov (United States)

    Thirumalai, Sundararajan; Shanmugavel, Balasivanandha Prabu

    2011-01-01

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

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

    Science.gov (United States)

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

    2016-11-01

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

  13. Critical evaluation of pressurized microwave-assisted digestion efficiency using nitric acid oxidizing systems (M7)

    International Nuclear Information System (INIS)

    Matusiewicz, H.

    2002-01-01

    Full text: The possibilities of enhancement of a medium-pressure microwave-assisted digestion system for sample preparation in trace element analysis of biological material was investigated. Based on optimal digestion conditions for oxidizing systems with nitric acid, different digestion procedures were examined to minimize residual carbon. The substitution of nitric acid and the addition of hydrogen peroxide and ozone to nitric acid was evaluated. The residual carbon content of the digestate was determined coulometrically. Addition of hydrogen peroxide during organic oxidation reactions does not lower the resolved carbon in the solution. Ozone was tested as an additional, potentially non-contaminating, digestion/oxidation system to the nitric acid used in the sample preparation method. (author)

  14. [Microwave assisted UV electrodeless discharge lamp photochemical degradation of 4-chlorophenol in aquatic solutions].

    Science.gov (United States)

    Ai, Zhi-hui; Jiang, Jun-qing; Yang, Peng; Zhou, Tao; Lu, Xiao-hua

    2004-07-01

    A microwave assisted UV electrodeless discharge lamp system (MW/UV) was used for photo-degradation of 4CP simulated wastewater. In order to evaluate the degradation efficiency of 4CP, UV spectrophotometry and ion chromatography were used for determination of 4CP and Cl- respectively. The degradation rate in MW/UV system was higher than that in the UV system within 120min, which were 52.40% and 21.56% respectively. The degradation efficiency was improved by increasing pH value of the solution, aerating O2 gas, enhancing light intensity, or adding H2O2 oxidant. The degradation of 4CP under MW/UV accords with the first order kinetics equation.

  15. Innovative microwave-assisted hydrolysis of ellagitannins and quantification as ellagic acid equivalents.

    Science.gov (United States)

    Theocharis, Grigorios; Andlauer, Wilfried

    2013-06-15

    The health-promoting effects of ellagic acid and its intestinal degradation products are well-known. In plants, ellagic acid mainly appears in the form of its precursors, the so-called ellagitannins. Therefore, determination of total ellagic acid content has been accomplished by cleaving ellagitannins with high temperatures and strong acids. Microwave-assisted extraction (MAE) has been shown to be a very effective and quick extraction technique. The aim of the present study was to establish an MAE-based method for a rapid hydrolysis of ellagitannins and to compare this method with a conventional acid hydrolysis. For this purpose, strawberries (Fragaria x ananassa), which have been identified as a major source of ellagitannins in human diet, were used as a model. The newly developed MAE method was quicker, less chemical-consuming and more effective in hydrolysing ellagitannins. Copyright © 2012 Elsevier Ltd. All rights reserved.

  16. Uranium oxide nanocrystals by microwave-assisted thermal decomposition. Electronic and structural properties

    International Nuclear Information System (INIS)

    Leduc, Jennifer; Mathur, Sanjay; Pacold, Joseph I.; Shuh, David K.; Dong, Chung-Li

    2018-01-01

    Uranium oxides have attracted much attention not only in the context of nuclear energy generation but also for their application as pristine catalysts or as supports for other (transition metal) oxides and (precious) metals. Their propensity to adopt high coordination numbers and manifest multiple oxidation states (from +II to +VI) makes them attractive candidates for catalyzed transformation reactions. Herein, we report a new synthesis route to phase-pure, crystalline UO 2 nanoparticles via microwave-assisted decomposition of a molecular uranium(IV) precursor. The electronic structure and optical absorption properties of these nanocrystals were investigated using spectroscopic methods to evaluate their suitability for photo(electro)catalytic applications. (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  17. Microwave-assisted activation for electroless nickel plating on PMMA microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Yen-Chung [Graduate School of Defense Science, Chung Cheng Institute of Technology, National Defense University, Tao-Yuan, Taiwan 335 (China); Materials and Electro-optics Research Division, Chung Shan Institute of Science and Technology, Tao-Yuan, Taiwan 325 (China); Liu, Robert Lian-Huey [Graduate School of Defense Science, Chung Cheng Institute of Technology, National Defense University, Tao-Yuan, Taiwan 335 (China); Department of Chemical and Materials Engineering, Minghsin University of Science and Technology, Hsinchu Taiwan 304 (China); Chen, Xin-Liang [Graduate School of Defense Science, Chung Cheng Institute of Technology, National Defense University, Tao-Yuan, Taiwan 335 (China); Shu, Hsiou-Jeng [Materials and Electro-optics Research Division, Chung Shan Institute of Science and Technology, Tao-Yuan, Taiwan 325 (China); Ger, Ming-Der, E-mail: mingderger@gmail.com [Department of Chemical and Materials Engineering, Chung Cheng Institute of Technology, National Defense University, Tao-Yuan, Taiwan 335 (China)

    2011-05-15

    A novel microwave-assisted activation method for electroless plating on PMMA microspheres is presented in this study. When the microwave irradiation was applied during the activation step, the amount of the Pd species adsorbed on PMMA surfaces was much higher than that of sample pretreated with a conventional activation process without microwave irradiation. With this activation method, it was also shown that the adsorbed Pd species with a size of 4-6 nm were uniformly distributed on the surfaces of the PMMA microspheres, thus a smooth and uniform nickel-phosphorus coating on the PMMA microspheres was obtained by subsequent electroless plating. The samples after each step were characterized by XPS, TEM, ICP and SEM.

  18. Fabrication of CdS films with superhydrophobicity by the microwave assisted chemical bath deposition.

    Science.gov (United States)

    Liu, Y; Tan, T; Wang, B; Zhai, R; Song, X; Li, E; Wang, H; Yan, H

    2008-04-15

    A simple method of microwave assisted chemical bath deposition (MA-CBD) was adopted to fabricate cadmium sulfide (CdS) thin films. The superhydrophobic surface with a water contact angle (CA) of 151 degrees was obtained. Via a scanning electron microscopy (SEM) observation, the film was proved having a porous micro/nano-binary structure which can change the property of the surface and highly enhance the hydrophobicity of the film. A possible mechanism was suggested to describe the growth of the porous structure, in which the microwave heating takes an important role in the formation of two distinct characteristic dimensions of CdS precipitates, the growth of CdS sheets in micro-scale and sphere particles in nano-scale. The superhydrophobic films may provide novel platforms for photovoltaic, sensor, microfluidic and other device applications.

  19. Microwave-assisted synthesis of anatase TiO2 nanorods with mesopores

    International Nuclear Information System (INIS)

    Jia Xingtao; He Wen; Zhang Xudong; Zhao Hongshi; Li Zhengmao; Feng Yingjun

    2007-01-01

    Pure anatase TiO 2 nanorods with mesopores were synthesized by a simple and low cost microwave-assisted method when tri-block copolymer was used as a structure stabilization agent and TiCl 4 as metal precursor. TEM investigation showed that larger nanorods were assembled by pearl-necklace-shaped nanorods following an oriented attachment mechanism in a specific direction. A proposed hypothetical scheme showed that the formation of lyotropic titania liquid crystal (TLC) serves a key role in the stabilization of nanorods, and the mesopores on nanorods are derived from the vacancy of inter-particles of nanorods and regions lacking inorganic precursors in the TLC structure. Control experiments showed that microwave treatment plays a key role in the maintenance of original morphologies and mesostructures free from destruction even under high temperature calcinations

  20. Microwave-assisted synthesis of anatase TiO{sub 2} nanorods with mesopores

    Energy Technology Data Exchange (ETDEWEB)

    Jia Xingtao [Department of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan, 250100 (China); He Wen [Department of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan, 250100 (China); Zhang Xudong [Department of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan, 250100 (China); Zhao Hongshi [Department of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan, 250100 (China); Li Zhengmao [Department of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan, 250100 (China); Feng Yingjun [Department of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan, 250100 (China)

    2007-02-21

    Pure anatase TiO{sub 2} nanorods with mesopores were synthesized by a simple and low cost microwave-assisted method when tri-block copolymer was used as a structure stabilization agent and TiCl{sub 4} as metal precursor. TEM investigation showed that larger nanorods were assembled by pearl-necklace-shaped nanorods following an oriented attachment mechanism in a specific direction. A proposed hypothetical scheme showed that the formation of lyotropic titania liquid crystal (TLC) serves a key role in the stabilization of nanorods, and the mesopores on nanorods are derived from the vacancy of inter-particles of nanorods and regions lacking inorganic precursors in the TLC structure. Control experiments showed that microwave treatment plays a key role in the maintenance of original morphologies and mesostructures free from destruction even under high temperature calcinations.

  1. 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.

  2. Uranium oxide nanocrystals by microwave-assisted thermal decomposition. Electronic and structural properties

    Energy Technology Data Exchange (ETDEWEB)

    Leduc, Jennifer; Mathur, Sanjay [Institute of Inorganic Chemistry, University of Cologne (Germany); Pacold, Joseph I.; Shuh, David K. [Chemical Sciences Division, The Glenn T. Seaborg Center, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Dong, Chung-Li [Department of Physics, Tamkang University, Tamsui, Taiwan (China)

    2018-01-17

    Uranium oxides have attracted much attention not only in the context of nuclear energy generation but also for their application as pristine catalysts or as supports for other (transition metal) oxides and (precious) metals. Their propensity to adopt high coordination numbers and manifest multiple oxidation states (from +II to +VI) makes them attractive candidates for catalyzed transformation reactions. Herein, we report a new synthesis route to phase-pure, crystalline UO{sub 2} nanoparticles via microwave-assisted decomposition of a molecular uranium(IV) precursor. The electronic structure and optical absorption properties of these nanocrystals were investigated using spectroscopic methods to evaluate their suitability for photo(electro)catalytic applications. (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

    Science.gov (United States)

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

    2016-01-01

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

  4. 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

  5. Advances in modern sample preparation techniques using microwaves assisted chemistry for metal species determination (W1)

    International Nuclear Information System (INIS)

    Ponard, O.F.X.

    2002-01-01

    Full text: Sample preparation has long been the bottleneck of environmental analysis for both total and species specific analysis. Digestion, extraction and preparation of the analytes are relying on a series of chemical reactions. The introduction of microwave assisted sample preparation has first been viewed as a mean to accelerate the kinetics of digestion of the matrix for total elements and fast samples preparation procedures. However, the extensive development and success of microwave digestion procedures in total elemental analysis has now allowed to have a larger insight of the perspectives offered by this technique. Microwave technologies now offer to have a precise control of the temperature and indirectly control the reaction kinetics taking place during the sample preparation procedures. Microwave assisted chemistry permits to perform simultaneously the fundamental steps required for metal species extraction and derivatization. The number of sample preparation steps used for organotin or organomercury species have been reduced to one and the total time of sample preparation brought down for a few hours to some minutes. Further, the developments of GC/ICP/MS techniques allow to routinely use speciated isotopic dilution methods has internal probe of the chemical reactions. These new approaches allow us to use the addition of the labeled species for isotopic dilution as a mean to evaluate and follow the chemical processes taking place during the extraction procedure. These procedures will help us to understand and check for the stability of the analytes during the chemistry of the sample preparation procedure and bring some insights of the chemistry taking place during the extraction. Understanding the different mechanisms involved in the sample preparation steps will allow us in return to further improve all theses procedures and bring us to the horizon of 'on-line sample preparation and detection'. (author)

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. Green Conversion of Agroindustrial Wastes into Chitin and Chitosan by Rhizopus arrhizus and Cunninghamella elegans Strains

    Science.gov (United States)

    Berger, Lúcia Raquel Ramos; Stamford, Thayza Christina Montenegro; Stamford-Arnaud, Thatiana Montenegro; de Alcântara, Sergio Roberto Cabral; da Silva, Antonio Cardoso; da Silva, Adamares Marques; do Nascimento, Aline Elesbão; de Campos-Takaki, Galba Maria

    2014-01-01

    This article sets out a method for producing chitin and chitosan by Cunninghamella elegans and Rhizopus arrhizus strains using a green metabolic conversion of agroindustrial wastes (corn steep liquor and molasses). The physicochemical characteristics of the biopolymers and antimicrobial activity are described. Chitin and chitosan were extracted by alkali-acid treatment, and characterized by infrared spectroscopy, viscosity and X-ray diffraction. The effectiveness of chitosan from C. elegans and R. arrhizus in inhibiting the growth of Listeria monocytogenes, Staphylococcus aureus, Pseudomonas aeruginosa, Salmonella enterica, Escherichia coli and Yersinia enterocolitica were evaluated by determining the minimum inhibitory concentrations (MIC) and the minimum bactericidal concentrations (MBC). The highest production of biomass (24.60 g/L), chitin (83.20 mg/g) and chitosan (49.31 mg/g) was obtained by R. arrhizus. Chitin and chitosan from both fungi showed a similar degree of deacetylation, respectively of 25% and 82%, crystallinity indices of 33.80% and 32.80% for chitin, and 20.30% and 17.80% for chitosan. Both chitin and chitosan presented similar viscosimetry of 3.79–3.40 cP and low molecular weight of 5.08 × 103 and 4.68 × 103 g/mol. They both showed identical MIC and MBC for all bacteria assayed. These results suggest that: agricultural wastes can be produced in an environmentally friendly way; chitin and chitosan can be produced economically; and that chitosan has antimicrobial potential against pathogenic bacteria. PMID:24853288

  11. [Simultaneous Determination of Sn and S in Methyltin Mercaptide by Microwave-Assisted Acid Digestion and ICP-OES].

    Science.gov (United States)

    Chen, Qian; Wu, Xi; Hou, Xian-deng; Xu, Kai-lai

    2015-09-01

    Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4 (v/v/v=9:3:1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing

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

    Science.gov (United States)

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

    2016-04-01

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

  13. 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.

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

    Science.gov (United States)

    Wei, Hao; Chai, Shuangzhi; Hu, Nantao; Yang, Zhi; Wei, Liangming; Wang, Lin

    2015-08-07

    We report the synthesis of a two-dimensional enamine-linked covalent organic framework (COF) using a rapid microwave-assisted solvothermal method in significantly less time and high yield under a relatively low temperature. This COF was found to have a high crystallinity, high stability, high BET surface area, and a high CO2 capacity and adsorption selectivity of CO2/N2.

  15. An efficient microwave-assisted synthesis and biological properties of polysubstituted pyrimidinyl- and 1,3,5-triazinylphosphonic acids

    Czech Academy of Sciences Publication Activity Database

    Jansa, Petr; Hradil, Ondřej; Baszczyňski, Ondřej; Dračínský, Martin; Klepetářová, Blanka; Holý, Antonín; Balzarini, J.; Janeba, Zlatko

    2012-01-01

    Roč. 68, č. 3 (2012), s. 865-871 ISSN 0040-4020 R&D Projects: GA AV ČR KJB400550903; GA MŠk 1M0508 Grant - others:K.U. Leuven(BE) GOA 10/014 Institutional research plan: CEZ:AV0Z40550506 Keywords : phosphonic acids * pyrimidines * 1,3,5-triazines * microwave-assisted synthesis * influenza virus Subject RIV: CC - Organic Chemistry Impact factor: 2.803, year: 2012

  16. Open focused microwave-assisted sample preparation for rapid total and mercury species determination in environmental solid samples

    OpenAIRE

    Tseng, C. M.; Garraud, H.; Amouroux, D.; Donard, O. F. X.; de Diego, A.

    1998-01-01

    This paper describes rapid, simple microwave-assisted leaching/ digestion procedures for total and mercury species determination in sediment samples and biomaterials. An open focused microwave system allowed the sample preparation time to be dramatically reduced to only 24 min when a power of 40-80 W was applied. Quantitative leaching of methylmercury from sediments by HNO3 solution and complete dissolution of biomaterials by an alkaline solution, such as 25% TMAH solution, were obtained. Met...

  17. 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.

  18. Microwave-assisted extraction of Nigella sativa L. essential oil and evaluation of its antioxidant activity.

    Science.gov (United States)

    Abedi, Abdol-Samad; Rismanchi, Marjan; Shahdoostkhany, Mehrnoush; Mohammadi, Abdorreza; Mortazavian, Amir Mohammad

    2017-11-01

    It has been previously reported that the essential oil of Nigella sativa L. seeds and its major active component, thymoquinone (TQ), possess a broad variety of biological activities and therapeutic properties. In this work, microwave-assisted extraction (MAE) of the essential oil from Nigella sativa L. seeds and its antioxidant activity were studied. Response surface methodology based on central composite design was used to evaluate the effects of extraction time, irradiation power and moisture content on extraction yield and TQ content. Optimal parameters obtained by CCD and RSM were extraction time 30 min, irradiation power 450 W, and moisture content 50%. The extraction yield and TQ content of the essential oil were 0.33 and 20% under the optimum conditions, respectively. In contrast, extraction yield and TQ amount of oil obtained by hydrodistillation (HD) were 0.23 and 3.71%, respectively. The main constituents of the essential oil extracted by MAE and HD were p -cymene, TQ, α-thujene and longifolene, comprising more than 60% of total peak area. The antioxidant capacity of essential oils extracted by different methods were evaluated using 2,2-diphenyl-1-picrylhydrazyl and Ferric reducing antioxidant power assays, and compared with traditional antioxidants. The results showed that MAE method was a viable alternative to HD for the essential oil extraction from N. sativa seeds due to the excellent extraction efficiency, higher thymoquinone content, and stronger antioxidant activity.

  19. 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.

  20. 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.

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

  2. Convenient, rapid synthesis of silver nanocubes and nanowires via a microwave-assisted polyol method

    Science.gov (United States)

    Chen, Dapeng; Qiao, Xueliang; Qiu, Xiaolin; Chen, Jianguo; Jiang, Renzhi

    2010-01-01

    Silver nanostructures have been synthesized via a microwave-assisted polyol method by adding sodium sulfide (Na2S) into the solution. An interesting morphology evolution can be observed by adjusting the concentration of Na2S and the heating power. It is found that the ideal concentration of Na2S is 31.25-500 µM for the fast reduction of Ag+ at 300 W under optimal conditions for producing monodispersed silver nanocubes. When the heating power is increased to 400 W, 62.5-250 µM is the ideal concentration of Na2S for the synthesis of silver nanocubes. On increasing the concentration of Na2S (>500 µM), a mixture of silver nanowires, nanocubes, bipyramids, and irregular/quasispherical particles is synthesized at 300 and 400 W. In particular, an increase in the concentration of Na2S to 750 µM at 400 W leads to the production of a quantity of silver nanowires. In addition, silver nanocubes with controllable sizes can be obtained by changing the concentration of Na2S and the heating power. Compared to traditional wet-chemical methods, this method has the advantage of a marked decrease in reaction time to 3.5 min. Finally, our work provides a simple strategy for fabricating silver nanostructures with controllable morphologies and sizes.

  3. Convenient, rapid synthesis of silver nanocubes and nanowires via a microwave-assisted polyol method

    Energy Technology Data Exchange (ETDEWEB)

    Chen Dapeng; Qiao Xueliang; Chen Jianguo; Jiang Renzhi [State Key Laboratory of Plastic Forming Simulation and Die and Mold Technology, Huazhong University of Science and Technology, Wuhan, 430074, Hubei (China); Qiu Xiaolin, E-mail: dpchenhust@yahoo.com.cn [Nanomaterials Research Center, Nanchang Institute of Technology, Nanchang, 330013, Jiangxi (China)

    2010-01-15

    Silver nanostructures have been synthesized via a microwave-assisted polyol method by adding sodium sulfide (Na{sub 2}S) into the solution. An interesting morphology evolution can be observed by adjusting the concentration of Na{sub 2}S and the heating power. It is found that the ideal concentration of Na{sub 2}S is 31.25-500 {mu}M for the fast reduction of Ag{sup +} at 300 W under optimal conditions for producing monodispersed silver nanocubes. When the heating power is increased to 400 W, 62.5-250 {mu}M is the ideal concentration of Na{sub 2}S for the synthesis of silver nanocubes. On increasing the concentration of Na{sub 2}S (>500 {mu}M), a mixture of silver nanowires, nanocubes, bipyramids, and irregular/quasispherical particles is synthesized at 300 and 400 W. In particular, an increase in the concentration of Na{sub 2}S to 750 {mu}M at 400 W leads to the production of a quantity of silver nanowires. In addition, silver nanocubes with controllable sizes can be obtained by changing the concentration of Na{sub 2}S and the heating power. Compared to traditional wet-chemical methods, this method has the advantage of a marked decrease in reaction time to 3.5 min. Finally, our work provides a simple strategy for fabricating silver nanostructures with controllable morphologies and sizes.

  4. Convenient, rapid synthesis of silver nanocubes and nanowires via a microwave-assisted polyol method

    International Nuclear Information System (INIS)

    Chen Dapeng; Qiao Xueliang; Chen Jianguo; Jiang Renzhi; Qiu Xiaolin

    2010-01-01

    Silver nanostructures have been synthesized via a microwave-assisted polyol method by adding sodium sulfide (Na 2 S) into the solution. An interesting morphology evolution can be observed by adjusting the concentration of Na 2 S and the heating power. It is found that the ideal concentration of Na 2 S is 31.25-500 μM for the fast reduction of Ag + at 300 W under optimal conditions for producing monodispersed silver nanocubes. When the heating power is increased to 400 W, 62.5-250 μM is the ideal concentration of Na 2 S for the synthesis of silver nanocubes. On increasing the concentration of Na 2 S (>500 μM), a mixture of silver nanowires, nanocubes, bipyramids, and irregular/quasispherical particles is synthesized at 300 and 400 W. In particular, an increase in the concentration of Na 2 S to 750 μM at 400 W leads to the production of a quantity of silver nanowires. In addition, silver nanocubes with controllable sizes can be obtained by changing the concentration of Na 2 S and the heating power. Compared to traditional wet-chemical methods, this method has the advantage of a marked decrease in reaction time to 3.5 min. Finally, our work provides a simple strategy for fabricating silver nanostructures with controllable morphologies and sizes.

  5. 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.

  6. Rapid immunohistochemical diagnosis of tobacco mosaic virus disease by microwave-assisted plant sample preparation

    Science.gov (United States)

    Zellnig, Günther; Möstl, Stefan; Zechmann, Bernd

    2013-01-01

    Immunoelectron microscopy is a powerful method to diagnose viral diseases and to study the distribution of the viral agent within plant cells and tissues. Nevertheless, current protocols for the immunological detection of viral diseases with transmission electron microscopy (TEM) in plants take between 3 and 6 days and are therefore not suited for rapid diagnosis of virus diseases in plants. In this study, we describe a method that allows rapid cytohistochemical detection of tobacco mosaic virus (TMV) in leaves of tobacco plants. With the help of microwave irradiation, sample preparation of the leaves was reduced to 90 min. After sample sectioning, virus particles were stained on the sections by immunogold labelling of the viral coat protein, which took 100 min. After investigation with the TEM, a clear visualization of TMV in tobacco cells was achieved altogether in about half a day. Comparison of gold particle density by image analysis revealed that samples prepared with the help of microwave irradiation yielded significantly higher gold particle density as samples prepared conventionally at room temperature. This study clearly demonstrates that microwave-assisted plant sample preparation in combination with cytohistochemical localization of viral coat protein is well suited for rapid diagnosis of plant virus diseases in altogether about half a day by TEM. PMID:23580761

  7. 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.

  8. Microwave assisted synthesis of manganese mixed oxide nanostructures using plastic templates

    Science.gov (United States)

    Leyva, A. G.; Stoliar, P.; Rosenbusch, M.; Lorenzo, V.; Levy, P.; Albonetti, C.; Cavallini, M.; Biscarini, F.; Troiani, H. E.; Curiale, J.; Sanchez, R. D.

    2004-11-01

    The synthesis method for obtaining sub-micrometric structures of rare earth manganese-based mixed oxide compounds is described. Pore wetting of porous polycarbonate templates with the liquid precursor was followed by a two-stage thermal treatment to obtain single phase La 0.325Pr 0.300Ca 0.375MnO 3 hollow and solid structures, with external diameter determined by the sacrificial template pore size. The first thermal stage, a microwave assisted denitration process, determines the shape of the structures. The second treatment, performed at 1073 K, allows to obtain the crystallographic structure of the compound. A variety of techniques (scanning and transmission electron microscopy, scanning probe microscopy) allowed to fully characterize the microstructure and morphology of these self-standing manganite nanostructures. For 1 μm pore size templates we obtained tubes, with external diameter around 800 nm and wall thickness around 150 nm; densely packed nanoparticles sized 20-50 nm are the building blocks of the walls. For pore size below 0.1 μm, solid nanowires were obtained, the size of constituent crystallites being around 10 nm. Overall obtained material exhibits ferromagnetic ordering below 200 K.

  9. Microwave-assisted extraction (MAE) of bioactive saponin from mahogany seed (Swietenia mahogany Jacq)

    Science.gov (United States)

    Waziiroh, E.; Harijono; Kamilia, K.

    2018-03-01

    Mahogany is frequently used for medicines for cancer, tumor, and diabetes, as it contains saponin and flavonoid. Saponin is a complex glycosydic compound consisted of triterpenoids or steroids. Saponin can be extracted from a plant by using a solvent extraction. Microwave Assisted Extraction (MAE) is a non-conventional extraction method that use micro waves in the process. This research was conducted by a Complete Random Design with two factors which were extraction time (120, 150, and 180 seconds) and solvent ratio (10:1, 15:1, and 20:1 v/w). The best treatment of MAE were the solvent ratio 15:1 (v/w) for 180 seconds. The best treatment resulting crude saponin extract yield of 41.46%, containing 11.53% total saponins, and 49.17% of antioxidant activity. Meanwhile, the treatment of maceration method were the solvent ratio 20:1 (v/w) for 48 hours resulting 39.86% yield of saponin crude extract, 9.26% total saponins and 56.23% of antioxidant activity. The results showed MAE was more efficient (less time of extraction and solvent amount) than maceration method.

  10. Microwave assisted direct saponification for the simultaneous determination of cholesterol and cholesterol oxides in shrimp.

    Science.gov (United States)

    Souza, Hugo A L; Mariutti, Lilian R B; Bragagnolo, Neura

    2017-05-01

    A novel microwave-assisted direct saponification method for the simultaneous determination of cholesterol and cholesterol oxides in shrimp was developed and validated. Optimal saponification conditions, determined by means of an experimental design, were achieved using 500mg of sample and 20mL of 1mol/L KOH ethanol solution for 16min at 45°C at maximum power at 200W and magnetic stirring at 120rpm. Higher extraction of cholesterol oxides in a reduced saponification time (∼75 times) was achieved in comparison with the direct cold saponification method. The new method showed low detection (≤0.57μg/mL) and quantification (≤1.73μg/mL) limits, good repeatability (≤10.50% intraday and ≤8.56% interday) and low artifact formation (evaluated by using a deuterated cholesterol-D6 standard). Raw, salted and dried-salted shrimps were successfully analyzed by the validated method. The content of cholesterol oxides increased after salting and decreased after drying. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. 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.

  12. 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.

  13. Focused microwave-assisted soxhlet:  an advantageous tool for sample extraction.

    Science.gov (United States)

    García-Ayuso, L E; Sánchez, M; Fernández de Alba, A; Luque de Castro, M D

    1998-06-01

    A new type of microwave-assisted Soxhlet is here reported. The device uses conventional Soxhlet glassware for solid sample extraction and a focused-microwave digester for irradiation of the sample cartridge at the required intervals while the fresh solvent (condensed vapors from the distillation flask) drips on and passes through the solid sample. In this way breaking of the analyte-matrix bonds is facilitated by application of the appropriate energy. The new approach has been checked in a comparative study by its application to the extraction of analyte families of different polarity (namely, alkanes, polyaromatic hydrocarbons, and herbicides) from the same soil matrix using dichloromethane as extractant. The reduction of the extraction times (from 8 h to 50-60 min, depending on the polarity of the analytes) with efficiency similar to or even higher than that afforded by the conventional Soxhlet technique supports the suitability of the new approach. In addition, recycling of the solvent during extract preconcentration enables minimal environmental contamination to be achieved.

  14. Extraction of polychlorinated biphenyls from soils by automated focused microwave-assisted Soxhlet extraction.

    Science.gov (United States)

    Luque-García, J L; de Castro, Luque

    2003-05-23

    The application of a new focused microwave-assisted Soxhlet extractor for the extraction of polychlorinated biphenyls from differently aged soils is here presented. The new extractor overcomes the disadvantages of previous devices based on the same principle and enables a fully automated extraction of two samples simultaneously. The variables affecting the extraction step (namely, power of irradiation, irradiation time, extractant volume, extractant composition and number of extraction cycles) have been optimized using experimental design methodology. The optimized method has also been applied to a certified reference material (CRM910-050 "real" contaminated soil) for quality assurance validation. Quantification of the target compounds has been performed by GC with ion-trap MS. The mass spectrometer was operated in the electron-ionization mode, with selected-ion monitoring at m/z 152, 186, 292, 326 and 498. The results obtained have demonstrated that this approach is as efficient as conventional Soxhlet but with a drastic reduction of both extraction time (70 min vs. 24 h for the "real" contaminated soil) and organic solvent disposal, as 75-80% of the extractant is recycled.

  15. Focused microwave-assisted Soxhlet extraction: a convincing alternative for total fat isolation from bakery products.

    Science.gov (United States)

    Priego-Capote, F; Luque de Castro, M D

    2005-01-15

    An approach for automated fast extraction of the fat content in bakery products based on focused microwave-assisted Soxhlet extraction (FMASE) and gravimetric determination is proposed. The main factors affecting the extraction efficiency-namely, power of irradiation, number of cycles and irradiation time-were optimized using experimental design methodology. The proposed method was applied to six samples, which were classified in two groups-namely, snacks and cookies. The results obtained agree with those provided by the AOAC 920.39 reference extraction method. No significant differences in the extraction efficiency of the fat content in bakery samples using FMASE versus the official method were found. Moreover, a drastic reduction in both the extraction time (60 and 35min versus 16 and 8h, respectively, for the two above commented groups) and sample handling are achieved with similar precision (expressed as repeatability and within-laboratory reproducibility standard deviation) to that provided by the AOAC 920.39 method. In addition, the proposed method is cleaner than the reference method as 75-80% of the extractant is recycled.

  16. 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.

  17. 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.

  18. Microwave-assisted synthesis and magnetic properties of M-SrFe12O19 nanoparticles

    Science.gov (United States)

    Grindi, B.; Beji, Z.; Viau, G.; BenAli, A.

    2018-03-01

    Strontium hexaferrite nanoparticles were synthesized by a microwave-assisted hydrothermal process. The variation of structure, morphology and magnetic properties of the as-produced particles and after annealing temperatures were carefully analysed. Pure M-SrFe12O19 powders were synthesized at T = 200 °C using a heating rate of 25 °C.min-1. The particles exhibited a magnetic coercivity of 95 kA.m-1 (μ0Hc = 0.12 T), explained by the shape of the particles that crystallized as very thin platelets with a micrometer size diameter and a very high aspect ratio in which a competition between shape and magnetocrystalline anisotropy takes place. The coercivity was strongly enhanced with Hc = 360 kA.m-1 (μ0 Hc = 0.445 T) by annealing at the optimum temperature of 1000 °C. In order to optimize the particle morphology and magnetic properties after annealing, the heating rate of the microwave synthesis was increased. At T = 200 °C using a heating rate of 40 °C.min-1 the particle exhibited a size in the range 20-100 nm. The powder crystallized as a mixture of hexaferrite and ferrihydrite. After annealing at 1000 °C, M-SrFe12O19 with a small amount of hematite (<15%) was obtained. The coercivity was strongly enhanced to reach the value Hc = 465 kA.m-1 (μ0Hc = 0.585 T).

  19. Comparison of microwave-assisted digestion procedures for total trace element content determination in calcareous soils.

    Science.gov (United States)

    Marin, B; Chopin, E I B; Jupinet, B; Gauthier, D

    2008-10-19

    The aim of the study was to determine total trace (Cd, Co, Cr, Cu, Mn, Pb and Zn) and major (Al and Fe) element concentrations in calcareous soils using microwave-assisted digestion procedures. The literature showing lack of consensus regarding digestion procedures and unsatisfying recoveries for calcareous materials, four procedures using various acid combinations (HCl, HNO(3), H(2)O(2), HF) and volumes were tested using a certified reference material (CRM 141R) and natural calcareous soil samples. Digests were analysed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Repeatability (R.S.D. 124%) due to complex formation or spectrochemical interferences, respectively. As digestion was not significantly influenced by the addition of H(2)O(2), the procedure corresponding to Aqua regia (HCl-HNO(3)) appeared as the best compromise and was selected for further multielemental environmental studies on calcareous materials, even if the absence of HF could lead to incomplete digestion of accessory silicate minerals. Results for a vineyard plot showed that the soils were contaminated (3.65 mg kg(-1) Cd, 67 mg kg(-1) Cr, 278 mg kg(-1) Cu, 143 mg kg(-1) Pb and 400 mg kg(-1) Zn) as a consequence of urban waste and copper-treatment applications.

  20. Microwave-assisted cationic polymerization of palm olein and their urea inclusion products

    Science.gov (United States)

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

    2018-01-01

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

  1. Microwave-assisted extraction and pharmacological evaluation of polysaccharides from Posidonia oceanica.

    Science.gov (United States)

    Ben Salem, Yosra; Abdelhamid, Amal; Mkadmini Hammi, Khaoula; Le Cerf, Didier; Bouraoui, Abderrahman; Majdoub, Hatem

    2017-10-01

    Microwave-assisted extraction was employed for the isolation of polysaccharides from Posidonia oceanica (PPO). The extracting parameters were optimized adopting response surface methodology. The highest polysaccharide yield (2.55 ± 0.09%), which is in concordance with the predicted value (2.76%), was obtained under the following conditions: extraction time 60 s, liquid-solid ratio of 50:1 (mL/g) and power of 800 W. This polysaccharide, with molecular weight of 524 KDa, characterized by gas chromatography-mass spectrometry showed that PPO was mainly composed of galactose, glucose, and arabinose with molar percentages 25.38, 24.37, and 21.64%, respectively. The pharmacological evaluation of PPO using animal models at the dose of 100 mg/kg indicated a significant anti-inflammatory activity with a percentage of inhibition of edema of 54.65% and a significant antinociceptive activity with 78.91% inhibition of writhing for peripheral analgesic activity and an increase in the hot plate reaction time for central analgesic activity.

  2. Convenient, rapid synthesis of silver nanocubes and nanowires via a microwave-assisted polyol method.

    Science.gov (United States)

    Chen, Dapeng; Qiao, Xueliang; Qiu, Xiaolin; Chen, Jianguo; Jiang, Renzhi

    2010-01-15

    Silver nanostructures have been synthesized via a microwave-assisted polyol method by adding sodium sulfide (Na(2)S) into the solution. An interesting morphology evolution can be observed by adjusting the concentration of Na(2)S and the heating power. It is found that the ideal concentration of Na(2)S is 31.25-500 microM for the fast reduction of Ag(+) at 300 W under optimal conditions for producing monodispersed silver nanocubes. When the heating power is increased to 400 W, 62.5-250 microM is the ideal concentration of Na(2)S for the synthesis of silver nanocubes. On increasing the concentration of Na(2)S (>500 microM), a mixture of silver nanowires, nanocubes, bipyramids, and irregular/quasispherical particles is synthesized at 300 and 400 W. In particular, an increase in the concentration of Na(2)S to 750 microM at 400 W leads to the production of a quantity of silver nanowires. In addition, silver nanocubes with controllable sizes can be obtained by changing the concentration of Na(2)S and the heating power. Compared to traditional wet-chemical methods, this method has the advantage of a marked decrease in reaction time to 3.5 min. Finally, our work provides a simple strategy for fabricating silver nanostructures with controllable morphologies and sizes.

  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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. 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 (X 1 ), microwave power (X 2 ), pH (X 3 ) and solid-to-liquid ratio (X 4 ) on the extraction yield was examined. The optimum conditions of MAE were as follows: X 1 =2.15min; X 2 =517W; X 3 =2.26 and X 4 =2g/30.6mL. The maximum obtained yield of pectin extraction was 12.57%. Total carbohydrate content of WSP is about 95.5% including 34.4% of Galacturonic acid. Pectin-related proteins represent only the 0.66% of WSP mass. HPSEC and light scattering analyses reveal that WSP is mostly constituted of high molecular pectin and FTIR measurements show that the microwave treatment does not alter the chemical structure of WSP, in which Galacturonic acid content and yield are 34.4% and 4.33%, respectively. Overall, application of MAE can give rise to high quality pectin. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Rapid microwave-assisted preparation of binary and ternary transition metal sulfide compounds

    Energy Technology Data Exchange (ETDEWEB)

    Butala, Megan M.; Perez, Minue A.; Arnon, Shiri; Göbel, Claudia; Preefer, Molleigh B.; Seshadri, Ram

    2017-12-01

    Transition metal chalcogenides are of interest for energy applications, including energy generation in photoelectrochemical cells and as electrodes for next-generation electrochemical energy storage. Synthetic routes for such chalcogenides typically involve extended heating at elevated temperatures for multiple weeks. We demonstrate here the feasibility of rapidly preparing select sulfide compounds in a matter of minutes, rather than weeks, using microwave-assisted heating in domestic microwaves. We report the preparations of phase pure FeS2, CoS2, and solid solutions thereof from the elements with only 40 min of heating. Conventional furnace and rapid microwave preparations of CuTi2S4 both result in a majority of the targeted phase, even with the significantly shorter heating time of 40 min for microwave methods relative to 12 days using a conventional furnace. The preparations we describe for these compounds can be extended to related structures and chemistries and thus enable rapid screening of the properties and performance of various compositions of interest for electronic, optical, and electrochemical applications.

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

    International Nuclear Information System (INIS)

    Xia Lixin; Wang Haibo; Wang Jian; Gong Ke; Jia Yi; Zhang Huili; Sun Mengtao

    2008-01-01

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

  7. Near UV excitable Eu-doped alumina nanophosphors synthesized by the microwave assisted solvothermal technique

    Science.gov (United States)

    Padilla-Rosales, I.; Cabañas-Moreno, J. G.; Jiménez, G. L.; Aguilar-Frutis, M. A.; Alarcón-Flores, G.; Falcony, C.

    2017-12-01

    Europium doped alumina nanophosphors have been synthesized by the microwave assisted solvothermal technique. The dependence of the photoluminescence response and structural features of these nanophosphors on the europium content and annealing temperature has been characterized for a wide range of compositions and thermal treatments. The nanophosphors are composed of a mixture of nanocrystalline γ-Al2O3 and EuAlO3, in addition to an amorphous alumina phase. The relative quantities of each phase depend on both the europium content and the annealing temperature. High europium content and/or annealing temperature lead to larger fractions of EuAlO3 nanocrystals having with poor luminescence characteristics, while lower temperatures and europium contents result in the predominance of γ-Al2O3 nanocrystals and amorphous alumina, showing much more efficient luminescent emission. The luminescence spectra from all samples show the characteristic red emission peaks from the Eu3+ ion associated with inter-electronic energy level transitions. However, the excitation spectra in these nanophosphors are dominated, by the 7F0–5L6 transition (395 nm), as opposed to the dominant charge-transfer related band at ~260 nm commonly reported for this material. The highest luminescence intensity was obtained for nanophosphors doped with 7.5 at.% of Eu, annealed at 900 °C, which exhibits a quantum yield of 45% when excited with 395 nm light.

  8. 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.

  9. Rapid preparation of functional polysaccharides from Pyropia yezoensis by microwave-assistant rapid enzyme digest system.

    Science.gov (United States)

    Lee, Ji-Hyeok; Kim, Hyung-Ho; Ko, Ju-Young; Jang, Jun-Ho; Kim, Gwang-Hoon; Lee, Jung-Suck; Nah, Jae-Woon; Jeon, You-Jin

    2016-11-20

    This study describes a simple preparation of functional polysaccharides from Pyropia yezoensis using a microwave-assistant rapid enzyme digest system (MAREDS) with various carbohydrases, and evaluates their antioxidative effects. Polysaccharide hydrolysates were prepared using MAREDS under different hydrolytic conditions of the carbohydrases and microwave powers. Polysaccharides less than 10kDa (Low molecular weight polysaccharides, LMWP, ≤10kDa) were efficiently obtained using an ultrafiltration (molecular weight cut-off of 10kDa). MAREDS increases AMG activation via an increased degree of hydrolysis; the best AMG hydrolysate was prepared using a 10:1 ratio of substrate to enzyme for 2h in MAREDS with 400W. LMWP consisted of galactose (27.3%), glucose (64.5%), and mannose (8.3%) from the AMG hydrolysate had stronger antioxidant effects than the high molecular weight polysaccharides (>10kDa). We rapidly prepared functional LMWPs by using MAREDS with carbohydrases, and suggest that LMWP might be potentially a valuable algal polysaccharide antioxidant. Copyright © 2016 Elsevier Ltd. All rights reserved.

  10. 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.

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

    Directory of Open Access Journals (Sweden)

    Claudia Carlucci

    2014-06-01

    Full Text Available 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, inductively coupled plasma-atomic emission spectroscopy (ICP-AES, X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, Raman spectroscopy and nitrogen absorption-desorption. Oleic acid coordinated on the nanocrystal surface was removed by the reduction of its carboxyl group, and the photocatalytic activity of bare TiO2 nanocrystals, under visible light irradiation, was also evaluated. The synthesized TiO2 anatase nanorods exhibited a good photoactivity and completely degraded Rhodamine B solution within three hours.

  12. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    International Nuclear Information System (INIS)

    Lou Zaixiang; Wang Hongxin; Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping

    2012-01-01

    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.

  13. Dynamic microwave assisted extraction coupled with dispersive micro-solid-phase extraction of herbicides in soybeans.

    Science.gov (United States)

    Li, Na; Wu, Lijie; Nian, Li; Song, Ying; Lei, Lei; Yang, Xiao; Wang, Kun; Wang, Zhibing; Zhang, Liyuan; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

    2015-09-01

    Non-polar solvent dynamic microwave assisted extraction was firstly applied to the treatment of high-fat soybean samples. In the dispersive micro-solid-phase extraction (D-µ-SPE), the herbicides in the high-fat extract were directly adsorbed on metal-organic frameworks MIL-101(Cr). The effects of several experimental parameters, including extraction solvent, microwave absorption medium, microwave power, volume and flow rate of extraction solvent, amount of MIL-101(Cr), and D-µ-SPE time, were investigated. At the optimal conditions, the limits of detection for the herbicides ranged from 1.56 to 2.00 μg kg(-1). The relative recoveries of the herbicides were in the range of 91.1-106.7%, and relative standard deviations were equal to or lower than 6.7%. The present method was simple, rapid and effective. A large amount of fat was also removed. This method was demonstrated to be suitable for treatment of high-fat samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Rapid microwave-assisted synthesis of dextran-coated iron oxide nanoparticles for magnetic resonance imaging

    International Nuclear Information System (INIS)

    Osborne, Elizabeth A; Atkins, Tonya M; Kauzlarich, Susan M; Gilbert, Dustin A; Liu Kai; Louie, Angelique Y

    2012-01-01

    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. (paper)

  15. Microwave-assisted co-pyrolysis of brown coal and corn stover for oil production.

    Science.gov (United States)

    Zhang, Yaning; Fan, Liangliang; Liu, Shiyu; Zhou, Nan; Ding, Kuan; Peng, Peng; Anderson, Erik; Addy, Min; Cheng, Yanling; Liu, Yuhuan; Li, Bingxi; Snyder, John; Chen, Paul; Ruan, Roger

    2018-07-01

    The controversial synergistic effect between brown coal and biomass during co-pyrolysis deserves further investigation. This study detailed the oil production from microwave-assisted co-pyrolysis of brown coal (BC) and corn stover (CS) at different CS/BC ratios (0, 0.33, 0.50, 0.67, and 1) and pyrolysis temperatures (500, 550, and 600 °C). The results showed that a higher CS/BC ratio resulted in higher oil yield, and a higher pyrolysis temperature increased oil yield for brown coal and coal/corn mixtures. Corn stover and brown coal showed different pyrolysis characteristics, and positive synergistic effect on oil yield was observed only at CS/BC ratio of 0.33 and pyrolysis temperature of 600 °C. Oils from brown coal mainly included hydrocarbons and phenols whereas oils from corn stover and coal/corn mixtures were dominated by ketones, phenols, and aldehydes. Positive synergistic effects were observed for ketones, aldehydes, acids, and esters whereas negative synergistic effects for hydrocarbons, phenols and alcohols. Copyright © 2018 Elsevier Ltd. All rights reserved.

  16. 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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  18. 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.

  19. Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

    Science.gov (United States)

    Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

    2014-12-01

    An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Effect of Ag on structural, optical and luminescence properties of ZnS nanoparticles synthesized by microwave-assisted chemical route

    Science.gov (United States)

    Patel, Kamakshi; Deshpande, M. P.; Chaki, S. H.

    2017-05-01

    Silver (Ag)-doped (0, 5, 10 and 15%) ZnS nanoparticles are synthesized by microwave-assisted chemical route using polyvinylpyrrolidone (PVP). We study the compositional, structural, optical and luminescence properties by energy-dispersive analysis of X-rays (EDAX), transmission electron microscopy (TEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), UV-Vis spectroscopy and photoluminescence (PL) spectroscopy, respectively. Synthesized Ag-doped ZnS nanoparticles do not possess any impurity as seen from EDAX spectra. TEM images show particles to be in spherical shape with agglomeration, and corresponding selected area electron diffraction (SAED) pattern showed that they are polycrystalline in nature. Allowed LO and TO modes corresponding to cubic phase for all the samples are observed in Raman spectra. FTIR spectroscopy is used to study the interaction between PVP and as-synthesized nanoparticles. Blue shift can be seen in pure and Ag-doped ZnS nanoparticles compared to bulk ZnS as seen from absorption spectra. Green emission is observed in PL spectra due to Ag doping without showing any quenching behavior.

  1. 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.

  2. 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.

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

    Science.gov (United States)

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

    2017-08-01

    The microwave-assisted production of solid lipid nanoparticles (SLNs) is a novel technique reported recently by our group. The small particle size, solid nature and use of physiologically well-tolerated lipid materials make SLNs an interesting and potentially efficacious drug carrier. The main purpose of this research work was to investigate the suitability of microwave-assisted microemulsion technique to encapsulate selected ionic drug substances such as miconazole nitrate and econazole nitrate. The microwave-produced SLNs had a small size (250-300nm), low polydispersity (microwave-produced SLNs. Data fitting of drug release data revealed that the release of both drugs from microwave-produced SLNs was governed by non-Fickian diffusion indicating that drug release was both diffusion- and dissolution- controlled. Anti-fungal efficacy of drug-loaded SLNs was evaluated on C. albicans. The cell viability studies showed that cytotoxicity of SLNs was concentration-dependent. These encouraging results suggest that the microwave-assisted procedure is suitable for encapsulation of ionic drugs and that microwave-produced SLNs can act as potential carriers of antifungal drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Microwave-assisted steam distillation with simultaneous liquid/liquid extraction of pentachlorophenol from organic wastes and soils.

    Science.gov (United States)

    Düring, Rolf-Alexander; Zhang, Xiaolei; Hummel, Hans E; Czynski, Janusz; Gäth, Stefan

    2003-02-01

    An efficient method for extracting pentachlorophenol (PCP) from organic solid matrices and soils using direct excitation of the fresh samples by microwave energy is presented. Steam-volatile PCP partitioned into the organic solvent n-hexane within the closed extraction vessel, resulting in recovery rates of 85-92% from aged samples. Condensed water provided a boundary layer between extract and sample thus preventing any contact of PCP with and re-partitioning into the sample. Duration of the microwave-assisted process was 35 min. Crude extracts were derivatized by heptafluorobutyric anhydride (HFBA) to improve selectivity and sensitivity resulting in detection limits of 1-2 micro g kg(-1). GC-MS/MS analyses proved that suitable extracts with only minor impurities were obtained. Common sample treatment steps like drying, thorough grinding, frequent transferring, and tedious clean-up, and concentration procedures which all can cause certain losses of analyte were minimized. The efficiency of the method was verified by comparison with an established ultrasonic extraction procedure. This microwave-assisted pressurized steam distillation with simultaneous partition into an organic phase thus provides a streamlined and efficient strategy which requires no additional investment in standard equipment for microwave-assisted extractions (MAE). Degradation of analytes at longer extraction times must be taken into account.

  5. 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. 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

  6. 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.

  7. Structural and optical characterization of CuInS{sub 2} quantum dots synthesized by microwave-assisted continuous flow methods

    Energy Technology Data Exchange (ETDEWEB)

    Fitzmorris, Robert C.; Oleksak, Richard P.; Zhou, Zheng [Oregon State University, School of Chemical, Biological, and Environmental Engineering (United States); Mangum, Benjamin D.; Kurtin, Juanita N. [Pacific Light Technologies (United States); Herman, Gregory S., E-mail: greg.herman@oregonstate.edu [Oregon State University, School of Chemical, Biological, and Environmental Engineering (United States)

    2015-07-15

    Semiconductor quantum dots (QDs) have recently been incorporated into consumer displays and lighting technologies. Now that these materials are being produced on industrial scales, it is important to investigate scalable synthetic methods and less toxic materials and chemistries. To achieve these goals, we have synthesized cadmium-free, visible light-emitting QDs using a microwave-assisted continuous flow reactor. After synthesis, the CuInS{sub 2} QD cores underwent a near-complete Zn cation exchange reaction in a batch reactor, followed by the growth of a ZnS shell. Analysis of X-ray diffraction, transmission electron microscopy, and Raman spectroscopy data indicate that the crystal structure changes from CuInS{sub 2} (chalcopyrite) to ZnS (zincblende) during the cation exchange reaction. Compositional analysis indicated that the core/shell QDs were ∼98 % ZnS, with Cu and In present at much lower concentrations. The photoluminescence (PL) peak position was blue shifted for longer cation exchange reactions, and it was found that the ZnS shell was necessary for improved PL stability. The synthesized QDs have a PL down conversion efficiency of ∼65 % when using a blue LED source.

  8. Microwave-assisted synthesis of palladium nanoparticles intercalated nitrogen doped reduced graphene oxide and their electrocatalytic activity for direct-ethanol fuel cells.

    Science.gov (United States)

    Kumar, Rajesh; da Silva, Everson T S G; Singh, Rajesh K; Savu, Raluca; Alaferdov, Andrei V; Fonseca, Leandro C; Carossi, Lory C; Singh, Arvind; Khandka, Sarita; Kar, Kamal K; Alves, Oswaldo L; Kubota, Lauro T; Moshkalev, Stanislav A

    2018-04-01

    Palladium nanoparticles decorated reduced graphene oxide (Pd-rGO) and palladium nanoparticles intercalated inside nitrogen doped reduced graphene oxide (Pd-NrGO) hybrids have been synthesized by applying a very simple, fast and economic route using microwave-assisted in-situ reduction and exfoliation method. The Pd-NrGO hybrids materials show good activity as catalyst for ethanol electro oxidation for direct ethanol fuel cells (DEFCs) as compared to Pd-rGO hybrids. The enhanced direct ethanol fuel cell can serve as alternative to fossil fuels because it is renewable and environmentally-friendly with a high energy conversion efficiency and low pollutant emission. As proof of concept, the electrocatalytic activity of Pd-NrGO hybrid material was accessed by cyclic voltammetry in presence of ethanol to evaluate its applicability in direct-ethanol fuel cells (DEFCs). The Pd-NrGO catalyst presented higher electro active surface area (∼6.3 m 2  g -1 ) for ethanol electro-oxidation when compared to Pd-rGO hybrids (∼3.7 m 2  g -1 ). Despite the smaller catalytic activity of Pd-NrGO, which was attributed to the lower exfoliation rate of this material in relation to the Pd-rGO, Pd-NrGO showed to be very promising and its catalytic activity can be further improved by tuning the synthesis parameters to increase the exfoliation rate. Copyright © 2018 Elsevier Inc. All rights reserved.

  9. Revealing the Formation Mechanism of CsPbBr3 Perovskite Nanocrystals Produced via a Slowed-Down Microwave-Assisted Synthesis.

    Science.gov (United States)

    Li, Yanxiu; Huang, He; Xiong, Yuan; Kershaw, Stephen V; Rogach, Andrey L

    2018-03-24

    We developed a microwave-assisted slowed-down synthesis of CsPbBr 3 perovskite nanocrystals, which retards the reaction and allows us to gather useful insights into the formation mechanism of these nanoparticles, by examining the intermediate stages of their growth. The trends in the decay of the emission intensity of CsPbBr 3 nanocrystals under light exposure are well correlated with their stability against decomposition in TEM under electron beam. The results show the change of the crystal structure of CsPbBr 3 nanocrystals from a deficient and easier to be destroyed lattice to a well crystallized one. Conversely the shift in the ease of degradation sheds light on the formation mechanism, indicating first the formation of a bromoplumbate ionic scaffold, with Cs-ion infilling lagging a little behind. Increasing the cation to halide ratio towards the stoichiometric level may account for the improved radiative recombination rates observed in the longer reaction time materials. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Directory of Open Access Journals (Sweden)

    Saravanan Devendran

    2014-01-01

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

  11. Design Principles for Covalent Organic Frameworks as Efficient Electrocatalysts in Clean Energy Conversion and Green Oxidizer Production.

    Science.gov (United States)

    Lin, Chun-Yu; Zhang, Lipeng; Zhao, Zhenghang; Xia, Zhenhai

    2017-05-01

    Covalent organic frameworks (COFs), an emerging class of framework materials linked by covalent bonds, hold potential for various applications such as efficient electrocatalysts, photovoltaics, and sensors. To rationally design COF-based electrocatalysts for oxygen reduction and evolution reactions in fuel cells and metal-air batteries, activity descriptors, derived from orbital energy and bonding structures, are identified with the first-principle calculations for the COFs, which correlate COF structures with their catalytic activities. The calculations also predict that alkaline-earth metal-porphyrin COFs could catalyze the direct production of H 2 O 2 , a green oxidizer and an energy carrier. These predictions are supported by experimental data, and the design principles derived from the descriptors provide an approach for rational design of new electrocatalysts for both clean energy conversion and green oxidizer production. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Robust microwave-assisted extraction protocol for determination of total mercury and methylmercury in fish tissues

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, L. Hinojosa; Rahman, G.M. Mizanur [Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, PA 15282 (United States); Kingston, H.M. Skip [Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, PA 15282 (United States)], E-mail: kingston@duq.edu

    2009-01-12

    A rapid and efficient closed vessel microwave-assisted extraction (MAE) method based on acidic leaching was developed and optimized for the extraction of total mercury (Hg), inorganic mercury (Hg{sup 2+}) and methylmercury (CH{sub 3}Hg{sup +}) from fish tissues. The quantitative extraction of total Hg and mercury species from biological samples was achieved by using 5 mol L{sup -1} HCl and 0.25 mol L{sup -1} NaCl during 10 min at 60 deg. C. Total Hg content was determined using inductively coupled plasma mass spectrometry (ICP-MS). Mercury species were measured by liquid chromatography hyphenated with inductively coupled plasma mass spectrometry (LC-ICP-MS). The method was validated using biological certified reference materials ERM-CE464, DOLT-3, and NIST SRM-1946. The analytical results were in good agreement with the certified reference values of total Hg and CH{sub 3}Hg{sup +} at a 95% confidence level. Further, accuracy validation using speciated isotope-dilution mass spectrometry (SIDMS, as described in the EPA Method 6800) was carried out. SIDMS was also applied to study and correct for unwanted species transformation reactions during and/or after sample preparation steps. For the studied reference materials, no statistically significant transformation between mercury species was observed during the extraction and determination procedures. The proposed method was successfully applied to fish tissues with good agreement between SIDMS results and external calibration (EC) results. Interspecies transformations in fish tissues were slightly higher than certified reference materials due to differences in matrix composition. Depending on the type of fish tissue, up to 10.24% of Hg{sup 2+} was methylated and up to 1.75% of CH{sub 3}Hg{sup +} was demethylated to Hg{sup 2+}.

  13. Speciation of heavy metals in untreated sewage sludge by using microwave assisted sequential extraction procedure.

    Science.gov (United States)

    Jamali, Muhammad K; Kazi, Tasneem G; Arain, Muhammad B; Afridi, Hassan I; Jalbani, Nusrat; Kandhro, Ghulam A; Shah, Abdul Q; Baig, Jameel A

    2009-04-30

    A fast microwave assisted extraction procedure was developed and optimized for their eventual exploitation in the three-stage sequential extraction procedure proposed by modified BCR protocol (the community Bureau of Reference now the European Union "Measurement and Testing Programme"). The effects of the microwave treatment on the extraction of Cd, Cr, Cu, Ni, Pb and Zn from untreated sewage sludge collected from Hyderabad city (Pakistan) were compared with those obtained from sequential BCR extraction procedure. In sequential BCR method, each extraction step takes 16 h, where as with the use of compromised microwave conditions, extraction steps could be completed in about 120 s, for each step, respectively. Extractable Cd, Cr, Pb and Ni obtained by both comparable methodologies were measured by electrothermal atomic absorption spectrometry (ETAAS), while for Cu and Zn flame atomic absorption spectrometry (FAAS) was used. The validations of both extraction techniques were compared by the analysis of certified reference material of soil amended with sewage sludge (BCR 483). The results of the partitioning study of untreated waste water sewage sludge, indicate that more easily mobilized forms (step 1) were predominant for Cd, Ni and Zn (28.3, 28.4 and 43.7%), in contrast, the largest amount of Cd and Pb (66.4 and 72.8%) was associated with the iron/manganese oxide while Cr and Ni (71.2 and 38.7%) in organic matter/sulphide fractions. The overall metal recoveries in steps 1-3 (excluding residual step) were 95.3-104% of those obtained with the sequential BCR protocol. The accuracy of the proposed microwave extraction method (expressed as %R.S.D.) was lower than 10% for all metals.

  14. 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. © 2014 Her Majesty the Queen in Right of Canada Journal of Food Science © 2014 Institute of Food Technologists® Reproduced with the permission of the Minister of Agriculture and Agri-Food Canada.

  15. Optimisation of microwave assisted digestion of sediments and determination of Sn and Hg

    Energy Technology Data Exchange (ETDEWEB)

    Navarro, P. [Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country, P.O. Box 644, Bilbao 48080, Basque Country (Spain)]. E-mail: qabnavip@lg.ehu.es; Raposo, J.C. [Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country, P.O. Box 644, Bilbao 48080, Basque Country (Spain); Arana, G. [Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country, P.O. Box 644, Bilbao 48080, Basque Country (Spain); Etxebarria, N. [Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country, P.O. Box 644, Bilbao 48080, Basque Country (Spain)

    2006-04-27

    The determination of Sn by flow injection-hydride generation-quartz furnace atomic absorption spectrometric (FI-HG-QFAAS) was optimised following different experimental designs. The best conditions were: 0.2% HCl (v/v), 0.5% NaBH{sub 4} (w/v) and the furnace temperature 875 deg. C. Under those conditions, the limit of detection was 0.17 ng dm{sup -3} and a precision of 5.3% was obtained. One of the aims of this work was to optimise the closed vessel microwave assisted digestion (MAD) of sediments for the determination of Sn and Hg in the same extract using the analytical conditions previously optimised for Sn in the FI-QFAAS. The optimisation of the MAD of sediments was accomplished following a D-optimal design, including the composition of the HCl-HNO{sub 3} mixture, the pressure and irradiation time. However, we could not determine tin in the extracts due to the formation of foams, the optimisation of the digestion conditions were taken from the FI-cold vapour (CV)-QFAAS measurements of mercury. The optimum conditions were: 2.1 bar of pressure during 10 min of irradiation and two local optima composition of the acid mixtures: 80% HCl-20% HNO{sub 3} and 60% H{sub 2}O-20% HCl-20% HNO{sub 3}. The determination of mercury in sediments was validated with the CRM-580. In order to determine Sn in sediments the solutions from the same D-optimal design were analysed using an ICP-MS and the digestion conditions were optimised for Sn and for other 8 metals. In this case the same optimal conditions were obtained (2.1 bar and 10 min) but different acid mixture composition 20% HCl-80% HNO{sub 3}. The determination of Sn and the other metals in sediments was validated using two other CRMs (PACS-2 and SGR-1)

  16. 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.

  17. Diagnostics of microwave assisted electron cyclotron resonance plasma source for surface modification of nylon 6

    Science.gov (United States)

    More, Supriya E.; Das, Partha Sarathi; Bansode, Avinash; Dhamale, Gayatri; Ghorui, S.; Bhoraskar, S. V.; Sahasrabudhe, S. N.; Mathe, Vikas L.

    2018-01-01

    Looking at the increasing scope of plasma processing of materials surface, here we present the development and diagnostics of a microwave assisted Electron Cyclotron Resonance (ECR) plasma system suitable for surface modification of polymers. Prior to the surface-treatment, a detailed diagnostic mapping of the plasma parameters throughout the reactor chamber was carried out by using single and double Langmuir probe measurements in Ar plasma. Conventional analysis of I-V curves as well as the elucidation form of the Electron Energy Distribution Function (EEDF) has become the source of calibration of plasma parameters in the reaction chamber. The high energy tail in the EEDF of electron temperature is seen to extend beyond 60 eV, at much larger distances from the ECR zone. This proves the suitability of the rector for plasma processing, since the electron energy is much beyond the threshold energy of bond breaking in most of the polymers. Nylon 6 is used as a representative candidate for surface processing in the presence of Ar, H2 + N2, and O2 plasma, treated at different locations inside the plasma chamber. In a typical case, the work of adhesion is seen to almost get doubled when treated with oxygen plasma. Morphology of the plasma treated surface and its hydrophilicity are discussed in view of the variation in electron density and electron temperature at these locations. Nano-protrusions arising from plasma treatment are set to be responsible for the hydrophobicity. Chemical sputtering and physical sputtering are seen to influence the surface morphology on account of sufficient electron energies and increased plasma potential.

  18. Microwave-Assisted Development of Orally Disintegrating Tablets by Direct Compression.

    Science.gov (United States)

    Kande, Kishor V; Kotak, Darsheen J; Degani, Mariam S; Kirsanov, Dmitry; Legin, Andrey; Devarajan, Padma V

    2017-08-01

    Orally disintegrating tablets (ODTs) are challenged by the need for simple technology to ensure good mechanical strength coupled with rapid disintegration. The objective of this work was to evaluate microwave-assisted development of ODTs based on simple direct compression tableting technology. Placebo ODTs comprising directly compressible mannitol and lactose as diluents, super disintegrants, and lubricants were prepared by direct compression followed by exposure to >97% relative humidity and then microwave irradiation for 5 min at 490 W. Placebo ODTs with hardness (>5 kg/cm 2 ) and disintegration time (microwave irradiation (MWI) was confirmed. Solubilization was achieved by complexation with beta-cyclodextrin (β-CD). LMG ODTs with optimal hardness and disintegration time (DT) were optimized by a 2 3 factorial design using Design Expert software. Taste masking using sweeteners and flavors was confirmed using a potentiometric multisensor-based electronic tongue, coupled with principal component analysis. Placebo ODTs with crospovidone as a superdisintegrant revealed a significant increase in hardness from ∼3 to ∼5 kg/cm 2 and a decrease in disintegration time (microwave irradiation. LMG ODTs had hardness >5 kg/cm 2 , DT < 30s, and rapid dissolution of LMG, and good stability was optimized by DOE and the design space derived. While β-CD complexation enabled rapid dissolution and moderate taste masking, palatability, which was achieved including flavors, was confirmed using an electronic tongue. A simple step of humidification enabled MWI-facilitated development of ODTs by direct compression presenting a practical and scalable advancement in ODT technology.

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

    Directory of Open Access Journals (Sweden)

    Vanja Lovrić

    2017-01-01

    Full Text Available 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.

  20. Optimisation of microwave assisted digestion of sediments and determination of Sn and Hg

    International Nuclear Information System (INIS)

    Navarro, P.; Raposo, J.C.; Arana, G.; Etxebarria, N.

    2006-01-01

    The determination of Sn by flow injection-hydride generation-quartz furnace atomic absorption spectrometric (FI-HG-QFAAS) was optimised following different experimental designs. The best conditions were: 0.2% HCl (v/v), 0.5% NaBH 4 (w/v) and the furnace temperature 875 deg. C. Under those conditions, the limit of detection was 0.17 ng dm -3 and a precision of 5.3% was obtained. One of the aims of this work was to optimise the closed vessel microwave assisted digestion (MAD) of sediments for the determination of Sn and Hg in the same extract using the analytical conditions previously optimised for Sn in the FI-QFAAS. The optimisation of the MAD of sediments was accomplished following a D-optimal design, including the composition of the HCl-HNO 3 mixture, the pressure and irradiation time. However, we could not determine tin in the extracts due to the formation of foams, the optimisation of the digestion conditions were taken from the FI-cold vapour (CV)-QFAAS measurements of mercury. The optimum conditions were: 2.1 bar of pressure during 10 min of irradiation and two local optima composition of the acid mixtures: 80% HCl-20% HNO 3 and 60% H 2 O-20% HCl-20% HNO 3 . The determination of mercury in sediments was validated with the CRM-580. In order to determine Sn in sediments the solutions from the same D-optimal design were analysed using an ICP-MS and the digestion conditions were optimised for Sn and for other 8 metals. In this case the same optimal conditions were obtained (2.1 bar and 10 min) but different acid mixture composition 20% HCl-80% HNO 3 . The determination of Sn and the other metals in sediments was validated using two other CRMs (PACS-2 and SGR-1)

  1. Conversion of Blue Water into Green Water for Improving Utilization Ratio of Water Resources in Degraded Karst Areas

    Directory of Open Access Journals (Sweden)

    Ke Chen

    2016-12-01

    Full Text Available Vegetation deterioration and soil loss are the main causes of more precipitation leakages and surface water shortages in degraded karst areas. In order to improve the utilization of water resources in such regions, water storage engineering has been considered; however, site selection and cost associated with the special karstic geological structure have made this difficult. According to the principle of the Soil Plant Atmosphere Continuum, increasing both vegetation cover and soil thickness would change water cycle process, resulting in a transformation from leaked blue water (liquid form into green water (gas or saturated water form for terrestrial plant ecosystems, thereby improving the utilization of water resources. Using the Soil Vegetation Atmosphere Transfer model and the geographical distributed approach, this study simulated the conversion from leaked blue water (leakage into green water in the environs of Guiyang, a typical degraded karst area. The primary results were as follows: (1 Green water in the area accounted for <50% of precipitation, well below the world average of 65%; (2 Vegetation growth played an important role in converting leakage into green water; however, once it increased to 56%, its contribution to reducing leakage decreased sharply; (3 Increasing soil thickness by 20 cm converted the leakage considerably. The order of leakage reduction under different precipitation scenarios was dry year > normal year > rainy year. Thus, increased soil thickness was shown effective in improving the utilization ratio of water resources and in raising the amount of plant ecological water use; (4 The transformation of blue water into green water, which avoids constructions of hydraulic engineering, could provide an alternative solution for the improvement of the utilization of water resources in degraded karst area. Although there are inevitable uncertainties in simulation process, it has important significance for overcoming similar

  2. PEG 400/Cerium Ammonium Nitrate Combined with Microwave-Assisted Synthesis for Rapid Access to Beta-Amino Ketones. An Easy-to-Use Protocol for Discovering New Hit Compounds

    Directory of Open Access Journals (Sweden)

    Giacomo Rossino

    2018-03-01

    Full Text Available Compound libraries are important requirement in target-based drug discovery. In the present work, a small focused compound library based on β-aminoketone scaffold has been prepared combining microwave-assisted organic synthesis (MAOS with polymer-assisted solution phase synthesis (PASPS and replacing reaction workup standard purification procedures with solid phase extraction (SPE. Specifically, the effects of solvent, such as dioxane, dimethylformamide (DMF, polyethylene glycol 400 (PEG 400, temperature, irradiation time, stoichiometric ratio of reagents, and catalysts (HCl, acetic acid, cerium ammonium nitrate (CAN were investigated to maximize both conversion and yield. The optimized protocol generally afforded the desired products in satisfying yields and purities. The designed library is a part of our current research on sigma 1 receptor modulators, a valuable tool for the identification of novel potential hit compounds.

  3. Applied orthogonal experiment design for the optimum microwave-assisted extraction conditions of polysaccharides from Rhodiolae Radix.

    Science.gov (United States)

    Li, Fenglin; Xiao, Furen; Gong, Jingli; Yu, Tian

    2013-01-01

    An experiment on polysaccharides from Rhodiolae Radix (PRR) extraction was carried out using microwave-assisted extraction (MAE) method with an objective to establishing the optimum MAE conditions of PRR. Single factor experiments were performed to determine the appropriate range of extraction conditions, and the optimum conditions were obtained using orthogonal experiment design. The results showed that the optimum MAE conditions of PRR were as follows: solid-liquid ratio of 1:45 g/mL, irradiation power of 480 W, and irradiation time of 8 min, while extraction yield of PRR was 3.24 %.

  4. 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.

  5. 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.

  6. Microwave-Assisted Extraction of Phenolic Compounds from Almond Skin Byproducts (Prunus amygdalus): A Multivariate Analysis Approach

    OpenAIRE

    Valdés, Arantzazu; Vidal, Lorena; Beltrán Sanahuja, Ana; Canals, Antonio; Garrigós, María del Carmen

    2015-01-01

    A microwave-assisted extraction (MAE) procedure to isolate phenolic compounds from almond skin byproducts was optimized. A three-level, three-factor Box–Behnken design was used to evaluate the effect of almond skin weight, microwave power, and irradiation time on total phenolic content (TPC) and antioxidant activity (DPPH). Almond skin weight was the most important parameter in the studied responses. The best extraction was achieved using 4 g, 60 s, 100 W, and 60 mL of 70% (v/v) ethanol. TPC,...

  7. 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.

  8. Microwave-assisted rapid synthesis of Pt/graphene nanosheet composites and their application for methanol oxidation

    Science.gov (United States)

    Liu, Sen; Wang, Lei; Tian, Jingqi; Lu, Wenbo; Zhang, Yingwei; Wang, Xiaodan; Sun, Xuping

    2011-10-01

    Polymer-free Pt/graphene nanosheet (GN) composites have been rapidly prepared by a one-step microwave-assisted reduction method, carried out by ethylene glycol reduction of H2PtCl6 in a graphene oxide suspension. Several analytic techniques including UV-vis spectroscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy have been used to characterize the resulting Pt/GN composites. It suggests that such composites exhibit good catalytic activity toward methanol oxidation.

  9. Land-use conversion and changing soil carbon stocks in China's 'Grain-for-Green' Program: a synthesis.

    Science.gov (United States)

    Deng, Lei; Liu, Guo-Bin; Shangguan, Zhou-Ping

    2014-11-01

    The establishment of either forest or grassland on degraded cropland has been proposed as an effective method for climate change mitigation because these land use types can increase soil carbon (C) stocks. This paper synthesized 135 recent publications (844 observations at 181 sites) focused on the conversion from cropland to grassland, shrubland or forest in China, better known as the 'Grain-for-Green' Program to determine which factors were driving changes to soil organic carbon (SOC). The results strongly indicate a positive impact of cropland conversion on soil C stocks. The temporal pattern for soil C stock changes in the 0-100 cm soil layer showed an initial decrease in soil C during the early stage (5 years) coincident with vegetation restoration. The rates of soil C change were higher in the surface profile (0-20 cm) than in deeper soil (20-100 cm). Cropland converted to forest (arbor) had the additional benefit of a slower but more persistent C sequestration capacity than shrubland or grassland. Tree species played a significant role in determining the rate of change in soil C stocks (conifer stock change after cropland conversion with higher initial soil C stock sites having a negative effect on soil C accumulation. Soil C sequestration significantly increased with restoration age over the long-term, and therefore, the large scale of land-use change under the 'Grain-for-Green' Program will significantly increase China's C stocks. © 2014 John Wiley & Sons Ltd.

  10. Green chemistry perspectives of methane conversion via oxidative methylation of aromatics over zeolite catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Adebajo, M.O. [University of Queensland, St Lucia, Qld. (Australia)

    2007-06-15

    This paper provides a general overview of the recent work that we and other researchers have done on the utilisation of methane for catalytic methylation of aromatic compounds and for direct coal liquefaction for the production of liquid hydrocarbons. In particular, the paper presents a detailed description of more recent substantial experimental evidence that we have provided for the requirement of oxygen as a stoichiometry reactant for benzene methylation with methane over moderately acidic zeolite catalysts. The reaction, which has been termed 'oxidative methylation', was thus postulated to involve a two-step mechanism involving intermediate methanol formation by methane partial oxidation, followed by benzene methylation with methanol in the second step. However, strongly acidic zeolites can cause cracking of benzene to yield methylated products in the absence of oxygen. The participation of methane and oxygen, and the effective use of zeolite catalysts in this methylation reaction definitely have some positive green chemistry implications. Thus, the results of these previous studies are also discussed in this review in light of the principles and tools of green chemistry. Various metrics were used to evaluate the greenness, cost-effectiveness, and material and energy efficiency of the oxidative methylation reaction.

  11. Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

    2017-07-01

    A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Microwave-Assisted Synthesis of Boron and Nitrogen co-doped Reduced Graphene Oxide for the Protection of Electromagnetic Radiation in Ku-Band.

    Science.gov (United States)

    Umrao, Sima; Gupta, Tejendra K; Kumar, Shiv; Singh, Vijay K; Sultania, Manish K; Jung, Jung Hwan; Oh, Il-Kwon; Srivastava, Anchal

    2015-09-09

    The electromagnetic interference (EMI) shielding of reduced graphene oxide (MRG), B-doped MRG (B-MRG), N-doped MRG (N-MRG), and B-N co-doped MRG (B-N-MRG) have been studied in the Ku-band frequency range (12.8-18 GHz). We have developed a green, fast, and cost-effective microwave assisted route for synthesis of doped MRG. B-N-MRG shows high electrical conductivity in comparison to MRG, B-MRG and N-MRG, which results better electromagnetic interference (EMI) shielding ability. The co-doping of B and N significantly enhances the electrical conductivity of MRG from 21.4 to 124.4 Sm(-1) because N introduces electrons and B provides holes in the system and may form a nanojunction inside the material. Their temperature-dependent electrical conductivity follows 2D-variable range hopping (2D-VRH) and Efros-Shklovskii-VRH (ES-VRH) conduction model in a low temperature range (T<50 K). The spatial configuration of MRG after doping of B and N enhances the space charge polarization, natural resonance, dielectric polarization, and trapping of EM waves by internal reflection leading to a high EMI shielding of -42 dB (∼99.99% attenuation) compared to undoped MRG (-28 dB) at a critical thickness of 1.2 mm. Results suggest that the B-N-MRG has great potential as a candidate for a new type of EMI shielding material useful in aircraft, defense industries, communication systems, and stealth technology.

  13. The physicochemical properties of microwave-assisted encapsulated anthocyanins from Ipomoea batatas as affected by different wall materials

    Science.gov (United States)

    Mohd Nawi, Norazlina; Muhamad, Ida Idayu; Mohd Marsin, Aishah

    2015-01-01

    This study focuses on the impact of different wall materials on the physicochemical properties of microwave-assisted encapsulated anthocyanins from Ipomoea batatas. Using the powder characterization technique, purple sweet potato anthocyanin (PSPAs) powders were analysed for moisture content, water activity, dissolution time, hygroscopicity, color and morphology. PSPAs were produced using different wall materials: maltodextrin (MD), gum arabic (GA) and a combination of gum arabic and maltodextrin (GA + MD) at a 1:1 ratio. Each of the wall materials was homogenized to the core material at a core/wall material ratio of 5 and were microencapsulated by microwave-assisted drying at 1100 W. Results indicated that encapsulated powder with the GA and MD combination presented better quality of powder with the lowest value of moisture content and water activity. With respect to morphology, the microcapsule encapsulated with GA + MD showed several dents in coating surrounding its core material, whereas other encapsulated powders showed small or slight dents entrapped onto the bioactive compound. Colorimetric analysis showed changes in values of L, a*, b*, hue and chroma in the reconstituted powder compared to the initial powder. PMID:25838887

  14. 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. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Microwave-assisted formulation of solid lipid nanoparticles loaded with non-steroidal anti-inflammatory drugs.

    Science.gov (United States)

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

    2016-12-30

    Stearic acid-based solid lipid nanoparticles (SLNs) were prepared using the microwave assisted one-pot microemulsions procedure pioneered by our group. In this study, non-steroidal anti-inflammatory drugs (NSAIDs) including indomethacin, ketoprofen and nimesulide were selected as ideal "test" drugs, based on their poor water solubility. The model drugs were incorporated within the SLNs by the microwave-assisted procedure at the time of SLN production. The microwave-produced drug-loaded SLNs were evaluated in terms of their physicochemical characteristics, drug release behavior and their uptake into against A549 cell line (human lung epithelial cells). The microwave-produced drug-loaded SLNs had a small particle size distribution, negative zeta potential and high encapsulation efficiency. The drug release studies were consistent with a core-shell structure of SLNs (probably a drug-loaded shell) which results in biphasic drug release from the SLNs. The drug release kinetics suggested a good fit of the release data to the Makoid-Banakar model and was governed by Fickian diffusion. The drug-loaded SLNs showed concentration-dependent cytotoxicity and reduced IL-6 and IL-8 secretion in lipopolysaccharide-induced cells. All of the above findings suggest that the microwave-produced SLNs could be promising drug carriers of NSAIDs and will further facilitate their development for topical, oral and/or nasal administration. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. The physicochemical properties of microwave-assisted encapsulated anthocyanins from Ipomoea batatas as affected by different wall materials.

    Science.gov (United States)

    Mohd Nawi, Norazlina; Muhamad, Ida Idayu; Mohd Marsin, Aishah

    2015-03-01

    This study focuses on the impact of different wall materials on the physicochemical properties of microwave-assisted encapsulated anthocyanins from Ipomoea batatas. Using the powder characterization technique, purple sweet potato anthocyanin (PSPAs) powders were analysed for moisture content, water activity, dissolution time, hygroscopicity, color and morphology. PSPAs were produced using different wall materials: maltodextrin (MD), gum arabic (GA) and a combination of gum arabic and maltodextrin (GA + MD) at a 1:1 ratio. Each of the wall materials was homogenized to the core material at a core/wall material ratio of 5 and were microencapsulated by microwave-assisted drying at 1100 W. Results indicated that encapsulated powder with the GA and MD combination presented better quality of powder with the lowest value of moisture content and water activity. With respect to morphology, the microcapsule encapsulated with GA + MD showed several dents in coating surrounding its core material, whereas other encapsulated powders showed small or slight dents entrapped onto the bioactive compound. Colorimetric analysis showed changes in values of L, a*, b*, hue and chroma in the reconstituted powder compared to the initial powder.

  17. 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.

  18. Microwave assisted synthesis of camellia oleifera shell-derived porous carbon with rich oxygen functionalities and superior supercapacitor performance

    Science.gov (United States)

    Liang, Jiyuan; Qu, Tingting; Kun, Xiang; Zhang, Yu; Chen, Shanyong; Cao, Yuan-Cheng; Xie, Mingjiang; Guo, Xuefeng

    2018-04-01

    Biomass-derived carbon (BDCs) materials are receiving extensive attention as electrode materials for energy storage because of the considerable economic value offering possibility for practical applications, but the electrochemical capacitance of BDCs are usually relatively low resulted from limited electric double layer capacitance. Herein, an oxygen-rich porous carbon (KMAC) was fabricated through a rapid and convenient microwave assisted carbonization and KOH activation of camellia oleifera shell. The obtained KMAC possesses three-dimensional porous architecture, large surface area (1229 m2/g) and rich oxygen functionalities (C/O ratio of 1.66). As the electrode materials for supercapacitor, KMAC exhibits superior supercapacitive performances as compared to the activated carbon (KAC) derived from direct carbonization/KOH activation method in 2.0 M H2SO4 (315 F/g vs. 202 F/g) and 6.0 M KOH (251 F/g vs. 214 F/g) electrolyte due to the rich oxygen-containing functional groups on the surface of porous carbon resulted from the developed microwave-assisted carbonization/activation approach.

  19. Green conversion of graphene oxide to graphene nanosheets and its biosafety study.

    Directory of Open Access Journals (Sweden)

    Adhiraj Dasgupta

    Full Text Available Chemical reduction of graphene oxide (GO to graphene employs the use of toxic and environmentally harmful reducing agents, hindering mass production of graphene which is of tremendous technological importance. In this study we report a green approach to the synthesis of graphene, bio-reduced by crude polysaccharide. The polysaccharide reduces exfoliated GO to graphene at room temperature in an aqueous medium. Transmission electron microscopy image provides clear evidence for the formation of few layer graphene. Characterization of the resulting polysaccharide reduced GO by Raman spectroscopy, Fourier transform infrared spectroscopy and Energy dispersive X-ray analysis confirms reduction of GO to graphene. We also investigated the degree of biosafety of the reduced GO and found it to be safe under 100 μg/ml.

  20. A facile microwave assisted green chemical synthesis of novel piperidino 2-thioxoimidazolidin-4-ones and their in vitro microbiological evaluation.

    Science.gov (United States)

    Kanagarajan, V; Thanusu, J; Gopalakrishnan, M

    2011-02-01

    A series of novel hybrid heterocyclic compounds, 3-(3-alkyl-2,6-diarylpiperin-4-ylidene)-2-thioxoimidazolidin-4-ones were synthesised and a comparative study was also carried out under microwave irradiation. The synthesised compounds were characterised by their melting points, elemental analysis, MS, FT-IR, one-dimensional NMR (1H, D(2)O exchanged 1H and (13)C), two dimensional HOMOCOSY and NOESY spectroscopic data. All the synthesised title compounds were screened for their in vitro antibacterial and antifungal activity against clinically isolated strains namely B. subtilis, M. luteus, S. typhii, S. paratyphii B, S. felxneri, P. vulgaris, A. niger, Mucor, Rhizopus and M. gypsuem and the results were discussed.

  1. Carbon dioxide conversion to fuels and chemicals using a hybrid green process

    International Nuclear Information System (INIS)

    Ramachandriya, Karthikeyan D.; Kundiyana, Dimple K.; Wilkins, Mark R.; Terrill, Jennine B.; Atiyeh, Hasan K.; Huhnke, Raymond L.

    2013-01-01

    Highlights: • A unique CO 2 conversion technology using microorganisms was demonstrated. • Corn steep liquor medium enhanced production of n-butanol and n-hexanol. • Cotton seed extract (CSE) medium promoted ethanol formation. • CSE medium without morpholinoethanesulfonic acid buffer reduced the cost by 99%. - Abstract: A unique hybrid technology that uses renewable hydrogen (H 2 ) and carbon dioxide (CO 2 ) sequestered from large point sources, to produce fuels and chemicals has been proposed and tested. The primary objective of this research was to determine the feasibility of using two acetogenic bacteria to metabolize H 2 and CO 2 for the production of ethanol. Three experiments were conducted in small scale reactors to select a bacterium, feed gas composition and nutrient medium source to produce ethanol. The results indicated that Clostridium carboxidivorans produced 33% more ethanol and 66% less acetic acid compared to Clostridium ragsdalei, making C. carboxidivorans the better candidate for ethanol production. Furthermore, the removal of morpholinoethanesulfonic acid (MES) buffer from cotton seed extract (CSE) medium offered a low-cost medium for fermentations. Additionally, we observed that corn steep liquor (CSL) in the medium diversified the product range with both bacteria. Maximum concentrations of ethanol, n-butanol, n-hexanol, acetic acid, butyric acid, and hexanoic acid from different fermentation treatments were 2.78 g L −1 , 0.70 g L −1 , 0.52 g L −1 , 4.06 g L −1 , 0.13 g L −1 and 0.42 g L −1 , respectively. This study highlights the important role that acetogenic microbes can offer for CO 2 conversion into valuable fuels and chemicals

  2. Process optimisation of microwave-assisted extraction of peony ( Paeonia suffruticosa Andr .) seed oil using hexane-ethanol mixture and its characterisation

    Science.gov (United States)

    Xiaoli Sun; Wengang Li; Jian Li; Yuangang Zu; Chung-Yun Hse; Jiulong Xie; Xiuhua Zhao

    2016-01-01

    Ethanol and hexane mixture agent microwave-assisted extraction (MAE) method was conducted to extract peony (Paeonia suffruticosa Andr.) seed oil (PSO). The aim of the study was to optimise the extraction for both yield and energy consumption in mixture agent MAE. The highest oil yield (34.49%) and lowest unit energy consumption (14 125.4 J g -1)...

  3. CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS: JOURNAL ARTICLE

    Science.gov (United States)

    NRMRL-CIN-1437 Jeselnik, M., Varma*, R.S., Polanc, S., and Kocevar, M. Catalyst-free Reactions under Solvent-fee Conditions: Microwave-assisted Synthesis of Heterocyclic Hydrazones below the Melting Point of Neat Reactants. Published in: Chemical Communications 18:1716-1717 (200...

  4. Mathematical modeling and Monte Carlo simulation of thermal inactivation of non-proteolytic Clostridium botulinum spores during continuous microwave-assisted pasteurization

    Science.gov (United States)

    The objective of this study is to develop a mathematical method to simulate the internal temperature history of products processed in a prototype microwave-assisted pasteurization system (MAPS) developed by Washington State University. Two products (10 oz. beef meatball trays and 16 oz. salmon fill...

  5. 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...

  6. One-pot Microwave-Assisted Synthesis of 1H-Phenanthro[9,10- d][1,2,3]triazole

    Directory of Open Access Journals (Sweden)

    Mehrak Faraji

    2008-09-01

    Full Text Available In this study, a fast and good yield one-pot microwave-assisted synthesis (45 seconds of 1H-phenanthro[9,10-d][1,2,3]triazole by a 1,3-dipolar cycloaddition reaction of sodium azide and 9-bromophenanthrene in the presence of potassium tert-butoxide in DMSO as solvent is reported.

  7. 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.

  8. Microwave Assisted Synthesis and Antimicrobial Activities of Some 2-Amino-4-aryl-3-cyano-6-(4’-hydroxy phenyl-pyridines

    Directory of Open Access Journals (Sweden)

    Priya Gothwal

    2011-01-01

    Full Text Available 4’-Hydroxy chalcones were treated with malononitrile in the presence of ammonium acetate under solventless microwave assisted condition to get 2-amino-4-aryl-3-cyano-6-(4’-hydroxy phenyl-pyridines. The prepared compounds were screened for their antimicrobial activity; some of them have exhibited promising antimicrobial activity.

  9. Optical and morphological properties of ZnO- and TiO2-derived nanostructures synthesized via a microwave-assisted hydrothermal method

    CSIR Research Space (South Africa)

    Moloto, N

    2012-01-01

    Full Text Available A microwave-assisted hydrothermal method was used to synthesize ZnO and TiO2 nanostructures. The experimental results show that the method resulted in crystalline monodispersed ZnO nanorods that have pointed tips with hexagonal crystal phase. TiO2...

  10. Microwave-Assisted Adsorptive Desulfurization of Model Diesel Fuel Using Synthesized Microporous Rare Earth Metal-Doped Zeolite Y

    Directory of Open Access Journals (Sweden)

    N. Salahudeen

    2015-06-01

    Full Text Available The microwave-assisted adsorptive desulfurization of model fuel (thiophene in n-heptane was investigated using a synthesized rare earth metal-doped zeolite Y (RE Y. Crystallinity of the synthesized zeolite was 89.5%, the silicon/aluminium (Si/Al molar ratio was 5.2, the Brunauer–Emmett–Teller (BET surface area was 980.9 m2/g, and the pore volume and diameter was 0.3494 cm3/g and 1.425 nm, respectively. The results showed that the microwave reactor could be used to enhance the adsorptive desulfurization process with best efficiency of 75% at reaction conditions of 100 °C and 15 minutes. The high desulfurization effect was likely due to the higher efficiency impact of microwave energy in the interaction between sulfur in thiophene and HO-La(OSiAl.

  11. Scavenging remazol brilliant blue R dye using microwave-assisted activated carbon from acacia sawdust: Equilibrium and kinetics studies

    Science.gov (United States)

    Yusop, M. F. M.; Aziz, H. A.; Ahmad, M. A.

    2017-10-01

    This work explores the feasibility of microwave-assisted acacia wood based activated carbon (AWAC) for remazol brilliant blue R (RBBR) dye removal from synthetic wastewater. Acacia wood (AW) was impregnated with potassium hydroxide (KOH) and heated using microwave, resulting tremendously high fixed carbon content, surface area, total pore volume and adsorption capacity of 81.14%, 1045.56m2/g, 0.535cm3/g and 263.16mg/g respectively. Batch study conducted divulged an increasing trend in RBBR uptake when initial RBBR concentration and contact time were increased. pH study revealed that RBBR adsorption was best at acidic condition. Langmuir isotherm model fitted well the adsorption equilibrium data while the adsorption kinetic was found to follow the pseudo-second-order kinetic model.

  12. Determination of flumequine and oxolinic acid in sediments and soils by microwave-assisted extraction and liquid chromatography-fluorescence

    International Nuclear Information System (INIS)

    Prat, M.D.; Ramil, D.; Compano, R.; Hernandez-Arteseros, J.A.; Granados, M.

    2006-01-01

    A method is reported for the determination of the quinolones oxolinic acid and flumequine in aquatic sediments and agricultural soils. The analytes are extracted by liquid-liquid partitioning between a sample homogenated in an aqueous buffer solution and dichloromethane. Microwave-assisted extraction (MAE) was tested to improve the speed and efficiency of the extraction process. The parameters affecting the efficiency of MAE, such as irradiation time and temperature, were studied. The clean-up consists of back-extraction in 1 M sodium hydroxide. The determination is carried out by reversed phase liquid chromatography on an octyl silica-based column and fluorimetric detection. The optimised method was applied to the analysis of two sediments and one agricultural soil spiked with the analytes. The absolute recovery rates for the whole process range from 79% to 94% (RSD 3-7%), and detection limits are in the low μg kg -1 level

  13. Sequential microwave-assisted extraction of oil from layer poultry feeds and GC-MS quantification of the fatty acids

    International Nuclear Information System (INIS)

    Mahesar, S.A.; Sherazi, S.T.H.; Bhanger, M.I.; Abro, K.; Kandhro, A.A.

    2010-01-01

    The present study reports the effect of sequential microwave-assisted extraction (SeMAE) on fatty acids composition (FAC) of layer poultry feed oil as compared to conventional Soxhlet extraction (SE) method. The FAC of extracted oil was determined by gas chromatography - mass spectrometry (GC-MS). There was no significant difference found in the amount of total extracted oil and FAC by SeMAE and SE. However, slightly greater content of trans fat in the samples revealed that SE lead to the formation of a little higher level of trans fat as compare to SeMAE. Therefore, the SeMAE could be used as a remarkable substitute to conventional SE for extraction of oil from the poultry feeds due to its faster speed, lesser solvent consumption, more environmental friendly. (author)

  14. Microwave-Assisted Synthesis of CuFe2O4 Nanoparticles and Starch-Based Magnetic Nanocomposites

    Directory of Open Access Journals (Sweden)

    Gh. Nabiyouni

    2013-06-01

    Full Text Available Magnetic CuFe2O4 nanoparticles were synthesized by a facile microwave-assisted reaction between Cu(NO32 and Fe(NO33. The magnetic nanoparticles were added to starch to make magnetic polymeric nanocomposite. The nanoparticles and nanocomposites were characterized using X-ray diffraction and scanning electron microscopy. The magnetic properties of the samples were investigated using an alternating gradient force magnetometer (AGFM. The copper ferrite nanoparticles exhibited ferromagnetic behavior at room temperature, with a saturation magnetization of 29emu/g and a coercivity of 136 Oe. The distribution of the CuFe2O4 nanoparticles into the polymeric matrixes decreases the coercivity (136 Oe to 66 Oe. The maximum coercivity of 82 Oe was found for 15% of CuFe2O4 distributed to the starch matrix.

  15. Microwave assisted synthesis of porous ZnO/SnS heterojunction and its application in visible light degradation of ciprofloxacin

    Energy Technology Data Exchange (ETDEWEB)

    Makama, A. B., E-mail: abmakama@hotmail.com; Salmiaton, A., E-mail: mie@upm.edu.my; Choong, T. S. Y., E-mail: csthomas@upm.edu.my; Abdullah, N., E-mail: nhafizah@upm.edu.my [Department of Chemical and Environmental Engineering, Faculty of Engineering, Universiti Putra Malaysia, Selangor, Serdang, UPM 43400 (Malaysia); Saion, E. B., E-mail: elias@upm.edu.my [Department of Physics, Faculty of Science, Universiti Putra Malaysia, Selangor, Serdang, UPM 43400 (Malaysia)

    2016-07-06

    Porous ZnO/SnS heterojunctions were successfully synthesized via microwave-assisted heating of aqueous solutions containing different amounts of SnS precursors (SnCl{sub 2} and Na{sub 2}S) in the presence of fixed amount of ZnCO{sub 3} nanoparticles. The experimental results revealed that the heterojunctions exhibited much higher visible light-driven photocatalytic activity for the degradation of the ciprofloxacin than pure SnS nanocrystals. The photocatalytic degradation efficiency (1-C{sub t}/C{sub 0}) of the pollutant for the most active heterogeneous nanostructure is about four times more efficient than pure SnS. The enhanced photocatalytic efficiency is ascribed to the synergic effect of high photon absorption and reduction in the recombination of electrons and holes because of efficient separation and electron transfer from the SnS to ZnO nanoparticles.

  16. A facile microwave assisted one pot synthesis of novel xanthene derivatives as potential anti-inflammatory and analgesic agents

    Directory of Open Access Journals (Sweden)

    Anupam G. Banerjee

    2016-09-01

    Full Text Available Microwave assisted irradiation of resorcinol and substituted aryl aldehydes using sulfamic acid as catalyst afforded novel 9-aryl-9H-xanthene-3,6-diol derivatives (1a–f in good yields. The newly synthesized compounds which were previously selected on the basis of PASS prediction were tested for anti-inflammatory activity using carrageenan-induced rat paw edema and analgesic activity using acetic acid induced writhing and formalin-induced paw edema in mice along with the estimation of gastric ulcerogenicity index. Compounds 1e and 1f exhibited significant anti-inflammatory and analgesic activities as compared to standard drug. The study also revealed that compounds (1a–f showed minimum or no ulcerogenicity in mice as that of the standard drug.

  17. Study of the feasibility of focused microwave-assisted soxhlet extraction of N-methylcarbamates from soil.

    Science.gov (United States)

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

    2002-04-12

    A study of the feasibility of a focused microwave-assisted Soxhlet device for the extraction of N-methylcarbamates from soil has been performed. The main factors contributing to the extraction efficiency-namely microwave power, irradiation time and number of cycles--were optimized by means of a two-level full factorial design. The extracts were analysed by HPLC-post-column fluorescence derivatization-detection at excitation wavelength 340 nm and emission wavelength 445 nm. The method has allowed the extraction of carbamate pesticides from contaminated soil with quantitative recoveries, similar to those provided by the US Environmental Protection Agency method 8318, without degradation of the target compounds during the extraction and using less organic solvent, as 75-80% of the extractant was recycled.

  18. Sequential Microwave-Assisted Extraction of Oil from Layer Poultry Feeds and GC-MS Quantification of the Fatty Acids

    Directory of Open Access Journals (Sweden)

    S. A. Mahesar

    2010-06-01

    Full Text Available The present study reports the effect of sequential microwave-assisted extraction (SeMAE on fatty acids composition (FAC of layer poultry feed oil as compared to conventional Soxhlet extraction (SE method. The FAC of extracted oil was determined by gas chromatography–mass spectrometry (GC-MS. There was no significant difference found in the amount of total extracted oil and FAC by SeMAE and SE. However, slightly greater content of trans fat in the samples revealed that SE lead to the formation of a little higher level of trans fat as compare to SeMAE. Therefore, the SeMAE could be used as a remarkable substitute to conventional SE for extraction of oil from the poultry feeds due to its faster speed, lesser solvent consumption, more environmental friendly.

  19. Determination of inorganic arsenic in white fish using microwave-assisted alkaline alcoholic sample dissolution and HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Engman, Joakim; Sloth, Jens Jørgen

    2005-01-01

    An analytical method for the determination of inorganic arsenic in fish samples using HPLC-ICP-MS has been developed. The fresh homogenised sample was subjected to microwave-assisted dissolution by sodium hydroxide in ethanol, which dissolved the sample and quantitatively oxidised arsenite (As......(V) at 104 +/- 7% (n=5) indicated good analytical accuracy. The uncertified inorganic arsenic content in the certified reference material TORT-2 was 0.186 +/- 0.014 ng g(-1) (n=6). The method was employed for the determination of total arsenic and inorganic arsenic in 60 fish samples including salmon from...... fresh and saline waters and in plaice. The majority of the results for inorganic arsenic were lower than the LOD of 3 ng g(-1), which corresponded to less than one per thousand of the total arsenic content in the fish samples. For mackerel, however, the recovery of As(III) was incomplete and the method...

  20. Microwave assisted preparation of n-butylacrylate grafted chitosan and its application for Cr(VI) adsorption.

    Science.gov (United States)

    Santhana Krishna Kumar, A; Uday Kumar, Chinta; Rajesh, Vidya; Rajesh, N

    2014-05-01

    Biopolymers such as chitosan possess excellent properties suited for varied applications. In this work, we describe a novel microwave assisted method for the preparation of n-butylacrylate grafted chitosan adsorbent and its utility for the adsorption of chromium(VI). A 3 min irradiation time was enough to prepare the adsorbent, and techniques such as FT-IR, powder XRD, SEM and EDS were used for comprehensive characterization. The adsorption was effective at pH 3.5 with 25 mL of 20 ppm Cr(VI) solution. Langmuir, Freundlich, Dubinin-Radushkevich, Temkin, Elovich and Redlich isotherms were studied in detail. The ΔG, ΔH and ΔS parameters were evaluated to understand the adsorption thermodynamics. The adsorption involves the interaction of Cr(VI) with the hydroxyl and amino groups in chitosan. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Innovative biofilm inhibition and anti-microbial behavior of molybdenum sulfide nanostructures generated by microwave-assisted solvothermal route

    Science.gov (United States)

    Qureshi, Nilam; Patil, Rajendra; Shinde, Manish; Umarji, Govind; Causin, Valerio; Gade, Wasudev; Mulik, Uttam; Bhalerao, Anand; Amalnerkar, Dinesh P.

    2015-03-01

    The incessant use of antibiotics against infectious diseases has translated into a vicious circle of developing new antibiotic drug and its resistant strains in short period of time due to inherent nature of micro-organisms to alter their genes. Many researchers have been trying to formulate inorganic nanoparticles-based antiseptics that may be linked to broad-spectrum activity and far lower propensity to induce microbial resistance than antibiotics. The way-out approaches in this direction are nanomaterials based (1) bactericidal and (2) bacteriostatic activities. We, herein, present hitherto unreported observations on microbial abatement using non-cytotoxic molybdenum disulfide nanostructures (MSNs) which are synthesized using microwave assisted solvothermal route. Inhibition of biofilm formation using MSNs is a unique feature of our study. Furthermore, this study evinces antimicrobial mechanism of MSNs by reactive oxygen species (ROS) dependent generation of superoxide anion radical via disruption of cellular functions.

  2. Microwave-assisted synthesis of TiO2 nanoparticles: photocatalytic activity of powders and thin films

    Science.gov (United States)

    Falk, G. S.; Borlaf, M.; López-Muñoz, M. J.; Fariñas, J. C.; Rodrigues Neto, J. B.; Moreno, R.

    2018-02-01

    A simple, rapid, and effective synthesis methodology for the preparation of high-performance TiO2 nanoparticles and thin films by combining colloidal sol-gel and microwave-assisted hydrothermal synthesis was developed. The obtained results indicate that the heating with microwaves at 180 °C for 20 min was enough to synthesize crystalline TiO2 nanoparticles, presenting anatase as a major phase with a crystal size of 7 nm and a specific surface area of 220 m2 g-1. A secondary thermal treatment improved the crystallinity and induced the anatase-to-rutile transformation. The highest photocatalytic activity was found for the as-synthesized powder without any additional thermal treatment. Thin films were also prepared by dip-coating and its high photocatalytic activity showed a kinetic curve comparable to that of a thin film of commercial TiO2 powder prepared under similar conditions.

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

    Science.gov (United States)

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

    2015-12-01

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

  4. Decentralized energy conversion of biomass from Amstelland. The feasibility of decentralized use of energy from green wastes in the municipality Amstelveen and its environs

    International Nuclear Information System (INIS)

    Brouwer, H.D.

    1997-10-01

    The aim of the study on the title subject is to determine the enviro-technical and economical feasibility of decentralized biomass conversion as part of the green area and energy infrastructure of the region Amstelland, Netherlands. The parts of the study concern a regional inventory of green wastes in Amstelland, an energy demand analysis of conversion sites in the region, a logistic analysis, an evaluation of technical options (cogeneration, combustion, gasification), business economical analysis of the investments, determining the support and willingness to contribute and cooperate, and drafting a final report. Based on the results of the report decisions can be made whether or not the design and installation of a decentralized biomass conversion system should be elaborated in detail. 16 refs

  5. 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.

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

    Science.gov (United States)

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

  7. Microwave-assisted synthesis of graphene-Prussian Blue networked nanocomposites for electrocatalysis

    DEFF Research Database (Denmark)

    Zhang, Minwei; Ulstrup, Jens; Chi, Qijin

    There has been a great deal of interest recently in Prussian blue functional graphene. Due to they displayed advantage of both Prussian blue and graphene, we presented a one-pot and green method to synthesize interlocked graphene-Prussian Blue nanocomposites. Considering that graphene oxide (GO...

  8. Microwave-assisted extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs) used to indoor air monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Esteve-Turrillas, Francesc A. [Analytical Chemistry Department, University of Valencia, Edifici Jeroni Munoz, 50th Dr. Moliner, 46100 Burjassot, Valencia (Spain); Pastor, Agustin [Analytical Chemistry Department, University of Valencia, Edifici Jeroni Munoz, 50th Dr. Moliner, 46100 Burjassot, Valencia (Spain)]. E-mail: agustin.pastor@uv.es; Guardia, Miguel de la [Analytical Chemistry Department, University of Valencia, Edifici Jeroni Munoz, 50th Dr. Moliner, 46100 Burjassot, Valencia (Spain)

    2006-02-23

    A rapid and environmentally friendly methodology was developed for the extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs), in which they were preconcentrated in gas phase. The method was based on gas chromatography mass-mass spectrometry determination after a microwave-assisted extraction, in front of the widely employed dialysis method. SPMDs were extracted twice with 30 mL hexane:acetone, irradiated with 250 W power output, until 90 deg. C in 10 min, this temperature being held for another 10 min. Clean-up of the extracts was performed by acetonitrile-hexane partitioning and solid-phase extraction (SPE) with a combined cartridge of 2 g basic-alumina, deactivated with 5% water, and 500 mg C{sub 18}. Pyrethroids investigated were Allethrin, Prallethrin, Tetramethrin, Bifenthrin, Phenothrin, {lambda}-Cyhalothrin, Permethrin, Cyfluthrin, Cypermethrin, Flucythrinate, Esfenvalerate, Fluvalinate and Deltamethrin. The main pyrethroid synergist compound, Pyperonyl Butoxide, was also studied. Limit of detection values ranging from 0.3 to 0.9 ng/SPMD and repeatability data, as relative standard deviation, from 2.9 to 9.4%, were achieved. Pyrethroid recoveries, for spiked SPMDs, with 100 ng of each one of the pyrethroids evaluated, were from 61 {+-} 8 to 103 {+-} 7% for microwave-assisted extraction, versus 54 {+-} 4 to 104 {+-} 3% for dialysis reference method. Substantial reduction of solvent consumed (from 400 to 60 mL) and analysis time (from 48 to 1 h) was achieved by using the developed procedure. High concentration levels of pyrethroid compounds, from 0.14 to 7.3 {mu}g/SPMD, were found in indoor air after 2 h of a standard application.

  9. Microwave-assisted one-pot synthesis of metal/metal oxide nanoparticles on graphene and their electrochemical applications

    International Nuclear Information System (INIS)

    Wang Shuangyin; Jiang San Ping; Wang Xin

    2011-01-01

    Graphical abstract: Display Omitted Research highlights: → Microwave polyol method is efficient to deposit nanoparticles on graphene. → SnO 2 /graphene is more efficient than graphene for supercapacitor. → PtRu/graphene is more active than commercial PtRu/C for methanol oxidation. - Abstract: An effective synthesis strategy of hybrid metal (PtRu)/metal oxide (SnO 2 ) nanoparticles on graphene nanocomposites is developed using a microwave-assisted one-pot reaction process. The mixture of ethylene glycol (EG) and water is used as both solvent and reactant. In the reaction system for the synthesis of SnO 2 /graphene nanocomposite, EG not only reduces graphene oxide (GO) to graphene, but also results in the formation of SnO 2 facilitated by the presence of a small amount of water. On the other hand, in the reaction system for preparation of PtRu/graphene nanocomposites, EG acts as solvent and reducing agent for reduction of PtRu nanoparticles from their precursors and reduction of graphene from graphene oxide. Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) characterizations confirm the feasibility of the microwave-assisted reaction system to simultaneously reduce graphene oxide and to form SnO 2 or PtRu nanoparticles. The as-synthesized SnO 2 /graphene hybrid composites show a much higher supercapacitance than the pure graphene, and the as-prepared PtRu/graphene show much better electrocatalytic activity for methanol oxidation compared to the commercial E-TEK PtRu/C electrocatalysts.

  10. Computation of adsorption parameters for the removal of dye from wastewater by microwave assisted sawdust: Theoretical and experimental analysis.

    Science.gov (United States)

    S, Suganya; P, Senthil Kumar; A, Saravanan; P, Sundar Rajan; C, Ravikumar

    2017-03-01

    In this research, the microwave assistance has been employed for the preparation of novel material from agro/natural bio-waste i.e. sawdust, for the effective removal of methylene blue (MB) dye from aqueous solution. The characterization of the newly prepared microwave assisted sawdust (MASD) material was performed by using FTIR, SEM and XRD analyses. In order to obtain the maximum removal of MB dye from wastewater, the adsorption experimental parameters such as initial dye concentration, contact time, solution pH and adsorbent dosage were optimized by trial and error approach. The obtained experimental results were applied to the different theoretical models to predict the system behaviour. The optimum conditions for the maximum removal MB dye from aqueous solution for an initial MB dye concentration of 25mg/L was calculated as: adsorbent dose of 3g/L, contact time of 90min, solution pH of 7.0 and at the temperature of 30°C. Freundlich and pseudo-second order models was best obeyed with the studied experimental data. Langmuir maximum monolayer adsorption capacity of MASD for MB dye removal was calculated as 58.14mg of MB dye/g of MASD. Adsorption diffusion model stated that the present adsorption system was controlled by intraparticle diffusion model. The obtained results proposed that, novel MASD was considered to be an effective and low-cost adsorbent material for the removal of dye from wastewater. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Synthesis, Characterization, and Atenolol Delivery Application of Functionalized Mesoporous Hydroxyapatite Nanoparticles Prepared by Microwave-Assisted Co-precipitation Method.

    Science.gov (United States)

    Mortazavi-Derazkola, Sobhan; Naimi-Jamal, Mohammad Reza; Ghoreishi, Seyedeh Masoumeh

    2016-01-01

    Atenolol has been used to treat angina and hypertension, either alone or with other antihypertensives. Despite its usefulness, it shows some side effects such as diarrhea and nausea in some patients. A method for slow release of atenolol in intestine is helpful to prevent such side effects. A facile co-precipitation microwave-assisted method was used to fabricate mesoporous hydroxyapatite nanoparticles (mHAp). It was then functionalized to have SO3H groups. The synthesized material was used for storage/slow release study of atenolol. Atenolol loaded mHAp shows immediate release of atenolol in pH 8, whileafter functionalizing shows up to ca. 30% release at the beginning. In pH 1, 50% of drug was released after 10 h from AT@mHAp and after 18h the drug was almost completely released.The drug release profiles of functionalized HAp at pH value 1 and 8reveals the complete release of atenolol in intestine pH, while no complete release is observed in stomach environment. The aims of this work were synthesis and characterization of mesoporous HAp through the microwave-assisted co-precipitation method and elucidate the underlying drug release capability of mesoporous HAp nanoparticles. The SO3H group was incorporated into the mesoporous HAp and then used as drug delivery carriers using atenolol as a model drug to investigate their drug storage/release properties in simulated body fluid (SBF). Increasing pH value to 8 causes increase in the drug release.

  12. Microwave-assisted hydrothermal synthesis of CePO4 nanostructures: Correlation between the structural and optical properties

    International Nuclear Information System (INIS)

    Palma-Ramírez, D.; Domínguez-Crespo, M.A.; Torres-Huerta, A.M.; Dorantes-Rosales, H.; Ramírez-Meneses, E.; Rodríguez, E.

    2015-01-01

    Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO 4 is presented. • Microwave energy can replace the energy by convection for obtaining CePO 4 . • CePO 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 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 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 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 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 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

  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 extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs) used to indoor air monitoring

    International Nuclear Information System (INIS)

    Esteve-Turrillas, Francesc A.; Pastor, Agustin; Guardia, Miguel de la

    2006-01-01

    A rapid and environmentally friendly methodology was developed for the extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs), in which they were preconcentrated in gas phase. The method was based on gas chromatography mass-mass spectrometry determination after a microwave-assisted extraction, in front of the widely employed dialysis method. SPMDs were extracted twice with 30 mL hexane:acetone, irradiated with 250 W power output, until 90 deg. C in 10 min, this temperature being held for another 10 min. Clean-up of the extracts was performed by acetonitrile-hexane partitioning and solid-phase extraction (SPE) with a combined cartridge of 2 g basic-alumina, deactivated with 5% water, and 500 mg C 18 . Pyrethroids investigated were Allethrin, Prallethrin, Tetramethrin, Bifenthrin, Phenothrin, λ-Cyhalothrin, Permethrin, Cyfluthrin, Cypermethrin, Flucythrinate, Esfenvalerate, Fluvalinate and Deltamethrin. The main pyrethroid synergist compound, Pyperonyl Butoxide, was also studied. Limit of detection values ranging from 0.3 to 0.9 ng/SPMD and repeatability data, as relative standard deviation, from 2.9 to 9.4%, were achieved. Pyrethroid recoveries, for spiked SPMDs, with 100 ng of each one of the pyrethroids evaluated, were from 61 ± 8 to 103 ± 7% for microwave-assisted extraction, versus 54 ± 4 to 104 ± 3% for dialysis reference method. Substantial reduction of solvent consumed (from 400 to 60 mL) and analysis time (from 48 to 1 h) was achieved by using the developed procedure. High concentration levels of pyrethroid compounds, from 0.14 to 7.3 μg/SPMD, were found in indoor air after 2 h of a standard application

  15. Green Synthesis of Carvenone by Montmorillonite-Catalyzed Isomerization of 1,2-Limonene Oxide

    DEFF Research Database (Denmark)

    Nguyen, Thao-Tran Thi; Chau, Duy-Khiem Nguyen; Duus, Fritz

    2013-01-01

    Montmorillonite was considered as a good heterogeneous catalyst for the isomerization of 1,2-limonene oxide into car-venone under solvent-free condition. Both conventional heating and green activations were tested in this research. The microwave-assisted isomerization afforded carvenone in high...

  16. Nitration of Phenols Using Cu(NO[subscript 3])[subscript 2]: Green Chemistry Laboratory Experiment

    Science.gov (United States)

    Yadav, Urvashi; Mande, Hemant; Ghalsasi, Prasanna

    2012-01-01

    An easy-to-complete, microwave-assisted, green chemistry, electrophilic nitration method for phenol using Cu(NO[subscript 3])[subscript 2] in acetic acid is discussed. With this experiment, students clearly understand the mechanism underlying the nitration reaction in one laboratory session. (Contains 4 schemes.)

  17. Optimization for microwave-assisted direct liquefaction of bamboo residue in glycerol/methanol mixtures

    Science.gov (United States)

    Jiulong Xie; Jinqiu Qi; Chungyun Hse; Todd F. Shupe

    2015-01-01

    Bamboo residues were liquefied in a mixture of glycerol and methanol in the presence of sulfuric acid using microwave energy. We investigated the effects of liquefaction conditions, including glycerol/methanol ratio, liquefaction temperature, and reaction time on the conversion yield. The optimal liquefaction conditions were under the temperature of 120

  18. Reporter system for the detection of in vivo gene conversion: changing colors from blue to green using GFP variants.

    Science.gov (United States)

    Sommer, Jeffrey R; Alderson, Jon; Laible, Goetz; Petters, Robert M

    2006-06-01

    We have devised a system for the study of in vivo gene correction based on the detection of color variants of the green fluorescent protein (GFP) from the jellyfish Aequorea victoria. The intensity and spectra of the fluorescence emitted by the blue (BFP) and red-shifted (EGFP) variants of GFP differ from each other. We modified one nucleotide from an EGFP expression vector that we predicted would yield a blue variant (TAC-CAC, Tyr(66)-His(66)). Cells that were either transiently or stably transfected with the reporter system were used to test the functionality and feasibility of the detection of in vivo gene correction. A thio-protected single-stranded oligonucleotide designed to convert the genotype of the blue variant to that of the EGFP variant by the correction of a single base pair was delivered to the reporter cells using a variety of methodologies and strategies.Conversion events were easily observed using fluorescent microscopy because of the enhanced emission intensity and different spectra of the EGFP variant.

  19. Microwave-assisted direct synthesis of butene from high-selectivity methane

    Science.gov (United States)

    Lu, Yi-heng; Li, Kang; Lu, Yu-wei

    2017-12-01

    Methane was directly converted to butene liquid fuel by microwave-induced non-oxidative catalytic dehydrogenation under 0.1-0.2 MPa. The results show that, under microwave heating in a two-stage fixed-bed reactor, in which nickel powder and NiOx-MoOy/SiO2 are used as the catalyst, the methane-hydrogen mixture is used as the raw material, with no acetylene detected. The methane conversion is more than 73.2%, and the selectivity of methane to butene is 99.0%. Increasing the hydrogen/methane feed volume ratio increases methane conversion and selectivity. Gas chromatography/electron impact ionization/mass spectrometry chromatographic analysis showed that the liquid fuel produced by methane dehydrogenation oligomerization contained 89.44% of butene, and the rest was acetic acid, ethanol, butenol and butyric acid, and the content was 1.0-3.0 wt%.

  20. Gold film-catalysed benzannulation by Microwave-Assisted, Continuous Flow Organic Synthesis (MACOS

    Directory of Open Access Journals (Sweden)

    Gjergji Shore

    2009-07-01

    Full Text Available Methodology has been developed for laying down a thin gold-on-silver film on the inner surface of glass capillaries for the purpose of catalysing benzannulation reactions. The cycloaddition precursors are flowed through these capillaries while the metal film is being heated to high temperatures using microwave irradiation. The transformation can be optimized rapidly, tolerates a wide number of functional groups, is highly regioselective, and proceeds in good to excellent conversion.

  1. Aqueous microwaves assisted cross-coupling reactions applied to unprotected nucleosides.

    Directory of Open Access Journals (Sweden)

    CHRISTOPHE eLEN

    2015-02-01

    Full Text Available Nucleoside analogues have attracted much attention due to their potential biological activities. Amongst all synthetic nucleosides, C5-modified pyrimidines and C7- or C8-modified purines have mostly been prepared using palladium cross-coupling reactions and then studied as antitumoral and antiviral agents. Our objective is to focus this review on the Suzuki-Miyaura and on the Heck cross-couplings of nucleosides using microwave irradiations which are an alternative technology compatible with green chemistry and sustainable development.

  2. green

    Directory of Open Access Journals (Sweden)

    Elena Grigoryeva

    2011-02-01

    Full Text Available The “green” topic follows the “youngsters”, which is quite natural for the Russian language.Traditionally these words put together sound slightly derogatory. However, “green” also means fresh, new and healthy.For Russia, and for Siberia in particular, “green” architecture does sound new and fresh. Forced by the anxious reality, we are addressing this topic intentionally. The ecological crisis, growing energy prices, water, air and food deficits… Alexander Rappaport, our regular author, writes: “ It has been tolerable until a certain time, but under transition to the global civilization, as the nature is destroyed, and swellings of megapolises expand incredibly fast, the size and the significance of all these problems may grow a hundredfold”.However, for this very severe Siberian reality the newness of “green” architecture may turn out to be well-forgotten old. A traditional Siberian house used to be built on principles of saving and environmental friendliness– one could not survive in Siberia otherwise.Probably, in our turbulent times, it is high time to fasten “green belts”. But we should keep from enthusiastic sticking of popular green labels or repainting of signboards into green color. We should avoid being drowned in paper formalities under “green” slogans. And we should prevent the Earth from turning into the planet “Kin-dza-dza”.

  3. Bioengineering of photosynthetic membranes. Requirement of magnesium for the conversion of chlorophyllide a to chlorophyll a during the greening of etiochloroplasts in vitro

    Energy Technology Data Exchange (ETDEWEB)

    Daniell, H.; Rebeiz, C.A.

    1984-01-01

    The massive conversion of delta-aminolevulinic acid (ALA) to protochlorophyllide (Pchlide) and the massive conversion of chlorophyllide a (Chlide a) to chlorophyll a (Chl a) are two essential conditions for the ALA-dependent assembly of photosynthetic membranes in vitro. In this work, the authors describe the development of a cell-free system capable of the forementioned biosynthetic activities at rates higher than in vivo, for the first 2 h of dark-incubation. The cell-free system consisted of 1) etiochloroplasts prepared from kinetin and gibberellic-acid-pretreated cucumber cotyledons, and 2) cofactors and additives described elsewhere and which are needed for the massive conversion of ALA to Pchlide, 3) high concentrations of ATP, MgCl/sub 2/, and an isoprenol alcohol such as phytol, were required for the massive conversion of Chlide a to Chl a. An absolute and novel requirement of Mg/sup 2 +/ for the conversion of Chlide a to Chl a was also demonstrated. In addition to the role of phytol as a substrate for the conversion of Chlide a to Chl a, the data suggested that this alcohol may also be involved in the regulation of the reactions between ALA and Pchlide. It is proposed that during greening, the conversion of Chlide a to Chl a may follow different biosynthetic rates, having different substrate and cofactor requirements, depending on the stage of plastid development.

  4. 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.

  5. Statistical modeling/optimization and process intensification of microwave-assisted acidified oil esterification

    International Nuclear Information System (INIS)

    Ma, Lingling; Lv, Enmin; Du, Lixiong; Lu, Jie; Ding, Jincheng

    2016-01-01

    Highlights: • Microwave irradiation was employed for the esterification of acidified oil. • Optimization and modeling of the process was performed by RSM and ANN. • Both models have reliable prediction abilities but the ANN was superior over the RSM. • Membrane vapor permeation and in-situ dehydration were used to shift the equilibrium. • Two dehydration approaches improved the FFAs conversion rate by 20.0% approximately. - Abstract: The esterification of acidified oil with ethanol under microwave radiation was modeled and optimized using response surface methodology (RSM) and artificial neural network (ANN). The impacts of mass ratio of ethanol to acidified oil, catalyst loading, microwave power and reaction time are evaluated by Box-Behnken design (BBD) of RSM and multi-layer perceptron (MLP) of ANN. RSM combined with BBD shows the optimal conditions as catalyst loading of 5.85 g, mass ratio of ethanol to acidified oil of 0.35 (20.0 g acidified oil), microwave power of 328 W and reaction time of 98.0 min with the free fatty acids (FFAs) conversion of 78.57%. Both of the models are fitted well with the experimental data, however, ANN exhibits better prediction accuracy than RSM based on the statistical analyses. Furthermore, membrane vapor permeation and in-situ molecular sieve dehydration were investigated to enhance the esterification under the optimized conditions.

  6. On-line continuous sampling dynamic microwave-assisted extraction coupled with high performance liquid chromatographic separation for the determination of lignans in Wuweizi and naphthoquinones in Zicao.

    Science.gov (United States)

    Gao, Shiqian; You, Jingyan; Wang, Ying; Zhang, Rui; Zhang, Hanqi

    2012-03-01

    The on-line continuous sampling dynamic microwave-assisted extraction (on-line CSDMAE) coupled with high-performance liquid chromatographic separation and determination of the lignans in Wuweizi and naphthoquinones in Zicao was developed. The extraction, separation and determination of target analytes were simultaneously carried out. The experimental parameters, including type of extraction solvent, microwave extraction power, solvent flow rate, amount of sample and particle size of the sample, were evaluated by the univariate method and orthogonal screening. The detection limits for schisandrin A, schisantherin A, deoxyschizandrin, shikonin and β,β'-dimethylacrylshikonin are 0.86, 0.90, 0.27, 0.42 and 0.92 μg mL⁻¹, respectively. Compared with the conventional extraction methods, such as off-line continuous microwave-assisted extraction, ultrasound-assisted extraction and Soxhlet extraction, the proposed method is quicker and more effective. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Determination of hexabromocyclododecane diastereoisomers in Sargassum fusiforme and comparison of the extraction efficiency of ultrasonication, microwave-assisted extraction, Soxhlet extraction and pressurised liquid extraction.

    Science.gov (United States)

    Han, Chao; Chen, Xiaomei; Xie, Wen; Zhu, Zhenou; Liu, Cuiping; Chen, Fan; Shen, Yan

    2010-11-01

    The concentrations of hexabromocyclododecanes (HBCD) in Sargassum fusiforme, the common Chinese edible seaweed, were investigated by LC-MS/MS. For the recovery of HBCD, the efficiency levels of ultrasonic-assisted extraction, microwave-assisted extraction, Soxhlet extraction and pressurised liquid extraction were compared under different conditions. Pressurised liquid extraction and ultrasonic-assisted extraction resulted in complete extraction of HBCD (92.7-102.5% recovery). Microwave-assisted extraction and Soxhlet extraction, on the other hand, offered relatively low extraction recoveries (82.1-90.6%). The instrumental LODs on columns in this study were 1.0, 0.3 and 0.7 ng/g for α-HBCD, β-HBCD and γ-HBCD, respectively. Because of its accuracy, this straightforward method is particularly suitable for routine HBCD analysis.

  8. Ionic Liquid-Based Vacuum Microwave-Assisted Extraction Followed by Macroporous Resin Enrichment for the Separation of the Three Glycosides Salicin, Hyperin and Rutin from Populus Bark

    OpenAIRE

    Fengli Chen; Kailin Mo; Zhaizhi Liu; Fengjian Yang; Kexin Hou; Shuangyang Li; Yuangang Zu; Lei Yang

    2014-01-01

    An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved,...

  9. Optimization of Microwave-assisted Extraction of Silymarin fromSilybum marianumStraws by Response Surface Methodology and Quantification by High-Performance Liquid Chromatograph Method.

    Science.gov (United States)

    Ruan, Hong-Sheng; Zhang, Hai-Feng; Teng, Kun

    2018-01-01

    Silybum marianum , a member of the Aster family, is a well-known Chinese herb and the source of a popular antioxidant that is extensively used in Asia. The abundant S. marianum straws are still underutilized and wastefully discarded to pollute the environment. To solve the above problem and better utilize S. marianum straws, the objective of this study was to optimize the conditions for extraction of silymarin from S. marianum straws. A combination of microwave-assisted extraction and response surface methodology (RSM) was used for silymarin from S. marianum straws and yield assessment by high-performance liquid chromatography method. The RSM was based on a five-level, four-variable central composite design (CCD). The results indicated that the optimal conditions to obtain highest yields of silymarin were microwave power of 146 W, extraction time of 117 s, liquid-to-solid ratio of 16:1 mL/g, and ethanol concentration of 43% (v/v). Validation tests indicated that under the optimized conditions, the actual yield of silymarin was 6.83 ± 0.57 mg/g with relative standard deviation of 0.92% ( n = 5), which was in good agreement with the predicted yield. The exploitation of the natural plant resources present very important impact for the economic development. The knowledge obtained from this work should be useful to further exploit and apply this material. Silymarin has been isolated from Silybum marianum straws by microwave-assisted extraction and response surface methodologyThe results obtained are helpful for the full utilization of S. marianum strawsThe microwave-assisted extraction is a very useful method for the extraction of important phytochemicals from plant materials. Abbreviations used: MAE: Microwave-assisted extraction, RSM: Response surface methodology, HPLC: High-performance liquid chromatography, CCD: Central composite design, ANOVA: Analysis of variance.

  10. Microwave-assisted hydrothermal synthesis of highly luminescent ZnSe-based quantum dots with a quantum yield higher than 90%

    Science.gov (United States)

    Lee, Yong-Shin; Nakano, Kaoru; Bu, Hang-Beom; Gwi Kim, Dae

    2017-06-01

    Highly luminescent ZnSe-based quantum dots (QDs) were synthesized by a microwave-assisted hydrothermal method. The characteristics of the ZnSe precursor solution strongly influenced the photoluminescence (PL) quantum yields (QYs) of the QDs. The PL QY of ZnSe-core QDs synthesized under the optimum conditions reached 60%. Furthermore, the PL QY further increased to higher than 90% when a ZnS shell was applied to prepare ZnSe/ZnS-core/shell QDs.

  11. Optimization of Microwave-Assisted Extraction of Curcumin From Curcuma longa L. (Turmeric) and Evaluation of Antioxidant Activity in Multi-Test Systems

    OpenAIRE

    Mustafa Bener; Mustafa Özyürek; Kubilay Güçlü; Reşat Apak

    2016-01-01

    Turmeric ( Curcuma longa L.) is a medicinal plant, and its biological activities mainly arise from the main constituent, known as diferuloylmethane or curcumin. In the present paper, microwave-assisted extraction (MAE) was investigated for the recovery of curcumin from turmeric in comparison to conventional heat-assisted extraction (CHAE) technique. Various experimental conditions, such as solvent concentration (0-100%, v/v), MAE temperature (30-130 oC) and MAE time (0-20 min) were investigat...

  12. One-step microwave-assisted synthesis of water-dispersible Fe3O4 magnetic nanoclusters for hyperthermia applications

    Science.gov (United States)

    Sathya, Ayyappan; Kalyani, S.; Ranoo, Surojit; Philip, John

    2017-10-01

    To realize magnetic hyperthermia as an alternate stand-alone therapeutic procedure for cancer treatment, magnetic nanoparticles with optimal performance, within the biologically safe limits, are to be produced using simple, reproducible and scalable techniques. Herein, we present a simple, one-step approach for synthesis of water-dispersible magnetic nanoclusters (MNCs) of superparamagnetic iron oxide by reducing of Fe2(SO4)3 in sodium acetate (alkali), poly ethylene glycol (capping ligand), and ethylene glycol (solvent and reductant) in a microwave reactor. The average size and saturation magnetization of the MNC's are tuned from 27 to 52 nm and 32 to 58 emu/g by increasing the reaction time from 10 to 600 s. Transmission electron microscopy images reveal that each MNC composed of large number of primary Fe3O4 nanoparticles. The synthesised MNCs show excellent colloidal stability in aqueous phase due to the adsorbed PEG layer. The highest SAR value of 215 ± 10 W/gFe observed in 52 nm size MNC at a frequency of 126 kHz and field of 63 kA/m suggest the potential use of these MNC in hyperthermia applications. This study further opens up the possibilities to develop metal ion-doped MNCs with tunable sizes suitable for various biomedical applications using microwave assisted synthesis.

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

    Science.gov (United States)

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

    2017-02-01

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

  14. Production of Bio-Ethanol by Integrating Microwave-Assisted Dilute Sulfuric Acid Pretreated Sugarcane Bagasse Slurry with Molasses.

    Science.gov (United States)

    Yu, Na; Tan, Li; Sun, Zhao-Yong; Tang, Yue-Qin; Kida, Kenji

    2017-11-04

    Sugarcane bagasse (SCB) and molasses, known as carbohydrate-rich biomass derived from sugar production, can serve as feedstock for bio-ethanol production. To establish a simple process, the production of bio-ethanol through integration of whole pretreated slurry (WPS) of SCB with molasses was investigated. The results showed that microwave-assisted dilute sulfuric acid pretreatment reduced the formation of toxic compounds compared to a pretreatment process involving "conventional heating". Pretreatment at 180 o C with 10% w v -1 solid loading and 0.5% w v -1 H 2 SO 4 was sufficient to achieve efficient enzymatic saccharification of WPS. By conducting separate hydrolysis and fermentation (SHF), an ethanol yield of 90.12% was obtained from the mixture of WPS and molasses, but the ethanol concentration of 33.48 g L -1 was relatively low. By adopting fed-batch SHF, the ethanol concentration reached 41.49 g L -1 . Assuming that the molasses were converted to ethanol at an efficiency of 87.21% (i.e., ethanol was obtained from fermentation of molasses alone), the ethanol yield from WPS when a mixture of WPS and molasses was fermented was 78.30%, which was higher than that of enzymatic saccharification of WPS (73.53%). These findings suggest that the production of bio-ethanol via integration of WPS with molasses is a superior method. Graphical Abstract ᅟ.

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

    Science.gov (United States)

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

    2017-06-24

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

  16. Facile and rapid one-pot microwave-assisted synthesis of Pd-Ni magnetic nanoalloys confined in mesoporous carbons

    Energy Technology Data Exchange (ETDEWEB)

    Martínez de Yuso, Alicia; Le Meins, Jean-Marc [Université de Strasbourg, Université de Haute-Alsace, Institut de Science des Matériaux de Mulhouse, CNRS UMR (France); Oumellal, Yassine; Paul-Boncour, Valérie; Zlotea, Claudia [Institut de Chimie et des Matériaux Paris Est, UMR 7182, CNRS-UPEC (France); Matei Ghimbeu, Camelia, E-mail: camelia.ghimbeu@uha.fr [Université de Strasbourg, Université de Haute-Alsace, Institut de Science des Matériaux de Mulhouse, CNRS UMR (France)

    2016-12-15

    An easy and rapid one-pot microwave-assisted soft-template synthesis method for the preparation of Pd-Ni nanoalloys confined in mesoporous carbon is reported. This approach allows the formation of mesoporous carbon and the growth of the particles at the same time, under short microwave irradiation (4 h) compared to the several days spent for the classical approach. In addition, the synthesis steps are diminished and no thermopolymerization step or reduction treatment being required. The influence of the Pd-Ni composition on the particle size and on the carbon characteristics was investigated. Pd-Ni solid solutions in the whole composition range could be obtained, and the metallic composition proved to have an important effect on the nanoparticle size but low influence on carbon textural properties. Small and uniformly distributed nanoparticles were confined in mesoporous carbon with uniform pore size distribution, and dependence between the nanoparticle size and the nanoalloy composition was observed, i.e., increase of the particle size with increasing the Ni content (from 5 to 14 nm). The magnetic properties of the materials showed a strong nanoparticle size and/or composition effect. The blocking temperature of Pd-Ni nanoalloys increases with the increase of Ni amount and therefore of particle size. The magnetization values are smaller than the bulk counterpart particularly for the Ni-rich compositions due to the formed graphitic shells surrounding the particles inducing a dead magnetic layer.

  17. Investigation of CdO nanostructures synthesized by microwave assisted irradiation technique for NO{sub 2} gas detection

    Energy Technology Data Exchange (ETDEWEB)

    Rajesh, N. [Department of Physics, KSR College of Engineering, Tiruchengode, Tamil Nadu 637215 (India); Kannan, J.C. [Department of Physics, KSR Institute for Engineering and Technology, Tiruchengode, Tamil Nadu 637215 (India); Leonardi, S.G.; Neri, G. [Department of Electronic Engineering, Chemistry and Industrial Engineering, University of Messina, Messina 98166 (Italy); Krishnakumar, T., E-mail: tkrishnakumar_nano@yahoo.co.in [Department of Physics, Tagore Institute of Engineering and Technology, Attur, Salem, Tamil Nadu 636112 (India)

    2014-09-01

    Cadmium oxide nanostructures were prepared with simple and cost-effective chemical route assisted by microwave irradiation. The synthesized samples were characterized by X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Selected Area Electron Diffraction (SAED), Energy Dispersive X-ray (EDX) analysis and Fourier Transform Infrared spectroscopy (FT-IR) techniques. Highly crystalline CdO nanostructures with different morphology (spherical and rod-like) have been obtained by the microwave-assisted procedure adopted without any post-synthesis annealing treatment. Furthermore, the formation of these CdO nanostructures can be easily addressed within short times (5–15 min) by a fine tuning of the microwave irradiation. The CdO nanostructures have been investigated as sensing layer in resistive sensors and tested for NO{sub 2} sensing at mild temperature. The sensors have shown high response to NO{sub 2} down to 0.5 ppm at low operating temperature of 100 °C and high selectivity against CO.

  18. Protective Effects Induced by Microwave-Assisted Aqueous Harpagophytum Extract on Rat Cortex Synaptosomes Challenged with Amyloid β-Peptide.

    Science.gov (United States)

    Ferrante, Claudio; Recinella, Lucia; Locatelli, Marcello; Guglielmi, Paolo; Secci, Daniela; Leporini, Lidia; Chiavaroli, Annalisa; Leone, Sheila; Martinotti, Sara; Brunetti, Luigi; Vacca, Michele; Menghini, Luigi; Orlando, Giustino

    2017-08-01

    Harpagophytum procumbens is a plant species that displays anti-inflammatory properties in multiple tissues. The iridoid glycosides arpagoside, harpagide, and procumbide appear to be the most therapeutically important constituents. In addition, harpagoside treatment exerted neuroprotective effects both in vitro and in vivo. Considering these findings, the aim of the present work is to explore the possible protective role of the previously described microwave-assisted aqueous extract of H. procumbens on rat hypothalamic (Hypo-E22) cells, and in rat cortex challenged with amyloid β-peptide (1-40). In this context, we assayed the protective effects induced by H. procumbens by measuring the levels of malondialdehyde, 3-hydroxykynurenine (3-HK), brain-derived neurotrophic factor, and tumor necrosis factor-α, 3-HK. Finally, we evaluated the effects of H. procumbens treatment on cortex levels of dopamine, norepinephrine, and serotonin. H. procumbens extract was well tolerated by Hypo-E22 cells and upregulated brain-derived neurotrophic factor gene expression but down-regulated tumor necrosis factor-α gene expression. In addition, the extract reduced amyloid β-peptide stimulation of malondialdehyde and 3-HK and blunted the decrease of dopamine, norepinephrine, and serotonin, in the cortex. In this context, our work supports further studies for the evaluation and confirmation of Harpagophytum in the management of the clinical symptoms related to Alzheimer's disease. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  19. Microwave-Assisted Synthesis of SiC Nanoparticles for the Efficient Adsorptive Removal of Nitroimidazole Antibiotics from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Ali Fakhri

    2017-02-01

    Full Text Available Environmental pollution caused by the improper disposal of pharmaceuticals is a matter of global concern, and warrants immediate attention. Of particular concern is the aquatic contamination caused by the increasing use of antibiotics, which could give rise to superbugs. While researchers have mainly focused on improving the adsorption capacity of mostly activated carbon-based adsorbents, we have developed a non-conventional adsorbent (SiC nanoparticles in the present work for the adsorptive removal of four different nitroimidazole antibiotics, namely metronidazole (MNZ, dimetridazole (DMZ, ronidazole (RNZ, and tinidazole (TNZ. In addition to the unique properties which are inherent to SiC, the present adsorbent not only possesses a high adsorption capacity, but also shows one of the highest adsorption rates; both of which are prerequisites for an efficient and cost-effective adsorption-based separation technology. Silicon carbide (SiC nanoparticles, synthesized by a microwave-assisted method, were thoroughly characterized using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and the Brunauer–Emmett–Teller method. The adsorption isotherm data were accurately described by the Langmuir isotherm model. On the other hand, the adsorption kinetics, closely represented by the pseudo-second order kinetic model, were faster than most previously reported adsorbents. The reaction rate constants were 0.0089, 0.0079, 0.0072, and 0.0055 g/(mg min, for MNZ, DMZ, RNZ, and TNZ, respectively.

  20. Microwave-Assisted Synthesis of Co3(PO42 Nanospheres for Electrocatalytic Oxidation of Methanol in Alkaline Media

    Directory of Open Access Journals (Sweden)

    Prabhakarn Arunachalam

    2017-04-01

    Full Text Available Low-cost and high-performance advanced electrocatalysts for direct methanol fuel cells are of key significance for the improvement of environmentally-pleasant energy technologies. Herein, we report the facile synthesis of cobalt phosphate (Co3(PO42 nanospheres by a microwave-assisted process and utilized as an electrocatalyst for methanol oxidation. The phase formation, morphological surface structure, elemental composition, and textural properties of the synthesized (Co3(PO42 nanospheres have been examined by powder X-ray diffraction (XRD, Fourier transform-infrared spectroscopy (FT-IR, field emission-scanning electron microscopy (FE-SEM, high-resolution transmission electron microscopy (HRTEM, X-ray photoelectron spectroscopy (XPS, and nitrogen adsorption-desorption isotherm investigations. The performance of an electrocatalytic oxidation of methanol over a Co3(PO42 nanosphere-modified electrode was evaluated in an alkaline solution using cyclic voltammetry (CV and chronopotentiometry (CP techniques. Detailed studies were made for the methanol oxidation by varying the experimental parameters, such as catalyst loading, methanol concentration, and long-term stability for the electro-oxidation of methanol. The good electrocatalytic performances of Co3(PO42 should be related to its good surface morphological structure and high number of active surface sites. The present investigation illustrates the promising application of Co3(PO42 nanospheres as a low-cost and more abundant electrocatalyst for direct methanol fuel cells.

  1. Hollow fiber-stir bar sorptive extraction and microwave assisted derivatization of amino acids in biological matrices.

    Science.gov (United States)

    Li, Jia; Qi, Huan-Yang; Wang, Yan-Bin; Su, Qiong; Wu, Shang; Wu, Lan

    2016-11-25

    A kind of solid phase microextraction configuration combining the principles of hollow fiber solid phase microextraction (HF-SPME) and stir bar sorptive extraction (SBSE) is presented. The main feature of HF-SBSE is the use of microporous hollow fiber acting as the carrier and filter, while a thin stainless steel wire and silica microspheres in the lumen of hollow fiber respectively acting as the magnetic stirrer and the dispersed sorbents for the collection and extraction of the target analytes, thus affording extraction process like SBSE. Moreover, the prepared hollow fiber stir bar was applied to direct microextraction and microwave assisted derivatization with N,O-Bis(trimethylsilyl)trifluroacetamide (BSTFA) of four amino acids in rats' urine and cerebrospinal fluid followed by gas chromatography mass spectrometric analysis. The limits of detection for four amino acids were found to be in the range of 0.0003-0.017μgmL -1 , and all the analytes did not exhibit any lack of fit. The extraction recoveries using HF-SBSE techniques ranged from 71.8% to 102.3%. The results indicated that hollow fiber stir bar sorptive extraction was a promising technique for the enrichment and direct derivatization of analytes extracted from biological matrices without sample clean-up. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Open focused microwave-assisted sample preparation for rapid total and mercury species determination in environmental solid samples.

    Science.gov (United States)

    Tseng, C M; Garraud, H; Amouroux, D; Donard, O F; de Diego, A

    1998-01-01

    This paper describes rapid, simple microwave-assisted leaching/ digestion procedures for total and mercury species determination in sediment samples and biomaterials. An open focused microwave system allowed the sample preparation time to be dramatically reduced to only 24 min when a power of 40-80 W was applied. Quantitative leaching of methylmercury from sediments by HNO(3) solution and complete dissolution of biomaterials by an alkaline solution, such as 25% TMAH solution, were obtained. Methylmercury compounds were kept intact without decomposition or losses by evaporation. Quantitative recoveries of total mercury were achieved with a two-step microwave attack using a combination of HNO(3) and H(2)0(2) solutions as extractant. The whole pretreatment procedure only takes 15 min, which can be further shortened by an automated robust operation with an open focused system. These analytical procedures were validated by the analysis of environmental certified reference materials. The results confirm that the open focused microwave technique is a promising tool for solid sample preparation in analytical and environmental chemistry.

  3. Microwave-assisted ionothermal synthesis of nanostructured anatase titanium dioxide/activated carbon composite as electrode material for capacitive deionization

    International Nuclear Information System (INIS)

    Liu, Po-I; Chung, Li-Ching; Shao, Hsin; Liang, Teh-Ming; Horng, Ren-Yang; Ma, Chen-Chi M.; Chang, Min-Chao

    2013-01-01

    The nanostructured anatase titanium dioxide/activated carbon composite material for capacitive deionization electrode was prepared in a short time by a lower temperature two-step microwave-assisted ionothermal (sol–gel method in the presence of ionic liquid) synthesis method. This method includes a reaction and a crystallization step. In the crystallization step, the ionic liquid plays a hydrothermal analogy role in driving the surface anatase crystallization of amorphous titanium dioxide nanoparticles formed in the reaction step. The energy dispersive spectroscopic study of the composite indicates that the anatase titanium dioxide nanoparticles are evenly deposited in the matrix of activated carbon. The electrochemical property of the composite electrode was investigated. In comparison to the pristine activated carbon electrode, higher specific capacitance was observed for the nanostructured anatase titanium dioxide/activated carbon composite electrode, especially when the composite was prepared with a molar ratio of titanium tetraisopropoxide/H 2 O equal to 1:15. Its X-ray photoelectron spectroscopic result indicates that it has the highest amount of Ti-OH. The Ti-OH group can enhance the wetting ability and the specific capacitance of the composite electrode. The accompanying capacitive deionization result indicates that the decay of electrosorption capacity of this composite electrode is insignificant after five cycle tests. It means that the ion electrosorption–desorption becomes a reversible process

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

    Science.gov (United States)

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

    2014-01-01

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

  5. N-Substituted 5-Amino-6-methylpyrazine-2,3-dicarbonitriles: Microwave-Assisted Synthesis and Biological Properties

    Directory of Open Access Journals (Sweden)

    Ondrej Jandourek

    2014-01-01

    Full Text Available In this work a series of 15 N-benzylamine substituted 5-amino-6-methyl-pyrazine-2,3-dicarbonitriles was prepared by the aminodehalogenation reactions using microwave assisted synthesis with experimentally set and proven conditions. This approach for the aminodehalogenation reaction was chosen due to its higher yields and shorter reaction times. The products of this reaction were characterized by IR, NMR and other analytical data. The compounds were evaluated for their antibacterial, antifungal and herbicidal activity. Compounds 3 (R = 3,4-Cl, 9 (R = 2-Cl and 11 (R = 4-CF3 showed good antimycobacterial activity against Mycobacterium tuberculosis (MIC = 6.25 µg/mL. It was found that the lipophilicity is important for antimycobacterial activity and the best substitution on the benzyl moiety of the compounds is a halogen or trifluoromethyl group according to Craig’s plot. The activities against bacteria or fungi were insignificant. The presented compounds also inhibited photosynthetic electron transport in spinach chloroplasts and the IC50 values of the active compounds varied in the range from 16.4 to 487.0 µmol/L. The most active substances were 2 (R = 3-CF3, 3 (R = 3,4-Cl and 11 (R = 4-CF3. A linear dependence between lipophilicity and herbicidal activity was observed.

  6. A simple fast microwave-assisted synthesis of thermoelectric bismuth telluride nanoparticles from homogeneous reaction-mixture

    Energy Technology Data Exchange (ETDEWEB)

    Pradhan, Susmita [Jadavpur University, Department of Instrumentation Science (India); Das, Rashmita [Jadavpur University, Department of Instrumentation and Electronics Engineering (India); Bhar, Radhaballabh [Jadavpur University, Department of Instrumentation Science (India); Bandyopadhyay, Rajib [Jadavpur University, Department of Instrumentation and Electronics Engineering (India); Pramanik, Panchanan, E-mail: pramanik1946@gmail.com [GLA University, Department of Chemistry and Nanoscience (India)

    2017-02-15

    A new simple chemical method for synthesis of nanocrystalline bismuth telluride (Bi{sub 2}Te{sub 3}) has been developed by microwave assisted reduction of homogeneous tartrate complexes of bismuth and tellurium metal ions with hydrazine. The reaction is performed at pH 10. The nano-crystallites have rhombohedral phase identified by XRD. The size distribution of nanoparticle is narrow and it ranges between 50 to 70 nm. FESEM shows that the fine powders are composed of small crystallites. The TEM micrographs show mostly deformed spherical particles and the lattice fringes are found to be 0.137 nm. Energy dispersive X-ray spectroscopy (EDX) analysis shows the atomic composition ratio between bismuth and tellurium is 2:3. Thermoelectric properties of the materials are studied after sintering by spark plasma sintering method (SPS). The grain size of the material after sintering is in the nanometer range. The material shows enhanced Seebeck coefficient and electrical conductivity value at 300 K. The figure of merit is found to be 1.18 at 300 K.

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

    Science.gov (United States)

    Moodley, Preshanthan; Kana, E B Gueguim

    2017-07-01

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

  8. Microwave-Assisted Extraction and Purification of Arctiin and Arctigenin from Fructus Arctii by High-Speed Countercurrent Chromatography.

    Science.gov (United States)

    Lü, Haitao; Sun, Zhaoyun; Shan, Hu; Song, Jiying

    2016-03-01

    An efficient method for the rapid extraction, separation and purification of bioactive lignans, arctiin and arctigenin, from Fructus arctii by microwave-assisted extraction coupled with high-speed countercurrent chromatography was developed. The optimal extraction conditions of arctiin and arctigenin were evaluated by orthogonal array. Arctigenin could be converted from arctiin by hydrochloric acid hydrolysis. The separations were performed at a preparative scale with two-phase solvents composed of ethyl acetate-ethanol-water (5 : 1 : 5, v/v/v) for arctiin, and n-hexane-ethyl acetate-ethanol-water (4 : 4 : 3 : 4, v/v/v/v) for arctigenin. From 500 mg of crude extract sample, 122.3 mg of arctiin and 45.7 mg of arctigenin were obtained with the purity of 98.46 and 96.57%, and the recovery of 94.3 and 81.6%, respectively. Their structures were determined by comparison with the high-performance liquid chromatography retention time of standard substance as well as UV, FT-IR, electrospray ion source (ESI)-MS, (1)H-NMR and (13)C-NMR spectrum. According to the antioxidant activity assay, arctigenin had stronger 1,1-diphenyl-2-picrylhydrazyl free radicals scavenging activity. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Microwave-assisted headspace solid-phase microextraction for the analysis of bioemissions from Eucalyptus citriodora leaves.

    Science.gov (United States)

    Xiong, Guohua; Goodridge, Carolyn; Wang, Limei; Chen, Yong; Pawliszyn, Janusz

    2003-12-31

    Microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) was developed as a simple and effective method for fast sampling of volatile organic compounds (VOCs) from Eucalyptus citriodora Hook (E. citriodora) leaves. During microwave heating, a simple shielding device made of aluminum foil was used to protect the SPME fiber from microwave irradiation while allowing the sample to be heated. A room temperature water bath was also used to allow microwave heating to be conducted in a more controlled manner. The inner heating caused by microwave irradiation dramatically accelerated the emission of VOCs from the sample, but no marked change in headspace temperature in the sample vial was found. Under optimum conditions, the extraction efficiencies obtained with microwave heating were much higher than those obtained without microwave heating for all fibers used, namely, 7-microm polydimethylsiloxane (PDMS), 100-microm polydimethylsiloxane (PDMS), 65-microm polydimethylsiloxane/divinylbenzene (PDMS/DVB), and 75-microm carboxen/polydimethylsiloxane (CAR/PDMS). The improvement of extraction efficiency using MA-HS-SPME allowed more VOC events to be detected, with more balanced extraction of VOCs of lower and higher molecular masses. Moreover, a good linear relationship was found between sample size and GC-FID response (total peak area of VOCs), indicating the usefulness of MA-HS-SPME for quantitative analysis of individual volatile compounds in E. citriodora leaves.

  10. SnO2 nanocrystals synthesized by microwave-assisted hydrothermal method: towards a relationship between structural and optical properties

    International Nuclear Information System (INIS)

    Mendes, Paulo G.; Moreira, Mario L.; Tebcherani, Sergio M.; Orlandi, Marcelo O.; Andrés, J.; Li, Maximu S.; Diaz-Mora, Nora; Varela, José A.; Longo, Elson

    2012-01-01

    The exploration of novel synthetic methodologies that control both size and shape of functional nanostructure opens new avenues for the functional application of nanomaterials. Here, we report a new and versatile approach to synthesize SnO 2 nanocrystals (rutile-type structure) using microwave-assisted hydrothermal method. Broad peaks in the X-ray diffraction spectra indicate the nanosized nature of the samples which were indexed as a pure cassiterite tetragonal phase. Chemically and physically adsorbed water was estimated by TGA data and FT-Raman spectra to account for a new broad peak around 560 cm −1 which is related to defective surface modes. In addition, the spherical-like morphology and low dispersed distribution size around 3–5 nm were investigated by HR-TEM and FE-SEM microscopies. Room temperature PL emission presents two broad bands at 438 and 764 nm, indicating the existence of different recombination centers. When the size of the nanospheres decreases, the relative intensity of 513 nm emission increases and the 393 nm one decreases. UV–Visible spectra show substantial changes in the optical absorbance of crystalline SnO 2 nanoparticles while the existence of a small tail points out the presence of localized levels inside the forbidden band gap and supplies the necessary condition for the PL emission.

  11. The influence of microwave-assisted drying techniques on the rehydration behavior of blueberries (Vaccinium corymbosum L.).

    Science.gov (United States)

    Zielinska, Magdalena; Markowski, Marek

    2016-04-01

    The aim of this study was to determine the effect of: (a) different drying methods, (b) hot air temperature in a convection oven, and (c) the moisture content of fruits dehydrated by multi-stage drying which involves a transition between different stages of drying, on the rehydration kinetics of dry blueberries. Models describing rehydration kinetics were also studied. Blueberries dehydrated by multi-stage microwave-assisted drying, which involved a hot air pre-drying step at 80 °C until the achievement of a moisture content of 1.95 kg H2O kg(-1)DM, were characterized by significantly higher rates of initial and successive rehydration as well as smaller initial loss of soluble solids in comparison with the samples dried by other methods. The highest initial rehydration rate and the smallest loss of soluble solids after 30 min of soaking were determined at 0.46 min(-1) and 0.29 kg DM kg(-1)DM, respectively. The Peleg model and the first-order-kinetic model fit the experimental data well. Copyright © 2015 Elsevier Ltd. All rights reserved.

  12. Optimization of microwave-assisted extraction of carbohydrates from industrial waste of corn starch production using response surface methodology.

    Science.gov (United States)

    Yoshida, Tomoki; Tsubaki, Shuntaro; Teramoto, Yoshikuni; Azuma, Jun-ichi

    2010-10-01

    Microwave-assisted extraction (MAE) was applied for production of carbohydrates mainly consisting of arabinoxylan from corn pericarp which is an industrial waste of corn starch production by using hot compressed water as a solvent. The solubilization rate increased with increase in heating temperature and reached 75.2% at 220 °C. The main extracted materials were carbohydrates consist of glucose, xylose and arabinose indicating solubilization of starch and hemicellulose, while residues were composed of cellulose. Four independent variables (heating temperature, come-up time, heating time and solid to liquid ratio) were optimized for maximizing the carbohydrates yield using the response surface methodology including fractional factorial design, the path of steepest ascent and central composite design. The optimized condition was as follows; heating temperature 176.5 °C, come-up time 2 min, heating time 16 min and solid to liquid ratio 1/20 (g/mL), respectively. The maximal yield attained 70.8% of carbohydrates with predominant production of xylo-oligosaccharides. Copyright © 2010 Elsevier Ltd. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Linganiso, Ella Cebisa [DST/CSIR Nanotech Innovation Centre, National Centre for Nano-structured Materials, Council for Scientific and Industrial Research, PO Box 395, Pretoria 0001 (South Africa); Molecular Sciences Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits, 2050 Johannesburg (South Africa); Mwakikunga, Bonex Wakufwa, E-mail: bmwakikunga@csir.co.za [DST/CSIR Nanotech Innovation Centre, National Centre for Nano-structured Materials, Council for Scientific and Industrial Research, PO Box 395, Pretoria 0001 (South Africa); Department of Physics and Biochemical Sciences, The Polytechnic of the University of Malawi, Private Bag 303, Chichiri, Blantyre 0003 (Malawi); Mhlanga, Sabelo Dalton [Department of Applied Chemistry, University of Johannesburg, PO Box 17011, Doornfontein, 2028 Johannesburg (South Africa); Coville, Neil John [Molecular Sciences Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits, 2050 Johannesburg (South Africa); DST/NRF Centre of Excellence in Strong Materials, University of the Witwatersrand, Private Bag 3, Wits, 2050 Johannesburg (South Africa)

    2014-11-15

    Nickel sulphide (NiS) nanostructures decorated with gold (Au) nanoparticles (NPs) were synthesized via a microwave-assisted hydrothermal technique. Binary phase NiS (α and β) crystalline nanostructures, bare, and decorated with Au NPs were obtained and confirmed by X-ray diffraction (XRD) studies. TEM analysis revealed that the NiS nanostructures were of various shapes. A quantum confinement effect was confirmed by the blue shift PL emissions and high optical energy band gap observed for the as-synthesized sample. A threefold light emission enhancement due to Au NP coatings was obtained when Au metal NP decoration concentrations was varied from 1% to 10%. These enhancements were attributed to the surface plasmon resonance (SPR) excitation of the surface decorated metal NPs which results in an increased rate of spontaneous emission. The PL enhancement factor was observed to vary at different NiS emissions as well as with the size of the Au NPs. The effect of metal NP decoration on the PL emission of NiS is to the best of our knowledge, presented for the first time. - Highlights: • Binary phase NiS decorated with gold nanoparticles. • Quantum confinement effect confirmed by PL analysis. • PL enhancement depending more on particle size distribution. • Effect of gold on NiS PL is to the best of our knowledge reported for the first time.

  14. Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

    Science.gov (United States)

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

    2015-09-01

    Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Microwave assisted hydrothermal synthesis of Ag/AgCl/WO3 photocatalyst and its photocatalytic activity under simulated solar light

    International Nuclear Information System (INIS)

    Adhikari, Rajesh; Gyawali, Gobinda; Sekino, Tohru; Wohn Lee, Soo

    2013-01-01

    Simulated solar light responsive Ag/AgCl/WO 3 composite photocatalyst was synthesized by microwave assisted hydrothermal process. The synthesized powders were characterized by X-Ray Diffraction (XRD) spectroscopy, X-Ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Diffuse Reflectance Spectroscopy (UV–Vis DRS), and BET surface area analyzer to investigate the crystal structure, morphology, chemical composition, optical properties and surface area of the composite photocatalyst. This photocatalyst exhibited higher photocatalytic activity for the degradation of rhodamine B under simulated solar light irradiation. Dye degradation efficiency of composite photocatalyst was found to be increased significantly as compared to that of the commercial WO 3 nanopowder. Increase in photocatalytic activity of the photocatalyst was explained on the basis of surface plasmon resonance (SPR) effect caused by the silver nanoparticles present in the composite photocatalyst. Highlights: ► Successful synthesis of Ag/AgCl/WO 3 nanocomposite. ► Photocatalytic experiment was performed under simulated solar light. ► Nanocomposite photocatalyst was very active as compared to WO 3 commercial powder. ► SPR effect due to Ag nanoparticles enhanced the photocatalytic activity.

  16. Microwave-assisted extraction versus Soxhlet extraction for the analysis of short-chain chlorinated alkanes in sediments.

    Science.gov (United States)

    Parera, J; Santos, F J; Galceran, M T

    2004-08-13

    Microwave-assisted extraction (MAE) was evaluated as a possible alternative to Soxhlet extraction for analysing short-chain chlorinated alkanes (commonly called short-chain chlorinated paraffins, SCCPs) in river sediment samples, using gas chromatography coupled to negative chemical ionisation mass spectrometry. For MAE optimisation, several extraction parameters such as solvent extraction mixture, extraction time and extraction temperature were studied. Maximum extraction efficiencies for SCCPs (90%) and for 12 polychlorinated biphenyl (PCB) congeners (91-95%) were achieved using 5 g of sediment sample, 30 ml of n-hexane-acetone (1:1, v/v) as solvent extraction, and 15 min and 115 degrees C of extraction time and temperature, respectively. Activated Florisil was used to clean-up the extracts, allowing highly selective separation of SCCPs from other organic contaminants such as PCBs. MAE was compared with a conventional extraction technique such as Soxhlet and good agreement in the results was obtained. Quality parameters of the optimised MAE method such as run-to-run (R.S.D. 7%) and day-to-day precision (R.S.D. 9%) were determined using spiked river sediment samples, with LODs of 1.5 ng g(-1). This method was successfully applied to the analysis of SCCPs in river sediment samples at concentrations below the ng g(-1) level. O 2004 Elsevier B.V. All rights reserved.

  17. Optimization of microwave-assisted extraction of hydrocarbons in marine sediments: comparison with the Soxhlet extraction method.

    Science.gov (United States)

    Vázquez Blanco, E; López Mahía, P; Muniategui Lorenzo, S; Prada Rodríguez, D; Fernández Fernández, E

    2000-02-01

    Microwave energy was applied to extract polycyclic aromatic hydrocarbons (PAHs) and linear aliphatic hydrocarbons (LAHs) from marine sediments. The influence of experimental conditions, such as different extracting solvents and mixtures, microwave power, irradiation time and number of samples extracted per run has been tested using real marine sediment samples; volume of the solvent, sample quantity and matrix effects were also evaluated. The yield of extracted compounds obtained by microwave irradiation was compared with that obtained using the traditional Soxhlet extraction. The best results were achieved with a mixture of acetone and hexane (1:1), and recoveries ranged from 92 to 106%. The extraction time is dependent on the irradiation power and the number of samples extracted per run, so when the irradiation power was set to 500 W, the extraction times varied from 6 min for 1 sample to 18 min for 8 samples. Analytical determinations were carried out by high-performance liquid chromatography (HPLC) with an ultraviolet-visible photodiode-array detector for PAHs and gas chromatography (GC) using a FID detector for LAHs. To test the accuracy of the microwave-assisted extraction (MAE) technique, optimized methodology was applied to the analysis of standard reference material (SRM 1941), obtaining acceptable results.

  18. Low temperature microwave-assisted pyrolysis of wood sawdust for phenolic rich compounds: Kinetics and dielectric properties analysis.

    Science.gov (United States)

    Luo, Hu; Bao, Liwei; Kong, Lingzhao; Sun, Yuhan

    2017-08-01

    Microwave-assisted pyrolysis of wood sawdust for phenolic rich compounds was carried out between 400 and 550°C in a batch reactor. An efficient preparation of liquid products was observed at 500°C with a yield of 58.50%, which was similar to conventional fast pyrolysis. The highest concentration of phenolic compounds in liquid product reached up to 78.7% (area) in which the alkoxy phenols contributed 81.8% at 500°C. Microwave thermogravimetric analysis using KAS method was used firstly to investigate the low-temperature pyrolytic behaviors and activation energy. The results indicated that effective pyrolytic range was 250-400°C and average activation energy was 42.78kJ/mol, which were 50-100°C and 50-100kJ/mol lower than conventional pyrolysis, respectively. Analysis on dielectric properties of pyrolytic products confirmed that accelerated pyrolysis and low temperature were attributed to the formation of instantaneous "hot spots". Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. CO and C3H8 Sensitivity Behavior of Zinc Antimonate Prepared by a Microwave-Assisted Solution Method

    International Nuclear Information System (INIS)

    Guillen-Bonilla, H.; Rodiguez Betancourtt, V. M.; Flores-Martinez, M.; Guillen-Bonilla, J. T.; Reyes-Gomez, J.; Gildo-Ortiz, L.; Olvera-Amador, M. L.; Santoyo-Salazar, J.

    2015-01-01

    ZnSb 2 O 6 has been synthesized by a microwave-assisted solution method in order to test its possible application as a gas sensor. Zinc nitrate, antimony trichloride, and ethylenediamine were used as precursors and deionized water as solvent. Microwave radiation, with a power of a pprox 3 50 W, was applied for solvent evaporation. The thermal decomposition of the precursors leads to the formation of ZnSb 2 O 6 at 600 degree. This oxide crystallized in a tetragonal structure with cell parameters a=4.66 angstrom sign, c=9.26 angstrom sign and space group P4 2 / mnm. Micro wires and micro rods formed by nano crystals were observed by means of scanning and transmission electron micros copies (SEM and TEM, resp.). Pellets of the oxide were tested as gas sensors in flowing atmospheres of carbon monoxide (CO) and propane (C 3 H 8 ). Sensitivity increased with the gas concentration (0-300 ppm) and working temperatures (ambient, 150 and 250 degree) increase. The results indicate high sensitivity of ZnSb 2 O 6 in both gases at different concentrations and operating temperatures.

  20. Rapid microwave-assisted synthesis of highly luminescent nitrogen-doped carbon dots for white light-emitting diodes

    Science.gov (United States)

    Wang, Yaling; Zheng, Jingxia; Wang, Junli; Yang, Yongzhen; Liu, Xuguang

    2017-11-01

    Highly luminescent nitrogen-doped carbon dots (N-CDs) were synthesized rapidly by one-step microwave-assisted hydrothermal method using citric acid as carbon source and ethylenediamine as dopant. The influences of reaction temperature, reaction time and raw material ratio on the fluorescence performance of N-CDs were investigated. Then N-CDs with the highest quantum yield were selected as fluorescent materials for fabricating white light-emitting diodes (LEDs). Highly luminescent N-CDs with the quantum yield of 75.96% and blue-to-red spectral composition of 51.48% were obtained at the conditions of 180 °C, 8 min and the molar ratio of citric acid to ethylenediamine 2:1. As-prepared highly luminescent N-CDs have an average size of 6.06 nm, possess extensive oxygen- and nitrogen-containing functional groups on their surface, and exhibit strong absorption in ultraviolet region. White LEDs based on the highly luminescent N-CDs emit warm white light with color coordinates of (0.42, 0.40) and correlated color temperature of 3416 K.

  1. Microwave-assisted preparation of nitrogen-doped biochars by ammonium acetate activation for adsorption of acid red 18

    Science.gov (United States)

    Wang, Li; Yan, Wei; He, Chi; Wen, Hang; Cai, Zhang; Wang, Zixuan; Chen, Zhengzheng; Liu, Weifeng

    2018-03-01

    Nitrogen-doped biochars derived from Phragmites australis (PA) were prepared using ammonium chloride (AC) and ammonium acetate (AA) as nitrogen sources by phosphoric acid activation via microwave assisted treatment. Their physicochemical properties, acid red 18 (AR18) adsorption performance and possible mechanisms were systematically evaluated. Nitrogen was successfully doped onto the biochar's surface in the formation of pyrrole-N, pyridine-N and oxidized-N with pyridine-N being the major component (64%). The pHiep and basic foundational groups of the biochars increased consequently however their surface areas slightly decreased. The adsorption kinetic data were best fit to the pseudo-second order model and the equilibrium data were well simulated by Freundlich model for all biochars, indicating the important role of chemical interactions. The maximum AR18 adsorption capacities of PAB-AA and PAB-AC were 1.41 and 1.18 times higher compared with the non N-doped biochar, which were mainly attributed to the π-π EDA interaction between the pyridine-N and AR18 as revealed by the comparison of XPS analyses before and after AR18 adsorption. Meanwhile, other mechanisms such as pore filling effect, Lewis acid-base interaction, electrostatic attraction and hydrogen bonding also existed as demonstrated by BET, XPS and FTIR analyses.

  2. Microwave-Assisted Extraction of Phenolic Compounds from Almond Skin Byproducts (Prunus amygdalus): A Multivariate Analysis Approach.

    Science.gov (United States)

    Valdés, Arantzazu; Vidal, Lorena; Beltrán, Ana; Canals, Antonio; Garrigós, María Carmen

    2015-06-10

    A microwave-assisted extraction (MAE) procedure to isolate phenolic compounds from almond skin byproducts was optimized. A three-level, three-factor Box-Behnken design was used to evaluate the effect of almond skin weight, microwave power, and irradiation time on total phenolic content (TPC) and antioxidant activity (DPPH). Almond skin weight was the most important parameter in the studied responses. The best extraction was achieved using 4 g, 60 s, 100 W, and 60 mL of 70% (v/v) ethanol. TPC, antioxidant activity (DPPH, FRAP), and chemical composition (HPLC-DAD-ESI-MS/MS) were determined by using the optimized method from seven different almond cultivars. Successful discrimination was obtained for all cultivars by using multivariate linear discriminant analysis (LDA), suggesting the influence of cultivar type on polyphenol content and antioxidant activity. The results show the potential of almond skin as a natural source of phenolics and the effectiveness of MAE for the reutilization of these byproducts.

  3. Microwave-assisted nonaqueous sol-gel deposition of different spinel ferrites and barium titanate perovskite thin films.

    Science.gov (United States)

    Kubli, Martin; Luo, Li; Bilecka, Idalia; Niederberger, Markus

    2010-01-01

    Rapid and selective heating of solvents by microwave irradiation coupled to nonaqueous sol-gel chemistry makes it possible to simultaneously synthesize metal oxide nanoparticles within minutes and deposit them on substrates. The simple immersion of substrates, such as glass slides, in the reaction solution results after microwave heating in the deposition of homogeneous porous thin films whose thickness can be adjusted through the precursor concentration. Here we use such a microwave-assisted nonaqueous sol-gel process for the formation of various spinel ferrite MFe2O4 (M = Fe, Co, Mn, Ni) and BaTiO3 nanoparticles and their deposition as thin films. The approach offers high flexibility with respect to controlling the crystal size by adjusting the reaction time and/or temperature. Based on the example of CoFe2O4 nanoparticles, we show how the crystal size can carefully be tuned from 4 to 8 nm, resulting in a continuous change of the magnetic properties.

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

    Directory of Open Access Journals (Sweden)

    Selin Şahin

    2017-06-01

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

  5. Can electromagnetic fields influence the structure and enzymatic digest of proteins? A critical evaluation of microwave-assisted proteomics protocols

    Science.gov (United States)

    Damm, Markus; Nusshold, Christoph; Cantillo, David; Rechberger, Gerald N.; Gruber, Karl; Sattler, Wolfgang; Kappe, C. Oliver

    2012-01-01

    This study reevaluates the putative advantages of microwave-assisted tryptic digests compared to conventionally heated protocols performed at the same temperature. An initial investigation of enzyme stability in a temperature range of 37–80 °C demonstrated that trypsin activity declines sharply at temperatures above 60 °C, regardless if microwave dielectric heating or conventional heating is employed. Tryptic digests of three proteins of different size (bovine serum albumin, cytochrome c and β-casein) were thus performed at 37 °C and 50 °C using both microwave and conventional heating applying accurate internal fiber-optic probe reaction temperature measurements. The impact of the heating method on protein degradation and peptide fragment generation was analyzed by SDS-PAGE and MALDI-TOF-MS. Time-dependent tryptic digestion of the three proteins and subsequent analysis of the corresponding cleavage products by MALDI-TOF provided virtually identical results for both microwave and conventional heating. In addition, the impact of electromagnetic field strength on the tertiary structure of trypsin and BSA was evaluated by molecular mechanics calculations. These simulations revealed that the applied field in a typical laboratory microwave reactor is 3–4 orders of magnitude too low to induce conformational changes in proteins or enzymes. PMID:22889711

  6. 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.

  7. Anti-Inflammatory Activity of Pinus koraiensis Cone Bark Extracts Prepared by Micro-Wave Assisted Extraction

    Science.gov (United States)

    Kang, Sun-Ae; Kim, Dong-Hee; Hong, Shin-Hyub; Park, Hye-Jin; Kim, Na-Hyun; Ahn, Dong-Hyun; An, Bong-Jeun; Kwon, Joong-Ho; Cho, Young-Je

    2016-01-01

    In this study, we compared the anti-inflammatory activity of Pinus koraiensis cone bark extracts prepared by conventional extraction and microwave-assisted extraction (MAE). Water extracts and 50% ethanol extracts prepared using MAE were applied to RAW 264.7 cell at 5, 10, 25, and 50 μg/mL of concentrations, and tested for cytoxicity. The group treated with 50 μg/mL of 50% ethanol extracts showed toxicity. In order to investigate the inhibition of nitric oxide (NO) production in RAW 264.7 cells, extracts of water and ethanol were treated with 5, 10, and 25 μg/mL concentrations. The inhibitory activity of water and 50% ethanol extracts groups were determined as 40% and 60% at 25 μg/mL concentration, respectively. We found concentration dependent decreases on inducible NO synthase. The inhibitory effect against forming inflammatory cytokines, prostaglandin E2, tumor necrosis factor-α, interleukin (IL)-6, and IL-1β, was also superior in the 25 μg/mL treated group than the control group. According to these results, the water extracts and 50% ethanol extracts both inhibited inflammatory mediators by reducing the inflammatory response. Therefore, The MAE extracts of P. koraiensis cone bark can be developed as a functional ingredient with anti-inflammatory activity. PMID:27752500

  8. Microwave-assisted synthesis of L-glutathione capped ZnSe QDs and its interaction with BSA by spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ding, Ling, E-mail: linda0911@163.com [College of Chemical Engineering and Technology, Wuhan University of Science and Technology, Wuhan 430081 (China); College of Resource and Environmental Sciences, Hubei Biomass-Resource Chemistry and Environmental Biotechnology Key Laboratory, Wuhan University, Wuhan 430079 (China); Zhou, Pei-Jiang, E-mail: zhoupj@whu.edu.cn [College of Resource and Environmental Sciences, Hubei Biomass-Resource Chemistry and Environmental Biotechnology Key Laboratory, Wuhan University, Wuhan 430079 (China); Zhan, Hong-Ju [College of Resource and Environmental Sciences, Hubei Biomass-Resource Chemistry and Environmental Biotechnology Key Laboratory, Wuhan University, Wuhan 430079 (China); Jingchu University of Technology, Jingmen 448000 (China); Chen, Chi [College of Resource and Environmental Sciences, Hubei Biomass-Resource Chemistry and Environmental Biotechnology Key Laboratory, Wuhan University, Wuhan 430079 (China); Hu, Wei [Wuhan Humanwell Pharmaceutical Co. Ltd, Wuhan 430064 (China); Zhou, Teng-Fei; Lin, Chao-Wang [College of Resource and Environmental Sciences, Hubei Biomass-Resource Chemistry and Environmental Biotechnology Key Laboratory, Wuhan University, Wuhan 430079 (China)

    2013-10-15

    Stable, water-soluble and biologically compatible ZnSe quantum dots (QDs) with L-glutathione (GSH) as a capping agent were synthesized in aqueous medium by microwave irradiation. The GSH/Zn/Se molar ratios, reaction temperature, time and pH are the crucial factors for properties of QDs. Fluorescence (FL) spectra, absorption spectra, transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) spectra studies showed that the optical properties of QDs were strong, shape of QDs was similar to spherical and the particle size was about 2–3 nm. The 42% quantum yield (QY) of QDs can be achieved without any post-preparative treatment. The interaction of QDs bioconjugated to bovine serum albumin (BSA) was also studied by absorption and FL spectra experiments. With addition of QDs, the FL intensity of BSA was largely quenched, which can be explained by static mechanism. The results suggested the QDs-BSA binding reaction was a static quenching. -- Highlights: • L-glutathione-capped ZnSe quantum dots were synthesized by microwave assisted in aqueous. • The facile synthesis of ZnSe QDs presented is simple and cost-effective. • Findings suggest the QDs possess highly quantum yield and narrow FWHM without any post-treatment. • The interaction mechanism between QDs and BSA is a static quenching.

  9. A novel application of microwave-assisted extraction of polyphenols from brewer's spent grain with HPLC-DAD-MS analysis.

    Science.gov (United States)

    Moreira, Manuela M; Morais, Simone; Barros, Aquiles A; Delerue-Matos, Cristina; Guido, Luís F

    2012-05-01

    This paper reports a novel application of microwave-assisted extraction (MAE) of polyphenols from brewer's spent grains (BSG). A 2(4) orthogonal composite design was used to obtain the optimal conditions of MAE. The influence of the MAE operational parameters (extraction time, temperature, solvent volume and stirring speed) on the extraction yield of ferulic acid was investigated through response surface methodology. The results showed that the optimal conditions were 15 min extraction time, 100 °C extraction temperature, 20 mL of solvent, and maximum stirring speed. Under these conditions, the yield of ferulic acid was 1.31 ± 0.04% (w/w), which was fivefold higher than that obtained with conventional solid-liquid extraction techniques. The developed new extraction method considerably reduces extraction time, energy and solvent consumption, while generating fewer wastes. HPLC-DAD-MS analysis indicated that other hydroxycinnamic acids and several ferulic acid dehydrodimers, as well as one dehydrotrimer were also present, confirming that BSG is a valuable source of antioxidant compounds.

  10. [Determination of Fe, Ti and V in vanadium and titanium magnetite by ICP-OES and microwave-assisted digestion].

    Science.gov (United States)

    Zhu, Xia-ping; Yin, Ji-xian; Chen, Wei-dong; Hu, Zi-Wen; Liang, Qing-xun; Chen, Tie-yao

    2010-08-01

    The method of determination of iron, titanium and vanadium in indissolvable vanadium and titanium magnetite has been established by inductively coupled plasma atomic emission spectroscopy through adding the complexant A and using microwave-assisted digestion. The optimal conditions are confirmed by orthogonal experiment: 0.1 g vanadium and titanium magnetite, 0.04 g complexant A, 12 mL concentrated HC1, 10 min digestion time, and 385 W microwave power. The newly-established method has been applied to digest vanadium and titanium magnetite of Panzhihua Iron and Steel Institute (GBW07226). The iron, titanium and vanadium were detected by ICP-OES, and both comparative error (Er%) and comparative standard deviation (RSD%) met the demand of analytical chemistry, and the complexant A can significantly accelerate the dissolution of vanadium and titanium magnetite through the complexation with the dissolved metal ions, and making the surface of sample and hydrochloric acid medium to update constantly. The determination of the main and trace elements of digestion solution at the same time was achieved by ICP-OES. The method has the advantages of less use of reagents, economy, rapidness, and being friendly to environment, and it meets the requirement for rapid and volume determination. So the method has the value of practical application for the entry-exit inspection and quarantine department of the state and other relevant inspection units.

  11. Microwave assisted synthesis of surfactant stabilized platinum/carbon nanotube electrocatalysts for direct methanol fuel cell applications

    Science.gov (United States)

    Sakthivel, M.; Schlange, A.; Kunz, U.; Turek, T.

    Platinum electrocatalysts deposited on multi-walled carbon nanotubes (CNT) with high loading were prepared using a microwave-assisted polyol reduction method and employed for direct methanol fuel cells (DMFC). A zwitterionic surfactant was used as a stabilizing agent for the formation of Pt nanoparticles. A uniform and narrow size distribution of highly dispersed Pt nanoparticles could be achieved by adjusting the weight ratio of surfactant to Pt precursor allowing for Pt loadings of up to 60 wt%. The heating time and the temperature for the ethylene glycol (EG) oxidation were found to be the key factors for depositing Pt nanoparticles homogeneously on carbon nanotubes. The smallest average particle diameter of 1.8 nm was obtained through microwave heating to 140 °C in 50 s. The structure, amount and morphology of the electrocatalysts were characterized with XRD, TGA, and TEM, respectively. Single cell DMFC measurements were performed in a membrane-electrode assembly (MEA) with 5 cm 2 active area and very low catalyst loading (0.25 mg cm -2 of noble metal on both anode and cathode). The DMFC performance of the surfactant stabilized cathode catalyst obtained by the new method described here revealed that the power density was three times higher than for a commercial catalyst used for comparison and two times higher than for an unstabilized CNT supported catalyst.

  12. Freeze drying reduces the extractability of organochlorine pesticides in fish muscle tissue by microwave-assisted method

    International Nuclear Information System (INIS)

    Zhang, Yanyan; Lin, Nan; Su, Shu; Shen, Guofeng; Chen, Yuanchen; Yang, Chunli; Li, Wei; Shen, Huizhong; Huang, Ye; Chen, Han; Wang, Xilong; Liu, Wenxin; Tao, Shu

    2014-01-01

    Samples of animal origin are usually dried before solvent extraction for analysis of organic contaminants. The freeze drying technique is preferred for hydrophobic organic compounds in practice. In this study, it was shown that the concentration of organochlorine pesticides (OCPs) extracted from fish muscle tissue significantly decreased after the samples were freeze dried. And the reason for this reduced extractability seemed to be the resistance of OCPs associated with freeze-dried muscle protein to solvent extraction. The extractability can be recovered by adding water prior to extraction. It suggests that the dietary exposure risk of OCPs from fish might be underestimated if freeze-dried samples are used. - Highlights: • Freeze drying significantly reduces extractability of OCPs in fish muscle sample. • It is the protein that causes the reduction in extractability of OCPs. • The extractability can be recovered by adding water before extraction. - Freeze drying significantly decreases the concentrations of OCPs extracted from fish muscle samples by microwave-assisted method

  13. Structural and optical study of CaF{sub 2} nanoparticles produced by a microwave-assisted hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Bezerra, Claudiane dos S., E-mail: cdsantos20@gmail.com; Valerio, Mário E.G.

    2016-11-15

    CaF{sub 2} nanoparticles were synthesized by the microwave-assisted hydrothermal method. With the addition of the ethylenediamine (EDA) as chelating agent, the size of the particles was reduced. The CaF{sub 2} exhibit single phase identified for X-ray diffraction (XRD) and confirmed by Rietveld refinement. Scanning electron microscopy (SEM) images showed nanoparticles with non-uniform morphology and statistical analysis of collections of particles reviewed that the EDA decreases both the average particle size and average aspect ratio of the particles. The chemical composition of the surface of the particles was investigated by X-ray Photoelectron Spectroscopy (XPS) and the results indicated the presence of reasonable amounts of hydroxyl groups and oxygen ions in the samples produced with EDA. Radioluminescence (RL) measurements showed that both types of nanoparticles presented intrinsic scintillation emission formed by two main bands and that the CaF{sub 2} samples produced without EDA presented higher emission intensity. The broad RL band centered at approximately 293 nm is related to self-trapped exciton (STE) emission of calcium fluoride, while the band at 428 nm can be due to the presence of F centers. The STE excitation and optical band gap were measured through photoluminescent excitation spectra in the VUV range.

  14. 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.

  15. Easy and fast preparation of TiO{sub 2} - based nanostructures using microwave assisted hydrothermal synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Bregadiolli, Bruna Andressa, E-mail: brunabregadiolli@fc.unesp.br [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Bauru, SP (Brazil); Fernandes, Silvia Leticia; Graeff, Carlos Frederico de Oliveira [Universidade Estadual Paulista de Mesquita Filho (UNESP), Araraquara, SP (Brazil)

    2017-07-15

    TiO{sub 2} derivatives with distinct morphologies have been successfully obtained by microwave assisted hydrothermal synthesis in acidic and alkaline medium using mild conditions. Titanium tetraisopropoxide (TTIP) was used as precursor in different environmental conditions under low temperatures, inferior to 150 °C, and short synthesis times, from 2 to 60 min. X ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N{sub 2} adsorption at 77 K (BET) were used to characterize the microstructural properties of the oxides. In the acidic synthesis the reaction time and temperature are not accompanied by significant changes in the structure of the material. However, in the basic conditions, the concentration of Na{sup +} ions strongly influences the particle morphology and growth. The morphology of the nanoparticles shows irregular spheres in acidic conditions, while in alkaline medium, needle like structures are formed as well as aggregated nanotube-like structures synthesized in only 30 min. Besides the difference in the morphology and structure, in both systems, high surface area was obtained. (author)

  16. Highly Luminescent Carbon Dots Synthesized by Microwave-Assisted Pyrolysis and Evaluation of Their Toxicity to Physa acuta.

    Science.gov (United States)

    Sun, Xiaobo; Jin, Xiaozhe; Pan, Wei; Guo, Enmian; Liu, Weijian; Li, Denghui; Lu, Kunchao; Si, Shuxin; Zhang, Nianxing; Jia, Zhenzhen; Shi, Yanping; Li, Qianqian; Wang, Jinping

    2016-01-01

    As a newly emerging class of nanomaterials, carbon dots have increasingly attracted researchers' attention. However, their potentially adverse environmental effects are yet largely unknown. In this work, the highly luminescent carbon dots were synthesized by microwave-assisted pyrolysis of tris(hydroxymethyl)aminomethane (Tris) and citric acid. Then acute and chronic toxicities of carbon dots to Physa acuta (P. acuta), as well as their effect on reproduction, were evaluated using the as-synthesized dots as an example. The quantum yield of the as-synthesized carbon dots was up to 53.5% excited at 360 nm with the most fluorescent fraction of 82.6% after simple purification by gel column. The results showed that no acute but chronic toxicities to P. acuta exposed to different treatment concentrations of the as-synthesized carbon dots were observed with dose- dependence. In addition, the fecundity of P. acuta was promoted significantly by the carbon dots at the concentrations of 0.5 and 1.0 mg/mL, yet inhibited at the concentration of 3.0 mg/mL after 12-day exposure. Mainly distributing in the visceral mass might be responsible for the effects of the carbon dots on the survival and fecundity of P. acuta. And there was no further evidence to confirm that the carbon dots can cause malformation in developing embryos.

  17. An innovative grape juice enriched in polyphenols by microwave-assisted extraction.

    Science.gov (United States)

    Al Bittar, Sheiraz; Périno-Issartier, Sandrine; Dangles, Olivier; Chemat, Farid

    2013-12-01

    The grape juice by-product obtained from grape traditional press was extracted by Microwave Hydrodiffusion and Gravity (MHG); a green extraction technique preliminarily optimized at 1 W/g. The MHG extract (MHGE) was analyzed by HPLC for identification and quantification of anthocyanins and other phenolic compounds. Then, MHGE was added to the natural juice (NJ) to produce an innovative grape juice (IJ). These three juices were evaluated for their total polyphenol content (TPC), total anthocyanin content (TAC) in addition to their sensorial characteristics. MHGE showed the highest values of TPC (21.41±0.04 mg GAE/g DW), TAC (4.49±0.01 μg MVGE/g DW). Moreover, IJ (grape juice enriched with MHGE) was richer in TPC (6.70±0.0 1mg GAE/g DW) and TAC (3.96±0.01 μg MVGE/g DW) than NJ (2.90±0.02 mg GAE/g DW and 3.63±0.06 μg MVGE/g DW, respectively). Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Biodiesel Production from Dry Microalga Biomass by Microwave-Assisted In-Situ Transesterification

    Directory of Open Access Journals (Sweden)

    Qadariyah Lailatul

    2018-01-01

    Full Text Available Microalga is one of the potential feedstocks in the manufacture of biodiesel because it contains high oil content. In this study, Chlorella sp. was selected because its high oil content about 28-32% of oil (based on its dry weight and its presence is abundant among other green algae. In situ transesterification was carried out in round neck flask under microwave irradiation. Microwave irradiation can facilitate the in situ transesterification by extracted the lipid of microalga and simultaneous convert to FAME. The purposes of this study are to investigate the effect of acid catalyst concentration, microwave power, reaction time and the addition of co-solvent (n-hexane on the yield of biodiesel, to get optimum operating conditions and to know the fatty acid compounds of biodiesel from Chlorella sp. The results of oil extraction and biodiesel were analyzed by GC-MS analysis. Based on the experiment, the yield of microalga oil was 11.37%. The optimum yield of biodiesel by in-situ transesterification was 75.68%. It was obtained at the microwave power of 450 watts, the reaction time of 60 minutes, an acid catalyst concentration of 0,2M of H2SO4, and the co-solvent addition of 10 ml.

  19. Microwave assisted synthesis, spectral, magnetic and bioevolution of few Mn (II)-amide complexes

    Energy Technology Data Exchange (ETDEWEB)

    Joshi, Gaurav [Department of Chemistry, Govt. Engineering College, Bikaner (India); Verma, K. K.; Gudesaria, D. D.; Bhojak, N., E-mail: drbhojak@rediffmail.com [GCRC, Department of Chemistry, Govt Dungar College, Bikaner-334003, Rajasthan (India)

    2016-05-06

    The importance and versatility of amide group containing ligands have promoted the selection of this class of ligands and their complexes for the study. The present work describes the synthesis, spectral and biological investigations on the complexes of amides derived from heterocyclic amines with Mn (II) ions. Four ligands derived 2-aminopyridine and their complexes with Mn (II) have been synthesized. A method for the synthesis of complexes has been developed by the use of microwave irradiation which is in agreement to Green chemistry approach. The complexes have been characterized on the basis of elemental analysis, infrared, electronic, ESR spectra and magnetic susceptibility studies. The diffuse reflectance spectrum of the complexes show bands in the region 20,000 cm{sup −1} to 26,000 cm{sup −1} assignable to {sup 6}A{sub 1g} → {sup 4}T{sub 2g} and {sup 6}A{sub 1g} → {sup 4}E{sub 1g} transitions. These are also typical of tetrahedral environment around the manganese. The magnetic moment (5.80 BM) of the complex indicates high spin tetrahedral environment. The microwave method of synthesis of complexes have been found easier, convenient and ecofriendly. Antimicrobial activities of compounds were also carried out against bacteria and fungi. Further minimal inhibitory concentration (MIC) was also determined for each compound.

  20. 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. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. 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.

  2. Optimization of microwave-assisted extraction conditions for preparing lignan-rich extract from Saraca asoca bark using Box-Behnken design.

    Science.gov (United States)

    Mishra, Shikha; Aeri, Vidhu

    2016-07-01

    Lyoniside is the major constituent of Saraca asoca Linn. (Caesalpiniaceae) bark. There is an immediate need to develop an efficient method to isolate its chemical constituents, since it is a therapeutically important plant. A rapid extraction method for lyoniside based on microwave-assisted extraction of S. asoca bark was developed and optimized using response surface methodology (RSM). Lyoniside was analyzed and quantified by high-performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). The extraction solvent ratio (%), material solvent ratio (g/ml) and extraction time (min) were optimized using Box-Behnken design (BBD) to obtain the highest extraction efficiency. The optimal conditions were the use of 1:30 material solvent ratio with 70:30 mixture of methanol:water for 10 min duration. The optimized microwave-assisted extraction yielded 9.4 mg/g of lyoniside content in comparison to reflux extraction under identical conditions which yielded 4.2 mg/g of lyoniside content. Under optimum conditions, the experimental values agreed closely with the predicted values. The analysis of variance (ANOVA) indicated a high goodness-of-fit model and the success of the RSM method for optimizing lyoniside extraction from the bark of S. asoca. All the three variables significantly affected the lyoniside content. Increased polarity of solvent medium enhances the lyoniside yield. The present study shows the applicability of microwave-assisted extraction in extraction of lyoniside from S. asoca bark.

  3. Facile and Green Synthesis of Saturated Cyclic Amines.

    Science.gov (United States)

    Hameed, Arruje; Javed, Sadia; Noreen, Razia; Huma, Tayyaba; Iqbal, Sarosh; Umbreen, Huma; Gulzar, Tahsin; Farooq, Tahir

    2017-10-12

    Single-nitrogen containing saturated cyclic amines are an important part of both natural and synthetic bioactive compounds. A number of methodologies have been developed for the synthesis of aziridines, azetidines, pyrrolidines, piperidines, azepanes and azocanes. This review highlights some facile and green synthetic routes for the synthesis of unsubstituted, multisubstituted and highly functionalized saturated cyclic amines including one-pot, microwave assisted, metal-free, solvent-free and in aqueous media.

  4. Facile and Green Synthesis of Saturated Cyclic Amines

    Directory of Open Access Journals (Sweden)

    Arruje Hameed

    2017-10-01

    Full Text Available Single-nitrogen containing saturated cyclic amines are an important part of both natural and synthetic bioactive compounds. A number of methodologies have been developed for the synthesis of aziridines, azetidines, pyrrolidines, piperidines, azepanes and azocanes. This review highlights some facile and green synthetic routes for the synthesis of unsubstituted, multisubstituted and highly functionalized saturated cyclic amines including one-pot, microwave assisted, metal-free, solvent-free and in aqueous media.

  5. Microwave assisted rapid synthesis and biological evaluation of stable copper nanoparticles using T. arjuna bark extract

    Science.gov (United States)

    Yallappa, S.; Manjanna, J.; Sindhe, M. A.; Satyanarayan, N. D.; Pramod, S. N.; Nagaraja, K.

    2013-06-01

    Terminalia arjuna (T. arjuna) bark extract is used to reduce Cu2+ → Cu0 under microwave irradiation. The formation of copper nanoparticles (CuNPs) is monitored by recording the UV-Vis absorption spectra for surface plasmon resonance (SPR) peak, ˜535 nm. The intensity of SPR increased linearly with increasing temperature of the reaction mixture. The formation mechanism of CuNPs is supported by the observed marginal decrease in pH and an increase in solution potential (E) of the reaction mixture. X-ray diffraction (XRD) pattern of the CuNPs agrees with the reported data for Cu metal and the crystallite size is ˜23 nm. Fourier transform infrared spectroscopy (FT-IR) and solid-state 13C NMR shows the presence of plant residues on the CuNPs, i.e., in situ bio-capping is possible by this method. Thermo gravimetric (TG) analysis shows the thermal degradation of plant residue and the conversion of Cu to CuO. Field emission electron microscopic (FESEM) image shows uniform spherical particles obtained here. Elemental analysis by energy dispersive X-ray (EDX) analysis confirms the presence of Cu alone, as expected. The in vitro antimicrobial activity is found to be effective for CuNPs dried at RT when compared to CuNPs dried at 70 °C. In addition, CuNPs shows very good antioxidant property.

  6. Microwave assisted rapid synthesis and biological evaluation of stable copper nanoparticles using T. arjuna bark extract.

    Science.gov (United States)

    Yallappa, S; Manjanna, J; Sindhe, M A; Satyanarayan, N D; Pramod, S N; Nagaraja, K

    2013-06-01

    Terminalia arjuna (T. arjuna) bark extract is used to reduce Cu(2+)→Cu(0) under microwave irradiation. The formation of copper nanoparticles (CuNPs) is monitored by recording the UV-Vis absorption spectra for surface plasmon resonance (SPR) peak, ~535 nm. The intensity of SPR increased linearly with increasing temperature of the reaction mixture. The formation mechanism of CuNPs is supported by the observed marginal decrease in pH and an increase in solution potential (E) of the reaction mixture. X-ray diffraction (XRD) pattern of the CuNPs agrees with the reported data for Cu metal and the crystallite size is ~23 nm. Fourier transform infrared spectroscopy (FT-IR) and solid-state (13)C NMR shows the presence of plant residues on the CuNPs, i.e., in situ bio-capping is possible by this method. Thermo gravimetric (TG) analysis shows the thermal degradation of plant residue and the conversion of Cu to CuO. Field emission electron microscopic (FESEM) image shows uniform spherical particles obtained here. Elemental analysis by energy dispersive X-ray (EDX) analysis confirms the presence of Cu alone, as expected. The in vitro antimicrobial activity is found to be effective for CuNPs dried at RT when compared to CuNPs dried at 70 °C. In addition, CuNPs shows very good antioxidant property. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. 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.

  8. Properties of ceria doped with gadolinia via microwave-assisted hydrothermal synthesis

    International Nuclear Information System (INIS)

    Carregosa, J.D.C.; Oliveira, R.M.P.B.; Macedo, D.A.; Nascimento, R.M.

    2016-01-01

    The solid solution of CeO 2 doped with Gd 3+ (CGO) is a promising candidate for electrolyte in Solid Oxide Full Cells (SOFCs) operating in intermediate and low temperatures. The reduction of the working temperature of these energy conversion devices is the great technological challenge to its marketing. In this work, nanocrystalline powders of Ce 1-x Gd x O 2-x/2 with x=0, x=0.1 e x=0.2 were obtained via microwave-hydrothermal synthesis at low temperature and times of synthesis (10 and 20 min at 120° C). The powders were analyzed by TG-DTA, DRX and dilatometry. The results showed characteristic peaks of the cubic fluorite-type structure, referring to the cerium oxide (CeO 2 ), without the presence of secondary peaks. It was also observed that the samples processed at levels of 10 and 20 minutes showed distinct behaviors in contrast to the concentrations of Gd 3+ . (author)

  9. Microwave-assisted Ni-La/γ-Al2O3 catalyst for benzene hydrogenation

    Science.gov (United States)

    Liu, Xianjun; Liu, Shuzhi; Xu, Peiqiang

    2017-11-01

    A series of Ni-La/γ-Al2O3 catalysts were prepared by adopting the methods of isometric impregnation and microwave impregnation. The catalysts were characterized with XRD, BET, and SEM, respectively. Inspecting the effects of adding La and the methods of impregnation on the hydrogenation activity of catalysts. The results show that adding a moderate amount of La promotes the dispersing of Ni on the carrier, the methods of microwave impregnation weaks the interaction between Ni and the carrier further, inhibits the formation of NiAl2O4, and the activity of catalyst prepared by the methods of microwave impregnation was significantly higher than that prepared by the methods of isometric impregnation. The hydrogenation activity of the Ni-La/γ-Al2O3 (WB) dipped with n(Ni): n(La) = 4: 1, microwave irradiation time 30 min with power 600W as well as calcined at 400°C exhibited the best performance. The conversion rate is 91.21% with reaction conditions: T = 160°C, p = 0.8 MPa, air speed 5 h-1, n(H2): n(benzene) = 2: 1.

  10. Fuel production from microwave assisted pyrolysis of coal with carbon surfaces

    International Nuclear Information System (INIS)

    Mushtaq, Faisal; Mat, Ramli; Ani, Farid Nasir

    2016-01-01

    Highlights: • MW heating of coal was carried out with uniformly distributed carbon surfaces. • The effects of carbon loading, MW power and N 2 flow rate were investigated. • Heating profile, pyrolysis products are influenced by the process variables. • Highest coal-tar obtained when final temperature sustained for longer duration. • Coal-tar is mainly composed of aromatics and saturated aliphatics hydrocarbons. - Abstract: In this study, coal solids were subjected to Microwave (MW) pyrolysis conditions. Coconut Activated Carbon (CAC) solids used as a MW absorber was distributed uniformly over coal solids to reduce hotspots. Three process parameters; CAC loading, MW power and N 2 flow rate were studies on pyrolysis heating performance. The highest coal-tar yield of 18.59 wt% was obtained with 600 W, 75 wt% CAC loading and 4 Liter per Minute (LPM) of N 2 flow rate. This improved coal-tar yield is mainly of the fact that higher MW power and CAC loading produced sustained pyrolysis conditions for longer duration for the complete conversion of pyrolysis solids. The coal-tar was composed mainly of aromatics (naphthalenes, benzenes and xylene) and saturated aliphatics (alkanes and alkenes) hydrocarbons. The gas produced from pyrolysis of coal is mainly of H 2 40.23–65.22 vol%.

  11. Ionic liquids as porogens in the microwave-assisted synthesis of methacrylate monoliths for chromatographic application

    Energy Technology Data Exchange (ETDEWEB)

    Singco, Brenda; Lin, Chen-Lan; Cheng, Yi-Jie; Shih, Yung-Han [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China); Huang, Hsi-Ya, E-mail: hyhuang@cycu.edu.tw [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China)

    2012-10-09

    ([C{sub 4}mim][BF{sub 4}]) and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([C{sub 4}mim][Tf{sub 2}N]) successfully decreased the denseness of the monolith, than when using [C{sub 4}mim][Tf{sub 2}N] IL alone, enabling a chromatographic run to be performed with 1:1 ratio produced baseline separation for the analytes. The combination of ILs and microwave irradiation made polymer synthesis very fast ({approx}10 min), entirely green (organic solvent-free) and energy saving process.

  12. Optimization of microwave-assisted extraction (MAE) of coriander phenolic antioxidants - response surface methodology approach.

    Science.gov (United States)

    Zeković, Zoran; Vladić, Jelena; Vidović, Senka; Adamović, Dušan; Pavlić, Branimir

    2016-10-01

    Microwave-assisted extraction (MAE) of polyphenols from coriander seeds was optimized by simultaneous maximization of total phenolic (TP) and total flavonoid (TF) yields, as well as maximized antioxidant activity determined by 1,1-diphenyl-2-picrylhydrazyl and reducing power assays. Box-Behnken experimental design with response surface methodology (RSM) was used for optimization of MAE. Extraction time (X1 , 15-35 min), ethanol concentration (X2 , 50-90% w/w) and irradiation power (X3 , 400-800 W) were investigated as independent variables. Experimentally obtained values of investigated responses were fitted to a second-order polynomial model, and multiple regression analysis and analysis of variance were used to determine fitness of the model and optimal conditions. The optimal MAE conditions for simultaneous maximization of polyphenol yield and increased antioxidant activity were an extraction time of 19 min, an ethanol concentration of 63% and an irradiation power of 570 W, while predicted values of TP, TF, IC50 and EC50 at optimal MAE conditions were 311.23 mg gallic acid equivalent per 100 g dry weight (DW), 213.66 mg catechin equivalent per 100 g DW, 0.0315 mg mL(-1) and 0.1311 mg mL(-1) respectively. RSM was successfully used for multi-response optimization of coriander seed polyphenols. Comparison of optimized MAE with conventional extraction techniques confirmed that MAE provides significantly higher polyphenol yields and extracts with increased antioxidant activity. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  13. Microwave-Assisted Extraction of Natural Antioxidants from the Exotic Gordonia axillaris Fruit: Optimization and Identification of Phenolic Compounds.

    Science.gov (United States)

    Li, Ya; Li, Sha; Lin, Sheng-Jun; Zhang, Jiao-Jiao; Zhao, Cai-Ning; Li, Hua-Bin

    2017-09-06

    Our previous study reported that the fruit of Gordonia axillaris , an edible wild fruit, possessed strong antioxidant activity. In this study, a microwave-assisted extraction (MAE) method was established to extract antioxidants from the fruit of Gordonia axillaris . The influence of five parameters, including ethanol concentration, solvent/material ratio, extraction time, extraction temperature and microwave power, was investigated by single-factor experiments. Three factors, namely ethanol concentration, solvent/material ratio, extraction time, were found to exert a major influence on extraction efficacy, and were further studied by response surface methodology to investigate their interactions. Ethanol concentration of 36.89%, solvent/material ratio of 29.56 mL/g, extraction time of 71.04 min, temperature of 40 °C, and microwave power of 400 W were found to be the optimal condition. The TEAC value was 198.16 ± 5.47 µmol Trolox/g DW under the optimal conditions, which was in conformity to the predicted value (200.28 µmol Trolox/g DW). In addition, the MAE method was compared with two conventional methods (Soxhlet extraction and maceration extraction). Results showed that the antioxidant capacity of the extract obtained by MAE method was stronger than that obtained by maceration (168.67 ± 3.88 µmol Trolox/g DW) or Soxhlet extraction (114.09 ± 2.01 µmol Trolox/g DW). Finally, several phenolic compounds in the extract were identified and quantified by UPLC-MS/MS, which were rutin, gallic acid, protocatechuic acid, epicatechin, epicatechin gallate, 2-hydrocinnamic acid, p -coumaric acid, quercetin, chlorogenic acid and ferulic acid.

  14. Microwave-Assisted Extraction of Cannabinoids in Hemp Nut Using Response Surface Methodology: Optimization and Comparative Study

    Directory of Open Access Journals (Sweden)

    Chih-Wei Chang

    2017-11-01

    Full Text Available Hemp nut is commonly incorporated into several food preparations; however, most countries set regulations for hemp products according to their cannabinoid content. In this study, we have developed an efficient microwave-assisted extraction (MAE method for cannabinoids (i.e., Δ9-tetrahydrocannabinol, cannabidiol, and cannabinol in hemp nut. Optimization of the MAE procedure was conducted through single factor experiments and response surface methodology (RSM. A comparative study was also conducted to determine the differences in the extraction yields and morphology of hemp nut between MAE and reference extraction methods, namely heat reflux extraction (HRE, Soxhlet extraction (SE, supercritical fluid extraction (SFE, and ultrasound-assisted extraction (UAE. Among the independent variables in RSM, the temperature was the most significant parameter. The optimal conditions of MAE were as follows: extraction solvent of methanol, microwave power of 375 W, temperature of 109 °C, and extraction time of 30 min. Compared with reference extraction methods, MAE achieved the highest extraction yields of total cannabinoids in hemp nut (6.09 μg/g for MAE; 4.15 μg/g for HRE; 5.81 μg/g for SE; 3.61 μg/g for SFE; 3.73 μg/g for UAE with the least solvent consumption and shortest time. Morphological observations showed that substantial cell rupturing occurred in the microstructure of hemp nut after MAE, indicating enhanced dissolution of the target compounds during the extraction process. The MAE method is thus a rapid, economic, and environmentally friendly extraction method that is both effective and practical for industrial applications.

  15. Rapid synthesis of Ti-MCM-41 by microwave-assisted hydrothermal method towards photocatalytic degradation of oxytetracycline.

    Science.gov (United States)

    Chen, Hanlin; Peng, Yen-Ping; Chen, Ku-Fan; Lai, Chia-Hsiang; Lin, Yung-Chang

    2016-06-01

    This study employed microwave-assisted hydrothermal method to synthesize Ti-MCM-41, which are mesoporous materials with a high surface area and excellent photocatalytic ability. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet-visible spectroscopy (UV-Vis) were employed. The XRD findings showed that Ti-MCM-41 exhibited a peak at 2θ of 2.2°, which was attributed to the hexagonal MCM-41 structure. The BET (Brunauer-Emmett-Teller) results agreed with the TEM findings that Ti-MCM-41 has a pore size of about 3-5nm and a high surface area of 883m(2)/g. FTIR results illustrated the existence of Si-O-Si and Si-O-Ti bonds in Ti-MCM-41. The appearance of Ti 2p peaks in the XPS results confirmed the FTIR findings that the Ti was successfully doped into the MCM-41 structure. Zeta (ζ)-potential results indicated that the iso-electric point (IEP) of Ti-MCM-41 was at about pH3.02. In this study, the photocatalytic degradation of oxytetracycline (OTC) at different pH was investigated under Hg lamp irradiation (wavelength 365nm). The rate constant (K'obs) for OTC degradation was 0.012min(-1) at pH3. Furthermore, TOC (total organic carbon) and high resolution LC-MS (liquid chromatography-mass spectrometry) analyses were conducted to elucidate the possible intermediate products and degradation pathway for OTC. The TOC removal efficiency of OTC degradation was 87.0%, 74.4% and 50.9% at pH3, 7 and 10, respectively. LC-MS analysis results showed that the degradation products from OTC resulted from the removal of functional groups from the OTC ring. Copyright © 2016. Published by Elsevier B.V.

  16. Microwave-assisted RAFT polymerization of well-constructed magnetic surface molecularly imprinted polymers for specific recognition of benzimidazole residues

    Science.gov (United States)

    Chen, Fangfang; Wang, Jiayu; Chen, Huiru; Lu, Ruicong; Xie, Xiaoyu

    2018-03-01

    Magnetic nanoparticles have been widely used as support core for fast separation, which could be directly separated from complicated matrices using an external magnet in few minutes. Surface imprinting based on magnetic core has shown favorable adsorption and separation performance, including good adsorption capacity, fast adsorption kinetics and special selectivity adsorption. Reversible addition-fragmentation chain transfer (RAFT) is an ideal choice for producing well-defined complex architecture with mild reaction conditions. We herein describe the preparation of well-constructed magnetic molecularly imprinted polymers (MMIPs) for the recognition of benzimidazole (BMZ) residues via the microwave-assisted RAFT polymerization. The merits of RAFT polymerization assisting with microwave heating allowed successful and more efficient preparation of well-constructed imprinted coats. Moreover, the polymerization time dramatically shortened and was just 1/24th of the time taken by conventional heating. The results indicated that a uniform nanoscale imprinted layer was formed on the Fe3O4 core successfully, and enough saturation magnetization of MMIPs (16.53 emu g-1) was got for magnetic separation. The desirable adsorption capacity (30.18 μmol g-1) and high selectivity toward template molecule with a selectivity coefficient (k) of 13.85 of MMIPs were exhibited by the adsorption isothermal assay and competitive binding assay, respectively. A solid phase extraction enrichment approach was successfully established for the determination of four BMZ residues from apple samples using MMIPs coupled to HPLC. Overall, this study provides a versatile approach for highly efficient fabrication of well-constructed MMIPs for enrichment and determination of target molecules from complicated samples.

  17. Optimisation of focused ultrasound extraction (FUSE) and microwave-assisted extraction (MAE) of hydrocarbons in geological chert samples.

    Science.gov (United States)

    Olivares, Maitane; Vallejo, Asier; Irazola, Mireia; Murelaga, Xabier; Baceta, Juan Ignacio; Tarriño, Andoni; Etxebarria, Nestor

    2010-12-15

    The analysis of hydrocarbons in chert rocks provides a worthwhile source of information regarding the geochemical features of a depositional setting. Since the typical analytical procedure requires long Soxhlet extractions and the use of large quantities of sample (30-50 g), in this work we have optimised the focused ultrasound extraction (FUSE) and the microwave-assisted extraction (MAE) to make available a less severe procedure. In both cases a full experimental design including solvent mixture composition (Dichloromethane/Hexane/Acetone) and process variables (sonication time and cycles, and extraction temperature and time) by means of D-optimal designs. In the extracted fractions hydrocarbons (C(16)-C(40)) were analysed by gas-chromatography-mass spectrometry. In the case of FUSE the process variables were the most sensitive variables and the optimum conditions were defined at 60:40 DCM/Hex mixture and a sonication time of 30 min and 9 cycles. In the case of MAE all the variables shown a significant effect on the extraction yield and the most adequate conditions (60:30:10 DCM/Hex/Ace mixture and an irradiation time of 15 min at 110 °C) were established from the analysis of the response surface. Both methods were systematically applied with different chert samples collected in Cucho (Trebiño County, Burgos, Spain) and we were able to assure quantitative extractions (>85%) in the first extraction. Additionally, from the distribution patterns of n-alkanes obtained in the different chert samples (nodular chert, laminar chert and massive-brechoid chert) collected in Cucho, we were able to distinguish different origins and diagenetic history. Copyright © 2010 Elsevier B.V. All rights reserved.

  18. Optimization of microwave-assisted extraction and supercritical fluid extraction of carbamate pesticides in soil by experimental design methodology.

    Science.gov (United States)

    Sun, Lei; Lee, Hian Kee

    2003-10-03

    Orthogonal array design (OAD) was applied for the first time to optimize microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) conditions for the analysis of four carbamates (propoxur, propham, methiocarb, chlorpropham) from soil. The theory and methodology of a new OA16 (4(4)) matrix derived from a OA16 (2(15)) matrix were developed during the MAE optimization. An analysis of variance technique was employed as the data analysis strategy in this study. Determinations of analytes were completed using high-performance liquid chromatography (HPLC) with UV detection. Four carbamates were successfully extracted from soil with recoveries ranging from 85 to 105% with good reproducibility (approximately 4.9% RSD) under the optimum MAE conditions: 30 ml methanol, 80 degrees C extraction temperature, and 6-min microwave heating. An OA8 (2(7)) matrix was employed for the SFE optimization. The average recoveries and RSD of the analytes from spiked soil by SFE were 92 and 5.5%, respectively except for propham (66.3+/-7.9%), under the following conditions: heating for 30 min at 60 degrees C under supercritical CO2 at 300 kg/cm2 modified with 10% (v/v) methanol. The composition of the supercritical fluid was demonstrated to be a crucial factor in the extraction. The addition of a small volume (10%) of methanol to CO2 greatly enhanced the recoveries of carbamates. A comparison of MAE with SFE was also conducted. The results indicated that >85% average recoveries were obtained by both optimized extraction techniques, and slightly higher recoveries of three carbamates (propoxur, propham and methiocarb) were achieved using MAE. SFE showed slightly higher recovery for chlorpropham (93 vs. 87% for MAE). The effects of time-aged soil on the extraction of analytes were examined and the results obtained by both methods were also compared.

  19. Microwave-Assisted Extraction of Cannabinoids in Hemp Nut Using Response Surface Methodology: Optimization and Comparative Study.

    Science.gov (United States)

    Chang, Chih-Wei; Yen, Ching-Chi; Wu, Ming-Tsang; Hsu, Mei-Chich; Wu, Yu-Tse

    2017-11-03

    Hemp nut is commonly incorporated into several food preparations; however, most countries set regulations for hemp products according to their cannabinoid content. In this study, we have developed an efficient microwave-assisted extraction (MAE) method for cannabinoids (i.e., Δ9-tetrahydrocannabinol, cannabidiol, and cannabinol) in hemp nut. Optimization of the MAE procedure was conducted through single factor experiments and response surface methodology (RSM). A comparative study was also conducted to determine the differences in the extraction yields and morphology of hemp nut between MAE and reference extraction methods, namely heat reflux extraction (HRE), Soxhlet extraction (SE), supercritical fluid extraction (SFE), and ultrasound-assisted extraction (UAE). Among the independent variables in RSM, the temperature was the most significant parameter. The optimal conditions of MAE were as follows: extraction solvent of methanol, microwave power of 375 W, temperature of 109 °C, and extraction time of 30 min. Compared with reference extraction methods, MAE achieved the highest extraction yields of total cannabinoids in hemp nut (6.09 μg/g for MAE; 4.15 μg/g for HRE; 5.81 μg/g for SE; 3.61 μg/g for SFE; 3.73 μg/g for UAE) with the least solvent consumption and shortest time. Morphological observations showed that substantial cell rupturing occurred in the microstructure of hemp nut after MAE, indicating enhanced dissolution of the target compounds during the extraction process. The MAE method is thus a rapid, economic, and environmentally friendly extraction method that is both effective and practical for industrial applications.

  20. Microwave-Assisted Extraction of Natural Antioxidants from the Exotic Gordonia axillaris Fruit: Optimization and Identification of Phenolic Compounds

    Directory of Open Access Journals (Sweden)

    Ya Li

    2017-09-01

    Full Text Available Our previous study reported that the fruit of Gordonia axillaris, an edible wild fruit, possessed strong antioxidant activity. In this study, a microwave-assisted extraction (MAE method was established to extract antioxidants from the fruit of Gordonia axillaris. The influence of five parameters, including ethanol concentration, solvent/material ratio, extraction time, extraction temperature and microwave power, was investigated by single-factor experiments. Three factors, namely ethanol concentration, solvent/material ratio, extraction time, were found to exert a major influence on extraction efficacy, and were further studied by response surface methodology to investigate their interactions. Ethanol concentration of 36.89%, solvent/material ratio of 29.56 mL/g, extraction time of 71.04 min, temperature of 40 °C, and microwave power of 400 W were found to be the optimal condition. The TEAC value was 198.16 ± 5.47 µmol Trolox/g DW under the optimal conditions, which was in conformity to the predicted value (200.28 µmol Trolox/g DW. In addition, the MAE method was compared with two conventional methods (Soxhlet extraction and maceration extraction. Results showed that the antioxidant capacity of the extract obtained by MAE method was stronger than that obtained by maceration (168.67 ± 3.88 µmol Trolox/g DW or Soxhlet extraction (114.09 ± 2.01 µmol Trolox/g DW. Finally, several phenolic compounds in the extract were identified and quantified by UPLC-MS/MS, which were rutin, gallic acid, protocatechuic acid, epicatechin, epicatechin gallate, 2-hydrocinnamic acid, p-coumaric acid, quercetin, chlorogenic acid and ferulic acid.

  1. Microwave-assisted synthesis, characterization and antibacterial activity of Ag/ZnO nanoparticles supported bentonite clay

    International Nuclear Information System (INIS)

    Motshekga, Sarah C.; Ray, Suprakas S.; Onyango, Maurice S.; Momba, Maggie N.B.

    2013-01-01

    Highlights: • A facile, fast and effective method was used for preparing metal–clay composites. • The metal/oxide loaded on clay exhibited narrow size range at nano scale. • The composites deactivate both Gram negative and Gram positive bacteria. • A combination of metal and metal oxide provides the best antibacterial property. -- Abstract: Composites of silver–zinc oxide nanoparticles supported on bentonite clay were synthesized by the microwave-assisted synthesis method for use as an antibacterial material. Silver nitrate was used as the precursor of silver nanoparticles while zinc oxide nanoparticles were commercially sourced. The composites were characterized by powder X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared (FTIR) and BET surface area measurements. XRD spectra showed peaks of silver confirming the formation of the silver and not of the silver nitrate or any other impurity of the metal. Meanwhile TEM confirmed the formation of silver and zinc oxide nanoparticles on the clay layers, with particle sizes ranging from 9–30 nm and 15–70 nm, respectively. The antibacterial activities of the composites were evaluated against Gram negative Escherichia coli bacteria and Gram positive Enterococcus faecalis bacteria by the disc diffusion method. Whereas both composites of Ag-clay and ZnO-clay showed good antibacterial activity against bacteria, a better antibacterial activity was observed with Ag/ZnO-clay composite. The results therefore reveal that Ag/ZnO-clay composite is a promising bactericide that can be used for deactivating microbes in water

  2. Microwave-assisted activated carbon from cocoa shell as adsorbent for removal of sodium diclofenac and nimesulide from aqueous effluents

    International Nuclear Information System (INIS)

    Saucier, Caroline; Adebayo, Matthew A.; Lima, Eder C.; Cataluña, Renato; Thue, Pascal S.; Prola, Lizie D.T.; Puchana-Rosero, M.J.; Machado, Fernando M.; Pavan, Flavio A.; Dotto, G.L.

    2015-01-01

    Highlights: • Microwave-assisted cocoa shell activated carbon was prepared and characterized. • The anti-inflammatories, diclofenac and nimesulide, were adsorbed onto MWCS-1.0. • Adsorption maximum values are 63.47 (diclofenac) and 74.81 mg g −1 (nimesulide). • General order kinetic model suitably explained the adsorption process. • MWCS-1.0 was effectively used for treatment of simulated hospital effluents. - Abstract: Microwave-induced chemical activation process was used to prepare an activated carbon from cocoa shell for efficient removal of two anti-inflammatories, sodium diclofenac (DFC) and nimesulide (NM), from aqueous solutions. A paste was obtained from a mixture of cocoa shell and inorganic components; with a ratio of inorganic: organic of 1 (CSC-1.0). The mixture was pyrolyzed in a microwave oven in less than 10 min. The CSC-1.0 was acidified with a 6 mol L −1 HCl under reflux to produce MWCS-1.0. The CSC-1.0 and MWCS-1.0 were characterized using FTIR, SEM, N 2 adsorption/desorption curves, X-ray diffraction, and point of zero charge (pH pzc ). Experimental variables such as initial pH of the adsorbate solutions and contact time were optimized for adsorptive characteristics of MWCS-1.0. The optimum pH for removal of anti-inflammatories ranged between 7.0 and 8.0. The kinetic of adsorption was investigated using general order, pseudo first-order and pseu do-second order kinetic models. The maximum amounts of DCF and NM adsorbed onto MWCS-1.0 at 25 °C are 63.47 and 74.81 mg g −1 , respectively. The adsorbent was tested on two simulated hospital effluents. MWCS-1.0 is capable of efficient removal of DCF and NM from a medium that contains high sugar and salt concentrations

  3. Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

    International Nuclear Information System (INIS)

    Sciancalepore, Corrado; Bondioli, Federica; Manfredini, Tiziano; Gualtieri, Alessandro

    2015-01-01

    An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals was followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe 3 O 4 nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis

  4. Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Sciancalepore, Corrado, E-mail: corrado.sciancalepore@unimore.it [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Pietro Vivarelli 10, 41100 Modena (Italy); Bondioli, Federica [Department of Industrial Engineering, University of Parma, Parco Area delle Scienze, 181/A, 43124 Parma (Italy); INSTM Consortium, Via G. Giusti 9, 51121 Firenze (Italy); Manfredini, Tiziano [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Pietro Vivarelli 10, 41100 Modena (Italy); INSTM Consortium, Via G. Giusti 9, 51121 Firenze (Italy); Gualtieri, Alessandro [Department of Chemical and Geological Science, University of Modena and Reggio Emilia, Via S. Eufemia 19, 41121 Modena Italy (Italy)

    2015-02-15

    An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals was followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.

  5. 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.

  6. Microwave-assisted synthesis, characterization and antibacterial activity of Ag/ZnO nanoparticles supported bentonite clay

    Energy Technology Data Exchange (ETDEWEB)

    Motshekga, Sarah C. [DST/CSIR National Centre for Nanostructured Materials, Council for Scientific and Industrial Research, Pretoria 0001 (South Africa); Department of Chemical, Metallurgical and Materials Engineering, Tshwane University of Technology, Pretoria 0001 (South Africa); Ray, Suprakas S. [DST/CSIR National Centre for Nanostructured Materials, Council for Scientific and Industrial Research, Pretoria 0001 (South Africa); Onyango, Maurice S., E-mail: OnyangoMS@tut.ac.za [Department of Chemical, Metallurgical and Materials Engineering, Tshwane University of Technology, Pretoria 0001 (South Africa); Momba, Maggie N.B. [Department of Environmental, Water and Earth Sciences, Tshwane University of Technology, Arcadia Campus, Pretoria 0001 (South Africa)

    2013-11-15

    Highlights: • A facile, fast and effective method was used for preparing metal–clay composites. • The metal/oxide loaded on clay exhibited narrow size range at nano scale. • The composites deactivate both Gram negative and Gram positive bacteria. • A combination of metal and metal oxide provides the best antibacterial property. -- Abstract: Composites of silver–zinc oxide nanoparticles supported on bentonite clay were synthesized by the microwave-assisted synthesis method for use as an antibacterial material. Silver nitrate was used as the precursor of silver nanoparticles while zinc oxide nanoparticles were commercially sourced. The composites were characterized by powder X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared (FTIR) and BET surface area measurements. XRD spectra showed peaks of silver confirming the formation of the silver and not of the silver nitrate or any other impurity of the metal. Meanwhile TEM confirmed the formation of silver and zinc oxide nanoparticles on the clay layers, with particle sizes ranging from 9–30 nm and 15–70 nm, respectively. The antibacterial activities of the composites were evaluated against Gram negative Escherichia coli bacteria and Gram positive Enterococcus faecalis bacteria by the disc diffusion method. Whereas both composites of Ag-clay and ZnO-clay showed good antibacterial activity against bacteria, a better antibacterial activity was observed with Ag/ZnO-clay composite. The results therefore reveal that Ag/ZnO-clay composite is a promising bactericide that can be used for deactivating microbes in water.

  7. Microwave-Assisted Extraction, Chemical Structures, and Chain Conformation of Polysaccharides from a Novel Cordyceps Sinensis Fungus UM01.

    Science.gov (United States)

    Cheong, Kit-Leong; Wang, Lan-Ying; Wu, Ding-Tao; Hu, De-Jun; Zhao, Jing; Li, Shao-Ping

    2016-09-01

    Cordyceps sinensis is a well-known tonic food with broad medicinal properties. The aim of the present study was to investigate the optimization of microwave-assisted extraction (MAE) and characterize chemical structures and chain conformation of polysaccharides from a novel C. sinensis fungus UM01. Ion-exchange and gel filtration chromatography were used to purify the polysaccharides. The chemical structure of purified polysaccharide was determined through gas chromatography-mass spectrometry. Moreover, high performance size exclusion chromatography combined with refractive index detector and multiangle laser light scattering were conducted to analyze the molecular weight (Mw ) and chain conformation of purified polysaccharide. Based on the orthogonal design L9 , optimal MAE conditions could be obtained through 1300 W of microwave power, with a 5-min irradiation time at a solid to water ratio of 1:60, generating the highest extraction yield of 6.20%. Subsequently, the polysaccharide UM01-S1 was purified. The UM01-S1 is a glucan-type polysaccharide with a (1→4)-β-d-glucosyl backbone and branching points located at O-3 of Glcp with a terminal-d-Glcp. The Mw , radius of gyration (Rg ) and hydrodynamic radius (Rh ) of UM01-S1 were determined as 5.442 × 10(6)  Da, 21.8 and 20.2 nm, respectively. Using the polymer solution theory, the exponent (ν) value of the power law function was calculated as 0.38, and the shape factor (ρ = Rg /Rh ) was 1.079, indicating that UM01-S1 has a sphere-like conformation with a branched structure in an aqueous solution. These results provide fundamental information for the future application of polysaccharides from cultured C. sinensis in health and functional food area. © 2016 Institute of Food Technologists®

  8. Fast low-pressurized microwave-assisted extraction of benzotriazole, benzothiazole and benezenesulfonamide compounds from soil samples.

    Science.gov (United States)

    Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Porta, Alessio; Profumo, Antonella

    2016-01-15

    Benzotriazoles (BTRs), benzothiazoles (BTs) and benzenesulfonamides (BSAs), compounds largely used in industrial and household applications, are ubiquitous emerging contaminants. In this work a novel, straightforward procedure for the simultaneous determination of two BTRs (1H-benzotriazole, 5-methyl-1H-benzotriazole), three BTs (benzothiazole, 2-hydroxybenzothiazole, 2-methylthiobenzothiazole) and two BSAs (benzenesulfonamide, toluenesulfonamide) in soil has been developed. The target analytes were extracted from soil by a single low-pressurized microwave-assisted extraction (MAE) cycle (120°C, 10min) and quantified by high-performance liquid chromatography with UV detection. For all the seven analytes, quantitative extraction yields (72-119%, n=4) were observed from recovery tests on soil samples (1g) spiked with 5, 10 and 50mg kg(-1), using 4mL water-methanol (85:15) as extracting solution. For the lower concentrations levels (100, 250 and 500μg kg(-1)), the analytes were extracted from soil samples (2-3g) using 6mL methanol, and the extract was pre-concentrated by evaporation before analysis; recoveries in the range 70-117% were obtained (n=4). Suitable intra-day and inter-day precision were observed, with values of relative standard deviation generally below 6% and 11% (n=4), respectively. Linearity was evaluated in the concentration range 0.5-10mg L(-1) by matrix-matched standards, obtaining r(2)>0.9996. The experimental method quantification limit (MQL) was 100μg kg(-1). The entire procedure has been successfully applied to the analysis of real impacted soil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. 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.

  10. Comparison of essential oil composition and antimicrobial activity of Coriandrum sativum L. extracted by hydrodistillation and microwave-assisted hydrodistillation.

    Science.gov (United States)

    Sourmaghi, Mohammad Hossein Salehi; Kiaee, Gita; Golfakhrabadi, Fereshteh; Jamalifar, Hossein; Khanavi, Mahnaz

    2015-04-01

    Coriander (Coriandrum sativum L.), is an annual herb in the Apiaceae family which disperses in Mediterranean and Middle Eastern regions. The Coriander essential oil has been used in food products, perfumes, cosmetics and pharmaceutical industries for its flavor and odor. In Iran, fruits of Coriander used in pickle, curry powders, sausages, cakes, pastries, biscuits and buns. The aim of this study was to investigate microwave radiation effects on quality, quantity and antimicrobial activity of essential oil of Coriander fruits. The essential oils were obtained from the Coriander fruits by hydrodistillation (HD) and Microwave-assisted hydrodistillation (MAHD) then, the oils were analyzed by GC and GC-MS. Antimicrobial activities of essential oils were evaluated against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa and Candida albicans by microdilution method. The results indicated that the HD and MAHD essential oils (EO) were dominated by monoterpenoids such as linalool, geranyl acetate and γ-terpinene. The major compound in both EO was linalool which its amount in HD and MAHD was 63 % and 66 %, respectively. The total amount of monoterpenes hydrocarbons in HD EO differ significantly with the amount in MAHD EO (12.56 % compare to 1.82 %). HD EO showed greater activity against Staphylococcus aureus and Candida albicans than MAHD EO. Moreover, their activities against Ecoli and P. aeruginosa were the same with Minimum Inhibitory Concentration (MIC) 0.781 and 6.25 μL mL(-1), respectively. By using MAHD method, it was superior in terms of saving energy and extraction time, although the oil yield and total composition decrease by using this method.

  11. Mesoporous upconversion nanoparticles modified with a Tb(III) complex to display both green upconversion and down conversion luminescence for in vitro bioimaging and sensing of temperature

    International Nuclear Information System (INIS)

    Ge, Xiaoqian; Sun, Lining; Liu, Jinliang; Xu, Yanxia; Wei, Zuwu; Shi, Liyi; Dang, Song; Zhang, Hongjie

    2015-01-01

    A new multifunctional nanocomposite is described that displays both upconversion and down conversion luminescence. It is based on upconversion nanoparticles (UCNPs) with a mesoporous coating that is boned with a terbium(III) complex. The modified mesoporous nanocomposite was characterized by transmission electron microscopy, X-ray powder diffraction, nitrogen adsorption-desorption isotherms, and photoluminescence spectra. They display dual (green and red) fluorescence under 980-nm excitation, and green fluorescence under 365-nm excitation. Both emissions can be easily detected by bare eyes. The material has low cytotoxicity and good biocompatibility as proven by the methyl thiazolyltetrazolium (MTT) assay. The nanocomposite was successfully applied to upconversion luminescence based in-vitro confocal imaging of the cytosol of murine macrophage cells (RAW264.7), and this resulted in images of excellent contrast. In addition, the particles display strongly temperature-dependent luminescence in the range from 280 K to 330 K. (author)

  12. A green approach to ethyl acetate: Quantitative conversion of ethanol through direct dehydrogenation in a Pd-Ag membrane reactor

    KAUST Repository

    Zeng, Gaofeng

    2012-11-07

    Pincers do the trick: The conversion of ethanol to ethyl acetate and hydrogen was achieved using a pincer-Ru catalyst in a Pd-Ag membrane reactor. Near quantitative conversions and yields could be achieved without the need for acid or base promoters or hydrogen acceptors (see scheme). © 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Integrated Electrochemical Processes for CO2 Capture and Conversion to Commodity Chemicals

    Energy Technology Data Exchange (ETDEWEB)

    Hatton, T. Alan [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States); Jamison, Timothy [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)

    2013-09-30

    The Massachusetts Institute of Technology (MIT) and Siemens Corporations (SCR) are developing new chemical synthesis processes for commodity chemicals from CO2. The process is assessed as a novel chemical sequestration technology that utilizes CO2 from dilute gas streams generated at industrial carbon emitters as a raw material to produce useful commodity chemicals. Work at Massachusetts Institute of Technology (MIT) commenced on October 1st, 2010, and finished on September 30th, 2013. During this period, we have investigated and accomplished five objectives that mainly focused on converting CO2 into high-value chemicals: 1) Electrochemical assessment of catalytic transformation of CO2 and epoxides to cyclic carbonates; 2) Investigation of organocatalytic routes to convert CO2 and epoxide to cyclic carbonates; 3) Investigation of CO2 Capture and conversion using simple olefins under continuous flow; 4) Microwave assisted synthesis of cyclic carbonates from olefins using sodium bicarbonates in a green pathway; 5) Life cycle analyses of integrated chemical sequestration process. In this final report, we will describe the detailed study performed during the three year period and findings and conclusions drawn from our research.

  14. Microwave-assisted synthesis and characterization of poly(acrylic)/SiO2-TiO2 core-shell nanoparticle hybrid thin films

    International Nuclear Information System (INIS)

    Chien, Wen-Chen; Yu, Yang-Yen; Chen, Po-Kan; Yu, Hui-Huan

    2011-01-01

    In this study, poly(acrylic)/SiO 2 -TiO 2 core-shell nanoparticle hybrid thin films were successfully synthesized by microwave-assisted polymerization. The coupling agent 3-(trimethoxysilyl) propyl methacrylate (MSMA) was hydrolyzed with colloidal SiO 2 -TiO 2 core-shell nanoparticles, and then polymerized with two acrylic monomers and initiator to form a precursor solution. The results of this study showed that the spin-coated hybrid films had relatively good surface planarity, high thermal stability, a tunable refractive index (1.525 2 -TiO 2 core-shell nanoparticle hybrid thin films, for potential use in optical applications.

  15. Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo [Universidad Autonoma de Tamaulipas, Reynosa (Mexico). Dept. de Farmacia y Quimica Medicinal; Monge, Antonio [Universidad de Navarra, Pamplona (Spain). Centro de Investigacion en Farmacobiologia Aplicada. Unidad de Investigacion y Desarrollo de Medicamentos

    2011-07-01

    We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

  16. Microwave-assisted convenient syntheses of 2-indolizine derivatives from Morita-Baylis-Hillman adducts: new in silico potential ion channel modulators

    International Nuclear Information System (INIS)

    Cunha, Saraghina M.D.; Oliveira, Ramon G. de; Vasconcellos, Mario L.A.A.

    2013-01-01

    In this work, a microwave-assisted synthesis study by microwave irradiation to produce indolizine-2-carbonitrile and indolizine-2-carboxylate in good to high yields (70 and 81%, respectively) in one step from Morita-Baylis-Hillman adducts (MBHA) is presented. These compounds were subsequently transformed to high yields (94 to 100%, respectively) in three 2-indolizine derivatives. The five synthesized compounds were designed in silico aiming to present potential selective activities as ion channel modulators. These activities were suggested by the score values using Molinspiration Cheminformatics program. (author)

  17. The synthesis of α-aryl-α-aminophosphonates and α-aryl-α-aminophosphine oxides by the microwave-assisted Pudovik reaction

    Directory of Open Access Journals (Sweden)

    Erika Bálint

    2017-01-01

    Full Text Available A family of α-aryl-α-aminophosphonates and α-aryl-α-aminophosphine oxides was synthesized by the microwave-assisted solvent-free addition of dialkyl phosphites and diphenylphosphine oxide, respectively, to imines formed from benzaldehyde derivatives and primary amines. After optimization, the reactivity was mapped, and the fine mechanism was evaluated by DFT calculations. Two α-aminophosphonates were subjected to an X-ray study revealing a racemic dimer formation made through a N–H···O=P intermolecular hydrogen bridges pair.

  18. Nano-organocatalyst: magnetically retrievable ferrite-anchored glutathione for microwave-assisted Paal–Knorr reaction, aza-Michael addition, and pyrazole synthesis

    KAUST Repository

    Polshettiwar, Vivek

    2010-01-01

    Postsynthetic Surface modification of magnetic nanoparticles by glutathione imparts desirable chemical functionality and enables the generation of catalytic sites on the surfaces of ensuing organocatalysts. In this article, we discuss the developments, unique activity, and high selectivity of nano-organocatalysts for microwave-assisted Paal-Knorr reaction, aza-Michael addition, and pyrazole synthesis. Their insoluble character Coupled with paramagnetic nature enables easy separation of these nano-catalysts from the reaction mixture using external magnet, which eliminates the requirement of catalyst filtration. Published by Elsevier Ltd.

  19. Accurate Analysis and Evaluation of Acidic Plant Growth Regulators in Transgenic and Nontransgenic Edible Oils with Facile Microwave-Assisted Extraction-Derivatization.

    Science.gov (United States)

    Liu, Mengge; Chen, Guang; Guo, Hailong; Fan, Baolei; Liu, Jianjun; Fu, Qiang; Li, Xiu; Lu, Xiaomin; Zhao, Xianen; Li, Guoliang; Sun, Zhiwei; Xia, Lian; Zhu, Shuyun; Yang, Daoshan; Cao, Ziping; Wang, Hua; Suo, Yourui; You, Jinmao

    2015-09-16

    Determination of plant growth regulators (PGRs) in a signal transduction system (STS) is significant for transgenic food safety, but may be challenged by poor accuracy and analyte instability. In this work, a microwave-assisted extraction-derivatization (MAED) method is developed for six acidic PGRs in oil samples, allowing an efficient (transgenic and nontransgenic oils, particularly 1-naphthaleneacetic acid (1-NAA), implying the PGRs induced variations of components and genes. This study provides, for the first time, an accurate and efficient determination for labile PGRs involved in STS and a promising concept for objectively evaluating the safety of transgenic foods.

  20. Microwave-assisted reductive cyclization: An easy entry to the indoloquinolines and spiro[2H-indole-2,30-oxindole].

    Digital Repository Service at National Institute of Oceanography (India)

    Parvatkar, P.T.; Majik, M.S.

    ., vol.4; 2014; 22481-22486 Microwave-assisted reductive cyclization: An easy entry to the indoloquinolines and spiro[2H-indole-2,3’-oxindole] Prakash T. Parvatkar* and Mahesh S. Majik Bio-organic Chemistry Laboratory, CSIR-National Institute... of this cyclization step under MW assisted condition delivered similar results indicating the reproducibility of this methodology. In case of entry 4 (Table 1), low yields of the two products (19 and 15) and no formation of compound 20 may be due to the temperature...

  1. Microwave-assisted convenient syntheses of 2-indolizine derivatives from Morita-Baylis-Hillman adducts: new in silico potential ion channel modulators

    Energy Technology Data Exchange (ETDEWEB)

    Cunha, Saraghina M.D.; Oliveira, Ramon G. de; Vasconcellos, Mario L.A.A., E-mail: mlaav@quimica.ufpb.br [Universidade Federal da Paraiba (UFPB), Joao Pessoa, PB (Brazil). Departamento de Quimica

    2013-03-15

    In this work, a microwave-assisted synthesis study by microwave irradiation to produce indolizine-2-carbonitrile and indolizine-2-carboxylate in good to high yields (70 and 81%, respectively) in one step from Morita-Baylis-Hillman adducts (MBHA) is presented. These compounds were subsequently transformed to high yields (94 to 100%, respectively) in three 2-indolizine derivatives. The five synthesized compounds were designed in silico aiming to present potential selective activities as ion channel modulators. These activities were suggested by the score values using Molinspiration Cheminformatics program. (author)

  2. Determination of triazine and chloroacetanilide herbicides in soils by microwave-assisted extraction (MAE) coupled to gas chromatographic analysis with either GC-NPD or GC-MS.

    Science.gov (United States)

    Vryzas, Zisis; Papadopoulou-Mourkidou, Euphemia

    2002-08-28

    A simple and rapid method based on microwave-assisted extraction (MAE) coupled to gas chromatographic analysis was developed for the analysis of triazine (atrazine, cyanazine, metribuzine, simazine and deethylatrazine, and deisopropylatrazine) and chloroacetanilide (acetochlor, alachlor, and metolachlor) herbicide residues in soils. Soil samples are processed by MAE for 5 min at 80 degrees C in the presence of acetonitrile (20 mL/sample). Mean recovery values of most solutes are >80% in the 10 to 500 microg/kg fortification range with respective RSDs (relative standard deviations) NPD) or a mass spectrometric detector (GC-MS).

  3. Microwave-assisted grafting polymerization modification of nylon 6 capillary-channeled polymer fibers for enhanced weak cation exchange protein separations

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Liuwei; Marcus, R. Kenneth, E-mail: marcusr@clemson.edu

    2017-02-15

    A weak cation exchange liquid chromatography stationary phase (nylon-COOH) was prepared by grafting polyacrylic acid on to native nylon 6 capillary-channeled polymer (C-CP) fibers via a microwave-assisted radical polymerization. To the best of our knowledge, this is the first study of applying microwave-assisted grafting polymerization to affect nylon material for protein separation. The C-CP fiber surfaces were characterized by attenuated total reflection (ATR) infrared spectroscopy and scanning electron microscope (SEM). The anticipated carbonyl peak at 1722.9 cm{sup −1} was found on the nylon-COOH fibers, but was not found on the native fiber, indicating the presence of the polyacrylic acid on nylon fibers after grafting. The nylon-COOH phase showed a ∼12× increase in lysozyme dynamic binding capacity (∼12 mg mL{sup −1}) when compared to the native fiber phase (∼1 mg mL{sup −1}). The loading capacity of the nylon-COOH phase is nearly independent of the lysozyme loading concentration (0.05–1 mg mL{sup −1}) and the mobile phase linear velocity (7.3–73 mm s{sup −1}). The reproducibility of the lysozyme recovery from the nylon-COOH (RSD = 0.3%, n = 10) and the batch-to-batch variability in the functionalization (RSD = 3%, n = 5) were also investigated, revealing very high levels of consistency. Fast baseline separations of myoglobin, α-chymotrypsinogen A, cytochrome c and lysozyme were achieved using the nylon-COOH column. It was found that a 5× increase in the mobile phase linear velocity (7.3-to-36.5 mm s{sup −1}) had little effect on the separation resolution. The microwave-assisted grafting polymerization has great potential as a generalized surface modification methodology across the applications of C-CP fibers. - Highlights: • A microwave-assisted grafting method to attach acrylic acid is described for the first time for chromatographic phases. • A high-density, weak cation exchange surface is created on a nylon

  4. Microwave assisted chemistry: A rapid and regioselective route for direct ortho-acylation of phenols and naphthols by methanesulfonic acid as catalyst

    Directory of Open Access Journals (Sweden)

    Hossein Naeimi

    2017-05-01

    Full Text Available Direct ortho-acylation of phenols and naphthols with methanesulfonic acid (MSA as the catalyst has been studied under microwave stimulation. The microwave assisted reaction was environmentally benign in terms of faster reaction, useful conditions and higher yield of the desired products. However, after 3–4 min reaction time at 200–300 Watt, selectivity to over 98% ortho-acylation products was obtained. These reactions have some advantages in competition with other methods such as; short reaction times, high yield and regioselectivity of products, mild reaction conditions and easy workup of the reactions.

  5. One-Pot Approach to N-Quinolyl 3'/4'-Biaryl Carboxamides by Microwave-Assisted Suzuki-Miyaura Coupling and N-Boc Deprotection.

    Science.gov (United States)

    Huang, Zhi-You; Yang, Jing-Fang; Song, Ke; Chen, Qian; Zhou, Shao-Lin; Hao, Ge-Fei; Yang, Guang-Fu

    2016-10-21

    N-Quinolyl biaryl carboxamides have received tremendous attention for their notable biological properties. Here we have described a general protocol for the preparation of N-quinolyl 3'/4'-biaryl carboxamides by microwave-assisted Suzuki-Miyaura cross-coupling reaction and N-Boc deprotection in one pot. This method, which did not require acids, was used to produce a series of N-quinolyl 3'/4'-biaryl carboxamides with excellent functional group tolerance and high yields (70% to 95%).

  6. Microwave-assisted activated carbon from cocoa shell as adsorbent for removal of sodium diclofenac and nimesulide from aqueous effluents

    Energy Technology Data Exchange (ETDEWEB)

    Saucier, Caroline [Institute of Chemistry, Federal University of Rio Grande do Sul (UFRGS), Av. Bento Gonçalves 9500, P.O. Box 15003, 91501-970 Porto Alegre, RS (Brazil); Adebayo, Matthew A. [Department of Chemical Sciences, Ajayi Crowther University, Oyo, Oyo State (Nigeria); Lima, Eder C., E-mail: eder.lima@ufrgs.br [Institute of Chemistry, Federal University of Rio Grande do Sul (UFRGS), Av. Bento Gonçalves 9500, P.O. Box 15003, 91501-970 Porto Alegre, RS (Brazil); Cataluña, Renato [Institute of Chemistry, Federal University of Rio Grande do Sul (UFRGS), Av. Bento Gonçalves 9500, P.O. Box 15003, 91501-970 Porto Alegre, RS (Brazil); Thue, Pascal S. [Institute of Chemistry, Federal University of Rio Grande do Sul (UFRGS), Av. Bento Gonçalves 9500, P.O. Box 15003, 91501-970 Porto Alegre, RS (Brazil); Department of Applied Chemistry, University of Ngaoundere, P.O. Box 455, Ngaoundere (Cameroon); Prola, Lizie D.T.; Puchana-Rosero, M.J. [Institute of Chemistry, Federal University of Rio Grande do Sul (UFRGS), Av. Bento Gonçalves 9500, P.O. Box 15003, 91501-970 Porto Alegre, RS (Brazil); Machado, Fernando M. [Technology Development Center, Federal University of Pelotas (UFPEL), Pelotas (Brazil); Pavan, Flavio A. [Institute of Chemistry, Federal University of Pampa (UNIPAMPA), Bagé, RS (Brazil); Dotto, G.L. [Chemical Engineering Department, Federal University of Santa Maria (UFSM), Santa Maria, RS (Brazil)

    2015-05-30

    Highlights: • Microwave-assisted cocoa shell activated carbon was prepared and characterized. • The anti-inflammatories, diclofenac and nimesulide, were adsorbed onto MWCS-1.0. • Adsorption maximum values are 63.47 (diclofenac) and 74.81 mg g{sup −1} (nimesulide). • General order kinetic model suitably explained the adsorption process. • MWCS-1.0 was effectively used for treatment of simulated hospital effluents. - Abstract: Microwave-induced chemical activation process was used to prepare an activated carbon from cocoa shell for efficient removal of two anti-inflammatories, sodium diclofenac (DFC) and nimesulide (NM), from aqueous solutions. A paste was obtained from a mixture of cocoa shell and inorganic components; with a ratio of inorganic: organic of 1 (CSC-1.0). The mixture was pyrolyzed in a microwave oven in less than 10 min. The CSC-1.0 was acidified with a 6 mol L{sup −1} HCl under reflux to produce MWCS-1.0. The CSC-1.0 and MWCS-1.0 were characterized using FTIR, SEM, N{sub 2} adsorption/desorption curves, X-ray diffraction, and point of zero charge (pH{sub pzc}). Experimental variables such as initial pH of the adsorbate solutions and contact time were optimized for adsorptive characteristics of MWCS-1.0. The optimum pH for removal of anti-inflammatories ranged between 7.0 and 8.0. The kinetic of adsorption was investigated using general order, pseudo first-order and pseu do-second order kinetic models. The maximum amounts of DCF and NM adsorbed onto MWCS-1.0 at 25 °C are 63.47 and 74.81 mg g{sup −1}, respectively. The adsorbent was tested on two simulated hospital effluents. MWCS-1.0 is capable of efficient removal of DCF and NM from a medium that contains high sugar and salt concentrations.

  7. Effect of Inductive Coil Geometry on the Thrust Efficiency of a Microwave Assisted Discharge Inductive Plasma Accelerator

    Science.gov (United States)

    Hallock, Ashley; Polzin, Kurt; Emsellem, Gregory

    2012-01-01

    Pulsed inductive plasma thrusters [1-3] are spacecraft propulsion devices in which electrical energy is capacitively stored and then discharged through an inductive coil. The 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 Discharge Inductive Plasma Accelerator (MAD-IPA) [4, 5] is a pulsed inductive plasma thruster that addressees this issue by partially ionizing propellant inside a conical inductive coil via an electron cyclotron resonance (ECR) discharge. The ECR plasma is produced using microwaves and permanent magnets that are 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 inductive coil is high. The use of a conical theta-pinch coil is under investigation. The conical geometry 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) [2, 3], however a conical coil imparts a direct radial acceleration of the current sheet that serves to rapidly decouple the propellant from the coil, limiting the direct axial electromagnetic acceleration in favor of an indirect acceleration mechanism that requires significant heating of the propellant within the volume bounded by the current sheet. In this paper, we describe thrust stand measurements performed to characterize the performance

  8. SHORT COMMUNICATION MICROWAVE ASSISTED ...

    African Journals Online (AJOL)

    a

    1Department of Chemistry, Government V. Y. T. P. G. Autonomous College, Durg – 491001,. (Chhattisgarh), India. 2School of Studies in Chemistry, Pt. Ravishankar Shukla University, Raipur-492010. (Chhattisgarh), India ... The optimum conditions and other analytical parameters were evaluated. The effect of interfering.

  9. 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...

  10. Determination of cobalt species in nutritional supplements using ICP-OES after microwave-assisted extraction and solid-phase extraction.

    Science.gov (United States)

    Bartosiak, Magdalena; Jankowski, Krzysztof; Giersz, Jacek

    2018-03-31

    Cobalt content (as vitamin B 12 and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and compared. Microwave-assisted acid digestion efficiently decomposed all cobalt-containing compounds, thus allowed obtaining total cobalt content in supplements examined. Vitamin B 12 was extracted from the samples with acetate buffer and potassium cyanide solution exposed to mild microwave radiation for 30 min, and cyanocobalamin was separated from the extract by on-column solid phase extraction using C-18 modified silica bed. About 100% of cobalt species was extracted using the triple microwave-assisted extraction procedure. Total cobalt content was 20-fold greater in Spirulina tablets than the declared cobalamin content (as Co). The ICP-OES method precision was about 3% and detection limit was 1.9 and 2.7 ng Co mL -1 for inorganic cobalt or cyanocobalamin, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2016-03-01

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

  12. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pena, M.T.; Pensado, Luis; Casais, M.C.; Mejuto, M.C.; Cela, Rafael [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia. Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2007-04-15

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 {mu}g kg{sup -1} dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. (orig.)

  13. imFASP: An integrated approach combining in-situ filter-aided sample pretreatment with microwave-assisted protein digestion for fast and efficient proteome sample preparation.

    Science.gov (United States)

    Zhao, Qun; Fang, Fei; Wu, Ci; Wu, Qi; Liang, Yu; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

    2016-03-17

    An integrated sample preparation method, termed "imFASP", which combined in-situ filter-aided sample pretreatment and microwave-assisted trypsin digestion, was developed for preparation of microgram and even nanogram amounts of complex protein samples with high efficiency in 1 h. For imFASP method, proteins dissolved in 8 M urea were loaded onto a filter device with molecular weight cut off (MWCO) as 10 kDa, followed by in-situ protein preconcentration, denaturation, reduction, alkylation, and microwave-assisted tryptic digestion. Compared with traditional in-solution sample preparation method, imFASP method generated more protein and peptide identifications (IDs) from preparation of 45 μg Escherichia coli protein sample due to the higher efficiency, and the sample preparation throughput was significantly improved by 14 times (1 h vs. 15 h). More importantly, when the starting amounts of E. coli cell lysate decreased to nanogram level (50-500 ng), the protein and peptide identified by imFASP method were improved at least 30% and 44%, compared with traditional in-solution preparation method, suggesting dramatically higher peptide recovery of imFASP method for trace amounts of complex proteome samples. All these results demonstrate that the imFASP method developed here is of high potential for high efficient and high throughput preparation of trace amounts of complex proteome samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

    Science.gov (United States)

    Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

    2018-01-01

    This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

  15. Microwave-assisted in situ synthesis of reduced graphene oxide-BiVO{sub 4} composite photocatalysts and their enhanced photocatalytic performance for the degradation of ciprofloxacin

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Yan [School of Chemistry and Chemical Engineering, Jiangsu University, Xuefu Road 301, Zhenjiang, 212013 (China); Sun, Shaofang [School of Chemistry and Chemical Engineering, Jiangsu University, Xuefu Road 301, Zhenjiang, 212013 (China); School of Environmental Science and Engineering, Chang’an University, Yanta Road 126, Xi’an, 710054 (China); Song, Yang; Yan, Xu [School of Chemistry and Chemical Engineering, Jiangsu University, Xuefu Road 301, Zhenjiang, 212013 (China); Guan, Weisheng [School of Environmental Science and Engineering, Chang’an University, Yanta Road 126, Xi’an, 710054 (China); Liu, Xinlin [School of Material Science and Engineering, Jiangsu University, Xuefu Road 301, Zhenjiang, 212013 (China); Shi, Weidong, E-mail: swd1978@ujs.edu.cn [School of Chemistry and Chemical Engineering, Jiangsu University, Xuefu Road 301, Zhenjiang, 212013 (China)

    2013-04-15

    Highlights: ► Microwave-assisted in situ growth of RGO-BiVO{sub 4} composite was proposed. ► A relatively small particle size with organic-additives free. ► Graphene was formed during the microwave-heating by oxygen capture. ► GB-2 sample exhibits the highest CIP degradation ratio (3 times over pure BiVO{sub 4}). ► The enhancements of activities result from the effective charge separation. -- Abstract: To improve the photodegradation efficiency for ciprofloxacin (CIP), a new-type microwave-assisted in situ growth method is developed for the preparation of reduced graphene oxide (RGO) -BiVO{sub 4} composite photocatalysts. The as-produced RGO-BiVO{sub 4} composite photocatalysts show extremely high enhancement of CIP degradation ratio over the pure BiVO{sub 4} photocatalyst under visible light. Specially, the 2 wt% RGO-BiVO{sub 4} composite photocatalyst exhibits the highest CIP degradation ratio (68.2%) in 60 min, which is over 3 times than that (22.7%) of the pure BiVO{sub 4} particles. The enhancement of photocatalytic activities of RGO-BiVO{sub 4} photocatalysts can be attributed to the effective separation of electron–hole pairs rather than the improvement of light absorption.

  16. Microwave-assisted extraction and rapid isolation of ursolic acid from the leaves of Eucalyptus × hybrida Maiden and its quantification using HPLC-diode array technique.

    Science.gov (United States)

    Verma, Subash C; Jain, Chhoten L; Kumari, Amita; Padhi, Madan M; Devalla, Ramesh B

    2013-04-01

    Ursolic acid (UA) is the most important bioactive phytoconstituent of Eucalyptus × hybrida Maiden leaves and exhibits anticancer, antimutagenic, anti-inflammatory, antioxidative, and antiprotozoal activities. In this study, microwave-assisted extraction technique was employed for rapid isolation of UA from the leaves of Eucalyptus × hybrida and simultaneously HPLC-diode array method was developed for the quantification of UA. Effects of several experimental parameters on the extraction efficiencies of UA, such as type and volume of extraction solvents, microwave power and extraction time, were evaluated. The optimal extraction conditions were found to be 20 mL of a mixture of chloroform/methanol, 60:40; liquid-to-material ratio, 4:1; preleaching time, 10 min; microwave power, 600 W; temperature, 50°C; and microwave irradiation time, 5 min. Under the optimum conditions, the yield of UA was found to be 1.95 ± 0.08% in the dry leaves of Eucalyptus × hybrida. The results showed that microwave-assisted extraction is a more rapid extraction method with higher yield and lower solvent consumptions than the conventional method. It is a faster, convenient, and appropriate method and it may be used for rapid isolation and quantification of UA and other important phytoconstituents present in the leaves of Eucalyptus × hybrida. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Facile and efficient one-pot solvothermal and microwave-assisted synthesis of stable colloidal solutions of MFe{sub 2}O{sub 4} spinel magnetic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Solano, Eduardo; Perez-Mirabet, Leonardo [Universitat Autonoma de Barcelona, Departament de Quimica (Spain); Martinez-Julian, Fernando; Guzman, Roger; Arbiol, Jordi; Puig, Teresa; Obradors, Xavier [Institut de Ciencia de Materials de Barcelona, ICMAB-CSIC (Spain); Yanez, Ramon [Universitat Autonoma de Barcelona, Departament de Quimica (Spain); Pomar, Alberto; Ricart, Susagna, E-mail: ricart@icmab.es [Institut de Ciencia de Materials de Barcelona, ICMAB-CSIC (Spain); Ros, Josep [Universitat Autonoma de Barcelona, Departament de Quimica (Spain)

    2012-08-15

    Well-defined synthesis conditions of high quality MFe{sub 2}O{sub 4} (M = Mn, Fe, Co, Ni, Zn, and Cu) spinel ferrite magnetic nanoparticles, with diameters below 10 nm, have been described based on facile and efficient one-pot solvothermal or microwave-assisted heating procedures. Both methods are reproducible and scalable and allow forming concentrated stable colloidal solutions in polar solvents, but microwave-assisted heating allows reducing 15 times the required annealing time and leads to an enhanced monodispersity of the nanoparticles. Non-agglomerated nanoparticles dispersions have been achieved using a simple one-pot approach where a single compound, triethyleneglycol, behaves at the same time as solvent and capping ligand. A narrow nanoparticle size distribution and high quality crystallinity have been achieved through selected nucleation and growth conditions. High resolution transmission electron microscopy images and electron energy loss spectroscopy analysis confirm the expected structure and composition and show that similar crystal faceting has been formed in both synthetic approaches. The spinel nanoparticles behave as ferrimagnets with a high saturation magnetization and are superparamagnetic at room temperature. The influence of synthesis route on phase purity and unconventional magnetic properties is discussed in some particular cases such as CuFe{sub 2}O{sub 4}, CoFe{sub 2}O{sub 4}, and ZnFe{sub 2}O{sub 4}.

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

    Science.gov (United States)

    Ng, Lay-Keow; Hupé, Michel

    2003-09-05

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

  19. Optimizing the conditions for the microwave-assisted direct liquefaction of Ulva prolifera for bio-oil production using response surface methodology

    International Nuclear Information System (INIS)

    Liu, Junhai; Zhuang, Yingbin; Li, Yan; Chen, Limei; Guo, Jingxue; Li, Demao; Ye, Naihao

    2013-01-01

    Microwave-assisted direct liquefaction (MADL) of Ulva prolifera was performed in ethylene glycol (EG) using sulfuric acid (H 2 SO 4 ) as a catalyst. Response Surface Methodology (RSM) based on central composite rotatable design (CCRD) was employed to optimize the conditions of three independent variables (catalyst content, solvent-to-feedstock ratio and temperature) for the liquefaction yield. And the bio-oil was analyzed by elementary analysis, Fourier transform infrared spectroscopic analysis (FT-IR) and gas chromatography–mass spectrometry (GC–MS). The maximum liquefaction yield was 93.17%, which was obtained under a microwave power of 600 W for 30 min at 165 °C with a solvent-to-feedstock ratio of 18.87:1 and 4.93% sulfuric acid. The bio-oil was mainly composed of phthalic acid esters, alkenes and a fatty acid methyl ester with a long chain from C 16 to C 20 . - Highlights: • Ulva prolifera was converted to bio-oil through microwave-assisted direct liquefaction. • Response surface methodology was used to optimize the liquefaction technology. • A maximum liquefaction rate of 93.17 wt% bio-oil was obtained. • The bio-oil was composed of carboxylic acids and esters

  20. Synthesis of BiFeO3 thin films on single-terminated Nb : SrTiO3 (111 substrates by intermittent microwave assisted hydrothermal method

    Directory of Open Access Journals (Sweden)

    Ivan Velasco-Davalos

    2016-06-01

    Full Text Available We report on a simple and fast procedure to create arrays of atomically flat terraces on single crystal SrTiO3 (111 substrates and the deposition of ferroelectric BiFeO3 thin films on such single-terminated surfaces. A microwave-assisted hydrothermal method in deionized water and ammonia solution selectively removes either (SrO34− or Ti4+ layers to ensure the same chemical termination on all terraces. Measured step heights of 0.225 nm (d111 and uniform contrast in the phase image of the terraces confirm the single termination in pure and Nb doped SrTiO3 single crystal substrates. Multiferroic BiFeO3 thin films were then deposited by the same microwave assisted hydrothermal process on Nb : SrTiO3 (111 substrates. Bi(NO33 and Fe(NO33 along with KOH served as the precursors solution. Ferroelectric behavior of the BiFeO3 films on Nb : SrTiO3 (100 substrates was verified by piezoresponse force microscopy.