SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

Science.gov (United States)

A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

Directory of Open Access Journals (Sweden)

Mª Esther Torres Padrón

2014-07-01

Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

Wall modified photonic crystal fibre capillaries as porous layer open tubular columns for in-capillary micro-extraction and capillary chromatography

International Nuclear Information System (INIS)

Kazarian, Artaches A.; Sanz Rodriguez, Estrella; Deverell, Jeremy A.; McCord, James; Muddiman, David C.; Paull, Brett

2016-01-01

Wall modified photonic crystal fibre capillary columns for in-capillary micro-extraction and liquid chromatographic separations is presented. Columns contained 126 internal parallel 4 μm channels, each containing a wall bonded porous monolithic type polystyrene-divinylbenzene layer in open tubular column format (PLOT). Modification longitudinal homogeneity was monitored using scanning contactless conductivity detection and scanning electron microscopy. The multichannel open tubular capillary column showed channel diameter and polymer layer consistency of 4.2 ± 0.1 μm and 0.26 ± 0.02 μm respectively, and modification of 100% of the parallel channels with the monolithic polymer. The modified multi-channel capillaries were applied to the in-capillary micro-extraction of water samples. 500 μL of water samples containing single μg L"−"1 levels of polyaromatic hydrocarbons were extracted at a flow rate of 10 μL min"−"1, and eluted in 50 μL of acetonitrile for analysis using HPLC with fluorescence detection. HPLC LODs were 0.08, 0.02 and 0.05 μg L"−"1 for acenaphthene, anthracene and pyrene, respectively, with extraction recoveries of between 77 and 103%. The modified capillaries were also investigated briefly for direct application to liquid chromatographic separations, with the retention and elution of a standard protein (cytochrome c) under isocratic conditions demonstrated, proving chromatographic potential of the new column format, with run-to-run retention time reproducibility of below 1%. - Highlights: • Novel PS-DVB modified photonic crystal fibres for in-capillary micro-extraction. • New method for micro-extraction of PAHs and HPLC-FL detection at sub-ppb levels. • Demonstration of PS-DVB modified photonic crystal fibres for capillary bioseparations.

Wall modified photonic crystal fibre capillaries as porous layer open tubular columns for in-capillary micro-extraction and capillary chromatography

Energy Technology Data Exchange (ETDEWEB)

Kazarian, Artaches A. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); W.M. Keck FT-ICR-MS Laboratory, Department of Chemistry, North Carolina State University, Raleigh, NC (United States); Sanz Rodriguez, Estrella; Deverell, Jeremy A. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); McCord, James; Muddiman, David C. [W.M. Keck FT-ICR-MS Laboratory, Department of Chemistry, North Carolina State University, Raleigh, NC (United States); Paull, Brett, E-mail: Brett.Paull@utas.edu.au [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); ARC Centre of Excellence for Electromaterials Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia)

2016-01-28

Wall modified photonic crystal fibre capillary columns for in-capillary micro-extraction and liquid chromatographic separations is presented. Columns contained 126 internal parallel 4 μm channels, each containing a wall bonded porous monolithic type polystyrene-divinylbenzene layer in open tubular column format (PLOT). Modification longitudinal homogeneity was monitored using scanning contactless conductivity detection and scanning electron microscopy. The multichannel open tubular capillary column showed channel diameter and polymer layer consistency of 4.2 ± 0.1 μm and 0.26 ± 0.02 μm respectively, and modification of 100% of the parallel channels with the monolithic polymer. The modified multi-channel capillaries were applied to the in-capillary micro-extraction of water samples. 500 μL of water samples containing single μg L{sup −1} levels of polyaromatic hydrocarbons were extracted at a flow rate of 10 μL min{sup −1}, and eluted in 50 μL of acetonitrile for analysis using HPLC with fluorescence detection. HPLC LODs were 0.08, 0.02 and 0.05 μg L{sup −1} for acenaphthene, anthracene and pyrene, respectively, with extraction recoveries of between 77 and 103%. The modified capillaries were also investigated briefly for direct application to liquid chromatographic separations, with the retention and elution of a standard protein (cytochrome c) under isocratic conditions demonstrated, proving chromatographic potential of the new column format, with run-to-run retention time reproducibility of below 1%. - Highlights: • Novel PS-DVB modified photonic crystal fibres for in-capillary micro-extraction. • New method for micro-extraction of PAHs and HPLC-FL detection at sub-ppb levels. • Demonstration of PS-DVB modified photonic crystal fibres for capillary bioseparations.

Evaluation of Carbon Nanotubes Functionalized Polydimethylsiloxane Based Coatings for In-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

OpenAIRE

Neus Jornet-Martínez; Pascual Serra-Mora; Yolanda Moliner-Martínez; Rosa Herráez-Hernández; Pilar Campíns-Falcó

2015-01-01

In the present work, the performance of carbon nanotubes (c-CNTs) functionalized polydimethylsiloxane (PDMS) based coatings as extractive phases for in-tube solid phase microextraction (IT-SPME) coupled to Capillary LC (CapLC) has been evaluated. Carboxylic-single walled carbon nanotubes (c-SWNTs) and carboxylic-multi walled carbon nanotubes (c-MWNTs) have been immobilized on the activated surface of PDMS capillary columns. The effect of different percentages of diphenyl groups in the PDMS ex...

Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

Science.gov (United States)

Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

2016-07-01

Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

2016-11-01

A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent Microextraction Techniques for Determination and Chemical Speciation of Selenium

Directory of Open Access Journals (Sweden)

Ibrahim Ahmed S. A.

2017-05-01

Full Text Available Research designed to improve extraction has led to the development of microextraction techniques (ME, which involve simple, low cost, and effective preconcentrationof analytes in various matrices. This review is concerned with the principles and theoretical background of ME, as well as the development of applications for selenium analysis during the period from 2008 to 2016. Among all ME, dispersive liquid-liquid microextraction was found to be most favorable for selenium. On the other hand, atomic absorption spectrometry was the most frequently used instrumentation. Selenium ME have rarely been coupled to spectrophotometry and X-ray spectrophotometry methods, and there is no published application of ME with electrochemical techniques. We strongly support the idea of using a double preconcentration process, which consists of microextraction prior to preconcentration, followed by selenium determination using cathodic stripping voltammetry (ME-CSV. More attention should focus on the development of accurate, precise, and green methods for selenium analysis.

III–Vs on Si for photonic applications—A monolithic approach

International Nuclear Information System (INIS)

Wang, Zhechao; Junesand, Carl; Metaferia, Wondwosen; Hu, Chen; Wosinski, Lech; Lourdudoss, Sebastian

2012-01-01

Highlights: ► Monolithic evanescently coupled silicon laser (MECSL) structure treated. ► Optical mode profiles and thermal resistivity of MECSL optimized by simulation. ► MECSL through epitaxial lateral overgrowth (ELOG) of InP on Si exemplified. ► Passive waveguide in MECSL also acts as the defect filtering mask in ELOG. ► Growth of dislocation free thin InP layer on Si by ELOG for MECSL demonstrated. - Abstract: Epitaxial lateral overgrowth (ELOG) technology is demonstrated as a viable technology to realize monolithic integration of III-Vs on silicon. As an alternative to wafer-to-wafer bonding and die-to-wafer bonding, ELOG provides an attractive platform for fabricating discrete and integrated components in high volume at low cost. A possible route for monolithic integration of III–Vs on silicon for silicon photonics is exemplified by the case of a monolithic evanescently coupled silicon laser (MECSL) by combining InP on Si/SiO 2 through ELOG. Passive waveguide in MECSL also acts as the defect filtering mask in ELOG. The structural design of a monolithic evanescently coupled silicon laser (MECSL) and its thermal resistivity are established through simulations. Material studies to realize the above laser through ELOG are undertaken by studying appropriate ELOG pattern designs to achieve InP on narrow regions of silicon. We show that defect-free InP can be obtained on SiO 2 as the first step which paves the way for realizing active photonic devices on Si/SiO 2 waveguides, e.g. an MECSL.

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

Science.gov (United States)

Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

2017-08-29

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

III-Vs on Si for photonic applications-A monolithic approach

Energy Technology Data Exchange (ETDEWEB)

Wang, Zhechao, E-mail: Zhechao.Wang@intec.ugent.be [School of ICT, Royal Institute of Technology, Electrum 229, Isafjordsgatan 22, 164 40 Kista (Sweden); Junesand, Carl; Metaferia, Wondwosen; Hu, Chen; Wosinski, Lech [School of ICT, Royal Institute of Technology, Electrum 229, Isafjordsgatan 22, 164 40 Kista (Sweden); Lourdudoss, Sebastian, E-mail: slo@kth.se [School of ICT, Royal Institute of Technology, Electrum 229, Isafjordsgatan 22, 164 40 Kista (Sweden)

2012-10-01

Highlights: Black-Right-Pointing-Pointer Monolithic evanescently coupled silicon laser (MECSL) structure treated. Black-Right-Pointing-Pointer Optical mode profiles and thermal resistivity of MECSL optimized by simulation. Black-Right-Pointing-Pointer MECSL through epitaxial lateral overgrowth (ELOG) of InP on Si exemplified. Black-Right-Pointing-Pointer Passive waveguide in MECSL also acts as the defect filtering mask in ELOG. Black-Right-Pointing-Pointer Growth of dislocation free thin InP layer on Si by ELOG for MECSL demonstrated. - Abstract: Epitaxial lateral overgrowth (ELOG) technology is demonstrated as a viable technology to realize monolithic integration of III-Vs on silicon. As an alternative to wafer-to-wafer bonding and die-to-wafer bonding, ELOG provides an attractive platform for fabricating discrete and integrated components in high volume at low cost. A possible route for monolithic integration of III-Vs on silicon for silicon photonics is exemplified by the case of a monolithic evanescently coupled silicon laser (MECSL) by combining InP on Si/SiO{sub 2} through ELOG. Passive waveguide in MECSL also acts as the defect filtering mask in ELOG. The structural design of a monolithic evanescently coupled silicon laser (MECSL) and its thermal resistivity are established through simulations. Material studies to realize the above laser through ELOG are undertaken by studying appropriate ELOG pattern designs to achieve InP on narrow regions of silicon. We show that defect-free InP can be obtained on SiO{sub 2} as the first step which paves the way for realizing active photonic devices on Si/SiO{sub 2} waveguides, e.g. an MECSL.

Determination of trace triazine and chloroacetamide herbicides in tile-fed drainage ditch water using solid-phase microextraction coupled with GC-MS

Energy Technology Data Exchange (ETDEWEB)

Rocha, Cleonice [Catholic University of Goias, Av. Universitaria, 1440 S. Universitario, Cx (Brazil); Pappas, Elizabeth A. [USDA ARS, National Soil Erosion Research Laboratory, 275 S. Russell Street, West Lafayette, IN 47907 (United States)], E-mail: bets@purdue.edu; Huang, C.-H. [USDA ARS, National Soil Erosion Research Laboratory, 275 S. Russell Street, West Lafayette, IN 47907 (United States)

2008-03-15

Solid-phase microextraction coupled with gas chromatography-mass spectrometry (SPME-GC-MS) was used to analyze two triazine (atrazine and simazine) and three chloroacetamide herbicides (acetochlor, alachlor, and metolachlor) in water samples from a midwest US agricultural drainage ditch for two growing seasons. The effects of salt concentration, sample volume, extraction time, and injection time on extraction efficiency using a 100-{mu}m polydimethylsiloxane-coated fiber were investigated. By optimizing these parameters, ditch water detection limits of 0.5 {mu}g L{sup -1} simazine and 0.25 {mu}g L{sup -1} atrazine, acetochlor, alachlor, and metolachlor were achieved. The optimum salt concentration was found to be 83% NaCl, while sample volume (10 or 20 mL) negligibly affected analyte peak areas. The optimum extraction time was 40 min, and the optimum injection time was 15 min. Results indicated that atrazine levels in the ditch water exceeded the US maximum contaminant level for drinking water 12% of the time, and atrazine was the most frequently detected among studied analytes. - Solid-phase microextraction methods were successfully developed to quantify low levels of herbicides in tile-fed drain water by gas chromatography-mass spectrometry.

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction

International Nuclear Information System (INIS)

Chisvert, Alberto; Benedé, Juan L.; Anderson, Jared L.; Pierson, Stephen A.; Salvador, Amparo

2017-01-01

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67–791), limits of detection (low ng L −1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87–113%, 91–117% and 89–115% for river, sea and swimming pool water samples, respectively). - Highlights: • A new microextraction method combining the

Rapid determination of 18 glucocorticoids in serum using reusable on-line SPE polymeric monolithic column coupled with LC-quadrupole/orbitrap high-resolution mass spectrometer.

Science.gov (United States)

Li, Hui; Ai, Lianfeng; Fan, Sufang; Wang, Yan; Sun, Dianxing

2017-10-15

A simple, rapid and sensitive method for the simultaneous determination of 18 glucocorticoids in serum was developed by coupling on-line solid-phase extraction (SPE) polymeric monolithic column to a liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometer. A simple poly(ethylene glycol dimethacrylate) monolith column (10mm×2.1mm i.d.) was fabricated, and the morphology, surface area and extraction performance of the monolithic column were characterized. Serum samples were extracted by acetonitrile (ACN). Then, online SPE was achieved on the synthesized monolithic column using a 10mmol/L ammonium acetate solution as the loading solvent. After the transfer from the monolith into analytical column (Capcell Pak ADME column) using ACN, the adsorbed analytes were separated on the analytical column and detected with a high-resolution hybrid quadrupole/orbitrap mass spectrometer with full scan/ddMS 2 scan mode Under optimized conditions, the method was linear with target linear correlation coefficient (R 2 ) higher than 0.995. Detection limits were in range of 0.1-0.6ng/mL, and the quantification limits were 0.3-1.5ng/mL. The recovery was between 71.9% and 89.2% in three spike levels with precision (n=5) of 5.40-12.1%. The serum sample was directly analyzed after a simple extraction procedure, and the on-line SPE and determination were achieved within only 16min. The method was used to analyze the dynamic contents variation of cortisone and hydrocortisone in serum before and after the surgery. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

Science.gov (United States)

Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

2006-11-01

Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden.

Monoliths in Bioprocess Technology

Directory of Open Access Journals (Sweden)

Vignesh Rajamanickam

2015-04-01

Full Text Available Monolithic columns are a special type of chromatography column, which can be used for the purification of different biomolecules. They have become popular due to their high mass transfer properties and short purification times. Several articles have already discussed monolith manufacturing, as well as monolith characteristics. In contrast, this review focuses on the applied aspect of monoliths and discusses the most relevant biomolecules that can be successfully purified by them. We describe success stories for viruses, nucleic acids and proteins and compare them to conventional purification methods. Furthermore, the advantages of monolithic columns over particle-based resins, as well as the limitations of monoliths are discussed. With a compilation of commercially available monolithic columns, this review aims at serving as a ‘yellow pages’ for bioprocess engineers who face the challenge of purifying a certain biomolecule using monoliths.

Metal oxide nanorod arrays on monolithic substrates

Energy Technology Data Exchange (ETDEWEB)

Gao, Pu-Xian; Guo, Yanbing; Ren, Zheng

2018-01-02

A metal oxide nanorod array structure according to embodiments disclosed herein includes a monolithic substrate having a surface and multiple channels, an interface layer bonded to the surface of the substrate, and a metal oxide nanorod array coupled to the substrate surface via the interface layer. The metal oxide can include ceria, zinc oxide, tin oxide, alumina, zirconia, cobalt oxide, and gallium oxide. The substrate can include a glass substrate, a plastic substrate, a silicon substrate, a ceramic monolith, and a stainless steel monolith. The ceramic can include cordierite, alumina, tin oxide, and titania. The nanorod array structure can include a perovskite shell, such as a lanthanum-based transition metal oxide, or a metal oxide shell, such as ceria, zinc oxide, tin oxide, alumina, zirconia, cobalt oxide, and gallium oxide, or a coating of metal particles, such as platinum, gold, palladium, rhodium, and ruthenium, over each metal oxide nanorod. Structures can be bonded to the surface of a substrate and resist erosion if exposed to high velocity flow rates.

Determination of Lactones in Wines by Headspace Solid-Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry

Directory of Open Access Journals (Sweden)

S. J. Pérez-Olivero

2014-01-01

Full Text Available Application of headspace solid-phase microextraction (HS-SPME coupled with high-resolution gas chromatographic (HRGC analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of γ-butyrolactone, γ-hexalactone, trans-whiskey lactone, γ-octalactone, cis-whiskey lactone, γ-nonalactone, γ-decalactone, δ-decalactone, and γ-undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for γ-butyrolactone was 0.17 mg/L and a few μg/L for the rest of the compounds. The optimized method has been applied to several wine samples.

One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

Science.gov (United States)

Liang, Pei; Kang, Caiyan; Mo, Yajun

2016-01-01

A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous Pre-Concentration of Cadmium and Lead in Environmental Water Samples with Dispersive Liquid-Liquid Microextraction and Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

Directory of Open Access Journals (Sweden)

M. Salahinejad

2013-06-01

Full Text Available The dispersive liquid–liquid microextraction (DLLME method for determination of Pb+2 and Cd+2 ions in the environmental water samples was combined with inductively coupled plasma-atomic emission spectrometry (ICP-AES. Ammonium pyrrolidine dithiocarbamate (APDC, chloroform and ethanol were used as chelating agent, extraction solvent and disperser solvent, respectively. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters included extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH, sample volume and amount of the chelating agent.   Under the optimum conditions, the enrichment factor of 75 and 105 for Cd+2 and Pb+2 ions respectively was obtained from only 5.00mL of water sample. The detection limit (S/N=3 was 12 and 0.8ngmL−1 for Pb and Cd respectively. The relative standard deviation (RSDs for five replicate measurements of 0.50 mgL−1 of lead and cadmium was 6.5 and 4.4 % respectively. Mineral, tap, river, sea, dam and spiked water samples were analyzed for Cd and Pb amount.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

Science.gov (United States)

de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

Liquid phase microextraction for the analysis of trace elements and their speciation

International Nuclear Information System (INIS)

Hu, Bin; He, Man; Chen, Beibei; Xia, Linbo

2013-01-01

Trace/ultra-trace elements and their speciation analysis in complex matrices usually require sample preparation procedures to achieve sample clean-up and analyte preconcentration. Sample preparation is often the bottleneck in trace elements and their speciation analysis which has a direct impact on accuracy, precision and limits of detection and is often the rate-determining step of the analytical process. Recent trends in sample preparation include miniaturization, automation, high-throughput performance and reduction in solvent/sample consumption and operation time. Liquid-phase microextraction (LPME) technique as a novel and promising alternative in sample preparation can meet these requirements and has become a very efficient sample preparation technique. This review updates the state of art of LPME for trace elements and their speciation analysis and discusses its promising prospects. The major thrust of the article highlights the applications of LPME including single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME) and solidified floating organic drop microextraction (SFODME) to the fields of elemental and their speciation analysis by atomic spectrometry-based methods, especially inductively coupled plasma mass spectrometry. General and specific concepts, different extraction formats and characteristics of LPME are described and compared, along with examples of recent innovations and applications presented to demonstrate its potential for trace elements and their speciation analysis in biological and environmental fields. Moreover, the application potential and an outlook on the combination of LPME and atomic spectrometry-based techniques for inorganic analysis are commentated. - Highlights: • The state of art of LPME for trace elements and their speciation analysis is updated. • Different extraction formats of LPME are described. • The application potential and future

Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

2014-11-01

An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

Science.gov (United States)

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Headspace single-drop microextraction coupled to microvolume UV-vis spectrophotometry for iodine determination

International Nuclear Information System (INIS)

Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2009-01-01

Headspace single-drop microextraction has been combined with microvolume UV-vis spectrophotometry for iodine determination. Matrix separation and preconcentration of iodide following in situ volatile iodine generation and extraction into a microdrop of N,N'-dimethylformamide is performed. An exhaustive characterization of the microextraction system and the experimental variables affecting iodine generation from iodide was carried out. The procedure employed consisted of exposing 2.5 μL of N,N'-dimethylformamide to the headspace of a 10 mL acidic (H 2 SO 4 2 mol L -1 ) aqueous solution containing 1.7 mol L -1 Na 2 SO 4 for 7 min. Addition of 1 mL of H 2 O 2 1 mol L -1 for in situ iodine generation was performed. The limit of detection was determined as 0.69 μg L -1 . The repeatability, expressed as relative standard deviation, was 4.7% (n = 6). The calibration working range was from 5 to 200 μg L -1 (r 2 = 0.9991). The large preconcentration factor obtained, ca. 623 in only 7 min, compensate for the 10-fold loss in sensitivity caused by the decreased optical path, which results in improved detection limits as compared to spectrophotometric measurements carried out with conventional sample cells. The method was successfully applied to the determination of iodine in water, pharmaceutical and food samples

Non-conventional solvents in liquid phase microextraction and aqueous biphasic systems.

Science.gov (United States)

An, Jiwoo; Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L

2017-06-02

The development of rapid, convenient, and high throughput sample preparation approaches such as liquid phase microextraction techniques have been continuously developed over the last decade. More recently, significant attention has been given to the replacement of conventional organic solvents used in liquid phase microextraction techniques in order to reduce toxic waste and to improve selectivity and/or extraction efficiency. With these objectives, non-conventional solvents have been explored in liquid phase microextraction and aqueous biphasic systems. The utilized non-conventional solvents include ionic liquids, magnetic ionic liquids, and deep eutectic solvents. They have been widely used as extraction solvents or additives in various liquid phase microextraction modes including dispersive liquid-liquid microextraction, single-drop microextraction, hollow fiber-liquid phase microextraction, as well as in aqueous biphasic systems. This review provides an overview into the use of non-conventional solvents in these microextraction techniques in the past 5 years (2012-2016). Analytical applications of the techniques are also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

Monolithic pixels on moderate resistivity substrate and sparsifying readout architecture

CERN Document Server

Giubilato, P; Snoeys, W; Bisello, D; Marchioro, A; Battaglia, M; Demaria, L; Mansuy, S C; Pantano, D; Rousset, J; Mattiazzo, S; Kloukinas, K; Potenza, A; Ikemoto, Y; Rivetti, A; Chalmet, P; Mugnier, H; Silvestrin, L

2013-01-01

The LePix projects aim realizing a new generation monolithic pixel detectors with improved performances at lesser cost with respect to both current state of the art monolithic and hybrid pixel sensors. The detector is built in a 90 nm CMOS process on a substrate of moderate resistivity. This allows charge collection by drift while maintaining the other advantages usually offered by MAPS, like having a single piece detector and using a standard CMOS production line. The collection by drift mechanism, coupled to the low capacitance design of the collecting node made possible by the monolithic approach, provides an excellent signal to noise ratio straight at the pixel cell together with a radiation tolerance far superior to conventional un-depleted MAPS. The excellent signal-to-noise performance is demonstrated by the device ability to separate the 6 keV Fe-55 double peak at room temperature. To achieve high granularity (10-20 mu m pitch pixels) over large detector areas maintaining high readout speed, a complet...

Dual jaw treatment of edentulism using implant-supported monolithic zirconia fixed prostheses.

Science.gov (United States)

Altarawneh, Sandra; Limmer, Bryan; Reside, Glenn J; Cooper, Lyndon

2015-01-01

This case report describes restoration of the edentulous maxilla and mandible with implant supported fixed prostheses using monolithic zirconia, where the incisal edges and occluding surfaces were made of monolithic zirconia. Edentulism is a debilitating condition that can be treated with either a removable or fixed dental prosthesis. The most common type of implant-supported fixed prosthesis is the metal acrylic (hybrid), with ceramo-metal prostheses being used less commonly in complete edentulism. However, both of these prostheses designs are associated with reported complications of screw loosening or fracture and chipping of acrylic resin and porcelain. Monolithic zirconia implant-supported fixed prostheses have the potential for reduction of such complications. In this case, the CAD/CAM concept was utilized in fabrication of maxillary and mandibular screw-retained implant-supported fixed prostheses using monolithic zirconia. Proper treatment planning and execution coupled with utilizing advanced technologies contributes to highly esthetic results. However, long-term studies are required to guarantee a satisfactory long-term outcome of this modality of treatment. This case report describes the clinical and technical procedures involved in fabrication of maxillary and mandibular implant-supported fixed prostheses using monolithic zirconia as a treatment of edentulism, and proposes the possible advantages associated with using monolithic zirconia in eliminating dissimilar interfaces in such prostheses that are accountable for the most commonly occurring technical complication for these prostheses being chipping and fracture of the veneering material. © 2015 Wiley Periodicals, Inc.

On-line liquid phase micro-extraction based on drop-in-plug sequential injection lab-at-valve platform for metal determination

Energy Technology Data Exchange (ETDEWEB)

Mitani, Constantina [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece); Anthemidis, Aristidis N., E-mail: anthemid@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece)

2013-04-10

Highlights: ► Drop-in-plug micro-extraction based on SI-LAV platform for metal preconcentration. ► Automatic liquid phase micro-extraction coupled with FAAS. ► Organic solvents with density higher than water are used. ► Lead determination in environmental water and urine samples. -- Abstract: A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 μL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 μg L{sup −1} and the precision expressed as relative standard deviation (RSD) at 50.0 μg L{sup −1} of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples.

Deltamethrin Binding to Triatoma infestans (Hemiptera: Reduviidae) Lipoproteins. Analysis by Solvent Bar Microextraction Coupled to Gas Chromatography.

Science.gov (United States)

Dulbecco, A B; Mijailovsky, S J; Girotti, J R; Juárez, M P

2015-11-01

The binding of deltamethrin (DLM) to the hemipteran Triatoma infestans (Klug) hemolymph lipoproteins was evaluated in vitro. After DLM incubation with the insect hemolymph, lipoproteins were fractioned by ultracentrifugation. DLM binding was analyzed by a microextractive technique-solvent bar microextraction-a solventless methodology to extract DLM from each lipoprotein fraction. This is a novel use of the technique applied to extract an insecticide from an insect fluid. Capillary gas chromatography with microelectron capture detection was used to detect DLM bound by the T. infestans hemolymph lipoproteins and to identify the preferred DLM carrier. We show that Lp and VHDLp I lipoproteins are mainly responsible for DLM transport in T. infestans, both in DLM-resistant and DLM-susceptible bugs. Our results also indicate that DLM amounts transported are not related to DLM susceptibility. © The Authors 2015. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Dispersive liquid-liquid microextraction coupled with magnetic nanoparticles for extraction of zearalenone in wheat samples

Directory of Open Access Journals (Sweden)

Mitra Amoli-Diva

2017-01-01

Full Text Available A new, sensitive and fast dispersive liquid-liquid microextraction (DLLME coupled with micro-solid phase extraction (μ-SPE was developed for determination of zearalenone (ZEN in wheat samples. The DLLME was performed using acetonitrile/water (80:20 v/v as the disperser solvent and 1-octanol as the extracting solvent.  The acetonitrile/water (80:20 v/v solvent was also used to extract ZEN from solid wheat matrix, and was directly applied as the disperser solvent for DLLME process. Additionally, hydrophobic oleic-acid-modified magnetic nanoparticles were used in μ-SPE approach to retrieve the analyte from the DLLME step. So, the method uses high surface area and strong magnetism properties of these nanoparticles to avoid time-consuming column-passing processes in traditional SPE. Main parameters affecting the extraction efficiency and signal enhancement were investigated and optimized. Under the optimum conditions, the calibration curve showed a good linearity in the range of 0.1-500 μg kg−1 (R2=0.9996 with low detection limit of 83 ng g−1. The intra-day and inter-day precisions (as RSD % in the range of 2.6-4.3 % and high recoveries ranging from 91.6 to 99.1 % were obtained. The pre-concentration factor was 3. The method is simple, inexpensive, accurate and remarkably free from interference effects.

Determination of 17 kinds of banned organochlorine pesticides in water by activated carbon fiber-solid phase microextraction coupled with GC-MS.

Science.gov (United States)

Sun, Tonghua; Jia, Jinping; Zhong, Dengjie; Wang, Yalin

2006-02-01

Activated carbon fiber (ACF) as extraction fiber for solid-phase microextraction (SPME) and its application for the analysis of banned organochlorine pesticides (OCPs) were investigated. Firstly, ACF was activated by different concentration of zinc chloride, which indicated that ACF activated by 60% zinc chloride had a reasonable specific surface area, pore volume and pore distribution. Secondly, the parameters for the ACF-SPME procedure, the adsorption and desorption conditions, were also optimized when coupled with gas chromatography-mass spectrometry (GC-MS). Thirdly, the ACF-SPME was used to analyze 17 kinds of OCPs in water. The linearity of most pesticides was found to be between 0.2 and 50 microg/l with GC-MS under the selected ion monitoring (SIM) acquisition mode. The limits of detection (LOD) at the sub microg/l were obtained. The work demonstrated here shows that ACF is a promising alternative for the SPME procedure.

Seismic waves and earthquakes in a global monolithic model

Science.gov (United States)

Roubíček, Tomáš

2018-03-01

The philosophy that a single "monolithic" model can "asymptotically" replace and couple in a simple elegant way several specialized models relevant on various Earth layers is presented and, in special situations, also rigorously justified. In particular, global seismicity and tectonics is coupled to capture, e.g., (here by a simplified model) ruptures of lithospheric faults generating seismic waves which then propagate through the solid-like mantle and inner core both as shear (S) or pressure (P) waves, while S-waves are suppressed in the fluidic outer core and also in the oceans. The "monolithic-type" models have the capacity to describe all the mentioned features globally in a unified way together with corresponding interfacial conditions implicitly involved, only when scaling its parameters appropriately in different Earth's layers. Coupling of seismic waves with seismic sources due to tectonic events is thus an automatic side effect. The global ansatz is here based, rather for an illustration, only on a relatively simple Jeffreys' viscoelastic damageable material at small strains whose various scaling (limits) can lead to Boger's viscoelastic fluid or even to purely elastic (inviscid) fluid. Self-induced gravity field, Coriolis, centrifugal, and tidal forces are counted in our global model, as well. The rigorous mathematical analysis as far as the existence of solutions, convergence of the mentioned scalings, and energy conservation is briefly presented.

Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

Science.gov (United States)

Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

2017-01-20

A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Acylhydrazone bond dynamic covalent polymer gel monolithic column online coupling to high-performance liquid chromatography for analysis of sulfonamides and fluorescent whitening agents in food.

Science.gov (United States)

Zhang, Chengjiang; Luo, Xialin; Wei, Tianfu; Hu, Yufei; Li, Gongke; Zhang, Zhuomin

2017-10-13

A new dynamic covalent polymer (DCP) gel was well designed and constructed based on imine chemistry. Polycondensation of 4,4'-biphenyldicarboxaldehyde and 1,3,5-benzenetricarbohydrazide via Schiff-base reaction resulted in an acylhydrazone bond gel (AB-gel) DCP. AB-gel DCP had three-dimensional network of interconnected nanoparticles with hierarchically porous structure. AB-gel DCP was successfully fabricated as a monolithic column by an in-situ chemical bonding method for online enrichment and separation purpose with excellent permeability. AB-gel DCP based monolithic column showed remarkable adsorption affinity towards target analytes including sulfonamides (SAs) and fluorescent whitening agents (FWAs) due to its strong π-π affinity, hydrophobic effect and hydrogen bonding interaction. Then, AB-gel DCP based monolithic column was applied for online separation and analysis of trace SAs and FWAs in food samples coupled with high-performance liquid chromatography (HPLC). Sulfathiazole (ST) and sulfadimidine (SM2) in one positive weever sample were actually found and determined with concentrations of 273.8 and 286.3μg/kg, respectively. 2,5-Bis(5-tert-butyl-2-benzoxazolyl) thiophene (FWA184) was actually quantified in one tea infusion sample with the concentration of 268.5ng/L. The spiked experiments suggested the good recoveries in range of 74.5-110% for SAs in weever and shrimp samples with relative standard deviations (RSDs) less than 9.7% and in range of 74.0-113% for FWAs in milk and tea infusion samples with RSDs less than 9.0%. AB-gel DCP monolithic column was proved to be a promising sample preparation medium for online separation and analysis of trace analytes in food samples with complex matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

Role of the substrate in monolithic AlGaAs nonlinear nanoantennas

Directory of Open Access Journals (Sweden)

Gili Valerio Flavio

2017-06-01

Full Text Available We report the effect of the aluminum oxide substrate on the emission of monolithic AlGaAs-on-insulator nonlinear nanoantennas. By coupling nonlinear optical measurements with electron diffraction and microscopy observations, we find that the oxidation-induced stress causes negligible crystal deformation in the AlGaAs nanostructures and only plays a minor role in the polarization state of the harmonic field. This result highlights the reliability of the wet oxidation of thick AlGaAs optical substrates and further confirms the bulk χ(2 origin of second harmonic generation at 1.55 μm in these nanoantennas, paving the way for the development of AlGaAs-on-insulator monolithic metasurfaces.

Online micro-solid-phase extraction based on boronate affinity monolithic column coupled with high-performance liquid chromatography for the determination of monoamine neurotransmitters in human urine.

Science.gov (United States)

Yang, Xiaoting; Hu, Yufei; Li, Gongke

2014-05-16

Quantification of monoamine neurotransmitters is very important in diagnosing and monitoring of patients with neurological disorders. We developed an online analytical method to selectively determine urinary monoamine neurotransmitters, which coupled the boronate affinity monolithic column micro-solid-phase extraction with high-performance liquid chromatography (HPLC). The boronate affinity monolithic column was prepared by in situ polymerization of vinylphenylboronic acid (VPBA) and N,N'-methylenebisacrylamide (MBAA) in a stainless capillary column. The prepared monolithic column showed good permeability, high extraction selectivity and capacity. The column-to-column reproducibility was satisfactory and the enrichment factors were 17-243 for four monoamine neurotransmitters. Parameters that influence the online extraction efficiency, including pH of sample solution, flow rate of extraction and desorption, extraction volume and desorption volume were investigated. Under the optimized conditions, the developed method exhibited low limit of detection (0.06-0.80μg/L), good linearity (with R(2) between 0.9979 and 0.9993). The recoveries in urine samples were 81.0-105.5% for four monoamine neurotransmitters with intra- and inter-day RSDs of 2.1-8.2% and 3.7-10.6%, respectively. The online analytical method was sensitive, accurate, selective, reliable and applicable to analysis of trace monoamine neurotransmitters in human urine sample. Copyright © 2014 Elsevier B.V. All rights reserved.

Liquid phase microextraction of pesticides: a review on current methods

International Nuclear Information System (INIS)

Farajzadeh, Mir Ali; Sorouraddin, Saeed Mohammad; Mogaddam, Mohammad Reza Afshar

2014-01-01

Liquid phase microextraction (LPME) enables analytes to be extracted with a few microliters of an organic solvent. LPME is a technique for sample preparation that is extremely simple, affordable and virtually a solvent-free. It can provide a high degree of selectivity and enrichment by eliminating carry-over between single runs. A variety of solvents are known for the extraction of the various analytes. These features have led to the development of techniques such as single drop microextraction, hollow fiber LPME, dispersive liquid-liquid microextraction, and others. LPME techniques have been applied to the analysis of pharmaceuticals, food, beverages, and pesticides. This review covers the history of LPME methods, and then gives a comprehensive collection of their application to the preconcentration and determination of pesticides in various matrices. Specific sections cover (a) sample treatment techniques in general, (b) single-drop microextraction, (c) extraction based on the use of ionic liquids, (d) solidified floating organic drop microextraction, and various other techniques. (author)

Ultra-trace determination of gold nanoparticles in environmental water by surfactant assisted dispersive liquid liquid microextraction coupled with electrothermal vaporization-inductively coupled plasma-mass spectrometry

Science.gov (United States)

Liu, Ying; He, Man; Chen, Beibei; Hu, Bin

2016-08-01

A new method by coupling surfactant assisted dispersive liquid liquid microextraction (SA-DLLME) with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) was proposed for the analysis of gold nanoparticles (AuNPs) in environmental water samples. Effective separation of AuNPs from ionic gold species was achieved by using sodium thiosulphate as a complexing agent. Various experimental parameters affecting SA-DLLME of AuNPs, such as the organic solvent, organic solvent volume, pH of the sample, the kind of surfactant, surfactant concentration, vortex time, speed of centrifugation, centrifugation time, and different coating as well as sizes of AuNPs were investigated carefully. Furthermore, the interference of coexisting ions, dissolved organic matter (DOM) and other metal nanoparticles (NPs) were studied. Under the optimal conditions, a detection limit of 2.2 ng L- 1 and an enrichment factor of 152-fold was achieved for AuNPs, and the original morphology of the AuNPs could be maintained during the extraction process. The developed method was successfully applied for the analysis of AuNPs in environmental water samples, including tap water, the East Lake water, and the Yangtze River water, with recoveries in the range of 89.6-102%. Compared with the established methods for metal NPs analysis, the proposed method has the merits of simple and fast operation, low detection limit, high selectivity, good tolerance to the sample matrix and no digestion or dilution required. It provides an efficient quantification methodology for monitoring AuNPs' pollution in the environmental water and evaluating its toxicity.

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

Science.gov (United States)

Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

2016-02-01

Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Liquid-phase microextraction and fibre-optics-based cuvetteless CCD-array micro-spectrophotometry for trace analysis

International Nuclear Information System (INIS)

Sharma, Nisha; Pillai, Aradhana K.K.V.; Pathak, Neeraj; Jain, Archana; Verma, Krishna K.

2009-01-01

Liquid-phase microextraction (LPME) has been investigated for trace analysis in the present work in conjunction with fibre-optic-based micro-spectrophotometry which accommodates sample volume of 1 μL placed between the two ends of optical fibres. Methods have been evolved for the determination of (i) 1-100 μM and 0.5-20 μM of thiols by single drop microextraction (SDME) and LPME in 25 μL of the organic solvent, respectively, involving their reaction with the Ellman reagent and ion pair microextraction of thiolate ion formed; (ii) 70 μg to 7 mg L -1 of chlorine/chlorine dioxide by headspace in-drop reaction with alternative reagents, viz., mixed phenylhydrazine-4-sulphonic acid and N-(1-naphthyl)ethylenediamine dihydrochloride, o-dianisidine, o-tolidine, and N,N-diethyl-p-phenylenediamine; (iii) 0.2-4 mg L -1 of ammonia by reaction with 2,4-dinitro-1-fluorobenzene to give 2,4-dinitroaniline which was diazotized and coupled with 1-naphthylamine, the resulting dye was subjected to preconcentration by solid-phase extraction and LPME; and (iv) 25-750 μg L -1 of iodide/total iodine by oxidation of iodide by 2-iodosobenzoate, microextraction of iodine in organic solvent, and re-extraction into aqueous starch-iodide reagent drop held in the organic phase. LPME using 25-30 μL of organic solvent was found to produce more sensitive results than SDME. The cuvetteless spectrophotometry as used in combination with sample handling techniques produced limits of detection of analytes which were better than obtained by previously reported spectrophotometry.

Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

Science.gov (United States)

Yang, Liu; Han, Qiang; Cao, Shuya; Yang, Jie; Yang, Junchao; Ding, Mingyu

2014-01-01

On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples. PMID:25384006

Design of a Modular Monolithic Implicit Solver for Multi-Physics Applications

Science.gov (United States)

Carton De Wiart, Corentin; Diosady, Laslo T.; Garai, Anirban; Burgess, Nicholas; Blonigan, Patrick; Ekelschot, Dirk; Murman, Scott M.

2018-01-01

The design of a modular multi-physics high-order space-time finite-element framework is presented together with its extension to allow monolithic coupling of different physics. One of the main objectives of the framework is to perform efficient high- fidelity simulations of capsule/parachute systems. This problem requires simulating multiple physics including, but not limited to, the compressible Navier-Stokes equations, the dynamics of a moving body with mesh deformations and adaptation, the linear shell equations, non-re effective boundary conditions and wall modeling. The solver is based on high-order space-time - finite element methods. Continuous, discontinuous and C1-discontinuous Galerkin methods are implemented, allowing one to discretize various physical models. Tangent and adjoint sensitivity analysis are also targeted in order to conduct gradient-based optimization, error estimation, mesh adaptation, and flow control, adding another layer of complexity to the framework. The decisions made to tackle these challenges are presented. The discussion focuses first on the "single-physics" solver and later on its extension to the monolithic coupling of different physics. The implementation of different physics modules, relevant to the capsule/parachute system, are also presented. Finally, examples of coupled computations are presented, paving the way to the simulation of the full capsule/parachute system.

Fibrous monolithic ceramics

International Nuclear Information System (INIS)

Kovar, D.; King, B.H.; Trice, R.W.; Halloran, J.W.

1997-01-01

Fibrous monolithic ceramics are an example of a laminate in which a controlled, three-dimensional structure has been introduced on a submillimeter scale. This unique structure allows this all-ceramic material to fail in a nonbrittle manner. Materials have been fabricated and tested with a variety of architectures. The influence on mechanical properties at room temperature and at high temperature of the structure of the constituent phases and the architecture in which they are arranged are discussed. The elastic properties of these materials can be effectively predicted using existing models. These models also can be extended to predict the strength of fibrous monoliths with an arbitrary orientation and architecture. However, the mechanisms that govern the energy absorption capacity of fibrous monoliths are unique, and experimental results do not follow existing models. Energy dissipation occurs through two dominant mechanisms--delamination of the weak interphases and then frictional sliding after cracking occurs. The properties of the constituent phases that maximize energy absorption are discussed. In this article, the authors examine the structure of Si 3 N 4 -BN fibrous monoliths from the submillimeter scale of the crack-deflecting cell-cell boundary features to the nanometer scale of the BN cell boundaries

Comprehensive two-dimensional HPLC to study the interaction of multiple components in Rheum palmatum L. with HSA by coupling a silica-bonded HSA column to a silica monolithic ODS column.

Science.gov (United States)

Hu, Lianghai; Li, Xin; Feng, Shun; Kong, Liang; Su, Xingye; Chen, Xueguo; Qin, Feng; Ye, Mingliang; Zou, Hanfa

2006-04-01

A mode of comprehensive 2-D LC was developed by coupling a silica-bonded HSA column to a silica monolithic ODS column. This system combined the affinity property of the HSA column and the high-speed separation ability of the monolithic ODS column. The affinity chromatography with HSA-immobilized stationary phase was applied to study the interaction of multiple components in traditional Chinese medicines (TCMs) with HSA according to their affinity to protein in the first dimension. Then the unresolved components retained on the HSA column were further separated on the silica monolithic ODS column in the second dimension. By hyphenating the 2-D separation system to diode array detector and MS detectors, the UV and molecular weight information of the separated compounds can also be obtained. The developed separation system was applied to analysis of the extract of Rheum palmatum L., a number of low-abundant components can be separated on a single peak from the HSA column after normalization of peak heights. Six compounds were preliminarily identified according to their UV and MS spectra. It showed that this system was very useful for biological fingerprinting analysis of the components in TCMs and natural products.

Monolithic integration of microfluidic channels and semiconductor lasers

Science.gov (United States)

Cran-McGreehin, Simon J.; Dholakia, Kishan; Krauss, Thomas F.

2006-08-01

We present a fabrication method for the monolithic integration of microfluidic channels into semiconductor laser material. Lasers are designed to couple directly into the microfluidic channel, allowing submerged particles pass through the output beams of the lasers. The interaction between particles in the channel and the lasers, operated in either forward or reverse bias, allows for particle detection, and the optical forces can be used to trap and move particles. Both interrogation and manipulation are made more amenable for lab-on-a-chip applications through monolithic integration. The devices are very small, they require no external optical components, have perfect intrinsic alignment, and can be created with virtually any planar configuration of lasers in order to perform a variety of tasks. Their operation requires no optical expertise and only low electrical power, thus making them suitable for computer interfacing and automation. Insulating the pn junctions from the fluid is the key challenge, which is overcome by using photo-definable SU8-2000 polymer.

Characterization of three agave species by gas chromatography and solid-phase microextraction-gas chromatography-mass spectrometry.

Science.gov (United States)

Peña-Alvarez, Araceli; Díaz, Laura; Medina, Alejandra; Labastida, Carmen; Capella, Santiago; Vera, Luz Elena

2004-02-20

Steam distillation (SD) extraction-solid-phase microextraction coupled to GC-MS was developed for the determination of terpenes and Bligh-Dyer extraction-derivatization coupled with GC for the determination of fatty acids such as ethyl esters were used. It was found that the three different Agave species have the same profile of fatty acids; the quantity of these compounds is different in each Agave variety. On the other hand, different terpenes were identified in the three Agave plants studied: nine in A. salmiana, eight in A. angustifolia and 32 in A. tequilana Weber var. azul.

Microextraction by Packed Sorbent (MEPS and Solid-Phase Microextraction (SPME as Sample Preparation Procedures for the Metabolomic Profiling of Urine

Directory of Open Access Journals (Sweden)

Catarina Silva

2014-01-01

Full Text Available For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS and solid-phase microextraction (SPME, completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review

Energy Technology Data Exchange (ETDEWEB)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review

International Nuclear Information System (INIS)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-01-01

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Rapid in situ growth of oriented titanium-nickel oxide composite nanotubes arrays coated on a nitinol wire as a solid-phase microextraction fiber coupled to HPLC-UV.

Science.gov (United States)

Zhen, Qi; Zhang, Min; Song, Wenlan; Wang, Huiju; Wang, Xuemei; Du, Xinzhen

2016-10-01

An oriented titanium-nickel oxide composite nanotubes coating was in situ grown on a nitinol wire by direct electrochemical anodization in ethylene glycol with ammonium fluoride and water for the first time. The morphology and composition of the resulting coating showed that the anodized nitinol wire provided a titania-rich coating. The titanium-nickel oxide composite nanotubes coated fiber was used for solid-phase microextraction of different aromatic compounds coupled to high-performance liquid chromatography with UV detection. The titanium-nickel oxide composite nanotubes coating exhibited high extraction capability, good selectivity, and rapid mass transfer for weakly polar UV filters. Thereafter the important parameters affecting extraction efficiency were investigated for solid-phase microextraction of UV filters. Under the optimized conditions, the calibration curves were linear in the range of 0.1-300 μg/L for target UV filters with limits of detection of 0.019-0.082 μg/L. The intraday and interday precision of the proposed method with the single fiber were 5.3-7.2 and 5.9-7.9%, respectively, and the fiber-to-fiber reproducibility ranged from 6.3 to 8.9% for four fibers fabricated in different batches. Finally, its applicability was evaluated by the extraction and determination of target UV filters in environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microextraction sample preparation techniques in biomedical analysis.

Science.gov (United States)

Szultka, Malgorzata; Pomastowski, Pawel; Railean-Plugaru, Viorica; Buszewski, Boguslaw

2014-11-01

Biologically active compounds are found in biological samples at relatively low concentration levels. The sample preparation of target compounds from biological, pharmaceutical, environmental, and food matrices is one of the most time-consuming steps in the analytical procedure. The microextraction techniques are dominant. Metabolomic studies also require application of proper analytical technique for the determination of endogenic metabolites present in biological matrix on trace concentration levels. Due to the reproducibility of data, precision, relatively low cost of the appropriate analysis, simplicity of the determination, and the possibility of direct combination of those techniques with other methods (combination types on-line and off-line), they have become the most widespread in routine determinations. Additionally, sample pretreatment procedures have to be more selective, cheap, quick, and environmentally friendly. This review summarizes the current achievements and applications of microextraction techniques. The main aim is to deal with the utilization of different types of sorbents for microextraction and emphasize the use of new synthesized sorbents as well as to bring together studies concerning the systematic approach to method development. This review is dedicated to the description of microextraction techniques and their application in biomedical analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dispersive liquid-liquid microextraction coupled with digital image colorimetric analysis for detection of total iron in water and food samples.

Science.gov (United States)

Peng, Bo; Chen, Guorong; Li, Kai; Zhou, Min; Zhang, Ji; Zhao, Shengguo

2017-09-01

A simple and low cost assay for total iron in various samples based on dispersive liquid-liquid microextraction (DLLME) coupled with digital scanning image analysis was proposed. Orthogonal experiment design was utilized to optimize the amount of extraction solvent and disperser solvent, O-phenanthroline concentration and buffer pH. Under the optimum conditions, the calibration curve was linear over the range of 0.047-1.0μgmL -1 (R 2 >0.99) of iron. The limit of detection (LOD) for iron was 14.1μgL -1 and limit of quantification (LOQ) was 46.5μgL -1 . The relative standard deviations for seven replicate determinations of 0.5μgmL -1 of iron was 3.75%. The method was successfully applied for analysis of total iron in water and food samples without using any spectral instrument and it could have a potential industrial impact in developing fast and portable devices to analyze the iron content in water and certain foods. Copyright © 2017 Elsevier Ltd. All rights reserved.

Monolithic exploding foil initiator

Science.gov (United States)

Welle, Eric J; Vianco, Paul T; Headley, Paul S; Jarrell, Jason A; Garrity, J. Emmett; Shelton, Keegan P; Marley, Stephen K

2012-10-23

A monolithic exploding foil initiator (EFI) or slapper detonator and the method for making the monolithic EFI wherein the exploding bridge and the dielectric from which the flyer will be generated are integrated directly onto the header. In some embodiments, the barrel is directly integrated directly onto the header.

Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

Directory of Open Access Journals (Sweden)

Liu Yang

2014-11-01

Full Text Available On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples.

Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

2013-01-01

Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C 2 mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences

Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Jiao, Jiao [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); Ma, Dan-Hui [College of Life Sciences, Northeast Forestry University, Harbin 150040 (China); Gai, Qing-Yan; Wang, Wei; Luo, Meng [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Fu, Yu-Jie, E-mail: yujie_fu2002@yahoo.com [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Ma, Wei, E-mail: mawei@hljucm.net [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); School of Pharmaceutical, Heilongjiang University of Chinese Medicine, Harbin 150040 (China)

2013-12-04

Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C{sub 2}mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences.

Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

International Nuclear Information System (INIS)

Nomngongo, Philiswa N.; Ngila, J. Catherine

2014-01-01

This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L −1 , n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L −1 and 0.3–0.9 μg L −1 , respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ

Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

Energy Technology Data Exchange (ETDEWEB)

Nomngongo, Philiswa N.; Ngila, J. Catherine, E-mail: jcngila@uj.ac.za

2014-08-01

This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L{sup −1}, n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L{sup −1} and 0.3–0.9 μg L{sup −1}, respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ.

Headspace solid-phase microextraction coupled to gas chromatography for the analysis of aldehydes in edible oils.

Science.gov (United States)

Ma, Chunhua; Ji, Jiaojiao; Tan, Connieal; Chen, Dongmei; Luo, Feng; Wang, Yiru; Chen, Xi

2014-03-01

Oxidation has important effects on the quality of edible oils. In particular, the generation of aldehydes produced by the oxidation of oils is one of the deteriorative factors to their quality. The aim of this study was to develop a method to determine the aldehydes as lipid oxidation markers in edible oils. Seven aldehydes generated from lipid oxidation were studied using headspace solid-phase microextraction coupled to gas chromatography with a flame ionization detector. The extraction efficiency of five commercial fibers was investigated and the influence of extraction temperature, extraction time, desorption temperature, and desorption time were optimized. The best result was obtained with 85 μm carboxen/polydimethylsiloxane, extraction at 50 °C for 15 min and desorption in the gas chromatography injector at 250 °C for 2 min. Under the optimized conditions, the content of hexanal was the highest of the seven aldehydes in all edible oils. The limits of detection for hexanal in the three oils were found to range from 4.6 to 10.2 ng L(-1). The reproducibility of the method was evaluated and the relative standard deviations were less than 8.9%. This developed approach was successfully applied to analyze hexanal in peanut oil, soy oil, and olive oil samples, and these results were compared with those obtained using the thiobarbituric acid-reactive substances (TBARs) method. © 2013 The Authors. Published by Elsevier B.V. All rights reserved.

Multiple solid-phase microextraction

NARCIS (Netherlands)

Koster, EHM; de Jong, GJ

2000-01-01

Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that

Monolithic pixels on moderate resistivity substrate and sparsifying readout architecture

International Nuclear Information System (INIS)

Giubilato, P.; Battaglia, M.; Bisello, D.; Caselle, M.; Chalmet, P.; Demaria, L.; Ikemoto, Y.; Kloukinas, K.; Mansuy, S.C.; Mattiazzo, S.; Marchioro, A.; Mugnier, H.; Pantano, D.; Potenza, A.; Rivetti, A.; Rousset, J.; Silvestrin, L.; Snoeys, W.

2013-01-01

The LePix projects aim realizing a new generation monolithic pixel detectors with improved performances at lesser cost with respect to both current state of the art monolithic and hybrid pixel sensors. The detector is built in a 90 nm CMOS process on a substrate of moderate resistivity. This allows charge collection by drift while maintaining the other advantages usually offered by MAPS, like having a single piece detector and using a standard CMOS production line. The collection by drift mechanism, coupled to the low capacitance design of the collecting node made possible by the monolithic approach, provides an excellent signal to noise ratio straight at the pixel cell together with a radiation tolerance far superior to conventional un-depleted MAPS. The excellent signal-to-noise performance is demonstrated by the device ability to separate the 6 keV 55 Fe double peak at room temperature. To achieve high granularity (10–20 µm pitch pixels) over large detector areas maintaining high readout speed, a completely new compressing architecture has been devised. This architecture departs from the mainstream hybrid pixel sparsification approach, which uses in-pixel logic to reduce data, by using topological compression to minimize pixel area and power consumption

Determination of some selected pesticide residues in apple juice by solid-phase microextraction coupled to gas chromatography – mass spectrometry

Directory of Open Access Journals (Sweden)

Andrea Hercegová

2011-01-01

Full Text Available The performance of solid phase microextraction (SPME for enrichment of pesticides from apple juice was investigated. Samples were diluted with water, extracted by solid-phase microextraction and analysed by gas chromatography using mass-spectrometry detector (MSD in selected ion monitoring mode (SIM. The method was tested for the following pesticides used mostly in fruit culturing at Slovakia: tebuthylazine, fenitrothion, chlorpyrifos, myclobutanil, cyprodinil, phosalone, pyrimethanil, tebuconazole, kresoxim-methyl, methidathion, penconazole. All pesticides were extracted with polydimethylsiloxane fibre 100 μm thickness. The linear concentration range of application was 0.05 μg dm−3–10 μg dm−3. The method described provides detectabilities complying with the maximum residue levels (MRLs set by regulatory organizations for pesticides in apple juice matrices. The solvent – free SPME procedure was found to be quicker and more cost effective then the solvent extraction methods commonly used.

In-coupled syringe assisted octanol-water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey.

Science.gov (United States)

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax

2015-07-01

A simple and fast method namely in-coupled syringe assisted octanol-water partition microextraction combined with high performance liquid chromatography (HPLC) has been developed for the extraction, preconcentration and determination of neonicotinoid insecticide residues (e.g. imidacloprid, acetamiprid, clothianidin, thiacloprid, thiamethoxam, dinotefuran, and nitenpyram) in honey. The experimental parameters affected the extraction efficiency, including kind and concentration of salt, kind of disperser solvent and its volume, kind of extraction solvent and its volume, shooting times and extraction time were investigated. The extraction process was carried out by rapid shooting of two syringes. Therefore, rapid dispersion and mass transfer processes was created between phases, and thus affects the extraction efficiency of the proposed method. The optimum extraction conditions were 10.00 mL of aqueous sample, 10% (w/v) Na2SO4, 1-octanol (100µL) as an extraction solvent, shooting 4 times and extraction time 2min. No disperser solvent and centrifugation step was necessary. Linearity was obtained within the range of 0.1-3000 ngmL(-1), with the correlation coefficients greater than 0.99. The high enrichment factor of the target analytes was 100 fold and low limit of detection (0.25-0.50 ngmL(-1)) could be obtained. This proposed method has been successfully applied in the analysis of neonicotinoid residues in honey, and good recoveries in the range of 96.93-107.70% were obtained. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of heterocyclic amines in hair by on-line in-tube solid-phase microextraction coupled with liquid chromatography−tandem mass spectrometry

International Nuclear Information System (INIS)

Kataoka, Hiroyuki; Inoue, Tsutomu; Saito, Keita; Kato, Hisato; Masuda, Kazufumi

2013-01-01

Graphical abstract: Mutagenic and carcinogenic heterocyclic amines are accumulated in the hair of smoker. -- Highlights: •On-line in-tube solid-phase microextraction of heterocyclic amines was optimized. •Fourteen heterocyclic amines were simultaneously determined by LC–MS/MS. •Pico gram levels of heterocyclic amines could be easily analyzed within 15 min. •Heterocyclic amines could be quantitatively analyzed from several milligrams of hair. •The method is useful for the assessment of long-term exposure to heterocyclic amines. -- Abstract: Mutagenic and carcinogenic heterocyclic amines (HCAs) are formed during heating of various proteinaceous foods, but human exposure to HCAs has not yet been elucidated in detail. To assess long-term exposure to HCAs, we developed a simple and sensitive method for measuring HCAs in hair by automated on-line in-tube solid-phase microextraction (SPME) coupled with liquid chromatography–tandem mass spectrometry (LC–MS/MS). Using a Zorbax Eclipse XDB-C8 column, 16 HCAs were analyzed within 15 min. The optimum in-tube SPME conditions were 20 draw/eject cycles of 40 μL sample at a flow rate of 200 μL min −1 using a Supel-Q PLOT capillary column as an extraction device. The extracted HCAs were easily desorbed from the column by passage of the mobile phase, with no carryover observed. This in-tube SPME LC–MS/MS method showed good linearity for HCAs in the range of 10–2000 pg mL −1 , with correlation coefficients above 0.9989 (n = 18), using stable isotope-labeled HCA internal standards. The detection limits (S/N = 3) of 14 HCAs except for MeAαC and Glu-P-1 were 0.10–0.79 pg mL −1 . This method was successfully utilized to analyze 14 HCAs in hair samples without any interference peaks, with quantitative limits (S/N = 10) of about 0.17–1.32 pg mg −1 hair. Using this method, we evaluated the exposure to HCAs in cigarette smoke and the suitability of using hair HCAs as exposure biomarkers

Determination of Trace Amounts of Lead with ETAAS After Single Drop Microextraction and Dispersive Liquid Liquid Microextraction Methods

Directory of Open Access Journals (Sweden)

Efeçınar M.

2013-04-01

Full Text Available Two liquid-phase microextraction procedures, single-drop microextraction (SDME and dispersive liquid–liquid microextraction (DLLME, have been developed for the determination of lead by electrothermal atomic absorption spectrometry (ETAAS. Both methods were based on the formation of lead iodide-Rhodamine B complex which is in phosphoric acid medium. In the presence of KI, anionic lead iodide was complexed with Rhodamine B as an ion-association complex. Several factors that may be affected on the SDME and DLLME methods were optimized. In the optimum experimental conditions, the limit of detection (3s and the enhancement factor were 0.008 μgL−1 and 152 for SDME and 0.0129 μgL−1 and 89 for DLLME respectively. The relative standard deviation (RSD for eight replicate determinations of 0.25 μgL−1 Pb was 4.6% for SDME and 0.5 μgL−1 Pb was 2.9% for DLLME. The developed methods were validated by the analysis of certified reference materials, and applied successfully to the determination of lead in several water and food samples.

Recent Developments and Applications of Solid Phase Microextraction (SPME in Food and Environmental Analysis—A Review

Directory of Open Access Journals (Sweden)

Sybille Merkle

2015-06-01

Full Text Available Solid-phase microextraction (SPME is a simple, sensitive, rapid and solvent-free technique for the extraction of analytes from gaseous, liquid and solid samples and takes a leading position among microextraction methods. Application of SPME in sample preparation has been increasing continuously over the last decade. It is most often used as an automatized fiber injection system coupled to chromatographic separation modules for the extraction of volatile and semivolatile organic compounds and also allows for the trace analysis of compounds in complex matrices. Since SPME was first introduced in the early 1990s, several modifications have been made to adapt the procedure to specific application requirements. More robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Automation and on-line coupling to analytical instruments have been achieved in many applications and new derivatization strategies as well as improved calibration procedures have been developed to overcome existing limitations regarding quantitation. Furthermore, devices using tubes, needles or tips for extraction instead of a fiber have been designed. In the field of food analysis, SPME has been most often applied to fruit/vegetables, fats/oils, wine, meat products, dairy and beverages whereas environmental applications focus on the analysis of air, water, soil and sediment samples.

A Symmetric Positive Definite Formulation for Monolithic Fluid Structure Interaction

Science.gov (United States)

2010-08-09

more likely to converge than simply iterating the partitioned approach to convergence in a simple Gauss - Seidel manner. Our approach allows the use of...conditions in a second step. These approaches can also be iterated within a given time step for increased stability, noting that in the limit if one... converges one obtains a monolithic (albeit expensive) approach. Other approaches construct strongly coupled systems and then solve them in one of several

Iminodiacetic acid functionalised organopolymer monoliths: application to the separation of metal cations by capillary high-performance chelation ion chromatography.

Science.gov (United States)

Moyna, Áine; Connolly, Damian; Nesterenko, Ekaterina; Nesterenko, Pavel N; Paull, Brett

2013-03-01

Lauryl methacrylate-co-ethylene dimethacrylate monoliths were polymerised within fused silica capillaries and subsequently photo-grafted with varying amounts of glycidyl methacrylate (GMA). The grafted monoliths were then further modified with iminodiacetic acid (IDA), resulting in a range of chelating ion-exchange monoliths of increasing capacity. The IDA functional groups were attached via ring opening of the epoxy group on the poly(GMA) structure. Increasing the amount of attached poly(GMA), via photo-grafting with increasing concentrations of GMA, from 15 to 35%, resulted in a proportional and controlled increase in the complexation capacity of the chelating monoliths. Scanning capacitively coupled contactless conductivity detection (sC(4)D) was used to characterise and verify homogenous distribution of the chelating ligand along the length of the capillaries non-invasively. Chelation ion chromatographic separations of selected transition and heavy metals were carried out, with retention factor data proportional to the concentration of grafted poly(GMA). Average peak efficiencies of close to 5,000 N/m were achieved, with the isocratic separation of Na, Mg(II), Mn(II), Co(II), Cd(II) and Zn(II) possible on a 250-mm-long monolith. Multiple monolithic columns produced to the same recipes gave RSD data for retention factors of ions). The monolithic chelating ion-exchanger was applied to the separation of alkaline earth and transition metal ions spiked in natural and potable waters.

Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

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Đurović-Pejčev Rada

2016-01-01

Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

Microfluidic devices and methods including porous polymer monoliths

Science.gov (United States)

Hatch, Anson V; Sommer, Gregory J; Singh, Anup K; Wang, Ying-Chih; Abhyankar, Vinay V

2014-04-22

Microfluidic devices and methods including porous polymer monoliths are described. Polymerization techniques may be used to generate porous polymer monoliths having pores defined by a liquid component of a fluid mixture. The fluid mixture may contain iniferters and the resulting porous polymer monolith may include surfaces terminated with iniferter species. Capture molecules may then be grafted to the monolith pores.

Polar and nonpolar organic polymer-based monolithic columns for capillary electrochromatography and high-performance liquid chromatography.

Science.gov (United States)

Rathnasekara, Renuka; Khadka, Shantipriya; Jonnada, Murthy; El Rassi, Ziad

2017-01-01

This review article is a continuation of the previous reviews on the area of monolithic columns covering the progress made in the field over the last couple of years from the beginning of the second half of 2014 until the end of the first half of 2016. It summarizes and evaluates the evolvement of both polar and nonpolar organic monolithic columns and their use in hydrophilic interaction LC and CEC and reversed-phase chromatography and RP-CEC. The review article discusses the results reported in a total of 62 references. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mixed functional monomers-based monolithic adsorbent for the effective extraction of sulfonylurea herbicides in water and soil samples.

Science.gov (United States)

Pei, Miao; Zhu, Xiangyu; Huang, Xiaojia

2018-01-05

Effective extraction is a key step in the determination of sulfonylurea herbicides (SUHs) in complicated samples. According to the chemical properties of SUHs, a new monolithic adsorbent utilizing acrylamidophenylboronic acid and vinylimidazole as mixed functional monomers was synthesized. The new adsorbent was employed as the extraction phase of multiple monolithic fiber solid-phase microextraction (MMF-SPME) of SUHs, and the extracted SUHs were determined by high-performance liquid chromatography with diode array detection (HPLC-DAD). Results well evidence that the prepared adsorbent could extract SUHs in environmental waters and soil effectively through multiply interactions such as boronate affinity, dipole-dipole and π-π interactions. Under the optimized extraction conditions, the limits of detection for target SUHs in environmental water and soil samples were 0.018-0.17μg/L and 0.14-1.23μg/kg, respectively. At the same time, the developed method also displayed some analytical merits including wide linear dynamic ranges, good method reproducibility, satisfactory sensitivity and low consume of organic solvent. Finally, the developed were successfully applied to monitor trace SUHs in environmental water and soil samples. The recoveries at three fortified concentrations were in the range of 70.6-119% with RSD below 11% in all cases. The obtained results well demonstrate the excellent practical applicability of the developed MMF-SPME-HPLC-DAD method for the monitoring of SUHs in water and soil samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Indium phosphide-based monolithically integrated PIN waveguide photodiode readout for resonant cantilever sensors

Energy Technology Data Exchange (ETDEWEB)

Siwak, N. P. [Department of Electrical and Computer Engineering, Institute for Systems Research, University of Maryland, College Park, Maryland 20742 (United States); Laboratory for the Physical Sciences, 8050 Greenmead Drive, College Park, Maryland 20740 (United States); Fan, X. Z.; Ghodssi, R. [Department of Electrical and Computer Engineering, Institute for Systems Research, University of Maryland, College Park, Maryland 20742 (United States); Kanakaraju, S.; Richardson, C. J. K. [Laboratory for the Physical Sciences, 8050 Greenmead Drive, College Park, Maryland 20740 (United States)

2014-10-06

An integrated photodiode displacement readout scheme for a microelectromechanical cantilever waveguide resonator sensing platform is presented. III-V semiconductors are used to enable the monolithic integration of passive waveguides with active optical components. This work builds upon previously demonstrated results by measuring the displacement of cantilever waveguide resonators with on-chip waveguide PIN photodiodes. The on-chip integration of the readout provides an additional 70% improvement in mass sensitivity compared to off-chip photodetector designs due to measurement stability and minimized coupling loss. In addition to increased measurement stability, reduced packaging complexity is achieved due to the simplicity of the readout design. We have fabricated cantilever waveguides with integrated photodetectors and experimentally characterized these cantilever sensors with monolithically integrated PIN photodiodes.

Monolithically integrated quantum dot optical modulator with semiconductor optical amplifier for thousand and original band optical communication

Science.gov (United States)

Yamamoto, Naokatsu; Akahane, Kouichi; Umezawa, Toshimasa; Matsumoto, Atsushi; Kawanishi, Tetsuya

2016-04-01

A monolithically integrated quantum dot (QD) optical gain modulator (OGM) with a QD semiconductor optical amplifier (SOA) was successfully developed with T-band (1.0 µm waveband) and O-band (1.3 µm waveband) QD optical gain materials for Gbps-order, high-speed optical data generation. The insertion loss due to coupling between the device and the optical fiber was effectively compensated for by the SOA section. It was also confirmed that the monolithic QD-OGM/SOA device enabled >4.8 Gbps optical data generation with a clear eye opening in the T-band. Furthermore, we successfully demonstrated error-free 4.8 Gbps optical data transmissions in each of the six wavelength channels over a 10-km-long photonic crystal fiber using the monolithic QD-OGM/SOA device in multiple O-band wavelength channels, which were generated by the single QD gain chip. These results suggest that the monolithic QD-OGM/SOA device will be advantageous in ultra-broadband optical frequency systems that utilize the T+O-band for short- and medium-range optical communications.

Monolithic spectrometer

Energy Technology Data Exchange (ETDEWEB)

Rajic, Slobodan (Knoxville, TN); Egert, Charles M. (Oak Ridge, TN); Kahl, William K. (Knoxville, TN); Snyder, Jr., William B. (Knoxville, TN); Evans, III, Boyd M. (Oak Ridge, TN); Marlar, Troy A. (Knoxville, TN); Cunningham, Joseph P. (Oak Ridge, TN)

1998-01-01

A monolithic spectrometer is disclosed for use in spectroscopy. The spectrometer is a single body of translucent material with positioned surfaces for the transmission, reflection and spectral analysis of light rays.

Monolithic Magneto-Optical Nanocomposites of Barium Hexaferrite Platelets in PMMA.

Science.gov (United States)

Ferk, Gregor; Krajnc, Peter; Hamler, Anton; Mertelj, Alenka; Cebollada, Federico; Drofenik, Miha; Lisjak, Darja

2015-06-12

The incorporation of magnetic barium hexaferrite nanoparticles in a transparent polymer matrix of poly(methyl methacrylate) (PMMA) is reported for the first time. The barium hexaferrite nanoplatelets doped with Sc(3+), i.e., BaSc0.5Fe11.5O12 (BaHF), having diameters in the range 20 to 130 nm and thicknesses of approximately 5 nm, are synthesized hydrothermally and stabilized in 1-butanol with dodecylbenzenesulfonic acid. This method enables the preparation of monolithic nanocomposites by admixing the BaHF suspension into a liquid monomer, followed by in-situ, bulk free-radical polymerization. The PMMA retains its transparency for loadings of BaHF nanoparticles up to 0.27 wt.%, meaning that magnetically and optically anisotropic, monolithic nanocomposites can be synthesized when the polymerization is carried out in a magnetic field. The excellent dispersion of the magnetic nanoparticles, coupled with a reasonable control over the magnetic properties achieved in this investigation, is encouraging for the magneto-optical applications of these materials.

Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples

Science.gov (United States)

Araujo, Lilia; Prieto, Avismelsi; Navalón, Alberto; Vílchez, José Luis; Valera, Paola; Zambrano, Ana; Dugas, Vincent

2017-01-01

A new analytical method coupling a (off-line) solid-phase microextraction with an on-line capillary electrophoresis (CE) sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE) using ultraviolet diode array detection (DAD). Further enhancement of concentration sensitivity detection was achieved by on-line CE “acetonitrile stacking” preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L−1 and 2.91 and 3.86 µg∙L−1, respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers. PMID:28686186

Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples

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Maria Espina-Benitez

2017-07-01

Full Text Available A new analytical method coupling a (off-line solid-phase microextraction with an on-line capillary electrophoresis (CE sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE using ultraviolet diode array detection (DAD. Further enhancement of concentration sensitivity detection was achieved by on-line CE “acetonitrile stacking” preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L−1 and 2.91 and 3.86 µg∙L−1, respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers.

Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples.

Science.gov (United States)

Espina-Benitez, Maria; Araujo, Lilia; Prieto, Avismelsi; Navalón, Alberto; Vílchez, José Luis; Valera, Paola; Zambrano, Ana; Dugas, Vincent

2017-07-07

A new analytical method coupling a (off-line) solid-phase microextraction with an on-line capillary electrophoresis (CE) sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE) using ultraviolet diode array detection (DAD). Further enhancement of concentration sensitivity detection was achieved by on-line CE "acetonitrile stacking" preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L -1 and 2.91 and 3.86 µg∙L -1 , respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers.

Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Jia Xiaoyu; Han Yi; Liu Xinli; Duan Taicheng; Chen Hangting

2011-01-01

The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg + ) and mercury (Hg 2+ ) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg + and Hg 2+ were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL -1 for MeHg + and 0.0014 ng mL -1 for Hg 2+ , respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL -1 MeHg + and Hg 2+ were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

Ceria nanocubic-ultrasonication assisted dispersive liquid-liquid microextraction coupled with matrix assisted laser desorption/ionization mass spectrometry for pathogenic bacteria analysis.

Science.gov (United States)

Abdelhamid, Hani Nasser; Bhaisare, Mukesh L; Wu, Hui-Fen

2014-03-01

A new ceria (CeO2) nanocubic modified surfactant is used as the basis of a novel nano-based microextraction technique for highly sensitive detection of pathogenic bacteria (Pseudomonas aeruginosa and Staphylococcus aureus). The technique uses ultrasound enhanced surfactant-assisted dispersive liquid-liquid microextraction (UESA-DLLME) with and without ceria (CeO2) followed by matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS). In order to achieve high separation efficiency, we investigated the influential parameters, including extraction time of ultrasonication, type and volume of the extraction solvent and surfactant. Among various surfactants, the cationic surfactants can selectively offer better extraction efficiency on bacteria analysis than that of the anionic surfactants due to the negative charges of bacteria cell membranes. Extractions of the bacteria lysate from aqueous samples via UESA-DLLME-MALDI-MS were successfully achieved by using cetyltrimethyl ammonium bromide (CTAB, 10.0 µL, 1.0×10(-3) M) as surfactants in chlorobenzene (10.0 µL) and chloroform (10.0 µL) as the optimal extracting solvent for P. aeruginosa and S. aureus, respectively. Ceria nanocubic was synthesized, and functionalized with CTAB (CeO2@CTAB) and then characterized using transmission electron microscopy (TEM) and optical spectroscopy (UV and FTIR). CeO2@CTAB demonstrates high extraction efficiency, improve peaks ionization, and enhance resolution. The prime reasons for these improvements are due to the large surface area of nanoparticles, and its absorption that coincides with the wavelength of MALDI laser (337 nm, N2 laser). CeO2@CTAB-based microextraction offers lowest detectable concentrations tenfold lower than that of without nanoceria. The present approach has been successfully applied to detect pathogenic bacteria at low concentrations of 10(4)-10(5) cfu/mL (without ceria) and at 10(3)-10(4) cfu/mL (with ceria) from bacteria suspensions. Finally, the

Time walk correction for TOF-PET detectors based on a monolithic scintillation crystal coupled to a photosensor array

International Nuclear Information System (INIS)

Vinke, R.; Loehner, H.; Schaart, D.R.; Dam, H.T. van; Seifert, S.; Beekman, F.J.; Dendooven, P.

2010-01-01

When optimizing the timing performance of a time-of-flight positron emission tomography (TOF-PET) detector based on a monolithic scintillation crystal coupled to a photosensor array, time walk as a function of annihilation photon interaction location inside the crystal needs to be considered. In order to determine the 3D spatial coordinates of the annihilation photon interaction location, a maximum likelihood estimation algorithm was developed, based on a detector characterization by a scan of a 511 keV photon beam across the front and one of the side surfaces of the crystal. The time walk effect was investigated using a 20 mmx20 mmx12 mm LYSO crystal coupled to a fast 4x4 multi-anode photomultiplier tube (MAPMT). In the plane parallel to the photosensor array, a spatial resolution of 2.4 mm FWHM is obtained. In the direction perpendicular to the MAPMT (depth-of-interaction, DOI), the resolution ranges from 2.3 mm FWHM near the MAPMT to 4 mm FWHM at a distance of 10 mm. These resolutions are uncorrected for the ∼1mm beam diameter. A coincidence timing resolution of 358 ps FWHM is obtained in coincidence with a BaF 2 detector. A time walk depending on the 3D annihilation photon interaction location is observed. Throughout the crystal, the time walk spans a range of 100 ps. Calibration of the time walk vs. interaction location allows an event-by-event correction of the time walk.

Activated Carbon Fiber Monoliths as Supercapacitor Electrodes

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Gelines Moreno-Fernandez

2017-01-01

Full Text Available Activated carbon fibers (ACF are interesting candidates for electrodes in electrochemical energy storage devices; however, one major drawback for practical application is their low density. In the present work, monoliths were synthesized from two different ACFs, reaching 3 times higher densities than the original ACFs’ apparent densities. The porosity of the monoliths was only slightly decreased with respect to the pristine ACFs, the employed PVDC binder developing additional porosity upon carbonization. The ACF monoliths are essentially microporous and reach BET surface areas of up to 1838 m2 g−1. SEM analysis reveals that the ACFs are well embedded into the monolith structure and that their length was significantly reduced due to the monolith preparation process. The carbonized monoliths were studied as supercapacitor electrodes in two- and three-electrode cells having 2 M H2SO4 as electrolyte. Maximum capacitances of around 200 F g−1 were reached. The results confirm that the capacitance of the bisulfate anions essentially originates from the double layer, while hydronium cations contribute with a mixture of both, double layer capacitance and pseudocapacitance.

Monolithic solid-state lasers for spaceflight

Science.gov (United States)

Krainak, Michael A.; Yu, Anthony W.; Stephen, Mark A.; Merritt, Scott; Glebov, Leonid; Glebova, Larissa; Ryasnyanskiy, Aleksandr; Smirnov, Vadim; Mu, Xiaodong; Meissner, Stephanie; Meissner, Helmuth

2015-02-01

A new solution for building high power, solid state lasers for space flight is to fabricate the whole laser resonator in a single (monolithic) structure or alternatively to build a contiguous diffusion bonded or welded structure. Monolithic lasers provide numerous advantages for space flight solid-state lasers by minimizing misalignment concerns. The closed cavity is immune to contamination. The number of components is minimized thus increasing reliability. Bragg mirrors serve as the high reflector and output coupler thus minimizing optical coatings and coating damage. The Bragg mirrors also provide spectral and spatial mode selection for high fidelity. The monolithic structure allows short cavities resulting in short pulses. Passive saturable absorber Q-switches provide a soft aperture for spatial mode filtering and improved pointing stability. We will review our recent commercial and in-house developments toward fully monolithic solid-state lasers.

Methacrylate monolithic columns functionalized with epinephrine for capillary electrochromatography applications.

Science.gov (United States)

Carrasco-Correa, Enrique Javier; Ramis-Ramos, Guillermo; Herrero-Martínez, José Manuel

2013-07-12

Epinephrine-bonded polymeric monoliths for capillary electrochromatography (CEC) were developed by nucleophilic substitution reaction of epoxide groups of poly(glycidyl-methacrylate-co-ethylenedimethacrylate) (poly(GMA-co-EDMA)) monoliths using epinephrine as nucleophilic reagent. The ring opening reaction under dynamic conditions was optimized. Successful chemical modification of the monolith surface was ascertained by in situ Raman spectroscopy characterization. In addition, the amount of epinephrine groups that was bound to the monolith surface was evaluated by oxidation of the catechol groups with Ce(IV), followed by spectrophotometric measurement of unreacted Ce(IV). About 9% of all theoretical epoxide groups of the parent monolith were bonded to epinephrine. The chromatographic behavior of the epinephrine-bonded monolith in CEC conditions was assessed with test mixtures of alkyl benzenes, aniline derivatives and substituted phenols. In comparison to the poly(GMA-co-EDMA) monoliths, the epinephrine-bonded monoliths exhibited a much higher retention and slight differences in selectivity. The epinephrine-bonded monolith was further modified by oxidation with a Ce(IV) solution and compared with the epinephrine-bonded monoliths. The resulting monolithic stationary phases were evaluated in terms of reproducibility, giving RSD values below 9% in the parameters investigated. Copyright © 2013 Elsevier B.V. All rights reserved.

Monitoring Pb in Aqueous Samples by Using Low Density Solvent on Air-Assisted Dispersive Liquid-Liquid Microextraction Coupled with UV-Vis Spectrophotometry.

Science.gov (United States)

Nejad, Mina Ghasemi; Faraji, Hakim; Moghimi, Ali

2017-04-01

In this study, AA-DLLME combined with UV-Vis spectrophotometry was developed for pre-concentration, microextraction and determination of lead in aqueous samples. Optimization of the independent variables was carried out according to chemometric methods in three steps. According to the screening and optimization study, 86 μL of 1-undecanol (extracting solvent), 12 times syringe pumps, pH 2.0, 0.00% of salt and 0.1% DDTP (chelating agent) were chosen as the optimum independent variables for microextraction and determination of lead. Under the optimized conditions, R = 0.9994, and linearity range was 0.01-100 µg mL -1 . LOD and LOQ were 3.4 and 11.6 ng mL -1 , respectively. The method was applied for analysis of real water samples, such as tap, mineral, river and waste water.

The recent developments in dispersive liquid–liquid microextraction for preconcentration and determination of inorganic analytes

Directory of Open Access Journals (Sweden)

H.M. Al-Saidi

2014-12-01

Full Text Available Recently, increasing interest on the use of dispersive liquid–liquid microextraction (DLLME developed in 2006 by Rezaee has been found in the field of separation science. DLLME is miniaturized format of liquid–liquid extraction in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In the present review, the combination of DLLME with different analytical techniques such as atomic absorption spectrometry (AAS, inductively coupled plasma-optical emission spectrometry (ICP-OES, gas chromatography (GC, and high-performance liquid chromatography (HPLC for preconcentration and determination of inorganic analytes in different types of samples will be discussed. Recent developments in DLLME, e.g., displacement-DLLME, the use of an auxiliary solvent for adjustment of density of extraction mixture, and the application of ionic liquid-based DLLME in determination of inorganic species even in the presence of high content of salts are presented in the present review. Finally, comparison of DLLME with the other liquid-phase microextraction approaches and limitations of this technique are provided.

Analysis of the Volatile Profile of Core Chinese Mango Germplasm by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

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Xiao-Wei Ma

2018-06-01

Full Text Available Despite abundant published research on the volatile characterization of mango germplasm, the aroma differentiation of Chinese cultivars remains unclear. Using headspace solid phase microextraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC-MS, the composition and relative content of volatiles in 37 cultivars representing the diversity of Chinese mango germplasm were investigated. Results indicated that there are distinct differences in the components and content of volatile compounds among and within cultivars. In total, 114 volatile compounds, including 23 monoterpenes, 16 sesquiterpenes, 29 non-terpene hydrocarbons, 25 esters, 11 aldehydes, five alcohols and five ketones, were identified. The total volatile content among cultivars ranged from 211 to 26,022 μg/kg fresh weight (FW, with 123-fold variation. Terpene compounds were the basic background volatiles, and 34 cultivars exhibited abundant monoterpenes. On the basis of hierarchical cluster analysis (HCA and principal component analysis (PCA, terpinolene and α-pinene were important components constituting the aroma of Chinese mango cultivars. Most obviously, a number of mango cultivars with high content of various aroma components were observed, and they can serve as potential germplasms for both breeding and direct use.

Mechanically stable, hierarchically porous Cu3(btc)2 (HKUST-1) monoliths via direct conversion of copper(II) hydroxide-based monoliths.

Science.gov (United States)

Moitra, Nirmalya; Fukumoto, Shotaro; Reboul, Julien; Sumida, Kenji; Zhu, Yang; Nakanishi, Kazuki; Furukawa, Shuhei; Kitagawa, Susumu; Kanamori, Kazuyoshi

2015-02-28

The synthesis of highly crystalline macro-meso-microporous monolithic Cu3(btc)2 (HKUST-1; btc(3-) = benzene-1,3,5-tricarboxylate) is demonstrated by direct conversion of Cu(OH)2-based monoliths while preserving the characteristic macroporous structure. The high mechanical strength of the monoliths is promising for possible applications to continuous flow reactors.

Synthesis of Porous Carbon Monoliths Using Hard Templates.

Science.gov (United States)

Klepel, Olaf; Danneberg, Nina; Dräger, Matti; Erlitz, Marcel; Taubert, Michael

2016-03-21

The preparation of porous carbon monoliths with a defined shape via template-assisted routes is reported. Monoliths made from porous concrete and zeolite were each used as the template. The porous concrete-derived carbon monoliths exhibited high gravimetric specific surface areas up to 2000 m²·g -1 . The pore system comprised macro-, meso-, and micropores. These pores were hierarchically arranged. The pore system was created by the complex interplay of the actions of both the template and the activating agent as well. On the other hand, zeolite-made template shapes allowed for the preparation of microporous carbon monoliths with a high volumetric specific surface area. This feature could be beneficial if carbon monoliths must be integrated into technical systems under space-limited conditions.

Evaluation of needle trap micro-extraction and solid-phase micro-extraction: Obtaining comprehensive information on volatile emissions from in vitro cultures.

Science.gov (United States)

Oertel, Peter; Bergmann, Andreas; Fischer, Sina; Trefz, Phillip; Küntzel, Anne; Reinhold, Petra; Köhler, Heike; Schubert, Jochen K; Miekisch, Wolfram

2018-05-14

Volatile organic compounds (VOCs) emitted from in vitro cultures may reveal information on species and metabolism. Owing to low nmol L -1 concentration ranges, pre-concentration techniques are required for gas chromatography-mass spectrometry (GC-MS) based analyses. This study was intended to compare the efficiency of established micro-extraction techniques - solid-phase micro-extraction (SPME) and needle-trap micro-extraction (NTME) - for the analysis of complex VOC patterns. For SPME, a 75 μm Carboxen®/polydimethylsiloxane fiber was used. The NTME needle was packed with divinylbenzene, Carbopack X and Carboxen 1000. The headspace was sampled bi-directionally. Seventy-two VOCs were calibrated by reference standard mixtures in the range of 0.041-62.24 nmol L -1 by means of GC-MS. Both pre-concentration methods were applied to profile VOCs from cultures of Mycobacterium avium ssp. paratuberculosis. Limits of detection ranged from 0.004 to 3.93 nmol L -1 (median = 0.030 nmol L -1 ) for NTME and from 0.001 to 5.684 nmol L -1 (median = 0.043 nmol L -1 ) for SPME. NTME showed advantages in assessing polar compounds such as alcohols. SPME showed advantages in reproducibility but disadvantages in sensitivity for N-containing compounds. Micro-extraction techniques such as SPME and NTME are well suited for trace VOC profiling over cultures if the limitations of each technique is taken into account. Copyright © 2018 John Wiley & Sons, Ltd.

Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

International Nuclear Information System (INIS)

He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

2010-01-01

A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

Capillary trap column with strong cation-exchange monolith for automated shotgun proteome analysis.

Science.gov (United States)

Wang, Fangjun; Dong, Jing; Jiang, Xiaogang; Ye, Mingliang; Zou, Hanfa

2007-09-01

A 150 microm internal diameter capillary monolithic column with a strong cation-exchange stationary phase was prepared by direct in situ polymerization of ethylene glycol methacrylate phosphate and bisacrylamide in a trinary porogenic solvent consisting dimethylsulfoxide, dodecanol, and N,N'-dimethylformamide. This phosphate monolithic column exhibits higher dynamic binding capacity, faster kinetic adsorption of peptides, and more than 10 times higher permeability than the column packed with commercially available strong cation-exchange particles. It was applied as a trap column in a nanoflow liquid chromatography-tandem mass spectrometry system for automated sample injection and online multidimensional separation. It was observed that the sample could be loaded at a flow rate as high as 40 microL/min with a back pressure of approximately 1300 psi and without compromising the separation efficiency. Because of its good orthogonality to the reversed phase separation mechanism, the phosphate monolithic trap column was coupled with a reversed-phase column for online multidimensional separation of 19 microg of the tryptic digest of yeast proteins. A total of 1522 distinct proteins were identified from 5608 unique peptides (total of 54,780 peptides) at the false positive rate only 0.46%.

Determination of Trichloroethylene in Water by Liquid–Liquid Microextraction Assisted Solid Phase Microextraction

Directory of Open Access Journals (Sweden)

Mengliang Zhang

2015-02-01

Full Text Available A method for the determination of trichloroethylene (TCE in water using portable gas chromatography/mass spectrometry (GC/MS was developed. A novel sample preparation method, liquid–liquid microextraction assisted solid phase microextraction (LLME–SPME, is introduced. In this method, 20 µL of hexane was added to 10 mL of TCE contaminated aqueous samples to assist headspace SPME. The extraction efficiency of SPME was significantly improved with the addition of minute amounts of organic solvents (i.e., 20 µL hexane. The absolute recoveries of TCE at different concentrations were increased from 11%–17% for the samples extracted by SPME to 29%–41% for the samples extracted by LLME–SPME. The method was demonstrated to be linear from 10 to 1000 ng mL−1 for TCE in water. The improvements on extraction efficiencies were also observed for toluene and 1, 2, 4-trichlorobenzene in water by using LLME–SPME method. The LLME–SPME method was optimized by using response surface modeling (RSM.

Development of a dispersive liquid-liquid microextraction method for the determination of polychlorinated biphenyls in water

International Nuclear Information System (INIS)

Rezaei, Fatemeh; Bidari, Araz; Birjandi, Afsoon Pajand; Milani Hosseini, Mohammad Reza; Assadi, Yaghoub

2008-01-01

A very simple and powerful microextraction procedure, the dispersive liquid-liquid microextraction (DLLME), was used for the determination of the content of 10 polychlorinated biphenyls (PCBs) in water samples, using gas chromatography coupled with electron-capture detection (GC-ECD). The appropriate amount of acetone (disperser solvent) and chlorobenzene (extraction solvent) at the microlevel volume was used for this procedure. The conditions for the microextraction performance were investigated and optimized. The optimized method exhibited a good linearity (R 2 > 0.996) over the studied range (0.005-2 μg L -1 ), illustrating a satisfactory precision level with R.S.D. values between 4.1% and 11.0%. The values of the detection limit (S/N = 3) were found to be lower than 0.002 μg L -1 . Furthermore, a large enrichment factor for the analytes (up to a 540-fold) was achieved in a very short time for only a 5.00-mL water sample. The effectiveness of the method towards real samples was tested by analyzing well, river and seawater samples. The relative recoveries of the well, river and seawater samples, which had been spiked with different levels of PCBs were equal to 92.0-114.0%, 97.0-102.0% and 96.0-103.0%, respectively. The attained results demonstrated that DLLME combined with GC-ECD was a fast and inexpensive technique for the PCBs determination in water samples

Fabrication and characterisation of gold nano-particle modified polymer monoliths for flow-through catalytic reactions and their application in the reduction of hexacyanoferrate

International Nuclear Information System (INIS)

Floris, Patrick; Twamley, Brendan; Nesterenko, Pavel N.; Paull, Brett; Connolly, Damian

2014-01-01

Polymer monoliths in capillary (100 μm i.d.) and polypropylene pipette tip formats (vol: 20 μL) were modified with gold nano-particles (AuNP) and subsequently used for flow-through catalytic reactions. Specifically, methacrylate monoliths were modified with amine-reactive monomers using a two-step photografting method and then reacted with ethylenediamine to provide amine attachment sites for the subsequent immobilisation of 4 nm, 7 nm or 16 nm AuNP. This was achieved by flushing colloidal suspensions of gold nano-particles through each aminated polymer monolith which resulted in a multi-point covalent attachment of gold via the lone pair of electrons on the nitrogen of the free amine groups. Field emission scanning electron microscopy and scanning capacitively coupled conductivity detection was used to characterise the surface coverage of AuNP on the monoliths. The catalytic activity of AuNP immobilised on the polymer monoliths in both formats was then demonstrated using the reduction of Fe(III) to Fe(II) by sodium borohydride as a model reaction by monitoring the reduction in absorbance of the hexacyanoferrate (III) complex at 420 nm. Catalytic activity was significantly enhanced on monoliths modified with smaller AuNP with almost complete reduction (95 %) observed when using monoliths agglomerated with 7 nm AuNPs. (author)

Biocompatible in-tube solid phase microextraction coupled with liquid chromatography-fluorescence detection for determination of interferon α in plasma samples.

Science.gov (United States)

Chaves, Andréa R; Silva, Bruno J G; Lanças, Fernando M; Queiroz, Maria Eugênia C

2011-05-27

The present work demonstrates the successful application of automated biocompatible in-tube solid-phase microextraction coupled with liquid chromatography (in-tube SPME/LC) for determination of interferon alpha(2a) (IFN α(2a)) in plasma samples for therapeutic drug monitoring. A restricted access material (RAM, protein-coated silica) was employed for preparation of a lab-made biocompatible in-tube SPME capillary that enables the direct injection of biological fluids as well as the simultaneous exclusion of macromolecules by chemical diffusion barrier and drug pre-concentration. The in-tube SPME variables, such as sample volume, draw/eject volume, number of draw-eject cycles, and desorption mode were optimized, to improve the sensitivity of the proposed method. The IFN α(2a) analyses in plasma sample were carried out within 25min (sample preparation and LC analyses). The response of the proposed method was linear over a dynamic range, from 0.06 to 3.0MIUmL(-1), with correlation coefficient equal to 0.998. The interday precision of the method presented coefficient of variation lower than 8%. The proposed automated method has adequate analytical sensitivity and selectivity for determination of IFN α(2a) in plasma samples for therapeutic drug monitoring. Copyright © 2010 Elsevier B.V. All rights reserved.

Evaluation of Carbon Nanotubes Functionalized Polydimethylsiloxane Based Coatings for In-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

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Neus Jornet-Martínez

2015-08-01

Full Text Available In the present work, the performance of carbon nanotubes (c-CNTs functionalized polydimethylsiloxane (PDMS based coatings as extractive phases for in-tube solid phase microextraction (IT-SPME coupled to Capillary LC (CapLC has been evaluated. Carboxylic-single walled carbon nanotubes (c-SWNTs and carboxylic-multi walled carbon nanotubes (c-MWNTs have been immobilized on the activated surface of PDMS capillary columns. The effect of different percentages of diphenyl groups in the PDMS extractive phase has also been evaluated. The extraction capability of the capillary columns has been tested for different organic pollutants, nitrogen heterocyclic compounds and polycyclic aromatic compounds (PAHs. The results indicated that the use of the c-CNTs-PDMS capillary columns improve pyriproxyfen and mainly PAH extraction. Triazines were better extracted by unmodified TRB-35 and modified c-CNTs-PDMSTRB-5. The results showed that the extraction capability of the c-CNT capillary columns depends not only on the polarity of the analytes (as it occurs with PDMS columns but also on the interactions that the analytes can establish with the immobilized c-CNTs on the PDMS columns. The extraction efficiency has been evaluated on the basis of the preconcentration rate that can be achieved, and, in this sense, the best c-CNTs-PDMS capillary column for each group of compounds can be proposed.

Application of the monolithic solid oxide fuel cell to space power systems

International Nuclear Information System (INIS)

Myles, K.M.; Bhattacharyya, S.K.

1991-01-01

The monolithic solid-oxide fuel cell (MSOFC) is a promising electrochemical power generation device that is currently under development at Argonne National Laboratory. The extremely high power density of the MSOFC leads to MSOFC systems that have sufficiently high energy densities that they are excellent candidates for a number of space missions. The fuel cell can also be operated in reverse, if it can be coupled to an external power source, to regenerate the fuel and oxidant from the water product. This feature further enhances the potential mission applications of the MSOFC. In this paper, the current status of the fuel cell development is presented---the focus being on fabrication and currently achievable performance. In addition, a specific example of a space power system, featuring a liquid metal cooled fast spectrum nuclear reactor and a monolithic solid oxide fuel cell, is presented to demonstrate the features of an integrated system

Application of the monolithic solid oxide fuel cell to space power systems

Science.gov (United States)

Myles, Kevin M.; Bhattacharyya, Samit K.

1991-01-01

The monolithic solid-oxide fuel cell (MSOFC) is a promising electrochemical power generation device that is currently under development at Argonne National Laboratory. The extremely high power density of the MSOFC leads to MSOFC systems that have sufficiently high energy densities that they are excellent candidates for a number of space missions. The fuel cell can also be operated in reverse, if it can be coupled to an external power source, to regenerate the fuel and oxidant from the water product. This feature further enhances the potential mission applications of the MSOFC. In this paper, the current status of the fuel cell development is presented—the focus being on fabrication and currently achievable performance. In addition, a specific example of a space power system, featuring a liquid metal cooled fast spectrum nuclear reactor and a monolithic solid oxide fuel cell, is presented to demonstrate the features of an integrated system.

Nano-Doped Monolithic Materials for Molecular Separation

Directory of Open Access Journals (Sweden)

Caleb Acquah

2017-01-01

Full Text Available Monoliths are continuous adsorbents that can easily be synthesised to possess tuneable meso-/macropores, convective fluid transport, and a plethora of chemistries for ligand immobilisation. They are grouped into three main classes: organic, inorganic, and hybrid, based on their chemical composition. These classes may also be differentiated by their unique morphological and physicochemical properties which are significantly relevant to their specific separation applications. The potential applications of monoliths for molecular separation have created the need to enhance their characteristic properties including mechanical strength, electrical conductivity, and chemical and thermal stability. An effective approach towards monolith enhancement has been the doping and/or hybridization with miniaturized molecular species of desirable functionalities and characteristics. Nanoparticles are usually preferred as dopants due to their high solid phase dispersion features which are associated with improved intermolecular adsorptive interactions. Examples of such nanomaterials include, but are not limited to, carbon-based, silica-based, gold-based, and alumina nanoparticles. The incorporation of these nanoparticles into monoliths via in situ polymerisation and/or post-modification enhances surface adsorption for activation and ligand immobilisation. Herein, insights into the performance enhancement of monoliths as chromatographic supports by nanoparticles doping are presented. In addition, the potential and characteristics of less common nanoparticle materials such as hydroxyapatite, ceria, hafnia, and germania are discussed. The advantages and challenges of nanoparticle doping of monoliths are also discussed.

Monolith electroplating process

Science.gov (United States)

Agarrwal, Rajev R.

2001-01-01

An electroplating process for preparing a monolith metal layer over a polycrystalline base metal and the plated monolith product. A monolith layer has a variable thickness of one crystal. The process is typically carried in molten salts electrolytes, such as the halide salts under an inert atmosphere at an elevated temperature, and over deposition time periods and film thickness sufficient to sinter and recrystallize completely the nucleating metal particles into one single crystal or crystals having very large grains. In the process, a close-packed film of submicron particle (20) is formed on a suitable substrate at an elevated temperature. The temperature has the significance of annealing particles as they are formed, and substrates on which the particles can populate are desirable. As the packed bed thickens, the submicron particles develop necks (21) and as they merge into each other shrinkage (22) occurs. Then as micropores also close (23) by surface tension, metal density is reached and the film consists of unstable metal grain (24) that at high enough temperature recrystallize (25) and recrystallized grains grow into an annealed single crystal over the electroplating time span. While cadmium was used in the experimental work, other soft metals may be used.

Translucency and Strength of High-Translucency Monolithic Zirconium-Oxide Materials

Science.gov (United States)

2016-05-12

Capt Todd D. Church APPROVED: Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide Materials C~t) Kraig/[ Vandewalle Date...copyrighted material in the thesis/dissertation manuscript entitled: "Translucency arid Strength of High-Translucency Monolithic Zirconium -Oxide...Translucency Monolithic Zirconium -Oxide Materials Abstract Dental materials manufacturers have developed more translucent monolithic zirconium oxide

Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Jia Xiaoyu; Han Yi; Liu Xinli [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Graduate School of Chinese Academy of Sciences, Beijing 100039 (China); Duan Taicheng, E-mail: tcduan@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Chen Hangting, E-mail: htchen@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China)

2011-01-15

The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg{sup +}) and mercury (Hg{sup 2+}) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg{sup +} and Hg{sup 2+} were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL{sup -1} for MeHg{sup +} and 0.0014 ng mL{sup -1} for Hg{sup 2+}, respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL{sup -1} MeHg{sup +} and Hg{sup 2+} were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

Selective oxidation of cyclohexene through gold functionalized silica monolith microreactors

Science.gov (United States)

Alotaibi, Mohammed T.; Taylor, Martin J.; Liu, Dan; Beaumont, Simon K.; Kyriakou, Georgios

2016-04-01

Two simple, reproducible methods of preparing evenly distributed Au nanoparticle containing mesoporous silica monoliths are investigated. These Au nanoparticle containing monoliths are subsequently investigated as flow reactors for the selective oxidation of cyclohexene. In the first strategy, the silica monolith was directly impregnated with Au nanoparticles during the formation of the monolith. The second approach was to pre-functionalize the monolith with thiol groups tethered within the silica mesostructure. These can act as evenly distributed anchors for the Au nanoparticles to be incorporated by flowing a Au nanoparticle solution through the thiol functionalized monolith. Both methods led to successfully achieving even distribution of Au nanoparticles along the length of the monolith as demonstrated by ICP-OES. However, the impregnation method led to strong agglomeration of the Au nanoparticles during subsequent heating steps while the thiol anchoring procedure maintained the nanoparticles in the range of 6.8 ± 1.4 nm. Both Au nanoparticle containing monoliths as well as samples with no Au incorporated were tested for the selective oxidation of cyclohexene under constant flow at 30 °C. The Au free materials were found to be catalytically inactive with Au being the minimum necessary requirement for the reaction to proceed. The impregnated Au-containing monolith was found to be less active than the thiol functionalized Au-containing material, attributable to the low metal surface area of the Au nanoparticles. The reaction on the thiol functionalized Au-containing monolith was found to depend strongly on the type of oxidant used: tert-butyl hydroperoxide (TBHP) was more active than H2O2, likely due to the thiol induced hydrophobicity in the monolith.

Quantitative analysis of 2-furfural and 5-methylfurfural in different Italian vinegars by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry using isotope dilution.

Science.gov (United States)

Giordano, Lucia; Calabrese, Roberto; Davoli, Enrico; Rotilio, Domenico

2003-10-31

A new method was developed for the determination of 2-furfural (2-F) and 5-methylfurfural (5-MF), two products of Maillard reaction in vinegar, with head-space solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). A divinylbenzene (DVB)/carboxen (CAR)/polydimethylsiloxane (PDMS) fibre was used and SPME conditions were optimised, studying ionic strength effect, temperature effect and adsorption time. Both analytes were determined by calibration established on 2-furfural-d4 (2-F-d4). The method showed good linearity in the range studied (from 16 to 0.12 mg/l), with a regression coefficient r2 of 0.9999. Inter-batch precision and accuracy were found between 14.9 and 6.0% and between -11.7 and 0.2%, respectively. Detection limit was 15 microg/l. The method is simple and accurate and it has been applied to a series of balsamic and non-balsamic vinegars.

Preparation of polyhedral oligomeric silsesquioxane based imprinted monolith.

Science.gov (United States)

Li, Fang; Chen, Xiu-Xiu; Huang, Yan-Ping; Liu, Zhao-Sheng

2015-12-18

Polyhedral oligomeric silsesquioxane (POSS) was successfully applied, for the first time, to prepare imprinted monolithic column with high porosity and good permeability. The imprinted monolithic column was synthesized with a mixture of PSS-(1-Propylmethacrylate)-heptaisobutyl substituted (MA 0702), naproxon (template), 4-vinylpyridine, and ethylene glycol dimethacrylate, in ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4). The influence of synthesis parameters on the retention factor and imprinting effect, including the amount of MA 0702, the ratio of template to monomer, and the ratio of monomer to crosslinker, was investigated. The greatest imprinting factor on the imprinted monolithic column prepared with MA 0702 was 22, about 10 times higher than that prepared in absence of POSS. The comparisons between MIP monoliths synthesized with POSS and without POSS were made in terms of permeability, column efficiency, surface morphology and pore size distribution. In addition, thermodynamic and Van Deemter analysis were used to evaluate the POSS-based MIP monolith. Copyright © 2015 Elsevier B.V. All rights reserved.

[Determination of nitroaromatics and cyclo ketones in sea water' by gas chromatography coupled with activated carbon fiber solid-phase micro-extraction].

Science.gov (United States)

Ma, Hanna; Zhu, Mengya; Wang, Yalin; Sun, Tonghua; Jia, Jinping

2009-05-01

A gas chromatography (GC) coupled with solid-phase micro-extraction using a special activated carbon fiber (ACF) was developed for the analysis of 6 nitroaromatics and cyclic ketones, nitrobenzene (NB), 1,3-dinitrobenzene (1,3-DNB), 2,4-dinitrotoluene (2,4-DNT), 2,6-dinitrotoluene (2,6-DNT), isophorone, 1,4-naphthaquinone (1,4-NPQ), in sea water samples. The sample was extracted for 30 min under saturation of NaCl at 1,500 r/min and 60 degrees C in head space. The desorption was performance at 280 degrees C for 2 min. The linear ranges were from 0.01 to 400 microg/L. The limits of detection (LODs) were 1.4 - 3.2 ng/L. This method has been successfully applied to the determination of nitroaromatics and cyclic ketones in the sea water samples obtained from East China Sea. The concentrations of nitrobenzene, 1,3-dinitrobenzene and 2,6-dinitrotoluene in the sea water sample were 0.756, 0.944, 0.890 microg/L, respectively. The recoveries were 86.3% - 101.8% with the relative standard deviations (RSDs) of 3.7% -7.8%. The method is suitable for analyzing nitroaromatics and cyclic ketones at low concentration levels in sea water samples.

Monolithic Ytterbium All-single-mode Fiber Laser with Direct Fiber-end Delivery of nJ-level Femtosecond Pulses

DEFF Research Database (Denmark)

Turchinovich, Dmitry

2008-01-01

We demonstrate a monolithic, i.e. without any free-space coupling, all-single-mode passively modelocked Yb-fiber laser, with direct fiber-end delivery of 364−405 fs pulses of 4 nJ pulse energy using a low-loss hollow-core photonic crystal fiber compression....

Protective Skins for Aerogel Monoliths

Science.gov (United States)

Leventis, Nicholas; Johnston, James C.; Kuczmarski, Maria A.; Meador, Ann B.

2007-01-01

A method of imparting relatively hard protective outer skins to aerogel monoliths has been developed. Even more than aerogel beads, aerogel monoliths are attractive as thermal-insulation materials, but the commercial utilization of aerogel monoliths in thermal-insulation panels has been inhibited by their fragility and the consequent difficulty of handling them. Therefore, there is a need to afford sufficient protection to aerogel monoliths to facilitate handling, without compromising the attractive bulk properties (low density, high porosity, low thermal conductivity, high surface area, and low permittivity) of aerogel materials. The present method was devised to satisfy this need. The essence of the present method is to coat an aerogel monolith with an outer polymeric skin, by painting or spraying. Apparently, the reason spraying and painting were not attempted until now is that it is well known in the aerogel industry that aerogels collapse in contact with liquids. In the present method, one prevents such collapse through the proper choice of coating liquid and process conditions: In particular, one uses a viscous polymer precursor liquid and (a) carefully controls the amount of liquid applied and/or (b) causes the liquid to become cured to the desired hard polymeric layer rapidly enough that there is not sufficient time for the liquid to percolate into the aerogel bulk. The method has been demonstrated by use of isocyanates, which, upon exposure to atmospheric moisture, become cured to polyurethane/polyurea-type coats. The method has also been demonstrated by use of commercial epoxy resins. The method could also be implemented by use of a variety of other resins, including polyimide precursors (for forming high-temperature-resistant protective skins) or perfluorinated monomers (for forming coats that impart hydrophobicity and some increase in strength).

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

Directory of Open Access Journals (Sweden)

Helena Prosen

2014-05-01

Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

Science.gov (United States)

Prosen, Helena

2014-05-23

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

Directory of Open Access Journals (Sweden)

Rada Đurović

2011-01-01

Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

Gas flow headspace liquid phase microextraction.

Science.gov (United States)

Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

2009-11-06

There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

Radio frequency regenerative oscillations in monolithic high-Q/V heterostructured photonic crystal cavities

International Nuclear Information System (INIS)

Yang, Jinghui; Gu, Tingyi; Zheng, Jiangjun; Wei Wong, Chee; Yu, Mingbin; Lo, Guo-Qiang; Kwong, Dim-Lee

2014-01-01

We report temporal and spectral domain observation of regenerative oscillation in monolithic silicon heterostructured photonic crystals cavities with high quality factor to mode volume ratios (Q/V). The results are interpreted by nonlinear coupled mode theory (CMT) tracking the dynamics of photon, free carrier population, and temperature variations. We experimentally demonstrate effective tuning of the radio frequency tones by laser-cavity detuning and laser power levels, confirmed by the CMT simulations with sensitive input parameters

Advanced Gasification Mercury/Trace Metal Control with Monolith Traps

Energy Technology Data Exchange (ETDEWEB)

Musich, Mark; Swanson, Michael; Dunham, Grant; Stanislowski, Joshua

2010-10-05

Two Corning monoliths and a non-carbon-based material have been identified as potential additives for mercury capture in syngas at temperatures above 400°F and pressure of 600 psig. A new Corning monolith formulation, GR-F1-2189, described as an active sample appeared to be the best monolith tested to date. The Corning SR Liquid monolith concept continues to be a strong candidate for mercury capture. Both monolith types allowed mercury reduction to below 5-μg/m{sup 3} (~5 ppb), a current U.S. Department of Energy (DOE) goal for trace metal control. Preparation methods for formulating the SR Liquid monolith impacted the ability of the monolith to capture mercury. The Energy & Environmental Research Center (EERC)-prepared Noncarbon Sorbents 1 and 2 appeared to offer potential for sustained and significant reduction of mercury concentration in the simulated fuel gas. The Noncarbon Sorbent 1 allowed sustained mercury reduction to below 5-μg/m{sup 3} (~5 ppb). The non-carbon-based sorbent appeared to offer the potential for regeneration, that is, desorption of mercury by temperature swing (using nitrogen and steam at temperatures above where adsorption takes place). A Corning cordierite monolith treated with a Group IB metal offered limited potential as a mercury sorbent. However, a Corning carbon-based monolith containing prereduced metallic species similar to those found on the noncarbon sorbents did not exhibit significant or sustained mercury reduction. EERC sorbents prepared with Group IB and IIB selenide appeared to have some promise for mercury capture. Unfortunately, these sorbents also released Se, as was evidenced by the measurement of H2Se in the effluent gas. All sorbents tested with arsine or hydrogen selenide, including Corning monoliths and the Group IB and IIB metal-based materials, showed an ability to capture arsine or hydrogen selenide at 400°F and 600 psig. Based on current testing, the noncarbon metal-based sorbents appear to be the most

ADVANCED GASIFICATION MERCURY/TRACE METAL CONTROL WITH MONOLITH TRAPS

Energy Technology Data Exchange (ETDEWEB)

Mark A. Musich; Michael L. Swanson; Grant E. Dunham; Joshua J. Stanislowski

2010-07-31

Two Corning monoliths and a non-carbon-based material have been identified as potential additives for mercury capture in syngas at temperatures above 400°F and pressure of 600 psig. A new Corning monolith formulation, GR-F1-2189, described as an active sample appeared to be the best monolith tested to date. The Corning SR Liquid monolith concept continues to be a strong candidate for mercury capture. Both monolith types allowed mercury reduction to below 5-μg/m3 (~5 ppb), a current U.S. Department of Energy (DOE) goal for trace metal control. Preparation methods for formulating the SR Liquid monolith impacted the ability of the monolith to capture mercury. The Energy & Environmental Research Center (EERC)-prepared Noncarbon Sorbents 1 and 2 appeared to offer potential for sustained and significant reduction of mercury concentration in the simulated fuel gas. The Noncarbon Sorbent 1 allowed sustained mercury reduction to below 5-μg/m3 (~5 ppb). The non-carbon-based sorbent appeared to offer the potential for regeneration, that is, desorption of mercury by temperature swing (using nitrogen and steam at temperatures above where adsorption takes place). A Corning cordierite monolith treated with a Group IB metal offered limited potential as a mercury sorbent. However, a Corning carbon-based monolith containing prereduced metallic species similar to those found on the noncarbon sorbents did not exhibit significant or sustained mercury reduction. EERC sorbents prepared with Group IB and IIB selenide appeared to have some promise for mercury capture. Unfortunately, these sorbents also released Se, as was evidenced by the measurement of H2Se in the effluent gas. All sorbents tested with arsine or hydrogen selenide, including Corning monoliths and the Group IB and IIB metal-based materials, showed an ability to capture arsine or hydrogen selenide at 400°F and 600 psig. Based on current testing, the noncarbon metal-based sorbents appear to be the most effective arsine

[Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction].

Science.gov (United States)

Liu, Jingke; Zhang, Aixia; Li, Shaohui; Zhao, Wei; Zhang, Yuzong; Xing, Guosheng

2017-11-08

To comprehensively understand flavor compounds and aroma characteristics of foxtail millet wine, extraction conditions were optimized with 85 μm polyacrylate (PA), 100 μm polydimethylsiloxane (PDMS), 75 μm carboxen (CAR)/PDMS and 50/30 μm divinylbenzene (DVB)/CAR/PDMS fibers. The flavor compounds in foxtail millet wine were investigated by gas chromatography-mass spectrometry (GC-MS) coupled with headspace solid phase microextraction (HS-SPME), and the odor characteristics and intensity were analyzed by odor active values (OAVs). The samples of 8 mL were placed in headspace vials with 1.5 g NaCl, then the headspace vials were heated at 60℃ for 40 min. Using HS-SPME with different fibers, a total of 55 flavor compounds were identified from the samples, including alcohols, esters, benzene derivatives, hydrocarbons, acids, aldehydes, ketones, terpenes, phenols and heterocycle compounds. The main flavor compounds were alcohols compounds. According to their OAVs, phenylethyl alcohol, styrene, 1-methyl-naphthalene, 2-methyl-naphthalene, benzaldehyde, benzeneacetaldehyde and 2-methoxy-phenol were established to be odor-active compounds. Phenylethyl alcohol and benzeneacetaldehyde were the most prominent odor-active compounds. PA and PDMS fibers had good extraction effect for polar and nonpolar compounds, respectively. CAR/PDMS and DVB/CAR/PDMS provided a similar compounds profile for moderate polar compounds. This research comprehensively determined flavor compounds of foxtail millet wine, and provided theoretical basis for product development and quality control.

Determination of phthalic acid esters in Chinese white spirit using dispersive liquid-liquid microextraction coupled with sweeping β-cyclodextrin-modified micellar electrokinetic chromatography.

Science.gov (United States)

Sun, Jianzhi; He, Hui; Liu, Shuhui

2014-07-01

A simple method that consumes low organic solvent is proposed for the analysis of phthalic acid esters in Chinese white spirit using dispersive liquid-liquid microextraction coupled with sweeping-micellar electrokinetic chromatography. Tetrachloromethane and white-spirit-containing ethanol were used as the extraction and dispersing solvents, respectively. The electrophoresis separation buffer was composed of 5 mM β-cyclodextrin, 50 mM sodium dodecyl sulfate and 25 mM borate buffer (pH 9.2) with 9% acetonitrile, enabling the baseline resolution of the analytes within 13 min. Under the optimum conditions, satisfactory linearities (5-1000 ng/mL, r ≥ 0.9909), good reproducibility (RSD ≤ 6.7% for peak area, and RSD ≤ 2.8% for migration time), low detection limits (0.4-0.8 ng/mL) and acceptable recovery rates (89.6-105.7%) were obtained. The proposed method was successfully applied to 22 Chinese white spirits, and the content of dibutyl phthalate in 55% of the samples exceeded the Specific Migration Limit of 0.3 mg/kg established by the domestic and international regulations. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dispersive liquid-liquid microextraction for simultaneous determination of cadmium, cobalt, lead and nickel in water samples by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Dos Santos Silva, E.; Correia, L.O.; Dos Santos, L.O.; Dos Santos Vieira, E.V.; Lemos, V.A.

2012-01-01

We report on a new method for the dispersive liquid-liquid microextraction of Cd(II), Co(II), Pb(II) and Ni (II) from water samples prior to their simultaneous determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on the injection of a ternary solvent system composed of appropriate quantities of extraction solvent (trichloroethylene), dispersive solvent (ethanol), and the chelating reagent 2-(2'-benzothiazolylazo)-p-cresol into the sample solution. The solution turns turbid immediately after injection, and the analytes are extracted into the droplets of the organic phase which was dried and dissolved in a mixture of Triton X-114, nitric acid, and ethanol. The metal ions in this mixture were quantified by ICP-OES. The detection limits under optimized conditions are 0.2, 0.3, 0.2 and 0.7 μg L -1 for Cd(II), Co(II), Pb(II) and Ni(II), respectively. The enrichment factors were also calculated for Cd (13), Co (11), Pb (11) and Ni (8). The procedure was applied to the determination of cadmium, cobalt, lead and nickel in certified reference material (waterway sediment) and water samples. (author)

Fast and robust direct immersion solid phase microextraction coupled with gas chromatography-time-of-flight mass spectrometry method employing a matrix compatible fiber for determination of triazole fungicides in fruits.

Science.gov (United States)

Silva, Érica A Souza; Lopez-Avila, Viorica; Pawliszyn, Janusz

2013-10-25

A fast and robust method was developed for the determination of ten triazole fungicides in fruit samples using direct immersion solid-phase microextraction coupled to gas chromatography with time-of-flight mass spectrometry detection (DI-SPME-GC-ToFMS). In this work, a newly developed concept of solid-phase microextraction (SPME) sorbent, which allows for direct immersion extraction in complex food matrices, has been applied in the analysis of 10 triazole fungicides in grapes and strawberries pulps. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction temperature, sample pH, and ionic strength, agitation speed, extraction and desorption times. Under optimized conditions, the method was linear for over 4 orders of magnitude in concentration, with linear regression coefficients (R(2)) greater than 0.99 for all test compounds in both matrices. Method reproducibility, as determined by analysis of spiked grapes and strawberries, was better than ±20%. The limits of quantitation objective (LOQs) ranged from 0.25 to 5 ng g(-1) for both matrices, well below the maximum residues levels allowed for those compounds in both matrices. The method was successfully applied in the analysis of commercial samples of grapes and strawberries. Finally, the new SPME method was compared to a modified version of t QuEChERS AOAC method: the limits of quantitation reached by SPME were at least one order of magnitude lower than those achieved by the QuEChERS method, whereas precision and accuracy were comparable for both methods. Copyright © 2013 Elsevier B.V. All rights reserved.

Dopamine-imprinted monolithic column for capillary electrochromatography.

Science.gov (United States)

Aşır, Süleyman; Sarı, Duygu; Derazshamshir, Ali; Yılmaz, Fatma; Şarkaya, Koray; Denizli, Adil

2017-11-01

A dopamine-imprinted monolithic column was prepared and used in capillary electrochromatography as stationary phase for the first time. Dopamine was selectively separated from aqueous solution containing the competitor molecule norepinephrine, which is similar in size and shape to the template molecule. Morphology of the dopamine-imprinted column was observed by scanning electron microscopy. The influence of the organic solvent content of mobile phase, applied pressure and pH of the mobile phase on the recognition of dopamine by the imprinted monolithic column has been evaluated, and the imprinting effect in the dopamine-imprinted monolithic polymer was verified. Developed dopamine-imprinted monolithic column resulted in excellent separation of dopamine from structurally related competitor molecule, norepinephrine. Separation was achieved in a short period of 10 min, with the electrophoretic mobility of 5.81 × 10 -5  m 2 V -1 s -1 at pH 5.0 and 500 mbar pressure. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

Science.gov (United States)

Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

2013-03-01

Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Distributed coupling high efficiency linear accelerator

Science.gov (United States)

Tantawi, Sami G.; Neilson, Jeffrey

2016-07-19

A microwave circuit for a linear accelerator includes multiple monolithic metallic cell plates stacked upon each other so that the beam axis passes vertically through a central acceleration cavity of each plate. Each plate has a directional coupler with coupling arms. A first coupling slot couples the directional coupler to an adjacent directional coupler of an adjacent cell plate, and a second coupling slot couples the directional coupler to the central acceleration cavity. Each directional coupler also has an iris protrusion spaced from corners joining the arms, a convex rounded corner at a first corner joining the arms, and a corner protrusion at a second corner joining the arms.

Pilot tests of a PET detector using the TOF-PET ASIC based on monolithic crystals and SiPMs

International Nuclear Information System (INIS)

Aguilar, A.; González-Montoro, A.; González, A.J.; Hernández, L.; Monzó, J.M.; Benlloch, J.M.; Bugalho, R.; Ferramacho, L.

2016-01-01

In this work we show pilot tests of PET detector blocks using the TOF-PET ASIC, coupled to SiPM detector arrays and different crystal configurations. We have characterized the main ASIC features running calibration processes to compensate the time dispersion among the different ASIC/SiPM paths as well as for the time walk on the arrival of optical photons. The aim of this work is to use of LYSO monolithic crystals and explore their photon Depth of Interaction (DOI) capabilities, keeping good energy and spatial resolutions. First tests have been carried out with crystal arrays. Here we made it possible to reach a coincidence resolving times (CRT) of 370 ps FWHM, with energy resolutions better than 20% and resolving well 2 mm sized crystal elements. When using monolithic crystals, a single-pixel LYSO reference crystal helped to explore the CRT performance. We studied different strategies to provide the best timestamp determination in the monolithic scintillator. Times around 1 ns FWHM have been achieved in these pilot studies. In terms of spatial and energy resolution, values of about 3 mm and better than 30% were found, respectively. We have also demonstrated the capability of this system (monolithic and ASIC) to return accurate DOI information.

Biomimetic small peptide functionalized affinity monoliths for monoclonal antibody purification.

Science.gov (United States)

Wang, Xiangyu; Xia, Donghai; Han, Hai; Peng, Kun; Zhu, Peijie; Crommen, Jacques; Wang, Qiqin; Jiang, Zhengjin

2018-08-09

The rapid development of monoclonal antibodies (mAbs) in therapeutic and diagnostic applications has necessitated the advancement of mAbs purification technologies. In this study, a biomimetic small peptide ligand 3,5-di-tert-butyl-4-hydroxybenzoic acid-Arg-Arg-Gly (DAAG) functionalized monolith was fabricated through a metal ion chelation-based multi-step approach. The resulting monolith showed good chromatographic performance. Compared with the Ni 2+ based IMAC monolith, the DAAG functionalized monolith exhibited not only excellent specificity but also higher dynamic binding capacity (DBC). The 10% DBC and 50% DBC for hIgG reached as high values as 26.0 and 34.6 mg/mL, respectively, at a ligand density of 8.8 μmol/mL, due to the high porosity and accessibility of the monolithic matrix. Moreover, the stability of the DAAG functionalized monolith in successive breakthrough experiments indicates that it has a promising potential for long-term use in mAbs purification. Finally, the DAAG functionalized monolith was successfully applied to the purification of trastuzumab or human immunoglobulin G (hIgG) from biological samples. Copyright © 2018 Elsevier B.V. All rights reserved.

The use of solid phase microextraction as sample preparation technique for determination of n-nitrosodimethylamine in water polluted by hydrazine-based rocket fuel

Directory of Open Access Journals (Sweden)

Bulat Kenessov

2009-05-01

Full Text Available A paper describes a method for determination of N-nitrosodimethylamine in water, polluted by spills of 1,1-dimethylhydrazine, based on solid phase microextraction coupled to gas chromatography/mass spectrometry. A method detection limit was determined to be 1 ug/kg, relative error was below 20%. A method is very sensitive and selective as well as quite simple, relatively cheap and fully automated.

Monolithic Active Pixel Matrix with Binary Counters (MAMBO) ASIC

International Nuclear Information System (INIS)

Khalid, Farah F.; Deptuch, Grzegorz; Shenai, Alpana; Yarema, Raymond J.

2010-01-01

Monolithic Active Matrix with Binary Counters (MAMBO) is a counting ASIC designed for detecting and measuring low energy X-rays from 6-12 keV. Each pixel contains analogue functionality implemented with a charge preamplifier, CR-RC 2 shaper and a baseline restorer. It also contains a window comparator which can be trimmed by 4 bit DACs to remove systematic offsets. The hits are registered by a 12 bit ripple counter which is reconfigured as a shift register to serially output the data from the entire ASIC. Each pixel can be tested individually. Two diverse approaches have been used to prevent coupling between the detector and electronics in MAMBO III and MAMBO IV. MAMBO III is a 3D ASIC, the bottom ASIC consists of diodes which are connected to the top ASIC using μ-bump bonds. The detector is decoupled from the electronics by physically separating them on two tiers and using several metal layers as a shield. MAMBO IV is a monolithic structure which uses a nested well approach to isolate the detector from the electronics. The ASICs are being fabricated using the SOI 0.2 (micro)m OKI process, MAMBO III is 3D bonded at T-Micro and MAMBO IV nested well structure was developed in collaboration between OKI and Fermilab.

Development of a new green non-dispersive ionic liquid microextraction method in a narrow glass column for determination of cadmium prior to couple with graphite furnace atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Naeemullah, E-mail: naeemullah433@yahoo.com [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Kazi, Tasneem Gul [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Tuzen, Mustafa [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Shah, Faheem; Afridi, Hassan Imran [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Citak, Demirhan [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey)

2014-02-17

Graphical abstract: -- Highlights: •A novel and rapid non-dispersive ionic liquid based microextractions. •We used a long narrow glass column to provide more contact area between two media (aqueous and extractive). •APDC using as complexing agent and analyzed by GFAAS. •Introduced a novel approach that reduced solvent consumption, effort, time. •It was applied for determination of understudy analytes in real water sample. -- Abstract: Easy and innovative non-dispersive ionic liquid based microextraction (NDILME) has been developed for preconcentration of trace level of cadmium (Cd) in aqueous real surface water samples prior to couple with graphite furnace atomic absorption spectrometry (GFAAS). A 200 cm long narrow glass column containing aqueous solution of standard/sample was used to increase phase transfer ratio by providing more contact area between two medium (aqueous and extractive), which drastically improve the recoveries of labile hydrophobic chelate of Cd ammonium pyrrolidinedithiocarbamate (APDC), into ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [C{sub 4}mim][PF{sub 6}]. Different aspect of the desire method have been investigated and optimized. Under the optimized key experimental variables, limit of detection (LOD) and enhancement factor (EF) were achieved to be 0.5 ng L{sup −1} and 150, respectively. Reliability of the model method was checked by relative standard deviation (%RSD), which was found to be < 5%. Validity and accuracy of the developed method was checked by analysis of certified reference water samples (SLRS-4 Riverine water) using standard addition method. Application of the model method was productively performed by analysis of Cd in real surface water samples (tap and sea)

Mechanical design of a single-axis monolithic accelerometer for advanced seismic attenuation systems

Energy Technology Data Exchange (ETDEWEB)

Bertolini, Alessandro [Dipartimento di Fisica dell' Universita di Pisa and INFM, Largo Pontecorvo 2, I-56127 Pisa (Italy) and LIGO Project, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States)]. E-mail: alessandro.bertolini@desy.de; DeSalvo, Riccardo [LIGO Project, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Fidecaro, Francesco [Dipartimento di Fisica dell' Universita di Pisa and INFM, Largo Pontecorvo 2, I-56127 Pisa (Italy); Francesconi, Mario [Dipartimento di Fisica dell' Universita di Pisa and INFM, Largo Pontecorvo 2, I-56127 Pisa (Italy); Marka, Szabolcs [Department of Physics, Columbia University, 538 W. 120th St., New York, NY 10027 (United States); Sannibale, Virginio [LIGO Project, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Simonetti, Duccio [Dipartimento di Fisica dell' Universita di Pisa and INFM, Largo Pontecorvo 2, I-56127 Pisa (Italy); Takamori, Akiteru [LIGO Project, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Earthquake Research Institute, University of Tokyo, 1-1-1 Yayoi, Bunkyo-Ku, Tokyo 113-0032 (Japan); Tariq, Hareem [LIGO Project, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States)

2006-01-15

The design and mechanics for a new very-low noise low frequency horizontal accelerometer is presented. The sensor has been designed to be integrated in an advanced seismic isolation system for interferometric gravitational wave detectors. The motion of a small monolithic folded-pendulum (FP) is monitored by a high resolution capacitance displacement sensor; a feedback force actuator keeps the mass at the equilibrium position. The feedback signal is proportional to the ground acceleration in the frequency range 0-150Hz. The very high mechanical quality factor, Q{approx}3000 at a resonant frequency of 0.5Hz, reduces the Brownian motion of the proof mass of the accelerometer below the resolution of the displacement sensor. This scheme enables the accelerometer to detect the inertial displacement of a platform with a root-mean-square noise less than 1nm, integrated over the frequency band from 0.01 to 150Hz. The FP geometry, combined with the monolithic design, allows the accelerometer to be extremely directional. A vertical-horizontal coupling ranging better than 10{sup -3} has been achieved. A detailed account of the design and construction of the accelerometer is reported here. The instrument is fully ultra-high vacuum compatible and has been tested and approved for integration in seismic attenuation system of japanese TAMA 300 gravitational wave detector. The monolithic design also makes the accelerometer suitable for cryogenic operation.

Three-phase hollow-fiber liquid-phase microextraction combined with HPLC-UV for the determination of isothiazolinone biocides in adhesives used for food packaging materials.

Science.gov (United States)

Rosero-Moreano, Milton; Canellas, Elena; Nerín, Cristina

2014-02-01

The present study deals with the development of a liquid microextraction procedure for enhancing the sensitivity of the determination of 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one in adhesives. The procedure involves a three-phase hollow-fiber liquid-phase microextraction using a semipermeable polypropylene membrane, which contained 1-octanol as the organic phase in the pores of the membrane. The donor and acceptor phases are aqueous acidic and alkaline media, respectively, and the final liquid phase (acceptor) is analyzed by HPLC coupled with diode array detection. The most appropriate conditions were extraction time 20 min, stirring speed 1400 rpm, extraction temperature 50°C. The quantification limits of the method were 0.123 and 0.490 μg/g for 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one, respectively. Three different adhesive samples were successfully analyzed. The procedure was compared to direct analysis using ultra high pressure liquid chromatography coupled with TOF-MS, where the identification of the compounds and the quantification values were confirmed. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extensible automated dispersive liquid–liquid microextraction

Energy Technology Data Exchange (ETDEWEB)

Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang, E-mail: hxgao@cau.edu.cn

2015-05-04

Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C{sub 8}MIM]NTf{sub 2}) is formed through the reaction between [C{sub 8}MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf{sub 2}) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL{sup −1}. The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL{sup −1}. The proposed

Extensible automated dispersive liquid–liquid microextraction

International Nuclear Information System (INIS)

Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang

2015-01-01

Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C 8 MIM]NTf 2 ) is formed through the reaction between [C 8 MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf 2 ) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL −1 . The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL −1 . The proposed method opens a new avenue

Aspartic acid incorporated monolithic columns for affinity glycoprotein purification.

Science.gov (United States)

Armutcu, Canan; Bereli, Nilay; Bayram, Engin; Uzun, Lokman; Say, Rıdvan; Denizli, Adil

2014-02-01

Novel aspartic acid incorporated monolithic columns were prepared to efficiently affinity purify immunoglobulin G (IgG) from human plasma. The monolithic columns were synthesised in a stainless steel HPLC column (20 cm × 5 mm id) by in situ bulk polymerisation of N-methacryloyl-L-aspartic acid (MAAsp), a polymerisable derivative of L-aspartic acid, and 2-hydroxyethyl methacrylate (HEMA). Monolithic columns [poly(2-hydroxyethyl methacrylate-N-methacryloyl-L-aspartic acid) (PHEMAsp)] were characterised by swelling studies, Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The monolithic columns were used for IgG adsorption/desorption from aqueous solutions and human plasma. The IgG adsorption depended on the buffer type, and the maximum IgG adsorption from aqueous solution in phosphate buffer was 0.085 mg/g at pH 6.0. The monolithic columns allowed for one-step IgG purification with a negligible capacity decrease after ten adsorption-desorption cycles. Copyright © 2013 Elsevier B.V. All rights reserved.

Fire resistance of prefabricated monolithic slab

Directory of Open Access Journals (Sweden)

Gravit Marina

2017-01-01

Full Text Available A prefabricated monolithic slab (PMS has a number of valuable advantages, they allow to significantly decrease the weight of construction keeping the necessary structural-load capacity, to speed up and cheapen work conduction, to increase the heat isolating properties of an enclosure structure [1]. In order to create a design method of prefabricated monolithic slab fire-resistance, it's necessary to perform a series of PMS testing, one of which is being described in this article. Subjected to the test is a fragment of prefabricated monolithic slab with polystyrene concrete inserts along the beams with bent metal profile 250 mm thick, with a 2.7 m span loaded with evenly spread load equal to 600 kg/m2. After 3 hour testing for fire-resistance [2] no signs of construction ultimate behavior were detected.

Extended Leach Testing of Simulated LAW Cast Stone Monoliths

Energy Technology Data Exchange (ETDEWEB)

Serne, R. Jeffrey [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Westsik, Joseph H. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Williams, Benjamin D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Jung, H. B. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Wang, Guohui [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2015-07-09

This report describes the results from long-term laboratory leach tests performed at Pacific Northwest National Laboratory (PNNL) for Washington River Protection Solutions (WRPS) to evaluate the release of key constituents from monoliths of Cast Stone prepared with four simulated low-activity waste (LAW) liquid waste streams. Specific objectives of the Cast Stone long-term leach tests described in this report focused on four activities: 1. Extending the leaching times for selected ongoing EPA-1315 tests on monoliths made with LAW simulants beyond the conventional 63-day time period up to 609 days reported herein (with some tests continuing that will be documented later) in an effort to evaluate long-term leaching properties of Cast Stone to support future performance assessment activities. 2. Starting new EPA-1315 leach tests on archived Cast Stone monoliths made with four LAW simulants using two leachants (deionized water [DIW] and simulated Hanford Integrated Disposal Facility (IDF) Site vadose zone pore water [VZP]). 3. Evaluating the impacts of varying the iodide loading (starting iodide concentrations) in one LAW simulant (7.8 M Na Hanford Tank Waste Operations Simulator (HTWOS) Average) by manufacturing new Cast Stone monoliths and repeating the EPA-1315 leach tests using DIW and the VZP leachants. 4. Evaluating the impacts of using a non-pertechnetate form of Tc that is present in some Hanford tanks. In this activity one LAW simulant (7.8 M Na HTWOS Average) was spiked with a Tc(I)-tricarbonyl gluconate species and then solidified into Cast Stone monoliths. Cured monoliths were leached using the EPA-1315 leach protocol with DIW and VZP. The leach results for the Tc-Gluconate Cast Stone monoliths were compared to Cast Stone monoliths pertechnetate.

Development of high-throughput analysis system using highly-functional organic polymer monoliths

International Nuclear Information System (INIS)

Umemura, Tomonari; Kojima, Norihisa; Ueki, Yuji

2008-01-01

The growing demand for high-throughput analysis in the current competitive life sciences and industries has promoted the development of high-speed HPLC techniques and tools. As one of such tools, monolithic columns have attracted increasing attention and interest in the last decade due to the low flow-resistance and excellent mass transfer, allowing for rapid separations and reactions at high flow rates with minimal loss of column efficiency. Monolithic materials are classified into two main groups: silica- and organic polymer-based monoliths, each with their own advantages and disadvantages. Organic polymer monoliths have several distinct advantages in life-science research, including wide pH stability, less irreversible adsorption, facile preparation and modification. Thus, we have so far tried to develop organic polymer monoliths for various chemical operations, such as separation, extraction, preconcentration, and reaction. In the present paper, recent progress in the development of organic polymer monoliths is discussed. Especially, the procedure for the preparation of methacrylate-based monoliths with various functional groups is described, where the influence of different compositional and processing parameters on the monolithic structure is also addressed. Furthermore, the performance of the produced monoliths is demonstrated through the results for (1) rapid separations of alklybenzenes at high flow rates, (2) flow-through enzymatic digestion of cytochrome c on a trypsin-immobilized monolithic column, and (3) separation of the tryptic digest on a reversed-phase monolithic column. The flexibility and versatility of organic polymer monoliths will be beneficial for further enhancing analytical performance, and will open the way for new applications and opportunities both in scientific and industrial research. (author)

Influence of different carbon monolith preparation parameters on pesticide adsorption

Directory of Open Access Journals (Sweden)

Vukčević Marija

2013-01-01

Full Text Available The capacity of carbon monolith for pesticide removal from water, and the mechanism of pesticide interaction with carbon surface were examined. Different carbon monolith samples were obtained by varying the carbonization and activation parameters. In order to examine the role of surface oxygen groups in pesticide adsorption, carbon monolith surface was functionalized by chemical treatment in HNO3, H2O2 and KOH. The surface properties of the obtained samples were investigated by BET surface area, pore size distribution and temperature-programmed desorption. Adsorption of pesticides from aqueous solution onto activated carbon monolith samples was studied by using five pesticides belonging to different chemical groups (acetamiprid, dimethoate, nicosulfuron, carbofuran and atrazine. Presented results show that higher temperature of carbonization and the amount of activating agent allow obtaining microporous carbon monolith with higher amount of surface functional groups. Adsorption properties of the activated carbon monolith were more readily affected by the amount of the surface functional groups than by specific surface area. Results obtained by carbon monolith functionalisation showed that π-π interactions were the main force for adsorption of pesticides with aromatic structure, while acidic groups play an important role in adsorption of pesticides with no aromatic ring in the chemical structure.

A poly(vinyl alcohol)/sodium alginate blend monolith with nanoscale porous structure.

Science.gov (United States)

Sun, Xiaoxia; Uyama, Hiroshi

2013-10-04

A stimuli-responsive poly(vinyl alcohol) (PVA)/sodium alginate (SA) blend monolith with nanoscale porous (mesoporous) structure is successfully fabricated by thermally impacted non-solvent induced phase separation (TINIPS) method. The PVA/SA blend monolith with different SA contents is conveniently fabricated in an aqueous methanol without any templates. The solvent suitable for the fabrication of the present blend monolith by TINIPS is different with that of the PVA monolith. The nanostructural control of the blend monolith is readily achieved by optimizing the fabrication conditions. Brunauer Emmett Teller measurement shows that the obtained blend monolith has a large surface area. Pore size distribution plot for the blend monolith obtained by the non-local density functional theory method reveals the existence of the nanoscale porous structure. Fourier transform infrared analysis reveals the strong interactions between PVA and SA. The pH-responsive property of the blend monolith is investigated on the basis of swelling ratio in different pH solutions. The present blend monolith of biocompatible and biodegradable PVA and SA with nanoscale porous structure has large potential for applications in biomedical and environmental fields.

Compound-specific nitrogen and carbon isotope analysis of nitroaromatic compounds in aqueous samples using solid-phase microextraction coupled to GC/IRMS.

Science.gov (United States)

Berg, Michael; Bolotin, Jakov; Hofstetter, Thomas B

2007-03-15

Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry was used to determine the delta15N and delta13C signatures of selected nitroaromatic contaminants such as the explosive 2,4,6-trinitrotoluene (TNT) for derivation of isotopic enrichment factors of contaminant transformation. Parameters for efficient extraction of nitroaromatic compounds (NACs) and substituted anilines from water samples were evaluated by SPME-GC/MS. delta13C signatures determined by SPME-GC/IRMS and elemental analyzer IRMS (EA-IRMS) were in good agreement, generally within +/-0.7 per thousand, except for 2,4-dinitrotoluene (2,4-DNT) and TNT, which showed slight deviations (IRMS were between 73 and 780 microg L-1 and correlated with the extraction efficiencies of the compounds determined by SPME-GC/MS. Nitrogen isotope measurements by SPME-GC/IRMS were of similar precision (standard deviations IRMS within +/-1.3 per thousand (+2.5 per thousand for TNT), but no systematic trend was found for the deviations. LODs of delta15N measurements ranged from 1.6 to 9.6 mg L-1 for nitrotoluenes, chlorinated NACs and DNTs (22 mg L-1 for TNT). The SPME-GC/IRMS method is well suited for the determination of isotopic enrichment factors of various NAC transformation processes and provides so far unexplored possibilities to elucidate behavior and degradation mechanisms of nitroaromatic contaminants in soils and groundwaters.

A facile approach for the synthesis of monolithic hierarchical porous carbons – high performance materials for amine based CO2 capture and supercapacitor electrode

KAUST Repository

Estevez, Luis; Dua, Rubal; Bhandari, Nidhi; Ramanujapuram, Anirudh; Wang, Peng; Giannelis, Emmanuel P.

2013-01-01

An ice templating coupled with hard templating and physical activation approach is reported for the synthesis of hierarchically porous carbon monoliths with tunable porosities across all three length scales (macro- meso- and micro), with ultrahigh

Acoustic of monolithic dome structures

Directory of Open Access Journals (Sweden)

Mostafa Refat Ismail

2018-03-01

The interior of monolithic domes have perfect, concave shapes to ensure that sound travels through the dome and perfectly collected at different vocal points. These dome structures are utilized for domestic use because the scale allows the focal points to be positioned across daily life activities, thereby affecting the sonic comfort of the internal space. This study examines the various acoustic treatments and parametric configurations of monolithic dome sizes. A geometric relationship of acoustic treatment and dome radius is established to provide architects guidelines on the correct selection of absorption needed to maintain the acoustic comfort of these special spaces.

Determination of partition coefficient and analysis of nitrophenols by three-phase liquid-phase microextraction coupled with capillary electrophoresis.

Science.gov (United States)

Sanagi, Mohd Marsin; Miskam, Mazidatulakmam; Wan Ibrahim, Wan Aini; Hermawan, Dadan; Aboul-Enein, Hassan Y

2010-07-01

A three-phase hollow fiber liquid-phase microextraction method coupled with CE was developed and used for the determination of partition coefficients and analysis of selected nitrophenols in water samples. The selected nitrophenols were extracted from 14 mL of aqueous solution (donor solution) with the pH adjusted to pH 3 into an organic phase (1-octanol) immobilized in the pores of the hollow fiber and finally backextracted into 40.0 microL of the acceptor phase (NaOH) at pH 12.0 located inside the lumen of the hollow fiber. The extractions were carried out under the following optimum conditions: donor solution, 0.05 M H(3)PO(4), pH 3.0; organic solvent, 1-octanol; acceptor solution, 40 microL of 0.1 M NaOH, pH 12.0; agitation rate, 1050 rpm; extraction time, 15 min. Under optimized conditions, the calibration curves for the analytes were linear in the range of 0.05-0.30 mg/L with r(2)>0.9900 and LODs were in the range of 0.01-0.04 mg/L with RSDs of 1.25-2.32%. Excellent enrichment factors of up to 398-folds were obtained. It was found that the partition coefficient (K(a/d)) values were high for 2-nitrophenol, 3-nitrophenol, 4-nitrophenol, 2,4-dinitrophenol and 2,6-dinitrophenol and that the individual partition coefficients (K(org/d) and K(a/org)) promoted efficient simultaneous extraction from the donor through the organic phase and further into the acceptor phase. The developed method was successfully applied for the analysis of water samples.

Media Presentation Synchronisation for Non-monolithic Rendering Architectures

NARCIS (Netherlands)

I. Vaishnavi (Ishan); D.C.A. Bulterman (Dick); P.S. Cesar Garcia (Pablo Santiago); B. Gao (Bo)

2007-01-01

htmlabstractNon-monolithic renderers are physically distributed media playback engines. Non-monolithic renderers may use a number of different underlying network connection types to transmit media items belonging to a presentation. There is therefore a need for a media based and inter-network- type

Determination of 2-Propenal Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography–Time-of-Flight Mass Spectrometry as a Marker for Authentication of Unrefined Sesame Oil

Directory of Open Access Journals (Sweden)

Ahmad Rois Mansur

2017-01-01

Full Text Available Ascertaining the authenticity of the unrefined sesame oil presents an ongoing challenge. Here, the determination of 2-propenal was performed by headspace solid-phase microextraction (HS-SPME under mild temperature coupled to gas chromatography with time-of-flight mass spectrometry, enabling the detection of adulteration of unrefined sesame oil with refined corn or soybean oil. Employing this coupled technique, 2-propenal was detected in all tested refined corn and soybean oils but not in any of the tested unrefined sesame oil samples. Using response surface methodology, the optimum extraction temperature, equilibrium time, and extraction time for the HS-SPME analysis of 2-propenal using carboxen/polydimethylsiloxane fiber were determined to be 55°C, 15 min, and 15 min, respectively, for refined corn oil and 55°C, 25 min, and 15 min, respectively, for refined soybean oil. Under these optimized conditions, the adulteration of unrefined sesame oil with refined corn or soybean oils (1–5% was successfully detected. The detection and quantification limits of 2-propenal were found to be in the range of 0.008–0.010 and 0.023–0.031 µg mL−1, respectively. The overall results demonstrate the potential of this novel method for the authentication of unrefined sesame oil.

Edge chipping and flexural resistance of monolithic ceramics☆

Science.gov (United States)

Zhang, Yu; Lee, James J.-W.; Srikanth, Ramanathan; Lawn, Brian R.

2014-01-01

Objective Test the hypothesis that monolithic ceramics can be developed with combined esthetics and superior fracture resistance to circumvent processing and performance drawbacks of traditional all-ceramic crowns and fixed-dental-prostheses consisting of a hard and strong core with an esthetic porcelain veneer. Specifically, to demonstrate that monolithic prostheses can be produced with a much reduced susceptibility to fracture. Methods Protocols were applied for quantifying resistance to chipping as well as resistance to flexural failure in two classes of dental ceramic, microstructurally-modified zirconias and lithium disilicate glass–ceramics. A sharp indenter was used to induce chips near the edges of flat-layer specimens, and the results compared with predictions from a critical load equation. The critical loads required to produce cementation surface failure in monolithic specimens bonded to dentin were computed from established flexural strength relations and the predictions validated with experimental data. Results Monolithic zirconias have superior chipping and flexural fracture resistance relative to their veneered counterparts. While they have superior esthetics, glass–ceramics exhibit lower strength but higher chip fracture resistance relative to porcelain-veneered zirconias. Significance The study suggests a promising future for new and improved monolithic ceramic restorations, with combined durability and acceptable esthetics. PMID:24139756

Solid-phase microextraction for bioconcentration studies according to OECD TG 305

Energy Technology Data Exchange (ETDEWEB)

Duering, Rolf-Alexander; Boehm, Leonard [Land Use and Nutrition (IFZ) Justus Liebig University Giessen, Institute of Soil Science and Soil Conservation, Research Centre for BioSystems, Giessen (Germany); Schlechtriem, Christian [Fraunhofer Institute for Molecular Biology and Applied Ecology (IME), Schmallenberg (Germany)

2012-12-15

An important aim of the European Community Regulation on chemicals and their safe use is the identification of (very) persistent, (very) bioaccumulative, and toxic substances. In other regulatory chemical safety assessments (pharmaceuticals, biocides, pesticides), the identification of such (very) persistent, (very) bioaccumulative, and toxic substances is of increasing importance. Solid-phase microextraction is especially capable of extracting total water concentrations as well as the freely dissolved fraction of analytes in the water phase, which is available for bioconcentration in fish. However, although already well established in environmental analyses to determine and quantify analytes mainly in aqueous matrices, solid-phase microextraction is still a rather unusual method in regulatory ecotoxicological research. Here, the potential benefits and drawbacks of solid-phase microextraction are discussed as an analytical routine approach for aquatic bioconcentration studies according to OECD TG 305, with a special focus on the testing of hydrophobic organic compounds characterized by log K{sub OW}> 5. (orig.)

Determination of parabens using two microextraction methods coupled with capillary liquid chromatography-UV detection.

Science.gov (United States)

Chen, Chen-Wen; Hsu, Wen-Chan; Lu, Ya-Chen; Weng, Jing-Ru; Feng, Chia-Hsien

2018-02-15

Parabens are common preservatives and environmental hormones. As such, possible detrimental health effects could be amplified through their widespread use in foods, cosmetics, and pharmaceutical products. Thus, the determination of parabens in such products is of particular importance. This study explored vortex-assisted dispersive liquid-liquid microextraction techniques based on the solidification of a floating organic drop (VA-DLLME-SFO) and salt-assisted cloud point extraction (SA-CPE) for paraben extraction. Microanalysis was performed using a capillary liquid chromatography-ultraviolet detection system. These techniques were modified successfully to determine four parabens in 19 commercial products. The regression equations of these parabens exhibited good linearity (r 2 =0.998, 0.1-10μg/mL), good precision (RSD<5%) and accuracy (RE<5%), reduced reagent consumption and reaction times (<6min), and excellent sample versatility. VA-DLLME-SFO was also particularly convenient due to the use of a solidified extract. Thus, the VA-DLLME-SFO technique was better suited to the extraction of parabens from complex matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

Quantum gate for Q switching in monolithic photonic-band-gap cavities containing two-level atoms

International Nuclear Information System (INIS)

Greentree, Andrew D.; Prawer, Steven; Hollenberg, Lloyd C. L.; Salzman, J.

2006-01-01

Photonic-band-gap cavities are prime solid-state systems to investigate light-matter interactions in the strong coupling regime. However, as the cavity is defined by the geometry of the periodic dielectric pattern, cavity control in a monolithic structure can be problematic. Thus, either the state coherence is limited by the read-out channel, or in a high-Q cavity, it is nearly decoupled from the external world, making measurement of the state extremely challenging. We present here a method for ameliorating these difficulties by using a coupled cavity arrangement, where one cavity acts as a switch for the other cavity, tuned by control of the atomic transition

Use of microextraction by packed sorbent directly coupled to an electron ionization single quadrupole mass spectrometer as an alternative for non-separative determinations.

Science.gov (United States)

Casas Ferreira, Ana María; Moreno Cordero, Bernardo; Pérez Pavón, José Luis

2017-02-01

Sometimes it is not necessary to separate the individual compounds of a sample to resolve an analytical problem, it is enough to obtain a signal profile of the sample formed by all the components integrating it. Within this strategy, electronic noses based on the direct coupling of a headspace sampler with a mass spectrometer (HS-MS) have been proposed. Nevertheless, this coupling is not suitable for the analysis of non-volatile compounds. In order to propose an alternative to HS-MS determinations for non-volatile compounds, here we present the first 'proof of concept' use of the direct coupling of microextraction by packed sorbents (MEPS) to a mass spectrometer device using an electron ionization (EI) and a single quadrupole as ionization source and analyzer, respectively. As target compounds, a set of analytes with different physic-chemical properties were evaluated (2-ethyl-1-hexanol, styrene, 2-heptanone, among others). The use of MEPS extraction present many advantages, such as it is fast, simple, easy to automate and requires small volumes of sample and organic solvents. Moreover, MEPS cartridges are re-usable as samples can be extracted more than 100 times using the same syringe. In order to introduce into the system all the elution volume from the MEPS extraction, a programmable temperature vaporizer (PTV) is proposed as the injector device. Results obtained with the proposed methodology (MEPS-PTV/MS) were compared with the ones obtained based on the separative scheme, i.e. using gas chromatography separation (MEPS-PTV-GC/MS), and both methods provided similar results. Limits of detection were found to be between 3.26 and 146.6μgL -1 in the non-separative scheme and between 0.02 and 1.72μgL -1 when the separative methodology was used. Repeatability and reproducibility were evaluated with values below 17% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

Monolithic Active Pixel Matrix with Binary Counters (MAMBO) ASIC

Energy Technology Data Exchange (ETDEWEB)

Khalid, Farah F.; Deptuch, Grzegorz; Shenai, Alpana; Yarema, Raymond J.; /Fermilab

2010-11-01

Monolithic Active Matrix with Binary Counters (MAMBO) is a counting ASIC designed for detecting and measuring low energy X-rays from 6-12 keV. Each pixel contains analogue functionality implemented with a charge preamplifier, CR-RC{sup 2} shaper and a baseline restorer. It also contains a window comparator which can be trimmed by 4 bit DACs to remove systematic offsets. The hits are registered by a 12 bit ripple counter which is reconfigured as a shift register to serially output the data from the entire ASIC. Each pixel can be tested individually. Two diverse approaches have been used to prevent coupling between the detector and electronics in MAMBO III and MAMBO IV. MAMBO III is a 3D ASIC, the bottom ASIC consists of diodes which are connected to the top ASIC using {mu}-bump bonds. The detector is decoupled from the electronics by physically separating them on two tiers and using several metal layers as a shield. MAMBO IV is a monolithic structure which uses a nested well approach to isolate the detector from the electronics. The ASICs are being fabricated using the SOI 0.2 {micro}m OKI process, MAMBO III is 3D bonded at T-Micro and MAMBO IV nested well structure was developed in collaboration between OKI and Fermilab.

Wideband Monolithic Microwave Integrated Circuit Frequency Converters with GaAs mHEMT Technology

OpenAIRE

Krozer, Viktor; Johansen, Tom Keinicke; Djurhuus, Torsten; Vidkjær, Jens

2005-01-01

We present monolithic microwave integrated circuit (MMIC) frequency converter, which can be used for up and down conversion, due to the large RF and IF port bandwidth. The MMIC converters are based on commercially available GaAs mHEMT technology and are comprised of a Gilbert mixer cell core, baluns and combiners. Single ended and balanced configurations DC and AC coupled have been investigated. The instantaneous 3 dB bandwidth at both the RF and the IF port of the frequency converters is ∼ 2...

Creating deep soil core monoliths: Beyond the solum

Science.gov (United States)

Soil monoliths serve as useful teaching aids in the study of the Earth’s critical zone where rock, soil, water, air, and organisms interact. Typical monolith preparation has so far been confined to the 1 to 2-m depth of the solum. Critical ecosystem services provided by soils include materials from ...

Detachable strong cation exchange monolith, integrated with capillary zone electrophoresis and coupled with pH gradient elution, produces improved sensitivity and numbers of peptide identifications during bottom-up analysis of complex proteomes.

Science.gov (United States)

Zhang, Zhenbin; Yan, Xiaojing; Sun, Liangliang; Zhu, Guijie; Dovichi, Norman J

2015-04-21

A detachable sulfonate-silica hybrid strong cation-exchange monolith was synthesized in a fused silica capillary, and used for solid phase extraction with online pH gradient elution during capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) proteomic analysis. Tryptic digests were prepared in 50 mM formic acid and loaded onto the strong cation-exchange monolith. Fractions were eluted using a series of buffers with lower concentration but higher pH values than the 50 mM formic acid background electrolyte. This combination of elution and background electrolytes results in both sample stacking and formation of a dynamic pH junction and allows use of relatively large elution buffer volumes while maintaining reasonable peak efficiency and resolution. A series of five pH bumps were applied to elute E. coli tryptic peptides from the monolith, followed by analysis using CZE coupled to an LTQ-Orbitrap Velos mass spectrometer; 799 protein groups and 3381 peptides were identified from 50 ng of the digest in a 2.5 h analysis, which approaches the identification rate for this organism that was obtained with an Orbitrap Fusion. We attribute the improved numbers of peptide and protein identifications to the efficient fractionation by the online pH gradient elution, which decreased the complexity of the sample in each elution step and improved the signal intensity of low abundance peptides. We also performed a comparative analysis using a nanoACQUITY UltraPerformance LCH system. Similar numbers of protein and peptide identifications were produced by the two methods. Protein identifications showed significant overlap between the two methods, whereas peptide identifications were complementary.

FLUIDIZED BED STEAM REFORMER MONOLITH FORMATION

International Nuclear Information System (INIS)

Jantzen, C

2006-01-01

Fluidized Bed Steam Reforming (FBSR) is being considered as an alternative technology for the immobilization of a wide variety of aqueous high sodium containing radioactive wastes at various DOE facilities in the United States. The addition of clay, charcoal, and a catalyst as co-reactants converts aqueous Low Activity Wastes (LAW) to a granular or ''mineralized'' waste form while converting organic components to CO 2 and steam, and nitrate/nitrite components, if any, to N 2 . The waste form produced is a multiphase mineral assemblage of Na-Al-Si (NAS) feldspathoid minerals with cage-like structures that atomically bond radionuclides like Tc-99 and anions such as SO 4 , I, F, and Cl. The granular product has been shown to be as durable as LAW glass. Shallow land burial requires that the mineralized waste form be able to sustain the weight of soil overburden and potential intrusion by future generations. The strength requirement necessitates binding the granular product into a monolith. FBSR mineral products were formulated into a variety of monoliths including various cements, Ceramicrete, and hydroceramics. All but one of the nine monoliths tested met the 2 durability specification for Na and Re (simulant for Tc-99) when tested using the Product Consistency Test (PCT; ASTM C1285). Of the nine monoliths tested the cements produced with 80-87 wt% FBSR product, the Ceramicrete, and the hydroceramic produced with 83.3 wt% FBSR product, met the compressive strength and durability requirements for an LAW waste form

Plant oil-based shape memory polymer using acrylic monolith

Directory of Open Access Journals (Sweden)

T. Tsujimoto

2015-09-01

Full Text Available This article deals with the synthesis of a plant oil-based material using acrylic monolith. An acrylic monolith bearing oxirane groups was prepared via simple technique that involved the dissolution of poly(glycidyl methacrylate-comethyl methacrylate (PGMA in ethanolic – aqueous solution by heating and subsequent cooling. The PGMA monolith had topologically porous structure, which was attributed to the phase separation of the polymer solution. The PGMA monolith was impregnated by epoxidized soybean oil (ESO containing thermally-latent catalyst, and the subsequent curing produced a crosslinked material with relatively good transparency. The Young’s modulus and the tensile strength of polyESO/PGMA increased compared with the ESO homopolymer. The strain at break of polyESO/PGMA was larger than that of the ESO homopolymer and crosslinked PGMA. Furthermore, polyESO/PGMA exhibited good shape memory-recovery behavior.

Data quality objectives summary report for the 105-N monolith off-gas issue

International Nuclear Information System (INIS)

Pisarcik, D.J.

1997-01-01

The 105-N Basin hardware waste with radiation exposure rates high enough to make above-water handling and packaging impractical has been designated high exposure rate hardware (HERH) waste. This material, consisting primarily of irradiated reactor components, is packaged underwater for subsequent disposal as a grout-encapsulated solid monolith. The third HERH waste package that was created (Monolith No. 3) was not immediately removed from the basin because of administrative delays. During a routine facility walkdown, Monolith No. 3 was observed to be emitting bubbles. Mass spectroscopic analysis of a gas sample from Monolith No. 3 indicated that the gas was 85.2% hydrogen along with a trace of fission gases (stable isotopes of xenon). Gamma energy analysis of a gas sample from Monolith No. 3 also identified trace quantities of 85 Kr. The monolith off-gas Data Quality Objective (DQO) process concluded the following: Monolith No. 3 and similar monoliths can be safely transported following installation of spacers between the lids of the L3-181 transport cask to vent the hydrogen gas; The 85 Kr does not challenge personnel or environmental safety; Fumaroles in the surface of gassing monoliths renders them incompatible with Hanford Site Solid Waste Acceptance Criteria requirements unless placed in a qualified high integrity container overpack; and Gassing monoliths do meet Environmental Restoration Disposal Facility Waste Acceptance Criteria requirements. This DQO Summary Report is both an account of the Monolith Off-Gas DQO Process and a means of documenting the concurrence of each of the stakeholder organizations

A poly(vinyl alcohol)/sodium alginate blend monolith with nanoscale porous structure

OpenAIRE

Sun, Xiaoxia; Uyama, Hiroshi

2013-01-01

A stimuli-responsive poly(vinyl alcohol) (PVA)/sodium alginate (SA) blend monolith with nanoscale porous (mesoporous) structure is successfully fabricated by thermally impacted non-solvent induced phase separation (TINIPS) method. The PVA/SA blend monolith with different SA contents is conveniently fabricated in an aqueous methanol without any templates. The solvent suitable for the fabrication of the present blend monolith by TINIPS is different with that of the PVA monolith. The nanostructu...

Energy Absorption of Monolithic and Fibre Reinforced Aluminium Cylinders

NARCIS (Netherlands)

De Kanter, J.L.C.G.

2006-01-01

Summary accompanying the thesis: Energy Absorption of Monolithic and Fibre Reinforced Aluminium Cylinders by Jens de Kanter This thesis presents the investigation of the crush behaviour of both monolithic aluminium cylinders and externally fibre reinforced aluminium cylinders. The research is based

Development of double chain phosphatidylcholine functionalized polymeric monoliths for immobilized artificial membrane chromatography.

Science.gov (United States)

Wang, Qiqin; Peng, Kun; Chen, Weijia; Cao, Zhen; Zhu, Peijie; Zhao, Yumei; Wang, Yuqiang; Zhou, Haibo; Jiang, Zhengjin

2017-01-06

This study described a simple synthetic methodology for preparing biomembrane mimicking monolithic column. The suggested approach not only simplifies the preparation procedure but also improves the stability of double chain phosphatidylcholine (PC) functionalized monolithic column. The physicochemical properties of the optimized monolithic column were characterized by scanning electron microscopy, energy-dispersive X-ray spectrometry, and nano-LC. Satisfactory column permeability, efficiency, stability and reproducibility were obtained on this double chain PC functionalized monolithic column. It is worth noting that the resulting polymeric monolith exhibits great potential as a useful alternative of commercial immobilized artificial membrane (IAM) columns for in vitro predication of drug-membrane interactions. Furthermore, the comparative study of both double chain and single chain PC functionalized monoliths indicates that the presence or absence of glycerol backbone and the number of acyl chains are not decisive for the predictive ability of IAM monoliths on drug-membrane interactions. This novel PC functionalized monolithic column also exhibited good selectivity for a protein mixture and a set of pharmaceutical compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

A symmetric positive definite formulation for monolithic fluid structure interaction

KAUST Repository

Robinson-Mosher, Avi; Schroeder, Craig; Fedkiw, Ronald

2011-01-01

In this paper we consider a strongly coupled (monolithic) fluid structure interaction framework for incompressible flow, as opposed to a loosely coupled (partitioned) method. This requires solving a single linear system that combines the unknown velocities of the structure with the unknown pressures of the fluid. In our previous work, we were able to obtain a symmetric formulation of this coupled system; however, it was also indefinite, making it more difficult to solve. In fact in practice there have been cases where we have been unable to invert the system. In this paper we take a novel approach that consists of factoring the damping matrix of deformable structures and show that this can be used to obtain a symmetric positive definite system, at least to the extent that the uncoupled systems were symmetric positive definite. We use a traditional MAC grid discretization of the fluid and a fully Lagrangian discretization of the structures for the sake of exposition, noting that our procedure can be generalized to other scenarios. For the special case of rigid bodies, where there are no internal damping forces, we exactly recover the system of Batty et al. (2007) [4]. © 2010 Elsevier Inc.

A symmetric positive definite formulation for monolithic fluid structure interaction

KAUST Repository

Robinson-Mosher, Avi

2011-02-01

In this paper we consider a strongly coupled (monolithic) fluid structure interaction framework for incompressible flow, as opposed to a loosely coupled (partitioned) method. This requires solving a single linear system that combines the unknown velocities of the structure with the unknown pressures of the fluid. In our previous work, we were able to obtain a symmetric formulation of this coupled system; however, it was also indefinite, making it more difficult to solve. In fact in practice there have been cases where we have been unable to invert the system. In this paper we take a novel approach that consists of factoring the damping matrix of deformable structures and show that this can be used to obtain a symmetric positive definite system, at least to the extent that the uncoupled systems were symmetric positive definite. We use a traditional MAC grid discretization of the fluid and a fully Lagrangian discretization of the structures for the sake of exposition, noting that our procedure can be generalized to other scenarios. For the special case of rigid bodies, where there are no internal damping forces, we exactly recover the system of Batty et al. (2007) [4]. © 2010 Elsevier Inc.

Vortex-assisted magnetic β-cyclodextrin/attapulgite-linked ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the fast determination of four fungicides in water samples.

Science.gov (United States)

Yang, Miyi; Xi, Xuefei; Wu, Xiaoling; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

2015-02-13

A novel microextraction technique combining magnetic solid-phase microextraction (MSPME) with ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) to determine four fungicides is presented in this work for the first time. The main factors affecting the extraction efficiency were optimized by the one-factor-at-a-time approach and the impacts of these factors were studied by an orthogonal design. Without tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimum conditions, good linearity and high enrichment factors were obtained for all analytes, with correlation coefficients ranging from 0.9998 to 1.0000 and enrichment factors ranging 135 and 159 folds. The recoveries for proposed approach were between 98% and 115%, the limits of detection were between 0.02 and 0.04 μg L(-1) and the RSDs changed from 2.96 to 4.16. The method was successfully applied in the analysis of four fungicides (azoxystrobin, chlorothalonil, cyprodinil and trifloxystrobin) in environmental water samples. The recoveries for the real water samples ranged between 81% and 109%. The procedure proved to be a time-saving, environmentally friendly, and efficient analytical technique. Copyright © 2015 Elsevier B.V. All rights reserved.

Monolithic multinozzle emitters for nanoelectrospray mass spectrometry

Science.gov (United States)

Wang, Daojing [Daly City, CA; Yang, Peidong [Kensington, CA; Kim, Woong [Seoul, KR; Fan, Rong [Pasadena, CA

2011-09-20

Novel and significantly simplified procedures for fabrication of fully integrated nanoelectrospray emitters have been described. For nanofabricated monolithic multinozzle emitters (NM.sup.2 emitters), a bottom up approach using silicon nanowires on a silicon sliver is used. For microfabricated monolithic multinozzle emitters (M.sup.3 emitters), a top down approach using MEMS techniques on silicon wafers is used. The emitters have performance comparable to that of commercially-available silica capillary emitters for nanoelectrospray mass spectrometry.

Decomposition of monolithic web application to microservices

OpenAIRE

Zaymus, Mikulas

2017-01-01

Solteq Oyj has an internal Wellbeing project for massage reservations. The task of this thesis was to transform the monolithic architecture of this application to microservices. The thesis starts with a detailed comparison between microservices and monolithic application. It points out the benefits and disadvantages microservice architecture can bring to the project. Next, it describes the theory and possible strategies that can be used in the process of decomposition of an existing monoli...

Large microwave tunability of GaAs-based multiferroic heterostructure for applications in monolithic microwave integrated circuits

International Nuclear Information System (INIS)

Chen Yajie; Gao Jinsheng; Vittoria, C; Harris, V G; Heiman, D

2010-01-01

Microwave magnetoelectric coupling in a ferroelectric/ferromagnetic/semiconductor multiferroic (MF) heterostructure, consisting of a Co 2 MnAl epitaxial film grown on a GaAs substrate bonded to a lead magnesium niobate-lead titanate (PMN-PT) crystal, is reported. Ferromagnetic resonance measurements were carried out at X-band under the application of electric fields. Results indicate a frequency tuning of 125 MHz for electric field strength of 8 kV cm -1 resulting in a magnetoelectric coupling coefficient of 3.4 Oe cm kV -1 . This work explores the potential of electronically controlled MF devices for use in future monolithic microwave integrated circuits.

Fracture-resistant monolithic dental crowns.

Science.gov (United States)

Zhang, Yu; Mai, Zhisong; Barani, Amir; Bush, Mark; Lawn, Brian

2016-03-01

To quantify the splitting resistance of monolithic zirconia, lithium disilicate and nanoparticle-composite dental crowns. Fracture experiments were conducted on anatomically-correct monolithic crown structures cemented to standard dental composite dies, by axial loading of a hard sphere placed between the cusps. The structures were observed in situ during fracture testing, and critical loads to split the structures were measured. Extended finite element modeling (XFEM), with provision for step-by-step extension of embedded cracks, was employed to simulate full failure evolution. Experimental measurements and XFEM predictions were self-consistent within data scatter. In conjunction with a fracture mechanics equation for critical splitting load, the data were used to predict load-sustaining capacity for crowns on actual dentin substrates and for loading with a sphere of different size. Stages of crack propagation within the crown and support substrate were quantified. Zirconia crowns showed the highest fracture loads, lithium disilicate intermediate, and dental nanocomposite lowest. Dental nanocomposite crowns have comparable fracture resistance to natural enamel. The results confirm that monolithic crowns are able to sustain high bite forces. The analysis indicates what material and geometrical properties are important in optimizing crown performance and longevity. Copyright © 2015 Academy of Dental Materials. All rights reserved.

Characterization of SOI monolithic detector system

Science.gov (United States)

Álvarez-Rengifo, P. L.; Soung Yee, L.; Martin, E.; Cortina, E.; Ferrer, C.

2013-12-01

A monolithic active pixel sensor for charged particle tracking was developed. This research is performed within the framework of an R&D project called TRAPPISTe (Tracking Particles for Physics Instrumentation in SOI Technology) whose aim is to evaluate the feasibility of developing a Monolithic Active Pixel Sensor (MAPS) with Silicon-on-Insulator (SOI) technology. Two chips were fabricated: TRAPPISTe-1 and TRAPPISTe-2. TRAPPISTe-1 was produced at the WINFAB facility at the Université catholique de Louvain (UCL), Belgium, in a 2 μm fully depleted (FD-SOI) CMOS process. TRAPPISTe-2 was fabricated with the LAPIS 0.2 μm FD-SOI CMOS process. The electrical characterization on single transistor test structures and of the electronic readout for the TRAPPISTe series of monolithic pixel detectors was carried out. The behavior of the prototypes’ electronics as a function of the back voltage was studied. Results showed that both readout circuits exhibited sensitivity to the back voltage. Despite this unwanted secondary effect, the responses of TRAPPISTe-2 amplifiers can be improved by a variation in the circuit parameters.

Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

International Nuclear Information System (INIS)

Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

2010-01-01

In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

Ring-opening metathesis polymerization based pore-size-selective functionalization of glycidyl methacrylate based monolithic media: access to size-stable nanoparticles for ligand-free metal catalysis.

Science.gov (United States)

Bandari, Rajendar; Höche, Thomas; Prager, Andrea; Dirnberger, Klaus; Buchmeiser, Michael R

2010-04-19

Monolithic polymeric supports have been prepared by electron-beam-triggered free-radical polymerization using a mixture of glycidyl methacrylate and trimethylolpropane triacrylate in 2-propanol, 1-dodecanol, and toluene. Under appropriate conditions, phase separation occurred, which resulted in the formation of a porous monolithic matrix that was characterized by large (convective) pores in the 30 μm range as well as pores of 7 nm were hydrolyzed by using poly(styrenesulfonic acid) (Mw = 69,400 g mol(-1), PDI=2.4). The remaining epoxy groups inside pores of nanoparticles 2 nm in diameter were formed. The palladium-nanoparticle-loaded monoliths were used in both Heck- and Suzuki-type coupling reactions achieving turnover numbers of up to 167,000 and 63,000, respectively. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Agglomerated polymer monoliths with bimetallic nano-particles as flow-through micro-reactors

International Nuclear Information System (INIS)

Floris, P.; Twamley, B.; Nesterenko, P.N.; Paull, B.; Connolly, D.

2012-01-01

Polymer monoliths in capillary format have been prepared as solid supports for the immobilisation of platinum/palladium bimetallic nano-flowers. Optimum surface coverage of nano-flowers was realised by photografting the monoliths with vinyl azlactone followed by amination with ethylenediamine prior to nano-particle immobilisation. Field emission SEM imaging was used as a characterisation tool for evaluating nano-particle coverage, together with BET surface area analysis to probe the effect of nano-particle immobilisation upon monolith morphology. Ion exchange chromatography was also used to confirm the nature of the covalent attachment of nano-flowers on the monolithic surface. In addition, EDX and ICP analyses were used to quantify platinum and palladium on modified polymer monoliths. Finally the catalytic properties of immobilised bimetallic Pd/Pt nano-flowers were evaluated in flow-through mode, exploiting the porous interconnected flow-paths present in the prepared monoliths (pore diameter ∼ 1-2 μm). Specifically, the reduction of Fe (III) to Fe (II) and the oxidation of NADH to NAD+ were selected as model redox reactions. The use of a porous polymer monolith as an immobilisation substrate (rather than aminated micro-spheres) eliminated the need for a centrifugation step after the reaction. (author)

Development of headspace solid-phase microextraction method for ...

African Journals Online (AJOL)

A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow ...

FLUIDIZED BED STEAM REFORMER MONOLITH FORMATION

Energy Technology Data Exchange (ETDEWEB)

Jantzen, C

2006-12-22

Fluidized Bed Steam Reforming (FBSR) is being considered as an alternative technology for the immobilization of a wide variety of aqueous high sodium containing radioactive wastes at various DOE facilities in the United States. The addition of clay, charcoal, and a catalyst as co-reactants converts aqueous Low Activity Wastes (LAW) to a granular or ''mineralized'' waste form while converting organic components to CO{sub 2} and steam, and nitrate/nitrite components, if any, to N{sub 2}. The waste form produced is a multiphase mineral assemblage of Na-Al-Si (NAS) feldspathoid minerals with cage-like structures that atomically bond radionuclides like Tc-99 and anions such as SO{sub 4}, I, F, and Cl. The granular product has been shown to be as durable as LAW glass. Shallow land burial requires that the mineralized waste form be able to sustain the weight of soil overburden and potential intrusion by future generations. The strength requirement necessitates binding the granular product into a monolith. FBSR mineral products were formulated into a variety of monoliths including various cements, Ceramicrete, and hydroceramics. All but one of the nine monoliths tested met the <2g/m{sup 2} durability specification for Na and Re (simulant for Tc-99) when tested using the Product Consistency Test (PCT; ASTM C1285). Of the nine monoliths tested the cements produced with 80-87 wt% FBSR product, the Ceramicrete, and the hydroceramic produced with 83.3 wt% FBSR product, met the compressive strength and durability requirements for an LAW waste form.

Fibroin/dodecanol floating solidification microextraction for the preconcentration of trace levels of flavonoids in complex matrix samples.

Science.gov (United States)

Chen, Xuan; Li, Jie; Hu, Shuang; Bai, Xiaohong; Zhao, Haodong; Zhang, Yi

2018-01-01

A new fibroin/dodecanol floating solidification microextraction, coupled with high performance liquid chromatography, was developed and applied for enrichment and quantification of the trace flavonoids in traditional Chinese medicine and biological samples. Also, fibroin sensibilization mechanism was described, and influence of sample matrix to enrichment factor was investigated. In this method, a homogeneous fibroin/dodecanol of dispersed solution was employed as microextraction phase to flavonoids (myricetin, quercetin, isorhamnetin, chrysin, kaempferide), the several critical parameters affecting the performance, such as organic extractant, amount of fibroin in organic extractant, volume of extraction phase, dispersant, salt concentration, pH of sample phase, stirring rate, extraction time, and volume of sample phase were tested and optimized. Under the optimized conditions, enrichment factor of flavonoids ranged from 42.4 to 238.1 in different samples, excellent linearities with r 2 ≥ 0.9968 for all analytes were achieved, limits of detection were less than or equal to 5.0ng/mL, average recoveries were 92.5% to 115.0% in different samples. The new procedure is simple, fast, low cost, environmentally friendly and high EF, it can also be applied to the concentration and enrichment of the trace flavonoids in other complex matrixes. Copyright © 2017. Published by Elsevier B.V.

Immobilisation of shredded soft waste in cement monolith

International Nuclear Information System (INIS)

Brown, D.J.; Dalton, M.J.; Smith, D.L.

1983-04-01

A grouting process for the immobilisation of shredded contaminated laboratory waste in a cement monolith is being developed at the Atomic Energy Establishment Winfrith. The objective is to produce a 'monolithic' type package which is acceptable both for sea and land disposal. The work carried out on this project in the period April 1982 - March 1983 is summarised in this report. (author)

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

International Nuclear Information System (INIS)

Catalá-Icardo, M.; Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C.; Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G.; Herrero-Martínez, J.M.

2017-01-01

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch"®), or mixtures of H_2O_2 and H_2SO_4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Catalá-Icardo, M., E-mail: mocaic@qim.upv.es [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C. [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G. [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain); Herrero-Martínez, J.M., E-mail: jmherrer@uv.es [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain)

2017-04-01

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch{sup ®}), or mixtures of H{sub 2}O{sub 2} and H{sub 2}SO{sub 4}, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

Increased thermal conductivity monolithic zeolite structures

Science.gov (United States)

Klett, James; Klett, Lynn; Kaufman, Jonathan

2008-11-25

A monolith comprises a zeolite, a thermally conductive carbon, and a binder. The zeolite is included in the form of beads, pellets, powders and mixtures thereof. The thermally conductive carbon can be carbon nano-fibers, diamond or graphite which provide thermal conductivities in excess of about 100 W/mK to more than 1,000 W/mK. A method of preparing a zeolite monolith includes the steps of mixing a zeolite dispersion in an aqueous colloidal silica binder with a dispersion of carbon nano-fibers in water followed by dehydration and curing of the binder is given.

Development and characterization of methacrylate-based hydrazide monoliths for oriented immobilization of antibodies.

Science.gov (United States)

Brne, P; Lim, Y-P; Podgornik, A; Barut, M; Pihlar, B; Strancar, A

2009-03-27

Convective interaction media (CIM; BIA Separations) monoliths are attractive stationary phases for use in affinity chromatography because they enable fast affinity binding, which is a consequence of convectively enhanced mass transport. This work focuses on the development of novel CIM hydrazide (HZ) monoliths for the oriented immobilization of antibodies. Adipic acid dihydrazide (AADH) was covalently bound to CIM epoxy monoliths to gain hydrazide groups on the monolith surface. Two different antibodies were afterwards immobilized to hydrazide functionalized monolithic columns and prepared columns were tested for their selectivity. One column was further tested for the dynamic binding capacity.

A Monolithically-Integrated μGC Chemical Sensor System

Directory of Open Access Journals (Sweden)

Davor Copic

2011-06-01

Full Text Available Gas chromatography (GC is used for organic and inorganic gas detection with a range of applications including screening for chemical warfare agents (CWA, breath analysis for diagnostics or law enforcement purposes, and air pollutants/indoor air quality monitoring of homes and commercial buildings. A field-portable, light weight, low power, rapid response, micro-gas chromatography (μGC system is essential for such applications. We describe the design, fabrication and packaging of mGC on monolithically-integrated Si dies, comprised of a preconcentrator (PC, μGC column, detector and coatings for each of these components. An important feature of our system is that the same mechanical micro resonator design is used for the PC and detector. We demonstrate system performance by detecting four different CWA simulants within 2 min. We present theoretical analyses for cost/power comparisons of monolithic versus hybrid μGC systems. We discuss thermal isolation in monolithic systems to improve overall performance. Our monolithically-integrated μGC, relative to its hybrid cousin, will afford equal or slightly lower cost, a footprint that is 1/2 to 1/3 the size and an improved resolution of 4 to 25%.

A novel photocatalytic monolith reactor for multiphase heterogeneous photocatalysis

NARCIS (Netherlands)

Du, P.; Carneiro, J.T.; Moulijn, J.A.; Mul, Guido

2008-01-01

A novel reactor for multi-phase photocatalysis is presented, the so-called internally illuminated monolith reactor (IIMR). In the concept of the IIMR, side light emitting fibers are placed inside the channels of a ceramic monolith, equipped with a TiO2 photocatalyst coated on the wall of each

A capillary monolithic trypsin reactor for efficient protein digestion in online and offline coupling to ESI and MALDI mass spectrometry.

Science.gov (United States)

Spross, Jens; Sinz, Andrea

2010-02-15

We describe the preparation of a capillary trypsin immobilized monolithic enzyme reactor (IMER) for a rapid and efficient digestion of proteins down to the femtomole level. Trypsin was immobilized on a poly(glycidyl methacrylate-co-acrylamide-co-ethylene glycol dimethycrylate) monolith using the glutaraldehyde technique. Digestion efficiencies of the IMER were evaluated using model proteins and protein mixtures as well as chemically cross-linked lysozyme regarding the addition of denaturants and increasing digestion temperature. The trypsin IMER described herein is applicable for the digestion of protein mixtures. Even at a 1000-fold molar excess of one protein, low-abundance proteins are readily identified, in combination with MS/MS analysis. An online setup of the IMER with reversed phase nano-HPLC separation and nano-ESI-MS/MS analysis was established. The great potential of the trypsin IMER for proteomics applications comprise short digestion times in the range of seconds to minutes, in addition to improved digestion efficiencies, compared to in-solution digestion.

Optimization of a single-drop microextraction method for multielemental determination by electrothermal vaporization inductively coupled plasma mass spectrometry following in situ vapor generation

International Nuclear Information System (INIS)

Gil, Sandra; Loos-Vollebregt, Margaretha T.C. de; Bendicho, Carlos

2009-01-01

A headspace single-drop microextraction (HS-SDME) method has been developed in combination with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) for the simultaneous determination of As, Sb, Bi, Pb, Sn and Hg in aqueous solutions. Vapor generation is carried out in a 40 mL volume closed-vial containing a solution with the target analytes in hydrochloric acid and potassium ferricyanide medium. Hydrides (As, Sb, Bi, Pb, Sn) and Hg vapor are trapped onto an aqueous single drop (3 μL volume) containing Pd(II), followed by the subsequent injection in the ETV. Experimental variables such as medium composition, sodium tetrahydroborate (III) volume and concentration, stirring rate, extraction time, sample volume, ascorbic acid concentration and palladium amount in the drop were fully optimized. The limits of detection (LOD) (3σ criterion) of the proposed method for As, Sb, Bi, Pb, Sn and Hg were 0.2, 0.04, 0.01, 0.07, 0.09 and 0.8 μg/L, respectively. Enrichment factors of 9, 85, 138, 130, 37 and 72 for As, Sb, Bi, Pb, Sn and Hg, respectively, were achieved in 210 s. The relative standard deviations (N = 5) ranged from 4 to 8%. The proposed HS-SDME-ETV-ICP-MS method has been applied for the determination of As, Sb, Bi, Pb, Sn and Hg in NWRI TM-28.3 certified reference material.

Novel strategies for sample preparation in forensic toxicology.

Science.gov (United States)

Samanidou, Victoria; Kovatsi, Leda; Fragou, Domniki; Rentifis, Konstantinos

2011-09-01

This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.

Monolithic JFET preamplifier for ionization chamber calorimeter

International Nuclear Information System (INIS)

Radeka, V.; Rescia, S.; Manfredi, P.F.; Speziali, V.

1990-10-01

A monolithic charge sensitive preamplifier using exclusively n-channel diffused JFETs has been designed and is now being fabricated by INTERFET Corp. by means of a dielectrically isolated process which allows preserving as much as possible the technology upon which discrete JFETs are based. A first prototype built by means of junction isolated process has been delivered. The characteristics of monolithically integrated JFETs compare favorably with discrete devices. First results of tests of a preamplifier which uses these devices are reported. 4 refs

An overview of monolithic zirconia in dentistry

Directory of Open Access Journals (Sweden)

Özlem Malkondu

2016-07-01

Full Text Available Zirconia restorations have been used successfully for years in dentistry owing to their biocompatibility and good mechanical properties. Because of their lack of translucency, zirconia cores are generally veneered with porcelain, which makes restorations weaker due to failure of the adhesion between the two materials. In recent years, all-ceramic zirconia restorations have been introduced in the dental sector with the intent to solve this problem. Besides the elimination of chipping, the reduced occlusal space requirement seems to be a clear advantage of monolithic zirconia restorations. However, scientific evidence is needed to recommend this relatively new application for clinical use. This mini-review discusses the current scientific literature on monolithic zirconia restorations. The results of in vitro studies suggested that monolithic zirconia may be the best choice for posterior fixed partial dentures in the presence of high occlusal loads and minimal occlusal restoration space. The results should be supported with much more in vitro and particularly in vivo studies to obtain a final conclusion.

Synthesis and application of in-situ molecularly imprinted silica monolithic in pipette-tip solid-phase microextraction for the separation and determination of gallic acid in orange juice samples.

Science.gov (United States)

Arabi, Maryam; Ghaedi, Mehrorang; Ostovan, Abbas

2017-03-24

A novel strategy was presented for the synthesis and application of functionalized silica monolithic as artificial receptor of gallic acid at micro-pipette tip. A sol-gel process was used to prepare the sorbent. In this in-situ polymerization reaction, tetraethyl orthosilicate (TEOS), 3-aminopropyl trimethoxysilane (APTMS), gallic acid and thiourea were used, respectively, as cross-linker, functionalized monomer, template and precursor to make crack-free and non-fragile structure. Such durable and inexpensive in-situ monolithic was successfully employed as useful tool for highly efficient extraction of gallic acid from orange juice samples. The effective parameters in extraction recovery were investigated and optimum conditions were obtained using experimental design methodology. Applying HPLC-UV for separation quantification at optimal conditions, the gallic acid was efficiently extracted without significant matrix interference. Good linearity for gallic acid in the range of 0.02-5.0mgL -1 with correlation coefficients of R 2 >0.999 revealed well applicability of the method for trace analysis. Copyright © 2017. Published by Elsevier B.V.

A 30 Mbps in-plane full-duplex light communication using a monolithic GaN photonic circuit

Science.gov (United States)

Gao, Xumin; Yuan, Jialei; Yang, Yongchao; Li, Yuanhang; Yuan, Wei; Zhu, Guixia; Zhu, Hongbo; Feng, Meixin; Sun, Qian; Liu, Yuhuai; Wang, Yongjin

2017-07-01

We propose, fabricate and characterize photonic integration of a InGaN/GaN multiple-quantum-well light-emitting diode (MQW-LED), waveguide, ring resonator and InGaN/GaN MQW-photodiode on a single chip, in which the photonic circuit is suspended by the support beams. Both experimental observations and simulation results illustrate the manipulation of in-plane light coupling and propagation by the waveguide and the ring resonator. The monolithic photonic circuit forms an in-plane data communication system using visible light. When the two suspended InGaN/GaN MQW-diodes simultaneously serve as the transmitter and the receiver, an in-plane full-duplex light communication is experimentally demonstrated with a transmission rate of 30 Mbps, and the superimposed signals are extracted using the self-interference cancellation method. The suspended photonic circuit creates new possibilities for exploring the in-plane full-duplex light communication and manufacturing complex GaN-based monolithic photonic integrations.

Fracture Strength of Aged Monolithic and Bilayer Zirconia-Based Crowns

Directory of Open Access Journals (Sweden)

Deborah Pacheco Lameira

2015-01-01

Full Text Available The purpose of this study was to evaluate the effect of design and surface finishing on fracture strength of yttria-tetragonal zirconia polycrystal (Y-TZP crowns in monolithic (1.5 mm thickness and bilayer (0.8 mm zirconia coping and 0.7 mm porcelain veneer configuration after artificial aging. Bovine incisors received crown preparation and Y-TZP crowns were manufactured using CAD/CAM technique, according to the following groups (n=10: Polished monolithic zirconia crowns (PM; Glazed monolithic zirconia crowns (GM; Bi-layer crowns (BL. Crowns were cemented with resin cement, submitted to artificial aging in a chewing simulator (2.5 million cycles/80 N/artificial saliva/37°C, and tested for fracture strength. Two remaining crowns referring to PM and GM groups were submitted to a chemical composition analysis to measure the level of yttrium after aging. One-way ANOVA and Tukey’s test (P=.05 indicated that monolithic zirconia crowns presented similar fracture strength (PM=3476.2 N ± 791.7; GM=3561.5 N ± 991.6, which was higher than bilayer crowns (2060.4 N ± 810.6. There was no difference in the yttrium content among the three surfaces evaluated in the monolithic crowns. Thus, monolithic zirconia crowns present higher fracture strength than bilayer veneered zirconia after artificial aging and surface finishing does not affect their fracture strength.

Dispersive liquid-liquid microextraction followed by flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) determination of 14 lanthanides from ground water

International Nuclear Information System (INIS)

Chandrasekaran, K.; Karunasagar, D.; Arunachalam, J.

2011-01-01

The aim of the present work was to develop a dispersive liquid-liquid microextraction (DLLME) method for the sensitive determination of REEs at a few parts per billion in groundwater by flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS). In the developed method, methanol (500 μl) and chloroform (200μl) were used as the disperser and extractant respectively. The REEs were complexed with 4-(2-pyridylazo resorcinol) (PAR) at a pH of 7. Acetate ion was added as an auxiliary ligand for neutralization of the charge on the lanthanide-PAR complex. The disperser (MeOH) - extraction solvent (CHCl 3 ) mixture was rapidly injected using a disposable syringe, thereby forming a cloudy solution. The lanthanide-PAR complex was extracted into the fine droplets of the chloroform dispersed in the aqueous phase. The solution was centrifuged and the aqueous layer at the top was discarded. The REEs were back extracted from the chloroform layer with nitric acid for determination by ICPMS. Important parameters for complex formation and extraction, such as volume of extraction/disperser solvent, extraction time, pH and concentration of the chelating agent and the auxiliary ligand are being optimized using ICP-MS. The optimization is being carried out at 5 μg L -1 concentration level of REE in the initial water sample. Preliminary studies have shown an extraction recovery of 80-85% for all the 14 lanthanide elements and these will be presented

Tannin-based monoliths from emulsion-templating

International Nuclear Information System (INIS)

Szczurek, A.; Martinez de Yuso, A.; Fierro, V.; Pizzi, A.; Celzard, A.

2015-01-01

Highlights: • Efficient preparation procedures are presented for new and “green” tannin-based organic polyHIPEs. • Highest homogeneity and strength are obtained at an oil fraction near the close-packing value. • Structural and mechanical properties abruptly change above such critical value. - Abstract: Highly porous monoliths prepared by emulsion-templating, frequently called polymerised High Internal Phase Emulsions (polyHIPEs) in the literature, were prepared from “green” precursors such as Mimosa bark extract, sunflower oil and ethoxylated castor oil. Various oil fractions, ranging from 43 to 80 vol.%, were used and shown to have a dramatic impact on the resultant porous structure. A critical oil fraction around 70 vol.% was found to exist, close to the theoretical values of 64% and 74% for random and compact sphere packing, respectively, at which the properties of both emulsions and derived porous monoliths changed. Such change of behaviour was observed by many different techniques such as viscosity, electron microscopy, mercury intrusion, and mechanical studies. We show and explain why this critical oil fraction is the one leading to the strongest and most homogeneous porous monoliths

All-optical SR flip-flop based on SOA-MZI switches monolithically integrated on a generic InP platform

Science.gov (United States)

Pitris, St.; Vagionas, Ch.; Kanellos, G. T.; Kisacik, R.; Tekin, T.; Broeke, R.; Pleros, N.

2016-03-01

At the dawning of the exaflop era, High Performance Computers are foreseen to exploit integrated all-optical elements, to overcome the speed limitations imposed by electronic counterparts. Drawing from the well-known Memory Wall limitation, imposing a performance gap between processor and memory speeds, research has focused on developing ultra-fast latching devices and all-optical memory elements capable of delivering buffering and switching functionalities at unprecedented bit-rates. Following the master-slave configuration of electronic Flip-Flops, coupled SOA-MZI based switches have been theoretically investigated to exceed 40 Gb/s operation, provided a short coupling waveguide. However, this flip-flop architecture has been only hybridly integrated with silica-on-silicon integration technology exhibiting a total footprint of 45x12 mm2 and intra-Flip-Flop coupling waveguide of 2.5cm, limited at 5 Gb/s operation. Monolithic integration offers the possibility to fabricate multiple active and passive photonic components on a single chip at a close proximity towards, bearing promises for fast all-optical memories. Here, we present for the first time a monolithically integrated all-optical SR Flip-Flop with coupled master-slave SOA-MZI switches. The photonic chip is integrated on a 6x2 mm2 die as a part of a multi-project wafer run using library based components of a generic InP platform, fiber-pigtailed and fully packaged on a temperature controlled ceramic submount module with electrical contacts. The intra Flip-Flop coupling waveguide is 5 mm long, reducing the total footprint by two orders of magnitude. Successful flip flop functionality is evaluated at 10 Gb/s with clear open eye diagram, achieving error free operation with a power penalty of 4dB.

Fabrication of mesoporous polymer monolith: a template-free approach.

Science.gov (United States)

Okada, Keisuke; Nandi, Mahasweta; Maruyama, Jun; Oka, Tatsuya; Tsujimoto, Takashi; Kondoh, Katsuyoshi; Uyama, Hiroshi

2011-07-14

Mesoporous polyacrylonitrile (PAN) monolith has been fabricated by a template-free approach using the unique affinity of PAN towards a water/dimethyl sulfoxide (DMSO) mixture. A newly developed Thermally Induced Phase Separation Technique (TIPS) has been used to obtain the polymer monoliths and their microstructures have been controlled by optimizing the concentration and cooling temperature.

Graphene oxide decorated with silver nanoparticles as a coating on a stainless-steel fiber for solid-phase microextraction.

Science.gov (United States)

Wang, Licheng; Hou, Xiudan; Li, Jubai; Liu, Shujuan; Guo, Yong

2015-07-01

A novel graphene oxide decorated with silver nanoparticles coating on a stainless-steel fiber for solid-phase microextraction was prepared. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid-phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single-fiber repeatability and fiber-to-fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4-116.3% with relative standard deviations less than 16.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Shear bond strength of indirect composite material to monolithic zirconia.

Science.gov (United States)

Sari, Fatih; Secilmis, Asli; Simsek, Irfan; Ozsevik, Semih

2016-08-01

This study aimed to evaluate the effect of surface treatments on bond strength of indirect composite material (Tescera Indirect Composite System) to monolithic zirconia (inCoris TZI). Partially stabilized monolithic zirconia blocks were cut into with 2.0 mm thickness. Sintered zirconia specimens were divided into different surface treatment groups: no treatment (control), sandblasting, glaze layer & hydrofluoric acid application, and sandblasting + glaze layer & hydrofluoric acid application. The indirect composite material was applied to the surface of the monolithic zirconia specimens. Shear bond strength value of each specimen was evaluated after thermocycling. The fractured surface of each specimen was examined with a stereomicroscope and a scanning electron microscope to assess the failure types. The data were analyzed using one-way analysis of variance (ANOVA) and Tukey LSD tests (α=.05). Bond strength was significantly lower in untreated specimens than in sandblasted specimens (Pcomposite material and monolithic zirconia.

Technology development for SOI monolithic pixel detectors

International Nuclear Information System (INIS)

Marczewski, J.; Domanski, K.; Grabiec, P.; Grodner, M.; Jaroszewicz, B.; Kociubinski, A.; Kucharski, K.; Tomaszewski, D.; Caccia, M.; Kucewicz, W.; Niemiec, H.

2006-01-01

A monolithic detector of ionizing radiation has been manufactured using silicon on insulator (SOI) wafers with a high-resistivity substrate. In our paper the integration of a standard 3 μm CMOS technology, originally designed for bulk devices, with fabrication of pixels in the bottom wafer of a SOI substrate is described. Both technological sequences have been merged minimizing thermal budget and providing suitable properties of all the technological layers. The achieved performance proves that fully depleted monolithic active pixel matrix might be a viable option for a wide spectrum of future applications

Gas-diffusion microextraction coupled with spectrophotometry for the determination of formaldehyde in cork agglomerates.

Science.gov (United States)

Brandão, Pedro F; Ramos, Rui M; Valente, Inês M; Almeida, Paulo J; Carro, Antonia M; Lorenzo, Rosa A; Rodrigues, José A

2017-04-01

In this work, a simple methodology was developed for the extraction and determination of free formaldehyde content in cork agglomerate samples. For the first time, gas-diffusion microextraction was used for the extraction of volatile formaldehyde directly from samples, with simultaneous derivatization with acetylacetone (Hantzsch reaction). The absorbance of the coloured solution was read in a spectrophotometer at 412 nm. Different extraction parameters were studied and optimized (extraction temperature, sample mass, volume of acceptor solution, extraction time and concentration of derivatization reagent) by means of an asymmetric screening. The developed methodology proved to be a reliable tool for the determination of formaldehyde in cork agglomerates with the following suitable method features: low LOD (0.14 mg kg -1 ) and LOQ (0.47 mg kg -1 ), r 2  = 0.9994, and intraday and interday precision of 3.5 and 4.9%, respectively. The developed methodology was applied to the determination of formaldehyde in different cork agglomerate samples, and contents between 1.9 and 9.4 mg kg -1 were found. Furthermore, formaldehyde was also determined by the standard method EN 717-3 for comparison purposes; no significant differences between the results of both methods were observed. Graphical abstract Representation of the GDME system and its main components.

Monolithic Chip-Integrated Absorption Spectrometer from 3-5 microns, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — A monolithically integrated indium phosphide (InP) to silicon-on-sapphire (SoS) platform is being proposed for a monolithic portable or handheld spectrometer between...

Surface characteristics and antibacterial activity of a silver-doped carbon monolith

Directory of Open Access Journals (Sweden)

Marija Vukčević et al

2008-01-01

Full Text Available A carbon monolith with a silver coating was prepared and its antimicrobial behaviour in a flow system was examined. The functional groups on the surface of the carbon monolith were determined by temperature-programmed desorption and Boehm's method, and the point of zero charge was determined by mass titration. The specific surface area was examined by N2 adsorption using the Brunauer, Emmett and Teller (BET method. As a test for the surface activity, the deposition of silver from an aqueous solution of a silver salt was used. The morphology and structure of the silver coatings were characterized by scanning electron microscopy and x-ray diffraction. The resistance to the attrition of the silver deposited on the carbon monolith was tested. The antimicrobial activity of the carbon monolith with a silver coating was determined using standard microbiological methods. Carbon monolith samples with a silver coating showed good antimicrobial activity against Escherichia coli, Staphylococcus aureus and Candida albicans, and are therefore suitable for water purification, particularly as personal disposable water filters with a limited capacity.

Molecularly Imprinted Porous Monolithic Materials from Melamine-Formaldehyde for Selective Trapping of Phosphopeptides

DEFF Research Database (Denmark)

Liu, Mingquan; Tran, Tri Minh; Abbas Elhaj, Ahmed Awad

2017-01-01

monoliths, chosen based on the combination of meso- and macropores providing optimal percolative flow and accessible surface area, was synthesized in the presence of N-Fmoc and O-Et protected phosphoserine and phosphotyrosine to prepare molecularly imprinted monoliths with surface layers selective...... for phosphopeptides. These imprinted monoliths were characterized alongside nonimprinted monoliths by a variety of techniques and finally evaluated by liquid chromatography-mass spectrometry in the capillary format to assess their abilities to trap and release phosphorylated amino acids and peptides from partly...

N-doped carbon nanotubes-reinforced hollow fiber solid-phase microextraction coupled with high performance liquid chromatography for the determination of phytohormones in tomatoes.

Science.gov (United States)

Han, Xiao-Fei; Chen, Juan; Shi, Yan-Ping

2018-08-01

A N-doped carbon nanotubes-reinforced hollow fiber solid-phase microextraction (N-doped CNTs-HF-SPME) method was developed for determination of two naphthalene-derived phytohormones, 1-naphthalene acetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA), at trace levels in tomatoes. N-doped CNTs were dispersed in ultrapure water with the assistance of surfactant, and then immobilized into the pores of hollow fiber by capillary forces and sonification. The resultant N-doped CNTs-HF was wetted with 1-octanol, subsequently immersed into the tomato samples to extract the target analytes under a magnetic stirring, and then desorbed with methanol by sonication prior to chromatographic analysis. Compared with CNTs, the surface hydrophilicity of N-doped CNTs was improved owing to the doping of nitrogen atoms, and a uniform dispersion was formed, thus greatly simplifying the preparation process and reducing waste of materials. In addition, N-doped CNTs-HF exhibits a more effective extraction performance for NAA and 2-NOA on account of the introduction of Lewis-basic nitrogen. It is worth to mention that owing to the clean-up function of HF, there are not any complicated sample pretreatment procedures prior to the microextraction. To achieve the highest extraction efficiency, important microextraction parameters including the length and the concentration level of N-doped CNTs in surfactant solution, extraction time, desorption conditions such as the type and volume of solvents, pH value, stirring rate and volume of the donor phase were thoroughly investigated and optimized. Under the optimal conditions, the method showed 165- and 123-fold enrichment factors of NAA and 2-NOA, good inter-fiber repeatability and batch-to-batch reproducibility, good linearity with correlation coefficients higher than 0.9990, low limits of detection and quantification (at ng g -1 levels), and satisfactory recoveries in the range of 83.10-108.32% at three spiked levels. The proposed method taking

Photoinitiated grafting of porous polymer monoliths and thermoplastic polymers for microfluidic devices

Science.gov (United States)

Frechet, Jean M. J. [Oakland, CA; Svec, Frantisek [Alameda, CA; Rohr, Thomas [Leiden, NL

2008-10-07

A microfluidic device preferably made of a thermoplastic polymer that includes a channel or a multiplicity of channels whose surfaces are modified by photografting. The device further includes a porous polymer monolith prepared via UV initiated polymerization within the channel, and functionalization of the pore surface of the monolith using photografting. Processes for making such surface modifications of thermoplastic polymers and porous polymer monoliths are set forth.

Liquid-phase microextraction approaches combined with atomic detection: A critical review

International Nuclear Information System (INIS)

Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2010-01-01

Liquid-phase microextraction (LPME) displays unique characteristics such as excellent preconcentration capability, simplicity, low cost, sample cleanup and integration of steps. Even though LPME approaches have the potential to be combined with almost every analytical technique, their use in combination with atomic detection techniques has not been exploited until recently. A comprehensive review dealing with the applications of liquid-phase microextraction combined with atomic detection techniques is presented. Theoretical features, possible strategies for these combinations as well as the effect of key experimental parameters influencing method development are addressed. Finally, a critical comparison of the different LPME approaches in terms of enrichment factors achieved, extraction efficiency, precision, selectivity and simplicity of operation is provided.

Fine-grain concrete from mining waste for monolithic construction

Science.gov (United States)

Lesovik, R. V.; Ageeva, M. S.; Lesovik, G. A.; Sopin, D. M.; Kazlitina, O. V.; Mitrokhin, A. A.

2018-03-01

The technology of a monolithic construction is a well-established practice among most Russian real estate developers. The strong points of the technology are low cost of materials and lower demand for qualified workers. The monolithic construction uses various types of reinforced slabs and foamed concrete, since they are easy to use and highly durable; they also need practically no additional treatment.

CHARACTERIZATION OF MONOLITHIC FUEL FOIL PROPERTIES AND BOND STRENGTH

International Nuclear Information System (INIS)

D E Burkes; D D Keiser; D M Wachs; J S Larson; M D Chapple

2007-01-01

Understanding fuel foil mechanical properties, and fuel/cladding bond quality and strength in monolithic plates is an important area of investigation and quantification. Specifically, what constitutes an acceptable monolithic fuel--cladding bond, how are the properties of the bond measured and determined, and what is the impact of fabrication process or change in parameters on the level of bonding? Currently, non-bond areas are quantified employing ultrasonic determinations that are challenging to interpret and understand in terms of irradiation impact. Thus, determining mechanical properties of the fuel foil and what constitutes fuel/cladding non-bonds is essential to successful qualification of monolithic fuel plates. Capabilities and tests related to determination of these properties have been implemented at the INL and are discussed, along with preliminary results

Controlling retention, selectivity and magnitude of EOF by segmented monolithic columns consisting of octadecyl and naphthyl monolithic segments--applications to RP-CEC of both neutral and charged solutes.

Science.gov (United States)

Karenga, Samuel; El Rassi, Ziad

2011-04-01

Monolithic capillaries made of two adjoining segments each filled with a different monolith were introduced for the control and manipulation of the electroosmotic flow (EOF), retention and selectivity in reversed phase-capillary electrochromatography (RP-CEC). These columns were called segmented monolithic columns (SMCs) where one segment was filled with a naphthyl methacrylate monolith (NMM) to provide hydrophobic and π-interactions, while the other segment was filled with an octadecyl acrylate monolith (ODM) to provide solely hydrophobic interaction. The ODM segment not only provided hydrophobic interactions but also functioned as the EOF accelerator segment. The average EOF of the SMC increased linearly with increasing the fractional length of the ODM segment. The neutral SMC provided a convenient way for tuning EOF, selectivity and retention in the absence of annoying electrostatic interactions and irreversible solute adsorption. The SMCs allowed the separation of a wide range of neutral solutes including polycyclic aromatic hydrocarbons (PAHs) that are difficult to separate using conventional alkyl-bonded stationary phases. In all cases, the k' of a given solute was a linear function of the fractional length of the ODM or NMM segment in the SMCs, thus facilitating the tailoring of a given SMC to solve a given separation problem. At some ODM fractional length, the fabricated SMC allowed the separation of charged solutes such as peptides and proteins that could not otherwise be achieved on a monolithic column made from NMM as an isotropic stationary phase due to the lower EOF exhibited by this monolith. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nearly 1000 Protein Identifications from 50 ng of Xenopus laevis Zygote Homogenate Using Online Sample Preparation on a Strong Cation Exchange Monolith Based Microreactor Coupled with Capillary Zone Electrophoresis.

Science.gov (United States)

Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Cox, Olivia F; Huber, Paul W; Dovichi, Norman J

2016-01-05

A sulfonate-silica hybrid strong cation exchange monolith microreactor was synthesized and coupled to a linear polyacrylamide coated capillary for online sample preparation and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) bottom-up proteomic analysis. The protein sample was loaded onto the microreactor in an acidic buffer. After online reduction, alkylation, and digestion with trypsin, the digests were eluted with 200 mM ammonium bicarbonate at pH 8.2 for CZE-MS/MS analysis using 1 M acetic acid as the background electrolyte. This combination of basic elution and acidic background electrolytes results in both sample stacking and formation of a dynamic pH junction. 369 protein groups and 1274 peptides were identified from 50 ng of Xenopus laevis zygote homogenate, which is comparable with an offline sample preparation method, but the time required for sample preparation was decreased from over 24 h to less than 40 min. Dramatically improved performance was produced by coupling the reactor to a longer separation capillary (∼100 cm) and a Q Exactive HF mass spectrometer. 975 protein groups and 3749 peptides were identified from 50 ng of Xenopus protein using the online sample preparation method.

Solid-phase microextraction

DEFF Research Database (Denmark)

Nilsson, Torben

The objective of this study has been to develop new analytical methods using the rapid, simple and solvent-free extraction technique solid-phase microextraction (SPME) for the quantitative analysis of organic pollutants at trace level in drinking water and environmental samples. The dynamics...... of SPME were examined for halogenated and non-halogenated volatile hydrocarbons, and a standard method for their quantitative analysis in aqueous samples was developed and validated in inter-laboratory studies on the basis of reference material and in comparison with the traditional methods....... The influences of some possible interferences on the SPME process were examined, and new SPME probes were tested for the in situ monitoring of groundwater pollutants. Inter-laboratory studies were carried out also for the validation of SPME for the quantitative analysis of organochlorine, organonitrogen...

Methacrylate-bonded covalent-organic framework monolithic columns for high performance liquid chromatography.

Science.gov (United States)

Liu, Li-Hua; Yang, Cheng-Xiong; Yan, Xiu-Ping

2017-01-06

Covalent-organic frameworks (COFs) are a newfangled class of intriguing microporous materials. Considering their unique properties, COFs should be promising as packing materials for high performance liquid chromatography (HPLC). However, the irregular shape and sub-micrometer size of COFs synthesized via the traditional methods render the main obstacles for the application of COFs in HPLC. Herein, we report the preparation of methacrylate-bonded COF monolithic columns for HPLC to overcome the above obstacles. The prepared COF bonded monolithic columns not only show good homogeneity and permeability, but also give high column efficiency, good resolution and precision for HPLC separation of small molecules including polycyclic aromatic hydrocarbons, phenols, anilines, nonsteroidal anti-inflammatory drugs and benzothiophenes. Compared with the bare polymer monolithic column, the COF bonded monolithic columns show enhanced hydrophobic, π-π and hydrogen bond interactions in reverse phase HPLC. The results reveal the great potential of COF bonded monoliths for HPLC and COFs in separation sciences. Copyright © 2016 Elsevier B.V. All rights reserved.

A new polyethylene glycol fiber prepared by coating porous zinc electrodeposited onto silver for solid-phase microextraction of styrene

International Nuclear Information System (INIS)

Sungkaew, Sakchaibordee; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

2010-01-01

A new polyethylene glycol fiber was developed for solid-phase microextraction (SPME) of styrene by electrodepositing porous Zn film on Ag wire substrate followed by coating with polyethylene glycol sol-gel (Ag/Zn/PEG sol-gel fiber). The scanning electron micrographs of fibers surface revealed a highly porous structure. The extraction property of the developed fiber-to-styrene residue from polystyrene packaged food was investigated by headspace solid-phase microextraction (HS-SPME) and analyzed with a gas chromatograph coupled with flame ionization detection (GC-FID). The new Ag/Zn/PEG sol-gel fiber is simple to prepare, low cost, robust, has high thermal stability and long lifetime, up to 359 extractions. Repeatability of one fiber (n = 6) was in the range of 4.7-7.5% and fiber-to-fiber reproducibility (n = 4) for five concentration values were in the range 3.4-10%. This Ag/Zn/PEG sol-gel fiber was compared to two commercial SPME fibers, 75 μm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 μm polydimethylsiloxane (PDMS). Under their optimum conditions, Ag/Zn/PEG sol-gel fiber showed the highest sensitivity and the lowest detection limit at 0.28 ± 0.01 ng mL -1 .

Two-dimensional thermal analysis of radial heat transfer of monoliths in small-scale steam methane reforming

DEFF Research Database (Denmark)

Cui, Xiaoti; Kær, Søren Knudsen

2018-01-01

Monolithic catalysts have received increasing attention for application in the small-scale steam methane reforming process. The radial heat transfer behaviors of monolith reformers were analyzed by two-dimensional computational fluid dynamic (CFD) modeling. A parameter study was conducted...... by a large number of simulations focusing on the thermal conductivity of the monolith substrate, washcoat layer, wall gap, radiation heat transfer and the geometric parameters (cell density, porosity and diameter of monolith). The effective radial thermal conductivity of the monolith structure, kr......,eff, showed good agreement with predictions made by the pseudo-continuous symmetric model. This influence of the radiation heat transfer is low for highly conductive monoliths. A simplified model has been developed to evaluate the importance of radiation for monolithic reformers under different conditions...

A novel surface modification technique for forming porous polymer monoliths in poly(dimethylsiloxane).

Science.gov (United States)

Burke, Jeffrey M; Smela, Elisabeth

2012-03-01

A new method of surface modification is described for enabling the in situ formation of homogenous porous polymer monoliths (PPMs) within poly(dimethylsiloxane) (PDMS) microfluidic channels that uses 365 nm UV illumination for polymerization. Porous polymer monolith formation in PDMS can be challenging because PDMS readily absorbs the monomers and solvents, changing the final monolith morphology, and because PDMS absorbs oxygen, which inhibits free-radical polymerization. The new approach is based on sequentially absorbing a non-hydrogen-abstracting photoinitiator and the monomers methyl methacrylate and ethylene diacrylate within the walls of the microchannel, and then polymerizing the surface treatment polymer within the PDMS, entangled with it but not covalently bound. Four different monolith compositions were tested, all of which yielded monoliths that were securely anchored and could withstand pressures exceeding the bonding strength of PDMS (40 psi) without dislodging. One was a recipe that was optimized to give a larger average pore size, required for low back pressure. This monolith was used to concentrate and subsequently mechanical lyse B lymphocytes.

Solid-phase microextraction for the analysis of biological samples

NARCIS (Netherlands)

Theodoridis, G; Koster, EHM; de Jong, GJ

2000-01-01

Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS

Directory of Open Access Journals (Sweden)

Shifu Peng

2013-01-01

Full Text Available Geosmin and 2-MIB are responsible for the majority of earthy and musty events related to the drinking water. These two odorants have extremely low odor threshold concentrations at ng L−1 level in the water, so a simple and sensitive method for the analysis of such trace levels was developed by headspace solid-phase microextraction coupled to gas chromatography/mass spectrometry. In this study, the orthogonal experiment design L32 (49 was applied to arrange and optimize experimental conditions. The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v; rotate-speed, 600 rpm; solution pH, 5.0. Under the optimized conditions, limits of detection (S/N=3 were 0.04 and 0.13 ng L−1 for geosmin and 2-MIB, respectively. Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them. Finally, the proposed method was applied to water samples, which were previously analyzed and confirmed to be free of target analytes. Besides, the proposal method was applied to test environmental water samples. The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

Microwave-assisted ionic liquid homogeneous liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of anthraquinones in Rheum palmatum L.

Science.gov (United States)

Wang, Zhibing; Hu, Jianxue; Du, Hongxia; He, Shuang; Li, Qing; Zhang, Hanqi

2016-06-05

The microwave-assisted ionic liquid homogeneous liquid-liquid microextraction (MA-IL-HLLME) coupled with high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones, including aloe-emodin, emodin, chrysophanol and physcion in root of Rheum palmatum L. Several experimental parameters influencing the extraction efficiency, including amount of sample, type and volume of ionic liquid, volume and pH value of extraction medium, microwave power and extraction time, concentration of NH4PF6 as well as centrifugal condition were optimized. When 140μL of ionic liquid ([C8MIM][BF4]) was used as an extraction solvent, target analytes can be extracted from sample matrix in one minute with the help of microwave irradiation. The MA-IL-HLLME is simple and quick. The calibration curves exhibited good linear relationship (r>0.9984). The limits of detection and quantification were in the range of 0.015-0.026 and 0.051-0.088μgmL(-1), respectively. The spiked recovery for each analyte was in the range of 81.13-93.07% with relative standard deviations lower than 6.89%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with ultrasonic and heat reflux extraction. The results indicated that the present method can be successfully applied to the determination of anthraquinones in medicinal plant. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

Science.gov (United States)

Hemmati, Maryam; Asghari, Alireza; Bazregar, Mohammad; Rajabi, Maryam

2016-11-01

In this research work, an efficient tandem dispersive liquid-liquid microextraction (TDLLME) procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was successfully applied for the determination of beta-blockers in human plasma and pharmaceutical wastewater samples. High clean-up and preconcentration factor are easily and rapidly feasible via this novel, cheap, and safe microextraction method, leading to high quality experimental data. It consists of two sequential dispersive liquid-liquid microextraction methods, accomplished via air/ultrasonic agitation and air agitation, respectively. In order to enrich the optimal values for the mentioned procedures, the Box-Behnken design (BBD) combined with the desirability function (DF) was used. The optimum values were found to be 11.0 % (w/v) of the salt amount, an initial pH value of 12.0, 103 μL of organic extractant phase, and 45 μL of aqueous extractant phase with pH value of 2.0, resulted in reasonable recovery percentages with a logical desirability. Under optimal experimental conditions, good linear ranges (3-2000 ng mL -1 for metoprolol and 2.5-2500 ng mL -1 for propranolol with the correlation of determinations (R 2 s) higher than 0.99) and low limits of detection (0.8 and 1.0 ng mL -1 for propranolol and metoprolol, respectively) were obtainable. Also, TDLLME-HPLC-UV provided good proper repeatabilities (relative standard deviations (RSDs) below 5.7 %, n = 3) and high enrichment factors (EFs) of 75-100. Graphical abstract TDLLME of beta-blockers from complicated matrices.

Affinity monolith chromatography: A review of principles and recent analytical applications

Science.gov (United States)

Pfaunmiller, Erika L.; Paulemond, Marie Laura; Dupper, Courtney M.; Hage, David S.

2012-01-01

Affinity monolith chromatography (AMC) is a type of liquid chromatography that uses a monolithic support and a biologically-related binding agent as a stationary phase. AMC is a powerful method for the selective separation, analysis or studies of specific target compounds in a sample. This review discusses the basic principles of AMC and recent developments or applications of this method, with particular emphasis being given to work that has appeared in the last five years. Various materials that have been used to prepare columns for AMC are examined, including organic monoliths, silica monoliths, agarose monoliths and cryogels. These supports have been used in AMC for formats that have ranged from traditional columns to disks, microcolumns and capillaries. Many binding agents have also been employed in AMC, such as antibodies, enzymes, proteins, lectins, immobilized metal-ions and dyes. Some applications that have been reported with these binding agents in AMC are bioaffinity chromatography, immunoaffinity chromatography or immunoextraction, immobilized metal-ion affinity chromatography, dye-ligand affinity chromatography, chiral separations and biointeraction studies. Examples are presented from fields that include analytical chemistry, pharmaceutical analysis, clinical testing and biotechnology. Current trends and possible future directions in AMC are also discussed. PMID:23187827

Preparation of porous polymer monoliths featuring enhanced surface coverage with gold nanoparticles

KAUST Repository

Lv, Yongqin

2012-10-01

A new approach to the preparation of porous polymer monoliths with enhanced coverage of pore surface with gold nanoparticles has been developed. First, a generic poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith was reacted with cystamine followed by the cleavage of its disulfide bonds with tris(2-carboxylethyl)phosphine, which liberated the desired thiol groups. Dispersions of gold nanoparticles with sizes varying from 5 to 40. nm were then pumped through the functionalized monoliths. The materials were then analyzed using both energy dispersive X-ray spectroscopy and thermogravimetric analysis. We found that the quantity of attached gold was dependent on the size of nanoparticles, with the maximum attachment of more than 60. wt% being achieved with 40. nm nanoparticles. Scanning electron micrographs of the cross sections of all the monoliths revealed the formation of a non-aggregated, homogenous monolayer of nanoparticles. The surface of the bound gold was functionalized with 1-octanethiol and 1-octadecanethiol, and these monolithic columns were used successfully for the separations of proteins in reversed phase mode. The best separations were obtained using monoliths modified with 15, 20, and 30. nm nanoparticles since these sizes produced the most dense coverage of pore surface with gold. © 2012 Elsevier B.V.

Chip-based magnetic solid phase microextraction coupled with ICP-MS for the determination of Cd and Se in HepG2 cells incubated with CdSe quantum dots.

Science.gov (United States)

Yu, Xiaoxiao; Chen, Beibei; He, Man; Wang, Han; Hu, Bin

2018-03-01

The quantification of trace Cd and Se in cells incubated with CdSe quantum dots (QDs) is critical to investigate the cytotoxicity of CdSe QDs. In this work, a miniaturized platform, namely chip-based magnetic solid phase microextraction (MSPME) packing with sulfhydryl group functionalized magnetic nanoparticles, was fabricated and combined with inductively coupled plasma mass spectrometry (ICP-MS) for the determination of trace Cd and Se in cells. Under the optimized conditions, the limits of detection (LOD) of the developed chip-based MSPME-ICP-MS system are 2.2 and 21ngL -1 for Cd and Se, respectively. The proposed method is applied successfully to the analysis of total and released small molecular fraction of Cd and Se in Human hepatocellular carcinoma cells (HepG2 cells) incubated with CdSe QDs, and the recoveries for the spiked samples are in the range of 86.0-109%. This method shows great promise to analyze cell samples and the obtained results are instructive to explore the cytotoxicity mechanism of CdSe QDs in cells. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwaves integrated circuits: hybrids and monolithics - fabrication technology

International Nuclear Information System (INIS)

Cunha Pinto, J.K. da

1983-01-01

Several types of microwave integrated circuits are presented together with comments about technologies and fabrication processes; advantages and disadvantages in their utilization are analysed. Basic structures, propagation modes, materials used and major steps in the construction of hybrid thin film and monolithic microwave integrated circuits are described. Important technological applications are revised and main activities of the microelectronics lab. of the University of Sao Paulo (Brazil) in the field of hybrid and monolithic microwave integrated circuits are summarized. (C.L.B.) [pt

Capillary electrochromatography immunoassay for alpha-fetoprotein based on poly(guanidinium ionic liquid) monolithic material.

Science.gov (United States)

Liu, Cuicui; Deng, Qiliang; Fang, Guozhen; Dang, Meng; Wang, Shuo

2017-08-01

Alpha-fetoprotein (AFP) is widely used as a tumor marker for the serum diagnosis of primary hepatoma. Sensitive detection of AFP level plays an important role in the early diagnosis of disease and highly reliable prediction. In this study, a novel non-competitive immunoassay (IA) based on poly(guanidinium ionic liquid) monolithic material was developed for detecting ultra trace levels of AFP in capillary electrochromatography (CEC) mode. The AFP was mixed with an excess amount of fluorescently labeled antibody. After incubation, the immunocomplex was separated from the free labeled antibody and detected by CEC coupled with laser-induced fluorescence detector. Under the optimized conditions, the developed CEC-IA performed a low detection limit of 0.05 μg L -1  (S/N = 3) and a wide linearity ranging from 0.1 to 1000 μg L -1 for AFP, which can be largely attributed to the high separation and enrichment efficiency of poly(guanidinium ionic liquid) monolithic material for the targets. The application of this method was demonstrated by determining AFP in human serum. Copyright © 2017. Published by Elsevier Inc.

Micro-Lid For Sealing Sample Reservoirs of micro-Extraction Systems

Data.gov (United States)

National Aeronautics and Space Administration — We propose to develop a proof-of-concept micro-Lid (µLid) to tightly seal a micro-sampler or micro-extraction system. Fabrication of µLid would be conducted in the...

Quantification of 4-hydroxy-2,5-dimethyl-3-furanone in fruit samples using solid phase microextraction coupled with gas chromatography-mass spectrometry.

Science.gov (United States)

Chen, Yong; Sidisky, Leonard M

2011-09-23

Furaneol is an important aroma compound. It is very difficult to extract furaneol from food matrices and separate it on a gas chromatography column due to its high polarity and instability. A new quantitative method was developed to quantify furaneol in aqueous samples by the use of derivatization/solid phase microextraction (SPME) coupled with gas chromatography/mass spectrometry (GC/MS). The derivatization was carried out by reacting pentafluorobenzyl bromide with furaneol in basic solutions at elevated temperatures. The derivative was stable and less polar so that SPME-GC/MS could be applied for extraction, separation and detection. The automated analytical method had a limit of detection (LOD) of 0.5 ng mL(-1), a limit of quantification (LOQ) of 2 ng mL(-1), a repeatability of 9.5%, and a linear range from 2 to 500 ng mL(-1). The method was applied to analyze fruit samples. And it was found that the concentrations of furaneol in tomato ranged from 95 to 173 μg kg(-1), in strawberries ranged from 1663 to 4852 μg kg(-1). The results were verified with a LC procedure. To facilitate analytical method development, some physico-chemical parameters for furaneol were determined in this work. Its solubility in water was determined as 0.315 g mL(-1) (25°C). Its LogD in water and LogP in 0.1 M phosphate buffer were -0.133 and 0.95 (20 °C), respectively. Its pKa was 8.56 (20 °C). Copyright © 2011 Elsevier B.V. All rights reserved.

Rapid method for the simultaneous detection of boar taint compounds by means of solid phase microextraction coupled to gas chromatography/mass spectrometry.

Science.gov (United States)

Verplanken, Kaat; Wauters, Jella; Van Durme, Jim; Claus, Dirk; Vercammen, Joeri; De Saeger, Sarah; Vanhaecke, Lynn

2016-09-02

Because of animal welfare issues, the voluntary ban on surgical castration of male piglets, starting January 2018 was announced in a European Treaty. One viable alternative is the fattening of entire male pigs. However, this can cause negative consumer reactions due to the occurrence of boar taint and possibly lead to severe economic losses in pig husbandry. In this study, headspace solid phase microextraction (HS-SPME) coupled to GC-MS was used in the development and optimization of a candidate method for fast and accurate detection of the boar taint compounds. Remarkably fast extraction (45s) of the boar taint compounds from adipose tissue was achieved by singeing the fat with a soldering iron while released volatiles were extracted in-situ using HS-SPME. The obtained method showed good performance characteristics after validation according to CD 2002/657/EC and ISO/IEC 17025 guidelines. Moreover, cross-validation with an in-house UHPLC-HR-Orbitrap-MS method showed good agreement between an in-laboratory method and the new candidate method for the fast extraction and detection of skatole and androstenone, which emphasizes the accuracy of this new SPME-GC-MS method. Threshold detection of the boar taint compounds on a portable GC-MS could not be achieved. However, despite the lack of sensitivity obtained on the latter instrument, a very fast method with run-to-run time of 3.5min for the detection of the boar taint compounds was developed. Copyright © 2016 Elsevier B.V. All rights reserved.

Role of nanoparticles in analytical solid phase microextraction (SPME)

NARCIS (Netherlands)

Zielinska, K.; Leeuwen, van H.P.

2013-01-01

Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

Determination of anabolic steroids in human urine by automated in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

Science.gov (United States)

Saito, Keita; Yagi, Katsuharu; Ishizaki, Atsushi; Kataoka, Hiroyuki

2010-09-05

A simple, rapid and sensitive method was developed for determining the presence of seven anabolic steroids (boldenone, nandrolone, testosterone, methyltestosterone, epiandrosterone, androsterone, and atnozolol) in human urine. Glucuronide-conjugates of these compounds were hydrolyzed with beta-glucuronidase. The anabolic steroids were analyzed by on-line in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). The steroids were separated within 14 min by high performance liquid chromatography using a Chromolith RP-18e column and 5 mM ammonium formate/methanol (35/65, v/v) as a mobile phase at a flow rate of 1.0 mL/min. Electrospray ionization conditions in the positive ion mode were optimized for the MS detection of these compounds. The optimum in-tube SPME conditions were 20 draw/eject cycles with a sample size of 40 microL using a Supel-Q PLOT capillary column for the extraction. The extracted compounds could be desorbed readily from the capillary column by flow of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM mode detection, good linearity of the calibration curve (r>0.995) was obtained in the concentration range of 0.5-20 ng/mL, except for stanozolol. The detection limits (S/N=3) of anabolic steroids were in the range 9-182 pg/mL and the proposed method showed 20-33-fold higher sensitivity than the direct injection method. The within-day and between-day precisions were below 4.0% and 7.3% (n=5), respectively. This method was applied successfully to the analysis of urine samples without the interference peaks. The recovery rates of anabolic steroids spiked into urine samples were above 85%. This method is useful to analyze the urinary levels of these compounds in anti-doping tests. 2010 Elsevier B.V. All rights reserved.

Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

Science.gov (United States)

Mills, G A; Walker, V

2000-12-01

Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

A Monolithic Perovskite Structure for Use as a Magnetic Regenerator

DEFF Research Database (Denmark)

Pryds, Nini; Clemens, Frank; Menon, Mohan

2011-01-01

A La0.67Ca0.26Sr0.07Mn1.05O3 (LCSM) perovskite was prepared for the first time as a ceramic monolithic regenerator used in a regenerative magnetic refrigeration device. The parameters influencing the extrusion process and the performance of the regenerator, such as the nature of the monolith paste...

Simple practical approach for sample loading prior to DNA extraction using a silica monolith in a microfluidic device.

Science.gov (United States)

Shaw, Kirsty J; Joyce, Domino A; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J

2009-12-07

A novel DNA loading methodology is presented for performing DNA extraction on a microfluidic system. DNA in a chaotropic salt solution was manually loaded onto a silica monolith orthogonal to the subsequent flow of wash and elution solutions. DNA was successfully extracted from buccal swabs using electro-osmotic pumping (EOP) coupled with in situ reagents contained within a 1.5% agarose gel matrix. The extracted DNA was of sufficient quantity and purity for polymerase chain reaction (PCR) amplification.

Monolithically integrated fiber-to-the-home diplexers and triplexers using a bilevel etched 2 x 2 optical coupler.

Science.gov (United States)

Zhang, Li; Wang, Lei; He, Jian-Jun

2009-09-01

A novel design of monolithically integrated diplexers and triplexers for fiber-to-the-home applications is presented. A bilevel etched asymmetrical 2 x 2 optical coupler is analyzed for efficient couplings of both upstream and downstream signals. The design of the diplexer is extended to a triplexer by adding an etched diffraction grating as an additional downstream demultiplexing element. The total size of the integrated diplexer and triplexer is smaller than 500 microm x 500 microm.

Cholesterol-imprinted macroporous monoliths: Preparation and characterization.

Science.gov (United States)

Stepanova, Mariia А; Kinziabulatova, Lilia R; Nikitina, Anna A; Korzhikova-Vlakh, Evgenia G; Tennikova, Tatiana B

2017-11-01

The development of sorbents for selective binding of cholesterol, which is a risk factor for cardiovascular disease, has a great importance for analytical science and medicine. In this work, two series of macroporous cholesterol-imprinted monolithic sorbents differing in the composition of functional monomers (methacrylic acid, butyl methacrylate, 2-hydroxyethyl methacrylate and ethylene dimethacrylate), amount of a template (4, 6 and 8 mol%) used for molecular imprinting, as well as mean pore size were synthesized by in situ free-radical process in stainless steel housing of 50 mm × 4.6 mm i.d. All prepared materials were characterized regarding to their hydrodynamic permeability and porous properties, as well as examined by BET and SEM methods. Imprinting factors, apparent dynamic dissociation constants, the maximum binding capacity, the number of theoretical plates and the height equivalent to a theoretical palate of MIP monoliths at different mobile phase flow rates were determined. The separation of a mixture of structural analogues, namely, cholesterol and prednisolone, was demonstrated. Additionally, the possibility of using the developed monoliths for cholesterol solid-phase extraction from simulated biological solution was shown. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Strength of normal sections of NPP composite monolithic constructions with ribbed reinforced panels

International Nuclear Information System (INIS)

Klyashitskij, V.I.; Kirillov, A.P.

1980-01-01

Strength characteristics and recommendations on designing composite-monolytic structures of NPP with ribbed reinforced panels are considered. Ribbed reinforced panel consists of a system of cross ribs joined with a comparatively thin (25 mm thick) plate. The investigations were carried on using models representing columns symmetrically reinforced with reinforced panels with a low percent of reinforcing. The monolithic structures consisting of ribbed reinforced panels and cast concrete for making monoliths as well as monolithic having analogous strength characteristics of extended and compressed zones have similar strengths. It is shown that calculation of supporting power of composite-monolithic structures is performed according to techniques developed for monolithic structures. Necessity of structural transverse fittings no longer arises in case of corresponding calculational substitution of stability of compressed parts of fittings. Supporting power of a structure decreases not more than by 10% in the presence of cracks in the reinforced panels of the compressed zone. Application of composite-monolithic structures during the construction of the Kursk, Smolensk and Chernobylskaya NPPs permitted to decrease labour content and reduce periods of accomplishment of these works which saves over 6 million roubles

Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

Science.gov (United States)

Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

2015-06-01

A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High density fuels using dispersion and monolithic fuel

Energy Technology Data Exchange (ETDEWEB)

Gomes, Daniel S.; Silva, Antonio T.; Abe, Alfredo Y.; Muniz, Rafael O.R.; Giovedi, Claudia, E-mail: dsgomes@ipen.br, E-mail: teixeira@ipen.br, E-mail: alfredo@ctmsp.mar.mil.br, E-mail: rafael.orm@gmail.com, E-mail: claudia.giovedi@ctmsp.mar.mil.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Universidade de São Paulo (USP), SP (Brazil). Departamento de Engenharia Naval e Oceânica

2017-07-01

Fuel plates used in high-performance research reactors need to be converted to low-enrichment uranium fuel; the fuel option based on a monolithic formulation requires alloys to contain 6 - 10 wt% Mo. In this case, the fuel plates are composed of the metallic alloy U-10Mo surrounded by a thin zirconium layer encapsulated in aluminum cladding. This study reviewed the physical properties of monolithic forms. The constraints produced during the manufacturing process were analyzed and compared to those of dispersed fuel. The bonding process used for dispersion fuels differs from the techniques applied to foil bonding used for pure alloys. The quality of monolithic plates depends on the fabrication method, which usually involves hot isostatic pressing and the thermal annealing effect of residual stress, which degrades the uranium cubic phase. The preservation of the metastable phase has considerable influence on fuel performance. The physical properties of the foil fuel under irradiation are superior to those of aluminum-dispersed fuels. The fuel meat, using zirconium as the diffusion barrier, prevents the interaction layer from becoming excessively thick. The problem with dispersed fuel is breakaway swelling with a medium fission rate. It has been observed that the fuel dispersed in aluminum was minimized in monolithic forms. The pure alloys exhibited a suitable response from a rate at least twice as much as the fission rate of dispersions. The foils can support fissile material concentration combined with a reduced swelling rate. (author)

High density fuels using dispersion and monolithic fuel

International Nuclear Information System (INIS)

Gomes, Daniel S.; Silva, Antonio T.; Abe, Alfredo Y.; Muniz, Rafael O.R.; Giovedi, Claudia; Universidade de São Paulo

2017-01-01

Fuel plates used in high-performance research reactors need to be converted to low-enrichment uranium fuel; the fuel option based on a monolithic formulation requires alloys to contain 6 - 10 wt% Mo. In this case, the fuel plates are composed of the metallic alloy U-10Mo surrounded by a thin zirconium layer encapsulated in aluminum cladding. This study reviewed the physical properties of monolithic forms. The constraints produced during the manufacturing process were analyzed and compared to those of dispersed fuel. The bonding process used for dispersion fuels differs from the techniques applied to foil bonding used for pure alloys. The quality of monolithic plates depends on the fabrication method, which usually involves hot isostatic pressing and the thermal annealing effect of residual stress, which degrades the uranium cubic phase. The preservation of the metastable phase has considerable influence on fuel performance. The physical properties of the foil fuel under irradiation are superior to those of aluminum-dispersed fuels. The fuel meat, using zirconium as the diffusion barrier, prevents the interaction layer from becoming excessively thick. The problem with dispersed fuel is breakaway swelling with a medium fission rate. It has been observed that the fuel dispersed in aluminum was minimized in monolithic forms. The pure alloys exhibited a suitable response from a rate at least twice as much as the fission rate of dispersions. The foils can support fissile material concentration combined with a reduced swelling rate. (author)

One-pot preparation of a mixed-mode organic-silica hybrid monolithic capillary column and its application in determination of endogenous gibberellins in plant tissues.

Science.gov (United States)

Zhang, Zheng; Hao, Yan-Hong; Ding, Jun; Xu, Sheng-Nan; Yuan, Bi-Feng; Feng, Yu-Qi

2015-10-16

A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix. Copyright © 2015 Elsevier B.V. All rights reserved.

Paladin Enterprises: Monolithic particle physics models global climate.

CERN Multimedia

2002-01-01

Paladin Enterprises presents a monolithic particle model of the universe which will be used by them to build an economical fusion energy system. The model is an extension of the work done by James Clerk Maxwell. Essentially, gravity is unified with electro-magnetic forces and shown to be a product of a closed loop current system, i.e. a particle - monolithic or sub atomic. This discovery explains rapid global climate changes which are evident in the geological record and also provides an explanation for recent changes in the global climate.

Solid-Phase Microextraction Coupled to Capillary Atmospheric Pressure Photoionization-Mass Spectrometry for Direct Analysis of Polar and Nonpolar Compounds.

Science.gov (United States)

Mirabelli, Mario F; Zenobi, Renato

2018-04-17

A novel capillary ionization source based on atmospheric pressure photoionization (cAPPI) was developed and used for the direct interfacing between solid-phase microextraction (SPME) and mass spectrometry (MS). The efficiency of the source was evaluated for direct and dopant-assisted photoionization, analyzing both polar (e.g., triazines and organophosphorus pesticides) and nonpolar (polycyclic aromatic hydrocarbons, PAHs) compounds. The results show that the range of compound polarity, which can be addressed by direct SPME-MS can be substantially extended by using cAPPI, compared to other sensitive techniques like direct analysis in real time (DART) and dielectric barrier discharge ionization (DBDI). The new source delivers a very high sensitivity, down to sub parts-per-trillion (ppt), making it a viable alternative when compared to previously reported and less comprehensive direct approaches.

A dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by injector port silylation coupled with gas chromatography-tandem mass spectrometry for the determination of nine bisphenols in bottled carbonated beverages.

Science.gov (United States)

Mandrah, Kapil; Satyanarayana, G N V; Roy, Somendu Kumar

2017-12-15

In the present study, a method has been efficiently developed for the first time to determine nine bisphenol analogues [bisphenol A (BPA), bisphenol C (BPC), bisphenol AF (BPAF), bisphenol E (BPE), bisphenol F (BPF), bisphenol G (BPG), bisphenol M (BPM), bisphenol S (BPS), and bisphenol Z (BPZ)] together in bottled carbonated beverages (collected from the local market of Lucknow, India) using dispersive liquid-liquid microextraction process. This is based on solidification of floating organic droplet (DLLME-SFO) followed by injector port silylation coupled with gas chromatography-tandem mass spectrometry. The process investigated parameters of DLLME-SFO (including the type of extraction and disperser solvents with their volumes, effect of pH, ionic strength, and the sample volume), factors influencing to injection port derivatization like, collision energy, injector port temperature, derivatizing reagent with sample injection volume, and type of organic solvent. BPA, BPF, BPZ, and BPS were detected in each sample; whereas, other bisphenols were also detected in some carbonated beverage samples. After optimizing the required conditions, good linearity of analytes was achieved in the range of 0.097-100ngmL -1 with coefficients of determination (R 2 )≥0.995. Intra-day and inter day precision of the method was good, with relative standard deviation (% RSD)≤10.95%. The limits of detection (LOD) and limits of quantification (LOQ) values of all bisphenols were ranged from 0.021 to 0.104ngmL -1 and 0.070 to 0.343ngmL -1 , respectively. The recovery of extraction was good (73.15-95.08%) in carbonated beverage samples and good enrichment factors (96.36-117.33) were found. Thus, the developed method of microextraction was highly precise, fast, and reproducible to determine the level of contaminants in bottled carbonated beverages. Copyright © 2017 Elsevier B.V. All rights reserved.

Broadband EM Performance Characteristics of Single Square Loop FSS Embedded Monolithic Radome

Directory of Open Access Journals (Sweden)

Raveendranath U. Nair

2013-01-01

Full Text Available A monolithic half-wave radome panel, centrally loaded with aperture-type single square loop frequency selective surface (SSL-FSS, is proposed here for broadband airborne radome applications. Equivalent transmission line method in conjunction with equivalent circuit model (ECM is used for modeling the SSL-FSS embedded monolithic half-wave radome panel and evaluating radome performance parameters. The design parameters of the SSL-FSS are optimized at different angles of incidence such that the new radome wall configuration offers superior EM performance from L-band to X-band as compared to the conventional monolithic half-wave slab of identical material and thickness. The superior EM performance of SSL-FSS embedded monolithic radome wall makes it suitable for the design of normal incidence and streamlined airborne radomes.

Fabrication of interfacial functionalized porous polymer monolith and its adsorption properties of copper ions

International Nuclear Information System (INIS)

Han, Jiaxi; Du, Zhongjie; Zou, Wei; Li, Hangquan; Zhang, Chen

2014-01-01

Highlights: • Interface functionalized PGMA porous monolith was fabricated. • The adsorption capacity of Cu 2+ was 35.3 mg/g. • The effects of porous structure on the adsorption of Cu 2+ were studied. • The adsorption behaviors of porous monolith were studied. - Abstract: The interfacial functionalized poly (glycidyl methacrylate) (PGMA) porous monolith was fabricated and applied as a novel porous adsorbent for copper ions (Cu 2+ ). PGMA porous material with highly interconnected pore network was prepared by concentrated emulsion polymerization template. Then polyacrylic acid (PAA) was grafted onto the interface of the porous monolith by the reaction between the epoxy group on PGMA and a carboxyl group on PAA. Finally, the porous monolith was interfacial functionalized by rich amount of carboxyl groups and could adsorb copper ions effectively. The chemical structure and porous morphology of the porous monolith were measured by Fourier transform infrared spectroscopy and scanning electron microscopy. Moreover, the effects of pore size distribution, pH value, co-existing ions, contacting time, and initial concentrations of copper ions on the adsorption capacity of the porous adsorbents were studied

Preparation and characterization of poly-(methacrylatoethyl trimethylammonium chloride-co-vinylbenzyl chloride-co-ethylene dimethacrylate monolith

Directory of Open Access Journals (Sweden)

Eko Malis

2015-05-01

Full Text Available A polymer monolithic column, poly-(methacrylatoethyltrimethylammonium chloride-co-vinylbenzyl chloride-co-ethylene dimethacrylate or poly-(MATE-co-VBC-co-EDMA was successfully prepared in the current study by one-step thermally initiated in situ polymerization, confined in a steel tubing of 0.5 mm i.d. and 1/16” o.d. The monoliths were prepared from methacrylatoethyltrimethylammonium chloride (MATE and vinylbenzyl chloride (VBC as monomer and ethylene dimethacrylate (EDMA as crosslinker using a binary porogen system of 1-propanol and 1,4-butanediol. The inner wall of steel tubing was pretreated with 3-methacryloxypropyl-trimethoxysilane (MAPS. In order to obtain monolith with adequate column efficiency and low flow resistance, some parameters such as total monomer concentration (%T and crosslinker concentration (%C were optimized. The morphology of this monolith was assessed by scanning electron microscopy (SEM. The properties of the monolithic column, such as permeability, binding capacity, and pore size distribution were also characterized in detail. From the results of the characterization of all monolith variation, monolith with %T 30 %C 50 and %T 35 %C 50 give the best characteristic. These monoliths have high permeability, adequate molecular recognition sites (represented with binding capacity value of over 20 mg/mL, and have over 80% flow through pores in their pore structure contribute to low flow resistance. The resulted monolithic columns have promising potential for dual mode liquid chromatography. MATE may contribute for anion-exchange while VBC may responsible for reversed-phase liquid chromatography.

Monolithic optoelectronic integrated broadband optical receiver with graphene photodetectors

Directory of Open Access Journals (Sweden)

Cheng Chuantong

2017-07-01

Full Text Available Optical receivers with potentially high operation bandwidth and low cost have received considerable interest due to rapidly growing data traffic and potential Tb/s optical interconnect requirements. Experimental realization of 65 GHz optical signal detection and 262 GHz intrinsic operation speed reveals the significance role of graphene photodetectors (PDs in optical interconnect domains. In this work, a novel complementary metal oxide semiconductor post-backend process has been developed for integrating graphene PDs onto silicon integrated circuit chips. A prototype monolithic optoelectronic integrated optical receiver has been successfully demonstrated for the first time. Moreover, this is a firstly reported broadband optical receiver benefiting from natural broadband light absorption features of graphene material. This work is a perfect exhibition of the concept of monolithic optoelectronic integration and will pave way to monolithically integrated graphene optoelectronic devices with silicon ICs for three-dimensional optoelectronic integrated circuit chips.

Monolithic optoelectronic integrated broadband optical receiver with graphene photodetectors

Science.gov (United States)

Cheng, Chuantong; Huang, Beiju; Mao, Xurui; Zhang, Zanyun; Zhang, Zan; Geng, Zhaoxin; Xue, Ping; Chen, Hongda

2017-07-01

Optical receivers with potentially high operation bandwidth and low cost have received considerable interest due to rapidly growing data traffic and potential Tb/s optical interconnect requirements. Experimental realization of 65 GHz optical signal detection and 262 GHz intrinsic operation speed reveals the significance role of graphene photodetectors (PDs) in optical interconnect domains. In this work, a novel complementary metal oxide semiconductor post-backend process has been developed for integrating graphene PDs onto silicon integrated circuit chips. A prototype monolithic optoelectronic integrated optical receiver has been successfully demonstrated for the first time. Moreover, this is a firstly reported broadband optical receiver benefiting from natural broadband light absorption features of graphene material. This work is a perfect exhibition of the concept of monolithic optoelectronic integration and will pave way to monolithically integrated graphene optoelectronic devices with silicon ICs for three-dimensional optoelectronic integrated circuit chips.

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid composite coating for the headspace solid-phase microextraction and gas chromatography determination of several alcohols in soft drinks.

Science.gov (United States)

Wu, Mian; Zhang, Haibo; Zhao, Faqiong; Zeng, Baizhao

2014-11-19

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid (i.e., 1-hydroxyethyl-3-methyl imidazolium-bis[(trifluoromethyl)sulfonyl]imide) composite film was electrodeposited on a Pt wire for headspace solid-phase microextraction. The film showed nodular structure and had large specific surface. In addition, it displayed high thermal stability (up to 300°C) and durable property (could be used for more than 200 times). Coupled with gas chromatography-flame ionization detection, the resulting fiber was applied to the headspace solid-phase microextraction and determination of several alcohols (i.e., linalool, nonanol, terpineol, geraniol, decanol and dodecanol). It presented higher extraction capability in comparison with the poly(3,4-ethylenedioxythiophene) and commercial polydimethylsiloxane/divinylbenzene fiber. Under the optimized conditions, the linear ranges exceeded three magnitudes with correlation coefficients above 0.9952 and the low limits of detection were 34.2-81.3ng L(-1). For different alcohols the repeatabilities (defined as RSD) were alcohols in real samples with acceptable recoveries from 81.1% to 106.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

Monolitni katalizatori i reaktori: osnovne značajke, priprava i primjena (Monolith catalysts and reactors: preparation and applications

Directory of Open Access Journals (Sweden)

Tomašić, V.

2004-12-01

Full Text Available Monolithic (honeycomb catalysts are continuous unitary structures containing many narrow, parallel and usually straight channels (or passages. Catalytically active components are dispersed uniformly over the whole porous ceramic monolith structure (so-called incorporated monolithic catalysts or are in a layer of porous material that is deposited on the walls of channels in the monolith's structure (washcoated monolithic catalysts. The material of the main monolithic construction is not limited to ceramics but includes metals, as well. Monolithic catalysts are commonly used in gas phase catalytic processes, such as treatment of automotive exhaust gases, selective catalytic reduction of nitrogen oxides, catalytic removal of volatile organic compounds from industrial processes, etc. Monoliths continue to be the preferred support for environmental applications due to their high geometric surface area, different design options, low pressure drop, high temperature durability, mechanical strength, ease of orientation in a reactor and effectiveness as a support for a catalytic washcoat. As known, monolithic catalysts belong to the class of the structured catalysts and/or reactors (in some cases the distinction between "catalyst" and "reactor" has vanished. Structured catalysts can greatly intensify chemical processes, resulting in smaller, safer, cleaner and more energy efficient technologies. Monolith reactors can be considered as multifunctional reactors, in which chemical conversion is advantageously integrated with another unit operation, such as separation, heat exchange, a secondary reaction, etc. Finally, structured catalysts and/or reactors appear to be one of the most significant and promising developments in the field of heterogeneous catalysis and chemical engineering of the recent years. This paper gives a description of the background and perspectives for application and development of monolithic materials. Different methods and techniques

Improved detection limits for phthalates by selective solid-phase micro-extraction

KAUST Repository

Zia, Asif I.; Afsarimanesh, Nasrin; Xie, Li; Nag, Anindya; Al-Bahadly, I. H.; Yu, P. L.; Kosel, Jü rgen

2016-01-01

Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid

Stanley Kubrick and B.F. Skinner : Is a Teaching Machine a Monolith ?

OpenAIRE

浜野, 保樹; ハマノ, ヤスキ; Yasuki, Hamano

1990-01-01

The teaching machine invented by B.F. Skinner was recog-nized as one of few clear achievements of scientific pedagogy and even appeared in SF. Arthur C. Clarke who wrote the script of the SF movie "2001: A Space Odyssey" with Stanley Kubrick wanted to scientifically define a monolith to be a God who had given intelligence to our ancestors. In other words, he wanted to describe a monolith as a teaching machine as well as a God. However Kubrick did not want to make clear about what a monolith i...

Application of non-ionic surfactant as a developed method for the enhancement of two-phase solvent bar microextraction for the simultaneous determination of three phthalate esters from water samples.

Science.gov (United States)

Bandforuzi, Samereh Ranjbar; Hadjmohammadi, Mohammad Reza

2018-08-03

The extraction of phthalate esters (PEs) from aqueous matrices using two-phase solvent bar microextraction by organic micellar phase was investigated. A short hollow fiber immobilized with reverse micelles of Brij 35 surfactant in 1-octanol was served as the solvent bar for microextraction. Experimental results show that the extraction efficiency were much higher using two-phase solvent bar microextraction based on non-ionic surfactant than conventional two-phase solvent bar microextraction because of a positive effect of surfactant-containing extraction phase in promoting the partition process by non-ionic intermolecular forces such as polar and hydrophobicity interactions. The nature of the extraction solvent, type and concentration of non-ionic surfactant, extraction time, sample pH, temperature, stirring rate and ionic strength were the effecting parameters which optimized to obtain the highest extraction recovery. Analysis of recovered analytes was carried out with high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). Under the optimum conditions, linearity was observed in the range of 1-800 ng mL -1 for dimethylphthalate (DMP) and 0.5-800 ng mL -1 for diethylphthalate (DEP) and di-n-butyl phthalate (DBP) with correlation determination values above 0.99 for them. The limits of detection and quantification were ranged from 0.012 to 0.03 ng mL -1 and 0.04-0.1 ng mL -1 , respectively. The ranges of intra-day and inter-day RSD (n = 3) at 20 ng mL -1 of PEs were 1.8-2.1% and 2.1-2.6%, respectively. Results showed that developed method can be a very powerful, innovative and promising sample preparation technique in PEs analysis from environmental and drinking water samples. Copyright © 2018. Published by Elsevier B.V.

Translucency and Strength of High Translucency Monolithic Zirconium Oxide Materials

Science.gov (United States)

2016-05-17

Zirconium -Oxide Materials presented at/published to the Journal of General Dentistry with MDWI 41-108, and has been assigned local file #16208. 2...Zirconia-Oxide Materials 6. TITLE OF MATERIAL TO BE PUBLISHED OR PRESENTED: Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide...OBSOLETE 48. DATE Page 3 of 3 Pages Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide Materials Abstract Dental materials

Rapid determination of octanol-water partition coefficient using vortex-assisted liquid-liquid microextraction.

Science.gov (United States)

Román, Iván P; Mastromichali, Anna; Tyrovola, Konstantina; Canals, Antonio; Psillakis, Elefteria

2014-02-21

Vortex-assisted liquid-liquid microextraction (VALLME) coupled with high-performance liquid chromatography (HPLC) is proposed here for the rapid determination of octanol-water partitioning coefficients (Kow). VALLME uses vortex agitation, a mild emulsification procedure, to disperse microvolumes of octanol in the aqueous phase thus increasing the interfacial contact area and ensuring faster partitioning rates. With VALLME, 2min were enough to achieve equilibrium conditions between the octanolic and aqueous phases. Upon equilibration, separation was achieved using centrifugation and the octanolic microdrop was collected and analyzed in a HPLC system. Six model compounds with logKow values ranging between ∼0.5 and 3.5 were used during the present investigations. The proposed method produced logKow values that were consistent with previously published values and the recorded uncertainty was well within the acceptable log unit range. Overall, the key features of the proposed Kow determination procedure comprised speed, reliability, simplicity, low cost and minimal solvent consumption. Copyright © 2014 Elsevier B.V. All rights reserved.

A novel, SiPM-array-based, monolithic scintillator detector for PET

International Nuclear Information System (INIS)

Schaart, Dennis R; Dam, Herman T van; Seifert, Stefan; Beekman, Freek J; Vinke, Ruud; Dendooven, Peter; Loehner, Herbert

2009-01-01

Silicon photomultipliers (SiPMs) are of great interest to positron emission tomography (PET), as they enable new detector geometries, for e.g., depth-of-interaction (DOI) determination, are MR compatible, and offer faster response and higher gain than other solid-state photosensors such as avalanche photodiodes. Here we present a novel detector design with DOI correction, in which a position-sensitive SiPM array is used to read out a monolithic scintillator. Initial characterization of a prototype detector consisting of a 4 x 4 SiPM array coupled to either the front or back surface of a 13.2 mm x 13.2 mm x 10 mm LYSO:Ce 3+ crystal shows that front-side readout results in significantly better performance than conventional back-side readout. Spatial resolutions 2 detector, equals 960 ps FWHM.

A multiscale finite element method for modeling fully coupled thermomechanical problems in solids

KAUST Repository

Sengupta, Arkaprabha; Papadopoulos, Panayiotis; Taylor, Robert L.

2012-01-01

This article proposes a two-scale formulation of fully coupled continuum thermomechanics using the finite element method at both scales. A monolithic approach is adopted in the solution of the momentum and energy equations. An efficient implementation of the resulting algorithm is derived that is suitable for multicore processing. The proposed method is applied with success to a strongly coupled problem involving shape-memory alloys. © 2012 John Wiley & Sons, Ltd.

A multiscale finite element method for modeling fully coupled thermomechanical problems in solids

KAUST Repository

Sengupta, Arkaprabha

2012-05-18

This article proposes a two-scale formulation of fully coupled continuum thermomechanics using the finite element method at both scales. A monolithic approach is adopted in the solution of the momentum and energy equations. An efficient implementation of the resulting algorithm is derived that is suitable for multicore processing. The proposed method is applied with success to a strongly coupled problem involving shape-memory alloys. © 2012 John Wiley & Sons, Ltd.

Kinetic aspects of hollow fiber liquid-phase microextraction and electromembrane extraction

DEFF Research Database (Denmark)

Gjelstad, Astrid; Jensen, Henrik; Rasmussen, Knut Einar

2012-01-01

In this paper, extraction kinetics was investigated experimentally and theoretically in hollow fiber liquid-phase microextraction (HF-LPME) and electromembrane extraction (EME) with the basic drugs droperidol, haloperidol, nortriptyline, clomipramine, and clemastine as model analytes. In HF...

Headspace Solid-Phase Microextraction Analysis of Volatile Components in Phalaenopsis Nobby’s Pacific Sunset

Directory of Open Access Journals (Sweden)

Chih-Hsin Yeh

2014-09-01

Full Text Available Phalaenopsis is the most important economic crop in the Orchidaceae family. There are currently numerous beautiful and colorful Phalaenopsis flowers, but only a few species of Phalaenopsis have an aroma. This study reports the analysis volatile components present in P. Nobby’s Pacific Sunset by solid-phase microextraction (SPME coupled with gas chromatography (GC and gas chromatography/mass spectrometry (GC-MS. The results show that the optimal extraction conditions were obtained by using a DVB/CAR/PDMS fiber. A total of 31 compounds were identified, with the major compounds being geraniol, linalool and α-farnesene. P. Nobby’s Pacific Sunset had the highest odor concentration from 09:00 to 13:00 on the eighth day of storage. It was also found that in P. Nobby’s Pacific Sunset orchids the dorsal sepals and petals had the highest odor concentrations, whereas the column had the lowest.

Simultaneous Determination of Food-Related Biogenic Amines and Precursor Amino Acids Using in Situ Derivatization Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction by Ultra-High-Performance Liquid Chromatography Tandem Mass Spectrometry.

Science.gov (United States)

He, Yongrui; Zhao, Xian-En; Wang, Renjun; Wei, Na; Sun, Jing; Dang, Jun; Chen, Guang; Liu, Zhiqiang; Zhu, Shuyun; You, Jinmao

2016-11-02

A simple, rapid, sensitive, selective, and environmentally friendly method, based on in situ derivatization ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) coupled with ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) using multiple reaction monitoring (MRM) mode has been developed for the simultaneous determination of food-related biogenic amines and amino acids. A new mass-spectrometry-sensitive derivatization reagent 4'-carbonyl chloride rosamine (CCR) was designed, synthesized, and first reported. Parameters and conditions of in situ DUADLLME and UHPLC-MS/MS were optimized in detail. Under the optimized conditions, the in situ DUADLLME was completed speedily (within 1 min) with high derivatization efficiencies (≥98.5%). With the cleanup and concentration of microextraction step, good analytical performance was obtained for the analytes. The results showed that this method was accurate and practical for quantification of biogenic amines and amino acids in common food samples (red wine, beer, wine, cheese, sausage, and fish).

Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

Science.gov (United States)

Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

2017-04-14

An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg + ), ethylmercury (EtHg + ) and inorganic mercury (Hg 2+ ) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL -1 for EtHg + and 5-450ngL -1 for MeHg + and Hg 2+ . Limits of detection were 3.0ngL -1 for EtHg + and 1.5ngL -1 for MeHg + and Hg 2+ . Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%. Copyright © 2017 Elsevier B.V. All rights reserved.

Sensitive and simple determination of zwitterionic morphine in human urine based on liquid-liquid micro-extraction coupled with surface-enhanced Raman spectroscopy.

Science.gov (United States)

Yu, Borong; Cao, Chentai; Li, Pan; Mao, Mei; Xie, Qiwen; Yang, Liangbao

2018-08-15

Morphine, a kind of illicit drugs, is also one of the main heroin metabolites. In consideration of a noninvasive way to monitor and identify drug abuse during forensic cases, the urine samples are usually detected. Here, colloidal gold nanorods (Au NRs) were introduced to act as active substrate, because of the strong optical extinction and spectral tunability of the longitudinal surface plasmon resonance (SPR). Thus, well surface-enhanced Raman spectra of morphine even at low concentrations could be obtained by portable Raman spectrometer. For the complex matrix environment of urine, liquid-liquid micro-extraction (LLME), a simple and inexpensive pretreatment, was employed to avoid the interferences. And then, the coupled surface-enhanced Raman spectroscopy (SERS) can give full play to the advantages of high sensitivity and unique spectroscopic fingerprint. According to the zwitterionic structure and physicochemical parameters of morphine molecules, the pH value of urine sample was adjusted to about 9 by buffer solution (KOH/NaB 4 O 7 ) and the mixture of chloroform and isopropyl alcohol (V/V=9:1) was chosen as extractant. Moreover, such pretreatment was proved to be appropriate for separation and concentration of morphine from urine. The developed LLME-SERS method could provide a detection limit less than 1 ppm in the human urine environment and the whole process of detection just needed take 5-6 min. What's more, the results of urine samples from heroin users exhibited application value of the proposed technique. The excellent performance makes it promising to become a rapid, reliable, and on-spot analyzer, especially for public safety and healthcare. Copyright © 2018 Elsevier B.V. All rights reserved.

The effect of charged groups on hydrophilic monolithic stationary phases on their chromatographic properties.

Science.gov (United States)

Li, Haibin; Liu, Chusheng; Wang, Qiqin; Zhou, Haibo; Jiang, Zhengjin

2016-10-21

In order to investigate the effect of charged groups present in hydrophilic monolithic stationary phases on their chromatographic properties, three charged hydrophilic monomers, i.e. N,N-dimethyl-N-acryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPDA), [2-(acryloyloxy)ethyl]trimethylammonium chloride (AETA), and 3-sulfopropyl acrylate potassium salt (SPA) were co-polymerized with the crosslinker N,N'-methylenebisacrylamide (MBA), respectively. The physicochemical properties of the three resulting charged hydrophilic monolithic columns were evaluated using scanning electron microscopy, ζ-potential analysis and micro-HPLC. High column efficiency was obtained on the three monolithic columns at a linear velocity of 1mm/s using thiourea as test compound. Comparative characterization of the three charged HILIC phases was then carried out using a set of model compounds, including nucleobases, nucleosides, benzoic acid derivatives, phenols, β-blockers and small peptides. Depending on the combination of stationary phase/mobile phase/solute, both hydrophilic interaction and other potential secondary interactions, including electrostatic interaction, hydrogen-bonding interaction, molecular shape selectivity, could contribute to the over-all retention of the analytes. Because of the strong electrostatic interaction provided by the quaternary ammonium groups in the poly (AETA-co-MBA) monolith, this cationic HILIC monolith exhibited the strongest retention for benzoic acid derivatives and small peptides with distorted peak shapes and the weakest retention for basic β-blockers. The sulfonyl groups on the poly (SPA-co-MBA) hydrophilic monolith could provide strong electrostatic attraction and hydrogen bonding for positively charged analytes and hydrogen-donor/acceptor containing analytes, respectively. Therefore, basic drugs, nucleobases and nucleotides exhibited the strongest retention on this anionic monolith. Because of the weak but distinct cation exchange properties of

Speciation of chromium by dispersive liquid–liquid microextraction followed by laser-induced breakdown spectrometry detection (DLLME–LIBS)

OpenAIRE

Gaubeur, Ivanise; Aguirre Pastor, Miguel Ángel; Kovachev, Nikolay; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

2015-01-01

In this study, an analytical methodology based on a combination of dispersive liquid–liquid microextraction with laser-induced breakdown spectrometry was evaluated for simultaneous pre-concentration, speciation and detection of Cr. The microextraction procedure was based on the injection of appropriated quantities of 1-undecanol and ethanol into a sample solution containing the complexes formed between Cr(VI) and diethyldithiocarbamate (DDTC). The main experimental factors affecting the compl...

Fabrication of interfacial functionalized porous polymer monolith and its adsorption properties of copper ions

Energy Technology Data Exchange (ETDEWEB)

Han, Jiaxi; Du, Zhongjie; Zou, Wei; Li, Hangquan; Zhang, Chen, E-mail: zhangch@mail.buct.edu.cn

2014-07-15

Highlights: • Interface functionalized PGMA porous monolith was fabricated. • The adsorption capacity of Cu{sup 2+} was 35.3 mg/g. • The effects of porous structure on the adsorption of Cu{sup 2+} were studied. • The adsorption behaviors of porous monolith were studied. - Abstract: The interfacial functionalized poly (glycidyl methacrylate) (PGMA) porous monolith was fabricated and applied as a novel porous adsorbent for copper ions (Cu{sup 2+}). PGMA porous material with highly interconnected pore network was prepared by concentrated emulsion polymerization template. Then polyacrylic acid (PAA) was grafted onto the interface of the porous monolith by the reaction between the epoxy group on PGMA and a carboxyl group on PAA. Finally, the porous monolith was interfacial functionalized by rich amount of carboxyl groups and could adsorb copper ions effectively. The chemical structure and porous morphology of the porous monolith were measured by Fourier transform infrared spectroscopy and scanning electron microscopy. Moreover, the effects of pore size distribution, pH value, co-existing ions, contacting time, and initial concentrations of copper ions on the adsorption capacity of the porous adsorbents were studied.

Covalent attachment of polymeric monolith to polyether ether ketone (PEEK) tubing.

Science.gov (United States)

Lv, Chunguang; Heiter, Jaana; Haljasorg, Tõiv; Leito, Ivo

2016-08-17

A new method of reproducible preparation of vinylic polymeric monolithic columns with a key step of covalently anchoring the monolith to PEEK surface is described. In order to chemically attach the polymer monolith to the tube wall, methacrylate functional groups were introduced onto PEEK surface by a three-step procedure, including surface etching, surface reduction and surface methacryloylation. The chemical state of the modified tubing surface was characterized by attenuated total reflectance infrared (ATR-IR) spectroscopy. It was found that the etching step is the key to successfully modifying the PEEK tubing surface. Poly(styrene-co-divinylbenzene) monoliths were in situ synthesized by thermally initiated free radical copolymerization within the confines of surface-vinylized PEEK tubings of dimensions close to ones conventionally used in HPLC and UHPLC (1.6 mm internal diameter, 10.0-12.5 cm length). Adhesion test was done by measuring the operating pressure drop, which the prepared stationary phases can withstand. Good pressure resistance, up to 140 bar/10 cm (flow rate 0.5 mL min(-1), acetonitrile as a mobile phase), indicates strong bonding of monolith to the tubing wall. The monolithic material was proven to have a permeability of 1.7 × 10 (-14) m(2), applying acetonitrile-water 70:30 (v/v) as a mobile phase. The column performance was reproducible from column to column and was evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode (acetonitrile-water 70:30, v/v). The numbers of plates per meter at optimal flow rate were found to be between 26 000 and 32 000 for the different analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

Highly crosslinked polymeric monoliths for reversed-phase capillary liquid chromatography of small molecules.

Science.gov (United States)

Liu, Kun; Tolley, H Dennis; Lee, Milton L

2012-03-02

Seven crosslinking monomers, i.e., 1,3-butanediol dimethacrylate (1,3-BDDMA), 1,4-butanediol dimethacrylate (1,4-BDDMA), neopentyl glycol dimethacrylate (NPGDMA), 1,5-pentanediol dimethacrylate (1,5-PDDMA), 1,6-hexanediol dimethacrylate (1,6-HDDMA), 1,10-decanediol dimethacrylate (1,10-DDDMA), and 1,12-dodecanediol dimethacrylate (1,12-DoDDMA), were used to synthesize highly cross-linked monolithic capillary columns for reversed-phase liquid chromatography (RPLC) of small molecules. Dodecanol and methanol were chosen as "good" and "poor" porogenic solvents, respectively, for these monoliths, and were investigated in detail to provide insight into the selection of porogen concentration using 1,12-DoDDMA. Isocratic elution of alkylbenzenes at a flow rate of 300 nL/min was conducted for all of the monoliths. Gradient elution of alkylbenzenes and alkylparabens provided high resolution separations. Optimized monoliths synthesized from all seven crosslinking monomers showed high permeability. Several of the monoliths demonstrated column efficiencies in excess of 50,000 plates/m. Monoliths with longer alkyl-bridging chains showed very little shrinking or swelling in solvents of different polarities. Column preparation was highly reproducible; the relative standard deviation (RSD) values (n=3) for run-to-run and column-to-column were less than 0.25% and 1.20%, respectively, based on retention times of alkylbenzenes. Copyright © 2012 Elsevier B.V. All rights reserved.

Multivariate study of parameters in the determination of pesticide residues in apple by headspace solid phase microextraction coupled to gas chromatography-mass spectrometry using experimental factorial design.

Science.gov (United States)

Abdulra'uf, Lukman Bola; Tan, Guan Huat

2013-12-15

Solid-phase microextraction (SPME) is a solvent-less sample preparation method which combines sample preparation, isolation, concentration and enrichment into one step. In this study, multivariate strategy was used to determine the significance of the factors affecting the solid phase microextraction of pesticide residues (fenobucarb, diazinon, chlorothalonil and chlorpyrifos) using a randomised factorial design. The interactions and effects of temperature, time and salt addition on the efficiency of the extraction of the pesticide residues were evaluated using 2(3) factorial designs. The analytes were extracted with 100 μm PDMS fibres according to the factorial design matrix and desorbed into a gas chromatography-mass spectrometry detector. The developed method was applied for the analysis of apple samples and the limits of detection were between 0.01 and 0.2 μg kg(-)(1), which were lower than the MRLs for apples. The relative standard deviations (RSD) were between 0.1% and 13.37% with average recovery of 80-105%. The linearity ranges from 0.5-50 μg kg(-)(1) with correlation coefficient greater than 0.99. Copyright © 2013 Elsevier Ltd. All rights reserved.

Molecularly imprinted sol-gel nanofibers based solid phase microextraction coupled on-line with high performance liquid chromatography for selective determination of acesulfame.

Science.gov (United States)

Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-Adergani, Behrouz

2015-03-01

Sol-gel based molecularly imprinted polymer (MIP) nanofiber was successfully fabricated by electrospinning technique on the surface of a stainless steel bar. The manufactured tool was applied for on-line selective solid phase microextraction (SPME) and determination of acesulfame (ACF) as an artificial sweetener with high performance liquid chromatography (HPLC). The selective ability of method for the extraction of ACF was investigated in the presence of some selected sweeteners such as saccharine (SCH), aspartame (ASP) and caffeine (CAF). Electrospinning of MIP sol-gel solution on the stainless steel bar provided an unbreakable sorbent with high thermal, mechanical, and chemical stability. Moreover, application of the MIP-SPME tool revealed a unique approach for the selective microextraction of the analyte in beverage samples. In this work, 3-(triethoxysilyl)-propylamine (TMSPA) was chosen as a precursor due to its ability to imprint the analyte by hydrogen bonding, Van der Walls, and dipole-dipole interactions. Nylon 6 was also added as a backbone and support for the precursor in which sol could greatly growth during the sol-gel process and makes the solution electrospinable. Various effective parameters in the extraction efficiency of the MIP-SPME tool such as loading time, flow rate, desorption time, selectivity, and the sample volume were evaluated. The linearity for the ACF in beverage sample was in the range of 0.78-100.5 ng mL(-1). Limit of detection (LOD) and quantification (LOQ) were 0.23 and 0.78 ng mL(-1) respectively. The RSD values (n=5) were all below 3.5%at the 20 ng mL(-1) level. Copyright © 2014 Elsevier B.V. All rights reserved.

A facile approach for the synthesis of monolithic hierarchical porous carbons – high performance materials for amine based CO2 capture and supercapacitor electrode

KAUST Repository

Estevez, Luis

2013-05-03

An ice templating coupled with hard templating and physical activation approach is reported for the synthesis of hierarchically porous carbon monoliths with tunable porosities across all three length scales (macro- meso- and micro), with ultrahigh specific pore volumes [similar]11.4 cm3 g−1. The materials function well as amine impregnated supports for CO2 capture and as supercapacitor electrodes.

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

Science.gov (United States)

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

Porous polymer monolithic col

Directory of Open Access Journals (Sweden)

Lydia Terborg

2015-05-01

Full Text Available A new approach has been developed for the preparation of mixed-mode stationary phases to separate proteins. The pore surface of monolithic poly(glycidyl methacrylate-co-ethylene dimethacrylate capillary columns was functionalized with thiols and coated with gold nanoparticles. The final mixed mode surface chemistry was formed by attaching, in a single step, alkanethiols, mercaptoalkanoic acids, and their mixtures on the free surface of attached gold nanoparticles. Use of these mixtures allowed fine tuning of the hydrophobic/hydrophilic balance. The amount of attached gold nanoparticles according to thermal gravimetric analysis was 44.8 wt.%. This value together with results of frontal elution enabled calculation of surface coverage with the alkanethiol and mercaptoalkanoic acid ligands. Interestingly, alkanethiols coverage in a range of 4.46–4.51 molecules/nm2 significantly exceeded that of mercaptoalkanoic acids with 2.39–2.45 molecules/nm2. The mixed mode character of these monolithic stationary phases was for the first time demonstrated in the separations of proteins that could be achieved in the same column using gradient elution conditions typical of reverse phase (using gradient of acetonitrile in water and ion exchange chromatographic modes (applying gradient of salt in water, respectively.

Solid State Characterizations of Long-Term Leached Cast Stone Monoliths

Energy Technology Data Exchange (ETDEWEB)

Asmussen, Robert M.; Pearce, Carolyn I.; Parker, Kent E.; Miller, Brian W.; Lee, Brady D.; Buck, Edgar C.; Washton, Nancy M.; Bowden, Mark E.; Lawter, Amanda R.; McElroy, Erin M.; Serne, R Jeffrey

2016-09-30

This report describes the results from the solid phase characterization of six Cast Stone monoliths from the extended leach tests recently reported on (Serne et al. 2016),that were selected for characterization using multiple state-of-the-art approaches. The Cast Stone samples investigated were leached for > 590 d in the EPA Method 1315 test then archived for > 390 d in their final leachate. After reporting the long term leach behavior of the monoliths (containing radioactive ⁹⁹Tc and stable ¹²⁷I spikes and for original Westsik et al. 2013 fabricated monoliths, ²³⁸U), it was suggested that physical changes to the waste forms and a depleting inventory of contaminants of potential concern may mean that effective diffusivity calculations past 63 d should not be used to accurately represent long-term waste form behavior. These novel investigations, in both length of leaching time and application of solid state techniques, provide an initial arsenal of techniques which can be utilized to perform such Cast Stone solid phase characterization work, which in turn can support upcoming performance assessment maintenance. The work was performed at Pacific Northwest National Laboratory (PNNL) for Washington River Protection Solutions (WRPS) to characterize several properties of the long- term leached Cast Stone monolith samples.

Solid phase microextraction.

Science.gov (United States)

Pawliszyn, J

2001-01-01

Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

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.

Ion-pair vortex assisted liquid-liquid microextraction with back extraction coupled with high performance liquid chromatography-UV for the determination of metformin in plasma.

Science.gov (United States)

Alshishani, Anas; Makahleh, Ahmad; Yap, Hui Fang; Gubartallah, Elbaleeq Adam; Salhimi, Salizawati Muhamad; Saad, Bahruddin

2016-12-01

A new sample preparation method, ion-pair vortex assisted liquid-liquid microextraction (VALLME-BE), for the determination of a highly polar anti-diabetic drug (metformin) in plasma sample was developed. The VALLME-BE was performed by diluting the plasma in borate buffer and extracted to 150µL 1-octanol containing 0.2M di-(2-ethylhexyl)phosphoric acid as intermediate phase. The drug was next back-extracted into 20µL of 0.075M HCl solution. The effects of pH, ion-pair concentration, type of organic solvent, volume of extraction phases, ionic strength, vortexing and centrifugation times on the extraction efficiency were investigated. The optimum conditions were at pH 9.3, 60s vortexing and 2min centrifugation. The microextract, contained metformin and buformin (internal standard), was directly injected into a HPLC unit using C1 column (250mm×4.6mm×10µm) and detected at 235nm. The method was validated and calibration curve was linear with r 2 >0.99 over the range of 20-2000µgL -1 . The limits of detection and quantitation were 1.4 and 4.1µgL -1 , respectively. The accuracy was within 94.8-108% of the nominal concentration. The relative standard deviation for inter- and intra-day precision was less than 10.8%. The method was conveniently applied for the determination of metformin in plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of benzo[a]pyrene in edible oils using phase-transfer-catalyst-assisted saponification and supramolecular solvent microextraction coupled to HPLC with fluorescence detection.

Science.gov (United States)

Wang, Jin; Liu, Laping; Shi, Ludi; Yi, Tingquan; Wen, Yuxia; Wang, Juanli; Liu, Shuhui

2017-01-01

For the analysis of edible oils, saponification is well known as a useful method for eliminating oil matrices. The conventional approach is conducted with alcoholic alkali; it consumes a large volume of organic solvents and impedes the retrieval of analytes by microextraction. In this study, a low-organic-solvent-consuming method has been developed for the analysis of benzo[a]pyrene in edible oils by high-performance liquid chromatography with fluorescence detection. Sample treatment involves aqueous alkaline saponification, assisted by a phase-transfer catalyst, and selective in situ extraction of the analyte with a supramolecular solvent. Comparison of the chromatograms of the oil extracts obtained by different microextraction methods showed that the supramolecular solvent has a better clean-up effect for the unsaponifiable matter from oil matrices. The method offered excellent linearity over a range of 0.03- 5.0 ng mL -1 (r > 0.999). Recovery rates varied from 94 to 102% (RSDs <5.0%). The detection limit and quantification limit were 0.06 and 0.19 μg kg -1 , respectively. The proposed method was applied for the analysis of 52 edible oils collected online in China; the analyte contents of 23 tested oil samples exceeded the maximum limit of 2 μg kg -1 for benzo[a]pyrene set by the Commission Regulation of the European Union. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of organophosphorus flame retardants in fish by pressurized liquid extraction using aqueous solutions and solid-phase microextraction coupled with gas chromatography-flame photometric detector.

Science.gov (United States)

Gao, Zhanqi; Deng, Yuehua; Yuan, Wenting; He, Huan; Yang, Shaogui; Sun, Cheng

2014-10-31

A novel method was developed for the determination of organophosphorus flame retardants (PFRs) in fish. The method consists of a combination of pressurized liquid extraction (PLE) using aqueous solutions and solid-phase microextraction (SPME), followed by gas chromatography-flame photometric detector (GC-FPD). The experimental parameters that influenced extraction efficiency were systematically evaluated. The optimal responses were observed by extracting 1g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150°C for 5min and acid-washed silica gel used as lipid sorbent. The obtained extract was then analyzed by SPME coupled with GC-FPD without any additional clean-up steps. Under the optimal conditions, the proposed procedure showed a wide linear range (0.90-5000ngg(-1)) obtained by analyzing the spiked fish samples with increasing concentrations of PFRs and correlation coefficient (R) ranged from 0.9900 to 0.9992. The detection limits (S/N=3) were in the range of 0.010-0.208ngg(-1) with standard deviations (RSDs) ranging from 2.0% to 9.0%. The intra-day and inter-day variations were less than 9.0% and 7.8%, respectively. The proposed method was successfully applied to the determination of PFRs in real fish samples with recoveries varying from 79.8% to 107.3%. The results demonstrate that the proposed method is highly effective for analyzing PFRs in fish samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication and Characterisation of Low-noise Monolithic Mode-locked Lasers

DEFF Research Database (Denmark)

Larsson, David

2007-01-01

This thesis deals with the fabrication and characterisation of monolithic semiconductor mode-locked lasers for use in optical communication systems. Other foreseeable applications may be as sources in microwave photonics and optical sampling. The thesis also deals with the design and fabrication...... of intracavity monolithically integrated filters. The common dnominator among the diffrent parts of the thesis is how to achieve and measure the lowest possible noise. Achieving low noise has been pinpointed as one of the most important and difficult challenges for semiconductor mode-locked lasers. The main...... result of this thesis are a fabrication process of a monolithic and deeply etched distributed Bragg reflector and a characterisation system for measurement of quantum limitid timing noise at high repetition rates. The Bragg reflector is a key component in achieving transform limited pulses with low noise...

Recent progress in low-temperature-process monolithic three dimension technology

Science.gov (United States)

Yang, Chih-Chao; Hsieh, Tung-Ying; Huang, Wen-Hsien; Shen, Chang-Hong; Shieh, Jia-Min; Yeh, Wen-Kuan; Wu, Meng-Chyi

2018-04-01

Monolithic three-dimension (3D) integration is an ultimate alternative method of fabricating high density, high performance, and multi-functional integrated circuits. It offers the promise of being a new approach to increase system performance. How to manage the thermal impact of multi-tiered processes, such as dopant activation, source/drain silicidation, and channel formation, and to prevent the degradation of pre-existing devices/circuits become key challenges. In this paper, we provide updates on several important monolithic 3D works, particularly in sequentially stackable channels, and our recent achievements in monolithic 3D integrated circuit (3D-IC). These results indicate that the advanced 3D architecture with novel design tools enables ultrahigh-density stackable circuits to have superior performance and low power consumption for future artificial intelligence (AI) and internet of things (IoTs) application.

Monolithic fiber optic sensor assembly

Science.gov (United States)

Sanders, Scott

2015-02-10

A remote sensor element for spectrographic measurements employs a monolithic assembly of one or two fiber optics to two optical elements separated by a supporting structure to allow the flow of gases or particulates therebetween. In a preferred embodiment, the sensor element components are fused ceramic to resist high temperatures and failure from large temperature changes.

Towards a Technique for Extracting Microservices from Monolithic Enterprise Systems

OpenAIRE

Levcovitz, Alessandra; Terra, Ricardo; Valente, Marco Tulio

2016-01-01

The idea behind microservices architecture is to develop a single large, complex application as a suite of small, cohesive, independent services. On the other way, monolithic systems get larger over the time, deviating from the intended architecture, and becoming risky and expensive to evolve. This paper describes a technique to identify and define microservices on monolithic enterprise systems. As the major contribution, our evaluation shows that our approach was able to identify relevant ca...

Determination of polychlorinated biphenyls in milk samples by saponification-solid-phase microextraction.

Science.gov (United States)

Llompart, M; Pazos, M; Landin, P; Cela, R

2001-12-15

A saponification-HSSPME procedure has been developed for the extraction of PCBs from milk samples. Saponification of the samples improves the PCB extraction efficiency and allows attaining lower background. A mixed-level fractional design has been used to optimize the sample preparation process. Five variables have been considered: extraction time, agitation, kind of microextraction fiber, concentration, and volume of NaOH aqueous solution. Also the kinetic of the process has been studied with the two fibers (100-microm PDMS and 65-microm PDMS-DVB) included in this study. Analyses were performed on a gas chromatograph equipped with an electron capture detector and a gas chromatograph coupled to a mass selective detector working in MS-MS mode. The proposed method is simple and rapid, and yields high sensitivity, with detection limits below 1 ng/mL, good linearity, and reproducibility. The method has been applied to liquid milk samples with different fat content covering the whole commercial range, and it has been validated with powdered milk certified reference material.

Neutron spectrometry with a monolithic silicon telescope.

Science.gov (United States)

Agosteo, S; D'Angelo, G; Fazzi, A; Para, A Foglio; Pola, A; Zotto, P

2007-01-01

A neutron spectrometer was set-up by coupling a polyethylene converter with a monolithic silicon telescope, consisting of a DeltaE and an E stage-detector (about 2 and 500 microm thick, respectively). The detection system was irradiated with monoenergetic neutrons at INFN-Laboratori Nazionali di Legnaro (Legnaro, Italy). The maximum detectable energy, imposed by the thickness of the E stage, is about 8 MeV for the present detector. The scatter plots of the energy deposited in the two stages were acquired using two independent electronic chains. The distributions of the recoil-protons are well-discriminated from those due to secondary electrons for energies above 0.350 MeV. The experimental spectra of the recoil-protons were compared with the results of Monte Carlo simulations using the FLUKA code. An analytical model that takes into account the geometrical structure of the silicon telescope was developed, validated and implemented in an unfolding code. The capability of reproducing continuous neutron spectra was investigated by irradiating the detector with neutrons from a thick beryllium target bombarded with protons. The measured spectra were compared with data taken from the literature. Satisfactory agreement was found.

Role of microextraction sampling procedures in forensic toxicology.

Science.gov (United States)

Barroso, Mário; Moreno, Ivo; da Fonseca, Beatriz; Queiroz, João António; Gallardo, Eugenia

2012-07-01

The last two decades have provided analysts with more sensitive technology, enabling scientists from all analytical fields to see what they were not able to see just a few years ago. This increased sensitivity has allowed drug detection at very low concentrations and testing in unconventional samples (e.g., hair, oral fluid and sweat), where despite having low analyte concentrations has also led to a reduction in sample size. Along with this reduction, and as a result of the use of excessive amounts of potentially toxic organic solvents (with the subsequent environmental pollution and costs associated with their proper disposal), there has been a growing tendency to use miniaturized sampling techniques. Those sampling procedures allow reducing organic solvent consumption to a minimum and at the same time provide a rapid, simple and cost-effective approach. In addition, it is possible to get at least some degree of automation when using these techniques, which will enhance sample throughput. Those miniaturized sample preparation techniques may be roughly categorized in solid-phase and liquid-phase microextraction, depending on the nature of the analyte. This paper reviews recently published literature on the use of microextraction sampling procedures, with a special focus on the field of forensic toxicology.

Detector block based on arrays of 144 SiPMs and monolithic scintillators: A performance study

International Nuclear Information System (INIS)

González, A.J.; Conde, P.; Iborra, A.; Aguilar, A.; Bellido, P.; García-Olcina, R.; Hernández, L.; Moliner, L.; Rigla, J.P.; Rodríguez-Álvarez, M.J.; Sánchez, F.; Seimetz, M.; Soriano, A.; Torres, J.; Vidal, L.F.; Benlloch, J.M.

2015-01-01

We have developed a detector block composed by a monolithic LYSO scintillator coupled to a custom made 12×12 SiPMs array. The design is mainly focused to applications such as Positron Emission Tomography. The readout electronics is based on 3 identical and scalable Application Specific Integrated Circuits (ASIC). We have determined the main performance of the detector block namely spatial, energy, and time resolution but also the system capability to determine the photon depth of interaction, for different crystal surface treatments. Intrinsic detector spatial resolution values as good as 1.7 mm FWHM and energies of 15% for black painted crystals were measured

Rapid measurement of 13C-enrichment of acetic, propionic and butyric acids in plasma with solid phase microextraction coupled to gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Moreau, N.M.; Delepee, R.; Maume, D.; Le Bizec, B.; Nguyen, P.G.; Champ, M.M.; Martin, L.J.; Dumon, H.J.

2004-01-01

An analytical procedure based on solid phase microextraction (SPME) has been developed to quantify [1- 13 C]-labelled short-chain fatty acids (SCFAs)--mainly acetic, propionic and butyric acids--in a small volume (120 μl) of deproteinised plasma (corresponding to 200 μl of raw plasma) by gas chromatography-mass spectrometry (GC-MS) analysis. Simultaneous SCFA extraction was optimal after 5 min using a 75 μm Carboxen/polydimethylsiloxane-coated fiber. The base peak of the three analytes has been characterised by middle-resolution mass spectrometry (R>6000). All these data allowed the specificity reinforcement of the measure. The validation of the method also considered the linearity and the repeatability of the [ 13 C]SCFA measurements by SPME-GC-MS. Results were linear in a range from 5 to 100 mol% of [ 13 C]SCFA enrichment and the method provided a good intra-day (R.S.D. 13 C]butyric acid) by cecal infusion before blood sampling in portal vein. Results of [1- 13 C]butyric acid enrichment showed an excellent correlation (r 2 =0.9832; n=30) with data obtained on the same samples using a previously published procedure based on diethyl extraction and derivatisation before GC-MS analyses. SPME coupled to GC-MS appears to be a powerful analytical tool for the direct isotopic measurements of low deproteinised plasma volume avoiding consequently preliminary treatment such as extraction or derivatisation. The presented method could be of great interest for real time [ 13 C]SCFA plasma determination of in metabolic in vivo studies in small animal models

A Simple Method for the Simultaneous Determination of Pharmaceuticals and Personal Care Products in River Sediment by Ultrasound-Assisted Extraction Followed by Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

Science.gov (United States)

Díaz, Alejandro; Peña-Alvarez, Araceli

2017-10-01

A simple method was developed using ultrasound-assisted extraction (UAE) combined with solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of eight different pharmaceuticals and personal care products (PPCPs) (ibuprofen, 2-benzyl-4-chlorophenol, naproxen, triclosan, ketoprofen, diclofenac, bisphenol A and estrone) in river sediment. UAE conditions were optimized involving extraction variables such as extraction solvent, extraction time, sample amount, extraction temperature, pH and salt addition. A 100 mg of sediment was extracted by optimized UAE process using 7 mL deionized water (pH 3) + 1% methanol as solvent, room temperature and 1 min extraction at 70% of amplitude. A 5 mL of supernatant was subsequently extracted by SPME; the extracted analytes were derivatized on fiber in head-space mode with N-methyl-N-(tertbutyldimethylsilyl) trifluoroacetamide and then analyzed by GC-MS. The developed method was evaluated by testing: precision (CV 0.98), recoveries (56-108%), limits of detection (simple and environmentally friendly, and provides straightforward analyses of these trace organic pollutants in sediment samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Antagonist wear of monolithic zirconia crowns after 2 years.

Science.gov (United States)

Lohbauer, Ulrich; Reich, Sven

2017-05-01

The aim of this study was to evaluate the amount of wear on the antagonist occlusal surfaces of clinically placed monolithic zirconia premolar and molar crowns (LAVA Plus, 3M ESPE). Fourteen in situ monolithic zirconia crowns and their opposing antagonists (n = 26) are the subject of an ongoing clinical trial and have been clinically examined at baseline and after 24 months. Silicone impressions were taken and epoxy replicas produced for qualitative SEM analysis and quantitative analysis using optical profilometry. Based on the baseline replicas, the follow-up situation has been scanned and digitally matched with the initial topography in order to calculate the mean volume loss (in mm 3 ) as well as the mean maximum vertical loss (in mm) after 2 years in service. The mean volume loss for enamel antagonist contacts (n = 7) was measured to 0.361 mm 3 and the mean of the maximum vertical loss to 0.204 mm. The mean volume loss for pure ceramic contacts (n = 10) was measured to 0.333 mm 3 and the mean of the maximum vertical loss to 0.145 mm. The wear rates on enamel contacts were not significantly different from those measured on ceramic antagonists. Based on the limitations of this study, it can be concluded for the monolithic zirconia material LAVA Plus that the measured wear rates are in consensus with other in vivo studies on ceramic restorations. Further, that no significant difference was found between natural enamel antagonists and ceramic restorations as antagonists. The monolithic zirconia restorations do not seem to be affected by wear within the first 2 years. The monolithic zirconia crowns (LAVA Plus) show acceptable antagonist wear rates after 2 years in situ, regardless of natural enamel or ceramics as antagonist materials.

A monolithic integrated photonic microwave filter

Science.gov (United States)

Fandiño, Javier S.; Muñoz, Pascual; Doménech, David; Capmany, José

2017-02-01

Meeting the increasing demand for capacity in wireless networks requires the harnessing of higher regions in the radiofrequency spectrum, reducing cell size, as well as more compact, agile and power-efficient base stations that are capable of smoothly interfacing the radio and fibre segments. Fully functional microwave photonic chips are promising candidates in attempts to meet these goals. In recent years, many integrated microwave photonic chips have been reported in different technologies. To the best of our knowledge, none has monolithically integrated all the main active and passive optoelectronic components. Here, we report the first demonstration of a tunable microwave photonics filter that is monolithically integrated into an indium phosphide chip. The reconfigurable radiofrequency photonic filter includes all the necessary elements (for example, lasers, modulators and photodetectors), and its response can be tuned by means of control electric currents. This is an important step in demonstrating the feasibility of integrated and programmable microwave photonic processors.

Monolithically integrated 8-channel WDM reflective modulator

NARCIS (Netherlands)

Stopinski, S.T.; Malinowski, M.; Piramidowicz, R.; Smit, M.K.; Leijtens, X.J.M.

2013-01-01

In this work the design and characterization of a monolithically integrated photonic circuit acting as a reflective modulator for eight WDM channels is presented. The chip was designed and fabricated in a generic integration technology

Monolithic Integrated Ceramic Waveguide Filters

OpenAIRE

Hunter, IC; Sandhu, MY

2014-01-01

Design techniques for a new class of integrated monolithic high permittivity ceramic waveguide filters are presented. These filters enable a size reduction of 50% compared to air-filled TEM filters with the same unloaded Q-Factor. Designs for both chebyshev and asymmetric generalized chebyshev filter are presented, with experimental results for an 1800 MHz chebyshev filter showing excellent agreement with theory.

Environmentally Benign Production of Stretchable and Robust Superhydrophobic Silicone Monoliths.

Science.gov (United States)

Davis, Alexander; Surdo, Salvatore; Caputo, Gianvito; Bayer, Ilker S; Athanassiou, Athanassia

2018-01-24

Superhydrophobic materials hold an enormous potential in sectors as important as aerospace, food industries, or biomedicine. Despite this great promise, the lack of environmentally friendly production methods and limited robustness remain the two most pertinent barriers to the scalability, large-area production, and widespread use of superhydrophobic materials. In this work, highly robust superhydrophobic silicone monoliths are produced through a scalable and environmentally friendly emulsion technique. It is first found that stable and surfactantless water-in-polydimethylsiloxane (PDMS) emulsions can be formed through mechanical mixing. Increasing the internal phase fraction of the precursor emulsion is found to increase porosity and microtexture of the final monoliths, rendering them superhydrophobic. Silica nanoparticles can also be dispersed in the aqueous internal phase to create micro/nanotextured monoliths, giving further improvements in superhydrophobicity. Due to the elastomeric nature of PDMS, superhydrophobicity can be maintained even while the material is mechanically strained or compressed. In addition, because of their self-similarity, the monoliths show outstanding robustness to knife-scratch, tape-peel, and finger-wipe tests, as well as rigorous sandpaper abrasion. Superhydrophobicity was also unchanged when exposed to adverse environmental conditions including corrosive solutions, UV light, extreme temperatures, and high-energy droplet impact. Finally, important properties for eventual adoption in real-world applications including self-cleaning, stain-repellence, and blood-repellence are demonstrated.

Ultrasound assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography designated for bioavailability studies of felodipine combinations in rat plasma.

Science.gov (United States)

Ahmed, Sameh; Atia, Noha N; Bakr Ali, Marwa Fathy

2017-03-01

Felodipine (FLD), a calcium channel antagonist, is commonly prescribed for the treatment of hypertension either with Metoprolol (MET) or Ramipril (RAM) in two different drug combinations. FLD has high plasma protein binding ability affecting its extraction recoveries from plasma samples. Hence, a specific ultrasound assisted dispersive liquid-liquid microextraction (UA-DLLME) method coupled with HPLC using photodiode array detector was developed and validated for the simultaneous determination of FLD, MET and RAM in rat plasma after oral administration of these combinations. The factors affecting UA-DLLME were carefully optimized. In this study, UA-DLLME method could provide simple and efficient plasma extraction procedures with superior recovery results. Under optimum condition, all target drugs were separated within 13min. The validation procedures was carried out in agreement with US-FDA guidelines and shown to be suitable for anticipated purposes. Linear calibration ranges were obtained in the range 0.05-2.0μgmL -1 for FLD and MET and 0.1-2.0μgmL -1 for RAM with detection limits of 0.013-0.031μgmL -1 for all the studied drug combinations. The%RSD for inter-day and intra-day precisions was in range of 0.63-3.85% and the accuracy results were in the range of 92.13-100.5%. The validated UA-DLLME-HPLC method was successfully applied for the bioavailability studies of FLD, MET and RAM. The pharmacokinetic parameters were calculated for all the investigated drugs in rats after single-dose administrations of two different drug combinations. Although FLD was bioequivalent in the two formulations, a small increase in plasma levels of MET and RAM was found in the presence of FLD. Copyright © 2017 Elsevier B.V. All rights reserved.

Optical properties of pre-colored dental monolithic zirconia ceramics.

Science.gov (United States)

Kim, Hee-Kyung; Kim, Sung-Hun

2016-12-01

The purposes of this study were to evaluate the optical properties of recently marketed pre-colored monolithic zirconia ceramics and to compare with those of veneered zirconia and lithium disilicate glass ceramics. Various shades of pre-colored monolithic zirconia, veneered zirconia, and lithium disilicate glass ceramic specimens were tested (17.0×17.0×1.5mm, n=5). CIELab color coordinates were obtained against white, black, and grey backgrounds with a spectrophotometer. Color differences of the specimen pairs were calculated by using the CIEDE2000 (ΔE 00 ) formula. The translucency parameter (TP) was derived from ΔE 00 of the specimen against a white and a black background. X-ray diffraction was used to determine the crystalline phases of monolithic zirconia specimens. Data were analyzed with 1-way ANOVA, Scheffé post hoc, and Pearson correlation testing (α=0.05). For different shades of the same ceramic brand, there were significant differences in L * , a * , b * , and TP values in most ceramic brands. With the same nominal shade (A2), statistically significant differences were observed in L * , a * , b * , and TP values among different ceramic brands and systems (Pceramics of the corresponding nominal shades ranged beyond the acceptability threshold. Due to the high L * values and low a * and b * values, pre-colored monolithic zirconia ceramics can be used with additional staining to match neighboring restorations or natural teeth. Due to their high value and low chroma, unacceptable color mismatch with adjacent ceramic restorations might be expected. Copyright © 2016 Elsevier Ltd. All rights reserved.

Highly improved operation of monolithic BGO-PET blocks

Science.gov (United States)

Gonzalez-Montoro, A.; Sanchez, F.; Majewski, S.; Zanettini, S.; Benlloch, J. M.; Gonzalez, A. J.

2017-11-01

In PET scanners both scintillation crystals and photosensors are key components defining the system's performance and cost. Original PET systems used BGO or NaI(Tl) scintillators but achieved limited performance due to its slow decay and relatively low light output. Moreover, NaI(Tl) has low stopping power for 511 keV annihilation photons. In this study we report the possibility to reintroduce BGO crystals, and in particular in the form of monolithic blocks, especially suitable for low-dose large-size PET scanners, offering significantly improved sensitivity at a highly reduced cost compared to LYSO type fast scintillators. We have studied the performance of a monolithic BGO block as large as 50 × 50 × 15 mm3 with black-painted lateral walls to reduce lights spread, enabling accurate photon depth of interaction (DOI) measurements. A directional optical layer, called retro-reflector, was coupled to the entrance face bouncing back the scintillation light in the direction of the emission source and, therefore, adding to the light signal while preserving the narrow light cone distribution. Four configurations namely 12 × 12 and 16 × 16 SiPM arrays (3 mm × 3 mm each) as photosensors, with or without a nanopattern treatment at the crystal exit face, have been studied. This structure consisted of a thin layer of a specific high refractive index material shaped with a periodic nanopattern, increasing the scintillation light extraction. The readout returned information for each SiPM row and column, characterizing the X-Y light distribution projections. We have studied the detector spatial resolution using collimated 22Na sources at normal incidence. The DOI resolution was evaluated using collimated gamma beams with lateral incidence. The overall best detector performance was obtained for the 16× 16 SiPM array offering higher readout granularity. We have determined the spatial resolution for 3 separated DOI layers, obtaining the best results for the DOI region near to

Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

NARCIS (Netherlands)

de Jong, GJ; Koster, EHM

2000-01-01

Solid-phase micro-extraction (SPME) is a never sample preparation technique that can be used for gaseous, liquid or solid samples in conjunction with GC, HPLC or CE (e.g. [1]). The use of SPME for the analysis of drugs in biofluids is also becoming popular (e.g. [2]). The principle is that a fused

New 'monolithic' templates and improved protocols for soft lithography and microchip fabrication

International Nuclear Information System (INIS)

Pallandre, Antoine; Pal, Debjani; Lambert, Bertrand de; Viovy, Jean-Louis; Fuetterer, Claus

2006-01-01

We report a new method for fast prototyping and fabrication of polydimethylsiloxane (PDMS) and plastic microfluidic chips. These methods share in common the preparation of monolithic masters which includes the fabrication of the planar support, the 'negative pattern' of the microchannels and the fluidic connectors. The monolithic templates are extremely robust compared to conventional ones made of silicon and SU-8, and easier to produce and cheaper than all-silicon or electroplated templates. In contrast to the above-mentioned methods, our process allows one to cast both micrometre- (e.g. the microchannel) and millimetre-sized structures (e.g. the fluidic connection to the outer world) in a single fabrication step. The 'monolithic template' strategy can be used to fabricate both elastomeric (e.g. poly(dimethyl siloxane (PDMS)) polyester thermoset masters and glassy polymeric (e.g. cyclic olefin copolymer (COC)) devices. In this study we also report on one step fabrication of elastomer chips and on surface modifications of the above mentioned monolithically fabricated masters in order to improve separation of the chip from the template

Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

2016-10-01

A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Speciation analysis of aqueous nanoparticulate diclofenac complexes by solid-phase microextraction

NARCIS (Netherlands)

Zielinska, K.; Leeuwen, van H.P.; Thibault, S.; Town, R.M.

2012-01-01

The dynamic sorption of an organic compound by nanoparticles (NPs) is analyzed by solid-phase microextraction (SPME) for the example case of the pharmaceutical diclofenac in dispersions of impermeable (silica, SiO(2)) and permeable (bovine serum albumin, BSA) NPs. It is shown that only the

Failure analysis of various monolithic posterior aesthetic dental crowns using finite element method

Science.gov (United States)

Porojan, Liliana; Topală, Florin

2017-08-01

The aim of the study was to assess the effect of material stiffness and load on the biomechanical performance of the monolithic full-coverage posterior aesthetic dental crowns using finite element analysis. Three restorative materials for monolithic dental crowns were selected for the study: zirconia; lithium disilicate glass-ceramic, and resin-based composite. Stresses were calculated in the crowns for all materials and in the teeth structures, under different load values. The experiments show that dental crowns made from all this new aesthetic materials processed by CAD/CAM technologies would be indicated as monolithic dental crowns for posterior areas.

Determination of Bisphenol A and Bisphenol AF in Vinegar samples by two-component mixed ionic liquid dispersive liquid-phase microextraction coupled with high performance liquid chromatography

International Nuclear Information System (INIS)

Tai, Z.; Liu, M.; Hu, X.; Yang, Y.

2014-01-01

This paper describes a sensitive and simple method for the determination of bisphenol A (BPA) and bisphenol AF (BPAF) in vinegar samples using two-component mixed ionic liquid dispersive liquid-phase microextraction coupled with high performance liquid chromatography. In this work, BPA and BPAF were selected as the model analytes, and two-component mixed ionic liquid included 1-butyl-3-methylimidazolium hexafluorophosphate ((C4Mim)PF6) and 1-hexyl-3-methyl-imidazolium hexafluorophosphate ((C6Mim)PF6) was used as the extraction solvent for the first time here. Parameters that affect the extraction efficiency were investigated. Under the optimum conditions, good linear relationships were discovered in the range of 1.0-100 micro g/L for BPA and 2.0-150 micro g/L for BPAF, respectively. Detection limits of proposed method based on the signal-to-noise ratio (S/N=3) were in the range of 0.15-0.38 micro g/L. The efficiencies of proposed method have also been demonstrated with spiked real vinegar samples. The result show this method/ procedure to be a more efficient approach for the determination of BPA and BPAF in real vinegar, presenting average recovery rate of 89.3-112 % and precision values of 0.9-13.5% (RSDs, n = 6). In comparison with traditional solid phase extraction procedures this method results in lower solvent consumption, low pollution levels, and faster sample preparation. (author)

Effect of pore size on performance of monolithic tube chromatography of large biomolecules.

Science.gov (United States)

Podgornik, Ales; Hamachi, Masataka; Isakari, Yu; Yoshimoto, Noriko; Yamamoto, Shuichi

2017-11-01

Effect of pore size on the performance of ion-exchange monolith tube chromatography of large biomolecules was investigated. Radial flow 1 mL polymer based monolith tubes of different pore sizes (1.5, 2, and 6 μm) were tested with model samples such as 20 mer poly T-DNA, basic proteins, and acidic proteins (molecular weight 14 000-670 000). Pressure drop, pH transient, the number of binding site, dynamic binding capacity, and peak width were examined. Pressure drop-flow rate curves and dynamic binding capacity values were well correlated with the nominal pore size. While duration of the pH transient curves depends on the pore size, it was found that pH duration normalized on estimated surface area was constant, indicating that the ligand density is the same. This was also confirmed by the constant number of binding site values being independent of pore size. The peak width values were similar to those for axial flow monolith chromatography. These results showed that it is easy to scale up axial flow monolith chromatography to radial flow monolith tube chromatography by choosing the right pore size in terms of the pressure drop and capacity. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

THE CHANGE IN DEFORMATION CHARACTERISTICS OF CONCRETE MONOLITHIC HIGH-RISE BUILDINGS

Directory of Open Access Journals (Sweden)

V. V. Punahin

2009-03-01

Full Text Available In the article results of studies of deformation features of concrete on actuate cement for monolithic high-altitude buildings are presented. It is shown that in construction of the high-altitude monolithic buildings in a summer period of a year one should take into account the character of changing the concrete elasticity and plasticity in time, which differs from the same indices for the concrete of normal hardening.

Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography.

Science.gov (United States)

Qin, Zhang-Na; Yu, Qiong-Wei; Wang, Ren-Qi; Feng, Yu-Qi

2018-04-27

A mixed-mode polymer monolithic column functionalized by arsonic acid groups was prepared by single-step in situ copolymerization of monomers p-methacryloylaminophenylarsonic acid (p-MAPHA) and pentaerythritol triacrylate (PETA). The prepared poly(p-MAPHA-co-PETA) monolithic column has a homogeneous monolithic structure with good permeability and mechanical stability. Zeta potential measurements reveal that the monolithic stationary phase holds a negative surface charge when the mobile phase resides in the pH range of 3.0-8.0. The retention mechanisms of prepared monolithic column are explored by the separation of selected polycyclic aromatic hydrocarbons (PAHs), nucleosides, and three basic compounds. The results indicate that the column functions in three different separation modes associated with reversed-phase chromatography based on hydrophobic interaction, hydrophilic interaction chromatography, and cation-exchange chromatography. The column efficiency of prepared monolithic column is estimated to be 70,000 and 76,000 theoretical plates/m for thiourea and naphthalene, respectively, at a linear flow velocity of 0.85 mm/s using acetonitrile/H 2 O (85/15, v/v) as the mobile phase. Furthermore, an analysis of the retention factors obtained for the PAHs indicates that the prepared monolithic column exhibits good reproducibility with relative standard deviations of 2.9%, 4.0%, and 4.7% based on run-to-run injections, column-to-column preparation, and batch-to-batch preparation, respectively. Finally, we investigate the separation performance of the proposed monolithic column for select phenols, sulfonamides, nucleobases and nucleosides. Copyright © 2018 Elsevier B.V. All rights reserved.

Silicon drift detectors coupled to CsI(Tl) scintillators for spaceborne gamma-ray detectors

International Nuclear Information System (INIS)

Marisaldi, M.; Fiorini, C.; Labanti, C.; Longoni, A.; Perotti, F.; Rossi, E.; Soltau, H.

2006-01-01

Silicon Drift Detectors (SDDs), thanks to their peculiar low noise characteristics, have proven to be excellent photodetectors for CsI(Tl) scintillation light detection. Two basic detector configurations have been developed: either a single SDD or a monolithic array of SDDs coupled to a single CsI(Tl) crystal. A 16 independent detectors prototype is under construction, designed to work in conjunction with the MEGA Compton telescope prototype under development at MPE, Garching, Germany. A single SDD coupled to a CsI(Tl) crystal has also been tested as a monolithic detector with an extended energy range between 1.5 keV and 1 MeV. The SDD is used as a direct X-ray detector for low energy photons interacting in silicon and as a scintillation light photodetector for photons interacting in the crystal. The type of interaction is identified by means of pulse shape discrimination technique. Detectors based on an array of SDDs coupled to a single CsI(Tl) crystal have also been built. The readout of these detectors is based on the Anger camera technique, and submillimeter spatial resolution can be achieved. The two detectors' approaches and their applications will be described

Review on recent and advanced applications of monoliths and related porous polymer gels in micro-fluidic devices

International Nuclear Information System (INIS)

Vazquez, Mercedes; Paull, Brett

2010-01-01

This review critically summarises recent novel and advanced achievements in the application of monolithic materials and related porous polymer gels in micro-fluidic devices appearing within the literature over the period of the last 5 years (2005-2010). The range of monolithic materials has developed rapidly over the past decade, with a diverse and highly versatile class of materials now available, with each exhibiting distinct porosities, pore sizes, and a wide variety of surface functionalities. A major advantage of these materials is their ease of preparation in micro-fluidic channels by in situ polymerisation, leading to monolithic materials being increasingly utilised for a larger variety of purposes in micro-fluidic platforms. Applications of porous polymer monoliths, silica-based monoliths and related homogeneous porous polymer gels in the preparation of separation columns, ion-permeable membranes, preconcentrators, extractors, electrospray emitters, micro-valves, electrokinetic pumps, micro-reactors and micro-mixers in micro-fluidic devices are discussed herein. Procedures used in the preparation of monolithic materials in micro-channels, as well as some practical aspects of the micro-fluidic chip fabrication are addressed. Recent analytical/bioanalytical and catalytic applications of the final micro-fluidic devices incorporating monolithic materials are also reviewed.

Solid phase micro-extraction in environmental atmosphere

International Nuclear Information System (INIS)

Tao Ping; Wei Lifan; Tan Yun

2002-01-01

Solid phase micro-extraction (SPME) is an advanced technique of sample pretreatment in environmental atmosphere analysis, i.e., a sampling method of extracting volatile organic compounds from environmental gas. According to the primary survey on the theory and application of SPME, a suitable extraction tip, i.e., a coated fused silica fiber, is selected to construct a SPME apparatus. This SPME apparatus is used to extract volatile organic compounds from environmental atmosphere and a qualitative detection is conducted in gas chromatography-mass spectrometer system. Good experimental results are obtained

Monolithic millimeter-wave and picosecond electronic technologies

International Nuclear Information System (INIS)

Talley, W.K.; Luhmann, N.C.

1996-01-01

Theoretical and experimental studies into monolithic millimeter-wave and picosecond electronic technologies have been undertaken as a collaborative project between the Lawrence Livermore National Laboratory (LLNL) and the University of California Department of Applied Science Coherent Millimeter-Wave Group under the auspices of the Laboratory Directed Research and Development Program at LLNL. The work involves the design and fabrication of monolithic frequency multiplier, beam control, and imaging arrays for millimeter-wave imaging and radar, as well as the development of high speed nonlinear transmission lines for ultra-wideband radar imaging, time domain materials characterization and magnetic fusion plasma applications. In addition, the Coherent Millimeter-Wave Group is involved in the fabrication of a state-of-the-art X-band (∼8-11 GHz) RF photoinjector source aimed at producing psec high brightness electron bunches for advanced accelerator and coherent radiation generation studies

Silicon monolithic microchannel-cooled laser diode array

International Nuclear Information System (INIS)

Skidmore, J. A.; Freitas, B. L.; Crawford, J.; Satariano, J.; Utterback, E.; DiMercurio, L.; Cutter, K.; Sutton, S.

2000-01-01

A monolithic microchannel-cooled laser diode array is demonstrated that allows multiple diode-bar mounting with negligible thermal cross talk. The heat sink comprises two main components: a wet-etched Si layer that is anodically bonded to a machined glass block. The continuous wave (cw) thermal resistance of the 10 bar diode array is 0.032 degree sign C/W, which matches the performance of discrete microchannel-cooled arrays. Up to 1.5 kW/cm 2 is achieved cw at an emission wavelength of ∼808 nm. Collimation of a diode array using a monolithic lens frame produced a 7.5 mrad divergence angle by a single active alignment. This diode array offers high average power/brightness in a simple, rugged, scalable architecture that is suitable for large two-dimensional areas. (c) 2000 American Institute of Physics

Innovative monolithic detector for tri-spectral (THz, IR, Vis) imaging

Science.gov (United States)

Pocas, S.; Perenzoni, M.; Massari, N.; Simoens, F.; Meilhan, J.; Rabaud, W.; Martin, S.; Delplanque, B.; Imperinetti, P.; Goudon, V.; Vialle, C.; Arnaud, A.

2012-10-01

Fusion of multispectral images has been explored for many years for security and used in a number of commercial products. CEA-Leti and FBK have developed an innovative sensor technology that gathers monolithically on a unique focal plane arrays, pixels sensitive to radiation in three spectral ranges that are terahertz (THz), infrared (IR) and visible. This technology benefits of many assets for volume market: compactness, full CMOS compatibility on 200mm wafers, advanced functions of the CMOS read-out integrated circuit (ROIC), and operation at room temperature. The ROIC houses visible APS diodes while IR and THz detections are carried out by microbolometers collectively processed above the CMOS substrate. Standard IR bolometric microbridges (160x160 pixels) are surrounding antenna-coupled bolometers (32X32 pixels) built on a resonant cavity customized to THz sensing. This paper presents the different technological challenges achieved in this development and first electrical and sensitivity experimental tests.

A compact D-band monolithic APDP-based sub-harmonic mixer

Science.gov (United States)

Zhang, Shengzhou; Sun, Lingling; Wang, Xiang; Wen, Jincai; Liu, Jun

2017-11-01

The paper presents a compact D-band monolithic sub-harmonic mixer (SHM) with 3 μm planar hyperabrupt schottky-varactor diodes offered by 70 nm GaAs mHEMT technology. According to empirical equivalent-circuit models, a wide-band large signal equivalent circuit model of the diode is proposed. Based on the extracted model, the mixer is implemented and optimized with a shunt-mounted anti-parallel diode pair (APDP) to fulfill the sub-harmonic mixing mechanism. Furthermore, a modified asymmetric three-transmission-line coupler is devised to achieve high-level coupling and minimize the chip size. The measured results show that the conversion gain varies between -13.9 dB and -17.5 dB from 110 GHz to 145 GHz, with a local oscillator (LO) power level of 14 dBm and an intermediate frequency (IF) of 1 GHz. The total chip size including probe GSG pads is 0.57 × 0.68mm2. In conclusion, the mixer exhibits outstanding figure-of-merits.

Carprofen-imprinted monolith prepared by reversible addition-fragmentation chain transfer polymerization in room temperature ionic liquids.

Science.gov (United States)

Ban, Lu; Han, Xu; Wang, Xian-Hua; Huang, Yan-Ping; Liu, Zhao-Sheng

2013-10-01

To obtain fast separation, ionic liquids were used as porogens first in combination with reversible addition-fragmentation chain transfer (RAFT) polymerization to prepare a new type of molecularly imprinted polymer (MIP) monolith. The imprinted monolithic column was synthesized using a mixture of carprofen (template), 4-vinylpyridine, ethylene glycol dimethacrylate, [BMIM]BF4, and chain transfer agent (CTA). Some polymerization factors, such as template-monomer molar ratio, the degree of crosslinking, the composition of the porogen, and the content of CTA, on the column efficiency and imprinting effect of the resulting MIP monolith were systematically investigated. Affinity screening of structurally similar compounds with the template can be achieved in 200 s on the MIP monolith due to high column efficiency (up to 12,070 plates/m) and good column permeability. Recognition mechanism of the imprinted monolith was also investigated.

Monoliths of activated carbon from coconut shell and impregnation with nickel and copper

International Nuclear Information System (INIS)

Giraldo, Liliana; Moreno, Juan

2008-01-01

A series of different monoliths of activated carbon were prepared from coconut shell By means of chemical activation with phosphoric acid at different concentrations Without using binders or plastics. The monolith that developed the biggest surface area was impregnated by humidic route with solutions of Ni and Cu at different molar relations. The structures were characterized by N2 adsorption at 77 K, and the morphology was explored by means of scanning electron microscopy. The carbonaceous materials obtained, Nickel-Copper-Monolith, were analyzed by Thermal Programmed Reduction (TPR). The experimental results indicated that the activation with the acid generated a micro porosity, with micropores volume between 0.40 and 0.81 cm 3 g-1 and surface areas between 703 and 1450 m 2 g-1, and a good mechanical properties. It shows that, both the copper and the nickel, are fixed to the monolith and TPR's results are interpreted when these molar relation are modified.

Poly(ethylenimine)-Functionalized Monolithic Alumina Honeycomb Adsorbents for CO2 Capture from Air.

Science.gov (United States)

Sakwa-Novak, Miles A; Yoo, Chun-Jae; Tan, Shuai; Rashidi, Fereshteh; Jones, Christopher W

2016-07-21

The development of practical and effective gas-solid contactors is an important area in the development of CO2 capture technologies. Target CO2 capture applications, such as postcombustion carbon capture and sequestration (CCS) from power plant flue gases or CO2 extraction directly from ambient air (DAC), require high flow rates of gas to be processed at low cost. Extruded monolithic honeycomb structures, such as those employed in the catalytic converters of automobiles, have excellent potential as structured contactors for CO2 adsorption applications because of the low pressure drop imposed on fluid moving through the straight channels of such structures. Here, we report the impregnation of poly(ethylenimine) (PEI), an effective aminopolymer reported commonly for CO2 separation, into extruded monolithic alumina to form structured CO2 sorbents. These structured sorbents are first prepared on a small scale, characterized thoroughly, and compared with powder sorbents with a similar composition. Despite consistent differences observed in the filling of mesopores with PEI between the monolithic and powder sorbents, their performance in CO2 adsorption is similar across a range of PEI contents. A larger monolithic cylinder (1 inch diameter, 4 inch length) is evaluated under conditions closer to those that might be used in large-scale applications and shows a similar performance to the smaller monoliths and powders tested initially. This larger structure is evaluated over five cycles of CO2 adsorption and steam desorption and demonstrates a volumetric capacity of 350 molCO2  m-3monolith and an equilibration time of 350 min under a 0.4 m s(-1) linear flow velocity through the monolith channels using 400 ppm CO2 in N2 as the adsorption gas at 30 °C. This volumetric capacity surpasses that of a similar technology considered previously, which suggested that CO2 could be removed from air at an operating cost as low as $100 per ton. © 2016 WILEY-VCH Verlag

Preparation of epoxy-based macroporous monolithic columns for the fast and efficient immunofiltration of Staphylococcus aureus.

Science.gov (United States)

Ott, Sonja; Niessner, Reinhard; Seidel, Michael

2011-08-01

Macroporous epoxy-based monolithic columns were used for immunofiltration of bacteria. The prepared monolithic polymer support is hydrophilic and has large pore sizes of 21 μm without mesopores. A surface chemistry usually applied for immobilization of antibodies on glass slides is successfully transferred to monolithic columns. Step-by-step, the surface of the epoxy-based monolith is hydrolyzed, silanized, coated with poly(ethylene glycol diamine) and activated with the homobifunctional crosslinker di(N-succinimidyl)carbonate for immobilization of antibodies on the monolithic columns. The functionalization steps are characterized to ensure the coating of each monolayer. The prepared antibody-immobilized monolithic column is optimized for immunofiltration to enrich Staphylococcus aureus as an important food contaminant. Different kinds of geometries of monolithic columns, flow rates and elution buffers are tested with the goal to get high recoveries in the shortest enrichment time as possible. An effective capture of S. aureus was achieved at a flow rate of 7.0 mL/min with low backpressures of 20.1±5.4 mbar enabling a volumetric enrichment of 1000 within 145 min. The bacteria were quantified by flow cytometry using a double-labeling approach. After immunofiltration the sensitivity was significantly increased and a detection limit of the total system of 42 S. aureus/mL was reached. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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

2016-03-11

This paper, for the first time, reported a speedy hyphenated technique of low toxic dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) for the simultaneous determination of 20(S)-protopanaxadiol (PPD) and 20(S)-protopanaxatriol (PPT). The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection using multiple-reaction monitoring (MRM) mode. A mass spectrometry sensitizing reagent, 4'-carboxy-substituted rosamine (CSR) with high reaction activity and ionization efficiency was synthesized and firstly used as derivatization reagent. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS conditions were all optimized in detail. Low toxic brominated solvents were used as extractant instead of traditional chlorinated solvents. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.010 and 0.015ng/mL for PPD and PPT, respectively) were achieved. The main advantages were rapid, sensitive and environmentally friendly, and exhibited high selectivity, accuracy and good matrix effect results. The proposed method was successfully applied to pharmacokinetics of PPD and PPT in rat plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

Package Holds Five Monolithic Microwave Integrated Circuits

Science.gov (United States)

Mysoor, Narayan R.; Decker, D. Richard; Olson, Hilding M.

1996-01-01

Packages protect and hold monolithic microwave integrated circuit (MMIC) chips while providing dc and radio-frequency (RF) electrical connections for chips undergoing development. Required to be compact, lightweight, and rugged. Designed to minimize undesired resonances, reflections, losses, and impedance mismatches.

Determination of organochlorine pesticides in water using dynamic hook-type liquid-phase microextraction

Energy Technology Data Exchange (ETDEWEB)

Chen, Pai-Shan; Huang, Shih-Pin [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Fuh, Ming-Ren, E-mail: msfuh@mail.scu.edu.tw [Department of Chemistry, Soochow University, Taipei, Taiwan (China); Huang, Shang-Da, E-mail: sdhuang@mx.nthu.edu.tw [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

2009-08-11

We developed a simple and efficient headspace liquid-phase microextraction (LPME) technique named dynamic hook-type liquid-phase microextraction (DHT-LPME) and used it in combination with gas chromatography-mass spectrometry (GC-MS) and an electron capture detector (ECD). Aqueous specimens of organochlorine pesticides (OCPs) were used as model compounds to demonstrate the effectiveness of the technique. In the present study, the calibration curves were linear over at least 2 orders of magnitude with R{sup 2} values of 0.997. The method detection limits (MDLs) varied from 2 to 44.0 ng L{sup -1}. The precision of DHT-LPME ranged from 6.5 to 14.4%. The relative recoveries of OCPs in rainwater were more than 84.2%. Enrichment factors (EF) in the range 275-1127 were obtained using DHT-LPME.

Determination of organochlorine pesticides in water using dynamic hook-type liquid-phase microextraction

International Nuclear Information System (INIS)

Chen, Pai-Shan; Huang, Shih-Pin; Fuh, Ming-Ren; Huang, Shang-Da

2009-01-01

We developed a simple and efficient headspace liquid-phase microextraction (LPME) technique named dynamic hook-type liquid-phase microextraction (DHT-LPME) and used it in combination with gas chromatography-mass spectrometry (GC-MS) and an electron capture detector (ECD). Aqueous specimens of organochlorine pesticides (OCPs) were used as model compounds to demonstrate the effectiveness of the technique. In the present study, the calibration curves were linear over at least 2 orders of magnitude with R 2 values of 0.997. The method detection limits (MDLs) varied from 2 to 44.0 ng L -1 . The precision of DHT-LPME ranged from 6.5 to 14.4%. The relative recoveries of OCPs in rainwater were more than 84.2%. Enrichment factors (EF) in the range 275-1127 were obtained using DHT-LPME.

[Determination of four phenolic endocrine disruptors in environmental water samples by high performance liquid chromatography-fluorescence detection using dispersive liquid-liquid microextraction coupled with derivatization].

Science.gov (United States)

Wang, Xiaoyan; Qi, Weimei; Zhao, Xian'en; Lü, Tao; Wang, Xiya; Zheng, Longfang; Yan, Yehao; You, Jinmao

2014-06-01

To achieve accurate, fast and sensitive detection of phenolic endocrine disruptors in small volume of environmental water samples, a method of dispersive liquid-liquid microextraction (DLLME) coupled with fluorescent derivatization was developed for the determination of bisphenol A, nonylphenol, octylphenol and 4-tert-octylphenol in environmental water samples by high performance liquid chromatography-fluorescence detection (HPLC-FLD). The DLLME and derivatization conditions were investigated, and the optimized DLLME conditions for small volume of environmental water samples (pH 4.0) at room temperature were as follows: 70 microL chloroform as extraction solvent, 400 microL acetonitrile as dispersing solvent, vortex mixing for 3 min, and then high-speed centrifugation for 2 min. Using 2-[2-(7H-dibenzo [a, g] carbazol-7-yl)-ethoxy] ethyl chloroformate (DBCEC-Cl) as precolumn derivatization reagent, the stable derivatives of the four phenolic endocrine disruptors were obtained in pH 10.5 Na2CO3-NaHCO3 buffer/acetonitrile at 50 degrees C for 3 min, and then separated within 10 min by HPLC-FLD. The limits of detection (LODs) were in the range of 0.9-1.6 ng/L, and the limits of quantification (LOQs) were in the range of 3.8-7.1 ng/L. This method had perfect linearity, precision and recovery results, and showed obvious advantages and practicality comparing to the previously reported methods. It is a convenient and validated method for the routine analysis of phenolic endocrine disruptors in waste water of paper mill, lake water, domestic wastewater, tap water, etc.

A novel ionic liquid monolithic column and its separation properties in capillary electrochromatography

International Nuclear Information System (INIS)

Wang Yu; Deng Qiliang; Fang Guozhen; Pan Mingfei; Yu Yang; Wang Shuo

2012-01-01

Highlights: ► ILs as functional monomer for capillary monolithic column. ► Separation of alkylbenzenes, thiourea analogues, and amino acids. ► The column generate a stable reversed EOF from pH 2.0 to 12.0. ► The column efficiency of 147,000 plates m −1 was obtained for thiourea. - Abstract: A novel ionic liquid (IL) monolithic capillary column was successfully prepared by thermal free radical copolymerization of IL (1-vinyl-3-octylimidazolium chloride, ViOcIm + Cl − ) together with lauryl methacrylate (LMA) as the binary functional monomers and ethylene dimethacrylate (EDMA) as the cross-linker in binary porogen. The proportion of monomers, porogens and cross-linker in the polymerization mixture was optimized in detail. The resulting IL-monolithic column could not only generate a stable reversed electroosmotic flow (EOF) in a wide pH range (2.0–12.0), but also effectively eliminate the wall adsorption of the basic analytes. The obtained IL-monolithic columns were examined by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). These results indicated that the IL-monolithic capillary column possessed good pore properties, mechanical stability and permeability. The column performance was also evaluated by separating different kinds of compounds, such as alkylbenzenes, thiourea and its analogues, and amino acids. The lowest plate height of ∼6.8 μm was obtained, which corresponded to column efficiency (theoretical plates, N) of ∼147,000 plates m −1 for thiourea. ILs, as a new type of functional monomer, present a promising option in the fabrication of the organic polymer-based monolithic columns in CEC.

Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent.

Science.gov (United States)

Miyaguchi, Hajime; Iwata, Yuko T; Kanamori, Tatsuyuki; Tsujikawa, Kenji; Kuwayama, Kenji; Inoue, Hiroyuki

2009-05-01

We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi-GC/MS. A washed hair sample (1-5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 microL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 microL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20-50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20-30 times use. The carry over was estimated to be about 1-2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods.

A Ferrite LTCC-Based Monolithic SIW Phased Antenna Array

KAUST Repository

Nafe, Ahmed A.; Ghaffar, Farhan A.; Farooqui, Muhammad Fahad; Shamim, Atif

2016-01-01

In this work, we present a novel configuration for realizing monolithic SIW-based phased antenna arrays using Ferrite LTCC technology. Unlike the current common schemes for realizing SIW phased arrays that rely on surface-mount component (p-i-n diodes, etc) for controlling the phase of the individual antenna elements, here the phase is tuned by biasing of the ferrite filling of the SIW. This approach eliminates the need for mounting of any additional RF components and enables seamless monolithic integration of phase shifters and antennas in SIW technology. As a proof of concept, a two-element slotted SIW-based phased array is designed, fabricated and measured. The prototype exhibits a gain of 4.9 dBi at 13.2 GHz and a maximum E-plane beam-scanning of 28 degrees using external windings for biasing the phase shifters. Moreover, the array can achieve a maximum beam-scanning of 19 degrees when biased with small windings that are embedded in the package. This demonstration marks the first time a fully monolithic SIW-based phased array is realized in Ferrite LTCC technology and paves the way for future larger-size implementations.

A Ferrite LTCC-Based Monolithic SIW Phased Antenna Array

KAUST Repository

Nafe, Ahmed

2016-11-17

In this work, we present a novel configuration for realizing monolithic SIW-based phased antenna arrays using Ferrite LTCC technology. Unlike the current common schemes for realizing SIW phased arrays that rely on surface-mount component (p-i-n diodes, etc) for controlling the phase of the individual antenna elements, here the phase is tuned by biasing of the ferrite filling of the SIW. This approach eliminates the need for mounting of any additional RF components and enables seamless monolithic integration of phase shifters and antennas in SIW technology. As a proof of concept, a two-element slotted SIW-based phased array is designed, fabricated and measured. The prototype exhibits a gain of 4.9 dBi at 13.2 GHz and a maximum E-plane beam-scanning of 28 degrees using external windings for biasing the phase shifters. Moreover, the array can achieve a maximum beam-scanning of 19 degrees when biased with small windings that are embedded in the package. This demonstration marks the first time a fully monolithic SIW-based phased array is realized in Ferrite LTCC technology and paves the way for future larger-size implementations.

Determination of 2-Octanone in Biological Samples Using Liquid–Liquid Microextractions Followed by Gas Chromatography–Flame Ionization Detectio

Directory of Open Access Journals (Sweden)

Abolghasem Jouyban, Maryam Abbaspour, Mir Ali Farajzadeh, Maryam Khoubnasabjafari

2017-06-01

Full Text Available Background: Analysis of chemicals in biological fluids is required in many areas of medical sciences. Rapid, highly efficient, and reliable dispersive and air assisted liquid–liquid microextraction methods followed by gas chromatography-flame ionization detection were developed for the extraction, preconcentration, and determination of 2-octanone in human plasma and urine samples. Methods: Proteins of plasma samples are precipitated by adding methanol and urine sample is diluted with water prior to performing the microextraction procedure. Fine organic solvent droplets are formed by repeated suction and injection of the mixture of sample solution and extraction solvent into a test tube with a glass syringe. After extraction, phase separation is performed by centrifuging and the enriched analyte in the sedimented organic phase is determined by the separation system. The main factors influencing the extraction efficiency including extraction solvent type and volume, salt addition, pH, and extraction times are investigated. Results: Under the optimized conditions, the proposed method showed good precision (relative standard deviation less than 7%. Limit of detection and lower limit of quantification for 2-octanone were obtained in the range of 0.1–0.5 µg mL−1. The linear ranges were 0.5-500 and 0.5-200 µg mL−1 in plasma and urine, respectively (r2 ≥ 0.9995. Enrichment factors were in the range of 13-37. Good recoveries (55–86% were obtained for the spiked samples. Conclusion: Preconcentration methods coupled with GC analysis were developed and could be used to monitor 2-octanone in biological samples.

Electrochromatography on acrylate-based monolith in cyclic olefin copolymer microchip: an attractive technology.

Science.gov (United States)

Ladner, Y; Cretier, G; Faure, K

2015-01-01

Electrochromatography (EC) on a porous monolithic stationary phase prepared within the channels of a microsystem is an attractive alternative for on-chip separation. It combines the separation mechanisms of electrophoresis and liquid chromatography. Moreover, the porous polymer monolithic materials have become popular as stationary phase due to the ease and rapidity of fabrication via free radical photopolymerization. Here, we describe a hexyl acrylate (HA)-based porous monolith which is simultaneously in situ synthesized and anchored to the inner walls of the channel of a cyclic olefin copolymer (COC) device in only 2 min. The baseline separation of a mixture of neurotransmitters including six amino acids and two catecholamines is realized.

Use of dispersive liquid-liquid microextraction for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium

International Nuclear Information System (INIS)

Mallah, M.H.; Atomic Energy Organization of Iran, Tehran; Shemirani, F.; Ghannadi Maragheh, M.

2008-01-01

A new preconcentration method of dispersive liquid-liquid microextraction (DLLME) was developed for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium. DLLME technique was successfully used as a sample preparation method. In this preconcentration method, an appropriate mixture of extraction solvent, disperser solvent was injected rapidly into an aqueous solution containing Sm, Eu, Gd and Dy after complex formation using chelating reagent of the 1-(2-pyridylazo)-2-naphthol (PAN). After phase separation, 0.5 mL of the settled phase containing enriched analytes was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The main factors affected the preconcentration of Sm, Eu, Gd and Dy were extraction and dispersive solvent type and their volume, extraction time, volume of chelating agent (PAN), centrifuge speed and drying temperature of the samples. Under the best operating condition simultaneous preconcentration factors of 80, 100, 103 and 78 were obtained for Sm, Eu, Gd and Dy, respectively. (author)

Numerical Simulation of Fluid Dynamics in a Monolithic Column

Directory of Open Access Journals (Sweden)

Kazuhiro Yamamoto

2017-01-01

Full Text Available As for the measurement of polycyclic aromatic hydrocarbons (PAHs, ultra-performance liquid chromatography (UPLC is used for PAH identification and densitometry. However, when a solvent containing a substance to be identified passes through a column of UPLC, a dedicated high-pressure-proof device is required. Recently, a liquid chromatography instrument using a monolithic column technology has been proposed to reduce the pressure of UPLC. The present study tested five types of monolithic columns produced in experiments. To simulate the flow field, the lattice Boltzmann method (LBM was used. The velocity profile was discussed to decrease the pressure drop in the ultra-performance liquid chromatography (UPLC system.

Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

International Nuclear Information System (INIS)

Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

2013-01-01

We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

Study and optimization of positioning algorithms for monolithic PET detectors blocks

International Nuclear Information System (INIS)

Acilu, P Garcia de; Sarasola, I; Canadas, M; Cuerdo, R; Mendes, P Rato; Romero, L; Willmott, C

2012-01-01

We are developing a PET insert for existing MRI equipment to be used in clinical PET/MR studies of the human brain. The proposed scanner is based on annihilation gamma detection with monolithic blocks of cerium-doped lutetium yttrium orthosilicate (LYSO:Ce) coupled to magnetically-compatible avalanche photodiodes (APD) matrices. The light distribution generated on the LYSO:Ce block provides the impinging position of the 511 keV photons by means of a positioning algorithm. Several positioning methods, from the simplest Anger Logic to more sophisticate supervised-learning Neural Networks (NN), can be implemented to extract the incidence position of gammas directly from the APD signals. Finally, an optimal method based on a two-step Feed-Forward Neural Network has been selected. It allows us to reach a resolution at detector level of 2 mm, and acquire images of point sources using a first BrainPET prototype consisting of two monolithic blocks working in coincidence. Neural networks provide a straightforward positioning of the acquired data once they have been trained, however the training process is usually time-consuming. In order to obtain an efficient positioning method for the complete scanner it was necessary to find a training procedure that reduces the data acquisition and processing time without introducing a noticeable degradation of the spatial resolution. A grouping process and posterior selection of the training data have been done regarding the similitude of the light distribution of events which have one common incident coordinate (transversal or longitudinal). By doing this, the amount of training data can be reduced to about 5% of the initial number with a degradation of spatial resolution lower than 10%.

A novel ionic liquid monolithic column and its separation properties in capillary electrochromatography.

Science.gov (United States)

Wang, Yu; Deng, Qi-Liang; Fang, Guo-Zhen; Pan, Ming-Fei; Yu, Yang; Wang, Shuo

2012-01-27

A novel ionic liquid (IL) monolithic capillary column was successfully prepared by thermal free radical copolymerization of IL (1-vinyl-3-octylimidazolium chloride, ViOcIm(+)Cl(-)) together with lauryl methacrylate (LMA) as the binary functional monomers and ethylene dimethacrylate (EDMA) as the cross-linker in binary porogen. The proportion of monomers, porogens and cross-linker in the polymerization mixture was optimized in detail. The resulting IL-monolithic column could not only generate a stable reversed electroosmotic flow (EOF) in a wide pH range (2.0-12.0), but also effectively eliminate the wall adsorption of the basic analytes. The obtained IL-monolithic columns were examined by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). These results indicated that the IL-monolithic capillary column possessed good pore properties, mechanical stability and permeability. The column performance was also evaluated by separating different kinds of compounds, such as alkylbenzenes, thiourea and its analogues, and amino acids. The lowest plate height of ~6.8 μm was obtained, which corresponded to column efficiency (theoretical plates, N) of ~147,000 plates m(-1) for thiourea. ILs, as a new type of functional monomer, present a promising option in the fabrication of the organic polymer-based monolithic columns in CEC. Copyright © 2011 Elsevier B.V. All rights reserved.

Behavior of micro-particles in monolith ceramic membrane filtration with pre-coagulation.

Science.gov (United States)

Yonekawa, H; Tomita, Y; Watanabe, Y

2004-01-01

This paper is intended to clarify the characteristics unique to monolith ceramic membranes with pre-coagulation by referring to the behavior of micro-particles. Flow analysis and experiments have proved that monolith ceramic membranes show a unique flow pattern in the channels within the element, causing extremely rapid flocculation in the channel during dead-end filtration. It was assumed that charge-neutralized micro-particles concentrated near the membrane surface grow in size due to flocculation, and as a result, coarse micro-particles were taken up by the shearing force to flow out. As the dead end points of flow in all the channels are located near the end of the channels with higher filterability, most of the flocculated coarse particles are formed to a columnar cake intensively at the dead end point. Therefore cake layer forming on the membrane other than around the dead end point is alleviated. This behavior of particle flocculation and cake formation at the dead end point within the channels are unique characteristics of monolith ceramic membranes. This is why all monolith ceramic membrane water purification systems operating in Japan do not have pretreatment equipment for flocculation and sedimentation.

Test of the TRAPPISTe monolithic detector system

Science.gov (United States)

Soung Yee, L.; Álvarez, P.; Martin, E.; Cortina, E.; Ferrer, C.

2013-12-01

A monolithic pixel detector named TRAPPISTe-2 has been developed in Silicon-on-Insulator (SOI) technology. A p-n junction is implanted in the bottom handle wafer and connected to readout electronics integrated in the top active layer. The two parts are insulated from each other by a buried oxide layer resulting in a monolithic detector. Two small pixel matrices have been fabricated: one containing a 3-transistor readout and a second containing a charge sensitive amplifier readout. These two readout structures have been characterized and the pixel matrices were tested with an infrared laser source. The readout circuits are adversely affected by the backgate effect, which limits the voltage that can be applied to the metal back plane to deplete the sensor, thus narrowing the depletion width of the sensor. Despite the low depletion voltages, the integrated pixel matrices were able to respond to and track a laser source.

Coupling carbon nanotube film microextraction with desorption corona beam ionization for rapid analysis of Sudan dyes (I-IV) and Rhodamine B in chilli oil.

Science.gov (United States)

Chen, Di; Huang, Yun-Qing; He, Xiao-Mei; Shi, Zhi-Guo; Feng, Yu-Qi

2015-03-07

A rapid analysis method by coupling carbon nanotube film (CNTF) microextraction with desorption corona beam ionization (DCBI) was developed for the determination of Sudan dyes (I-IV) and Rhodamine B in chilli oil samples. Typically, CNTF was immersed into the diluted solution of chilli oil for extraction, which was then placed directly under the visible plasma beam tip of the DCBI source for desorption and ionization. Under optimized conditions, five dyes were simultaneously determined using this method. Results showed that the analytes were enriched by the CNTF through the π-π interactions, and the proposed method could significantly improve the sensitivities of these compounds, compared to the direct analysis by DCBI-MS/MS. The method with a linear range of 0.08-12.8 μg g(-1) and good linear relationships (R(2) > 0.93) in a multiple reaction monitoring (MRM) mode was developed. Satisfactory reproducibility was achieved. Relative standard deviations (RSDs) were less than 20.0%. The recoveries ranged from 80.0 to 110.0%, and the limits of detection (LODs) were in the range of 1.4-21 ng g(-1). Finally, the feasibility of the method was further exhibited by the determination of five illegal dyes in chilli powder. These results demonstrate that the proposed method consumes less time and solvent than conventional HPLC-based methods and avoids the contamination of chromatographic column and ion source from non-volatile oil. With the help of a 72-well shaker, multiple samples could be treated simultaneously, which ensures high throughput for the entire pretreatment process. In conclusion, it provides a rapid and high-throughput approach for the determination of such illicit additions in chilli products.

Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microextraction.

Science.gov (United States)

Benedé, Juan L; Anderson, Jared L; Chisvert, Alberto

2018-01-01

In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) system. The main parameters involved in TD, as well as in the extraction step affecting the extraction efficiency (i.e., MIL amount, extraction time and ionic strength) were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ng L -1 level, good intra- and inter-day repeatability (RSD < 13%) and good enrichment factors (18 - 717). This sensitive analytical method was applied to the determination of trace amounts of PAHs in three natural water samples (river, tap and rainwater) with satisfactory relative recovery values (84-115%), highlighting that the matrices under consideration do not affect the extraction process. Copyright © 2017 Elsevier B.V. All rights reserved.

Novel porous fly-ash containing geopolymer monoliths for lead adsorption from wastewaters

Energy Technology Data Exchange (ETDEWEB)

Novais, Rui M., E-mail: ruimnovais@ua.pt; Buruberri, L.H.; Seabra, M.P.; Labrincha, J.A.

2016-11-15

Highlights: • Porous fly ash containing-geopolymer monoliths for lead adsorption were developed. • Geopolymers’ porosity and pH of the ion solution controls the adsorption capacity. • Lead adsorption by the geopolymer monoliths up to 6.34 mg/g was observed. • These novel adsorbents can be used in packed beds that are easily collected. • The reuse of biomass fly ash wastes as raw material ensures waste valorization. - Abstract: In this study novel porous biomass fly ash-containing geopolymer monoliths were produced using a simple and flexible procedure. Geopolymers exhibiting distinct total porosities (ranging from 41.0 to 78.4%) and low apparent density (between 1.21 and 0.44 g/cm{sup 3}) were fabricated. Afterwards, the possibility of using these innovative materials as lead adsorbents under distinct conditions was evaluated. Results demonstrate that the geopolymers’ porosity and the pH of the ion solution strongly affect the lead adsorption capacity. Lead adsorption by the geopolymer monoliths ranged between 0.95 and 6.34 mg{sub lead}/g{sub geopolymer}. More porous geopolymers presented better lead removal efficiency, while higher pH in the solution reduced their removal ability, since metal precipitation is enhanced. These novel geopolymeric monoliths can be used in packed beds that are easily collected when exhausted, which is a major advantage in comparison with the use of powdered adsorbents. Furthermore, their production encompasses the reuse of biomass fly-ash, mitigating the environmental impact associated with this waste disposal, while decreasing the adsorbents production costs.

Cold vapor-solid phase microextraction using amalgamation in different Pd-based substrates combined with direct thermal desorption in a modified absorption cell for the determination of Hg by atomic absorption spectrometry

International Nuclear Information System (INIS)

Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos

2011-01-01

In this work, different Pd-based substrates (i.e. Pd wire, Pd-coated stainless steel wire and Pd-coated SiO 2 ) are tried for microextraction of Hg prior to its release into a modified quartz T-cell so as to develop a cost-effective, sensitive and easy-to-handle coupling between solid-phase microextraction (SPME) and atomic absorption spectrometry. The new design allows a direct sample injection from the SPME device into a quartz T-cell thus avoiding analyte dilution. Mercury amalgamation onto a Pd wire provided the best performance in respect to sensitivity and fiber lifetime, but Pd wires could not be implemented in the SPME device due to their poor mechanical characteristics. On the contrary, Pd-coated SiO 2 fibers could be easily adapted to the typical sampling device used for SPME. Narrow time-dependent absorption signal profiles that could be integrated within 25 s were obtained. The detection limit was 90 pg mL -1 of Hg, and the repeatability expressed as relative standard deviation was 4.3%.

Evaluation of solid-phase microextraction conditions for the determination of polycyclic aromatic hydrocarbons in aquatic species using gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

2008-06-15

This paper describes a headspace solid-phase microextraction (HS-SPME) procedure coupled to gas chromatography with mass spectrometric detection (GC-MS) for the determination of eight PAHs in aquatic species. The influence of various parameters on the PAH extraction efficiency was carefully examined. At 75 C and for an extraction time of 60 min, a polydimethylsiloxane-divinylbenzene (PDMS/DVB) fiber coating was found to be most suitable. Under the optimized conditions, detection limits ranged from 8 to 450 pg g{sup -1}, depending on the compound and the sample matrix. The repeatability varied between 7 and 15% (RSD). Accuracy was tested using the NIST SRM 1974b reference material. The method was successfully applied to different samples, and the studied PAHs were detected in several of the samples. (orig.)

Feedhorn-Coupled Transition-Edge Superconducting Bolometer Arrays for Cosmic Microwave Background Polarimetry

Science.gov (United States)

Hubmayr, J.; Austermann, J.; Beall, J.; Becker, D.; Cho, H.-M.; Datta, R.; Duff, S. M.; Grace, E.; Halverson, N.; Henderson, S. W.;

CAISSON TYPE HOLLOW FLOOR SLABS OF MONOLITHIC MULTI-STOREYED BUILDINGS

Directory of Open Access Journals (Sweden)

Malakhova Anna Nikolaevna

2016-06-01

Full Text Available One of the disadvantages of building structures made of reinforced concrete is their considerable weight. One of the trends to decrease the weight of concrete structures, including floor slabs, is the arrangement of voids in the cross-sectional building structures. In Russian and foreign practice paper, cardboard and plastic tubes has been used for creation of voids in the construction of monolithic floor slabs. Lightweight concretes were also used for production of precast hollow core floor slabs. The article provides constructive solutions of precast hollow core floor slabs and solid monolithic slabs that were used in the construction of buildings before wide use of large precast hollow core floor slabs. The article considers the application of caisson hollow core floor slabs for modern monolithic multi-storeyed buildings. The design solutions of such floor slabs, experimental investigations and computer modeling of their operation under load were described in this article. The comparative analysis of the calculation results of computer models of a hollow slabs formed of rod or plastic elements showed the similarity of calculation results.

LePIX: First results from a novel monolithic pixel sensor

International Nuclear Information System (INIS)

Mattiazzo, S.; Battaglia, M.; Bisello, D.; Caselle, M.; Chalmet, P.; Demaria, N.; Giubilato, P.; Ikemoto, Y.; Kloukinas, K.; Mansuy, C.; Marchioro, A.; Mugnier, H.; Pantano, D.; Potenza, A.; Rivetti, A.; Rousset, J.; Silvestrin, L.; Snoeys, W.; Wyss, J.

2013-01-01

We present a monolithic pixel sensor developed in the framework of the LePIX project aimed at tracking/triggering tasks where high granularity, low power consumption, material budget, radiation hardness and production costs are a concern. The detector is built in a 90 nm CMOS process on a substrate of moderate resistivity. This maintains the advantages usually offered by Monolithic Active Pixel Sensors (MAPS), like a low input capacitance, having a single piece detector and using a standard CMOS production line, but offers charge collection by drift from a depleted region and therefore an excellent signal to noise ratio and a radiation tolerance superior to conventional undepleted MAPS. Measurement results obtained with the first prototypes from laser, radioactive source and beam test experiments are described. The excellent signal-to-noise performance is demonstrated by the capability of the device to separate the peaks in the spectrum of a 55 Fe source. We will also highlight the interaction between pixel cell design and architecture which points toward a very precise direction in the development of such depleted monolithic pixel devices for high energy physics

Bubbles in solvent microextraction: the influence of intentionally introduced bubbles on extraction efficiency.

Science.gov (United States)

Williams, D Bradley G; George, Mosotho J; Meyer, Riaan; Marjanovic, Ljiljana

2011-09-01

Significant improvements to microdrop extractions of triazine pesticides are realized by the intentional incorporation of an air bubble into the solvent microdroplet used in this microextraction technique. The increase is attributed partly to greater droplet surface area resulting from the air bubble being incorporated into the solvent droplet as opposed to it sitting thereon and partly to thin film phenomena. The method is useful at nanogram/liter levels (LOD 0.002-0.012 μg/L, LOQ 0.007-0.039 μg/L), is precise (7-12% at 10 μg/L concentration level), and is validated against certified reference materials containing 0.5 and 5.0 μg/L analyte. It tolerates water and fruit juice as matrixes without serious matrix effects. This new development brings a simple, inexpensive, and efficient preconcentration technique to bear which rivals solid phase microextraction methods.

In situ synthesis of metal-organic frameworks in a porous polymer monolith as the stationary phase for capillary liquid chromatography.

Science.gov (United States)

Yang, Shengchao; Ye, Fanggui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

2015-04-21

In this study, HKUST-1 was synthesized in situ on the porous polymer monolith as the stationary phase for capillary liquid chromatography (cLC). The unique carboxyl functionalized poly(methacrylic acid-co-ethylene dimethacrylate) (poly(MAA-co-EDMA)) monolith was used as a support to directly grow HKUST-1 by a controlled layer-by-layer self-assembly strategy. X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry, and Fourier transform infrared spectroscopy of the resulting HKUST-1-poly(MAA-co-EDMA) monoliths indicated that HKUST-1 was successfully grafted onto the pore surface of the poly(MAA-co-EDMA) monolith. The column performance of HKUST-1-poly(MAA-co-EDMA) monoliths for the separation of various small molecules, such as benzenediols, xylenes, ethylbenzenes, and styrenes, was evaluated. The chromatographic performance was found to improve with increasing HKUST-1 density, and the column efficiencies and resolutions of HKUST-1-poly(MAA-co-EDMA) monoliths were 18 320-19 890 plates m(-1) and 1.62-6.42, respectively, for benzenediols. The HKUST-1-poly(MAA-co-EDMA) monolith displayed enhanced resolution for the separation of positional isomers when compared to the traditional C18 and HKUST-1 incorporated polymer monoliths. Hydrophobic, π-π, and hydrogen bonding interactions within the HKUST-1-poly(MAA-co-EDMA) monolith were observed in the separation of small molecules. The results showed that the HKUST-1-poly(MAA-co-EDMA) monoliths are promising stationary phases for cLC.

Antireflective sub-wavelength structures for improvement of the extraction efficiency and color rendering index of monolithic white light-emitting diode

DEFF Research Database (Denmark)

Ou, Yiyu; Corell, Dennis Dan; Dam-Hansen, Carsten

2011-01-01

We have theoretically investigated the influence of antireflective sub-wavelength structures on a monolithic white light-emitting diode (LED). The simulation is based on the rigorous coupled wave analysis (RCWA) algorithm, and both cylinder and moth-eye structures have been studied in the work. Our...... simulation results show that a moth-eye structure enhances the light extraction efficiency over the entire visible light range with an extraction efficiency enhancement of up to 26 %. Also for the first time to our best knowledge, the influence of sub-wavelength structures on both the color rendering index...

A video Hartmann wavefront diagnostic that incorporates a monolithic microlens array

International Nuclear Information System (INIS)

Toeppen, J.S.; Bliss, E.S.; Long, T.W.; Salmon, J.T.

1991-07-01

we have developed a video Hartmann wavefront sensor that incorporates a monolithic array of microlenses as the focusing elements. The sensor uses a monolithic array of photofabricated lenslets. Combined with a video processor, this system reveals local gradients of the wavefront at a video frame rate of 30 Hz. Higher bandwidth is easily attainable with a camera and video processor that have faster frame rates. When used with a temporal filter, the reconstructed wavefront error is less than 1/10th wave

Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

NARCIS (Netherlands)

Zielinska, K.

2014-01-01

Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid

Vortex-assisted liquid-liquid microextraction for the rapid screening of short-chain chlorinated paraffins in water.

Science.gov (United States)

Chang, Chia-Yu; Chung, Wu-Hsun; Ding, Wang-Hsien

2016-01-01

The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 μL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 μg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 μg/L. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Advanced digital modulation: Communication techniques and monolithic GaAs technology

Science.gov (United States)

Wilson, S. G.; Oliver, J. D., Jr.; Kot, R. C.; Richards, C. R.

1983-01-01

Communications theory and practice are merged with state-of-the-art technology in IC fabrication, especially monolithic GaAs technology, to examine the general feasibility of a number of advanced technology digital transmission systems. Satellite-channel models with (1) superior throughput, perhaps 2 Gbps; (2) attractive weight and cost; and (3) high RF power and spectrum efficiency are discussed. Transmission techniques possessing reasonably simple architectures capable of monolithic fabrication at high speeds were surveyed. This included a review of amplitude/phase shift keying (APSK) techniques and the continuous-phase-modulation (CPM) methods, of which MSK represents the simplest case.

Numerical simulation research on rolling process of monolithic nuclear fuel plate

International Nuclear Information System (INIS)

Wan Jibo; Kong Xiangzhe; Ding Shurong; Xu Hongbin; Huo Yongzhong

2015-01-01

For the strain-rate-dependent constitutive relation of zircaloy cladding in UMo monolithic nuclear fuel plates, the three-dimensional stress updating algorithm was derived out, and the corresponding VUMAT subroutine to define its constitutive relation was developed and validated; the finite element model was built to simulate the frame rolling process of UMo monolithic nuclear fuel plates; with the explicit dynamic finite element method, the evolution rules of the deformation and contact pressure during the rolling process within the composite slab were obtained and analyzed. The research results indicate that it is convenient and efficient to define the strain-rate- dependent constitutive relations of materials with the user-defined material subroutine VUMAT; the rolling-induced contact pressure between the fuel meat and the covers varies with time, and the maximum pressure exits at the symmetric plane along the plate width direction. This study supplies a foundation and a computation method for optimizing the processing parameters to manufacture UMo monolithic nuclear fuel plates. (authors)

Facile preparation of organic-silica hybrid monolith for capillary hydrophilic liquid chromatography based on "thiol-ene" click chemistry.

Science.gov (United States)

Chen, Ming-Luan; Zhang, Jun; Zhang, Zheng; Yuan, Bi-Feng; Yu, Qiong-Wei; Feng, Yu-Qi

2013-04-05

In this work, a one-step approach to facile preparation of organic-inorganic hybrid monoliths was successfully developed. After vinyl-end organic monomers and azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethoxysilane (TMOS) and 3-mercaptopropyltrimethoxysilane (MPTMS), the homogeneous mixture was introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the organic-silica hybrid monoliths. By employing this strategy, two types of organic-silica hybrid monoliths with positively charged quaternary ammonium and amide groups were prepared, respectively. The functional groups were successfully introduced onto the monoliths during the sol-gel process with "thiol-ene" click reaction, which was demonstrated by ζ-potential assessment, energy dispersive X-ray spectroscopy (EDX), and Fourier transform infrared (FT-IR) spectroscopy. The porous structure of the prepared monolithic columns was examined by scanning electron microscopy (SEM), nitrogen adsorption-desorption measurement, and mercury intrusion porosimetry. These results indicate the prepared organic-silica hybrid monoliths possess homogeneous column bed, large specific surface area, good mechanical stability, and excellent permeability. The prepared monolithic columns were then applied for anion-exchange/hydrophilic interaction liquid chromatography. Different types of analytes, including benzoic acids, inorganic ions, nucleosides, and nucleotides, were well separated with high column efficiency around 80,000-130,000 plates/m. Taken together, we present a facile and universal strategy to prepare organic-silica hybrid monoliths with a variety of organic monomers using one-step approach. Copyright © 2013 Elsevier B.V. All rights reserved.

An All Silicon Feedhorn-Coupled Focal Plane for Cosmic Microwave Background Polarimetry

Science.gov (United States)

Hubmayr, J.; Appel, J. W.; Austermann, J. E.; Beall, J. A.; Becker, D.; Benson, B. A.; Bleem, L. E.; Carlstrom, J. E.; Chang, C. L.; Cho, H. M.;

High-temperature oxidation behavior of dense SiBCN monoliths: Carbon-content dependent oxidation structure, kinetics and mechanisms

International Nuclear Information System (INIS)

Li, Daxin; Yang, Zhihua; Jia, Dechang; Wang, Shengjin; Duan, Xiaoming; Zhu, Qishuai; Miao, Yang; Rao, Jiancun; Zhou, Yu

2017-01-01

Highlights: •The scale growth for all investigated monoliths at 1500 °C cannot be depicted by a linear or parabolic rate law. •The carbon-rich monoliths oxidize at 1500 °C according to a approximately linear weight loss equation. •The excessive carbon in SiBCN monoliths deteriorates the oxidation resistance. •The oxidation resistance stems from the characteristic oxide structures and increased oxidation resistance of BN(C). -- Abstract: The high temperature oxidation behavior of three SiBCN monoliths: carbon-lean SiBCN with substantial Si metal, carbon-moderate SiBCN and carbon-rich SiBCN with excessive carbon, was investigated at 1500 °C for times up to15 h. Scale growth for carbon-lean and −moderate monoliths at 1500 °C cannot be described by a linear or parabolic rate law, while the carbon-rich monoliths oxidize according to a approximately linear weight loss equation. The microstructures of the oxide scale compose of three distinct layers. The passivating layer of carbon and boron containing amorphous SiO 2 and increased oxidation resistance of BN(C) both benefit the oxidation resistance.

High-Q/V Monolithic Diamond Microdisks Fabricated with Quasi-isotropic Etching.

Science.gov (United States)

Khanaliloo, Behzad; Mitchell, Matthew; Hryciw, Aaron C; Barclay, Paul E

2015-08-12

Optical microcavities enhance light-matter interactions and are essential for many experiments in solid state quantum optics, optomechanics, and nonlinear optics. Single crystal diamond microcavities are particularly sought after for applications involving diamond quantum emitters, such as nitrogen vacancy centers, and for experiments that benefit from diamond's excellent optical and mechanical properties. Light-matter coupling rates in experiments involving microcavities typically scale with Q/V, where Q and V are the microcavity quality-factor and mode-volume, respectively. Here we demonstrate that microdisk whispering gallery mode cavities with high Q/V can be fabricated directly from bulk single crystal diamond. By using a quasi-isotropic oxygen plasma to etch along diamond crystal planes and undercut passivated diamond structures, we create monolithic diamond microdisks. Fiber taper based measurements show that these devices support TE- and TM-like optical modes with Q > 1.1 × 10(5) and V < 11(λ/n) (3) at a wavelength of 1.5 μm.

Monolithic Inorganic ZnO/GaN Semiconductors Heterojunction White Light-Emitting Diodes.

Science.gov (United States)

Jeong, Seonghoon; Oh, Seung Kyu; Ryou, Jae-Hyun; Ahn, Kwang-Soon; Song, Keun Man; Kim, Hyunsoo

2018-01-31

Monolithic light-emitting diodes (LEDs) that can generate white color at the one-chip level without the wavelength conversion through packaged phosphors or chip integration for photon recycling are of particular importance to produce compact, cost-competitive, and smart lighting sources. In this study, monolithic white LEDs were developed based on ZnO/GaN semiconductor heterojunctions. The electroluminescence (EL) wavelength of the ZnO/GaN heterojunction could be tuned by a post-thermal annealing process, causing the generation of an interfacial Ga 2 O 3 layer. Ultraviolet, violet-bluish, and greenish-yellow broad bands were observed from n-ZnO/p-GaN without an interfacial layer, whereas a strong greenish-yellow band emission was the only one observed from that with an interfacial layer. By controlled integration of ZnO/GaN heterojunctions with different postannealing conditions, monolithic white LED was demonstrated with color coordinates in the range (0.3534, 0.3710)-(0.4197, 0.4080) and color temperatures of 4778-3349 K in the Commission Internationale de l'Eclairage 1931 chromaticity diagram. Furthermore, the monolithic white LED produced approximately 2.1 times higher optical output power than a conventional ZnO/GaN heterojunction due to the carrier confinement effect at the Ga 2 O 3 /n-ZnO interface.

Single-mode very wide tunability in laterally coupled semiconductor lasers with electrically controlled reflectivities

Science.gov (United States)

Griffel, Giora; Chen, Howard Z.; Grave, Ilan; Yariv, Amnon

1991-04-01

The operation of a novel multisection structure comprised of laterally coupled gain-guided semiconductor lasers is demonstrated. It is shown that tunable single longitudinal mode operation can be achieved with a high degree of frequency selectivity. The device has a tuning range of 14.5 nm, the widest observed to date in a monolithic device.

Exceptionally stable and hierarchically porous self-standing zeolite monolith based on a solution-mediated and solid-state transformation synergistic mechanism

Energy Technology Data Exchange (ETDEWEB)

Do, Manh Huy [Key Laboratory of Biomass Chemical Engineering of Ministry of Education, Zhejiang University, Hangzhou 310027, Zhejiang (China); College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, Zhejiang (China); Institute of Chemical Technology, Vietnamese Academy of Science and Technology, 01 Mac Dinh Chi, District 1, Ho Chi Minh (Viet Nam); Cheng, Dang-guo, E-mail: dgcheng@zju.edu.cn [College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, Zhejiang (China); Chen, Fengqiu [Key Laboratory of Biomass Chemical Engineering of Ministry of Education, Zhejiang University, Hangzhou 310027, Zhejiang (China); College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, Zhejiang (China); Zhan, Xiaoli [College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, Zhejiang (China)

2015-11-15

Although many strategies exist for fabricating hierarchical zeolite monolith, it is still challenging to synthesize pure hierarchical zeolite monolith with intracrystalline meso-/macropores and stability suitable for industrial application in a general and efficient process. Here we describe a simple quasi-solid gel crystallization route to prepare hierarchical self-standing ZSM-5 zeolite monolith via the use of Na{sup +} and OH{sup −} as counterions to modify the breaking and remaking of T–O–T (T = Si or Al) bonds. X-ray diffraction (XRD), scanning electron microcopy (SEM), transmission electron microscopy (TEM), laser scan confocal microscopy (LSCM), N{sub 2} adsorption–desorption, mercury porosimetry, solid-state nuclear magnetic resonance (NMR), and compression mechanical testing were applied to elucidate the structure and mechanical stability of the obtained monolith. The self-standing monolith is composed of self-interconnected meso-/macroporous MFI crystals with tunable intracrystalline meso-/macropores and possesses an unusually mechanical stability with a crushing strength of 5.01 MPa. Combined with controllable structure of the defect-free membrane layer on the monolith top, the self-standing zeolite monolith should widen their potential applications. - Highlights: • Hierarchical self-standing MFI zeolite monoliths were synthesized via a facile method. • Na{sup +} and OH{sup −} are used as counterions for breaking and remaking of T–O–T (T = Si or Al) bonds. • Hierarchical self-standing MFI zeolite monoliths result from zeolite crystal intergrowth. • Self-standing zeolite monolith has an excellent mechanical stability with tunable intracrystalline meso-/macropores.

Application of Microextraction Techniques Including SPME and MESI to the Thermal Degradation of Polymers: A Review.

Science.gov (United States)

Kaykhaii, Massoud; Linford, Matthew R

2017-03-04

Here, we discuss the newly developed micro and solventless sample preparation techniques SPME (Solid Phase Microextraction) and MESI (Membrane Extraction with a Sorbent Interface) as applied to the qualitative and quantitative analysis of thermal oxidative degradation products of polymers and their stabilizers. The coupling of these systems to analytical instruments is also described. Our comprehensive literature search revealed that there is no previously published review article on this topic. It is shown that these extraction techniques are valuable sample preparation tools for identifying complex series of degradation products in polymers. In general, the number of products identified by traditional headspace (HS-GC-MS) is much lower than with SPME-GC-MS. MESI is particularly well suited for the detection of non-polar compounds, therefore number of products identified by this technique is not also to the same degree of SPME. Its main advantage, however, is its ability of (semi-) continuous monitoring, but it is more expensive and not yet commercialized.

On the fixed-stress split scheme as smoother in multigrid methods for coupling flow and geomechanics

NARCIS (Netherlands)

F.J. Gaspar Lorenz (Franscisco); C. Rodrigo (Carmen)

2017-01-01

textabstractThe fixed-stress split method has been widely used as solution method in the coupling of flow and geomechanics. In this work, we analyze the behavior of an inexact version of this algorithm as smoother within a geometric multigrid method, in order to obtain an efficient monolithic solver

Fiber-based monolithic columns for liquid chromatography.

Science.gov (United States)

Ladisch, Michael; Zhang, Leyu

2016-10-01

Fiber-based monoliths for use in liquid chromatographic separations are defined by columns packed with aligned fibers, woven matrices, or contiguous fiber structures capable of achieving rapid separations of proteins, macromolecules, and low molecular weight components. A common denominator and motivating driver for this approach, first initiated 25 years ago, was reducing the cost of bioseparations in a manner that also reduced residence time of retained components while achieving a high ratio of mass to momentum transfer. This type of medium, when packed into a liquid chromatography column, minimized the fraction of stagnant liquid and resulted in a constant plate height for non-adsorbing species. The uncoupling of dispersion from eluent flow rate enabled the surface chemistry of the stationary phase to be considered separately from fluid transport phenomena and pointed to new ways to apply chemistry for the engineering of rapid bioseparations. This paper addresses developments and current research on fiber-based monoliths and explains how the various forms of this type of chromatographic stationary phase have potential to provide new tools for analytical and preparative scale separations. The different stationary phases are discussed, and a model that captures the observed constant plate height as a function of mobile phase velocity is reviewed. Methods that enable hydrodynamically stable fiber columns to be packed and operated over a range of mobile phase flow rates, together with the development of new fiber chemistries, are shown to provide columns that extend the versatility of liquid chromatography using monoliths, particularly at the preparative scale. Graphical Abstract Schematic representation of a sample mixture being separated by a rolled-stationary phase column, resulting separated peaks shown in the chromatogram.

Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

Directory of Open Access Journals (Sweden)

Abuzar Kabir

2017-12-01

Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

Application of monolithic polycapillary focusing optics in MXRF

International Nuclear Information System (INIS)

Gao, N.; Ponomarev, I.; Xiao, Q.F.; Gibson, W.M.

1996-01-01

A monolithic polycapillary focusing optic, consisting of hundreds of thousands of small tapered glass capillaries, can collect a large solid angle of x rays from a point source and guide them through the capillaries by multiple total reflections to form an intense focused beam. Such a focused beam has many applications in microbeam x-ray fluorescence (MXRF) analysis. Two monolithic polycapillary focusing optics were tested and characterized in a MXRF set-up using a microfocusing x-ray source (50microm x 10microm). For the Cu K α line, the measured focal spot sizes of these optics were 105microm and 43microm Full-Width-Half-Maximum (FWHM), respectively. When the source was operated at 16W, the average Cu K α intensities over the focal spots were measured to be 2.4 x 10 4 photons/s/microm 2 and 8.9 x 10 4 photons/s/microm 2 , respectively. When the authors compared the monolithic optics to straight monocapillary optics (single channel capillary) with approximately the same output beam sizes, intensity gains of 16 and 44 were obtained. The optics were applied to the MXRF set-up to analyze trace elements in various samples and a Minimum Detection Limit (MDL) of about 2 pg was achieved for the transition elements (V, Cr, Mn, and Fe). The optics were also used to map the distributions of trace elements in various samples

High-density 3D graphene-based monolith and related materials, methods, and devices

Energy Technology Data Exchange (ETDEWEB)

Worsley, Marcus A.; Baumann, Theodore F.; Biener, Juergen; Charnvanichborikarn, Supakit; Kucheyev, Sergei; Montalvo, Elizabeth; Shin, Swanee; Tylski, Elijah

2017-03-21

A composition comprising at least one high-density graphene-based monolith, said monolith comprising a three-dimensional structure of graphene sheets crosslinked by covalent carbon bonds and having a density of at least 0.1 g/cm.sup.3. Also provided is a method comprising: preparing a reaction mixture comprising a suspension and at least one catalyst, said suspension selected from a graphene oxide (GO) suspension and a carbon nanotube suspension; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel, said drying step is substantially free of supercritical drying and freeze drying; and pyrolyzing the dry gel to produce a high-density graphene-based monolith. Exceptional combinations of properties are achieved including high conductive and mechanical properties.

Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

NARCIS (Netherlands)

Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

Monolithic optofluidic mode coupler for broadband thermo- and piezo-optical characterization of liquids.

Science.gov (United States)

Pumpe, Sebastian; Chemnitz, Mario; Kobelke, Jens; Schmidt, Markus A

2017-09-18

We present a monolithic fiber device that enables investigation of the thermo- and piezo-optical properties of liquids using straightforward broadband transmission measurements. The device is a directional mode coupler consisting of a multi-mode liquid core and a single-mode glass core with pronounced coupling resonances whose wavelength strongly depend on the operation temperature. We demonstrated the functionality and flexibility of our device for carbon disulfide, extending the current knowledge of the thermo-optic coefficient by 200 nm at 20 °C and uniquely for high temperatures. Moreover, our device allows measuring the piezo-optic coefficient of carbon disulfide, confirming results first obtained by Röntgen in 1891. Finally, we applied our approach to obtain the dispersion of the thermo-optic coefficients of benzene and tetrachloroethylene between 450 and 800 nm, whereas no data was available for the latter so far.

Fast preparation of hybrid monolithic columns via photo-initiated thiol-yne polymerization for capillary liquid chromatography.

Science.gov (United States)

Ma, Shujuan; Zhang, Haiyang; Li, Ya; Li, Yanan; Zhang, Na; Ou, Junjie; Ye, Mingliang; Wei, Yinmao

2018-02-23

Although several approaches have been developed to fabricate hybrid monoliths, it would still take a few hours to finish the formation of monoliths. Herein, photo-initiated thiol-yne polymerization was first adopted to in situ fabricate hybrid monoliths within the confines of UV-transparent fused-silica capillary. A silicon-containing diyne (1,3-diethynyltetramethyl-disiloxane, DYDS) was copolymerized with three multithiols, 1,6-hexanedithiol, trimethylolpropane tris(3-mercaptopropionate) and pentaerythriol tetrakis(3-mercaptopropionate), by using a binary porogenic system of diethylene glycol diethyl ether (DEGDE)/poly(ethylene glycol) (PEG200) within 10 min. Several characterizations of three hybrid monoliths (assigned as I, II and III, respectively) were performed. The results showed that these hybrid monoliths possessed bicontinuous porous structure, which was remarkably different from that via typical free-radical polymerization. The highest column efficiency of 76,000 plates per meter for butylbenzene was obtained on the column I in reversed-phase liquid chromatography (RPLC). It was observed that the efficiencies for strong-retained butylbenzene were almost close to those of weak-retained benzene, indicating a retention-independent efficient performance of small molecules on hybrid column I. The surface area of this hybrid monolith was very small in the dry state (less than 10.0 m 2 /g), and the chromatographic behavior of hybrid monolithic columns would be possibly explained by radical-mediated step-growth process of thiol-yne polymerization. Finally, the column I was applied for separation of BSA tryptic digest by cLC-MS/MS, indicating satisfactory separation ability for complicated samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation of polyhedral oligomeric silsesquioxane based hybrid monoliths by ring-opening polymerization for capillary LC and CEC.

Science.gov (United States)

Lin, Hui; Zhang, Zhenbin; Dong, Jing; Liu, Zhongshan; Ou, Junjie; Zou, Hanfa

2013-09-01

A new organic-inorganic hybrid monolith was prepared by the ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxane (POSS) with 1,4-butanediamine (BDA) using 1-propanol, 1,4-butanediol, and PEG 10,000 as a porogenic system. Benefiting from the moderate phase separation process, the resulting poly(POSS-co-BDA) hybrid monolith possessed a uniform microstructure and exhibited excellent performance in chromatographic applications. Neutral, acidic, and basic compounds were successfully separated on the hybrid monolith in capillary LC (cLC), and high column efficiencies were achieved in all of the separations. In addition, as the amino groups could generate a strong EOF, the hybrid monolith was also applied in CEC for the separation of neutral and polar compounds, and a satisfactory performance was obtained. These results demonstrate that the poly(POSS-co-BDA) hybrid monolith is a good separation media in chromatographic separations of various types of compounds by both cLC and CEC. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microchip-based monolithic column for high performance liquid chromatography

Data.gov (United States)

National Aeronautics and Space Administration — We have developed microchip based monolithic columns that can be used for liquid chromatography of small organic molecules, as well as, macromolecules such as...

Comparing monolithic and fused core HPLC columns for fast chromatographic analysis of fat-soluble vitamins.

Science.gov (United States)

Kurdi, Said El; Muaileq, Dina Abu; Alhazmi, Hassan A; Bratty, Mohammed Al; Deeb, Sami El

2017-06-27

HPLC stationary phases of monolithic and fused core type can be used to achieve fast chromatographic separation as an alternative to UPLC. In this study, monolithic and fused core stationary phases are compared for fast separation of four fat-soluble vitamins. Three new methods on the first and second generation monolithic silica RP-18e columns and a fused core pentafluoro-phenyl propyl column were developed. Application of three fused core columns offered comparable separations of retinyl palmitate, DL-α-tocopheryl acetate, cholecalciferol and menadione in terms of elution speed and separation efficiency. Separation was achieved in approx. 5 min with good resolution (Rs > 5) and precision (RSD ≤ 0.6 %). Monolithic columns showed, however, a higher number of theoretical plates, better precision and lower column backpressure than the fused core column. The three developed methods were successfully applied to separate and quantitate fat-soluble vitamins in commercial products.

Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean

International Nuclear Information System (INIS)

Zhai, Haiyun; Su, Zihao; Chen, Zuanguang; Liu, Zhenping; Yuan, Kaisong; Huang, Lu

2015-01-01

Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g −1 . - Abstract: A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC–LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001–2.0 μg mL −1 (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL −1 . Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC–LIF method can be applied to sensitively determine phloxine B in coffee bean

Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean

Energy Technology Data Exchange (ETDEWEB)

Zhai, Haiyun, E-mail: zhaihaiyun@126.com [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Su, Zihao [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Chen, Zuanguang, E-mail: chenzg@mail.sysu.edu.cn [School of Pharmaceutical Science, Sun Yat-sen University, Guangzhou 510006 (China); Liu, Zhenping; Yuan, Kaisong; Huang, Lu [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China)

2015-03-20

Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g{sup −1}. - Abstract: A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC–LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001–2.0 μg mL{sup −1} (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL{sup −1}. Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC–LIF method can be applied to sensitively determine phloxine B in coffee bean.

Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

International Nuclear Information System (INIS)

Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

2008-01-01

Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Pena, Francisco; Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain)], E-mail: bendicho@uvigo.es

2008-04-15

Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 {mu}g/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters.

Applications of Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry (SPME-GC/MS in the Study of Grape and Wine Volatile Compounds

Directory of Open Access Journals (Sweden)

Annarita Panighel

2014-12-01

Full Text Available Volatile compounds are responsible for the wine “bouquet”, which is perceived by sniffing the headspace of a glass, and of the aroma component (palate-aroma of the overall flavor, which is perceived on drinking. Grape aroma compounds are transferred to the wine and undergo minimal alteration during fermentation (e.g., monoterpenes and methoxypyrazines; others are precursors of aroma compounds which form in winemaking and during wine aging (e.g., glycosidically-bound volatile compounds and C13-norisoprenoids. Headspace solid phase microextraction (HS-SPME is a fast and simple technique which was developed for analysis of volatile compounds. This review describes some SPME methods coupled with gas chromatography/mass spectrometry (GC/MS used to study the grape and wine volatiles.

Study of monolithic prestressed reinforced concrete overhead road.

Directory of Open Access Journals (Sweden)

Ya.I. Kovalchyk

2011-12-01

Full Text Available Results of inspection and testing of monolithic prestressed reinforced concrete road trestle built in Kyiv are considered. The analysis of the gained results has shown that parametres correspond to the requirements of current standards on design of bridges.

Monolithic all-PM femtosecond Yb-doped fiber laser using photonic bandgap fibers

DEFF Research Database (Denmark)

Liu, Xiaomin; Lægsgaard, Jesper; Turchinovich, Dmitry

2009-01-01

We present a monolithic Yb fiber laser, dispersion managed by an all-solid photonic bandgap fiber, and pulse compressed in a hollow-core photonic crystal fiber. The laser delivers 9 nJ, 275-fs long pulses at 1035 nm.......We present a monolithic Yb fiber laser, dispersion managed by an all-solid photonic bandgap fiber, and pulse compressed in a hollow-core photonic crystal fiber. The laser delivers 9 nJ, 275-fs long pulses at 1035 nm....

Low frequency seismic noise acquisition and analysis with tunable monolithic horizontal sensors

Science.gov (United States)

Acernese, Fausto; De Rosa, Rosario; Giordano, Gerardo; Romano, Rocco; Vilasi, Silvia; Barone, Fabrizio

2011-04-01

In this paper we describe the scientific data recorded mechanical monolithic horizontal sensor prototypes located in the Gran Sasso Laboratory of the INFN. The mechanical monolithic sensors, developed at the University of Salerno, are placed, in thermally insulating enclosures, onto concrete slabs connected to the bedrock. The main goal of this experiment is to characterize seismically the sites in the frequency band 10-4 ÷ 10Hz and to get all the necessary information to optimize the sensor.

Development of an analytical method coupling cell membrane chromatography with gas chromatography-mass spectrometry via microextraction by packed sorbent and its application in the screening of volatile active compounds in natural products.

Science.gov (United States)

Li, Miao; Wang, Sicen; He, Langchong

2015-01-01

Natural products (NPs) are important sources of lead compounds in modern drug discovery. To facilitate the screening of volatile active compounds in NPs, we have developed a new biochromatography method that uses rat vascular smooth muscle cells (VSMC), which are rich in L-type calcium channels (LCC), to prepare the stationary phase. This integrated method, which couples cell membrane chromatography (CMC) with gas chromatography-mass spectrometry (GC-MS) via microextraction by packed sorbent (MEPS) technology, has been termed VSMC/CMC-MEPS-GC-MS. Methodological validation confirmed its specificity, reliability and convenience. Screening results for Radix Angelicae Dahuricae and Fructus Cnidii obtained using VSMC/CMC-MEPS-GC-MS were consistent with those obtained using VSMC/CMC-offline-GC-MS. MEPS connection plays as simplified solid-phase extraction and replaces the uncontrollable evaporation operation in reported offline connections, so our new method is supposed to be more efficient and reliable than the offline ones, especially for compounds that are volatile, thermally unstable or difficult to purify. In application, senkyunolide A and ligustilide were preliminary identified as the volatile active components in Rhizoma Chuanxiong. We have thus confirmed the suitability of VSMC/CMC-MEPS-GC-MS for volatile active compounds screening in NP. Copyright © 2014 Elsevier B.V. All rights reserved.

An on-line push/pull perfusion-based hollow-fiber liquid-phase microextraction system for high-performance liquid chromatographic determination of alkylphenols in water samples.

Science.gov (United States)

Chao, Yu-Ying; Jian, Zhi-Xuan; Tu, Yi-Ming; Wang, Hsaio-Wen; Huang, Yeou-Lih

2013-06-07

In this study, we employed a novel on-line method, push/pull perfusion hollow-fiber liquid-phase microextraction (PPP-HF-LPME), to extract 4-tert-butylphenol, 2,4-di-tert-butylphenol, 4-n-nonylphenol, and 4-n-octylphenol from river and tap water samples; we then separated and quantified the extracted analytes through high-performance liquid chromatography (HPLC). Using this approach, we overcame the problem of fluid loss across the porous HF membrane to the donor phase, permitting on-line coupling of HF-LPME to HPLC. In our PPP-HF-LPME system, we used a push/pull syringe pump as the driving source to perfuse the acceptor phase, while employing a heating mantle and an ultrasonic probe to accelerate mass transfer. We optimized the experimental conditions such as the nature of the HF supported intermediary phase and the acceptor phase, the composition of the donor and acceptor phases, the sample temperature, and the sonication conditions. Our proposed method provided relative standard deviations of 3.1-6.2%, coefficients of determination (r(2)) of 0.9989-0.9998, and limits of detection of 0.03-0.2 ng mL(-1) for the analytes under the optimized conditions. When we applied this method to analyses of river and tap water samples, our results confirmed that this microextraction technique allows reliable monitoring of alkylphenols in water samples.

Influence of the linking spacer length and type on the enantioseparation ability of β-cyclodextrin functionalized monoliths.

Science.gov (United States)

Guo, Jialiang; Xiao, Yuan; Lin, Yuanjing; Zhang, Qiaoxuan; Chang, Yiqun; Crommen, Jacques; Jiang, Zhengjin

2016-05-15

In order to investigate the effect of the linking spacer on the enantioseparation ability of β-cyclodextrin (β-CD) functionalized polymeric monoliths, three β-CD-functionalized organic polymeric monoliths with different spacer lengths were prepared by using three amino-β-CDs, i.e. mono-6-amino-6-deoxy-β-CD, mono-6-ethylenediamine-6-deoxy-β-CD, mono-6-hexamethylenediamine-6-deoxy-β-CD, as starting materials. These amino-β-CDs reacted with glycidyl methacrylate to produce functional monomers which were then copolymerized with ethylene dimethacrylate. The enantioseparation ability of the three monoliths was evaluated using 14 chiral acidic compounds, including mandelic acid derivatives, nonsteroidal anti-inflammatory drugs, N-derivatized amino acids, and chiral herbicides under optimum chromatographic conditions. Notably, the poly(GMA-NH2-β-CD-co-EDMA) column provides higher enantioresolution and enantioselectivity than the poly(GMA-EDA-β-CD-co-EDMA) and poly(GMA-HDA-β-CD-co-EDMA) columns for most tested chiral analytes. Furthermore, the enantioseparation performance of triazole-linker containing monoliths was compared to that of ethylenediamine-linker containing monoliths. The results indicate that the enantioselectivity of β-CD monolithic columns is strongly related to the length and type of spacer tethering β-CD to the polymeric support. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid and simple preparation of thiol-ene emulsion-templated monoliths and their application as enzymatic microreactors

DEFF Research Database (Denmark)

Lafleur, Josiane P; Senkbeil, Silja; Novotny, Jakub

2015-01-01

A novel, rapid and simple method for the preparation of emulsion-templated monoliths in microfluidic channels based on thiol-ene chemistry is presented. The method allows monolith synthesis and anchoring inside thiol-ene microchannels in a single photoinitiated step. Characterization by scanning...... electron microscopy showed that the methanol-based emulsion templating process resulted in a network of highly interconnected and regular thiol-ene beads anchored solidly inside thiol-ene microchannels. Surface area measurements indicate that the monoliths are macroporous, with no or little micro...

Monolithic Perovskite Silicon Tandem Solar Cells with Advanced Optics

Energy Technology Data Exchange (ETDEWEB)

Goldschmidt, Jan C.; Bett, Alexander J.; Bivour, Martin; Blasi, Benedikt; Eisenlohr, Johannes; Kohlstadt, Markus; Lee, Seunghun; Mastroianni, Simone; Mundt, Laura; Mundus, Markus; Ndione, Paul; Reichel, Christian; Schubert, Martin; Schulze, Patricia S.; Tucher, Nico; Veit, Clemens; Veurman, Welmoed; Wienands, Karl; Winkler, Kristina; Wurfel, Uli; Glunz, Stefan W.; Hermle, Martin

2016-11-14

For high efficiency monolithic perovskite silicon tandem solar cells, we develop low-temperature processes for the perovskite top cell, rear-side light trapping, optimized perovskite growth, transparent contacts and adapted characterization methods.

Monolithic junction field-effect transistor charge preamplifier for calorimetry at high luminosity hadron colliders

International Nuclear Information System (INIS)

Radeka, V.; Rescia, S.; Rehn, L.A.; Manfredi, P.F.; Speziali, V.

1991-11-01

The outstanding noise and radiation hardness characteristics of epitaxial-channel junction field-effect transistors (JFET) suggest that a monolithic preamplifier based upon them may be able to meet the strict specifications for calorimetry at high luminosity colliders. Results obtained so far with a buried layer planar technology, among them an entire monolithic charge-sensitive preamplifier, are described

Comparing monolithic and fused core HPLC columns for fast chromatographic analysis of fat-soluble vitamins

Directory of Open Access Journals (Sweden)

Kurdi Said El

2017-06-01

Full Text Available HPLC stationary phases of monolithic and fused core type can be used to achieve fast chromatographic separation as an alternative to UPLC. In this study, monolithic and fused core stationary phases are compared for fast separation of four fat-soluble vitamins. Three new methods on the first and second generation monolithic silica RP-18e columns and a fused core pentafluoro-phenyl propyl column were developed. Application of three fused core columns offered comparable separations of retinyl palmitate, DL-α-tocopheryl acetate, cholecalciferol and menadione in terms of elution speed and separation efficiency. Separation was achieved in approx. 5 min with good resolution (Rs > 5 and precision (RSD ≤ 0.6 %. Monolithic columns showed, however, a higher number of theoretical plates, better precision and lower column backpressure than the fused core column. The three developed methods were successfully applied to separate and quantitate fat-soluble vitamins in commercial products.

Chiral monolithic absorbent constructed by optically active helical-substituted polyacetylene and graphene oxide: preparation and chiral absorption capacity.

Science.gov (United States)

Li, Weifei; Wang, Bo; Yang, Wantai; Deng, Jianping

2015-02-01

Chiral monolithic absorbent is successfully constructed for the first time by using optically active helical-substituted polyacetylene and graphene oxide (GO). The preparative strategy is facile and straightforward, in which chiral-substituted acetylene monomer (Ma), cross-linker (Mb), and alkynylated GO (Mc) undergo copolymerization to form the desired monolithic absorbent in quantitative yield. The resulting monoliths are characterized by circular dichroism, UV-vis absorption, scanning electron microscopy (SEM), FT-IR, Raman, energy-dispersive spectrometer (EDS), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), XPS, and thermogravimetric analysis (TGA) techniques. The polymer chains derived from Ma form chiral helical structures and thus provide optical activity to the monoliths, while GO sheets contribute to the formation of porous structures. The porous structure enables the monolithic absorbents to demonstrate a large swelling ratio in organic solvents, and more remarkably, the helical polymer chains provide optical activity and further enantio-differentiating absorption ability. The present study establishes an efficient and versatile methodology for preparing novel functional materials, in particular monolithic chiral materials based on substituted polyacetylene and GO. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid–liquid microextraction in a multicommuted flow system for direct spectrophotometric determination of iodine value in biodiesel

Energy Technology Data Exchange (ETDEWEB)

Pereira, Andréia C.; Rocha, Fábio R.P., E-mail: frprocha@cena.usp.br

2014-06-01

Highlights: • First flow-based procedure for iodine value determination in biodiesel. • Simple, fast and reliable procedure. • Detection without sample pretreatment or phase separation. • Liquid–liquid microextraction with low sample and reagent volumes. • Avoid toxic reagents and organic solvent used in the reference procedure. Abstract: A flow-based procedure was developed for the direct spectrophotometric determination of the iodine value (IV) in biodiesel. The procedure was based on the microextraction/reaction of unsaturated compounds with triiodide ions in an aqueous medium by inserting the reagent solution between the aliquots of biodiesel without any pretreatment. The interaction occurred through the biodiesel film formed on the inner walls of the hydrophobic tube used as the reactor and at the aqueous/biodiesel interfaces. The spectrophotometric detection was based on the discoloration of the I₃⁻ reagent in the aqueous phase by using a glass tube coupled to a fiber-optic spectrophotometer as the detection cell. Reference solutions were prepared by dilution of biodiesel samples with previously determined IV in hexane. The analytical response was linear for IV from 13 to 135 g I₂/100 g with a detection limit of 5 g I₂/100 g. A coefficient of variation of 1.7% (n = 10) and a sampling rate of 108 determinations per hour were achieved by consuming 224 μL of the sample and 200 μg of I₂ per determination. The slopes of analytical curves obtained with three different biodiesel samples were in agreement (variations in slopes lower than 3.1%), thus indicating an absence of any matrix effects. Results for biodiesel samples from different sources agreed with the volumetric official procedure at the 95% confidence level. The proposed procedure is therefore a simple, fast, and reliable alternative for estimating the iodine value of biodiesel.

Liquid–liquid microextraction in a multicommuted flow system for direct spectrophotometric determination of iodine value in biodiesel

International Nuclear Information System (INIS)

Pereira, Andréia C.; Rocha, Fábio R.P.

2014-01-01

Highlights: • First flow-based procedure for iodine value determination in biodiesel. • Simple, fast and reliable procedure. • Detection without sample pretreatment or phase separation. • Liquid–liquid microextraction with low sample and reagent volumes. • Avoid toxic reagents and organic solvent used in the reference procedure. - Abstract: A flow-based procedure was developed for the direct spectrophotometric determination of the iodine value (IV) in biodiesel. The procedure was based on the microextraction/reaction of unsaturated compounds with triiodide ions in an aqueous medium by inserting the reagent solution between the aliquots of biodiesel without any pretreatment. The interaction occurred through the biodiesel film formed on the inner walls of the hydrophobic tube used as the reactor and at the aqueous/biodiesel interfaces. The spectrophotometric detection was based on the discoloration of the I 3 − reagent in the aqueous phase by using a glass tube coupled to a fiber-optic spectrophotometer as the detection cell. Reference solutions were prepared by dilution of biodiesel samples with previously determined IV in hexane. The analytical response was linear for IV from 13 to 135 g I 2 /100 g with a detection limit of 5 g I 2 /100 g. A coefficient of variation of 1.7% (n = 10) and a sampling rate of 108 determinations per hour were achieved by consuming 224 μL of the sample and 200 μg of I 2 per determination. The slopes of analytical curves obtained with three different biodiesel samples were in agreement (variations in slopes lower than 3.1%), thus indicating an absence of any matrix effects. Results for biodiesel samples from different sources agreed with the volumetric official procedure at the 95% confidence level. The proposed procedure is therefore a simple, fast, and reliable alternative for estimating the iodine value of biodiesel

Preparation and characterization of fluorophenylboronic acid-functionalized affinity monolithic columns for the selective enrichment of cis-diol-containing biomolecules.

Science.gov (United States)

Li, Qianjin; Liu, Zhen

2015-01-01

Boronate affinity monolithic columns have been developed into an important means for the selective recognition and capture of cis-diol-containing biomolecules, such as glycoproteins, nucleosides and saccharides. The ligands of boronic acids are playing an important role in boronate affinity monolithic columns. Although several boronate affinity monoliths with high affinity toward cis-diol-containing biomolecules have been reported, only few publications are focused on their detailed procedures for preparation and characterization. This chapter describes in detail the preparation and characterization of a boronate affinity monolithic column applying 2,4-difluoro-3-formyl-phenylboronic acid (DFFPBA) as a ligand. The DFFPBA-functionalized monolithic column not only exhibited an ultrahigh boronate affinity toward cis-diol-containing biomolecules, but also showed great potential for the selective enrichment of cis-diol-containing biomolecules in real samples.

Comparison of Membrane Chromatography and Monolith Chromatography for Lactoferrin and Bovine Serum Albumin Separation

Directory of Open Access Journals (Sweden)

Chalore Teepakorn

2016-09-01

Full Text Available These last few decades, membranes and monoliths have been increasingly used as stationary phases for chromatography. Their fast mass transfer is mainly based on convection, which leads to reduced diffusion, which is usually observed in resins. Nevertheless, poor flow distribution, which causes inefficient binding, remains a major challenge for the development of both membrane and monolith devices. Moreover, the comparison of membranes and monoliths for biomolecule separation has been very poorly investigated. In this paper, the separation of two proteins, bovine serum albumin (BSA and lactoferrin (LF, with similar sizes, but different isoelectric points, was investigated at a pH of 6.0 with a BSA-LF concentration ratio of 2/1 (2.00 mg·mL−1 BSA and 1.00 mg·mL−1 LF solution using strong cation exchange membranes and monoliths packed in the same housing, as well as commercialized devices. The feeding flow rate was operated at 12.0 bed volume (BV/min for all devices. Afterward, bound LF was eluted using a phosphate-buffered saline solution with 2.00 M NaCl. Using membranes in a CIM housing from BIA Separations (Slovenia with porous frits before and after the membrane bed, higher binding capacities, sharper breakthrough curves, as well as sharper and more symmetric elution peaks were obtained. The monolith and commercialized membrane devices showed lower LF binding capacity and broadened and non-symmetric elution peaks.

Analysis of amino acid and monoamine neurotransmitters and their metabolites in rat urine of Alzheimer's disease using in situ ultrasound-assisted derivatization dispersive liquid-liquid microextraction with UHPLC-MS/MS.

Science.gov (United States)

Zhao, Xian-En; He, Yongrui; Li, Meng; Chen, Guang; Wei, Na; Wang, Xiao; Sun, Jing; Zhu, Shuyun; You, Jinmao

2017-02-20

Neurotransmitters (NTs) may play an important role in neurodegenerative disorders such as Alzheimer's disease (AD). In order to investigate the potential links, a new simple, fast, accurate and sensitive analytical method, based on in situ ultrasound-assisted derivatization dispersive liquid-liquid microextraction (in situ UA-DDLLME) coupled with ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS), has been developed and validated. The quantitation of amino acid neurotransmitters (AANTs) and monoamine neurotransmitters (MANTs) in urine of AD rats were performed in this work. The in situ UA-DDLLME procedure involved the rapid injection of the mixture of low toxic 4-bromoanisole (extractant) and acetonitrile (dispersant), which containing the new designed and synthesized 4'-carbonyl chloride rosamine (CCR) as derivatization reagent, into the aqueous phase of real sample and buffer. Under the selected conditions, the derivatization and microextraction of analytes were simultaneously completed within 1min. Good linearity for each analyte (R>0.992) was observed with low limit of detections (LODs, S/N>3). Moreover, the proposed method was compared with direct detection or other reported methods, and the results showed that low matrix effects and good recoveries results were obtained in this work. Taken together, in situ UA-DDLLME coupled with UHPLC-MS/MS analysis was demonstrated to be a good method for sensitive, accurate and simultaneous monitoring of AANTs and MANTs. This method would be expected to be highly useful in AD diseases' clinical diagnostics and may have potential value in monitoring the efficacy of treatment. Copyright © 2016 Elsevier B.V. All rights reserved.

Solid-phase microextraction of Methylene Blue using carboxy graphene-modified steel wires, and its detection by electrochemiluminescence

International Nuclear Information System (INIS)

Wang, Sui; Lv, Shasha; Guo, Zhiyong; Jiang, Feng

2014-01-01

We report on a new solid phase for microextraction (SPME) of Methylene Blue (MB). It was obtained by immobilizing carboxy graphene (G-COOH) on a stainless steel wire. Scanning electron micrography showed the surface to be homogeneous, porous and wrinkled. The effects of sample solution pH, extraction time, stirring rate, desorption time and of desorption solvent on the efficiency of extraction of MB were optimized. The new SPME was coupled to electrochemiluminescence detection of MB and gave a linear analytical range from 2.7 nM to 1.3 μM, and the detection limit is 0.89 nM which is better than other methods. When considering the enrichment factor of ∼20, the resulting detection limit is estimated to be 45 pM. The new SPME fiber was successfully applied to the analysis of MB in spiked real water samples. Recoveries range from 95.7 % to 113.0 %, and relative standard deviations are <5.0 %, which showed the good reproducibility of the method. (author)

Material Engineering for Monolithic Semiconductor Mode-Locked Lasers

DEFF Research Database (Denmark)

Kulkova, Irina

This thesis is devoted to the materials engineering for semiconductor monolithic passively mode-locked lasers (MLLs) as a compact energy-efficient source of ultrashort optical pulses. Up to the present day, the achievement of low-noise sub-picosecond pulse generation has remained a challenge...

[Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

Science.gov (United States)

Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

2015-11-01

To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

Fabrication of Monolithic Dye-Sensitized Solar Cell Using Ionic Liquid Electrolyte

Directory of Open Access Journals (Sweden)

Seigo Ito

2012-01-01

Full Text Available To improve the durability of dye-sensitized solar cells (DSCs, monolithic DSCs with ionic liquid electrolyte were studied. Deposited by screen printing, a carbon layer was successfully fabricated that did not crack or peel when annealing was employed beforehand. Optimized electrodes exhibited photovoltaic characteristics of 0.608 V open-circuit voltage, 6.90 cm−2 mA short-circuit current, and 0.491 fill factor, yielding 2.06% power conversion efficiency. The monolithic DSC using ionic liquid electrolyte was thermally durable and operated stably for 1000 h at 80°C.

Monolithic Parallel Tandem Organic Photovoltaic Cell with Transparent Carbon Nanotube Interlayer

Science.gov (United States)

Tanaka, S.; Mielczarek, K.; Ovalle-Robles, R.; Wang, B.; Hsu, D.; Zakhidov, A. A.

2009-01-01

We demonstrate an organic photovoltaic cell with a monolithic tandem structure in parallel connection. Transparent multiwalled carbon nanotube sheets are used as an interlayer anode electrode for this parallel tandem. The characteristics of front and back cells are measured independently. The short circuit current density of the parallel tandem cell is larger than the currents of each individual cell. The wavelength dependence of photocurrent for the parallel tandem cell shows the superposition spectrum of the two spectral sensitivities of the front and back cells. The monolithic three-electrode photovoltaic cell indeed operates as a parallel tandem with improved efficiency.

Design for an 8 Meter Monolithic UV/OIR Space Telescope

Science.gov (United States)

Stahl, H. Philip; Postman, Marc; Hornsby, Linda; Hopkins, Randall; Mosier, Gary E.; Pasquale, Bert A.; Arnold, William R.

2009-01-01

ATLAST-8 is an 8-meter monolithic UV/optical/NIR space observatory to be placed in orbit at Sun-Earth L2 by NASA's planned Ares V cargo launch vehicle. The ATLAST-8 will yield fundamental astronomical breakthroughs. The mission concept utilizes two enabling technologies: planned Ares-V launch vehicle (scheduled for 2019) and autonomous rendezvous and docking (AR&D). The unprecedented Ares-V payload and mass capacity enables the use of a massive, monolithic, thin-meniscus primary mirror - similar to a VLT or Subaru. Furthermore, it enables simple robust design rules to mitigate cost, schedule and performance risk. AR&D enables on-orbit servicing, extending mission life and enhancing science return.

Continuous-Flow Monolithic Silica Microreactors with Arenesulphonic Acid Groups: Structure–Catalytic Activity Relationships

Directory of Open Access Journals (Sweden)

Agnieszka Ciemięga

2017-08-01

Full Text Available The performance of monolithic silica microreactors activated with sulphonic acid groups and a packed bed reactor with Amberlyst 15 resin were compared in the esterification of acetic acid with n-butanol. The monolithic microreactors were made of single silica rods with complex pore architecture, differing in the size of mesopores, and in particular, flow-through macropores which significantly affected the flow characteristic of the continuous system. The highest ester productivity of 105.2 mol·molH+−1·h−1 was achieved in microreactor M1 with the largest porosity, characterized by a total pore volume of 4 cm3·g−1, mesopores with 20 nm diameter, and large flow-through macropores 30–50 μm in size. The strong impact of the permeability of the monoliths on a reaction kinetics was shown.

Assessment of the Grouted IXC Monolith in Support of K East Basin Hazard Categorization

Energy Technology Data Exchange (ETDEWEB)

Short, Steven M.; Dodson, Michael G.; Alzheimer, James M.; Meyer, Perry A.

2007-10-12

Addendum to original report updating the structural analysis of the I-beam accident to reflect a smaller I-beam than originally assumed (addendum is 2 pages). The K East Basin currently contains six ion exchange columns (IXCs) that were removed from service over 10 years ago. Fluor Hanford plans to immobilize the six ion exchange columns (IXCs) in place in a concrete monolith. PNNL performed a structural assessment of the concrete monolith to determine its capability to absorb the forces imposed by postulated accidents and protect the IXCs from damage and thus prevent a release of radioactive material. From this assessment, design specifications for the concrete monolith were identified that would prevent a release of radioactive material for any of the postulated hazardous conditions.

Error analysis for a monolithic discretization of coupled Darcy and Stokes problems

KAUST Repository

Girault, V.; Kanschat, G.; Riviè re, B.

2014-01-01

© de Gruyter 2014. The coupled Stokes and Darcy equations are approximated by a strongly conservative finite element method. The discrete spaces are the divergence-conforming velocity space with matching pressure space such as the Raviart

Impact of gastric acidic challenge on surface topography and optical properties of monolithic zirconia.

Science.gov (United States)

Sulaiman, Taiseer A; Abdulmajeed, Aous A; Shahramian, Khalil; Hupa, Leena; Donovan, Terrence E; Vallittu, Pekka; Närhi, Timo O

2015-12-01

To evaluate the surface topography and optical properties of monolithic zirconia after immersion in simulated gastric acid. Four partially stabilized (PSZ) and one fully stabilized (FSZ) zirconia materials were selected for the study: Prettau (PRT, Zirkonzahn), Zenostar (ZEN, Ivoclar), Bruxzir (BRX, Glidewell), Katana (KAT, Noritake) and FSZ Prettau Anterior (PRTA, Zirkonzahn). IPS e.max (Ivoclar) was used as a control. The specimens (10×10×1.2mm, n=5 per material) were cut, sintered, polished and cleaned before immersed in 5ml of simulated gastric acid solution (Hydrochloric acid (HCl) 0.06M, 0.113% solution in deionized distal water, pH 1.2) for 96h in a 37°C incubator. Specimens were weighed and examined for morphological changes under scanning electron microscope (SEM) coupled with energy dispersive X-ray spectroscopy (EDX). Surface roughness was evaluated by a confocal microscope. Surface gloss and translucency parameter (TP) values were determined by a reflection spectrophotometer before and after acid immersion. The data was analyzed by one-way ANOVA followed by Tukey's HSD post hoc test (pgloss of ZEN, PRTA and IPS e.max increased (p<0.05). Monolithic zirconia materials show some surface alterations in an acidic environment with minimum effect on their optical properties. Whether a smoother surface is in fact a sign of true corrosion resistance or is purely the result of an evenly progressive corrosive process is yet to be confirmed by further research. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Chromatographic selectivity of poly(alkyl methacrylate-co-divinylbenzene) monolithic columns for polar aromatic compounds by pressure-driven capillary liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

2016-10-05

In this study, divinylbenzene (DVB) was used as the cross-linker to prepare alkyl methacrylate (AlMA) monoliths for incorporating π-π interactions between the aromatic analytes and AlMA-DVB monolithic stationary phases in capillary LC analysis. Various AlMA/DVB ratios were investigated to prepare a series of 30% AlMA-DVB monolithic stationary phases in fused-silica capillaries (250-μm i.d.). The physical properties (such as porosity, permeability, and column efficiency) of the synthesized AlMA-DVB monolithic columns were investigated for characterization. Isocratic elution of phenol derivatives was first employed to evaluate the suitability of the prepared AlMA-DVB columns for small molecule separation. The run-to-run (0.16–1.20%, RSD; n = 3) and column-to-column (0.26–2.95%, RSD; n = 3) repeatabilities on retention times were also examined using the selected AlMA-DVB monolithic columns. The π-π interactions between the aromatic ring and the DVB-based stationary phase offered better recognition on polar analytes with aromatic moieties, which resulted in better separation resolution of aromatic analytes on the AlMA-DVB monolithic columns. In order to demonstrate the capability of potential environmental and/or food safety applications, eight phenylurea herbicides with single benzene ring and seven sulfonamide antibiotics with polyaromatic moieties were analyzed using the selected AlMA-DVB monolithic columns. - Highlights: • First investigation on chromatographic selectivity of AlMA-DVB monolithic columns. • Good run-to-run/column-to-column repeatability (<3%) on AlMA-DVB monolithic columns. • Efficient separation of phenylurea herbicides and sulfonamides on AlMA-DVB columns.

Monolithic microwave integrated circuit with integral array antenna

International Nuclear Information System (INIS)

Stockton, R.J.; Munson, R.E.

1984-01-01

A monolithic microwave integrated circuit including an integral array antenna. The system includes radiating elements, feed network, phasing network, active and/or passive semiconductor devices, digital logic interface circuits and a microcomputer controller simultaneously incorporated on a single substrate by means of a controlled fabrication process sequence

Preparation and characterization of Au/CeO{sub 2}-Al{sub 2}O{sub 3} monoliths

Energy Technology Data Exchange (ETDEWEB)

Gawel, Bartlomiej; Lambrechts, Kalle [Ugelstad Laboratory, Department of Chemical Engineering, Norwegian University of Science and Technology (NTNU), N-7491 Trondheim (Norway); Oye, Gisle, E-mail: gisle.oye@chemeng.ntnu.no [Ugelstad Laboratory, Department of Chemical Engineering, Norwegian University of Science and Technology (NTNU), N-7491 Trondheim (Norway)

2012-05-15

Highlights: Black-Right-Pointing-Pointer A facile method for preparing Au/CeO{sub 2}-Al{sub 2}O{sub 3} monoliths with hierarchical porosity. Black-Right-Pointing-Pointer Continuous-flow testing of the monoliths in liquid-phase oxidation of glucose. Black-Right-Pointing-Pointer Increased catalytic activity in the presence of cerium oxide (stirred-batch tests). - Abstract: Porous CeO{sub 2}-Al{sub 2}O{sub 3} monoliths with hierarchical pore structure were prepared by mixing boehmite particles with solutions containing different amounts of cerium chloride and aluminum nitrate. The monoliths were functionalized with gold nanoparticles using the incipient wetness method. The resulting materials were characterized by X-ray diffraction, nitrogen sorption, mercury porosimetry, UV-vis spectroscopy and transmission electron microscopy. The catalysts were tested in liquid phase glucose oxidation, comparing continuously stirred batch reactor and continuous-flow fix-bed reactor setups.

Fabrication of a novel hemin-based monolithic column and its application in separation of protein from complex bio-matrix.

Science.gov (United States)

Jiang, Xiaoya; Zhang, Doudou; Li, Xueying; Wang, Xixi; Bai, Ligai; Liu, Haiyan; Yan, Hongyuan

2017-05-10

A novel polymer-based monolithic column was prepared via redox initiation system within the confines of a stainless steel column with 4.6mm i.d. In the processes, hemin and lauryl methacrylate were used as co-monomers; ethylene dimethacrylate as crosslinking agent; n-butyl alcohol, ethanediol, and N, N-dimethylformamide as tri-porogens; benzoyl peroxide and N, N-dimethyl aniline as redox initiation system. The resulting polymer-based monolithic columns were characterized by scanning electron microscopy, nitrogen adsorption-desorption instrument, and mercury intrusion porosimeter, respectively. The results illustrated that the improved monolith had relative uniform porous structure, good permeability, and low back pressure. Aromatic compounds were used to test the chromatographic behavior of the monolith, resulting in highest column efficiency of 19 880 plates per meter with reversed-phase mechanism. Furthermore, the homemade monolith was used as the stationary phase of high performance liquid chromatography to separate proteins from complex bio-matrix, including human plasma, egg white, and snailase. The results showed that the monolithic column occupied good separation ability with these complex bio-samples. Excellent specific character of the homemade hemin-based monolith was that it could simultaneously remove high-abundance proteins (including human serum albumin, immunoglobulin G, and human fibrinogen) from human plasma and separate other proteins to different fractions. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrastrong light-matter coupling in electrically doped microcavity organic light emitting diodes

Energy Technology Data Exchange (ETDEWEB)

Mazzeo, M., E-mail: marco.mazzeo@unisalento.it [Dipartimento di Matematica e Fisica “Ennio De Giorgi”, Università del Salento, Via Monteroni, 73100 Lecce (Italy); NNL, Istituto Nanoscienze - CNR, Via Arnesano, 73100 Lecce (Italy); Genco, A. [Dipartimento di Matematica e Fisica “Ennio De Giorgi”, Università del Salento, Via Monteroni, 73100 Lecce (Italy); Gambino, S. [NNL, Istituto Nanoscienze - CNR, Via Arnesano, 73100 Lecce (Italy); CBN, Istituto Italiano Tecnologia, Via Barsanti 1, 73010 Lecce (Italy); Ballarini, D.; Mangione, F.; Sanvitto, D. [NNL, Istituto Nanoscienze - CNR, Via Arnesano, 73100 Lecce (Italy); Di Stefano, O.; Patanè, S.; Savasta, S. [Dipartimento di Fisica e Scienze della Terra, Università di Messina, Viale F. Stagno d' Alcontres 31, 98166 Messina (Italy); Gigli, G. [Dipartimento di Matematica e Fisica “Ennio De Giorgi”, Università del Salento, Via Monteroni, 73100 Lecce (Italy); NNL, Istituto Nanoscienze - CNR, Via Arnesano, 73100 Lecce (Italy); CBN, Istituto Italiano Tecnologia, Via Barsanti 1, 73010 Lecce (Italy)

2014-06-09

The coupling of the electromagnetic field with an electronic transition gives rise, for strong enough light-matter interactions, to hybrid states called exciton-polaritons. When the energy exchanged between light and matter becomes a significant fraction of the material transition energy an extreme optical regime called ultrastrong coupling (USC) is achieved. We report a microcavity embedded p-i-n monolithic organic light emitting diode working in USC, employing a thin film of squaraine dye as active layer. A normalized coupling ratio of 30% has been achieved at room temperature. These USC devices exhibit a dispersion-less angle-resolved electroluminescence that can be exploited for the realization of innovative optoelectronic devices. Our results may open the way towards electrically pumped polariton lasers.

Development of stable monolithic wide-field Michelson interferometers.

Science.gov (United States)

Wan, Xiaoke; Ge, Jian; Chen, Zhiping

2011-07-20

Bulk wide-field Michelson interferometers are very useful for high precision applications in remote sensing and astronomy. A stable monolithic Michelson interferometer is a key element in high precision radial velocity (RV) measurements for extrasolar planets searching and studies. Thermal stress analysis shows that matching coefficients of thermal expansion (CTEs) is a critical requirement for ensuring interferometer stability. This requirement leads to a novel design using BK7 and LAK7 materials, such that the monolithic interferometer is free from thermal distortion. The processes of design, fabrication, and testing of interferometers are described in detail. In performance evaluations, the field angle is typically 23.8° and thermal sensitivity is typically -2.6×10(-6)/°C near 550 nm, which corresponds to ∼800 m/s/°C in the RV scale. Low-cost interferometer products have been commissioned in multiple RV instruments, and they are producing high stability performance over long term operations. © 2011 Optical Society of America

Facile preparation of multifunctional carbon nanotube/magnetite/polyaniline nanocomposite offering a strong option for efficient solid-phase microextraction coupled with GC-MS for the analysis of phenolic compounds.

Science.gov (United States)

Tafazoli, Zahra; Azar, Parviz Aberoomand; Tehrani, Mohammad Saber; Husain, Syed Waqif

2018-04-20

The aim of this study the synthesis of a highly efficient organic-inorganic nanocomposite. In this research, the carbon nanotube/magnetite/polyaniline nanocomposite was successfully prepared through a facile route. Monodisperse magnetite nanospheres were prepared through the coprecipitation route, and polyaniline nanolayer as a modified shell with a high surface area was synthesized by an in situ growth route and characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and energy dispersive X-ray spectroscopy. The prepared nanocomposite was immobilized on a stainless-steel wire for the fabrication of the solid-phase microextraction fiber. The combination of headspace solid-phase microextraction using carbon nanotube/magnetite/polyaniline nanocomposite fiber with gas chromatography and mass spectrometry can achieve a low limit of detection and can be applied to determine phenolic compounds in water samples. The effects of the extraction and desorption parameters including extraction temperature and time, ionic strength, stirring rate, pH, and desorption temperature and time have been studied. Under the optimum conditions, the dynamic linear range was 0.01-500 ng mL -1 and the limits of detection of phenol, 4-chlorophenol, 2,6-dichlorophenol, and 2,4,6-trichlorophenol were the lowest (0.008 ng mL -1 ) for three times. The coefficient of determination of all calibration curves was more than 0.990. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Dispersive solid phase micro-extraction of mercury(II from environmental water and vegetable samples with ionic liquid modified graphene oxide nanoparticles

Directory of Open Access Journals (Sweden)

Nasrollahpour Atefeh

2017-01-01

Full Text Available A new dispersive solid phase micro-extraction (dispersive-SPME method for separation and preconcentration of mercury(II using ionic liquid modified magnetic reduced graphene oxide (IL-MrGO nanoparticles, prior to the measurement by cold vapour atomic absorption spectrometry (CV-AAS has been developed. The IL-MrGO composite was characterized by Brunauer– Emmett–Teller method (BET for adsorption-desorption measurement, thermogravimetric analysis (TGA, powder X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS. The method is based on the sorption of mercury( II on IL-MrGO nanoparticles due to electrostatic interaction and complex formation of ionic liquid part of IL-MrGO with mercury(II. The effect of experimental parameters for preconcentration of mercury(II, such as solution type, concentration and volume of the eluent, pH, time of the sorption and desorption, amount of the sorbent and coexisting ion concentration have been optimized. Under the optimized conditions, a linear response was obtained in the concentration range of 0.08–10 ng mL-1 with a determination coefficient of 0.9995. The limit of detection (LOD of the method at a signal to noise ratio of 3 was 0.01 ng mL-1. Intra-day and inter-day precisions were obtained equal to 3.4 and 4.5 %, respectively. The dispersive solid phase micro-extraction of mercury(II on IL-MrGO nanoparticles coupled with cold vapour atomic absorption spectrometry was successfully used for extraction and determination of mercury(II in water and vegetable samples.

Microstructural characteristics of HIP-bonded monolithic nuclear fuels with a diffusion barrier

Science.gov (United States)

Jue, Jan-Fong; Keiser, Dennis D.; Breckenridge, Cynthia R.; Moore, Glenn A.; Meyer, Mitchell K.

2014-05-01

Due to the limitation of maximum uranium load achievable by dispersion fuel type, the Global Threat Reduction Initiative is developing an advanced monolithic fuel to convert US high-performance research reactors to low-enriched uranium. Hot-isostatic-press (HIP) bonding was the single process down-selected to bond monolithic U-Mo fuel meat to aluminum alloy cladding. A diffusion barrier was applied to the U-Mo fuel meat by roll-bonding process to prevent extensive interaction between fuel meat and aluminum-alloy cladding. Microstructural characterization was performed on fresh fuel plates fabricated at Idaho National Laboratory. Interfaces between the fuel meat, the cladding, and the diffusion barrier, as well as between the U-10Mo fuel meat and the Al-6061 cladding, were characterized by scanning electron microscopy. Preliminary results indicate that the interfaces contain many different phases while decomposition, second phases, and chemical banding were also observed in the fuel meat. The important attributes of the HIP-bonded monolithic fuel are: line. Some of these attributes might be critical to the irradiation performance of monolithic U-10Mo nuclear fuel. There are several issues or concerns that warrant more detailed study, such as precipitation along the cladding-to-cladding bond line, chemical banding, uncovered fuel-zone edge, and the interaction layer between the U-Mo fuel meat and zirconium. Future post-irradiation examination results will focus, among other things, on identifying in-reactor failure mechanisms and, eventually, directing further fresh fuel characterization efforts.

Imaging monolithic silicon detector telescopes

International Nuclear Information System (INIS)

Amorini, F.; Sipala, V.; Cardella, G.; Boiano, C.; Carbone, B.; Cosentino, L.; Costa, E.; Di Pietro, A.; Emanuele, U.; Fallica, G.; Figuera, P.; Finocchiaro, P.; La Guidara, E.; Marchetta, C.; Pappalardo, A.; Piazza, A.; Randazzo, N.; Rizzo, F.; Russo, G.V.; Russotto, P.

2008-01-01

We show the results of some test beams performed on a new monolithic strip silicon detector telescope developed in collaboration with the INFN and ST-microelectronics. Using an appropriate design, the induction on the ΔE stages, generated by the charge released in the E stage, was used to obtain the position of the detected particle. The position measurement, together with the low threshold for particle charge identification, allows the new detector to be used for a large variety of applications due to its sensitivity of only a few microns measured in both directions

A monolithic lipase reactor for biodiesel production by transesterification of triacylglycerides into fatty acid methyl esters

KAUST Repository

Urban, Jiří T.

2011-09-26

An enzymatic reactor with lipase immobilized on a monolithic polymer support has been prepared and used to catalyze the transesterification of triacylglycerides into the fatty acid methyl esters commonly used for biodiesel. A design of experiments procedure was used to optimize the monolithic reactor with variables including control of the surface polarity of the monolith via variations in the length of the hydrocarbon chain in alkyl methacrylate monomer, time of grafting of 1-vinyl-4,4-dimethylazlactone used to activate the monolith, and time used for the immobilization of porcine lipase. Optimal conditions involved the use of a poly(stearyl methacrylate-co-ethylene dimethacrylate) monolith, grafted first with vinylazlactone, then treated with lipase for 2h to carry out the immobilization of the enzyme. Best conditions for the transesterification of glyceryl tributyrate included a temperature of 37°C and a 10min residence time of the substrate in the bioreactor. The reactor did not lose its activity even after pumping through it a solution of substrate equaling 1,000 reactor volumes. This enzymatic reactor was also used for the transesterification of triacylglycerides from soybean oil to fatty acid methyl esters thus demonstrating the ability of the reactor to produce biodiesel. © 2011 Wiley Periodicals, Inc.

A monolithic lipase reactor for biodiesel production by transesterification of triacylglycerides into fatty acid methyl esters

KAUST Repository

Urban, Jiří T.; Švec, František; Frechet, Jean

2011-01-01

An enzymatic reactor with lipase immobilized on a monolithic polymer support has been prepared and used to catalyze the transesterification of triacylglycerides into the fatty acid methyl esters commonly used for biodiesel. A design of experiments procedure was used to optimize the monolithic reactor with variables including control of the surface polarity of the monolith via variations in the length of the hydrocarbon chain in alkyl methacrylate monomer, time of grafting of 1-vinyl-4,4-dimethylazlactone used to activate the monolith, and time used for the immobilization of porcine lipase. Optimal conditions involved the use of a poly(stearyl methacrylate-co-ethylene dimethacrylate) monolith, grafted first with vinylazlactone, then treated with lipase for 2h to carry out the immobilization of the enzyme. Best conditions for the transesterification of glyceryl tributyrate included a temperature of 37°C and a 10min residence time of the substrate in the bioreactor. The reactor did not lose its activity even after pumping through it a solution of substrate equaling 1,000 reactor volumes. This enzymatic reactor was also used for the transesterification of triacylglycerides from soybean oil to fatty acid methyl esters thus demonstrating the ability of the reactor to produce biodiesel. © 2011 Wiley Periodicals, Inc.

A monolithic lipase reactor for biodiesel production by transesterification of triacylglycerides into fatty acid methyl esters.

Science.gov (United States)

Urban, Jiri; Svec, Frantisek; Fréchet, Jean M J

2012-02-01

An enzymatic reactor with lipase immobilized on a monolithic polymer support has been prepared and used to catalyze the transesterification of triacylglycerides into the fatty acid methyl esters commonly used for biodiesel. A design of experiments procedure was used to optimize the monolithic reactor with variables including control of the surface polarity of the monolith via variations in the length of the hydrocarbon chain in alkyl methacrylate monomer, time of grafting of 1-vinyl-4,4-dimethylazlactone used to activate the monolith, and time used for the immobilization of porcine lipase. Optimal conditions involved the use of a poly(stearyl methacrylate-co-ethylene dimethacrylate) monolith, grafted first with vinylazlactone, then treated with lipase for 2 h to carry out the immobilization of the enzyme. Best conditions for the transesterification of glyceryl tributyrate included a temperature of 37°C and a 10 min residence time of the substrate in the bioreactor. The reactor did not lose its activity even after pumping through it a solution of substrate equaling 1,000 reactor volumes. This enzymatic reactor was also used for the transesterification of triacylglycerides from soybean oil to fatty acid methyl esters thus demonstrating the ability of the reactor to produce biodiesel. Copyright © 2011 Wiley Periodicals, Inc.

Effect of accelerated aging on translucency of monolithic zirconia

Directory of Open Access Journals (Sweden)

O. Abdelbary

2016-12-01

Conclusion: Thickness of zirconia has significant effect on translucency. Aging has significant effect on thinner sections of zirconia. More research is required on zirconia towards making the material more translucent for its potential use as esthetic monolithic restoration.

Improved Optics in Monolithic Perovskite/Silicon Tandem Solar Cells with a Nanocrystalline Silicon Recombination Junction

KAUST Repository

Sahli, Florent

2017-10-09

Perovskite/silicon tandem solar cells are increasingly recognized as promi­sing candidates for next-generation photovoltaics with performance beyond the single-junction limit at potentially low production costs. Current designs for monolithic tandems rely on transparent conductive oxides as an intermediate recombination layer, which lead to optical losses and reduced shunt resistance. An improved recombination junction based on nanocrystalline silicon layers to mitigate these losses is demonstrated. When employed in monolithic perovskite/silicon heterojunction tandem cells with a planar front side, this junction is found to increase the bottom cell photocurrent by more than 1 mA cm−2. In combination with a cesium-based perovskite top cell, this leads to tandem cell power-conversion efficiencies of up to 22.7% obtained from J–V measurements and steady-state efficiencies of up to 22.0% during maximum power point tracking. Thanks to its low lateral conductivity, the nanocrystalline silicon recombination junction enables upscaling of monolithic perovskite/silicon heterojunction tandem cells, resulting in a 12.96 cm2 monolithic tandem cell with a steady-state efficiency of 18%.

Analysis of Catalytic Material Effect on the Photovoltaic Properties of Monolithic Dye-sensitized Solar Cells

Directory of Open Access Journals (Sweden)

Natalita Maulani Nursam

2017-12-01

Full Text Available Dye-sensitized solar cells (DSSC are widely developed due to their attractive appearance and simple fabrication processes. One of the challenges that arise in the DSSC fabrication involves high material cost associated with the cost of conductive substrate. DSSC with monolithic configuration was then developed on the basis of this motivation. In this contribution, titanium dioxide-based monolithic type DSSCs were fabricated on a single fluorine-doped transparent oxide coated glass using porous ZrO2 as spacer. Herein, the catalytic material for the counter-electrode was varied using carbon composite and platinum in order to analyze their effect on the solar cell efficiency. Four-point probe measurement revealed that the carbon composite exhibited slightly higher conductivity with a sheet resistance of 9.8 Ω/sq and 10.9 Ω/sq for carbon and platinum, respectively. Likewise, the photoconversion efficiency of the monolithic cells with carbon counter-electrode almost doubled the efficiency of the cells with platinum counter-electrode. Our results demonstrate that carbon could outperform the performance of platinum as catalytic material in monolithic DSSC.

Improved Optics in Monolithic Perovskite/Silicon Tandem Solar Cells with a Nanocrystalline Silicon Recombination Junction

KAUST Repository

Sahli, Florent; Kamino, Brett A.; Werner, Jé ré mie; Brä uninger, Matthias; Paviet-Salomon, Bertrand; Barraud, Loris; Monnard, Raphaë l; Seif, Johannes Peter; Tomasi, Andrea; Jeangros, Quentin; Hessler-Wyser, Aï cha; De Wolf, Stefaan; Despeisse, Matthieu; Nicolay, Sylvain; Niesen, Bjoern; Ballif, Christophe

2017-01-01

Perovskite/silicon tandem solar cells are increasingly recognized as promi­sing candidates for next-generation photovoltaics with performance beyond the single-junction limit at potentially low production costs. Current designs for monolithic tandems rely on transparent conductive oxides as an intermediate recombination layer, which lead to optical losses and reduced shunt resistance. An improved recombination junction based on nanocrystalline silicon layers to mitigate these losses is demonstrated. When employed in monolithic perovskite/silicon heterojunction tandem cells with a planar front side, this junction is found to increase the bottom cell photocurrent by more than 1 mA cm−2. In combination with a cesium-based perovskite top cell, this leads to tandem cell power-conversion efficiencies of up to 22.7% obtained from J–V measurements and steady-state efficiencies of up to 22.0% during maximum power point tracking. Thanks to its low lateral conductivity, the nanocrystalline silicon recombination junction enables upscaling of monolithic perovskite/silicon heterojunction tandem cells, resulting in a 12.96 cm2 monolithic tandem cell with a steady-state efficiency of 18%.

Application of novel activated carbon fiber solid-phase, microextraction to the analysis of chlorinated hydrocarbons in water by gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Sun Tonghua; Jia Jinping; Fang Nenghu; Wang Yalin

2005-01-01

This paper presents a study on the performance of activated carbon fiber (ACF) used as extraction fiber for solid-phase microextraction (SPME) and its application for analysis of chlorinated hydrocarbons in water. By means of evaluating scanning electron microscope (SEM) images, specific surface area, pore volume, pore distribution, and properties of adsorption and desorption, the optimal active concentration of phosphoric acid has been determined. Coupled with gas chromatograph-mass spectrometry (GC-MS), ACF-SPME is suitable for determination chlorinated hydrocarbons in water with headspace. Experimental parameters such as adsorption and desorption conditions were studied. The optimized method has an acceptable linearity, good precision, with R.S.D. values <10% for each compound. Compared with commercial fibers, ACF has many advantages such as better resistance to organic solvents, better endurance to high temperature and longer lifetime

Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

Science.gov (United States)

Lima Gomes, Paulo C F; Barnes, Brian B; Santos-Neto, Álvaro J; Lancas, Fernando M; Snow, Nicholas H

2013-07-19

Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.6 to 1200μgL(-1) and limits of detection and quantitation from 0.02 to 100μgL(-1). A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC-ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants. Copyright © 2013 Elsevier B.V. All rights reserved.

Mathematical Modelling of Optimization of Structures of Monolithic Coverings Based on Liquid Rubbers

Science.gov (United States)

Turgumbayeva, R. Kh; Abdikarimov, M. N.; Mussabekov, R.; Sartayev, D. T.

2018-05-01

The paper considers optimization of monolithic coatings compositions using a computer and MPE methods. The goal of the paper was to construct a mathematical model of the complete factorial experiment taking into account its plan and conditions. Several regression equations were received. Dependence between content components and parameters of rubber, as well as the quantity of a rubber crumb, was considered. An optimal composition for manufacturing the material of monolithic coatings compositions was recommended based on experimental data.

Novel design of low-jitter 10 GHz all-active monolithic mode-locked lasers

DEFF Research Database (Denmark)

Larsson, David; Yvind, Kresten; Christiansen, Lotte Jin

2004-01-01

Using a novel design, we have fabricated 10 GHz all-active monolithic mode-locked semiconductor lasers that generate 1.4 ps pulses with record-low timing jitter. The dynamical properties of lasers with 1 and 2 QWs are compared.......Using a novel design, we have fabricated 10 GHz all-active monolithic mode-locked semiconductor lasers that generate 1.4 ps pulses with record-low timing jitter. The dynamical properties of lasers with 1 and 2 QWs are compared....

Regional waste treatment with monolith disposal for low-level radioactive waste

International Nuclear Information System (INIS)

Forsberg, C.W.

1983-01-01

An alternative system is proposed for the disposal of low-level radioactive waste. This system, called REgional Treatment with MOnolith Disposal (RETMOD), is based on integrating three commercial technologies: automated package warehousing, whole-barrel rotary kiln incineration, and cement-based grouts for radioactive waste disposal. In the simplified flowsheet, all the sludges, liquids, resins, and combustible wastes are transported to regional facilities where they are incinerated. The ash is then mixed with special cement-based grouts, and the resulting mixture is poured into trenches to form large waste-cement monoliths. Wastes that do not require treatment, such as damaged and discarded equipment, are prepositioned in the trenches with the waste-cement mixture poured on top. The RETMOD system may provide higher safety margins by conversion of wastes into a solidified low-leach form, creation of low-surface area waste-cement monoliths, and centralization of waste processing into a few specialized facilities. Institutional problems would be simplified by placing total responsibility for safe disposal on the disposal site operator. Lower costs may be realized through reduced handling costs, the economics of scale, simplified operations, and less restrictive waste packaging requirements

Development of a bi-functional silica monolith for electro-osmotic pumping and DNA clean-up/extraction using gel-supported reagents in a microfluidic device.

Science.gov (United States)

Oakley, Jennifer A; Shaw, Kirsty J; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J

2009-06-07

A silica monolith used to support both electro-osmotic pumping (EOP) and the extraction/elution of DNA coupled with gel-supported reagents is described. The benefits of the combined EOP extraction/elution system were illustrated by combining DNA extraction and gene amplification using the polymerase chain reaction (PCR) process. All the reagents necessary for both processes were supported within pre-loaded gels that allow the reagents to be stored at 4 degrees C for up to four weeks in the microfluidic device. When carrying out an analysis the crude sample only needed to be hydrodynamically introduced into the device which was connected to an external computer controlled power supply via platinum wire electrodes. DNA was extracted with 65% efficiency after loading lysed cells onto a silica monolith. Ethanol contained within an agarose gel matrix was then used to wash unwanted debris away from the sample by EOP (100 V cm(-1) for 5 min). The retained DNA was subsequently eluted from the monolith by water contained in a second agarose gel, again by EOP using an electric field of 100 V cm(-1) for 5 min, and transferred into the PCR reagent containing gel. The eluted DNA in solution was successfully amplified by PCR, confirming that the concept of a complete self-contained microfluidic device could be realised for DNA sample clean up and amplification, using a simple pumping and on-chip reagent storage methodology.

A hybrid monolithic column based on boronate-functionalized graphene oxide nanosheets for online specific enrichment of glycoproteins.

Science.gov (United States)

Zhou, Chanyuan; Chen, Xiaoman; Du, Zhuo; Li, Gongke; Xiao, Xiaohua; Cai, Zongwei

2017-05-19

A hybrid monolithic column based on aminophenylboronic acid (APBA)-functionalized graphene oxide (GO) has been developed and used for selective enrichment of glycoproteins. The APBA/GO composites were homogeneously incorporated into a polymer monolithic column with the help of oligomer matrix and followed by in situ polymerization. The effect of dispersion of APBA/GO composites in the polymerization mixture on the performance of the monolithic column was explored in detail. The presence of graphene oxide not only enlarged the BET surface area from 6.3m 2 /g to 169.4m 2 /g, but also provided abundant boronic acid moieties for glycoprotein extraction, which improved the enrichment selectivity and efficiency for glycoproteins. The APBA/GO hybrid monolithic column was incorporated into a sequential injection system, which facilitated online extraction of proteins. Combining the superior properties of extraordinary surface area of GO and the affinity interaction of APBA to glycoproteins, the APBA/GO hybrid monolithic column showed higher enrichment factors for glycoproteins than other proteins without cis-diol-containing groups. Also, under comparable or even shorter processing time and without the addition of any organic solvent, it showed higher binding capacity toward glycoproteins compared with the conventional boronate affinity monolithic column. The practical applicability of this system was demonstrated by processing of egg white samples for extraction of ovalbumin and ovotransferrin, and satisfactory results were obtained by assay with SDS-PAGE. Copyright © 2017 Elsevier B.V. All rights reserved.

Sub-millimetre DOI detector based on monolithic LYSO and digital SiPM for a dedicated small-animal PET system

International Nuclear Information System (INIS)

Marcinkowski, Radosław; Mollet, Pieter; Van Holen, Roel; Vandenberghe, Stefaan

2016-01-01

The mouse model is widely used in a vast range of biomedical and preclinical studies. Thanks to the ability to detect and quantify biological processes at the molecular level in vivo, PET has become a well-established tool in these investigations. However, the need to visualize and quantify radiopharmaceuticals in anatomic structures of millimetre or less requires good spatial resolution and sensitivity from small-animal PET imaging systems. In previous work we have presented a proof-of-concept of a dedicated high-resolution small-animal PET scanner based on thin monolithic scintillator crystals and Digital Photon Counter photosensor. The combination of thin monolithic crystals and MLE positioning algorithm resulted in an excellent spatial resolution of 0.7 mm uniform in the entire field of view (FOV). However, the limitation of the scanner was its low sensitivity due to small thickness of the lutetium-yttrium oxyorthosilicate (LYSO) crystals (2 mm). Here we present an improved detector design for a small-animal PET system that simultaneously achieves higher sensitivity and sustains a sub-millimetre spatial resolution. The proposed detector consists of a 5 mm thick monolithic LYSO crystal optically coupled to a Digital Photon Counter. Mean nearest neighbour (MNN) positioning combined with depth of interaction (DOI) decoding was employed to achieve sub-millimetre spatial resolution. To evaluate detector performance the intrinsic spatial resolution, energy resolution and coincidence resolving time (CRT) were measured. The average intrinsic spatial resolution of the detector was 0.60 mm full-width-at-half-maximum (FWHM). A DOI resolution of 1.66 mm was achieved. The energy resolution was 23% FWHM at 511 keV and CRT of 529 ps were measured. The improved detector design overcomes the sensitivity limitation of the previous design by increasing the nominal sensitivity of the detector block and retains an excellent intrinsic spatial resolution. (paper)

The synthesis of weak acidic type hybrid monolith via thiol-ene click chemistry and its application in hydrophilic interaction chromatography.

Science.gov (United States)

Zeng, Jiao; Liu, Shengquan; Wang, Menglin; Yao, Shouzhuo; Chen, Yingzhuang

2017-05-01

In this work, a porous structure and good permeability monolithic column was polymerized in UV transparent fused-silica capillaries via photo-initiated thiol-ene click polymerization of 2,4,6,8-tetravinyl-2,4,6,8-tetramethylcyclotetrasiloxane (TMTVS), pentaerythritol tetra(3-mercaptopropionate)(PETMP), itaconic acid, respectively, in the presence of porogenic solvents (tetrahydrofuranand methanol) and an initiator (2,2-dimethoxy-2-phenylacetophenone) (DMPA) within 30 min. The physical properties of this monolith were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and nitrogen adsorption/desorption measurements. For an overall evaluation of the monolith in chromatographic application, separations of polycyclic aromatic hydrocarbons (PAHs), phenols, amides and bases were carried out. The column efficiency of this monolith could be as high as 112 560 N/m. It also possesses a potential application in fabrication of monoliths with high efficiency for c-LC. In addition, the resulting monolithic column demonstrated the potential use in analysis of environment waters. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of trace bisphenol A in environmental water by high-performance liquid chromatography using magnetic reduced graphene oxide based solid-phase extraction coupled with dispersive liquid-liquid microextraction.

Science.gov (United States)

Li, Danping; Ma, Xiaoguo; Wang, Rui; Yu, Yumian

2017-02-01

Bisphenol A (BPA), an endocrine-disrupting chemical, has received much attention from researchers and the general public. In this paper, a novel method of determining BPA at trace levels was developed, using magnetic reduced graphene oxide (rGO-Fe 3 O 4 )-based solid-phase extraction coupled with dispersive liquid-liquid microextraction (DLLME), followed by high-performance liquid chromatographic determination. The rGO-Fe 3 O 4 was prepared and then characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, and vibrating sample magnetometry. The greatest saturation magnetization of rGO-Fe 3 O 4 was up to 43.8 emu g -1 , which allowed rapid isolation of the rGO-Fe 3 O 4 from solutions upon applying an appropriate magnetic field. The effects of solution pH, adsorbent amount, type and volume of eluent and extraction solvent, extraction time, and salt concentration on the extraction efficiency of BPA were examined and optimized. Under the optimum conditions, an enrichment factor of 5217 and an LOD of 0.01 μg L -1 for BPA were obtained. The reusability of rGO-Fe 3 O 4 for at least 12 repeated cycles without any significant decrease in the extraction recovery of BPA was demonstrated. The proposed method was applied to the determination of BPA in different real water samples, with relative recoveries of 84.8-104.9 % and RSDs of 0.8-8.3 % in the spiked concentration range 1-10 μg L -1 .

Optimization of two different dispersive liquid-liquid microextraction methods followed by gas chromatography-mass spectrometry determination for polycyclic aromatic hydrocarbons (PAHs) analysis in water.

Science.gov (United States)

Tseng, Wan-Chi; Chen, Pai-Shan; Huang, Shang-Da

2014-03-01

Novel sample preparation methods termed "up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME)" and "water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction (WLSEME)" coupled with gas chromatography-mass spectrometry (GC-MS) have been developed for the analysis of 11 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. For UDSA-DLLME, an up-and-down shaker-assisted emulsification was employed. Extraction was complete in 3min. Only 14 μL of 1-heptanol was required, without a dispersive solvent. Under the optimum conditions, the linear range was 0.08-100 µg L(-1), and the LODs were in the range 0.022-0.060 µg L(-1). The enrichment factors (EFs) ranged from 392 to 766. Relative recoveries were between 84% and 113% for river, lake, and field water. In WLSEME, 9 μL of 1-nonanol as extraction solvent and 240 μL of 1 mg L(-1) Triton X-100 as surfactant were mixed in a microsyringe to form a cloudy emulsified solution, which was then injected into the samples. Compared with other surfactant-assisted emulsion methods, WLSEME uses much less surfactant. The linear range was 0.08-100 µg L(-1), and the LODs were 0.022-0.13 µg L(-1). The EFs ranged from 388 to 649. The relative recoveries were 86-114% for all three water specimens. Copyright © 2013 Elsevier B.V. All rights reserved.

Catalytic Oxidation of Cyanogen Chloride over a Monolithic Oxidation Catalyst

National Research Council Canada - National Science Library

Campbell, Jeffrey

1997-01-01

The catalytic oxidation of cyanogen chloride was evaluated over a monolithic oxidation catalyst at temperatures between 200 and 300 deg C in air employing feed concentrations between 100 and 10,000 ppm...

Fundamental properties of monolithic bentonite buffer material formed by cold isostatic pressing for high-level radioactive waste repository

International Nuclear Information System (INIS)

Kawakami, S.; Yamanaka, Y.; Kato, K.; Asano, H.; Ueda, H.

1999-01-01

The methods of fabrication, handling, and emplacement of engineered barriers used in a deep geological repository for high level radioactive waste should be planned as simply as possible from the engineering and economic viewpoints. Therefore, a new concept of a monolithic buffer material around a waste package have been proposed instead of the conventional concept with the use of small blocks, which would decrease the cost for buffer material. The monolithic buffer material is composed of two parts of highly compacted bentonite, a cup type body and a cover. As the forming method of the monolithic buffer material, compaction by the cold isostatic pressing process (CIP) has been employed. In this study, monolithic bentonite bodies with the diameter of about 333 mm and the height of about 455 mm (corresponding to the approx. 1/5 scale for the Japanese reference concept) were made by the CIP of bentonite powder. The dry densities: ρd of the bodies as a whole were measured and the small samples were cut from several locations to investigate the density distribution. The swelling pressure and hydraulic conductivity as function of the monolithic body density for CIP-formed specimens were also measured. High density (ρd: 1.4--2.0 Mg/m 3 ) and homogeneous monolithic bodies were formed by the CIP. The measured results of the swelling pressure (3--15 MPa) and hydraulic conductivity (0.5--1.4 x 10 -13 m/s) of the specimens were almost the same as those for the uniaxial compacted bentonite in the literature. It is shown that the vacuum hoist system is an applicable handling method for emplacement of the monolithic bentonite

Specially Treated Aramid Fiber Stabilized Gel-Emulsions: Preparation of Porous Polymeric Monoliths and Highly Efficient Removing of Airborne HCHO.

Science.gov (United States)

Liu, Jianfei; Chen, Xiangli; Wang, Pei; Fu, Xuwei; Liu, Kaiqiang; Fang, Yu

2017-08-01

Porous polymeric monoliths with densities as low as ≈0.060 g cm -3 are prepared in a gel-emulsion template way, of which the stabilizer employed is a newly discovered acidified aramid fiber that is so efficient that 0.05% (w/v, accounts for continuous phase) is enough to gel the system. The porous monoliths as obtained can be dried at ambient conditions, avoiding energy-consuming processes. Importantly, the monoliths show selective adsorption to HCHO, and the corresponding adsorption capacity (M6) is ≈2700 mg g -1 , the best result that is reported until now. More importantly, the monoliths can be reused after drying. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A star-shaped polythiophene dendrimer coating for solid-phase microextraction of triazole agrochemicals.

Science.gov (United States)

Abolghasemi, Mir Mahdi; Habibiyan, Rahim; Jaymand, Mehdi; Piryaei, Marzieh

2018-02-14

A nanostructured star-shaped polythiophene dendrimer was prepared and used as a fiber coating for headspace solid phase microextraction of selected triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole) from water samples. The dendrimer with its large surface area was characterized by thermogravimetric analysis, UV-Vis spectroscopy and field emission scanning electron microscopy. It was placed on a stainless steel wire for use in SPME. The experimental conditions for fiber coating, extraction, stirring rate, ionic strength, pH value, desorption temperature and time were optimized. Following thermal desorption, the pesticides were quantified by GC-MS. Under optimum conditions, the repeatability (RSD) for one fiber (for n = 3) ranges from 4.3 to 5.6%. The detection limits are between 8 and 12 pg mL -1 . The method is fast, inexpensive (in terms of equipment), and the fiber has high thermal stability. Graphical abstract Schematic presentation of a nanostructured star-shaped polythiophene dendrimer for use in headspace solid phase microextraction of the triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole). They were then quantified by gas chromatography-mass spectrometry.

Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages.

Science.gov (United States)

Ruiz-Delgado, Ana; Arrebola-Liébanas, Francisco Javier; Romero-González, Roberto; López-Ruiz, Rosalía; Garrido Frenich, Antonia

2016-10-01

A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO 2 on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R 2  > 0.98) within the tested range (1-50 ng l -1 ). Recoveries were evaluated at three different levels (1, 5 and 50 ng l -1 ) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l -1 , which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l -1 .

Influence of the preparation design and artificial aging on the fracture resistance of monolithic zirconia crowns.

Science.gov (United States)

Mitov, Gergo; Anastassova-Yoshida, Yana; Nothdurft, Frank Phillip; von See, Constantin; Pospiech, Peter

2016-02-01

The aim of this study was to evaluate the fracture resistance and fracture behavior of monolithic zirconia crowns in accordance with the preparation design and aging simulation method. An upper first molar was prepared sequentially with three different preparation designs: shoulderless preparation, 0.4 mm chamfer and 0.8 mm chamfer preparation. For each preparation design, 30 monolithic zirconia crowns were fabricated. After cementation on Cr-Co alloy dies, the following artificial aging procedures were performed: (1) thermal cycling and mechanical loading (TCML): 5000 cycles of thermal cycling 5℃-55℃ and chewing simulation (1,200,000 cycles, 50 N); (2) Low Temperature Degradation simulation (LTD): autoclave treatment at 137℃, 2 bar for 3 hours and chewing simulation; and (3) no pre-treatment (control group). After artificial aging, the crowns were loaded until fracture. The mean values of fracture resistance varied between 3414 N (LTD; 0.8 mm chamfer preparation) and 5712 N (control group; shoulderless preparation). Two-way ANOVA analysis showed a significantly higher fracture loads for the shoulderless preparation, whereas no difference was found between the chamfer preparations. In contrast to TCML, after LTD simulation the fracture strength of monolithic zirconia crowns decreased significantly. The monolithic crowns tested in this study showed generally high fracture load values. Preparation design and LTD simulation had a significant influence on the fracture strength of monolithic zirconia crowns.

Determination of phthalate esters in distillates by ultrasound-vortex-assisted dispersive liquid-liquid micro-extraction (USVADLLME) coupled with gas chromatography/mass spectrometry.

Science.gov (United States)

Montevecchi, Giuseppe; Masino, Francesca; Zanasi, Luca; Antonelli, Andrea

2017-04-15

A method for the extraction of phthalate esters (PAEs) by Ultrasound-Vortex-Assisted Dispersive Liquid-Liquid Micro-Extraction (USVADLLME) approach was optimised and applied for the first time to a historical series of brandies. These contaminants are widely spread in the environment as a consequence of about half century of use in different fields of applications. The concern about these substances and the recent legal restrictions of China in distillates import need a quick and sensitive method for their quantification. The proposed method, moreover, is environmentally oriented due to the disposal of micro-quantities of solvent required. In fact, sub-ppm-limits of detection were achieved with a solvent volume as low as 160μL. The analysed samples were within the legal limits, except for some very ancient brandies whose contamination was probably due to a PAEs concentration effect as a consequence of long ageing and for the use of plastic pipelines no more operative. Copyright © 2016 Elsevier Ltd. All rights reserved.

Incorporation of metal-organic framework HKUST-1 into porous polymer monolithic capillary columns to enhance the chromatographic separation of small molecules.

Science.gov (United States)

Yang, Shengchao; Ye, Fanggui; Lv, Qinghui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

2014-09-19

Metal-organic framework (MOF) HKUST-1 nanoparticles have been incorporated into poly(glycidyl methacrylate-co-ethylene dimethacrylate) (HKUST-1-poly(GMA-co-EDMA)) monoliths to afford stationary phases with enhanced chromatographic performance of small molecules in the reversed phase capillary liquid chromatography. The effect of HKUST-1 nanoparticles in the polymerization mixture on the performance of the monolithic column was explored in detail. While the bare poly(GMA-co-EDMA) monolith exhibited poor resolution (RsHKUST-1 nanoparticles to the polymerization mixture provide high increased resolution (Rs≥1.3) and high efficiency ranged from 16,300 to 44,300plates/m. Chromatographic performance of HKUST-1-poly(GMA-co-EDMA) monolith was demonstrated by separation of various analytes including polycyclic aromatic hydrocarbons, ethylbenzene and styrene, phenols and aromatic acids using a binary polar mobile phase (CH3CN/H2O). The HKUST-1-poly(GMA-co-EDMA) monolith displayed enhanced hydrophobic and π-π interaction characteristics in the reversed phase separation of test analytes compared to the bare poly(GMA-co-EDMA) monolith. The experiment results showed that HKUST-1-poly(GMA-co-EDMA) monoliths are an alternative to enhance the chromatographic separation of small molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

Monolithic stabilized Yb-fiber All-PM laser directly delivering nJ-level femtosecond pulses

DEFF Research Database (Denmark)

Turchinovich, Dmitry; Liu, Xiaomin; Lægsgaard, Jesper

2008-01-01

We present a monolithic, self-starting, all-PM, stabilized Yb-fiber laser, pulse-compressed in a hollow-core PM photonic crystal fiber, providing the 370 fs pulses of 4 nJ energy with high mode quality.......We present a monolithic, self-starting, all-PM, stabilized Yb-fiber laser, pulse-compressed in a hollow-core PM photonic crystal fiber, providing the 370 fs pulses of 4 nJ energy with high mode quality....

Development and applications of femtosecond monolithic Yb-doped fiber chirped-pulse amplifiers

International Nuclear Information System (INIS)

Zhu, L.

2011-01-01

In the past few years, compact and environmentally stable high-energy ultrashort pulse laser sources have been broadly utilized in many different applications. Fiber lasers offer big practical advantages over bulk solid-state laser systems in terms of flexibility, compactness, reliability, cost effectiveness and turn-key operability. Moreover, thermal effects are dramatically reduced due to the large surface-to-volume ratio of an optical fiber, and good spatial mode quality can be ensured by its waveguiding property. Therefore, a fiber-based laser system is considered to be the preferred laser architecture. The main theme of this thesis is the development of various femtosecond monolithic Yb-doped fiber chirped-pulse-amplification (FCPA) system and their applications. We demonstrate an ultrafast high-energy monolithic Yb-doped FCPA system in which the pulse fidelity is preserved by weakening the nonlinear effects via a substantial level of temporal stretching of the seed pulses and by using highly doped active fibers as amplifying media. The presented monolithic FCPA delivers up to ∼ 25 μJ diffraction-limited pulses that can be recompressed to sub-200 fs duration, and the pulse quality has been confirmed through the second-harmonic-generation (SHG) conversion efficiency of over 52%. Improved dispersion and nonlinearity management schemes of the FCPA system allowing substantial pulse energy scaling in the monolithic format as well as methods for overcoming a series of technological challenges are reported. Three different types of Yb-doped fiber oscillators have been developed and built in the course of this PhD work. First, we compare two oscillator types that are based on the all-normal-dispersion (ANDi) regime and the dispersion-managed (DM) regime. Both of them have been tested as the seed-pulse source of the monolithic Yb-doped FCPA system. Then we introduce another novel design based on higher-order-mode (HOM) dispersion management that competes with a

A monolithic silicon detector telescope

International Nuclear Information System (INIS)

Cardella, G.; Amorini, F.; Cabibbo, M.; Di Pietro, A.; Fallica, G.; Franzo, G.; Figuera, P.; Papa, M.; Pappalardo, G.; Percolla, G.; Priolo, F.; Privitera, V.; Rizzo, F.; Tudisco, S.

1996-01-01

An ultrathin silicon detector (1 μm) thick implanted on a standard 400 μm Si-detector has been built to realize a monolithic telescope detector for simultaneous charge and energy determination of charged particles. The performances of the telescope have been tested using standard alpha sources and fragments emitted in nuclear reactions with different projectile-target colliding systems. An excellent charge resolution has been obtained for low energy (less than 5 MeV) light nuclei. A multi-array lay-out of such detectors is under construction to charge identify the particles emitted in reactions induced by low energy radioactive beams. (orig.)

Probing the Effects of Templating on the UV and Visible Light Photocatalytic Activity of Porous Nitrogen-Modified Titania Monoliths for Dye Removal.

Science.gov (United States)

Nursam, Natalita M; Wang, Xingdong; Tan, Jeannie Z Y; Caruso, Rachel A

2016-07-13

Porous nitrogen-modified titania (N-titania) monoliths with tailored morphologies were prepared using phase separation and agarose gel templating techniques. The doping and templating process were simultaneously carried out in a one-pot step using alcohol amine-assisted sol-gel chemistry. The amount of polymer used in the monoliths that were prepared using phase separation was shown to affect both the physical and optical properties: higher poly(ethylene glycol) content increased the specific surface area, porosity, and visible light absorption of the final materials. For the agarose-templated monoliths, the infiltration conditions affected the monolith morphology. A porous monolith with high surface area and the least shrinkage was obtained when the N containing alkoxide precursor was infiltrated into the agarose scaffolds at 60 °C. The effect of the diverse porous morphologies on the photocatalytic activity of N-titania was studied for the decomposition of methylene blue (MB) under visible and UV light irradiation. The highest visible light activity was achieved by the agarose-templated N-titania monolith, in part due to higher N incorporation. This sample also showed better UV activity, partly because of the higher specific surface area (up to 112 m(2) g(-1)) compared to the phase separation-induced monoliths (up to 103 m(2) g(-1)). Overall, agarose-templated, porous N-titania monoliths provided better features for effectively removing the MB contaminant.

Solid-phase microextraction method for the determination of hexanal in hazelnuts as an indicator of the interaction of active packaging materials with food aroma compounds.

Science.gov (United States)

Pastorelli, S; Valzacchi, S; Rodriguez, A; Simoneau, C

2006-11-01

Fatty foods are susceptible to lipid oxidation resulting in deterioration of product quality due to the generation of off-flavours. Hexanal is a good indicator of rancidity. Therefore, a method based on solid-phase microextraction (SPME) coupled to gas chromatograph with flame ionization detection was developed to determine hexanal formation in hazelnuts during storage. Optimum conditions were as follows: carboxen-polydimethylsiloxane 75 microm fibre, extraction time 10 min, equilibrium time 10 min and equilibrium temperature 60 degrees C. The effect of oxygen scavengers on the oxidation process was also evaluated by measuring hexanal formation in hazelnuts stored with/without oxygen absorber sachets. Oxygen scavengers were shown to reduce oxidation; however, analysis of the sachet revealed that other volatile compounds from the headspace were also absorbed.

10Gbps monolithic silicon FTTH transceiver for PON

Science.gov (United States)

Zhang, J.; Liow, T. Y.; Lo, G. Q.; Kwong, D. L.

2010-05-01

We propose a new passive optical network (PON) configuration and a novel silicon photonic transceiver architecture for optical network unit (ONU), eliminating the need for an internal laser source in ONU. We adopt dual fiber network configuration. The internal light source in each of the ONUs is eliminated. Instead, an extra seed laser source in the optical line termination (OLT) operates in continuous wave mode to serve the ONUs in the PON as a shared and centralized laser source. λ1 from OLT Tx and λ2 from the seed laser are combined by using a WDM combiner and connected to serve the multiple ONUs through the downstream fibers. The ONUs receive the data in λ1. Meanwhile, the ONUs encode and transmit data in λ2, which are sent back to OLT. The monolithic ONU transceiver contains a wavelength-division-multiplexing (WDM) filter component, a silicon modulator and a Ge photo-detector. The WDM in ONU selectively guides λ1 to the Ge-PD where the data in λ1 are detected and converted to electrical signals, and λ2 to the transmitter where the light is modulated by upstream data. The modulated optical signals in λ2 from ONUs are connected back to OLT through upstream fibers. The monolithic ONU transceiver chip size is only 2mm by 4mm. The crosstalk between the Tx and Rx is measured to be less than -20dB. The transceiver chip is integrated on a SFP+ transceiver board. Both Tx and Rx demonstrated data rate capabilities of up to 10Gbps. By implementing this scheme, the ONU transceiver size can be significantly reduced and the assembly processes will be greatly simplified. The results demonstrate the feasibility of mass manufacturing monolithic silicon ONU transceivers via low cost

A compact narrow-linewidth laser with a low-Q monolithic cavity

International Nuclear Information System (INIS)

Peng, Yu

2013-01-01

We demonstrate an approach to narrowing the linewidth of a diode laser to around 15×10 3 Hz with a compact setup of confocal and parallel monolithic Fabry–Perot cavities (MFCs). Resonances of the confocal and parallel MFCs with low finesse are obtained. Diode lasers with optical feedback from confocal and parallel monolithic MFCs are demonstrated. The frequency could be tuned 80×10 6 Hz by changing the grating position of the external cavity diode laser based on the confocal MFC, and 100×10 6 Hz by tuning the temperature of the plane MFC over 0.02 ° C for the external cavity diode laser based on the parallel MFC. (paper)

Monolithically integrated Helmholtz coils by 3-dimensional printing

Energy Technology Data Exchange (ETDEWEB)

Li, Longguang [Department of Electrical Engineering, University of Michigan–Shanghai Jiao Tong University Joint Institute, Shanghai Jiao Tong University, Shanghai 200240 (China); Abedini-Nassab, Roozbeh; Yellen, Benjamin B., E-mail: yellen@duke.edu [Department of Electrical Engineering, University of Michigan–Shanghai Jiao Tong University Joint Institute, Shanghai Jiao Tong University, Shanghai 200240 (China); Department of Mechanical Engineering and Materials Science, Duke University, P.O. Box 90300, Hudson Hall, Durham, North Carolina 27708 (United States)

2014-06-23

3D printing technology is of great interest for the monolithic fabrication of integrated systems; however, it is a challenge to introduce metallic components into 3D printed molds to enable broader device functionality. Here, we develop a technique for constructing a multi-axial Helmholtz coil by injecting a eutectic liquid metal Gallium Indium alloy (EGaIn) into helically shaped orthogonal cavities constructed in a 3D printed block. The tri-axial solenoids each carry up to 3.6 A of electrical current and produce magnetic field up to 70 G. Within the central section of the coil, the field variation is less than 1% and is in agreement with theory. The flow rates and critical pressures required to fill the 3D cavities with liquid metal also agree with theoretical predictions and provide scaling trends for filling the 3D printed parts. These monolithically integrated solenoids may find future applications in electronic cell culture platforms, atomic traps, and miniaturized chemical analysis systems based on nuclear magnetic resonance.

Monolithically integrated Helmholtz coils by 3-dimensional printing

International Nuclear Information System (INIS)

Li, Longguang; Abedini-Nassab, Roozbeh; Yellen, Benjamin B.

2014-01-01

3D printing technology is of great interest for the monolithic fabrication of integrated systems; however, it is a challenge to introduce metallic components into 3D printed molds to enable broader device functionality. Here, we develop a technique for constructing a multi-axial Helmholtz coil by injecting a eutectic liquid metal Gallium Indium alloy (EGaIn) into helically shaped orthogonal cavities constructed in a 3D printed block. The tri-axial solenoids each carry up to 3.6 A of electrical current and produce magnetic field up to 70 G. Within the central section of the coil, the field variation is less than 1% and is in agreement with theory. The flow rates and critical pressures required to fill the 3D cavities with liquid metal also agree with theoretical predictions and provide scaling trends for filling the 3D printed parts. These monolithically integrated solenoids may find future applications in electronic cell culture platforms, atomic traps, and miniaturized chemical analysis systems based on nuclear magnetic resonance.

Monolithic Yb-fiber femtosecond laser using photonic crystal fiber

DEFF Research Database (Denmark)

Liu, Xiaomin; Lægsgaard, Jesper; Turchinovich, Dmitry

2008-01-01

We demonstrate, both experimentally and theoretically, an environmentally stable monolithic all-PM modelocked femtosecond Yb-fiber laser, with laser output pulse compressed in a spliced-on low-loss hollow-core photonic crystal fiber. Our laser provides direct fiber-end delivery of 4 nJ pulses...

Monolithic dual-band HgCdTe infrared detector structure

CSIR Research Space (South Africa)

Parish, G

1997-07-01

Full Text Available A monolithic HgCdTe photoconductive device structure is presented that is suitable for dual-band optically registered infrared photodetection in the two atmospheric transmission windows of 3-5 mu m and 8-12 mu m, which correspond to the mid...

Application of fluid-structure coupling to predict the dynamic behavior of turbine components

Energy Technology Data Exchange (ETDEWEB)

Huebner, B; Seidel, U [Voith Hydro Holding GmbH and Co. KG, Alexanderstr. 11, 89522 Heidenheim (Germany); Roth, S, E-mail: bjoern.huebner@voith.co [Laboratory for Hydraulic Machines, EPFL, Avenue de Cour 33 Bis, 1007 Lausanne (Switzerland)

2010-08-15

In hydro turbine design, fluid-structure interaction (FSI) may play an important role. Examples are flow induced inertia and damping effects, vortex induced vibrations in the lock-in vicinity, or hydroelastic instabilities of flows in deforming gaps (e.g. labyrinth seals). In contrast to aeroelasticity, hydroelastic systems require strongly (iteratively) coupled or even monolithic solution procedures, since the fluid mass which is moving with the structure (added-mass effect) is much higher and changes the dynamic behavior of submerged structures considerably. Depending on the mode shape, natural frequencies of a turbine runner in water may be reduced to less than 50% of the corresponding frequencies in air, and flow induced damping effects may become one or two orders of magnitude higher than structural damping. In order to reduce modeling effort and calculation time, the solution strategy has to be adapted precisely to a given application. Hence, depending on the problem to solve, different approximations may apply. Examples are the calculation of natural frequencies and response spectra in water using an acoustic fluid formulation, the determination of flow induced damping effects by means of partitioned FSI including complex turbulent flows, and the identification of hydroelastic instabilities using monolithic coupling of non-linear structural dynamics and water flow.

Hollow fiber liquid phase microextraction combined with graphite furnace atomic absorption spectrometry for the determination of methylmercury in human hair and sludge samples

Energy Technology Data Exchange (ETDEWEB)

Jiang Hongmei [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn; Chen Beibei; Zu Wanqing [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

2008-07-15

Two methods, based on hollow fiber liquid-liquid-liquid (three phase) microextraction (HF-LLLME) and hollow fiber liquid phase (two phase) microextraction (HF-LPME), have been developed and critically compared for the determination of methylmercury content in human hair and sludge by graphite furnace atomic absorption spectrometry (GFAAS). In HF-LPME, methylmercury was extracted into the organic phase (toluene) prior to its determination by GFAAS, while inorganic mercury remained as a free species in the sample solution. In HF-LLLME, methylmercury was first extracted into the organic phase (toluene) and then into the acceptor phase (4% thiourea in 1 mol L{sup -1} HCl) prior to its determination by GFAAS, while inorganic mercury remained in the sample solution. The total mercury was determined by inductively coupled plasma-mass spectrometry (ICP-MS), and the levels of inorganic mercury in both HF-LLLME and HF-LPME were obtained by subtracting methylmercury from total mercury. The factors affecting the microextraction of methylmercury, including organic solvent, extraction time, stirring rate and ionic strength, were investigated and the optimal extraction conditions were established for both HF-LLLPME and HF-LPME. With a consumption of 3.0 mL of the sample solution, the enrichment factors were 204 and 55 for HF-LLLPME and HF-LPME, respectively. The limits of detection (LODs) for methylmercury were 0.1 {mu}g L{sup -1} and 0.4 {mu}g L{sup -1} (as Hg) with precisions (RSDs (%), c = 5 {mu}g L{sup -1} (as Hg), n = 5) of 13% and 11% for HF-LLLPME-GFAAS and HF-LPME-GFAAS, respectively. For ICP-MS determination of total mercury, a limit of detection of 39 ng L{sup -} {sup 1} was obtained. Finally, HF-LLLME-GFAAS was applied to the determination of methylmercury content in human hair and sludge, and the recoveries for the spiked samples were in the range of 99-113%. In order to validate the method, HF-LLLME-GFAAS was also applied to the analysis of a certified reference

The influence of cladding on fission gas release from irradiated U-Mo monolithic fuel

Energy Technology Data Exchange (ETDEWEB)

Burkes, Douglas E., E-mail: Douglas.Burkes@pnnl.gov; Casella, Amanda J.; Casella, Andrew M.

2017-04-01

The monolithic uranium-molybdenum (U-Mo) alloy has been proposed as a fuel design capable of converting the world's highest power research reactors from use of high enriched uranium to low enriched uranium. However, a zirconium (Zr) diffusion barrier must be used to eliminate interactions that form between the U-Mo monolith and aluminum alloy 6061 (AA6061) cladding during fabrication and are enhanced during irradiation. One aspect of fuel development and qualification is to demonstrate an appropriate understanding of the extent of fission product release from the fuel under anticipated service environments. An exothermic reaction has previously been observed between the AA6061 cladding and Zr diffusion layer. In this paper, two fuel segments with different irradiation history were subjected to specified thermal profiles under a controlled atmosphere using a thermogravimetric/differential thermal analyzer coupled with a mass spectrometer inside a hot cell. Samples from each segment were tested with cladding and without cladding to investigate the effect, if any, that the exothermic reaction has on fission gas release mechanisms. Measurements revealed there is an instantaneous effect of the cladding/Zr exothermic reaction, but not necessarily a cumulative effect above approximately 973 K (700 °C). The mechanisms responsible for fission gas release events are discussed. - Highlights: •Complementary fission gas release events are reported for U-Mo fuel with and without cladding. •Exothermic reaction between Zr diffusion layer and cladding influences fission gas release. •Mechanisms responsible for fission gas release are similar, but with varying timing and magnitude. •Behavior of samples is similar after 800 °C signaling the onset of superlattice destabilization.

Water and Solute Mass Transport in Soils Developed on glacial Drift: A Br Tracer Investigation Using Instrumented Soil Monoliths at an Agricultural Long Term Ecological Research Site (Kellogg Biological Station, Hickory Corners, Southern Michigan)

Science.gov (United States)

Jin, L.; Hamilton, S. K.; Walter, L. M.

2004-12-01

Hydrologic processes control the residence time of water in the soil column. This is of central importance in understanding mineral weathering rates in terms of reaction kinetics and solute transport. In order to better quantify the coupling between water and solute mass transport and to better define controls on carbonate and aluminosilicates weathering rates, we have conducted bromide-tracer introduction experiments at four replicate soil monoliths (4 m3 volume) instrumented and managed by the KBS-LTER. Monolith soils are developed on the pitted outwash plain of the morainic system left by the last retreat of the Wisconsin glaciation, around 12,000 years ago. Soil profiles from the monolith sections extend to 200 cm and they were sampled and characterized texturally and mineralogically. Quartz and feldspar are dominant throughout the soil profile, while carbonates and hornblende occur only in deeper soil horizons. The four replicate monoliths are instrumented with gas and soil water sampling devices (Prenart tension lysimeters) at various depths. The monoliths also have a large capacity tray at the bottom, which permits collection of water for weight and chemical determinations. A bromide tracer solution (as lithium bromide) was applied to coincide as closely as possible with a major snowmelt event (2/27/04). The saturated and unsaturated transport of bromide through the four monoliths was followed as a function of time and soil profile depth for the duration of the snowmelt as well as intermittent rain events. Because the soil was saturated at the time of bromide application, the bromide solution is expected to move rapidly through macropores, followed by slower movement into micropores. The unsaturated transport of bromide is largely controlled by the intensity and duration of the rains if it is dominated by piston flow as opposed to preferential channel flow. In general, the tracer moved through the shallow soils very quickly, which is shown by early sharp

Nanostructured polypyrrole for automated and electrochemically controlled in-tube solid-phase microextraction of cationic nitrogen compounds

International Nuclear Information System (INIS)

Asiabi, Hamid; Yamini, Yadollah; Rezaei, Fatemeh; Seidi, Shahram

2015-01-01

The authors describe an efficient method for microextraction and preconcentration of trace quantities of cationic nitrogen compounds, specifically of anilines. It relies on a combination of electrochemically controlled solid-phase microextraction and on-line in-tube solid-phase microextraction (SPME) using polypyrrole-coated capillaries. Nanostructured polypyrrole was electrically deposited on the inner surface of a stainless steel tube and used as the extraction phase. It also acts as a polypyrrole electrode that was used as a cation exchanger, and a platinum electrode that was used as the anode. The solution to be extracted is passed over the inner surface of the polypyrrole electrode, upon which cations are extracted by applying a negative potential under flow conditions. This method represents an ideal technique for SPME of protonated anilines because it is fast, easily automated, solvent-free, and inexpensive. Under optimal conditions, the limits of detection are in the 0.10–0.30 μg L -1 range. The method works in the 0.10 to 300 μg L -1 concentration range. The inter- and intra-assay precisions (RSD%; for n = 3) range from 5.1 to 7.5 % and from 4.7 to 6.0 % at the concentration levels of 2, 10 and 20 μg L -1 , respectively. The EC-in-tube SPME method was successfully applied to the analysis of methyl-, 4-chloro-, 3-chloro and 3,4-dichloroanilines in (spiked) water samples. (author)

Switchable polarity solvent for liquid phase microextraction of Cd(II) as pyrrolidinedithiocarbamate chelates from environmental samples

Energy Technology Data Exchange (ETDEWEB)

Yilmaz, Erkan, E-mail: kimyager_erkan@hotmail.com; Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr

2015-07-30

A switchable polarity solvent was synthesized from triethylamine (TEA)/water/CO{sub 2} (Dry ice) via proton transfer reaction has been used for the microextraction of cadmium(II) as pyrrolidinedithiocarbamate (APDC) chelate. Cd(II)-APDC chelate was extracted into the switchable polarity solvent drops by adding 2 mL 10 M sodium hydroxide solution. Analytical parameters affecting the complex formation and microextraction efficiency such as pH, amount of ligand, volume of switchable polarity solvent and NaOH, sample volume were optimized. The effects of foreign ions were found tolerably. Under optimum conditions, the detection limit was 0.16 μg L{sup −1} (3Sb/m, n = 7) and the relative standard deviation was 5.4% (n = 7). The method was validated by the analysis of certified reference materials (TMDA-51.3 fortified water, TMDA-53.3 fortified water and SPS-WW2 waste water, 1573a Tomato Leaves and Oriental Basma Tobacco Leaves (INCT-OBTL-5)) and addition/recovery tests. The method was successfully applied to determination of cadmium contents of water, vegetable, fruit and cigarette samples. - Highlights: • Switchable polarity solvent was synthesized from triethylamine (TEA)/water/CO{sub 2}. • The switchable polarity solvent has been used for the microextraction of cadmium(II). • The important factors were optimized. • The method was applied to determination of cadmium in real samples.

Trace analysis of three antihistamines in human urine by on-line single drop liquid-liquid-liquid microextraction coupled to sweeping micellar electrokinetic chromatography and its application to pharmacokinetic study.

Science.gov (United States)

Gao, Wenhua; Chen, Yunsheng; Chen, Gaopan; Xi, Jing; Chen, Yaowen; Yang, Jianying; Xu, Ning

2012-09-01

A rapid and efficient dual preconcentration method of on-line single drop liquid-liquid-liquid microextraction (SD-LLLME) coupled to sweeping micellar electrokinetic chromatography (MEKC) was developed for trace analysis of three antihistamines (mizolastine, chlorpheniramine and pheniramine) in human urine. Three analytes were firstly extracted from donor phase (4 mL urine sample) adjusted to alkaline condition (0.5 M NaOH). The unionized analytes were subsequently extracted into a drop of n-octanol layered over the urine sample, and then into a microdrop of acceptor phase (100 mM H(3)PO(4)) suspended from a capillary inlet. The enriched acceptor phase was on-line injected into capillary with a height difference and then analyzed directly by sweeping MEKC. Good linear relationships were obtained for all analytes in a range of 6.25 × 10(-6) to 2.5 × 10(-4)g/L with correlation coefficients (r) higher than 0.987. The proposed method achieved limits of detections (LOD) varied from 1.2 × 10(-7) to 9.5 × 10(-7)g/L based on a signal-to-noise of 3 (S/N=3) with 751- to 1372-fold increases in detection sensitivity for analytes, and it was successfully applied to the pharmacokinetic study of three antihistamines in human urine after an oral administration. The results demonstrated that this method was a promising combination for the rapid trace analysis of antihistamines in human urine with the advantages of operation simplicity, high enrichment factor and little solvent consumption. Copyright © 2012 Elsevier B.V. All rights reserved.

A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

Energy Technology Data Exchange (ETDEWEB)

Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

2008-06-15

A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

Properties of InGaAs quantum dot saturable absorbers in monolithic mode-locked lasers

DEFF Research Database (Denmark)

Thompson, M.G.; Marinelli, C.; Chu, Y.

Saturable absorbers properties are characterised in monolithic mode-locked InGaAs quantum dot lasers. We analyse the impact of weak quantum confined Stark effect, fast absorber recovery time and low absorber saturation power on the mode-locking performance.......Saturable absorbers properties are characterised in monolithic mode-locked InGaAs quantum dot lasers. We analyse the impact of weak quantum confined Stark effect, fast absorber recovery time and low absorber saturation power on the mode-locking performance....

Synthesis and Textural Characterization of Mesoporous and Meso-/Macroporous Silica Monoliths Obtained by Spinodal Decomposition

Directory of Open Access Journals (Sweden)

Anne Galarneau

2016-04-01

Full Text Available Silica monoliths featuring either mesopores or flow-through macropores and mesopores in their skeleton are prepared by combining spinodal phase separation and sol-gel condensation. The macroporous network is first generated by phase separation in acidic medium in the presence of polyethyleneoxides while mesoporosity is engineered in a second step in alkaline medium, possibly in the presence of alkylammonium cations as surfactants. The mesoporous monoliths, also referred as aerogels, are obtained in the presence of alkylpolyethylene oxides in acidic medium without the use of supercritical drying. The impact of the experimental conditions on pore architecture of the monoliths regarding the shape, the ordering, the size and the connectivity of the mesopores is comprehensively discussed based on a critical appraisal of the different models used for textural analysis.

The Health Risk Assessment of Pb and Cr leachated from fly ash monolith landfill

International Nuclear Information System (INIS)

Hung, Ming-Lung; Wu, Sheng-Yao; Chen, Yen-Chuan; Shih, Hsiu-Ching; Yu, Yue-Hwa; Ma, Hwong-wen

2009-01-01

As of 2004, nearly two hundred thousand tons of fly ash monoliths are created each year in Taiwan to confine heavy metals for reducing the leaching quantity by precipitation. However, due to abnormal monolith fracture, poorly liner quality or exceeding usage over designed landfill capacity, serious groundwater pollution of the landfills has been reported. This research focuses on Pb and Cr leaching from monolithic landfill to assess the risk of groundwater pollution in the vicinity. The methodology combines water budget simulations using HELP model with fate and risk simulations using MMSOILS model for 5 kinds of landfill structures and 2 types of leaching models, and calculates the risk distribution over 400 grids in the down gradient direction of groundwater. The results demonstrated that the worst liner quality will cause the largest risk and the most significant exposure pathway is groundwater intake, which accounted for 98% of the total risk. Comparing Pb and Cr concentrations in the groundwater with the drinking water standards, only 14.25% of the total grids are found to be under 0.05 mg/L of Pb, and over 96.5% of the total grids are in the safety range of Cr. It indicates that Pb leaching from fly ash monolithic landfills may cause serious health risks. Without consideration of the parameters uncertainty, the cancer and noncancer risk of Pb with the sanitary landfill method was 4.23E-07 and 0.63, respectively, both under acceptable levels. However, by considering the parameters uncertainty, the non-carcinogenic risk of Pb became 1.43, exceeding the acceptable level. Only under the sealed landfill method was the hazard quotient below 1. It is important to use at least the sealed landfill for fly ash monoliths containing lead to effectively reduce health risks.

Synthesis and applications of crack-free SiO2 monolith containing CdSe/ZnS quantum dots as passive lighting sources.

Science.gov (United States)

Yi, Dong Kee

2008-09-01

A reverse microemulsion technique has been used to synthesize quantum dot nanocomposites within a SiO2 surface coating. With this approach, the unique optical properties of the CdSe/ZnS quantum dots were preserved. CdSe/ZnS/SiO2 nanoparticles were homogeneously distributed in a tetramethyl orthosilicate ethanol solution and gelation process was initiated within a 10 min, and was left over night at room temperature and dried fully to achieve a solid SiO, monolith. The resulting monolith was transparent and fluorescent under ultraviolet (UV) lamp. Moreover the monolith produced was crack-free. Further studies on the photo stability of the monolith were performed using a high power UV LED device. Remarkably, quantum dots in the SiO, monolith showed better photo stability compared with those dispersed in a polymer matrix.

Reliability Analysis and Optimal Design of Monolithic Vertical Wall Breakwaters

DEFF Research Database (Denmark)

Sørensen, John Dalsgaard; Burcharth, Hans F.; Christiani, E.

1994-01-01

Reliability analysis and reliability-based design of monolithic vertical wall breakwaters are considered. Probabilistic models of the most important failure modes, sliding failure, failure of the foundation and overturning failure are described . Relevant design variables are identified...

Long-lived monolithic micro-optics for multispectral GRIN applications.

Science.gov (United States)

Lepicard, Antoine; Bondu, Flavie; Kang, Myungkoo; Sisken, Laura; Yadav, Anupama; Adamietz, Frederic; Rodriguez, Vincent; Richardson, Kathleen; Dussauze, Marc

2018-05-09

The potential for realizing robust, monolithic, near-surface refractive micro-optic elements with long-lived stability is demonstrated in visible and infrared transmitting glasses capable of use in dual band applications. Employing an enhanced understanding of glass chemistry and geometric control of mobile ion migration made possible with electrode patterning, flat, permanent, thermally-poled micro-optic structures have been produced and characterized. Sub-surface (t~5-10 µm) compositional and structural modification during the poling process results in formation of spatially-varying refractive index profiles, exhibiting induced Δn changes up to 5 × 10 -2 which remain stable for >15 months. The universality of this approach applied to monolithic vis-near infrared [NIR] oxide and NIR-midwave infrared [MIR] chalcogenide glass materials is demonstrated for the first time. Element size, shape and gradient profile variation possible through pattern design and fabrication is shown to enable a variety of design options not possible using other GRIN process methodologies.

Effects of surface treatments on the translucency, opalescence, and surface texture of dental monolithic zirconia ceramics.

Science.gov (United States)

Kim, Hee-Kyung; Kim, Sung-Hun; Lee, Jai-Bong; Ha, Seung-Ryong

2016-06-01

Surface polishing or glazing may increase the appearance of depth of monolithic zirconia restorations. The purpose of this in vitro study was to investigate the effects of surface treatments on the translucency, opalescence, and surface texture of dental monolithic zirconia ceramics. Forty-five monolithic zirconia specimens (16.3×16.4×2.0 mm) were divided into groups I to V, according to the number of colorings each received. Each group was then divided into 3 subgroups (n=3) according to the surface treatment: N=no treatment; P=polished; and G=glazed. CIElab color coordinates were obtained relative to D65 on a reflection spectrophotometer. The translucency parameter (TP) and opalescence parameter (OP) were calculated. One specimen per subgroups I and V was selected for evaluation of surface roughness (Ra) and was examined with scanning electron microscopy (SEM). Data were analyzed with 2-way ANOVA and pairwise comparisons (α=.05). Statistical powers were verified to evaluate results (α=.05). The interaction effects of surface treatments combined with the number of colorings were significant for TP, OP, and Ra (P.05), whereas glazing significantly decreased OP and Ra in most groups. SEM images demonstrated that surface treatments affected the surface texture of monolithic zirconia ceramics. Surface treatments combined with coloring strongly affect the surface texture of dental monolithic zirconia ceramics. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Chromatographic assessment of two hybrid monoliths prepared via epoxy-amine ring-opening polymerization and methacrylate-based free radical polymerization using methacrylate epoxy cyclosiloxane as functional monomer.

Science.gov (United States)

Wang, Hongwei; Ou, Junjie; Lin, Hui; Liu, Zhongshan; Huang, Guang; Dong, Jing; Zou, Hanfa

2014-11-07

Two kinds of hybrid monolithic columns were prepared by using methacrylate epoxy cyclosiloxane (epoxy-MA) as functional monomer, containing three epoxy moieties and one methacrylate group. One column was in situ fabricated by ring-opening polymerization of epoxy-MA and 1,10-diaminodecane (DAD) using a porogenic system consisting of isopropanol (IPA), H2O and ethanol at 65°C for 12h. The other was prepared by free radical polymerization of epoxy-MA and ethylene dimethacrylate (EDMA) using 1-propanol and 1,4-butanediol as the porogenic solvents at 60°C for 12h. Two hybrid monoliths were investigated on the morphology and chromatographic assessment. Although two kinds of monolithic columns were prepared with epoxy-MA, their morphologies looked rather different. It could be found that the epoxy-MA-DAD monolith possessed higher column efficiencies (25,000-34,000plates/m) for the separation of alkylbenzenes than the epoxy-MA-EDMA monolith (12,000-13,000plates/m) in reversed-phase nano-liquid chromatography (nano-LC). Depending on the remaining epoxy or methacrylate groups on the surface of two pristine monoliths, the epoxy-MA-EDMA monolith could be easily modified with 1-octadecylamine (ODA) via ring-opening reaction, while the epoxy-MA-DAD monolith could be modified with stearyl methacrylate (SMA) via free radical reaction. The chromatographic performance for the separation of alkylbenzenes on SMA-modified epoxy-MA-DAD monolith was remarkably improved (42,000-54,000 plates/m) when compared with that on pristine epoxy-MA-DAD monolith, while it was not obviously enhanced on ODA-modified epoxy-MA-EDMA monolith when compared with that on pristine epoxy-MA-EDMA monolith. The enhancement of the column efficiency of epoxy-MA-DAD monolith after modification might be ascribed to the decreased mass-transfer resistence. The two kinds of hybrid monoliths were also applied for separations of six phenols and seven basic compounds in nano-LC. Copyright © 2014 Elsevier B.V. All

Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

Science.gov (United States)

Tran, MinhPhuong; Turner, Erica B; Segro, Scott S; Fang, Li; Seyyal, Emre; Malik, Abdul

2017-11-03

A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrochemically modified carbon fiber bundles as selective sorbent for online solid-phase microextraction of sulfonamides

International Nuclear Information System (INIS)

Ling, Xu; Zhang, Wenpeng; Chen, Zilin

2016-01-01

The authors show that carbon fiber bundles electrochemically modified with the conducting polymer poly(3,4-ethylenedioxythiophene) (PEDOT) is a viable sorbent for online solid-phase microextraction (SPME) of the sulfonamides (sulfadiazine, sulfadimidine and sulfamethoxazole) prior to their determination by HPLC. The fibers were packed in a tube loop made from polyether ether ketone (PEEK) that was coupled to the HPLC system for online SPME. Preconcentration factors can reach values of up to 300, and the limit of detection (at an S/N ration of 3) can be as low as 0.05 ng⋅mL −1 . The method was applied to the analysis of the sulfonamides in spiked rat plasma with intra-day and inter-day RSDs of <3.33 and <4.57 %, and with recoveries in the range from 91.7 to 97.8 % in spiked plasma. The in-tube SPME was also applied to the determination of the 3 sulfonamides in rat plasma after oral administration (tablet powder) with high sensitivity. In addition to its efficient extraction, the PEEK tube based SPME has chemical and mechanical stability under even harsh conditions. (author)

Periodic imidazolium-bridged hybrid monolith for high-efficiency capillary liquid chromatography with enhanced selectivity.

Science.gov (United States)

Qiao, Xiaoqiang; Zhang, Niu; Han, Manman; Li, Xueyun; Qin, Xinying; Shen, Shigang

2017-03-01

A novel periodic imidazolium-bridged hybrid monolithic column was developed. With diene imidazolium ionic liquid 1-allyl-3-vinylimidazolium bromide as both cross-linker and organic functionalized reagent, a new periodic imidazolium-bridged hybrid monolithic column was facilely prepared in capillary with homogeneously distributed cationic imidazolium by a one-step free-radical polymerization with polyhedral oligomeric silsesquioxane methacryl substituted. The successful preparation of the new column was verified by Fourier transform infrared spectroscopy, scanning electron microscopy, elemental analysis, and surface area analysis. Most interestingly, the bonded amount of 1-allyl-3-vinylimidazolium bromide of the new column is three times higher than that of the conventional imidazolium-embedded hybrid monolithic column and the specific surface area of the column reached 478 m 2 /g. The new column exhibited high stability, excellent separation efficiency, and enhanced separation selectivity. The column efficiency reached 151 000 plates/m for alkylbenzenes. Furthermore, the new column was successfully used for separation of highly polar nucleosides and nucleic acid bases with pure water as mobile phase and even bovine serum albumin tryptic digest. All these results demonstrate the periodic imidazolium-bridged hybrid monolithic column is a good separation media and can be used for chromatographic separation of small molecules and complex biological samples with high efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The application of a monolithic triphenylphosphine reagent for conducting Ramirez gem-dibromoolefination reactions in flow.

Science.gov (United States)

Roper, Kimberley A; Berry, Malcolm B; Ley, Steven V

2013-01-01

The application of a monolithic form of triphenylphosphine to the Ramirez gem-dibromoolefination reaction using flow chemistry techniques is reported. A variety of gem-dibromides were synthesised in high purity and excellent yield following only removal of solvent and no further off-line purification. It is also possible to perform the Appel reaction using the same monolith and the relationship between the mechanisms of the two reactions is discussed.

Monolithically Integrated Ge-on-Si Active Photonics

Directory of Open Access Journals (Sweden)

Jifeng Liu

2014-07-01

Full Text Available Monolithically integrated, active photonic devices on Si are key components in Si-based large-scale electronic-photonic integration for future generations of high-performance, low-power computation and communication systems. Ge has become an interesting candidate for active photonic devices in Si photonics due to its pseudo-direct gap behavior and compatibility with Si complementary metal oxide semiconductor (CMOS processing. In this paper, we present a review of the recent progress in Ge-on-Si active photonics materials and devices for photon detection, modulation, and generation. We first discuss the band engineering of Ge using tensile strain, n-type doping, Sn alloying, and separate confinement of Γ vs. L electrons in quantum well (QW structures to transform the material towards a direct band gap semiconductor for enhancing optoelectronic properties. We then give a brief overview of epitaxial Ge-on-Si materials growth, followed by a summary of recent investigations towards low-temperature, direct growth of high crystallinity Ge and GeSn alloys on dielectric layers for 3D photonic integration. Finally, we review the most recent studies on waveguide-integrated Ge-on-Si photodetectors (PDs, electroabsorption modulators (EAMs, and laser diodes (LDs, and suggest possible future research directions for large-scale monolithic electronic-photonic integrated circuits on a Si platform.

Sensing dissolved sediment porewater concentrations of persistent and bioaccumulative poolutants using disposable solid-phase microextraction fibers

NARCIS (Netherlands)

Mayer, P.; Vaes, W.H.J.; Wijnker, F.; Legierse, K.C.H.M.; Kraaij, R.H.; Tolls, J.; Hermens, J.L.M.

2000-01-01

Polymer coated glass fibers were applied as disposable samplers to measure dissolved concentrations of persistent and bioaccumulative pollutants (PBPs) in sediment porewater. The method is called matrix solid-phase microextraction (matrix-SPME), because it utilizes the entire sediment matrix as a

High-temperature nanoporous ceramic monolith prepared from a polymeric bicontinuous microemulsion template.

Science.gov (United States)

Jones, Brad H; Lodge, Timothy P

2009-02-11

Nanoporous ceramic with a unique pore structure was derived from an all-hydrocarbon polymeric bicontinuous microemulsion (BmuE). The BmuE was designed to allow facile removal of one phase, resulting in a nanoporous polymer monolith with BmuE-like structure. The pores were filled with a commercially available, polymeric precursor to nonoxide, Si-based ceramics. Pyrolysis resulted in a monolith of nanoporous ceramic, stable to at least 1000 degrees C, with a BmuE-like pore structure. The pore structure is disordered and 3-D continuous. Microscopy and gas sorption measurements suggest a well-defined pore size distribution spanning roughly 60-100 nm, sizes previously unattainable through related techniques.

Dynamic speciation analysis of atrazine in aqueous latex nanoparticle dispersions using solid phase microextraction (SPME)

NARCIS (Netherlands)

Benhabib, K.; Town, R.M.; Leeuwen, van H.P.

2009-01-01

Solid phase microextraction (SPME) is applied in the dynamic speciation analysis of the pesticide atrazine in an aqueous medium containing sorbing latex nanoparticles. It is found that the overall rate of extraction of the analyte is faster than in the absence of nanoparticles and governed by the

Fabrication of an ionic-liquid-based polymer monolithic column and its application in the fractionation of proteins from complex biosamples.

Science.gov (United States)

Zhang, Doudou; Zhang, Qian; Bai, Ligai; Han, Dandan; Liu, Haiyan; Yan, Hongyuan

2018-05-01

An ionic-liquid-based polymer monolithic column was synthesized by free radical polymerization within the confines of a stainless-steel column (50 mm × 4.6 mm id). In the processes, ionic liquid and stearyl methacrylate were used as dual monomers, ethylene glycol dimethacrylate as the cross-linking agent, and polyethylene glycol 200 and isopropanol as co-porogens. Effects of the prepolymerization solution components on the properties of the resulting monoliths were studied in detail. Scanning electron microscopy, nitrogen adsorption-desorption measurements, and mercury intrusion porosimetry were used to investigate the morphology and pore size distribution of the prepared monoliths, which showed that the homemade ionic-liquid-based monolith column possessed a relatively uniform macropore structure with a total macropore specific surface area of 44.72 m 2 /g. Compared to a non-ionic-liquid-based monolith prepared under the same conditions, the ionic-liquid-based monolith exhibited excellent selectivity and high performance for separating proteins from complex biosamples, such as egg white, snailase, bovine serum albumin digest solution, human plasma, etc., indicating promising applications in the fractionation and analysis of proteins from the complex biosamples in proteomics research. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Structure and Electromagnetic Properties of Cellular Glassy Carbon Monoliths with Controlled Cell Size

Directory of Open Access Journals (Sweden)

Andrzej Szczurek

2018-05-01

Full Text Available Electromagnetic shielding is a topic of high importance for which lightweight materials are highly sought. Porous carbon materials can meet this goal, but their structure needs to be controlled as much as possible. In this work, cellular carbon monoliths of well-defined porosity and cell size were prepared by a template method, using sacrificial paraffin spheres as the porogen and resorcinol-formaldehyde (RF resin as the carbon precursor. Physicochemical studies were carried out for investigating the conversion of RF resin into carbon, and the final cellular monoliths were investigated in terms of elemental composition, total porosity, surface area, micropore volumes, and micro/macropore size distributions. Electrical and electromagnetic (EM properties were investigated in the static regime and in the Ka-band, respectively. Due to the phenolic nature of the resin, the resultant carbon was glasslike, and the special preparation protocol that was used led to cellular materials whose cell size increased with density. The materials were shown to be relevant for EM shielding, and the relationships between those properties and the density/cell size of those cellular monoliths were elucidated.

Fabrication of single-walled carbon nanohorns incorporated a monolithic column for capillary electrochromatography.

Science.gov (United States)

Zhao, Hongyan; Wang, Yizhou; Cheng, Heyong; Wang, Yuanchao

2017-08-01

Single-walled carbon nanohorns have received great interest for their unique properties and diverse potential applications. Herein, we demonstrated the feasibility of single-walled carbon nanohorns incorporated poly(styrene-divinylbenzene) monolith as the stationary phase for capillary electrochromatography, which were prepared by one-step in situ copolymerization. Single-walled carbon nanohorns were dispersed in styrene to give a stable and homogeneous suspension. The monolithic column gave effective separation for a wide range of aromatic compounds, which was based on hydrophobicity and π-π electrostatic stacking of single-walled carbon nanohorns. The precisions of migration time and peak area varied in the ranges of 1.4-1.9% for intraday trials and 1.7-3.5% for interday trials, and 3.2-6.7% for intraday trials and 4.1-7.4% for interday trials, and 3.6-7.2% for inter-column trials and 5.2-21.3% for inter-column trials, respectively, indicating the good reproducibility of single-walled carbon nanohorns embedded monolithic columns. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Lin, Shu-Ling; Wu, Yu-Ru; Lin, Tzuen-Yeuan; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

2015-04-29

Highlights: • Methacrylic acid (MAA) was used to increase hydrophilicity of polymeric monoliths. • Fast separation of phenol derivatives was achieved in 5 min using MAA-incorporated column. • Separations of aflatoxins and phenicol antibiotics were achieved using MAA-incorporated column. - Abstract: In this study, methacrylic acid (MAA) was incorporated with alkyl methacrylates to increase the hydrophilicity of the synthesized ethylene dimethacrylate-based (EDMA-based) monoliths for separating polar small molecules by capillary LC analysis. Different alkyl methacrylate–MAA ratios were investigated to prepare a series of 30% alkyl methacrylate–MAA–EDMA monoliths in fused-silica capillaries (250-μm i.d.). The porosity, permeability, and column efficiency of the synthesized MAA-incorporated monolithic columns were characterized. A mixture of phenol derivatives is employed to evaluate the applicability of using the prepared monolithic columns for separating small molecules. Fast separation of six phenol derivatives was achieved in 5 min with gradient elution using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. In addition, the effect of acetonitrile content in mobile phase on retention factor and plate height as well as the plate height-flow velocity curves were also investigated to further examine the performance of the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Moreover, the applicability of prepared polymer-based monolithic column for potential food safety applications was also demonstrated by analyzing five aflatoxins and three phenicol antibiotics using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column.

Organic monolith frits encased in polyether ether ketone tubing with improved durability for liquid chromatography.

Science.gov (United States)

Park, Sin Young; Cheong, Won Jo

2015-09-01

This study introduces a preparation method for polymer-encased monolith frits with improved durability for liquid chromatography columns. The inner surface of the polyether ether ketone tubing is pretreated with sulfuric acid in the presence of catalysts (vanadium oxide and sodium sulfate). The tubing was rinsed with water and acetone, flushed with nitrogen, and treated with glycidyl methacrylate. After washing, the monolith reaction mixture composed of lauryl methacrylate, ethylene glycol dimethacrylate, initiator, and porogenic solvent was filled in the tubing and subjected to in situ polymerization. The tubing was cut into thin slices and used as frits for microcolumns. To check their durability, the frit slices were placed in a vial and a heavy impact was applied on the vial by a vortex mixer for various periods. The frits made in the presence of catalysts were found to be more durable than those made without catalysts. Furthermore, when the monolith-incorporated tubing was used as a chromatography column, the column prepared in the presence of catalysts resulted in a better separation efficiency. The separation performance of the columns installed with the polyether ether ketone encased monolith frits was comparable to that of the columns installed with the commercial stainless-steel screen frits. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polymethacrylate-based monoliths as stationary phases for separation of biopolymers and immobilization of enzymes.

Science.gov (United States)

Martinović, Tamara; Josić, Djuro

2017-11-01

The experiences in the production and application of polymethacrylate-based monolithic supports, since their development almost thirty years ago, are presented. The main driving force for the development of new chromatographic supports was the necessity for the isolation and separation of physiologically active biopolymers and their use for therapeutic purposes. For this sake, a development of a method for fast separation, preventing denaturation and preserving their biological activity was necessary. Development of polysaccharide-based supports, followed by the introduction of polymer-based chromatographic media, is shortly described. This development was followed by the advances in monolithic media that are now used for both large- and small-scale separation of biopolymers and nanoparticles. Finally, a short overview is given about the applications of monoliths for sample displacement chromatography, resulting in isolation of physiologically active biomolecules, such as proteins, protein complexes, and nucleic acid, as well as high-throughput sample preparation for proteomic investigations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A monolithically fabricated gas chromatography separation column with an integrated high sensitivity thermal conductivity detector

International Nuclear Information System (INIS)

Kaanta, Bradley C; Zhang, Xin; Chen, Hua

2010-01-01

The monolithic integration of a high sensitivity detector with a gas chromatography (GC) separation column creates many potential advantages over the discrete components of a traditional chromatography system. In miniaturized high-speed GC systems, component interconnections can cause crucial errors and loss of fidelity during detection and analysis. A monolithically integrated device would eliminate the need to create helium-tight interconnections, which are bulky and labor intensive. Additionally, batch fabrication of integrated devices that no longer require expensive and fragile detectors can decrease the cost of micro GC systems through economies of scale. We present the design, fabrication and operation of a monolithic GC separation column and detector. Our device is able to separate nitrogen, methane and carbon dioxide within 30 s. This method of device integration could be applied to the existing wealth of column geometries and chemistries designed for specialized applications.

Partial Coefficient System for the Design of Monolithic Vertical Breakwaters Considering Sliding and Rupture Failure of the Foundation

DEFF Research Database (Denmark)

Burcharth, Hans F.; Christiani, Erik; Sørensen, John Dalsgaard

1995-01-01

The main object is to present a set of calibrated partial coefficients for monolithic vertical breakwater failure modes. A preliminary design of the monolithic breakwater will be considered, which will be designed from existing partial coefficients, documented in Eurocode 7 (1994). From this desi...

Integration trends in monolithic power ICs: Application and technology challenges

NARCIS (Netherlands)

Rose, M.; Bergveld, H.J.

2016-01-01

This paper highlights the general trend towards further monolithic integration in power applications by enabling power management and interfacing solutions in advanced CMOS nodes. The need to combine high-density digital circuits, power-management circuits, and robust interfaces in a single

Measurement of the denitrification in soil monoliths from grassland and arable soil by means of 15N techniques

International Nuclear Information System (INIS)

Lippold, H.; Foerster, I.

1980-01-01

Losses of fertilizer nitrogen by denitrification were determined in soil monoliths from two sites (loess chernozem and clay ranker). The monoliths were isolated by driving plastic pipes into the plots, and fertilized with 15 N-labelled ammonium nitrate. Emission spectrometric techniques were applied to measure the N 2 and N 2 O quantities released in the isolated atmospheric layer above the monolith. The considerable losses, especially on grassland soils (up to a maximum of 30 kg N/ha), indicate the influence of rainfalls and mean temperature at the 5 dates of sampling (end of March to mid-October). (author)

Elemental analysis by surface-enhanced Laser-Induced Breakdown Spectroscopy combined with liquid–liquid microextraction

International Nuclear Information System (INIS)

Aguirre, M.A.; Legnaioli, S.; Almodóvar, F.; Hidalgo, M.; Palleschi, V.; Canals, A.

2013-01-01

In this work, the possibility of using Laser-Induced Breakdown Spectrometry (LIBS) combined with liquid–liquid microextraction techniques is evaluated as a simple and fast method for trace elemental analysis. Two different strategies for LIBS analysis of manganese contained in microdroplets of extraction solvent (Triton X-114) are studied: (i) analysis by direct laser irradiation of microdroplets; and (ii) analysis by laser irradiation of microdroplets dried on metallic substrates (surface-enhanced LIBS — SENLIBS). Experiments were carried out using synthetic samples with different concentrations of manganese in a 10% w/w Triton X-114 matrix. The analysis by direct laser irradiation of microdroplets showed low precision, sensitivity and poor linearity across the concentration range evaluated (R 2 −1 of Mn. - Highlights: ► LIBS combined with microextraction procedures for trace analysis is proposed. ► The proposed combination depends on LIBS ability to analyze sample microvolumes. ► A surface-enhanced LIBS methodology for microdroplet analysis was evaluated. ► Results indicate this combination to be promising for trace analysis in liquids