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Sample records for hybridization sample preparation

  1. Sample preparation and in situ hybridization techniques for automated molecular cytogenetic analysis of white blood cells

    Energy Technology Data Exchange (ETDEWEB)

    Rijke, F.M. van de; Vrolijk, H.; Sloos, W. [Leiden Univ. (Netherlands)] [and others

    1996-06-01

    With the advent in situ hybridization techniques for the analysis of chromosome copy number or structure in interphase cells, the diagnostic and prognostic potential of cytogenetics has been augmented considerably. In theory, the strategies for detection of cytogenetically aberrant cells by in situ hybridization are simple and straightforward. In practice, however, they are fallible, because false classification of hybridization spot number or patterns occurs. When a decision has to be made on molecular cytogenetic normalcy or abnormalcy of a cell sample, the problem of false classification becomes particularly prominent if the fraction of aberrant cells is relatively small. In such mosaic situations, often > 200 cells have to be evaluated to reach a statistical sound figure. The manual enumeration of in situ hybridization spots in many cells in many patient samples is tedious. Assistance in the evaluation process by automation of microscope functions and image analysis techniques is, therefore, strongly indicated. Next to research and development of microscope hardware, camera technology, and image analysis, the optimization of the specimen for the (semi)automated microscopic analysis is essential, since factors such as cell density, thickness, and overlap have dramatic influences on the speed and complexity of the analysis process. Here we describe experiments that have led to a protocol for blood cell specimen that results in microscope preparations that are well suited for automated molecular cytogenetic analysis. 13 refs., 4 figs., 1 tab.

  2. An integrated hybrid system for genetic analysis combining EWOD sample preparation and magnetic detection

    Energy Technology Data Exchange (ETDEWEB)

    Brennan, Des; Dinca, Mihai; Aherne, Margaret; Galvin, Paul [Tyndall National Institute, University College, Cork, Lee Maltings, Prospect Row, Cork (Ireland); Jary, Dorothee; Peponnet, Christine [CEA-LETI, Department of Technology for Biology and Health, 17 Avenue Des Martyrs, 38054 Grenoble (France); Cardosa, Filipe; Freitas, Paolo, E-mail: des.brennan@tyndall.ie [INESC-MN, Rua Alves Redol, 9, 1000-029 Lisbon (Portugal)

    2011-08-17

    Over the last decade microelectronic technologies have delivered significant advances in devices for point of care diagnostics. Complex microfluidic systems integrate components such as valves, pumps etc. to manipulate liquids. In recent years, the drive is to combine biochemical protocols in a single system, delivering 'sample in answer out'. An Electrowetting on Dielectric (EWOD) device offers the possibility to move and manipulate 64nl volumes implementing biochemical processes, while the magnetic sensor facilitates hybridisation detection. We outline an injection molding approach where EWOD and magnetic devices are integrated into a hybrid microfluidic system with the potential to implement 'sample in answer out' biological protocols.

  3. An integrated hybrid system for genetic analysis combining EWOD sample preparation and magnetic detection

    Science.gov (United States)

    Brennan, Des; Jary, Dorothee; Peponnet, Christine; Cardosa, Filipe; Freitas, Paolo; Dinca, Mihai; Aherne, Margaret; Galvin, Paul

    2011-08-01

    Over the last decade microelectronic technologies have delivered significant advances in devices for point of care diagnostics. Complex microfluidic systems integrate components such as valves, pumps etc. to manipulate liquids. In recent years, the drive is to combine biochemical protocols in a single system, delivering "sample in answer out". An Electrowetting on Dielectric (EWOD) device offers the possibility to move and manipulate 64nl volumes implementing biochemical processes, while the magnetic sensor facilitates hybridisation detection. We outline an injection molding approach where EWOD and magnetic devices are integrated into a hybrid microfluidic system with the potential to implement "sample in answer out" biological protocols.

  4. Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coatings for sample preparation. Ι. Capillary microextraction of catecholamine neurotransmitters.

    Science.gov (United States)

    Alhendal, Abdullah; Mengis, Stephanie; Matthews, Jacob; Malik, Abdul

    2016-10-14

    Nonhydrolytic sol-gel (NHSG) route was used for the creation of novel zirconia-polypropylene oxide (ZrO2-PPO) sol-gel hybrid sorbents in the form of surface coatings for the extraction and preconcentration of catecholamine neurotransmitters and molecules structurally related to their deaminated metabolites. In comparison to other sorbents made of inorganic transition metal oxides, the presented hybrid organic-inorganic sorbents facilitated reversible sorption properties that allowed for efficient desorption of the extracted analytes by LC-MS compatible mobile phases. The presented sol-gel hybrid sorbents effectively overcame the major drawbacks of traditional silica- or polymer-based sorbents by providing superior pH stability (pH range: 0-14), and a variety of intermolecular interactions. Nonaqueous sol-gel treatment of PPO with ZrCl4 was employed for the derivatization of the terminal hydroxyl groups on PPO, providing zirconium trichloride-containing end groups characterized by enhanced sol-gel reactivity. NHSG ZrO2-PPO sorbent provided excellent microextraction performance for catecholamines, low detection limits (5.6-9.6pM), high run-to-run reproducibility (RSD 0.6-5.1%), high desorption efficiency (95.0-99.5%) and high enrichment factors (∼1480-2650) for dopamine and epinephrine, respectively, extracted from synthetic urine samples. The presented sol-gel sorbents provided effective alternative to conventional extraction media providing unique physicochemical characteristics and excellent extraction capability.

  5. Sample preparation and biopharmaceutical analysis

    OpenAIRE

    Farrelly, Gillian

    1998-01-01

    In chapter 1, an overview is given of sample preparation methods and analytical techniques in use today. Each one is discussed, and relevant examples are given. In chapter 2, the development of a method for the HPLC analysis of taurine in human plasma using acetonitrile precipitation and pre-column derivatisation with fluorescamine is presented. This procedure was found to be faster and easier to use than previous taurine assays. In chapter 3, the evaluation of novel aspirin derivativ...

  6. Microfluidic Sample Preparation for Immunoassays

    Energy Technology Data Exchange (ETDEWEB)

    Visuri, S; Benett, W; Bettencourt, K; Chang, J; Fisher, K; Hamilton, J; Krulevitch, P; Park, C; Stockton, C; Tarte, L; Wang, A; Wilson, T

    2001-08-09

    Researchers at Lawrence Livermore National Laboratory are developing means to collect and identify fluid-based biological pathogens in the forms of proteins, viruses, and bacteria. to support detection instruments, they are developing a flexible fluidic sample preparation unit. The overall goal of this Microfluidic Module is to input a fluid sample, containing background particulates and potentially target compounds, and deliver a processed sample for detection. They are developing techniques for sample purification, mixing, and filtration that would be useful to many applications including immunologic and nucleic acid assays. Many of these fluidic functions are accomplished with acoustic radiation pressure or dielectrophoresis. They are integrating these technologies into packaged systems with pumps and valves to control fluid flow through the fluidic circuit.

  7. Sample Preparation for Bioanalytical and Pharmaceutical Analysis.

    Science.gov (United States)

    Clark, Kevin D; Zhang, Cheng; Anderson, Jared L

    2016-12-06

    Biological and pharmaceutical samples represent formidable challenges in sample preparation that hold important consequences for bioanalysis and genotoxic impurity quantification. This Feature will emphasize significant advances toward the development of rapid, sensitive, and selective sample preparation methods.

  8. Preparation, Characterization and Properties of Graphene-silver Sulphide Hybrid

    Institute of Scientific and Technical Information of China (English)

    CHEN Guang-yi; WEI Zhi-yong; LIANG Ce; WANG De-jin; LIANG Ji-cai; ZHANG Wan-xi

    2012-01-01

    A facile and efficient strategy was reported for the preparation of graphene nanosheets-Ag2S hybrid by a simple hydrothermal process.First,Ag2S particles deposited on the surface of graphene oxide(GO) sheet.GO was then reduced by hydrazine hydrate to graphcne.The results of X-ray diffraction(XRD) and Fourier transform infrared(FTIR) demonstrated the efficient reduction of GO to graphene.Transmission electron microscopy(TEM) image of the sample reveals the morphology of the architecture of graphene-Ag2S hybrid.Ultraviolet-visible spectroscopy(UV-Vis) and photoluminescence(PL) measurement were further employed to study the optical properties of the obtained nanocomposite.This work can be extended to design other graphene-based hybrid nanomaterials,and the as-grown architectures may hold promise for many applications.

  9. METALLOGRAPHIC SAMPLE PREPARATION STATION-CONSTRUCTIVE CONCEPT

    Directory of Open Access Journals (Sweden)

    AVRAM Florin Timotei

    2016-11-01

    Full Text Available In this paper we propose to present the issues involved in the case of the constructive conception of a station for metallographic sample preparation. This station is destined for laboratory work. The metallographic station is composed of a robot ABB IRB1600, a metallographic microscope, a gripping device, a manipulator, a laboratory grinding and polishing machine. The robot will be used for manipulation of the sample preparation and the manipulator take the sample preparation for processing.

  10. Final Report BW Sample Collection& Preparation Device

    Energy Technology Data Exchange (ETDEWEB)

    Koopman, R P; Belgrader, P; Meyer, G; Benett, W J; Richards, J B; Hadley, D R; Stratton, P L; Milanovich, F P

    2002-01-31

    The objective of this project was to develop the technique needed to prepare a field collected sample for laboratory analysis and build a portable integrated biological detection instrument with new miniaturized and automated sample purification capabilities. The device will prepare bacterial spores, bacterial vegetative cells, and viral particles for PCR amplification.

  11. Modular microfluidic system for biological sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Rose, Klint A.; Mariella, Jr., Raymond P.; Bailey, Christopher G.; Ness, Kevin Dean

    2015-09-29

    A reconfigurable modular microfluidic system for preparation of a biological sample including a series of reconfigurable modules for automated sample preparation adapted to selectively include a) a microfluidic acoustic focusing filter module, b) a dielectrophoresis bacteria filter module, c) a dielectrophoresis virus filter module, d) an isotachophoresis nucleic acid filter module, e) a lyses module, and f) an isotachophoresis-based nucleic acid filter.

  12. Facile Preparation of Optically Tailored Hybrid Nanocomposite

    Directory of Open Access Journals (Sweden)

    Susana Fernández de Ávila

    2014-01-01

    Full Text Available Lead sulfide nanoparticles (PbS NPs have been synthesized directly in poly[2-methoxy-5-(3′,7′-dimethyloctyloxy-1,4-phenylenevinylene] (MDMO-PPV semiconducting polymer by a simple low temperature method. Hybrid solutions with different concentrations of PbS with respect to the polymer have been prepared and characterized first in solution and then as thin film nanocomposites deposited on quartz substrates by spin coating. Quenching of photoluminescence emission is observed both in solutions and thin films when the ratio of PbS NPs increases with respect to the polymer, suggesting the occurrence of Dexter energy transfer from the polymer to the PbS NPs. Optical absorption is markedly increased for hybrid solutions compared to pure polymer. In thin nanocomposite films an enhancement of absorbance is observed with increasing PbS NPs concentration, which is more pronounced below 400 nm. The reported results could lead to the development of a method for tailoring the optical response of devices based on PbS NP-polymer nanocomposite by controlling the PbS NP concentration inside the polymer matrix.

  13. Automated sample preparation for CE-SDS.

    Science.gov (United States)

    Le, M Eleanor; Vizel, Alona; Hutterer, Katariina M

    2013-05-01

    Traditionally, CE with SDS (CE-SDS) places many restrictions on sample composition. Requirements include low salt content, known initial sample concentration, and a narrow window of final sample concentration. As these restrictions require buffer exchange for many sample types, sample preparation is often tedious and yields poor sample recoveries. To improve capacity and streamline sample preparation, an automated robotic platform was developed using the PhyNexus Micro-Extractor Automated Instrument (MEA) for both the reduced and nonreduced CE-SDS assays. This automated sample preparation normalizes sample concentration, removes salts and other contaminants, and adds the required CE-SDS reagents, essentially eliminating manual steps during sample preparation. Fc-fusion proteins and monoclonal antibodies were used in this work to demonstrate benefits of this approach when compared to the manual method. With optimized conditions, this application has demonstrated decreased analyst "hands on" time and reduced total assay time. Sample recovery greater than 90% can be achieved, regardless of initial composition and concentration of analyte.

  14. Sample preparation in biological mass spectrometry

    CERN Document Server

    Ivanov, Alexander R

    2011-01-01

    The aim of this book is to provide the researcher with important sample preparation strategies in a wide variety of analyte molecules, specimens, methods, and biological applications requiring mass spectrometric analysis as a detection end-point.

  15. Molecularly imprinted polymers for bioanalytical sample preparation.

    Science.gov (United States)

    Gama, Mariana Roberto; Bottoli, Carla Beatriz Grespan

    2017-02-01

    Molecularly imprinted polymers (MIP) are stable polymers with molecular recognition abilities, provided by the presence of a template during their synthesis, and are excellent materials with high selectivity for sample preparation in bioanalytical methods. This short review discusses aspects of MIP preparation and its applications as a sorbent material in pharmaceutical and biomedical analysis. MIP in different extraction configurations, including classical solid-phase extraction, solid-phase microextraction, magnetic molecularly imprinted solid-phase extraction, microextraction by packed sorbent and solid-phase extraction in pipette tips, are used to illustrate the good performance of this type of sorbent for sample preparation procedures of complex matrices, especially prior to bioanalytical approaches.

  16. Preparation and Characterization of Organic/Inorganic Hybrid Nanofibers

    Institute of Scientific and Technical Information of China (English)

    WU Ning; WEI Qu-fu; LI Qi; XU Wen-zheng

    2006-01-01

    A new class of nanocomposites based on organic and inorganic species integrated at a nanoscale has obtained more attention these years. Organic-inorganic hybrids have both the advantages of organic materials, such as light weight, flexibility and good moldability, and inorganic materials, such as high strength, heat stability and chemical resistance. In this work, PVAc/TiO2 organicinorganic hybrid was prepared by sol-gel process. Electrospinning technique was used to fabricate PVAc/TiO2hybrid nanofibers. The structures and properties of the hybrid nanofibers were characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscope (AFM),Differential Scanning Calorimeter (DSC) and Fouriertransform infrared (FTIR) spectra. SEM and AFM were employed to study the topography of the hybrid nanofibers.The chemical structure of the hybrid nanofibers were examined by FTIR. The DSC scansrevealed the second order transition temperature of the hybrid materials were higher than PVAc.

  17. Sample preparation for SEM of plant surfaces

    OpenAIRE

    A.K. Pathan; Bond, J.; R.E. Gaskin

    2010-01-01

    Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniq...

  18. Sample preparation method for scanning force microscopy

    CERN Document Server

    Jankov, I R; Szente, R N; Carreno, M N P; Swart, J W; Landers, R

    2001-01-01

    We present a method of sample preparation for studies of ion implantation on metal surfaces. The method, employing a mechanical mask, is specially adapted for samples analysed by Scanning Force Microscopy. It was successfully tested on polycrystalline copper substrates implanted with phosphorus ions at an acceleration voltage of 39 keV. The changes of the electrical properties of the surface were measured by Kelvin Probe Force Microscopy and the surface composition was analysed by Auger Electron Spectroscopy.

  19. Preparation of PAA/AM/MMT Hybrid by Intercalation Polymerization

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    @@ Over the last few years, Montmorillonite (MMT) was widely used as a special inorganic material for preparing Polymer/MMT nanocompsites. MMT is a clay imineral consisting of stacked silicate sheets whose thickness is about 10A. Through intercalation a large number of polymer-clay nanocomposites have been prepared such as Nylon-clay hybrid [1], PS-clay hybrid [2], Poly (methyl methacrylate) (PMMA)-clay hybrid [3], etc. In this article, the synthesis and properties of Poly (acrylic acid/acrylamide)/MMT hybrid (PAAAM/MMT) were studied. X-ray diffraction and Transmission electron microscopy were used to characterize the hybrid material. DSC has been used to study its property. Results showed that the intercalating reagents have entered the space of MMT's layers and enlarged them. At the same time, the MMT dispersed homogeneously in acrylic acid and acrylamide monomers that allow MMT to disperse in PAAAM matrix in the monolayer form.

  20. Scanning Electron Microscopy Sample Preparation and Imaging.

    Science.gov (United States)

    Nguyen, Jenny Ngoc Tran; Harbison, Amanda M

    2017-01-01

    Scanning electron microscopes allow us to reach magnifications of 20-130,000× and resolve compositional and topographical images with intense detail. These images are created by bombarding a sample with electrons in a focused manner to generate a black and white image from the electrons that bounce off of the sample. The electrons are detected using positively charged detectors. Scanning electron microscopy permits three-dimensional imaging of desiccated specimens or wet cells and tissues by using variable pressure chambers. SEM ultrastructural analysis and intracellular imaging supplement light microscopy for molecular profiling of prokaryotes, plants, and mammals. This chapter demonstrates how to prepare and image samples that are (a) desiccated and conductive, (b) desiccated and nonconductive but coated with an electron conductive film using a gold sputter coater, and (c) wet and maintained in a hydrated state using a Deben Coolstage.

  1. Recent advances in sample preparation techniques for effective bioanalytical methods.

    Science.gov (United States)

    Kole, Prashant Laxman; Venkatesh, Gantala; Kotecha, Jignesh; Sheshala, Ravi

    2011-01-01

    This paper reviews the recent developments in bioanalysis sample preparation techniques and gives an update on basic principles, theory, applications and possibilities for automation, and a comparative discussion on the advantages and limitation of each technique. Conventional liquid-liquid extraction (LLE), protein precipitation (PP) and solid-phase extraction (SPE) techniques are now been considered as methods of the past. The last decade has witnessed a rapid development of novel sample preparation techniques in bioanalysis. Developments in SPE techniques such as selective sorbents and in the overall approach to SPE, such as hybrid SPE and molecularly imprinted polymer SPE, have been addressed. Considerable literature has been published in the area of solid-phase micro-extraction and its different versions, e.g. stir bar sorptive extraction, and their application in the development of selective and sensitive bioanalytical methods. Techniques such as dispersive solid-phase extraction, disposable pipette extraction and micro-extraction by packed sorbent offer a variety of extraction phases and provide unique advantages to bioanalytical methods. On-line SPE utilizing column-switching techniques is rapidly gaining acceptance in bioanalytical applications. PP sample preparation techniques such as PP filter plates/tubes offer many advantages like removal of phospholipids and proteins in plasma/serum. Newer approaches to conventional LLE techniques (salting-out LLE) are also covered in this review article.

  2. HASE - The Helsinki adaptive sample preparation line

    Energy Technology Data Exchange (ETDEWEB)

    Palonen, V., E-mail: vesa.palonen@helsinki.fi [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Pesonen, A. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland); Herranen, T.; Tikkanen, P. [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Oinonen, M. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland)

    2013-01-15

    We have designed and built an adaptive sample preparation line with separate modules for combustion, molecular sieve handling, CO{sub 2} gas cleaning, CO{sub 2} storage, and graphitization. The line is also connected to an elemental analyzer. Operation of the vacuum equipment, a flow controller, pressure sensors, ovens, and graphitization reactors are automated with a reliable NI-cRIO real-time system. Stepped combustion can be performed in two ovens at temperatures up to 900 Degree-Sign C. Depending on the application, CuO or O{sub 2}-flow combustion can be used. A flow controller is used to adjust the O{sub 2} flow and pressure during combustion. For environmental samples, a module for molecular sieve regeneration and sample desorption is attached to the line replacing the combustion module. In the storage module, CO{sub 2} samples can be stored behind a gas-tight diaphragm valve and either stored for later graphitization or taken for measurements with separate equipment (AMS gas ion source or a separate mass spectrometer). The graphitization module consists of four automated reactors, capable of graphitizing samples with masses from 3 mg down to 50 {mu}g.

  3. Sample preparation for SEM of plant surfaces

    Directory of Open Access Journals (Sweden)

    A.K. Pathan

    2010-01-01

    Full Text Available Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniques on different leaf types are discussed. Comparative examples are depicted from our lab using similar techniques; the pros and cons for specific techniques are discussed. New promising techniques and microscopes, which can alleviate some of the problems encountered in conventional methods of leaf sample processing and visualisation, are also discussed. It is concluded that the choice of technique for a specific leaf sample is dictated by the surface features that need to be preserved (such as trichomes, epidermal cells or wax microstructure, the resolution to be achieved, availability of the appropriate processing equipment and the technical capabilities of the available electron microscope.

  4. Fluorescence In Situ Hybridization Probe Preparation.

    Science.gov (United States)

    Tolomeo, Doron; Stanyon, Roscoe R; Rocchi, Mariano

    2017-01-01

    The public human genome sequencing project utilized a hierarchical approach. A large number of BAC/PAC clones, with an insert size approximate from 50 kb to 300 kb, were identified and finely mapped with respect to the Sequence Tagged Site (STS) physical map and with respect to each other. A "golden path" of BACs, covering the entire human genome, was then selected and each clone was fully sequenced. The large number of remaining BACs was not fully sequenced, but the availability of the end sequence (~800-1000 bp) at each end allowed them to be very precisely mapped on the human genome.The search for copy number variations of the human genome used several strategies. One of these approaches took advantage of the fact that fosmid clones, contrary to BAC/PAC clones, have a fixed insert size (~40 kb) (Kidd et al., Nature 453: 56-64, 2008). In this context, the ends of ~7 million fosmid clones were sequenced, and therefore it was possible to precisely map these clones on the human genome.In summary, a large number of genomic clones (GC) are available for FISH experiments. They usually yield bright FISH signals and are extremely precious for molecular cytogenetics, and in particular cancer cytogenetics. The already-labeled probes available commercially are usually based on a combination of such GCs. The present chapter summarizes the protocols for extracting, labeling, and hybridization onto slides of DNA obtained from GC.

  5. Preparation of PAA/AM/MMT Hybrid by Intercalation Polymerization

    Institute of Scientific and Technical Information of China (English)

    WANG; YunPu

    2001-01-01

    Over the last few years, Montmorillonite (MMT) was widely used as a special inorganic material for preparing Polymer/MMT nanocompsites. MMT is a clay imineral consisting of stacked silicate sheets whose thickness is about 10A. Through intercalation a large number of polymer-clay nanocomposites have been prepared such as Nylon-clay hybrid [1], PS-clay hybrid [2], Poly (methyl methacrylate) (PMMA)-clay hybrid [3], etc.  In this article, the synthesis and properties of Poly (acrylic acid/acrylamide)/MMT hybrid (PAAAM/MMT) were studied. X-ray diffraction and Transmission electron microscopy were used to characterize the hybrid material. DSC has been used to study its property. Results showed that the intercalating reagents have entered the space of MMT's layers and enlarged them. At the same time, the MMT dispersed homogeneously in acrylic acid and acrylamide monomers that allow MMT to disperse in PAAAM matrix in the monolayer form.  ……

  6. Antibacterial continuous nanofibrous hybrid yarn through in situ synthesis of silver nanoparticles: Preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Barani, Hossein, E-mail: barani@birjand.ac.ir

    2014-10-01

    Nanofibrous hybrid yarns of polyvinyl alcohol (PVA) and poly-L-lactide acid (PLLA) with the antibacterial activity were prepared that contains 0, 5, 10, 20, and 30 wt.% of silver nanoparticles according to the PVA polymer content. This was performed by electrospinning using distilled water and 2, 2, 2-trifluoroethanol as a solvent for PVA and PLLA respectively, and sodium borohydride was used as a reducing agent. The scanning electron microscope observation confirmed the formation of AgNPs into the PVA nanofiber structure, and they were uniform, bead free, cylindrical and smooth. The diameter of hybrid yarns and their nanofiber component was decreased as the silver nitrate concentration in electrospinning solutions was increased. The differential scanning calorimetry results indicated that the silver nanoparticles can form interactions with polymer chains and decrease the melting enthalpy. The mechanical analysis showed a lower stress and strain at break of the AgNP-loaded nanofibrous hybrid yarns than the unloaded hybrid yarn. However, there wasn't a statistically significant difference between the strain at break of electrospun nanofibrous hybrid yarns. Moreover, the bactericidal efficiency of all loaded samples was over 99.99%. - Highlights: • Nanofibrous hybrid yarns of PVA/PLLA with antibacterial activity were prepared. • The diameter of nanofibers was decreased as the AgNP concentration was increased. • AgNPs make interactions with amorphous phase of polymer and increase the Tg. • All loaded samples presented a good bactericidal and bacteriostatic efficiency.

  7. FISHprep: A Novel Integrated Device for Metaphase FISH Sample Preparation

    DEFF Research Database (Denmark)

    Shah, Pranjul Jaykumar; Vedarethinam, Indumathi; Kwasny, Dorota;

    2011-01-01

    We present a novel integrated device for preparing metaphase chromosomes spread slides (FISHprep). The quality of cytogenetic analysis from patient samples greatly relies on the efficiency of sample pre-treatment and/or slide preparation. In cytogenetic slide preparation, cell cultures are routin...... with minimal handling for metaphase FISH slide preparation....

  8. Congener Production in Blood Samples During Preparation and Storage

    DEFF Research Database (Denmark)

    Felby, Søren; Nielsen, Erik

    1995-01-01

    Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone......Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone...

  9. Preparation of hybrid biomaterials for bone tissue engineering

    Directory of Open Access Journals (Sweden)

    Vilma Conceição Costa

    2007-03-01

    Full Text Available Tissue engineering has evolved from the use of biomaterials for bone substitution that fulfill the clinical demands of biocompatibility, biodegradability, non-immunogeneity, structural strength and porosity. Porous scaffolds have been developed in many forms and materials, but few reached the need of adequate physical, biological and mechanical properties. In the present paper we report the preparation of hybrid porous polyvinyl alcohol (PVA/bioactive glass through the sol-gel route, using partially and fully hydrolyzed polyvinyl alcohol, and perform structural characterization. Hybrids containing PVA and bioactive glass with composition 58SiO2-33CaO-9P2O5 were synthesized by foaming a mixture of polymer solution and bioactive glass sol-gel precursor solution. Sol-gel solution was prepared from mixing tetraethoxysilane (TEOS, triethylphosphate (TEP, and calcium chloride as chemical precursors. The hybrid composites obtained after aging and drying at low temperature were chemically and morphologically characterized through infrared spectroscopy and scanning electron microscopy. The degree of hydrolysis of PVA, concentration of PVA solution and different PVA-bioglass composition ratios affect the synthesis procedure. Synthesis parameters must be very well combined in order to allow foaming and gelation. The hybrid scaffolds obtained exhibited macroporous structure with pore size varying from 50 to 600 µm.

  10. Preparation and Property of the Water Absorbent Hybrid Resin

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    @@ Water absorption material has been attracted much more attention for its wide use in soil and water conservation, agriculture, etc. But this material will actually apply in agriculture, soil and water conservation only when it is cheap enough. Pulp fiber and starch to prepare high absorbing-water resin is a good method for decreasing the cost [1,2]. However, it still has a long way to turn it into reality. Now the montmorillonite is widely used in preparing nanocomposites [3]. But used it in preparing absorbing-water resin has little report. In this article the water absorption hybrid resin has been prepared by one step intercalation polymerization method. In the process of intercalation the partly neutralization acrylic acid and urea have been used as intercalating reagent. Beside that, the urea also has been used as cross-linking agent.

  11. Preparation and Property of the Water Absorbent Hybrid Resin

    Institute of Scientific and Technical Information of China (English)

    WANG; YunPu

    2001-01-01

    Water absorption material has been attracted much more attention for its wide use in soil and water conservation, agriculture, etc. But this material will actually apply in agriculture, soil and water conservation only when it is cheap enough. Pulp fiber and starch to prepare high absorbing-water resin is a good method for decreasing the cost [1,2]. However, it still has a long way to turn it into reality.  Now the montmorillonite is widely used in preparing nanocomposites [3]. But used it in preparing absorbing-water resin has little report. In this article the water absorption hybrid resin has been prepared by one step intercalation polymerization method. In the process of intercalation the partly neutralization acrylic acid and urea have been used as intercalating reagent. Beside that, the urea also has been used as cross-linking agent.   ……

  12. Effect of sample storage time on detection of hybridization signals in Checkerboard DNA-DNA hybridization.

    Science.gov (United States)

    do Nascimento, Cássio; Muller, Katia; Sato, Sandra; Albuquerque Junior, Rubens Ferreira

    2012-04-01

    Long-term sample storage can affect the intensity of the hybridization signals provided by molecular diagnostic methods that use chemiluminescent detection. The aim of this study was to evaluate the effect of different storage times on the hybridization signals of 13 bacterial species detected by the Checkerboard DNA-DNA hybridization method using whole-genomic DNA probes. Ninety-six subgingival biofilm samples were collected from 36 healthy subjects, and the intensity of hybridization signals was evaluated at 4 different time periods: (1) immediately after collecting (n = 24) and (2) after storage at -20 °C for 6 months (n = 24), (3) for 12 months (n = 24), and (4) for 24 months (n = 24). The intensity of hybridization signals obtained from groups 1 and 2 were significantly higher than in the other groups (p  0.05). The Checkerboard DNA-DNA hybridization method was suitable to detect hybridization signals from all groups evaluated, and the intensity of signals decreased significantly after long periods of sample storage.

  13. Method of 14C Sample Preparation for AMS Measurement

    Directory of Open Access Journals (Sweden)

    YANG Xu-ran

    2015-02-01

    Full Text Available In order to carry out the application research of 14C by accelerator mass spectrometry (AMS, the principle of sample preparation were systematically studied and more attention was paid to improve the preparation process efficiently. The set of integrated system of sample preparation was built up on the research. The experimental results showed that the sample preparation scheme was able to meet the demand of AMS measurement.

  14. Preparation of Magnetic Hybrid Microspheres with Well-Defined Yolk-Shell Structure

    Directory of Open Access Journals (Sweden)

    Yuan Zhao

    2016-01-01

    Full Text Available A facile and efficient route was reported to prepare a kind of yolk-shell magnetic hybrid microspheres by suspension polymerization and calcinations method. The morphology, structure, and composition of the magnetic microspheres were characterized by FTIR, XRD, TEM, SEM, and TGA analysis. The vibrating-sample magnetometry (VSM results clearly showed that the magnetic particles were superparamagnetic with saturation magnetization of 32.82 emu/g which makes the microcomposites easily controlled by an external magnetic field. The results revealed that the magnetic hybrid microspheres might have important applications in magnetic bioseparation and drug delivery.

  15. Heat-capacity measurements on small samples: The hybrid method

    NARCIS (Netherlands)

    Klaasse, J.C.P.; Brück, E.H.

    2008-01-01

    A newly developed method is presented for measuring heat capacities on small samples, particularly where thermal isolation is not sufficient for the use of the traditional semiadiabatic heat-pulse technique. This "hybrid technique" is a modification of this heat-pulse method in case the temperature

  16. Heat-capacity measurements on small samples: The hybrid method

    NARCIS (Netherlands)

    Klaasse, J.C.P.; Brück, E.H.

    2008-01-01

    A newly developed method is presented for measuring heat capacities on small samples, particularly where thermal isolation is not sufficient for the use of the traditional semiadiabatic heat-pulse technique. This "hybrid technique" is a modification of this heat-pulse method in case the temperature

  17. Homogeneous sample preparation of raw shrimp using dry ice.

    Science.gov (United States)

    Bunch, E A; Altwein, D M; Johnson, L E; Farley, J R; Hammersmith, A A

    1995-01-01

    Sample homogeneity is critical to accurate and reproducible analysis of trace residues in foods. A method of uniform sample preparation using dry ice is described for shrimp. Other sample preparation techniques for raw shrimp produce nonhomogeneous samples. Sample homogeneity was determined through analysis of chloramphenicol added to intact tiger or white shrimp prior to sample preparation. Simulated chloramphenicol residue levels were 50, 15, 10, and 5 ppb. No significant differences were noted when analyses of shrimp inoculated with chlor-amphenicol prior to sample preparation with dry ice were compared with analyses of shrimp spiked after grinding with dry ice. Grinding shrimp with dry ice produced samples with homogeneous chloramphenicol residues. This technique should be applicable to other tissues and vegetable products.

  18. Universal Sample Preparation Module for Molecular Analysis in Space Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Lynntech proposes to develop and demonstrate the ability of a compact, light-weight, and automated universal sample preparation module (USPM) to process samples from...

  19. Preparation of protein samples for gel electrophoresis by sequential extraction

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 等

    2002-01-01

    Since preparation and solubilization of protein samples are crucial factors in proteome research,the authors established a sequential extraction technique to prepare protein samples from the body wall of the 5th instar larvae of silkworm.Bombyx mori.Two kinds of protein samples were obtained from the body wall using the method.Between the two types of samples only about 15% proteins were identical;the majority were different,indicating that more species of proteins could be obtained with the sequential extraction method;which will be useful for preparation of protein samples for proteome study.

  20. Preparation of protein samples for gel electrophoresis by sequential extraction

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 方维焕

    2002-01-01

    Since preparation and solubilization of protein samples are crucial factors in proteome research, the authors established a sequential extraction technique to prepare protein samples from the body wall of the 5th instar larvae of silkworm, Bombyx mori. Two kinds of protein samples were obtained from the body wall using the method. Between the two types of samples only about 15% proteins were identical; the majority were different, indicating that more species of proteins could be obtained with the sequential extraction method; which will be useful for preparation of protein samples for proteome study.

  1. Preparation of Ionic Silsesquioxanes with Regular Structures and Their Hybridization

    Directory of Open Access Journals (Sweden)

    Yoshiro Kaneko

    2012-01-01

    Full Text Available This paper deals with our recent studies on the preparation of ionic silsesquioxanes (SQs with regular structures. Cationic ladder-like polySQs (PSQs with hexagonally stacked structures were successfully prepared by the sol-gel reactions of amino group-containing organotrialkoxysilanes in strong acid aqueous solutions. Self-organization of an ion pair (a salt prepared from the amino group in the organotrialkoxysilane and an acid is the key factor for the formation of such regular structures of the PSQs. It is also reported that the control of the conformational structure of the PSQs was performed by the introduction of the chiral moieties. In addition, we investigated the correlation between the of acid-catalysts and the structures of SQs prepared by the hydrolytic condensation of amino group-containing organotrialkoxysilane, that is, the use of the superacid aqueous solution resulted in the formation of cage-like octaSQ, while the ladder-like PSQs with hexagonally stacked structures were formed from the strong acid aqueous solutions under the same reaction conditions. Furthermore, anion-exchange behaviors of the cationic ladder-like PSQ were investigated with various organic and inorganic compounds, such as anionic surfactants, a polymer, and layered clay minerals, to obtain the functional hybrid materials.

  2. Preparation, characterization and antimicrobial property of ag+- nano Chitosan/ZSM-5: novel Hybrid Biocomposites

    Directory of Open Access Journals (Sweden)

    Maasoumeh Khatamiana

    2016-10-01

    Full Text Available Objective(s: Binary hybrids of chitosan-zeolite have many interesting applications in separation and bacteriostatic activity. Materials and Methods: Template free ZSM-5 zeolite was synthesized by hydrothermal method, physical hydrogels of nano chitosan in the colloidal domain were obtained in the absence of toxic organic solvent and then nano chitosan/ZSM-5 hybrid composites with nano chitosan contents of 0.35%, 3.5%, 35% wt.% were prepared. The as prepared hybrid composites were ion-exchanged with Ag cations. Results: XRD and FT-IR results revealed a good crystalinity of as synthesized template frees ZSM-5 with BET surface area of 307 m2g-1. Presence of chitosan in composites was confirmed by XRD patterns and FT-IR spectroscopic analysis, the chitosan content in composite was obtained with TG analysis. SEM analysis of composites shows that chitosan particles were dispersed within the nanometer scale. The antimicrobial activity of different samples was investigated and the results showed that the Ag+-exchanged samples have the highest antibacterial properties. Cancer cell line A549 cell line were cultured in designated medium treated with Ag+-exchanged samples at the concentration of 0.01 to 0.5 mg/ml. After 24 and 48 hours incubation, the efficacy of Ag+-exchanged samples to treat cancer cell lines were measured by means of cell viability test via MTT assay. Concentrations of 0.05 and 0.1 mg/ml of Ag+-exchanged samples induced a very low toxicity. Conclusion: These hybrid composite materials have potential applications on tissue engineering and antimicrobial food packaging.

  3. COMPARISON OF SAMPLE PREPARATION METHODS FOR CHIP-CHIP ASSAYS

    OpenAIRE

    O'Geen, Henriette; Nicolet, Charles M.; Blahnik, Kim; Green, Roland; Farnham, Peggy J.

    2006-01-01

    A single ChIP sample does not provide enough DNA for hybridization to a genomic tiling array. A commonly used technique for amplifying the DNA obtained from ChIP assays is linker-mediated PCR (LMPCR). However, using this amplification method, we could not identify Oct4 binding sites on genomic tiling arrays representing 1% of the human genome (ENCODE arrays). In contrast, hybridization of a pool of 10 ChIP samples to the arrays produced reproducible binding patterns and low background signals...

  4. Alternative sample preparation methods for MALDI-MS

    Energy Technology Data Exchange (ETDEWEB)

    Hurst, G.B.; Buchanan, M.V. [Oak Ridge National Lab., TN (United States); Czartoski, T.J. [Kenyon College, Gambier, OH (United States)

    1994-12-31

    Since the introduction of matrix-assisted laser desorption and ionization (MALDI), sample preparation has been a limiting step in the applicability of this important technique for mass spectrometric analysis of biomolecules. A number of variations on the original sample preparation method for have been described. The {open_quotes}standard{close_quotes} method of MALDI sample preparation requires mixing a solution containing the analyte and a large excess of matrix, and allowing a small volume of this solution to dry on a probe tip before insertion into the mass spectrometer. The resulting sample can fairly inhomogeneous. As a result, the process of aiming the desorption laser at a favorable spot on the dried sample can be tedious and time-consuming. The authors are evaluating several approaches to MALDI sample preparation, with the goal of developing a faster and more reproducible method.

  5. Snow White Trench Prepared for Sample Collection

    Science.gov (United States)

    2008-01-01

    The informally named 'Snow White' trench is the source for the next sample to be acquired by NASA's Phoenix Mars Lander for analysis by the wet chemistry lab. The Surface Stereo Imager on Phoenix took this shadow-enhanced image of the trench, on the eastern end of Phoenix's work area, on Sol 103, or the 103rd day of the mission, Sept. 8, 2008. The trench is about 23 centimeters (9 inches) wide. The wet chemistry lab is part of Phoenix's Microscopy, Electrochemistry and Conductivity suite of instruments. The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASA's Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  6. Sample preparation for atomic spectroscopy: evolution and future trends

    Directory of Open Access Journals (Sweden)

    Oliveira Elisabeth de

    2003-01-01

    Full Text Available Sample preparation is the critical step of any analytical protocol, and involves steps from simple dilution to partial or total dissolution. The methods include dry or wet decomposition of the samples in open or closed systems, using thermal, ultrasonic or radiant (infrared, ultraviolet and microwaves energy. This review emphasizes sample preparation for atomic spectroscopy. The present and future tendencies for sample preparation also involve on-line dissolution, extraction of the analytes, speciation, solid sample and slurry analysis, in situ and in vivo procedures, etc. Nowadays the goals are the best result, in the shortest time, with minimum contamination, using the smallest quantities of reagents and samples, and having low residue and waste generation, as well as maintaining the integrity of the sample and the traceability of the results, to have quality and confidence in the measurements as the primordial attributes required by the community and by the users.

  7. γ-ray spectrometry results versus sample preparation methods

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    According to recommended conditions two bio-samples, tea leave and flour, are prepared with different methods: grounding into powder and reducing to ash, then they were analyzed by γ ray spectrometry. Remarkable difference was shown between the measured values of tea samples prepared with these different methods. One of the reasons may be that the method of reducing to ash makes some nuclides lost. Compared with the "non-destructive"method of grounding into powder, the method of reducing to ash can be much more sensible to the loss of some nuclides. The probable reasons are discussed for the varied influences of different preparation methods of tea leave and flour samples.

  8. Method for isolating chromosomal DNA in preparation for hybridization in suspension

    Science.gov (United States)

    Lucas, Joe N.

    2000-01-01

    A method is provided for detecting nucleic acid sequence aberrations using two immobilization steps. According to the method, a nucleic acid sequence aberration is detected by detecting nucleic acid sequences having both a first nucleic acid sequence type (e.g., from a first chromosome) and a second nucleic acid sequence type (e.g., from a second chromosome), the presence of the first and the second nucleic acid sequence type on the same nucleic acid sequence indicating the presence of a nucleic acid sequence aberration. In the method, immobilization of a first hybridization probe is used to isolate a first set of nucleic acids in the sample which contain the first nucleic acid sequence type. Immobilization of a second hybridization probe is then used to isolate a second set of nucleic acids from within the first set of nucleic acids which contain the second nucleic acid sequence type. The second set of nucleic acids are then detected, their presence indicating the presence of a nucleic acid sequence aberration. Chromosomal DNA in a sample containing cell debris is prepared for hybridization in suspension by treating the mixture with RNase. The treated DNA can also be fixed prior to hybridization.

  9. Novel flavonolignan hybrid antioxidants: From enzymatic preparation to molecular rationalization.

    Science.gov (United States)

    Vavříková, Eva; Křen, Vladimír; Jezova-Kalachova, Lubica; Biler, Michal; Chantemargue, Benjamin; Pyszková, Michaela; Riva, Sergio; Kuzma, Marek; Valentová, Kateřina; Ulrichová, Jitka; Vrba, Jiří; Trouillas, Patrick; Vacek, Jan

    2017-02-15

    A series of antioxidants was designed and synthesized based on conjugation of the hepatoprotective flavonolignan silybin with l-ascorbic acid, trolox alcohol or tyrosol via a C12 aliphatic linker. These hybrid molecules were prepared from 12-vinyl dodecanedioate-23-O-silybin using the enzymatic regioselective acylation procedure with Novozym 435 (lipase B) or with lipase PS. Voltammetric analyses showed that the silybin-ascorbic acid conjugate exhibited excellent electron donating ability, in comparison to the other conjugates. Free radical scavenging, antioxidant activities and cytoprotective action were evaluated. The silybin-ascorbic acid hybrid exhibited the best activities (IC50 = 30.2 μM) in terms of lipid peroxidation inhibition. The promising protective action of the conjugate against lipid peroxidation can be attributed to modulated electron transfer abilities of both the silybin and ascorbate moieties, but also to the hydrophobic C12 linker facilitating membrane insertion. This was supported experimentally and theoretically by density functional theory (DFT) and molecular dynamics (MD) calculations. The results presented here can be used in the further development of novel multipotent antioxidants and cytoprotective agents, in particular for substances acting at an aqueous/lipid interface. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  10. Microscale sample preparation for PCR of C. difficile infected stool

    Science.gov (United States)

    Gillers, Sara; Atkinson, Christopher D.; Bartoo, Aaron C.; Mahalanabis, Madhumita; Boylan, Michael O.; Schwartz, John H.; Klapperich, Catherine; Singh, Satish K.

    2015-01-01

    In this paper, we describe the design of a microfluidic sample preparation chip for human stool samples infected with Clostridium difficile. We established a polymerase chain reaction able to distinguish C. difficile in the presence of several other organisms found in the normal intestinal flora. A protocol for on-chip extraction of nucleic acids from clinical samples is described that can detect target DNA down to 5.0×10−3 ng of template. The assay and sample preparation chip were then validated using known positive and known negative clinical samples. The work presented has potential applications in both the developed and developing world. PMID:19505511

  11. The effect of sample preparation and testing procedure on the ...

    African Journals Online (AJOL)

    The effect of sample preparation and testing procedure on the geotechnical ... of conventional laboratory testing, classification and evaluation systems, which were ... It should not be used to classify them based on conventional methods ...

  12. Preparation of Cytology Samples: Tricks of the Trade.

    Science.gov (United States)

    Moore, A Russell

    2017-01-01

    General principles and techniques for collection, preparation, and staining of cytologic samples in the general practice setting are reviewed. Tips for collection of digital images are also discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  13. Hybrid microsystem with functionalized silicon substrate and PDMS sample operating microchannel: A reconfigurable microfluidics scheme

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    A hybrid microsystem with separately functioned temperature controlling substrate and sample operating fluidic microchannel was developed to demonstrate a reconfigurable microfluidics scheme.The temperature controlling substrate integrated a micro heater and a temperature sensor by using traditional silicon-based micromechanical system(MEMS)technique,which guaranteed high performance and robust reliability for repeatable usage.The sample operating fluidic microchannel was prepared by poly-(dimethylsiloxane) (PDMS)based soft lithography technique,which made it cheap enough for disposable applications.The PDMS microchannel chip was attached to the temperature controlling substrate for reconfigurable thermal applications.A thin PDMS film was used to seal the microchannel and bridge the functionalized substrate and the sample inside the channel,which facilitated heat transferring and prevented sample contaminating the temperature controlling substrate.Demonstrated by a one dimensional thermal resistance model,the thin PDMS film was important for the present reconfiguration applications.Thermal performance of this hybrid microsystem was examined,and the experimental results demonstrated that the chip system could work stably over hours with temperature variation less than 0.1oC.Multiple PDMS microchannel chips were tested on one heating substrate sequentially with a maximum intra-chip temperature difference of 1.0oC.DNA extracted from serum of a chronic hepatitis B virus(HBV)patient was amplified by this hybrid microsystem and the gel electrophoresis result indicated that the present reconfigurable microfluidic scheme worked successfully.

  14. Modern methods of sample preparation for GC analysis

    OpenAIRE

    de Koning; Janssen, H.-G.; Brinkman, U.A.T.

    2009-01-01

    Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number of ‘modern’ sample-preparation techniques has been introduced, which have partly superseded their ‘classical’ counterparts. These novel techniques include off-line and on-line (sometimes semi- or f...

  15. Hybrid molecularly imprinted polymers synthesized with 3-aminopropyltriethoxysilane-methacrylic acid monomer for miniaturized solid-phase extraction: A new and economical sample preparation strategy for determination of acyclovir in urine.

    Science.gov (United States)

    Yan, Hongyuan; Wang, Mingyu; Han, Yehong; Qiao, Fengxia; Row, Kyung Ho

    2014-06-13

    The miniaturized molecularly imprinted solid-phase extraction (mini-MISPE) coupled with high-performance liquid chromatography was proposed for the determination of acyclovir in urine. 1.5-mL tapered plastic centrifuge tube filled with hybrid molecularly imprinted polymers (HMIPs) was used as the cartridge of mini-MISPE, and the HMIPs synthesized with 3-aminopropyltriethoxy silane-methacrylic acid as monomer exhibited good recognition and selectivity for acyclovir. Under the optimized condition, good linear calibration was obtained in a range of 0.5-15μgmL(-1) with the correlation coefficient of 0.9994, and the recoveries at three spiked levels were 91.6-103.3% in urine with the relative standard deviation (RSD) of ≤3.5%. Excellent intra-day and inter-day repeatability were achieved with RSD of ≤2.6% and 4.0% in three different concentrations. This method combined the advantages of HMIPs and mini-MISPE, and it could become an alternative tool for analyzing the residues of acyclovir in complex urine matrices.

  16. Curatorial Works for the Hayabusa-Returned Sample and Preparation for Hayabusa2 Sample Curation

    Science.gov (United States)

    Yada, T.; Abe, M.; Okada, T.; Yurimoto, H.; Uesugi, M.; Karouji, Y.; Nakato, A.; Hashiguchi, M.; Nishimura, M.; Kumagai, K.; Matsui, S.; Yoshitake, M.; Sakamoto, K.; Nakano, Y.; Kawasaki, N.; Fujimoto, M.

    2016-08-01

    We continue describing Hayabusa-returned samples after its return in 2010. The number of described particles reaches around 650 and >540 of them are identified as Itokawa origin. We also start preparation for Hayabusa2 sample curation.

  17. Hybrid layer thickness and morphology: Influence of cavity preparation with air abrasion.

    Science.gov (United States)

    Barceleiro, Marcos Oliveira; de Mello, Jose Benedicto; Porto, Celso Luis de Angelis; Dias, Katia Regina Hostilio Cervantes; de Miranda, Mauro Sayao

    2011-01-01

    Dentinal surfaces prepared with air abrasion have considerably different characteristics from those prepared with conventional instruments. Different hybrid layer morphology and thickness occur, which can result in differences in the quality of restorations placed on dentinal surfaces prepared with a diamond bur compared to surfaces prepared using air abrasion. The objective of this study was to compare the hybrid layer thickness and morphology formed utilizing Scotchbond Multi-Purpose Plus (SBMP) on dentin prepared with a diamond bur in a high-speed handpiece and on dentin prepared using air abrasion. Flat dentin surfaces obtained from five human teeth were prepared using each method, then treated with the dentin adhesive system according to manufacturer's instructions. After a layer of composite was applied, specimens were sectioned, flattened, polished, and prepared for scanning electron microscopy. Ten different measurements of hybrid layer thickness were obtained along the bonded surface in each specimen. SBMP produced a 3.43 ± 0.75 µm hybrid layer in dentin prepared with diamond bur. This hybrid layer was regular and found consistently. In the air abrasion group, SBMP produced a 4.94 ± 1.28 µm hybrid layer, which was regular and found consistently. Statistical ANOVA (P = 0.05) indicated that there was a statistically significant difference between the groups. These data indicate that the air abrasion, within the parameters used in this study, provides a thick hybrid layer formation.

  18. Comparison of noninvasive sample collection procedures for canine leishmaniasis diagnosis by PCR-hybridization

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Sidney de Almeida; Andrade, Antero Silva Ribeiro de [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)]. E-mail: vidasnino@yahoo.com.br; antero@cdtn.br; Ituassu, Leonardo Trindade; Melo, Maria Norma de [Universidade Federal de Minas Gerais, Belo Horizonte, MG (Brazil)]. E-mail: melo@mono.icb.ufmg.br; ltituassu@yahoo.com.br

    2007-07-01

    The dogs are the main reservoir of the visceral leishmaniasis etiological agent Leishmania chagasi and these animals have to be systematically monitored. The aim of present work was to standardize a method for canine leishmaniasis diagnosis using DNA samples obtained by a noninvasive ways. Two kind of samples were compared: conjunctival swab and blood. The samples were analyzed by the Polymerase Chain Reaction (PCR) associated with the hybridization of {sup 32}P labeled DNA probes. An in vitro test was carried out using cotton swabs seeded with L. chagasi parasites at different cell numbers. After that, the PCR and hybridization sensitivity was evaluated in two groups of 23 seropositive dogs. Conjunctival swabs and 1,0 mL of blood were collected from each animal. 90 {mu}L of these blood were spotted onto filter paper and the remaining used to prepare the buffy coat. The DNA purification from cotton swabs was carried out through the phenol-chloroform (group 1) or boiling (group 2). The Wizard kit was used to DNA extraction from buffy coat. The filters were treated according to Dialab protocol. The analysis of the seeded samples showed that the PCR was able to identify until ten parasites while the following hybridization of the PCR products allows the detection of until one parasite. The PCR positivity for the conjunctival swabs were 73.9% and 52.2% respectively to the groups 1 and 2. For buffy coat the positivities were 43.5% and 56.5% respectively. The filters presented the lowest positivity. The hybridization step was not accomplished yet for these samples. (author)

  19. Nanostructure of PDMS–TEOS–PrZr hybrids prepared by direct deposition of gamma radiation energy

    Energy Technology Data Exchange (ETDEWEB)

    Lancastre, Joana J.H., E-mail: jlancastre@ctn.ist.utl.pt [C2TN, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139.7), 2695-066 Bobadela, LRS (Portugal); Falcão, António N. [C2TN, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139.7), 2695-066 Bobadela, LRS (Portugal); Margaça, Fernanda M.A., E-mail: fmargaca@ctn.ist.utl.pt [C2TN, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139.7), 2695-066 Bobadela, LRS (Portugal); Ferreira, Luís M. [C2TN, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139.7), 2695-066 Bobadela, LRS (Portugal); Miranda Salvado, Isabel M. [CICECO & Departamento de Engenharia de Materiais e Cerâmica, Universidade de Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Almásy, László [Wigner Research Centre for Physics, Institute for Solid State Physics and Optics, PO Box 49, 1525 Budapest (Hungary); Casimiro, Maria H. [REQUIMTE/CQFB, Departamento de Química, Faculdade de Ciências e Tecnologia, FCT, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal); Meiszterics, Anikó [Gedeon Richter Ltd., PO Box 27, H-1475 Budapest (Hungary)

    2015-10-15

    Highlights: • Hybrid materials were prepared by direct energy deposition. • The influence of the catalyst content (PrZr) was investigated. • The developed oxide network was found to be strongly dependent on the PrZr content. • A model is proposed for the development of the oxide network in these materials. - Abstract: Organic–inorganic materials have been the object of intense research due to their wide range of properties and therefore innumerous applications. We prepared organic–inorganic hybrid materials by direct energy deposition on a mixture of polydimethylsiloxane silanol terminated (33 wt% fixed content), tetraethylorthosilicate and a minor content of zirconium propoxide that varied from 1 to 5 wt% using gamma radiation from a Co-60 source. The samples, dried in air at room temperature, are bulk, flexible and transparent. Their nanostructure was investigated by small angle neutron scattering. It was found that the inorganic oxide network has fractal structure, which becomes denser as the zirconium propoxide content decreases. The results suggest that oxide nanosized regions grow from the OH terminal group of PDMS which are the condensation seeds. Their number and position remains unaltered with the variation of zirconium propoxide content that only affects their microstructure. A model is proposed for the nanostructure of the oxide network that develops in the irradiation processed hybrid materials.

  20. Preparation and characterization of ZnO/ZnS hybrid photocatalysts via microwave-hydrothermal method

    Institute of Scientific and Technical Information of China (English)

    Jinglian ZHAO; Liang ZHAO; Xinping WANG

    2008-01-01

    The photocatalytic performance of ZnO/ZnS hybrid nanocomposite was largely higher than that of the mere ZnO or ZnS nanoparticles, but the complicated procedure and misdistribution of final products limited its large-scale productions. The exploration of a novel syn-thesis route of ZnO/ZnS hybrid photocatalysts with high catalytic performance is becoming a crucial step for the large-scale application of ZnO/ZnS hybrid photocatalytic technique. Preparation and characterization of nanosized ZnO/ZnS hybrid photocatalysts were studied in this paper. The photocatalysts were obtained via microwave-hydrothermal crystallization with the help of sodium cit-rate. The products were characterized by X-ray diffrac-tion (XRD), transmission electron microscopy (TEM), particle size distribution (PSD), and Fourier transformed infrared spectroscopy (FT-IR). The results indicated that so-synthesized ZnO/ZnS samples consisted of the high pure cubic (sphalerite) ZnS and hexagonal ZnO nanocrys-tallines with a narrow particle size distribution. The pos-sible formation mechanisms of ZnO/ZnS nanocrystallines were mainly attributed to the superficially protective effect of citrate. The photocatalytic experiments demon-strated that the ZnO/ZnS photocatalysts exhibited a higher catalytic activity for the degradation of acid fuchs-ine than other monocomponents.

  1. Sample Preparation (SS): SE51_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available e Master NEO, BMS, Tokyo, Japan), and the seed powder was extracted with 1 mL of extraction buffer (0.1% HCO...trifugation (4 ℃, 10,000 rpm, 5 min), the sample tubes were subjected to sample preparation (buffer transfer

  2. Classifier Directed Data Hybridization for Geographic Sample Supervised Segment Generation

    Directory of Open Access Journals (Sweden)

    Christoff Fourie

    2014-11-01

    Full Text Available Quality segment generation is a well-known challenge and research objective within Geographic Object-based Image Analysis (GEOBIA. Although methodological avenues within GEOBIA are diverse, segmentation commonly plays a central role in most approaches, influencing and being influenced by surrounding processes. A general approach using supervised quality measures, specifically user provided reference segments, suggest casting the parameters of a given segmentation algorithm as a multidimensional search problem. In such a sample supervised segment generation approach, spatial metrics observing the user provided reference segments may drive the search process. The search is commonly performed by metaheuristics. A novel sample supervised segment generation approach is presented in this work, where the spectral content of provided reference segments is queried. A one-class classification process using spectral information from inside the provided reference segments is used to generate a probability image, which in turn is employed to direct a hybridization of the original input imagery. Segmentation is performed on such a hybrid image. These processes are adjustable, interdependent and form a part of the search problem. Results are presented detailing the performances of four method variants compared to the generic sample supervised segment generation approach, under various conditions in terms of resultant segment quality, required computing time and search process characteristics. Multiple metrics, metaheuristics and segmentation algorithms are tested with this approach. Using the spectral data contained within user provided reference segments to tailor the output generally improves the results in the investigated problem contexts, but at the expense of additional required computing time.

  3. New materials for sample preparation techniques in bioanalysis.

    Science.gov (United States)

    Nazario, Carlos Eduardo Domingues; Fumes, Bruno Henrique; da Silva, Meire Ribeiro; Lanças, Fernando Mauro

    2017-02-01

    The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Preparation of hybrid scaffold from fibrin and biodegradable polymer fiber.

    Science.gov (United States)

    Hokugo, Akishige; Takamoto, Tomoaki; Tabata, Yasuhiko

    2006-01-01

    A biodegradable hybrid scaffold was prepared from fibrin and poly(glycolic acid) (PGA) fiber. Mixed fibrinogen and thrombin solution homogeneously dispersed in the presence of various amounts (0, 1.5, 3.0, and 6.0mg) of PGA fiber was freeze-dried to obtain fibrin sponges with or without PGA fiber incorporation. By scanning electron microscopy observation, the fibrin sponges had an interconnected pore structure, irrespective of the amount of PGA fiber incorporated. PGA fiber incorporation enabled the fibrin sponges to significantly enhance their compression strength. In vitro cell culture studies revealed that the number of L929 fibroblasts initially attached was significantly larger for any fibrin sponge with PGA fiber incorporation than for the fibrin sponge without PGA fiber. The shrinkage of sponges after cell seeding was suppressed by fiber incorporation. It is possible that the shrinkage suppression of sponges maintains their intraspace, resulting in the superior cell attachment of a sponge with PGA fiber incorporation. After subcutaneous implantation into the backs of mice, the residual volume of a fibrin sponge with PGA fiber incorporation was significant compared with that of a fibrin sponge without PGA fiber. Larger number of cells infiltrated deep inside the fibrin sponges with PGA fiber incorporation implanted subcutaneously. It is concluded that the fibrin sponge reinforced by fiber incorporation is a promising three-dimensional scaffold of cells for tissue engineering.

  5. Preparation and characterization of polyimide/silica hybrid films

    Institute of Scientific and Technical Information of China (English)

    ZHANG Ming-yan; ZENG Shu-jin; DONG Tie-quan; ZHOU Sheng; FAN Yong; ZHANG Xiao-hong; LEI Qing-quan

    2006-01-01

    A kind of hybrid polyimide films was prepared by synthesizing poly( amic acid ) /Silica matrix resin through sol-gel technique and then followed by positing it on a silex glass plate and drying at high temperature.The effect of silica content on the corona-resistant property of the films was studied. The miscibility between the organic and inorganic phases and its effect on the corona-resistant property were investigated with aminopropyltriethoxysilane, which served as a coupling agent, added into the polyimide composite system. The chemical structure and the surface morphology of the films were characterized by FTIR and AFM respectively. The corona-resistant property of the films was tested by a rod-plate electrode. It proved that the corona-resistant property was enhanced with silica content. It also turned ont that the improvement of the miscibility between the two phases due to the presence of covalent force as a result of the addition of the coupling agent had, to some extent,effect on the corona-resistant property of the films. Furthermore, a theory on the corona-resistant property was put forward preliminarily.

  6. A novel fluorescent in situ hybridization technique for detection of Rickettsia spp. in archival samples

    DEFF Research Database (Denmark)

    Svendsen, Claus Bo; Boye, Mette; Struve, Carsten

    2009-01-01

    A novel, sensitive and specific method for detecting Rickettsia spp. in archival samples is described. The method involves the use of fluorescently marked oligonucleotide probes for in situ hybridization. Specific hybridization of Ricekttsia was found without problems of cross-reactions with bact......A novel, sensitive and specific method for detecting Rickettsia spp. in archival samples is described. The method involves the use of fluorescently marked oligonucleotide probes for in situ hybridization. Specific hybridization of Ricekttsia was found without problems of cross...

  7. Facile preparation of TiO{sub 2}–polyvinyl alcohol hybrid nanoparticles with improved visible light photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Filippo, Emanuela [Department of Innovation Engineering, University of Salento, Monteroni Street, 73100, Lecce (Italy); Carlucci, Claudia; Capodilupo, Agostina Lina [National Nanotechnology Laboratory (NNL), Nanoscience Institure – CNR, Arnesano Street, 73100 Lecce (Italy); Perulli, Patrizia [Department of Innovation Engineering, University of Salento, Monteroni Street, 73100, Lecce (Italy); Conciauro, Francesca [National Nanotechnology Laboratory (NNL), Nanoscience Institure – CNR, Arnesano Street, 73100 Lecce (Italy); Corrente, Giuseppina Anna [University of Calabria, Pietro Bucci Street, 87036 Arcavacata di Rende, Cosenza (Italy); Gigli, Giuseppe [National Nanotechnology Laboratory (NNL), Nanoscience Institure – CNR, Arnesano Street, 73100 Lecce (Italy); Center for Biomolecular Nanotechnologies (CBN) of Italian Institute of Technology (IIT), Barsanti Street 1, 73010 Arnesano (Italy); Department of Physics, University of Salento, Monteroni Street, 73100, Lecce (Italy); Ciccarella, Giuseppe, E-mail: giuseppe.ciccarella@unisalento.it [Department of Innovation Engineering, University of Salento, Monteroni Street, 73100, Lecce (Italy); National Nanotechnology Laboratory (NNL), Nanoscience Institure – CNR, Arnesano Street, 73100 Lecce (Italy)

    2015-03-15

    Graphical abstract: - Highlights: • Hybrid TiO{sub 2}/PVA core/shell nanoparticles were prepared through a two step procedure. • TiO{sub 2}–PVA samples were prepared based on different TiO{sub 2}–PVA weight ratios. • All samples were characterized using XRD, TEM, FT-IR and BET analysis. • The photocatalytic performance was evaluated. - Abstract: Hybrid inorganic/organic core/shell nanoparticles were prepared through a two step synthesis procedure. In the first step, pure anatase TiO{sub 2} nanoparticles were synthesized though a rapid microwave assisted non-aqueous route. Then, the obtained titania nanoparticles were coated with polyvinyl alcohol (PVA) using a simple solution method followed by relatively low temperature treatment. The PVA-coated titania nanoparticles samples were prepared at different TiO{sub 2}–PVA weight ratio and they were characterized using X-Ray diffraction, transmission electron microscopy, infrared spectroscopy and Brunauer–Emmett–Teller (BET) analysis. Photocatalytic performance was also evaluated for all samples and the results indicated that TiO{sub 2}:PVA weight ratio was a key factor to obtain an improvement of the photocatalytic activity with respect to bare TiO{sub 2} nanoparticles, since PVA concentration influenced the surface area and the aggregation of nanoparticles and the thickness of the coating layer. This inexpensive system provides a simple, quick and effective approach which allows to obtain core/shell hybrid nanostructures.

  8. Microfluidic Sample Preparation Methods for the Analysis of Milk Contaminants

    Directory of Open Access Journals (Sweden)

    Andrea Adami

    2016-01-01

    Full Text Available In systems for food analysis, one of the major challenges is related to the quantification of specific species into the complex chemical and physical composition of foods, that is, the effect of “matrix”; the sample preparation is often the key to a successful application of biosensors to real measurements but little attention is traditionally paid to such aspects in sensor research. In this critical review, we discuss several microfluidic concepts that can play a significant role in sample preparation, highlighting the importance of sample preparation for efficient detection of food contamination. As a case study, we focus on the challenges related to the detection of aflatoxin M1 in milk and we evaluate possible approaches based on inertial microfluidics, electrophoresis, and acoustic separation, compared with traditional laboratory and industrial methods for phase separation as a baseline of thrust and well-established techniques.

  9. Fluidics platform and method for sample preparation and analysis

    Energy Technology Data Exchange (ETDEWEB)

    Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

    2014-08-19

    Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

  10. Biomolecular hybrid material and process for preparing same and uses for same

    Science.gov (United States)

    Kim, Jungbae [Richland, WA

    2010-11-23

    Disclosed is a composition and method for fabricating novel hybrid materials comprised of, e.g., carbon nanotubes (CNTs) and crosslinked enzyme clusters (CECs). In one method, enzyme-CNT hybrids are prepared by precipitation of enzymes which are subsequently crosslinked, yielding crosslinked enzyme clusters (CECs) on the surface of the CNTs. The CEC-enzyme-CNT hybrids exhibit high activity per unit area or mass as well as improved enzyme stability and longevity over hybrid materials known in the art. The CECs in the disclosed materials permit multilayer biocatalytic coatings to be applied to surfaces providing hybrid materials suitable for use in, e.g., biocatalytic applications and devices as described herein.

  11. Sample preparation for quantitation of tritium by accelerator mass spectrometry.

    Science.gov (United States)

    Chiarappa-Zucca, Marina L; Dingley, Karen H; Roberts, Mark L; Velsko, Carol A; Love, Adam H

    2002-12-15

    The capability to prepare samples accurately and reproducibly for analysis of tritium (3H) content by accelerator mass spectrometry (AMS) greatly facilitates isotopic tracer studies in which attomole levels of 3H can be measured in milligram-sized samples. A method has been developed to convert the hydrogen of organic samples to a solid, titanium hydride, which can be analyzed by AMS. Using a two-step process, the sample is first oxidized to carbon dioxide and water. In the second step, the water is transferred within a heated manifold into a quartz tube, reduced to hydrogen gas using zinc, and reacted with titanium powder. The 3H/1H ratio of the titanium hydride is measured by AMS and normalized to standards whose ratios were determined by decay counting to calculate the amount of 3H in the original sample. Water, organic compounds, and biological samples with 3H activities measured by liquid scintillation counting were utilized to develop and validate the method. The 3H/1H ratios were quantified in samples that spanned 5 orders of magnitude, from 10(-10) to 10(-15), with a detection limit of 3.0 x 10(-15), which is equivalent to 0.02 dpm tritium/mg of material. Samples smaller than 2 mg were analyzed following addition of 2 mg of a tritium-free-hydrogen carrier. Preparation of organic standards containing both 14C and 3H in 2-mg organic samples demonstrated that this sample preparation methodology can also be applied to quantify both of these isotopes from a single sample.

  12. Basic tree-ring sample preparation techniques for aging aspen

    Science.gov (United States)

    Lance A. Asherin; Stephen A. Mata

    2001-01-01

    Aspen is notoriously difficult to age because of its light-colored wood and faint annual growth rings. Careful preparation and processing of aspen ring samples can overcome these problems, yield accurate age and growth estimates, and concisely date disturbance events present in the tree-ring record. Proper collection of aspen wood is essential in obtaining usable ring...

  13. 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.

  14. Preparing Students for Success in Hybrid Learning Environments with Academic Resource Centers

    Science.gov (United States)

    Newman, Daniel; Dickinson, Michael

    2017-01-01

    This chapter describes institutional and andragogical best practices for preparing students to succeed in hybrid courses through the programming of academic resource centers, offers information on how to create peer support systems for students, and outlines some of the common pitfalls for students encountering a hybrid course for the first time.

  15. Applications of reversible covalent chemistry in analytical sample preparation.

    Science.gov (United States)

    Siegel, David

    2012-12-07

    Reversible covalent chemistry (RCC) adds another dimension to commonly used sample preparation techniques like solid-phase extraction (SPE), solid-phase microextraction (SPME), molecular imprinted polymers (MIPs) or immuno-affinity cleanup (IAC): chemical selectivity. By selecting analytes according to their covalent reactivity, sample complexity can be reduced significantly, resulting in enhanced analytical performance for low-abundance target analytes. This review gives a comprehensive overview of the applications of RCC in analytical sample preparation. The major reactions covered include reversible boronic ester formation, thiol-disulfide exchange and reversible hydrazone formation, targeting analyte groups like diols (sugars, glycoproteins and glycopeptides, catechols), thiols (cysteinyl-proteins and cysteinyl-peptides) and carbonyls (carbonylated proteins, mycotoxins). Their applications range from low abundance proteomics to reversible protein/peptide labelling to antibody chromatography to quantitative and qualitative food analysis. In discussing the potential of RCC, a special focus is on the conditions and restrictions of the utilized reaction chemistry.

  16. Retrospective study of trisomy 18 in chorionic villi with fluorescent in situ hybridization on archival direct preparations

    OpenAIRE

    Van Opstal, Diane; Berg, Cardi; Jahoda, M.; Brandenburg, Helen; Los, F.J.; in 't Veld, Peter

    1995-01-01

    textabstractTrisomy 18 in direct chorionic villus preparations needs further investigation since the chromosome abnormality may be confined to the placenta and may not represent the actual fetal karyotype. We performed, retrospectively, fluorescent in situ hybridization (FISH) with the chromosome 18 centromere probe (L1.84) on interphase nuclei of destained slides of all cases of full trisomy 18 (n=22) and mosaic trisomy 18 (n=8) detected among 7600 first-trimester chorionic villus samples du...

  17. [Optimized sample preparation for metabolome studies on Streptomyces coelicolor].

    Science.gov (United States)

    Li, Yihong; Li, Shanshan; Ai, Guomin; Wang, Weishan; Zhang, Buchang; Yang, Keqian

    2014-04-01

    Streptomycetes produce many antibiotics and are important model microorgansims for scientific research and antibiotic production. Metabolomics is an emerging technological platform to analyze low molecular weight metabolites in a given organism qualitatively and quantitatively. Compared to other Omics platform, metabolomics has greater advantage in monitoring metabolic flux distribution and thus identifying key metabolites related to target metabolic pathway. The present work aims at establishing a rapid, accurate sample preparation protocol for metabolomics analysis in streptomycetes. In the present work, several sample preparation steps, including cell quenching time, cell separation method, conditions for metabolite extraction and metabolite derivatization were optimized. Then, the metabolic profiles of Streptomyces coelicolor during different growth stages were analyzed by GC-MS. The optimal sample preparation conditions were as follows: time of low-temperature quenching 4 min, cell separation by fast filtration, time of freeze-thaw 45 s/3 min and the conditions of metabolite derivatization at 40 degrees C for 90 min. By using this optimized protocol, 103 metabolites were finally identified from a sample of S. coelicolor, which distribute in central metabolic pathways (glycolysis, pentose phosphate pathway and citrate cycle), amino acid, fatty acid, nucleotide metabolic pathways, etc. By comparing the temporal profiles of these metabolites, the amino acid and fatty acid metabolic pathways were found to stay at a high level during stationary phase, therefore, these pathways may play an important role during the transition between the primary and secondary metabolism. An optimized protocol of sample preparation was established and applied for metabolomics analysis of S. coelicolor, 103 metabolites were identified. The temporal profiles of metabolites reveal amino acid and fatty acid metabolic pathways may play an important role in the transition from primary to

  18. Preparation and characterization of functional silica hybrid magnetic nanoparticles

    Science.gov (United States)

    Digigow, Reinaldo G.; Dechézelles, Jean-François; Dietsch, Hervé; Geissbühler, Isabelle; Vanhecke, Dimitri; Geers, Christoph; Hirt, Ann M.; Rothen-Rutishauser, Barbara; Petri-Fink, Alke

    2014-08-01

    We report on the synthesis and characterization of functional silica hybrid magnetic nanoparticles (SHMNPs). The co-condensation of 3-aminopropyltriethoxysilane (APTES) and tetraethyl orthosilicate (TEOS) in presence of superparamagnetic iron oxide nanoparticles (SPIONs) leads to hybrid magnetic silica particles that are surface-functionalized with primary amino groups. In this work, a comprehensive synthetic study is carried out and completed by a detailed characterization of hybrid particles' size and morphology, surface properties, and magnetic responses using different techniques. Depending on the mass ratio of SPIONs and the two silanes (TEOS and APTES), we were able to adjust the number of surface amino groups and tune the magnetic properties of the superparamagnetic hybrid particles.

  19. Preparation and characterization of perfluorosulfonic resin/titania hybrid transparent films

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Preparation and characterization of perfluorosulfonic resin/titania organic-inorganic hybrid films were presented. The transparent hybrid films were prepared by hydrothermal treatment at low temperature of a mixed solution of tetrabutyl titanate and perfluorosulfonic resin with the help of acetylacetone. The characterization was carried out by SEM,XRD,FT-IR,UV-Vis and TGA. The results showed that the perfluorosulfonic resin/titania hybrid transparent films were composed of titania particles dispersed in the perfluorosulfonic resin matrix very well and the titania was of anatase phase. Its diameter de-creased with increasing weight ratio of titania to perfluorosulfonic resin.

  20. Preparation and characterization of perfluorosulfonic resin/titania hybrid transparent films

    Institute of Scientific and Technical Information of China (English)

    LI JianMei; XUE MinZhao; ZHANG YongMing; LIU YanGang

    2007-01-01

    Preparation and characterization of perfluoroaulfonic resin/titaniaorganic-inorganic hybrid films were presented. The transparent hybrid films were prepared by hydrothermal treatment at low temperature of a mixed solution of tetrabutyl titanata and perfluorosulfonic resin with the help of acetylacetone. The charactarization was carried out by SEM, XRD, FT-IR, UV-Vis and TGA. The results showed that the perfiuorosulfonic resin/titania hybrid transparent films were composed of titania particles dispersed in the perfluorosulfonic resin matrix very well and the titania was of anatase phase. Its diameter decreased with increasing weight ratio of titania to perfluorosulfonic resin.

  1. Facile approach to prepare Pt decorated SWNT/graphene hybrid catalytic ink

    Energy Technology Data Exchange (ETDEWEB)

    Mayavan, Sundar, E-mail: sundarmayavan@cecri.res.in [Centre for Innovation in Energy Research, CSIR–Central Electrochemical Research Institute, Karaikudi 630006, Tamil Nadu (India); Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, Daejeon, 305-701 (Korea, Republic of); Mandalam, Aditya; Balasubramanian, M. [Centre for Innovation in Energy Research, CSIR–Central Electrochemical Research Institute, Karaikudi 630006, Tamil Nadu (India); Sim, Jun-Bo [Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, Daejeon, 305-701 (Korea, Republic of); Choi, Sung-Min, E-mail: sungmin@kaist.ac.kr [Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, Daejeon, 305-701 (Korea, Republic of)

    2015-07-15

    Highlights: • Pt NPs were in situ synthesized onto CNT–graphene support in aqueous solution. • The as-prepared material was used directly as a catalyst ink without further treatment. • Catalyst ink is active toward methanol oxidation. • This approach realizes both scalable and greener production of hybrid catalysts. - Abstract: Platinum nanoparticles were in situ synthesized onto hybrid support involving graphene and single walled carbon nanotube in aqueous solution. We investigate the reduction of graphene oxide, and platinum nanoparticle functionalization on hybrid support by X-ray photoelectron spectroscopy, Raman spectroscopy, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The as-prepared platinum on hybrid support was used directly as a catalyst ink without further treatment and is active toward methanol oxidation. This work realizes both scalable and greener production of highly efficient hybrid catalysts, and would be valuable for practical applications of graphene based fuel cell catalysts.

  2. Preparation of SELEX Samples for Next-Generation Sequencing.

    Science.gov (United States)

    Tolle, Fabian; Mayer, Günter

    2016-01-01

    Fuelled by massive whole genome sequencing projects such as the human genome project, enormous technological advancements and therefore tremendous price drops could be achieved, rendering next-generation sequencing very attractive for deep sequencing of SELEX libraries. Herein we describe the preparation of SELEX samples for Illumina sequencing, based on the already established whole genome sequencing workflow. We describe the addition of barcode sequences for multiplexing and the adapter ligation, avoiding associated pitfalls.

  3. Conjugated polymers/semiconductor nanocrystals hybrid materials--preparation, electrical transport properties and applications.

    Science.gov (United States)

    Reiss, Peter; Couderc, Elsa; De Girolamo, Julia; Pron, Adam

    2011-02-01

    This critical review discusses specific preparation and characterization methods applied to hybrid materials consisting of π-conjugated polymers (or oligomers) and semiconductor nanocrystals. These materials are of great importance in the quickly growing field of hybrid organic/inorganic electronics since they can serve as active components of photovoltaic cells, light emitting diodes, photodetectors and other devices. The electronic energy levels of the organic and inorganic components of the hybrid can be tuned individually and thin hybrid films can be processed using low cost solution based techniques. However, the interface between the hybrid components and the morphology of the hybrid directly influences the generation, separation and transport of charge carriers and those parameters are not easy to control. Therefore a large variety of different approaches for assembling the building blocks--conjugated polymers and semiconductor nanocrystals--has been developed. They range from their simple blending through various grafting procedures to methods exploiting specific non-covalent interactions between both components, induced by their tailor-made functionalization. In the first part of this review, we discuss the preparation of the building blocks (nanocrystals and polymers) and the strategies for their assembly into hybrid materials' thin films. In the second part, we focus on the charge carriers' generation and their transport within the hybrids. Finally, we summarize the performances of solar cells using conjugated polymer/semiconductor nanocrystals hybrids and give perspectives for future developments.

  4. Preparation of fluorescent-dye-labeled cDNA from RNA for microarray hybridization.

    Science.gov (United States)

    Ares, Manuel

    2014-01-01

    This protocol describes how to prepare fluorescently labeled cDNA for hybridization to microarrays. It consists of two steps: first, a mixture of anchored oligo(dT) and random hexamers is used to prime amine-modified cDNA synthesis by reverse transcriptase using a modified deoxynucleotide with a reactive amine group (aminoallyl-dUTP) and an RNA sample as a template. Second, the cDNA is purified and exchanged into bicarbonate buffer so that the amine groups in the cDNA react with the dye N-hydroxysuccinimide (NHS) esters, covalently joining the dye to the cDNA. The dye-coupled cDNA is purified again, and the amount of dye incorporated per microgram of cDNA is determined.

  5. Optimization for Peptide Sample Preparation for Urine Peptidomics

    Energy Technology Data Exchange (ETDEWEB)

    Sigdel, Tara K.; Nicora, Carrie D.; Hsieh, Szu-Chuan; Dai, Hong; Qian, Weijun; Camp, David G.; Sarwal, Minnie M.

    2014-02-25

    Analysis of native or endogenous peptides in biofluids can provide valuable insights into disease mechanisms. Furthermore, the detected peptides may also have utility as potential biomarkers for non-invasive monitoring of human diseases. The non-invasive nature of urine collection and the abundance of peptides in the urine makes analysis by high-throughput ‘peptidomics’ methods , an attractive approach for investigating the pathogenesis of renal disease. However, urine peptidomics methodologies can be problematic with regards to difficulties associated with sample preparation. The urine matrix can provide significant background interference in making the analytical measurements that it hampers both the identification of peptides and the depth of the peptidomics read when utilizing LC-MS based peptidome analysis. We report on a novel adaptation of the standard solid phase extraction (SPE) method to a modified SPE (mSPE) approach for improved peptide yield and analysis sensitivity with LC-MS based peptidomics in terms of time, cost, clogging of the LC-MS column, peptide yield, peptide quality, and number of peptides identified by each method. Expense and time requirements were comparable for both SPE and mSPE, but more interfering contaminants from the urine matrix were evident in the SPE preparations (e.g., clogging of the LC-MS columns, yellowish background coloration of prepared samples due to retained urobilin, lower peptide yields) when compared to the mSPE method. When we compared data from technical replicates of 4 runs, the mSPE method provided significantly improved efficiencies for the preparation of samples from urine (e.g., mSPE peptide identification 82% versus 18% with SPE; p = 8.92E-05). Additionally, peptide identifications, when applying the mSPE method, highlighted the biology of differential activation of urine peptidases during acute renal transplant rejection with distinct laddering of specific peptides, which was obscured for most proteins

  6. Preparation of a Hybrid Zirconium Phytate and Its Application for the Removal of Fluorine in Metal-Precoating Effluent

    Directory of Open Access Journals (Sweden)

    Cheng Wenkai

    2016-01-01

    Full Text Available A hybrid zirconium phytate (ZrxIP6 with porous surface was synthesized via the direct precipitation method. The as-prepared ZrxIP6 was characterized by SEM, EDS, FT-IR. The sample obtained from P/Zr = 3:1(mol/mol indicated that a hybrid material might be formed through coordination of the zirconium ions with the –COPO3 groups in phytic acid molecules. An attempt to employ the hybrid ZrxIP6 as a sorbent in the removal of fluoride ions in metal-precoating wastewater was performed. The adsorption capacity qe and the residual F- ions concentration Ce using the ZrxIP6 (P/Zr = 3:1 as an adsorbent, were 1.21 mg.g-1 and 1.47 mg.L-1, respectively.

  7. SEM evaluation of the hybrid layer after cavity preparation with Er:YAG laser.

    Science.gov (United States)

    de Barceleiro, Marcos Oliveira; Dias, Kátia Regina Hostílio Cervantes; Sales, Helena Xavier; Silva, Bárbara Carvalho; Barceleiro, Cristiane Gomes

    2008-01-01

    This study compared the thickness of the hybrid layer formed using Scotchbond Multi-Purpose Plus, Single Bond 2, Prime & Bond 2.1 and Xeno III on a dentin surface prepared with a diamond bur in a high speed handpiece or prepared with an Er:YAG laser used with two parameters of pulse energy (200 and 400 mJ) and two parameters of frequency (4 and 6 Hz). Flat dentin surfaces obtained from 20 human third molars were treated with the two methods and were then prepared with the dentin adhesive systems according to the manufacturers' instructions. After a layer of composite was applied, the specimens were sectioned, flattened, polished and prepared for Scanning Electronic Microscopy observation. Five different measurements of the hybrid layer thickness were obtained along the bonded surface in each specimen. The results were statistically analyzed using Analysis of Variance and Student-Newman-Keuls tests (p cavity preparation method, four groups were formed: Group I (diamond bur) > Group II (Laser 200 mJ/4 Hz) = Group III (Laser 200 mJ/6 Hz) > Group IV (Laser 400 mJ/4 Hz) > Group V (Laser 400 mJ/6 Hz). When comparing the dentin adhesive systems, there were no statistically significant differences. These results showed that the four tested dentin adhesive systems produced a 2.90 +/- 1.71 microm hybrid layer in dentin prepared with a diamond bur. This hybrid layer was regular and routinely found. In the laser groups, the dentin adhesive systems produced hybrid layers ranging from 0.41 +/- 1.00 microm to 2.06 +/- 2.49 microm, which were very irregular and not routinely found. It was also concluded that the Er:YAG laser, with the parameters used in this experiment, has a negative influence on the formation of a hybrid layer and cavity preparation methods influence formation of the hybrid layer.

  8. Radiocarbon accelerator mass spectrometry (AMS) sample preparation laboratory in Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Macario, Kita D.; Gomes, Paulo R. S.; Anjos, Roberto M. dos; Linares, Roberto; Queiroz, Eduardo; Oliveira, Fabiana M. de; Cardozo, Laio [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil); Carvalho, Carla R.A. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil)

    2011-07-01

    Full text: For decades Accelerator Mass Spectrometry has been widely used for radiocarbon measurements all over the world with application in several fields of science from archaeology to geosciences. This technique provides ultrasensitive analysis of reduced size samples or even specific compounds since sample atoms are accelerated to high energies and measured using nuclear particle detectors. Sample preparation is extremely important for accurate radiocarbon measurement and includes chemical pre-treatment to remove all possible contaminants. For beam extraction in the accelerator ion source, samples are usually converted to graphite. In this work we report a new radiocarbon sample preparation facility installed at the Physics Institute of Universidade Federal Fluminense (UFF), in Brazil. At the Nuclear Chronology Laboratory (LACRON) samples are chemically treated and converted to carbon dioxide by hydrolysis or combustion. A stainless steel based vacuum line was constructed for carbon dioxide separation and graphitization is performed in sealed quartz tubes in a muffle oven. Successful graphite production is important to provide stable beam currents and to minimize isotopic fractionation. Performance tests for graphite production are currently under way and isotopic analysis will soon be possible with the acquisition of a Single Stage AMS System by our group. The Single Stage Accelerator produced by National Electrostatic Corporation is a 250 kV air insulated accelerator especially constructed to measure the amount of {sup 14}C in small modern graphite samples to a precision of 0.3 % or better. With the installation of such equipment in the first half of 2012, UFF will be ready to perform the 14C -AMS technique. (author)

  9. Preparation of LiMn2O4 Graphene Hybrid Nanostructure by Combustion Synthesis and Their Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Dinesh Rangappa

    2014-10-01

    Full Text Available The LiMn2O4 graphene hybrid cathode material has been synthesized by spray drying combustion process. The spinel structure cubic phase LiMn2O4 graphene hybrid material was prepared by spray drying process at 120 ℃ and subsequent heat treatment at 700 ℃ for 1 hour. The result indicates that the spinel shaped LiMn2O4 particles wrapped with graphene sheets were formed with particle size in the range of 60-70 nm. The charge-discharge measurement indicates that the LiMn2O4 graphene hybrid material shows an improved discharge capacity of 139 mAh/g at 0.1C rate. The pristine LiMn2O4 nano crystals present only about 132 mAh/g discharge capacity. The LiMn2O4 graphene hybrid samples show good cyclic performance with only 13% of capacity fading in 30 cycles when compared to the pristine LiMn2O4 that shows 22% of capacity fading in 30 cycles. The capacity retention of the LiMn2O4 graphene hybrid samples is about 10% higher than the pristine cycle after 30 cycles.

  10. Preparation of alpha-bisabolol and phenylethyl resorcinol/TiO2 hybrid composites for potential applications in cosmetics.

    Science.gov (United States)

    Leong, H J; Jang, I; Hyun, K-S; Jung, S-K; Hong, G-H; Jeong, H-A; Oh, S-G

    2016-10-01

    Bifunctional alpha-bisabolol and phenylethyl resorcinol/TiO2 hybrids were prepared to apply in cosmetic fields, particularly in anti-ageing and hyperpigmentation treatment. The synergistic effect of combined antioxidant and UV filtering properties was achieved through functionalization of TiO2 particles with skin-lightening materials such as alpha-bisabolol and phenylethyl resorcinol. TiO2 microspheres with a diameter of about 1 μm were synthesized through surfactant-assisted sol-gel method for use as supporting materials in the formation of hybrid composites. Carboxylation treatment was performed for surface modification of the TiO2 surface with carboxyl groups as chemical binders. Esterification reaction between carboxyl groups of carboxylated TiO2 and hydroxyl groups of alpha-bisabolol or phenylethyl resorcinol was performed. The hybrids were characterized using various techniques such as FE-SEM, DLS, EDS, ATR-FTIR, XPS and TGA. For application of prepared TiO2 composites in the field of cosmetics, the anti-radicular antioxidant abilities were evaluated using ABTS and DPPH colorimetric antioxidant assay. Organic/inorganic hybrid composites were successfully formed using esterification reaction between the carboxyl groups at TiO2 surface and the hydroxyl groups of the skin-lightening materials. The results demonstrate that both functionalized microspheres show scavenging ability towards the ABTS(•) and DPPH(•) radicals. Specifically, the phenylethyl resorcinol/TiO2 composites exhibited the highest antioxidant ability among the prepared samples owing to the presence of phenolic groups to scavenge free radicals. Using this strategy, it could be possible to prepare not only inorganic UV filter but also hybrid organic/inorganic materials with multifunctions and advantages which would be in a great demand for cosmetic applications. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  11. Amorphous semiconductor sample preparation for transmission EXAFS measurements

    Energy Technology Data Exchange (ETDEWEB)

    Ridgway, M.C.; Glover, C.J.; Tan, H.H. [Australian National Univ., Canberra (Australia). Dept. of Electronic Materials Engineering] [and others

    1998-12-31

    A novel methodology has been developed for the preparation of amorphous semiconductor samples for use in transmission extended x-ray absorption fine structure (EXAFS) measurements. Epitaxial heterostructures were fabricated by metal organic chemical vapor deposition (group III-Vs) or molecular beam epitaxy (group IVs). An epitaxial layer of {approximately} 2 {micro}m thickness was separated from the underlying substrate by selective chemical etching of an intermediate sacrificial layer. Ion implantation was utilized to amorphize the epitaxial layer either before or after selective chemical etching. The resulting samples were both stoichiometric and homogeneous in contrast to those produced by conventional techniques. The fabrication of amorphous GaAs, InP, In{sub 0.53}Ga{sub 0.47}As and Si{sub x}Ge{sub 1{minus}x} samples is described. Furthermore, EXAFS measurements comparing both fluorescence and transmission detection, and crystalline and amorphized GaAs, are shown.

  12. Hands-free sample preparation platform for nucleic acid analysis.

    Science.gov (United States)

    Baier, T; Hansen-Hagge, T E; Gransee, R; Crombé, A; Schmahl, S; Paulus, C; Drese, K S; Keegan, H; Martin, C; O'Leary, J J; Furuberg, L; Solli, L; Grønn, P; Falang, I M; Karlgård, A; Gulliksen, A; Karlsen, F

    2009-12-07

    A Lab-On-Chip system with an instrument is presented which is capable of performing total sample preparation and automated extraction of nucleic acid from human cell samples fixed in a methanol based solution. The target application is extraction of mRNA from cervical liquid based cytology specimens for detection of transformed HPV-infections. The device accepts 3 ml of sample and performs the extraction in a disposable polymer chip of credit card size. All necessary reagents for cell lysis, washing, and elution are stored on-chip and the extraction is performed in two filter stages; one for cell pre-concentration and the other for nucleic acid capture. Tests performed using cancer cell lines and cervical liquid based cytology specimens confirm the extraction of HPV-mRNA by the system.

  13. A fast method to prepare water samples for 15N analysis

    Institute of Scientific and Technical Information of China (English)

    肖化云; 刘丛强

    2001-01-01

    Automatic element analyser is often used to prepare organic matters tor 15N analysis. It is seldom used to prepare water samples. Water samples are conventionally dealt with by Kjeldahl-Rittenberg technique. But it requires tedious and labor-intensive sample preparation. A fast and reliable method is proposed in this paper to prepare water samples for 15N analysis.

  14. Nanostructure of PDMS-TEOS-PrZr hybrids prepared by direct deposition of gamma radiation energy

    Science.gov (United States)

    Lancastre, Joana J. H.; Falcão, António N.; Margaça, Fernanda M. A.; Ferreira, Luís M.; Miranda Salvado, Isabel M.; Almásy, László; Casimiro, Maria H.; Meiszterics, Anikó

    2015-10-01

    Organic-inorganic materials have been the object of intense research due to their wide range of properties and therefore innumerous applications. We prepared organic-inorganic hybrid materials by direct energy deposition on a mixture of polydimethylsiloxane silanol terminated (33 wt% fixed content), tetraethylorthosilicate and a minor content of zirconium propoxide that varied from 1 to 5 wt% using gamma radiation from a Co-60 source. The samples, dried in air at room temperature, are bulk, flexible and transparent. Their nanostructure was investigated by small angle neutron scattering. It was found that the inorganic oxide network has fractal structure, which becomes denser as the zirconium propoxide content decreases. The results suggest that oxide nanosized regions grow from the OH terminal group of PDMS which are the condensation seeds. Their number and position remains unaltered with the variation of zirconium propoxide content that only affects their microstructure. A model is proposed for the nanostructure of the oxide network that develops in the irradiation processed hybrid materials.

  15. Sample Preparation (SS) - Metabolonote | LSDB Archive [Life Science Database Archive metadata

    Lifescience Database Archive (English)

    Full Text Available 908/lsdba.nbdc01324-008 Description of data contents Detailed information regarding sample preparations comm...ed to by S (Sample information). Data file File name: metabolonote_sample_preparation..._details.zip File URL: ftp://ftp.biosciencedbc.jp/archive/metabolonote/LATEST/metabolonote_sample_preparation..._details.zip File size: 13 KB Simple search URL http://togodb.biosciencedbc.jp/togodb/view/metabolonote_sample_preparation... Preparation ID are merged into ID in the Simple search.) Sample Preparation ID The sample preparation detai

  16. Preparation and Characterization of Organic-Inorganic Hybrid Hydrogel Electrolyte Using Alkaline Solution

    Directory of Open Access Journals (Sweden)

    Masanobu Chiku

    2011-09-01

    Full Text Available Organic-inorganic hybrid hydrogel electrolytes were prepared by mixing hydrotalcite, cross-linked potassium poly(acrylate and 6 M KOH solution. The organic-inorganic hybrid hydrogel electrolytes had high ionic conductivity (0.456–0.540 S cm−1 at 30 °C. Moreover, the mechanical strength of the hydrogel electrolytes was high enough to form a 2–3 mm thick freestanding membrane because of the reinforcement with hydrotalcite.

  17. Preparation and properties of a POSS-containing organic-inorganic hybrid crosslinked polymer

    Institute of Scientific and Technical Information of China (English)

    Wang Yan Nie; Gang Li; Yang Li; Hong Yao Xu

    2009-01-01

    A novel POSS-containing organic-inorganic hybrid crosslinked polymer was prepared by hydrosilylation reaction of octahydridosilsesquioxane (T8H8) with 4,4'-bis(4-allyloxybenzoyloxy)phenyl (diene A). Its structure and property was character-ized by FTIR, 29Si NMR, TGA and ellipsometer, respectively. The results show that the hybrid polymer possesses high thermal stability and low dielectric constant of 1.97 at optical frequencies.

  18. Preparation and characterization of UV-cured hybrid polyvinyl alcohol nanofiber membranes by electrospinning

    OpenAIRE

    2014-01-01

    The present study investigated the possibility of preparing polyvinyl alcoholic (PVA) organic-inorganic hybrid nanofiber membranes by electrospinning with UV irradiation. To this end, PVA, PVA/SiO2 organic-inorganic hybrid obtained with Geniosil® XL 33 as a SiO2 source, and imidazole-functionalized mesoporous PVA/SiO2/N=N nanofiber membranes were synthesized. These membranes were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differen...

  19. On sample preparation and dielectric breakdown in nanostructured epoxy resins

    Energy Technology Data Exchange (ETDEWEB)

    Reading, M; Xu, Z; Lewin, P L; Vaughan, A S, E-mail: asv@ecs.soton.ac.uk [Tony Davies High Voltage Laboratory, University of Southampton (United Kingdom)

    2011-08-12

    There are many methods available to achieve a good dispersion of fillers within a polymeric matrix. This investigation considered several methods of dispersing three chosen fillers within an epoxy resin; the same processes were also performed on unfilled materials to investigate any effects they may have on the host material. For this investigation, the epoxy system (EP) was combined with sodium montmorillonite (MMT), micrometric silicon dioxide (SD) or nanometric silicon dioxide (NSD) as fillers. The effect of the different sample preparation routes on breakdown behaviour was then evaluated. While more thorough mixing protocols were found to lead to improved breakdown behaviour in the case of the various filled systems, surprisingly, an entirely equivalent form of behaviour was also seen in the unfilled epoxy. The influence of changes in sample geometry on the breakdown strength was established.

  20. Closer to the native state. Critical evaluation of cryo-techniques for Transmission Electron Microscopy: preparation of biological samples.

    Science.gov (United States)

    Mielanczyk, Lukasz; Matysiak, Natalia; Michalski, Marek; Buldak, Rafal; Wojnicz, Romuald

    2014-01-01

    Over the years Transmission Electron Microscopy (TEM) has evolved into a powerful technique for the structural analysis of cells and tissues at various levels of resolution. However, optimal sample preservation is required to achieve results consistent with reality. During the last few decades, conventional preparation methods have provided most of the knowledge about the ultrastructure of organelles, cells and tissues. Nevertheless, some artefacts can be introduced at all stagesofstandard electron microscopy preparation technique. Instead, rapid freezing techniques preserve biological specimens as close as possible to the native state. Our review focuses on different cryo-preparation approaches, starting from vitrification methods dependent on sample size. Afterwards, we discuss Cryo-Electron Microscopy Of VItreous Sections (CEMOVIS) and the main difficulties associated with this technique. Cryo-Focused Ion Beam (cryo-FIB) is described as a potential alternative for CEMOVIS. Another post-processing route for vitrified samples is freeze substitution and embedding in resin for structural analysis or immunolocalization analysis. Cryo-sectioning according to Tokuyasu is a technique dedicated to high efficiency immunogold labelling. Finally, we introduce hybrid techniques, which combine advantages of primary techniques originally dedicated to different approaches. Hybrid approaches permit to perform the study of difficult-to-fix samples and antigens or help optimize the sample preparation protocol for the integrated Laser and Electron Microscopy (iLEM) technique.

  1. Preparation and applications of hybrid organic-inorganic monoliths: a review.

    Science.gov (United States)

    Zhu, Tao; Row, Kyung Ho

    2012-06-01

    This review presents an overview of the properties of hybrid organic-inorganic monolithic materials and summarizes the recent developments in the preparation and applications of these hybrid monolithic materials. Hybrid monolithic materials with porosities, surface functionalities, and fast dynamic transport have developed rapidly, and have been used in a wide range of applications owing to the low cost, good stability, and excellent performance. Basically, these materials can be divided into two major types according to the chemical composition: hybrid silica-based monolith (HSM) and hybrid polymer-based monolith (HPM). Compared to the HPM, HSM monolith has been attracting most wide attentions, and it is commonly synthesized by the sol-gel process. The conventional preparation procedures of two type's hybrid organic-inorganic monoliths are addressed. Applications of hybrid organic-inorganic monoliths in optical devices, capillary microextraction (CME), capillary electrochromatography (CEC), high performance liquid chromatography (HPLC), and chiral separation are also reviewed. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Preparation of tissue samples for X-ray fluorescence microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Chwiej, Joanna [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland)]. E-mail: jchwiej@novell.ftj.agh.edu.pl; Szczerbowska-Boruchowska, Magdalena [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Lankosz, Marek [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Wojcik, Slawomir [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Falkenberg, Gerald [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron, Notkestr. 85, Hamburg (Germany); Stegowski, Zdzislaw [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Setkowicz, Zuzanna [Department of Neuroanatomy, Institute of Zoology, Jagiellonian University, Ingardena 6, 30-060 Cracow (Poland)

    2005-12-15

    As is well-known, trace elements, especially metals, play an important role in the pathogenesis of many disorders. The topographic and quantitative elemental analysis of pathologically changed tissues may shed some new light on processes leading to the degeneration of cells in the case of selected diseases. An ideal and powerful tool for such purpose is the Synchrotron Microbeam X-ray Fluorescence technique. It enables the carrying out of investigations of the elemental composition of tissues even at the single cell level. The tissue samples for histopathological investigations are routinely fixed and embedded in paraffin. The authors try to verify the usefulness of such prepared tissue sections for elemental analysis with the use of X-ray fluorescence microscopy. Studies were performed on rat brain samples. Changes in elemental composition caused by fixation in formalin or paraformaldehyde and embedding in paraffin were examined. Measurements were carried out at the bending magnet beamline L of the Hamburger Synchrotronstrahlungslabor HASYLAB in Hamburg. The decrease in mass per unit area of K, Br and the increase in P, S, Fe, Cu and Zn in the tissue were observed as a result of the fixation. For the samples embedded in paraffin, a lower level of most elements was observed. Additionally, for these samples, changes in the composition of some elements were not uniform for different analyzed areas of rat brain.

  3. Chitosan-nanosilica hybrid materials: Preparation and properties

    Energy Technology Data Exchange (ETDEWEB)

    Podust, T.V., E-mail: tania_list@yahoo.com [Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kyiv 03164 (Ukraine); Kulik, T.V., E-mail: tanyakulyk@i.ua [Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kyiv 03164 (Ukraine); Palyanytsya, B.B.; Gun’ko, V.M. [Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kyiv 03164 (Ukraine); Tóth, A. [Department of Physical Chemistry and Material Science, Budapest University of Technology and Economics, H-1521 Budapest (Hungary); Mikhalovska, L. [School of Pharmacy and Biomolecular Sciences, University of Brighton, Lewes Road, Brighton BN2 4GJ (United Kingdom); Menyhárd, A. [Department of Physical Chemistry and Material Science, Budapest University of Technology and Economics, H-1521 Budapest (Hungary); Institute of Materials Science and Environmental Chemistry, Research Centre for Natural Sciences, Hungarian Academy of Sciences (Hungary); László, K. [Department of Physical Chemistry and Material Science, Budapest University of Technology and Economics, H-1521 Budapest (Hungary)

    2014-11-30

    Highlights: • Hybrid chitosan-nanosilica materials were synthesized using an adsorption modification method. • The chitosan adsorption capacity is higher on the silica/titania and silica/alumina than on the fumed silica. • Nanosilicas undergo structural and textural alterations due to modification by chitosan. • The more severe chitosan thermodestruction occurs on the silica/titania and silica/alumina surfaces than on the plain silica surface. - Abstract: The research focuses on the synthesis of novel organic–inorganic hybrid materials based on polysaccharide chitosan and nanosilicas (SiO{sub 2}, TiO{sub 2}/SiO{sub 2} and Al{sub 2}O{sub 3}/SiO{sub 2}). The chitosan modified nanooxides were obtained by the equilibrium adsorption method. The chitosan adsorption capacities of silica/titania and silica/alumina are higher than of the plain silica due to the additional active sites present on the surfaces of the mixed oxides. The hybrid materials were characterized by low-temperature nitrogen adsorption/desorption, photon correlation spectroscopy (PCS), scanning electron microscopy (SEM), thermogravimetry (TG/DTG) and temperature-programmed desorption with mass spectrometry control (TPD MS) methods. The chitosan treatment only modestly influences the surface area S{sub BET} of the nanooxides but the rearrangement of the secondary and tertiary structures (aggregates and agglomerates) results in an enhancement of the mesoporosity and affects the size of the aggregates. The more severe thermodestruction of the polysaccharide desorbing from the modified mixed silicas indicates a stronger interaction between the chitosan and the mixed oxides compared to the silanol groups of the plain silica surface.

  4. Biologic effect of a hybrid preparation of human chorionic gonadotropin in human subjects.

    Science.gov (United States)

    Rosemberg, E

    1982-01-01

    Alpha and beta-hCG subunits were recombined generating a hybrid hCG preparation (AB1ER-CR-2XY) which met the required specifications of a pharmaceutical product. The biologic activity contained in each vial of AB1ER-CR-2XY was equivalent to 10 000IU of hCG-IS. This preparation was given as a single dose of 10 000IU by the i.m. route to four female subjects presenting unexplained infertility. The hCG hybrid was demonstrated to effect gonadal stimulation in humans.

  5. Chitosan-nanosilica hybrid materials: Preparation and properties

    Science.gov (United States)

    Podust, T. V.; Kulik, T. V.; Palyanytsya, B. B.; Gun'ko, V. M.; Tóth, A.; Mikhalovska, L.; Menyhárd, A.; László, K.

    2014-11-01

    The research focuses on the synthesis of novel organic-inorganic hybrid materials based on polysaccharide chitosan and nanosilicas (SiO2, TiO2/SiO2 and Al2O3/SiO2). The chitosan modified nanooxides were obtained by the equilibrium adsorption method. The chitosan adsorption capacities of silica/titania and silica/alumina are higher than of the plain silica due to the additional active sites present on the surfaces of the mixed oxides. The hybrid materials were characterized by low-temperature nitrogen adsorption/desorption, photon correlation spectroscopy (PCS), scanning electron microscopy (SEM), thermogravimetry (TG/DTG) and temperature-programmed desorption with mass spectrometry control (TPD MS) methods. The chitosan treatment only modestly influences the surface area SBET of the nanooxides but the rearrangement of the secondary and tertiary structures (aggregates and agglomerates) results in an enhancement of the mesoporosity and affects the size of the aggregates. The more severe thermodestruction of the polysaccharide desorbing from the modified mixed silicas indicates a stronger interaction between the chitosan and the mixed oxides compared to the silanol groups of the plain silica surface.

  6. Preparation of zeolite-A/chitosan hybrid composites and their bioactivities and antimicrobial activities

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Liang; Gong, Jie [State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China); Zeng, Changfeng [College of Mechanic and Power Engineering, Nanjing University of Technology, Nanjing 210009 (China); Zhang, Lixiong, E-mail: lixiongzhang@yahoo.com [State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China)

    2013-10-15

    Zeolite-A/chitosan hybrid composites with zeolite contents of 20–55 wt.% were prepared by in situ transformation of silica/chitosan mixtures in a sodium aluminate alkaline solution through impregnation–gelation–hydrothermal synthesis. The products were characterized by X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, thermogravimetric analysis, and mercury penetration porosimetry. Their in vitro bioactivities were examined using as-synthesized and Ca{sup 2+}-exchanged hybrid composites in simulated body fluid (SBF) for hydroxyapatite (HAP) growth. Their antimicrobial activities for Escherichia coli (E. coli) in trypticase soy broth (TSB) were evaluated using Ag{sup +}-exchanged hybrid composites. The zeolite-A/chitosan hybrid composites could be prepared as various shapes, including cylinders, plates and thin films. They possessed macropores with pore sizes ranging from 100 to 300 μm and showed compressive mechanical strength as high as 3.2 MPa when the zeolite content was 35 wt.%. Fast growth on the Ca{sup 2+}-exchanged hybrid composites was observed with the highest weight gain of 51.4% in 30 days. The 35 wt.% Ag{sup +}-exchanged hybrid composite showed the highest antimicrobial activity, which could reduce the 9 × 10{sup 6} CFU mL{sup −1}E. coli concentration to zero within 4 h of incubation time with the Ag{sup +}-exchanged hybrid composite amount of 0.4 g L{sup −1}. The bioactivity and antimicrobial activity could be combined by ion-exchanging the composites first with Ca{sup 2+} and then with Ag{sup +}. These zeolite-A/chitosan hybrid composites have potential applications on tissue engineering and antimicrobial food packaging. - Graphical abstract: Zeolite A/chitosan hybrid composites were prepared by in situ transformation of precursors in the chitosan matrix, which possess macroporous structures and exhibit superior bioactivity and antimicrobial activity and potential biomedical

  7. Sample preparation strategies for food and biological samples prior to nanoparticle detection and imaging

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Löschner, Katrin

    2014-01-01

    fractionation (AFFF, or AF4) coupled on-line to various detectors including static and dynamic light scattering (LS), UV or fluorescence (FL) spectroscopies and ICP-MS have proven useful and powerful [1, 2, 3]. Furthermore, additional information obtained by an imaging method such as transmission electron...... microscopy (TEM) proved to be necessary for trouble shooting of results obtained from AFFF-LS-ICP-MS. Aqueous and enzymatic extraction strategies were tested for thorough sample preparation aiming at degrading the sample matrix and to liberate the AgNPs from chicken meat into liquid suspension. The resulting...

  8. Preparation of an imogolite/poly(acrylic acid) hybrid gel.

    Science.gov (United States)

    Lee, Hoik; Ryu, Jungju; Kim, Donghyun; Joo, Yongho; Lee, Sang Uck; Sohn, Daewon

    2013-09-15

    Many efforts in the field of hydrogels have been focused toward increasing the mechanical strength of the gel using inorganic materials. In this study, we synthesized a hydrogel that has excellent mechanical properties using surface-modified inorganic nanofibers composed of imogolite (Al2SiO3(OH)4), which is a hydrated aluminum silicate that has a hollow tube structure. Gamma ray radiation generates peroxide radicals on the nanofibers (imogolite), resulting in an additive free hybrid hydrogel. Structural optimization was carried out by changing the composition of imogolite and poly(acrylic acid). Chemical bonding between the nanofiber and the polymer was simulated by a cluster model and characterized by wide area Raman spectroscopy. The results indicate that imogolite embedded in a polymer matrix can align along the direction of an elongational force, as confirmed by small angle X-ray scattering (SAXS).

  9. Facile preparation of hybrid core-shell nanorods for photothermal and radiation combined therapy

    Science.gov (United States)

    Deng, Yaoyao; Li, Erdong; Cheng, Xiaju; Zhu, Jing; Lu, Shuanglong; Ge, Cuicui; Gu, Hongwei; Pan, Yue

    2016-02-01

    The hybrid platinum@iron oxide core-shell nanorods with high biocompatibility were synthesized and applied for combined therapy. These hybrid nanorods exhibit a good photothermal effect on cancer cells upon irradiation with a NIR laser. Furthermore, due to the presence of a high atomic number element (platinum core), the hybrid nanorods show a synergistic effect between photothermal and radiation therapy. Therefore, the as-prepared core-shell nanorods could play an important role in facilitating synergistic therapy between photothermal and radiation therapy to achieve better therapeutic efficacy.The hybrid platinum@iron oxide core-shell nanorods with high biocompatibility were synthesized and applied for combined therapy. These hybrid nanorods exhibit a good photothermal effect on cancer cells upon irradiation with a NIR laser. Furthermore, due to the presence of a high atomic number element (platinum core), the hybrid nanorods show a synergistic effect between photothermal and radiation therapy. Therefore, the as-prepared core-shell nanorods could play an important role in facilitating synergistic therapy between photothermal and radiation therapy to achieve better therapeutic efficacy. Electronic supplementary information (ESI) available: Details of general experimental procedures. See DOI: 10.1039/c5nr09102k

  10. Shear-bond-strength of orthodontic brackets to aged nano-hybrid composite-resin surfaces using different surface preparation.

    Science.gov (United States)

    Demirtas, Hatice Kubra; Akin, Mehmet; Ileri, Zehra; Basciftci, Faruk Ayhan

    2015-01-01

    The aim of this study was to evaluate the effects of different surface preparation methods on the shear bond strength (SBS) of orthodontic metal brackets to aged nano-hybrid resin composite surfaces in vitro. A total of 100 restorative composite resin discs, 6 mm in diameter and 3 mm thick, were obtained and treated with an ageing procedure. After ageing, the samples were randomly divided as follows according to surface preparation methods: (1)Control, (2)37% phosphoric acid gel, (3)Sandblasting, (4)Diamond bur, (5)Air-flow and 20 central incisor teeth were used for the control etched group. SBS test were applied on bonded metal brackets to all samples. SBS values and residual adhesives were evaluated. Analysis of variance showed a significant difference (phybrid composite resin surfaces.

  11. Preparation, characterisation, engine performance and emission characteristics of coconut oil based hybrid fuels

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Pranil J.; Singh, Anirudh [Division of Physics, School of Engineering and Physics, Faculty of Science, Technology and Environment, University of the South Pacific, 325 Fletcher Road, Suva (Fiji); Khurma, Jagjit [Division of Chemistry, School of Biological, Chemical and Environmental Sciences, Faculty of Science, Technology and Environment, University of the South Pacific, Suva (Fiji)

    2010-09-15

    In this study, hybrid fuels consisting of coconut oil, aqueous ethanol and a surfactant (butan-1-ol) were prepared and tested as a fuel in a direct injection diesel engine. After determining fuel properties such as the density, viscosity and gross calorific values of these fuels, they were used to run a diesel engine. The engine performance and exhaust emissions were investigated and compared with that of diesel. The experimental results show that the efficiency of the hybrid fuels is comparable to that of diesel. As the viscosity of the hybrid fuels decreased and approached that of diesel, the efficiency increased progressively towards that of diesel. The exhaust emissions were lower than those for diesel, except carbon monoxide emissions, which increased. Hence, it is concluded that these hybrid fuels can be used successfully as an alternative fuel in diesel engines without any modifications. Their completely renewable nature ensures that they are environmentally friendly with regard to their emissions characteristics. (author)

  12. Preparation of stable food-grade double emulsions with a hybrid premix membrane emulsification system

    NARCIS (Netherlands)

    Eisinaite, Viktorija; Juraite, Dovile; Schroën, Karin; Leskauskaite, Daiva

    2016-01-01

    In this study we demonstrate that food-grade double emulsions can be successfully prepared using a hybrid premix emulsification system. A coarse emulsion containing beetroot juice as inner water phase, sunflower oil as oil phase and 0.5% or 1.0% whey protein isolate solution as outer water phase

  13. Structure of hybrid organic-inorganic sols for the preparation of hydrothermally stable membranes

    NARCIS (Netherlands)

    Castricum, H.L.; Sah, A.; Geenevasen, J.A.J.; Kreiter, R.; Blank, D.H.A.; Vente, J.F.; ten Elshof, J.E.

    2008-01-01

    A procedure for the preparation of hybrid sols for the synthesis of organic-inorganic microporous materials and thin film membranes is reported. We describe silane reactivity and sol structure for acid-catalysed colloidal sols from mixtures of either tetraethylorthosilicate (TEOS) and methyltriethox

  14. Preparation and characterization of cellulose acetate organic/inorganic hybrid films

    Science.gov (United States)

    Saeed S. Shojaie; Timothy G. Rials; Stephen S. Kelley

    1995-01-01

    A series of organic/inorganic hybrid (OIH) films were prepared using cellulose acetate (CA) as the organic component and tetraethyl orthosilicate (TEOS) as the inorganic component. The chemical, morphological, and mechanical properties of these films were evaluated with a variety of analytical techniques. The results of these evaluations showed that crosslinked CA OIH...

  15. Preparation and Characterization of Hybrid Luminescence Mesoporous MCM-48 Doped with Eu( Ⅲ ) Complex

    Institute of Scientific and Technical Information of China (English)

    Meng Qingguo; Li Huanrong; Peng Chunyun; Zhang Hongjie; Boutinaud P; Franville A C; Mahiou R

    2004-01-01

    The preparation of hybrid mesoporous MCM-48 grafted by vinyl group via post-grafting process was reported and studied by X-ray diffraction, BET and 29Si solid MAS NMR.An organic β-diketonate Europium complex the corresponding luminescence property was characterized.

  16. Metal nanoparticle deposited inorganic nanostructure hybrids, uses thereof and processes for their preparation

    Science.gov (United States)

    Tenne, Reshef; Tsverin, Yulia; Burghaus, Uwe; Komarneni, Mallikharjuna Rao

    2016-01-26

    This invention relates to a hybrid component comprising at least one nanoparticle of inorganic layered compound (in the form of fullerene-like structure or nanotube), and at least one metal nanoparticle, uses thereof as a catalyst, (e.g. photocatalysis) and processes for its preparation.

  17. Effect of sample preparation on charged impurities in graphene substrates

    Science.gov (United States)

    Burson, K. M.; Dean, C. R.; Watanabe, K.; Taniguchi, T.; Hone, J.; Kim, P.; Cullen, W. G.; Fuhrer, M. S.

    2013-03-01

    The mobility of graphene as fabricated on SiO2 has been found to vary widely depending on sample preparation conditions. Additionally, graphene mobility on SiO2 appears to be limited to ~20,000 cm2/Vs, likely due to charged impurities in the substrate. Here we present a study of the effect of fabrication procedures on substrate charged impurity density (nimp) utilizing ultrahigh-vacuum Kelvin probe force microscopy. We conclude that even minimal SEM exposure, as from e-beam lithography, induces an increased impurity density, while heating reduces the number of charges for sample substrates which already exhibit a higher impurity density. We measure both SiO2 and h-BN and find that all nimp values observed for SiO2 are higher than those observed for h-BN; this is consistent with the observed improvement in mobility for graphene devices fabricated on h-BN over those fabricated on SiO2 substrates. This work was supported by the US ONR MURI program, and the University of Maryland NSF-MRSEC under Grant No. DMR 05-20471.

  18. Miniaturized sample preparation method for determination of amphetamines in urine.

    Science.gov (United States)

    Nishida, Manami; Namera, Akira; Yashiki, Mikio; Kimura, Kojiro

    2004-07-16

    A simple and miniaturized sample preparation method for determination of amphetamines in urine was developed using on-column derivatization and gas chromatography-mass spectrometry (GC-MS). Urine was directly applied to the extraction column that was pre-packed with Extrelut and sodium carbonate. Amphetamine (AP) and methamphetamine (MA) in urine were adsorbed on the surface of Extrelut. AP and MA were then converted to a free base and derivatized to N-propoxycarbonyl derivatives using propylchloroformate on the column. Pentadeuterated MA was used as an internal standard. The recoveries of AP and MA from urine were 100 and 102%, respectively. The calibration curves showed linearity in the range of 0.50-50 microg/mL for AP and MA in urine. When urine samples containing two different concentrations (0.50 and 5.0 microg/mL) of AP and MA were determined, the intra-day and inter-day coefficients of variation were 1.4-7.7%. This method was applied to 14 medico-legal cases of MA intoxication. The results were compared and a good agreement was obtained with a HPLC method.

  19. Ultrasound: a subexploited tool for sample preparation in metabolomics.

    Science.gov (United States)

    Luque de Castro, M D; Delgado-Povedano, M M

    2014-01-02

    Metabolomics, one of the most recently emerged "omics", has taken advantage of ultrasound (US) to improve sample preparation (SP) steps. The metabolomics-US assisted SP step binomial has experienced a dissimilar development that has depended on the area (vegetal or animal) and the SP step. Thus, vegetal metabolomics and US assisted leaching has received the greater attention (encompassing subdisciplines such as metallomics, xenometabolomics and, mainly, lipidomics), but also liquid-liquid extraction and (bio)chemical reactions in metabolomics have taken advantage of US energy. Also clinical and animal samples have benefited from US assisted SP in metabolomics studies but in a lesser extension. The main effects of US have been shortening of the time required for the given step, and/or increase of its efficiency or availability for automation; nevertheless, attention paid to potential degradation caused by US has been scant or nil. Achievements and weak points of the metabolomics-US assisted SP step binomial are discussed and possible solutions to the present shortcomings are exposed. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Automated acoustic matrix deposition for MALDI sample preparation.

    Science.gov (United States)

    Aerni, Hans-Rudolf; Cornett, Dale S; Caprioli, Richard M

    2006-02-01

    Novel high-throughput sample preparation strategies for MALDI imaging mass spectrometry (IMS) and profiling are presented. An acoustic reagent multispotter was developed to provide improved reproducibility for depositing matrix onto a sample surface, for example, such as a tissue section. The unique design of the acoustic droplet ejector and its optimization for depositing matrix solution are discussed. Since it does not contain a capillary or nozzle for fluid ejection, issues with clogging of these orifices are avoided. Automated matrix deposition provides better control of conditions affecting protein extraction and matrix crystallization with the ability to deposit matrix accurately onto small surface features. For tissue sections, matrix spots of 180-200 microm in diameter were obtained and a procedure is described for generating coordinate files readable by a mass spectrometer to permit automated profile acquisition. Mass spectral quality and reproducibility was found to be better than that obtained with manual pipet spotting. The instrument can also deposit matrix spots in a dense array pattern so that, after analysis in a mass spectrometer, two-dimensional ion images may be constructed. Example ion images from a mouse brain are presented.

  1. Effect of probiotic preparation for chemical composition of meat cocks different combinations of hybrid chicks

    Directory of Open Access Journals (Sweden)

    Peter Haščík

    2011-01-01

    Full Text Available In the experiment were verified the application of probiotic preparation through a water supply for feeding of cock’s hybrids Ross 308, Hubbard JV and Cobb 500 in the chemical composition of the most valuable parts of the carcass. Probiotic was based on the strain Lactobacillus fermentum with containing of 1.109 cfu.g−1 and potentially components of maltodextrin and oligofructose in 1% concentration. Length of feeding period was 42 days. Cocks were fed an ad libitum with the same starter mixture HYD-01 to 21th day and from 22nd to 42nd day of feeding with mixture HYD-02 in powdery form. The average of protein content of breast muscle was highest in Hubbard JV hybrid (23.93 g.100 g−1, lower in Cobb 500 hybrid (23.90 g.100 g−1 and lowest in Ross 308 hybrid (23.73 g.100 g−1, without significant differences (P ≥ 0.05 between hybrids and hybrids groups. Effect of probiotics had increased the protein content (P ≥ 0.05 in breast muscle of Ross 308 and Cobb 500 cocks and at the Hubbard JV only lower doses application during the feeding. The average of fat content in 100 g of breast muscle was lowest in Cobb 500 hybrid (1.09 g, higher in Hubbard JV hybrid (1.28 g and highest in Ross 308 hybrid (1.35 g. Effect of probiotic to reduce fat content in breast muscle of cocks was at Ross 308 hybrid (1.33 and 1.23 g.100 g−1, Cobb 500 hybrid (0.98 and 1.02 g.100 g−1 and in second experimental group at Hubbard JV hybrid (1.03 g.100 g−1 statistically significant (P ≥ 0.05 in compared with control group, but significantly (P ≤ 0.05 between hybrids Cobb 500 and Hubbard JV in the first test groups. The average of energy value in 100 g of breast muscle was highest in Hubbard JV hybrid (449.24 kJ, lower in Ross 308 hybrid (448.40 kJ and lowest in Cobb 500 hybrid (441.45 kJ, without significant differences (P ≥ 0.05 between hybrids and hybrids groups. The average of protein content of the femur was highest in Ross 308 hybrid (18.56 g.100

  2. DIELECTRIC PROPERTIES OF STRAINED ICE. II : EFFECT OF SAMPLE PREPARATION METHOD

    OpenAIRE

    Itagaki, K.; Lemieux, G.

    1987-01-01

    Since most commonly used sample preparation methods for ice dielectric studies involve rather heavy mechanical straining, the effects of straining were studied and compared with more strain-free sample preparation methods.

  3. Polymer/Carbon-Based Hybrid Aerogels: Preparation, Properties and Applications

    Directory of Open Access Journals (Sweden)

    Lizeng Zuo

    2015-10-01

    Full Text Available Aerogels are synthetic porous materials derived from sol-gel materials in which the liquid component has been replaced with gas to leave intact solid nanostructures without pore collapse. Recently, aerogels based on natural or synthetic polymers, called polymer or organic aerogels, have been widely explored due to their porous structures and unique properties, such as high specific surface area, low density, low thermal conductivity and dielectric constant. This paper gives a comprehensive review about the most recent progresses in preparation, structures and properties of polymer and their derived carbon-based aerogels, as well as their potential applications in various fields including energy storage, adsorption, thermal insulation and flame retardancy. To facilitate further research and development, the technical challenges are discussed, and several future research directions are also suggested in this review.

  4. Preparation of a Novel Coal Gangue-Polyacrylamide Hybrid Flocculant and Its Flocculation Performance

    Institute of Scientific and Technical Information of China (English)

    Xiangao Quan; Huiyun Wang

    2014-01-01

    A novel flocculant based on hybrid coal gangue-polyacrylamide (HCGPAM) has been prepared by using modified coal gangue and polyacrylamide. Factors related to the preparation such as reaction time, temperature, concentration of the polymer monomer and ratio of initiators are investigated. The product is characterized by infrared spectra (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD), aswell as viscometry. The flocculating tests on oilfield drilling wastewater show that the removal efficiency is 85.5% and the light transmittance is 53.6%. The results indicate that the coal gangue could be used for the preparation of inorganic-organic hybrid flocculant and the removal efficiency is much higher than that of commercial polyacrylamide (PAM) or PAM/ coal gangue blend.

  5. One-pot preparation of mercaptotetrazole-silica hybrid monoliths by the thiol-ene click reaction for mixed-mode capillary liquid chromatography.

    Science.gov (United States)

    Wang, Haojiang; Hu, Wenli; Zheng, Qiong; Bian, Wei; Lin, Zian

    2017-06-01

    A novel mercaptotetrazole-silica hybrid monolithic column was prepared for capillary liquid chromatography, in which the thiol-end mercaptotetrazole was mixed with hydrolyzed γ-methacryloxypropyltrimethoxysilane and tetramethyloxysilane for the co-polycondensation and thiol-ene click reaction in a one-pot process. The effects of the molar ratio of silanes, the amount of mercaptotetrazole, and the volume of porogen on the morphology, permeability and pore properties of the as-prepared mercaptotetrazole-silica hybrid monoliths were investigated in detail. A series of test compounds including alkylbenzenes, amides and anilines were employed for evaluating the retention behaviors of the mercaptotetrazole-silica hybrid monolithic columns. The results demonstrated that the mercaptotetrazole-silica hybrid monoliths exhibited hydrophobic, hydrophilic as well as ion-exchange interaction. The run-to-run, column-to-column and batch-to-batch reproducibilities of the mercaptotetrazole-silica hybrid monoliths were satisfactory with the relative standard deviations less than 1.4 (n = 5), 3.9 (n = 3) and 4.0% (n = 5), respectively. In addition, the mercaptotetrazole-silica hybrid monolith was further applied to the separation of sulfonamides, nucleobases and protein tryptic digests. These successful applications confirmed the promising potential of the mercaptotetrazole-silica hybrid monolith in the separation of complex samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Hybrid nested sampling algorithm for Bayesian model selection applied to inverse subsurface flow problems

    Energy Technology Data Exchange (ETDEWEB)

    Elsheikh, Ahmed H., E-mail: aelsheikh@ices.utexas.edu [Institute for Computational Engineering and Sciences (ICES), University of Texas at Austin, TX (United States); Institute of Petroleum Engineering, Heriot-Watt University, Edinburgh EH14 4AS (United Kingdom); Wheeler, Mary F. [Institute for Computational Engineering and Sciences (ICES), University of Texas at Austin, TX (United States); Hoteit, Ibrahim [Department of Earth Sciences and Engineering, King Abdullah University of Science and Technology (KAUST), Thuwal (Saudi Arabia)

    2014-02-01

    A Hybrid Nested Sampling (HNS) algorithm is proposed for efficient Bayesian model calibration and prior model selection. The proposed algorithm combines, Nested Sampling (NS) algorithm, Hybrid Monte Carlo (HMC) sampling and gradient estimation using Stochastic Ensemble Method (SEM). NS is an efficient sampling algorithm that can be used for Bayesian calibration and estimating the Bayesian evidence for prior model selection. Nested sampling has the advantage of computational feasibility. Within the nested sampling algorithm, a constrained sampling step is performed. For this step, we utilize HMC to reduce the correlation between successive sampled states. HMC relies on the gradient of the logarithm of the posterior distribution, which we estimate using a stochastic ensemble method based on an ensemble of directional derivatives. SEM only requires forward model runs and the simulator is then used as a black box and no adjoint code is needed. The developed HNS algorithm is successfully applied for Bayesian calibration and prior model selection of several nonlinear subsurface flow problems.

  7. Fluoroscence in situ hybridization of chicken intestinal samples with bacterial rRNA targeted oligonucleotide probes

    DEFF Research Database (Denmark)

    Olsen, Katja Nyholm; Francesch, M.; Christensen, Henrik

    2006-01-01

    The objective was to develop a fast and accurate molecular method for the quantification of the intestinal flora in chickens by rRNA fluorescence in situ hybridization (FISH). Seven weeks old conventionally reared Lohmann hens were used to set up the method. To sample ileal intestinal content......, the distal part from Meckels diverticulum to the ileo-caecal junction was removed. Fixation was performed in ethanol and phosphate buffered saline. After washing by centrifugation, the sample was resuspended in pre-heated hybridization buffer with oligonucleotide probe labelled with Cy3 (10ng/µl). The cells...... were hybridized for 24-72h, centrifuged, washed with pre-heated hybridization buffer, centrifuged and resuspended in Millipore quality water before filtration onto a 0.22 µm black polycarbonate filter. The probes used in this study were, LGC354A, LGC354B, LGC354C, Strc493, Bacto1080, Sal3, Chis150, EUB...

  8. The Electrochemical Characteristics of Hybrid Capacitor Prepared by Chemical Activation of NaOH

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Jeong Eun; Bae, Ga Yeong; Yang, Jeong Min; Lee, Jong Dae [Chungbuk National Univ., Chungju (Korea, Republic of)

    2013-06-15

    Active carbons with high specific surface area and micro pore structure were prepared from the coconut shell char using the chemical activation method of NaOH. The preparation process has been optimized through the analysis of experimental variables such as activating chemical agents to char ratio and the flow rate of gas during carbonization. The active carbons with the surface area (2,481m{sup 2}/g) and mean pore size (2.32 nm) were obtained by chemical activation with NaOH. The electrochemical performances of hybrid capacitor were investigated using LiMn{sub 2}O{sub 4}, LiCoO{sub 2} as the positive electrode and prepared active carbon as the negative electrode. The electrochemical behaviors of hybrid capacitor using organic electrolytes (LiPF{sub 6}, TEABF{sub 4}) were characterized by constant current charge/discharge, cyclic voltammetry, cycle and leakage tests. The hybrid capacitor using LiMn{sub 2}O{sub 4}/AC electrodes had better capacitance than other hybrid systems and was able to deliver a specific energy as high as 131 Wh/kg at a specific power of 1,448 W/kg.

  9. Sample preparation issues in NMR-based plant metabolomics: optimisation for Vitis wood samples.

    Science.gov (United States)

    Halabalaki, Maria; Bertrand, Samuel; Stefanou, Anna; Gindro, Katia; Kostidis, Sarantos; Mikros, Emmanuel; Skaltsounis, Leandros A; Wolfender, Jean-Luc

    2014-01-01

    Nuclear magnetic resonance (NMR) is one of the most commonly used analytical techniques in plant metabolomics. Although this technique is very reproducible and simple to implement, sample preparation procedures have a great impact on the quality of the metabolomics data. Investigation of different sample preparation methods and establishment of an optimised protocol for untargeted NMR-based metabolomics of Vitis vinifera L. wood samples. Wood samples from two different cultivars of V. vinifera with well-defined phenotypes (Gamaret and 2091) were selected as reference materials. Different extraction solvents (successively, dichloromethane, methanol and water, as well as ethyl acetate and 7:3 methanol-water (v/v)) and deuterated solvents (methanol-d4, 7:3 chloroform-d-methanol-d4 (v/v), dimethylsulphoxide-d6 and 9:1 dimethylsulphoxide-d6-water-d2 (v/v)) were evaluated for NMR acquisition, and the spectral quality was compared. The optimal extract concentration, chemical shift stability and peak area repeatability were also investigated. Ethyl acetate was found to be the most satisfactory solvent for the extraction of all representative chemical classes of secondary metabolites in V. vinifera wood. The optimal concentration of dried extract was 10 mg/mL and 7:3 chloroform-d-methanol-d4 (v/v) was the most suitable solvent system for NMR analysis. Multivariate data analysis was used to estimate the biological variation and clustering between different cultivars. Close attention should be paid to all required procedures before NMR analysis, especially to the selection of an extraction solvent and a deuterated solvent system to perform an extensive metabolomic survey of the specific matrix. Copyright © 2014 John Wiley & Sons, Ltd.

  10. Sample Preparation Report of the Fourth OPCW Confidence Building Exercise on Biomedical Sample Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Udey, R. N. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Corzett, T. H. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Alcaraz, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2014-07-03

    Following the successful completion of the 3rd biomedical confidence building exercise (February 2013 – March 2013), which included the analysis of plasma and urine samples spiked at low ppb levels as part of the exercise scenario, another confidence building exercise was targeted to be conducted in 2014. In this 4th exercise, it was desired to focus specifically on the analysis of plasma samples. The scenario was designed as an investigation of an alleged use of chemical weapons where plasma samples were collected, as plasma has been reported to contain CWA adducts which remain present in the human body for several weeks (Solano et al. 2008). In the 3rd exercise most participants used the fluoride regeneration method to analyze for the presence of nerve agents in plasma samples. For the 4th biomedical exercise it was decided to evaluate the analysis of human plasma samples for the presence/absence of the VX adducts and aged adducts to blood proteins (e.g., VX-butyrylcholinesterase (BuChE) and aged BuChE adducts using a pepsin digest technique to yield nonapeptides; or equivalent). As the aging of VX-BuChE adducts is relatively slow (t1/2 = 77 hr at 37 °C [Aurbek et al. 2009]), soman (GD), which ages much more quickly (t1/2 = 9 min at 37 °C [Masson et al. 2010]), was used to simulate an aged VX sample. Additional objectives of this exercise included having laboratories assess novel OP-adducted plasma sample preparation techniques and analytical instrumentation methodologies, as well as refining/designating the reporting formats for these new techniques.

  11. Preparation and Characterization of Novel Electrospinnable PBT/POSS Hybrid Systems Starting from c-PBT

    Directory of Open Access Journals (Sweden)

    Lorenza Gardella

    2015-01-01

    Full Text Available Novel hybrid systems based on poly(butyleneterephthalate (PBT and polyhedral oligomeric silsesquioxanes (POSS have been prepared by applying the ring-opening polymerization of cyclic poly(butyleneterephthalate oligomers. Two types of POSS have been used: one characterized by hydroxyl functionalities (named POSS-OH and another without specific reactive groups (named oib-POSS. It was demonstrated that POSS-OH acts as an initiator for the polymerization reaction, leading to the direct insertion of the silsesquioxane into the polymer backbone. Among the possible applications of the PBT/POSS hybrid system, the possibility to obtain nanofibers has been assessed in this work.

  12. White-light emission of polyvinyl alcohol/ZnO hybrid nanofibers prepared by electrospinning

    Science.gov (United States)

    Sui, X. M.; Shao, C. L.; Liu, Y. C.

    2005-09-01

    Polyvinyl alcohol/ZnO (PVA/ZnO) hybrid nanofibers were prepared by the electrospinning technique. The structural and spectral information of the nanofibers was characterized by scanning electron microscopy, x-ray diffraction, Fourier transform infrared spectroscopy, differential scanning calorimetry, resonant Raman, and photoluminescence (PL). The results indicate that ZnO were successfully embedded in the one-dimensional hybrid fibers via chemical interactions between ZnO and PVA. PL results show the PVA/ZnO nanofibers have an intense white-light emission, which originates from the simultaneous emission of three bands covering from the UV to visible range. A possible PL mechanism was proposed accordingly.

  13. Sol-gel Process in Preparation of Organic-inorganic Hybrid Materials

    Directory of Open Access Journals (Sweden)

    Macan, J

    2008-07-01

    Full Text Available Organic-inorganic hybrid materials are a sort of nanostructured material in which the organic and inorganic phases are mixed at molecular level. The inorganic phase in hybrid materials is formed by the sol-gel process, which consists of reactions of hydrolysis and condensation of metal (usually silicon alkoxides. Flexibility of sol-gel process enables creation of hybrid materials with varying organic and inorganic phases in different ratios, and consequently fine-tuning of their properties. In order to obtain true hybrid materials, contact between the phases should be at molecular level, so phase separation between thermodynamically incompatible organic and inorganic phases has to be prevented. Phase interaction can be improved by formation of hydrogen or covalent bonds between them during preparation of hybrid materials. Covalent bond can be introduced by organically modified silicon alkoxides containing a reactive organic group (substituent capable of reacting with the organic phase. In order to obtain hybrid materials with desired structures, a detailed knowledge of hydrolysis and condensation mechanism is necessary. The choice of catalyst, whether acid or base, has the most significant influence on the structure of the inorganic phase. Other important parameters are alkoxide concentration, water: alkoxide ratio, type of alkoxide groups, solvent used, temperature, purity of chemicals used, etc. Hydrolysis and condensation of organically modified silicon alkoxides are additionally influenced by nature and size of the organic supstituent.

  14. Optimization and validation of sample preparation for metagenomic sequencing of viruses in clinical samples.

    Science.gov (United States)

    Lewandowska, Dagmara W; Zagordi, Osvaldo; Geissberger, Fabienne-Desirée; Kufner, Verena; Schmutz, Stefan; Böni, Jürg; Metzner, Karin J; Trkola, Alexandra; Huber, Michael

    2017-08-08

    Sequence-specific PCR is the most common approach for virus identification in diagnostic laboratories. However, as specific PCR only detects pre-defined targets, novel virus strains or viruses not included in routine test panels will be missed. Recently, advances in high-throughput sequencing allow for virus-sequence-independent identification of entire virus populations in clinical samples, yet standardized protocols are needed to allow broad application in clinical diagnostics. Here, we describe a comprehensive sample preparation protocol for high-throughput metagenomic virus sequencing using random amplification of total nucleic acids from clinical samples. In order to optimize metagenomic sequencing for application in virus diagnostics, we tested different enrichment and amplification procedures on plasma samples spiked with RNA and DNA viruses. A protocol including filtration, nuclease digestion, and random amplification of RNA and DNA in separate reactions provided the best results, allowing reliable recovery of viral genomes and a good correlation of the relative number of sequencing reads with the virus input. We further validated our method by sequencing a multiplexed viral pathogen reagent containing a range of human viruses from different virus families. Our method proved successful in detecting the majority of the included viruses with high read numbers and compared well to other protocols in the field validated against the same reference reagent. Our sequencing protocol does work not only with plasma but also with other clinical samples such as urine and throat swabs. The workflow for virus metagenomic sequencing that we established proved successful in detecting a variety of viruses in different clinical samples. Our protocol supplements existing virus-specific detection strategies providing opportunities to identify atypical and novel viruses commonly not accounted for in routine diagnostic panels.

  15. Preparation of supramolecular hydrogel-enzyme hybrids exhibiting biomolecule-responsive gel degradation.

    Science.gov (United States)

    Shigemitsu, Hajime; Fujisaku, Takahiro; Onogi, Shoji; Yoshii, Tatsuyuki; Ikeda, Masato; Hamachi, Itaru

    2016-09-01

    Hydrogelators are small, self-assembling molecules that form supramolecular nanofiber networks that exhibit unique dynamic properties. Development of supramolecular hydrogels that degrade in response to various biomolecules could potentially be used for applications in areas such as drug delivery and diagnostics. Here we provide a synthetic procedure for preparing redox-responsive supramolecular hydrogelators that are used to create hydrogels that degrade in response to oxidizing or reducing conditions. The synthesis takes ∼2-4 d, and it can potentially be carried out in parallel to prepare multiple hydrogelator candidates. This described solid-phase peptide synthesis protocol can be used to produce previously described hydrogelators or to construct a focused molecular library to efficiently discover and optimize new hydrogelators. In addition, we describe the preparation of redox-responsive supramolecular hydrogel-enzyme hybrids that are created by mixing aqueous solutions of hydrogelators and enzymes, which requires 2 h for completion. The resultant supramolecular hydrogel-enzyme hybrids exhibit gel degradation in response to various biomolecules, and can be rationally designed by connecting the chemical reactions of the hydrogelators with enzymatic reactions. Gel degradation in response to biomolecules as triggers occurs within a few hours. We also describe the preparation of hydrogel-enzyme hybrids arrayed on flat glass slides, enabling high-throughput analysis of biomolecules such as glucose, uric acid, lactate and so on by gel degradation, which is detectable by the naked eye. The protocol requires ∼6 h to prepare the hydrogel-enzyme hybrid array and to complete the biomolecule assay.

  16. Preparation of hybrid nano biocomposite κ-carrageenan/cellulose nanocrystal/nanoclay

    Science.gov (United States)

    Zakuwan, Siti Zarina; Ahmad, Ishak; Ramli, Nazaruddin

    2013-11-01

    Biodegradable composites film based on κ-carrageenan and nano particles as filler was prepared to study the mechanical strength of carrageenan composites. Solution casting technique was used to prepare_this biocomposite. Preparation of composite film and nano filler involve two stages, preparation of cellulose nanocrystals (CNC) from kenaf with alkali treatment, bleaching, and hydrolysis followed by the preparation of two types of nano composite. Tensile test was carried on the composite film based on κ-carrageenan with the variation percentage of CNC and nano clay to obtain the optimum CNC and nano clay loading. After that hybrid nano-biocomposite film based on κ-carrageenan with the variation percentage of CNC/nano clay (OMMT) according to optimum value of composite carrageenan/CNC and composite carrageenan/nano clay film was prepared. The effect of nano filler on the mechanical properties of carrageenan films was examined. κ-carrageenan biocomposite increased with the optimum at 4% CNC and nano clay composition. Additional improvement of tensile strength with hybridization of CNC and nanoclay indicated better mechanical properties.

  17. Reduced leakage current and improved ferroelectricity in magneto-electric composite ceramics prepared with microwave assisted radiant hybrid sintering

    Directory of Open Access Journals (Sweden)

    Sanjay Kumar Upadhyay

    2015-04-01

    Full Text Available Structural, electrical and magnetic properties of magneto-electric composite ceramics viz., 0.9 BaTi0.95Sn0.05O3 (BTSO- 0.1 Ni0.8Zn0.2Fe2O4 (NZFO prepared with microwave assisted radiant hybrid sintering (MARH are reported. Phase purity and isovalent substitution of Ti4+ by Sn4+ of the samples is confirmed from x-ray diffraction and 119Sn Mossbauer measurements respectively. Significant suppression of leakage current and improvement of ferroelectricity is observed for the composites prepared with MARH. The observed results are explained in terms of uniform dispersion of ferrite (NZFO phase in the ferroelectric (BTSO matrix as evidenced from back-scattered scanning electron micrographs.

  18. Facile preparation of TiO2-polyvinyl alcohol hybrid nanoparticles with improved visible light photocatalytic activity

    Science.gov (United States)

    Filippo, Emanuela; Carlucci, Claudia; Capodilupo, Agostina Lina; Perulli, Patrizia; Conciauro, Francesca; Corrente, Giuseppina Anna; Gigli, Giuseppe; Ciccarella, Giuseppe

    2015-03-01

    Hybrid inorganic/organic core/shell nanoparticles were prepared through a two step synthesis procedure. In the first step, pure anatase TiO2 nanoparticles were synthesized though a rapid microwave assisted non-aqueous route. Then, the obtained titania nanoparticles were coated with polyvinyl alcohol (PVA) using a simple solution method followed by relatively low temperature treatment. The PVA-coated titania nanoparticles samples were prepared at different TiO2-PVA weight ratio and they were characterized using X-Ray diffraction, transmission electron microscopy, infrared spectroscopy and Brunauer-Emmett-Teller (BET) analysis. Photocatalytic performance was also evaluated for all samples and the results indicated that TiO2:PVA weight ratio was a key factor to obtain an improvement of the photocatalytic activity with respect to bare TiO2 nanoparticles, since PVA concentration influenced the surface area and the aggregation of nanoparticles and the thickness of the coating layer. This inexpensive system provides a simple, quick and effective approach which allows to obtain core/shell hybrid nanostructures.

  19. Preparation and Photochromic Properties of Hybrid Thin Films Based on Heteropolyoxometallate and Polyacrylamide

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    series of photochromic hybrid films were prepared through entrapping Dawson type tungsten heteropolyoxometallates (P2W18O626-) and molybdenum heteropolyoxometallate (P2Mo18O626-) into polyacrylamide matrix. FTIR results showed that the Dawson geometry of heteropolyoxometallates is still preserved inside the composites and strong coulombic interaction is built between heteropolyoxometallates and polyacrylamide via hydrogen bonding. Irradiated with ultraviolet light, the transparent films change from colorless to blue and show reversible photochromism.The bleaching process occurs when the films are in contact with air or O2 in the dark. The molybdenum heteropolyoxometallate hybrid film has higher photochromic efficiency and slower bleaching reaction than tungsten heteropolyoxometallate hybrid film. ESR results indicated that polyacrylamide is a hydrogen donor and the photoreduced process is in accordance with the radical mechanism.

  20. Preparation and gas sensing properties of novel CdS-supramolecular organogel hybrid films

    Science.gov (United States)

    Xia, Huiyun; Peng, Junxia; Liu, Kaiqiang; Li, Chen; Fang, Yu

    2008-05-01

    A novel CdS-supramolecular organogel hybrid film with unusual morphology has been fabricated by exposing a supramolecular organogel film containing Cd(Ac)2 in an H2S atmosphere at room temperature. The organogel film was prepared by spin-coating a LMOG (low-molecular weight organic gelator) gel of dmethyl sulfoxide onto a glass plate substrate. XRD, SEM, EDS, TG-DTA, UV-vis, PL (photoluminescence) spectroscopy and PL lifetime measurements were employed to characterize the film. It was shown that the organogel film had functioned as a template to control the morphology of the final hybrid film. The quantities and sizes of the CdS particles embedded in the organogel films can be easily altered by varying the initial concentration of Cd(Ac)2. Importantly, the PL of the hybrid film is sensitive to the presence of some volatile organic monoamines and diamines. The selectivity and reversibility of the sensing process were investigated.

  1. Fluorescence in situ hybridization of old G-banded and mounted chromosome preparations

    DEFF Research Database (Denmark)

    Gerdes, A M; Pandis, N; Bomme, L;

    1997-01-01

    , that the amount of added probe is increased approximately 2.5 times, and that the amplification of signals is performed twice. The applicability of the method, which allows double painting with two differently labeled probes using two differently fluorescing colors, was tested on 11 cases involving different......An improved method for fluorescence in situ hybridization (FISH) investigation of old, previously G-banded, mounted chromosome preparations with chromosome specific painting probes and centromere-specific probes is described. Before hybridization, the slides are incubated in xylene until...... the coverslips detach spontaneously; any mechanical manipulation will jeopardize the results. The success of chromosome painting is improved by excluding the regular RNase treatment step prior to hybridization. Additional changes compared with standard FISH protocols are that the 2 x SSC step is omitted...

  2. Preparation and Characterization of New Geopolymer-Epoxy Resin Hybrid Mortars

    Directory of Open Access Journals (Sweden)

    Raffaele Cioffi

    2013-07-01

    Full Text Available The preparation and characterization of metakaolin-based geopolymer mortars containing an organic epoxy resin are presented here for the first time. The specimens have been prepared by means of an innovative in situ co-reticulation process, in mild conditions, of commercial epoxy based organic resins and geopolymeric slurry. In this way, geopolymer based hybrid mortars characterized by a different content of normalized sand (up to 66% in weight and by a homogeneous dispersion of the organic resin have been obtained. Once hardened, these new materials show improved compressive strength and toughness in respect to both the neat geopolymer and the hybrid pastes since the organic polymer provides a more cohesive microstructure, with a reduced amount of microcracks. The microstructural characterization allows to point out the presence of an Interfacial Transition Zone similar to that observed in cement based mortars and concretes. A correlation between microstructural features and mechanical properties has been studied too.

  3. Biotemplated preparation of CdS nanoparticles/bacterial cellulose hybrid nanofibers for photocatalysis application.

    Science.gov (United States)

    Yang, Jiazhi; Yu, Junwei; Fan, Jun; Sun, Dongping; Tang, Weihua; Yang, Xuejie

    2011-05-15

    In this work, we describe a novel facile and effective strategy to prepare micrometer-long hybrid nanofibers by deposition of CdS nanoparticles onto the substrate of hydrated bacterial cellulose nanofibers (BCF). Hexagonal phase CdS nanocrystals were achieved via a simple hydrothermal reaction between CdCl(2) and thiourea at relatively low temperature. The prepared pristine BCF and the CdS/BCF hybrid nanofibers were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), UV-vis absorption spectroscopy (UV-vis), and X-ray photoelectron spectroscopy (XPS). The results reveal that the CdS nanoparticles were homogeneously deposited on the BCF surface and stabilized via coordination effect. The CdS/BCF hybrid nanofibers demonstrated high-efficiency photocatalysis with 82% methyl orange (MO) degradation after 90 min irradiation and good recyclability. The results indicate that the CdS/BCF hybrid nanofibers are promising candidate as robust visible light responsive photocatalysts.

  4. Preparation of collagen/hydroxyapatite/alendronate hybrid hydrogels as potential scaffolds for bone regeneration.

    Science.gov (United States)

    Ma, Xin; He, Zhiwei; Han, Fengxuan; Zhong, Zhiyuan; Chen, Liang; Li, Bin

    2016-07-01

    Development of biomimetic scaffolds represents a promising direction in bone tissue engineering. In this study, we designed a two-step process to prepare a type of biomimetic hybrid hydrogels that were composed of collagen, hydroxyapatite (HAP) and alendronate (ALN), an anti-osteoporosis drug. First, water-soluble ALN-conjugated HAP (HAP-ALN) containing 4.0wt.% of ALN was synthesized by treating HAP particles with ALN. Hydrogels were then formed from HAP-ALN conjugate and collagen under physiological conditions using genipin (GNP) as the crosslinker. Depending on the ALN/collagen molar ratio and GNP concentration, the gelation time of hydrogels ranged from 5 to 37min. Notably, these hybrid hydrogels exhibited markedly improved mechanical property (storage modulus G'=38-187kPa), higher gel contents, and lower swelling ratios compared to the hydrogels prepared from collagen alone under similar conditions. Moreover, they showed tunable degradation behaviors against collagenase. The collagen/HAP-ALN hybrid hydrogels supported the adhesion and growth of murine MC3T3-E1 osteoblastic cells well. Such tough yet enzymatically degradable hybrid hydrogels hold potential as scaffolds for bone tissue engineering.

  5. One-step preparation of organometal/Fe{sub 3}O{sub 4} hybrid microspheres and their electromagnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Wei Junji; Zhan Yingqing; Yang Xulin; Meng Fanbin; Ma Zhen; Zhao Rui; Zhong Jiachun; Zhang Jiandong [Research Branch of Functional Materials, Institute of Microelectronic and Solid State Electronic, University of Electronic Science and Technology of China, Chengdu 610054 (China); Liu Xiaobo, E-mail: liuxb@uestc.edu.cn [Research Branch of Functional Materials, Institute of Microelectronic and Solid State Electronic, University of Electronic Science and Technology of China, Chengdu 610054 (China)

    2011-12-15

    Novel organometal/Fe{sub 3}O{sub 4} hybrid microspheres were prepared from bisphthalonitrile-benzoxine resin containing ferrocene (FPNBZ) and FeCl{sub 3}.6H{sub 2}O via a one-step solvent-thermal method. The phase structure, composition and morphology of as-prepared hybrid microspheres were characterized by X-ray powder diffraction, Fourier transform infrared spectrophotometer and scanning electron microscopy. The results revealed that crystallinity, dispersity and size of hybrid microspheres can be controlled by altering the reaction parameters. Density measurement showed that the density is decreased with increasing FPNBZ concentration in the hybrid materials. Electromagnetic properties of the FPNBZ/Fe{sub 3}O{sub 4} hybrid microspheres were measured at 2-18 GHz. The electromagnetic measurement indicated that the resonance peaks of complex permittivity, complex permeability, dielectric loss and magnetic loss were shifted to the high frequencies, with the increasing amount of FPNBZ. The as-prepared hybrid materials are believed to have broad applications both in microwave absorption materials in a wide frequency range and in biomedical fields. - Highlights: > The as-prepared hybrid microspheres showed high resistivity, good thermal stability and low density. > Morphology, size, magnetism and electromagnetic properties of hybrid microspheres can illicit by altering the reaction parameters. > Hybrids is alleged to have wide applications both in microwave absorption materials in a wide frequency range and in biomedical fields.

  6. Facile preparation of smooth perovskite films for efficient meso/planar hybrid structured perovskite solar cells.

    Science.gov (United States)

    Zhang, Meng; Yu, Hua; Yun, Jung-Ho; Lyu, Miaoqiang; Wang, Qiong; Wang, Lianzhou

    2015-06-21

    Smooth organolead halide perovskite films for meso/planar hybrid structured perovskite solar cells were prepared by a simple compressed air blow-drying method under ambient conditions. The resultant perovskite films show high surface coverage, leading to a device power conversion efficiency of over 10% with an open circuit voltage up to 1.003 V merely using pristine poly(3-hexylthiophene) (P3HT) as a hole transporter.

  7. Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process.

    Science.gov (United States)

    Rashti, Ali; Yahyaei, Hossein; Firoozi, Saman; Ramezani, Sara; Rahiminejad, Ali; Karimi, Roya; Farzaneh, Khadijeh; Mohseni, Mohsen; Ghanbari, Hossein

    2016-12-01

    Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants.

  8. Amphiphilic mediated sample preparation for micro-flow cytometry

    Energy Technology Data Exchange (ETDEWEB)

    Clague, David S. (Livermore, CA); Wheeler, Elizabeth K. (Livermore, CA); Lee, Abraham P. (Irvine, CA)

    2009-03-17

    A flow cytometer includes a flow cell for detecting the sample, an oil phase in the flow cell, a water phase in the flow cell, an oil-water interface between the oil phase and the water phase, a detector for detecting the sample at the oil-water interface, and a hydrophobic unit operatively connected to the sample. The hydrophobic unit is attached to the sample. The sample and the hydrophobic unit are placed in an oil and water combination. The sample is detected at the interface between the oil phase and the water phase.

  9. Uniform sampling analysis of a hybrid phase-locked loop with a sample-and-hold phase detector

    Science.gov (United States)

    Barab, S.; Mcbride, A. L.

    1975-01-01

    Phase-locked-loop (PLL) bit synchronizers often employ integrate-and-dump type phase detectors that provide phase error information only at discrete points in time. Usually these phase detectors are followed by sample-and-hold circuits to produce a stairstep error voltage as the input to a standard analog circuit loop filter. When the loop is configured in this manner, it is referred to as a hybrid PLL. Sampled-data analysis methods (Z transforms) are used to determine the stability and transient response of this loop.

  10. Final LDRD report : development of sample preparation methods for ChIPMA-based imaging mass spectrometry of tissue samples.

    Energy Technology Data Exchange (ETDEWEB)

    Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.; Wiese-Smith, Deneille

    2007-12-01

    The objective of this short-term LDRD project was to acquire the tools needed to use our chemical imaging precision mass analyzer (ChIPMA) instrument to analyze tissue samples. This effort was an outgrowth of discussions with oncologists on the need to find the cellular origin of signals in mass spectra of serum samples, which provide biomarkers for ovarian cancer. The ultimate goal would be to collect chemical images of biopsy samples allowing the chemical images of diseased and nondiseased sections of a sample to be compared. The equipment needed to prepare tissue samples have been acquired and built. This equipment includes an cyro-ultramicrotome for preparing thin sections of samples and a coating unit. The coating unit uses an electrospray system to deposit small droplets of a UV-photo absorbing compound on the surface of the tissue samples. Both units are operational. The tissue sample must be coated with the organic compound to enable matrix assisted laser desorption/ionization (MALDI) and matrix enhanced secondary ion mass spectrometry (ME-SIMS) measurements with the ChIPMA instrument Initial plans to test the sample preparation using human tissue samples required development of administrative procedures beyond the scope of this LDRD. Hence, it was decided to make two types of measurements: (1) Testing the spatial resolution of ME-SIMS by preparing a substrate coated with a mixture of an organic matrix and a bio standard and etching a defined pattern in the coating using a liquid metal ion beam, and (2) preparing and imaging C. elegans worms. Difficulties arose in sectioning the C. elegans for analysis and funds and time to overcome these difficulties were not available in this project. The facilities are now available for preparing biological samples for analysis with the ChIPMA instrument. Some further investment of time and resources in sample preparation should make this a useful tool for chemical imaging applications.

  11. Preparation of polyaniline/sodium alanate hybrid using a spray-drying process

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, B. R., E-mail: bru-rms@yahoo.com.br, E-mail: fabiopassador@gmail.com, E-mail: pessan@ufscar.br; Passador, F. R., E-mail: bru-rms@yahoo.com.br, E-mail: fabiopassador@gmail.com, E-mail: pessan@ufscar.br; Pessan, L. A., E-mail: bru-rms@yahoo.com.br, E-mail: fabiopassador@gmail.com, E-mail: pessan@ufscar.br [Dep. de Engenharia de Materiais, Federal University of São Carlos (Brazil)

    2014-05-15

    Nowadays, hydrogen is highly interesting as an energy source, in particular in the automotive field. In fact, hydrogen is attractive as a fuel because it prevents air pollution and greenhouse emissions. One of the main problems with the utilization of hydrogen as a fuel is its on-board storage. The purpouse of this work was to develop a new hybrid material consisting of a polyaniline matrix with sodium alanate (NaAlH{sub 4}) using a spray-drying process. The polyaniline used for this experiment was synthesized by following a well-established method for the synthesis of the emeraldine base form of polyaniline using dodecylbenzenesulfonic acid as dopant. Micro particles of polyaniline/sodium alanate hybrids with 30 and 50 wt% of sodium alanate were prepared by using a spray-drying technique. Dilute solutions of polyaniline/sodium alanate were first prepared, 10g of the solid materials were mixed with 350 ml of toluene under stirring at room temperature for 24h and the solutions were dried using spray-dryer (Büchi, Switzerland) with 115°C of an inlet temperature. The hybrids were analyzed by differential scanning calorimetry, FT-IR and scanning electron microscopy (SEM). The addition of sodium alanate decreased the glass transition temperature of the hybrids when compared to neat polyaniline. FT-IR spectrum analysis was performed to identify the bonding environment of the synthesized material and was observed that simply physically mixture occurred between polyaniline and sodium alanate. The SEM images of the hybrids showed the formation of microspheres with sodium alanate dispersed in the polymer matrix.

  12. Comparison of clinical samples for visceral Leishmaniasis diagnosis in asymptomatic dogs by PCR hybridization

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Sidney A.; Ituassu, Leonardo T.; Melo, Maria N. [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Parasitologia], e-mail: saninoalmeida@gmail.com, e-mail: Itituassu@yahoo.com.br, e-mail: melo@icb.ufmg.br; Leite, Rodrigo S.; Andrade, Antero S.R. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN-CNEN/MG), Belo Horizonte, MG (Brazil)], e-mail: rleite2005@gmail.com, e-mail: antero@cdtn.br

    2009-07-01

    The canine visceral leishmaniasis (CVL) diagnosis still represents a challenge because of complexity of this disease. The aim of present study was to compare different clinical samples for diagnosis of CVL by Polymerase Chain Reaction (PCR) combined with hybridization of {sup 32}P labeled probes. Bone marrow (BM), skin biopsy (SB), peripheral blood (PB) and conjunctival swab (CS) were used in this work. With this purpose 40 asymptomatic dogs, all positive by parasitological test, were obtained. From each animal were collected SB with sterile punches from ear internal surface, 1.0 mL of PB, BM aspirates from sternum and CS from both lower eyelid. Each clinical sample was submitted to suitable DNA purification process and PCR-hybridization assays. The positive results obtained with PCR were 55%, 25%, 30% and 22.5% for CS, BM, SB and PB respectively while the PCR followed by hybridization showed a positivity of 87.5%, 50%, 45% and 27.5% respectively. The hybridization assay was able to increase the PCR positivity in all kinds of clinical samples. The best performance was obtained using CS samples. We concluded that the PCR associated with DNA radioactive probes was a very sensitive tool for diagnosis of CVL in asymptomatic dogs and the CS has an important potential for regular screening of dogs. (author)

  13. Hybrid algorithm of ensemble transform and importance sampling for assimilation of non-Gaussian observations

    Directory of Open Access Journals (Sweden)

    Shin'ya Nakano

    2014-05-01

    Full Text Available A hybrid algorithm that combines the ensemble transform Kalman filter (ETKF and the importance sampling approach is proposed. Since the ETKF assumes a linear Gaussian observation model, the estimate obtained by the ETKF can be biased in cases with nonlinear or non-Gaussian observations. The particle filter (PF is based on the importance sampling technique, and is applicable to problems with nonlinear or non-Gaussian observations. However, the PF usually requires an unrealistically large sample size in order to achieve a good estimation, and thus it is computationally prohibitive. In the proposed hybrid algorithm, we obtain a proposal distribution similar to the posterior distribution by using the ETKF. A large number of samples are then drawn from the proposal distribution, and these samples are weighted to approximate the posterior distribution according to the importance sampling principle. Since the importance sampling provides an estimate of the probability density function (PDF without assuming linearity or Gaussianity, we can resolve the bias due to the nonlinear or non-Gaussian observations. Finally, in the next forecast step, we reduce the sample size to achieve computational efficiency based on the Gaussian assumption, while we use a relatively large number of samples in the importance sampling in order to consider the non-Gaussian features of the posterior PDF. The use of the ETKF is also beneficial in terms of the computational simplicity of generating a number of random samples from the proposal distribution and in weighting each of the samples. The proposed algorithm is not necessarily effective in case that the ensemble is located distant from the true state. However, monitoring the effective sample size and tuning the factor for covariance inflation could resolve this problem. In this paper, the proposed hybrid algorithm is introduced and its performance is evaluated through experiments with non-Gaussian observations.

  14. Selecting Sample Preparation Workflows for Mass Spectrometry-Based Proteomic and Phosphoproteomic Analysis of Patient Samples with Acute Myeloid Leukemia

    Directory of Open Access Journals (Sweden)

    Maria Hernandez-Valladares

    2016-08-01

    Full Text Available Global mass spectrometry (MS-based proteomic and phosphoproteomic studies of acute myeloid leukemia (AML biomarkers represent a powerful strategy to identify and confirm proteins and their phosphorylated modifications that could be applied in diagnosis and prognosis, as a support for individual treatment regimens and selection of patients for bone marrow transplant. MS-based studies require optimal and reproducible workflows that allow a satisfactory coverage of the proteome and its modifications. Preparation of samples for global MS analysis is a crucial step and it usually requires method testing, tuning and optimization. Different proteomic workflows that have been used to prepare AML patient samples for global MS analysis usually include a standard protein in-solution digestion procedure with a urea-based lysis buffer. The enrichment of phosphopeptides from AML patient samples has previously been carried out either with immobilized metal affinity chromatography (IMAC or metal oxide affinity chromatography (MOAC. We have recently tested several methods of sample preparation for MS analysis of the AML proteome and phosphoproteome and introduced filter-aided sample preparation (FASP as a superior methodology for the sensitive and reproducible generation of peptides from patient samples. FASP-prepared peptides can be further fractionated or IMAC-enriched for proteome or phosphoproteome analyses. Herein, we will review both in-solution and FASP-based sample preparation workflows and encourage the use of the latter for the highest protein and phosphorylation coverage and reproducibility.

  15. Preparation, characterization and electrocatalytic properties of poly(luminol) and polyoxometalate hybrid film modified electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Yu-Tsern; Lin, Kuo-Chiang; Chen, Shen-Ming [National Taipei University of Technology, Taipei 106 (Taiwan). Department of Chemical Engineering

    2005-10-20

    Hybrid films composed of poly(luminol) and nanometer-sized clusters of polyoxometalate, SiMo{sub 12}O{sub 40}{sup 4-} and PMo{sub 12}O{sub 40}{sup 3-} have been prepared in acidic aqueous solutions. These films are stable and electrochemically active, and produced on glassy carbon, platinum, gold and transparent semiconductor tin oxide electrodes. The electrochemical quartz crystal microbalance and cyclic voltammetry were used to study in situ growth of the hybrid poly(luminol)/SiMo{sub 12}O{sub 40}{sup 4-} and poly(luminol)/PMo{sub 12}O{sub 40}{sup 3-}. Both the poly(luminol)/SiMo{sub 12}O{sub 40}{sup 4-} and poly(luminol)/PMo{sub 12}O{sub 40}{sup 3-} hybrid films showed four redox couples and the electrochemical properties were compared to SiMo{sub 12}O{sub 40}{sup 4-} and PMo{sub 12}O{sub 40}{sup 3-}. When transferred to various acidity aqueous solutions, the four redox couples and the formal potentials of two hybride film were observed to be pH-dependent. The electrocatalytic reduction of ClO{sub 3}{sup -}, BrO{sub 3}{sup -}, IO{sub 3}{sup -}, S{sub 2}O{sub 8}{sup 2-} and NO{sub 2}{sup -}by a poly(luminol)/PMo{sub 12}O{sub 40}{sup 3-} hybrid film in an acidic aqueous solution showed an electrocatalytic reduction activity of IO{sub 3}{sup -} > BrO{sub 3}{sup -} and ClO{sub 3}{sup -}. The electrocatalytic oxidation of dopamine and epinephrine by a poly(luminol)/PMo{sub 12}O{sub 40}{sup 3-} hybrid film was also investigated. (author)

  16. Preparation of porous chitosan-poly(acrylic acid)-calcium phosphate hybrid nanoparticles via mineralization

    Institute of Scientific and Technical Information of China (English)

    CHEN ChangJing; DENG Yu; YAN ErYun; HU Yong; JIANG XiQun

    2009-01-01

    In this work,the preparation of chitosan-poly(acrylic acid)-calcium phosphate hybrid nanoparticles (CS-PAA-CaP NP) based on the mineralization of calcium phosphate (CAP) on the surface of chitosan-poly (acrylic acid) nanoparticles (CS-PAA NPs) was reported. CS-PAA-CaP NPs were achieved by directly adding ammonia to the aqueous solution of CS-PAA nanoparticles or by thermal decomposition of urea in the aqueous solution of CS-PAA nanoparticles,resulting in the mineralization of CaP on the surface of CS-PAA NPs. Through these two routes,especially using urea as a pH-regulator,the precipitation of CS-PAA NPs,a common occurrence in basic environment,was avoided. The size,morphology and ingredient of CS-PAA-CaP hybrid nanoparticles were characterized by dynamic light scattering (DLS),transmission electron microscope (TEM),scanning electron microscope (SEM),thermogravimetry analysis (TGA) and X-ray diffractometer (XRD). When urea was used as the pH regulator to facilitate the mineralization during the thermal urea decomposition procedure,regular CS-PAA-CaP hybrid nanoparticles with a porosity-structural CaP shells and 400-600 nm size were obtained. TGA result revealed that the hybrid NPs contained approximately 23% inorganic component,which was consistent with the ratio of starting materials. The XRD spectra of hybrid nanoparticles indicated that dicalcium phosphate (DCP:CaHPO4) crystal was a dominant component of mineralization.The porous structure of the CS-PAA-CaP hybrid NPs might be greatly useful in pharmaceutical and other medical applications.

  17. One-pot preparation of glutathione-silica hybrid monolith for mixed-mode capillary liquid chromatography based on "thiol-ene" click chemistry.

    Science.gov (United States)

    Lin, Zian; Tan, Xiaoqing; Yu, Ruifang; Lin, Jiashi; Yin, Xiaofei; Zhang, Lan; Yang, Huanghao

    2014-08-15

    A novel glutathione (GSH)-silica hybrid monolithic column synthesized via a combination of thiol-ene click reaction and one-pot process was described, where thiol-end GSH organic monomer and 2,2-azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethyloxysilane (TMOS) and γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and then introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the GSH-silica hybrid monolith. The effects of the molar ratio of TMOS/γ-MAPS, the amount of GSH, and the volume of porogen on the morphology, permeability and pore properties of the prepared GSH-silica hybrid monoliths were studied in detail. A uniform monolithic network with high porosity was obtained. A series of test compounds including alkylbenzenes, amides, and anilines were used to evaluate the retention behaviors of the GSH-silica hybrid monolithic column. The results demonstrated that the prepared GSH-silica hybrid monolith exhibited multiple interactions including hydrophobicity, hydrophilicity, as well as cation exchange interaction. The run-to-run, column-to-column and batch-to-batch reproducibilities of the GSH-silica hybrid monolith for phenols' retention were satisfactory with the relative standard deviations (RSDs) less than 1.3% (n=5), 2.6% (n=3) and 3.2% (n=3), respectively, indicating the effectiveness and practicability of the proposed method. In addition, the GSH-silica hybrid monolith was applied to the separation of nucleotides, peptides and protein tryptic digests, respectively. The successful applications suggested the potential of the GSH-silica hybrid monolith in complex sample analysis.

  18. Physicochemical properties of hybrid graphene-lead sulfide quantum dots prepared by supercritical ethanol

    Science.gov (United States)

    Tavakoli, Mohammad Mahdi; Tayyebi, Ahmad; Simchi, Abdolreza; Aashuri, Hossein; Outokesh, Mohmmad; Fan, Zhiyong

    2015-01-01

    Recently, hybrid graphene-quantum dot systems have attracted increasing attention for the next-generation optoelectronic devices such as ultrafast photo-detectors and solar energy harvesting. In this paper, a novel, one-step, reproducible, and solution-processed method is introduced to prepare hybrid graphene-PbS colloids by employing supercritical ethanol. In the hybrid nanocomposite, PbS quantum dots ( 3 nm) are decorated on the reduced graphene oxide (rGO) nanosheets ( 1 nm thickness and less than 1 micron lengths). By employing X-ray photoelectron and Raman and infrared spectroscopy techniques, it is shown that the rGO nanosheets are bonded to PbS nanocrystals through carboxylic bonds. Passivation of {111} planes of PbS quantum dots with rGO nanosheets is demonstrated by employing density function theory. Quenching of the photoluminescence emission of PbS nanocrystals through coupling with graphene sheets is also shown. In order to illustrate that the developed preparation method does not impair the quantum efficiency of the PbS nanocrystals, the photovoltaic efficiency of solar cell device is reported and compared with oleic acid-capped PbS colloidal quantum dot solar cells. By employing the "Hall effect" measurement, it is shown that the carrier mobility is significantly increased (by two orders of magnitudes) in the presence of graphene nanosheets.

  19. Physicochemical properties of hybrid graphene–lead sulfide quantum dots prepared by supercritical ethanol

    Energy Technology Data Exchange (ETDEWEB)

    Tavakoli, Mohammad Mahdi [Sharif University of Technology, Department of Materials Science and Engineering (Iran, Islamic Republic of); Tayyebi, Ahmad [Sharif University of Technology, Department of Energy (Iran, Islamic Republic of); Simchi, Abdolreza, E-mail: simchi@sharif.edu; Aashuri, Hossein [Sharif University of Technology, Department of Materials Science and Engineering (Iran, Islamic Republic of); Outokesh, Mohmmad [Sharif University of Technology, Department of Energy (Iran, Islamic Republic of); Fan, Zhiyong [Hong Kong University of Science and Technology, Department of Electronic and Computer Engineering (Hong Kong)

    2015-01-15

    Recently, hybrid graphene–quantum dot systems have attracted increasing attention for the next-generation optoelectronic devices such as ultrafast photo-detectors and solar energy harvesting. In this paper, a novel, one-step, reproducible, and solution-processed method is introduced to prepare hybrid graphene–PbS colloids by employing supercritical ethanol. In the hybrid nanocomposite, PbS quantum dots (∼3 nm) are decorated on the reduced graphene oxide (rGO) nanosheets (∼1 nm thickness and less than 1 micron lengths). By employing X-ray photoelectron and Raman and infrared spectroscopy techniques, it is shown that the rGO nanosheets are bonded to PbS nanocrystals through carboxylic bonds. Passivation of {111} planes of PbS quantum dots with rGO nanosheets is demonstrated by employing density function theory. Quenching of the photoluminescence emission of PbS nanocrystals through coupling with graphene sheets is also shown. In order to illustrate that the developed preparation method does not impair the quantum efficiency of the PbS nanocrystals, the photovoltaic efficiency of solar cell device is reported and compared with oleic acid-capped PbS colloidal quantum dot solar cells. By employing the “Hall effect” measurement, it is shown that the carrier mobility is significantly increased (by two orders of magnitudes) in the presence of graphene nanosheets.

  20. Preparation of layered double hydroxide/chlorophyll a hybrid nano-antennae: a key step.

    Science.gov (United States)

    Sommer Márquez, Alicia E; Lerner, Dan A; Fetter, Geolar; Bosch, Pedro; Tichit, Didier; Palomares, Eduardo

    2014-07-21

    In the first step to obtain an efficient nano-antenna in a bottom-up approach, new hybrid materials were synthesized using a set of layered double hydroxides (LDHs) with basic properties and pure chlorophyll a (Chl a). The stability of the adsorbed monolayer of Chl a was shown to be dependent on the nature and the ratio of the different metal ions present in the LDHs tested. The hybrid materials turned out to be adequate for stabilizing Chl a on Mg/Al LDHs for more than a month under ambient conditions while a limited catalytic decomposition was observed for the Ni/Al LDHs leading to the formation of pheophytin. These changes were followed by namely XRD, DR-UV-vis and fluorescence spectroscopies of the hybrid antennae and of the solutions obtained from their lixiviation with acetone or diethylether. On Mg/Al hydrotalcites the stability of the adsorbed Chl a was equivalent for values of the metal atom ratio ranging from 2 to 4. The latter hybrids should constitute a good basis to form efficient nanoscale light harvesting units following intercalation of selected dyes. This work describes an efficient preparation of Chl a that allows scale-up as well as the obtention of a stable Chl a monolayer on the surface of various LDHs.

  1. Preparation and antibacterial properties of hybrid-zirconia films with silver nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Azocar, Ignacio, E-mail: manuel.azocar@usach.cl [Departamento de Quimica de los Materiales, Facultad de Quimica y Biologia, Universidad de Santiago de Chile, USACH, Avenida Bernardo O' Higgins 3363, Casilla 40, Correo 33, Santiago (Chile); Vargas, Esteban [Facultad de Ingenieria, Departamento de Metalurgia, Universidad de Santiago de Chile, USACH (Chile); Duran, Nicole [Departamento de Quimica de los Materiales, Facultad de Quimica y Biologia, Universidad de Santiago de Chile, USACH, Avenida Bernardo O' Higgins 3363, Casilla 40, Correo 33, Santiago (Chile); Arrieta, Abel [Departamento de Biologia, Facultad de Quimica y Biologia, Universidad de Santiago de Chile, USACH (Chile); Gonzalez, Evelyn [Departamento de Quimica de los Materiales, Facultad de Quimica y Biologia, Universidad de Santiago de Chile, USACH, Avenida Bernardo O' Higgins 3363, Casilla 40, Correo 33, Santiago (Chile); Facultad de Ingenieria, Departamento de Metalurgia, Universidad de Santiago de Chile, USACH (Chile); Departamento de Biologia, Facultad de Quimica y Biologia, Universidad de Santiago de Chile, USACH (Chile); Departamento de Quimica Farmacologica y Toxicologica, Facultad de Ciencias Quimicas, Universidad de Chile, Sergio Livingstone Polhammer 1007, Santiago (Chile); and others

    2012-11-15

    The antimicrobial effect of incorporating silver nanoparticles (AgNps) into zirconia matrix-polyether glycol was studied. AgNps of 4-6 nm in size were synthesized using the inverse micelles method, and different doses of metallic nanoparticles were incorporated into zirconia-polyether glycol mixtures during the ageing procedure. Atomic force microscopy (AFM) of the modified hybrid film showed a homogenous distribution of 20-80 nm diameter AgNps, indicating agglomeration of these structures during film modification; such agglomerations were greater when increasing the dosage of the colloidal system. The AgNps-hybrid films showed higher antimicrobial activity against Gram-positive bacteria than for Gram-negative bacteria. Hybrid films prepared with dioctyl sodium sulfosuccinate (AOT) stabilized AgNps presented enhanced antibacterial activity compared to that obtained through the addition of a high AgNO{sub 3} concentration (0.3 wt%). -- Graphical abstract: Atomic Force Micrographs, top and cross section view, showing silver nanoparticles embedded in a zirconia-polyether glycol hybrid film. Highlights: Black-Right-Pointing-Pointer Antibacterial activity of films (zirconia-polyether glycol) modified with silver nanoparticles. Black-Right-Pointing-Pointer Biofilm formation is prevented. Black-Right-Pointing-Pointer High sensibility against gram positive bacteria.

  2. Preparation and characterization of SiO₂/CMC/Ag hybrids with antibacterial properties.

    Science.gov (United States)

    Rangelova, Nadezhda; Aleksandrov, Lyubomir; Angelova, Tsvetelina; Georgieva, Nelly; Müller, Rudolf

    2014-01-30

    Amorphous hybrids based on sodium salt of carboxymethyl cellulose (CMC) and tetraethoxysilane (TEOS) containing silver nanoparticles were prepared by sol-gel method. The amorphous structure, morphology and antibacterial behavior were clarified. The thermal stability of obtained hybrids decreased with the increase in silver content from 0.5 to 1.5 wt%. Infrared spectra of the material suggest that the main interaction between the cellulose ether and silica network is via hydrogen bonds (bands at approximately 3,540 and 3,625 cm(-1)). According to UV-vis spectra the silver is present in two different states Ag(+) (absorption band at approximately 210 nm) and Ag(0) (band at approximately 300 nm). The different sizes of silver particles are present as clusters. It was demonstrated that these hybrids have a well pronounced antibacterial activity against B. subtilis and E. coli K12. Even the hybrid with 0.5 wt% Ag has efficient antibacterial activity for both Gram-positive and Gram-negative bacteria.

  3. Mobilization Protocols for Hybrid Sensors for Environmental AOP Sampling (HySEAS) Observations

    Science.gov (United States)

    Hooker, Stanford B.

    2014-01-01

    The protocols presented here enable the proper mobilization of the latest-generation instruments for measuring the apparent optical properties (AOPs) of aquatic ecosystems. The protocols are designed for the Hybrid Sensors for Environmental AOP Sampling (HySEAS) class of instruments, but are applicable to the community of practice for AOP measurements. The protocols are organized into eleven sections beyond an introductory overview: a) cables and connectors, b) HySEAS instruments, c) platform preparation, d) instrument installation, e) cable installation, f) test deployment, g) test recovery, h) maintenance, i) shipping, j) storage, and k) smallboat operations. Each section concentrates on documenting how to prevent the most likely faults, remedy them should they occur, and accomplishing both with the proper application of a modest set of useful tools. Within the twelve sections, there are Socratic exercises to stimulate thought, and the answers to these exercises appear in Appendix A. Frequently asked questions (FAQs) are summarized in a separate section after the answers to the exercises in Appendix B. For practitioners unfamiliar with the nautical terms used throughout this document plus others likely encountered at sea, an abbreviated dictionary of nautical terms appears in Appendix C. An abbreviated dictionary of radiotelephone terms is presented in Appendix D. To ensure familiarity with many of the tools that are presented, Appendix E provides a description of the tools alongside a thumbnail picture. Abbreviated deployment checklists and cable diagrams are provided in Appendix F. The document concludes with an acknowledgments section, a glossary of acronyms, a definition of symbols, and a list of references.

  4. Support for the 7-factor hybrid model of PTSD in a community sample.

    Science.gov (United States)

    Seligowski, Antonia V; Orcutt, Holly K

    2016-03-01

    Research suggests that 4-factor models of posttraumatic stress disorder (PTSD) may be improved upon by the addition of novel factors, such as Dysphoric Arousal, Externalizing Behaviors, and Anhedonia. However, a novel 7-factor hybrid model has demonstrated superior fit in veteran and undergraduate samples. The current study sought to replicate this finding in a trauma-exposed community sample and examined relations with positive (PA) and negative affect (NA). Participants included 403 adults (M(age) = 37.75) recruited through Amazon's MTurk. PTSD was measured using the PTSD Checklist-5 (PCL-5). Confirmatory factor analyses were conducted in Mplus. The 7-factor hybrid model demonstrated good fit: CFI = .96, TLI = .95, RMSEA = .06 (90% CI [.05, .07]), SRMR = .03. This model was superior to the 5- and 6-factor models. All factors demonstrated significant relations with PA and NA, the largest of which were the Externalizing Behaviors (with NA) and Anhedonia (with PA) factors. Results provide support for the 7-factor hybrid model of PTSD using the PCL-5 in a community sample. Findings replicate previous research suggesting that PTSD is highly related to NA, which has been purported as an underlying dimension of PTSD. It is recommended that future research use clinical measures to further examine the hybrid model. (PsycINFO Database Record (c) 2016 APA, all rights reserved).

  5. Preview of the NASA NNWG NDE Sample Preparation Handbook

    Science.gov (United States)

    2010-01-01

    This viewgraph presents a step-by-step how-to fabrication documentation of every kind of sample that is fabricated for MSFC by UA Huntsville, including photos and illustrations. The tabulation of what kind of samples are being fabricated for what NDE method, detailed instructions/documentation of the inclusion/creation of defects, detailed specifications for materials, processes, and equipment, case histories and/or experiences with the different fabrication methods and defect inclusion techniques, discussion of pitfalls and difficulties associated with sample fabrication and defect inclusion techniques, and a discussion of why certain fabrication techniques are needed as related to the specific NDE methods are included in this presentation.

  6. Sample Preparation (SS): SE45_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available tration of 15 ng µl-1 for each 1-µl injection. After 5-min centrifugation at 15,1...0 mg/ml in pyridine) was added to the sample. After 24 h of derivatization at room temperature, the sample w...µl of methoxyamine hydrochloride (20 mg ml-1 in pyridine) were added to the sample. After 24 h of derivatiza...f MSTFA at 37°C with shaking. After silylation 30 µl of n-heptane were added. All derivatization steps were

  7. Coupled thermal model of photovoltaic-thermoelectric hybrid panel for sample cities in Europe

    DEFF Research Database (Denmark)

    Rezaniakolaei, Alireza; Sera, Dezso; Rosendahl, Lasse Aistrup

    2016-01-01

    generation by the TEG is insignificant compared to electrical output by the PV panel, and the TEG plays only a small role on power generation in the hybrid PV/TEG panel. However, contribution of the TEG in the power generation can be improved via higher ZT thermoelectric materials and geometry optimization......In general, modeling of photovoltaic-thermoelectric (PV/TEG) hybrid panels have been mostly simplified and disconnected from the actual ambient conditions and thermal losses from the panel. In this study, a thermally coupled model of PV/TEG panel is established to precisely predict performance...... of the hybrid system under different weather conditions. The model takes into account solar irradiation, wind speed and ambient temperature as well as convective and radiated heat losses from the front and rear surfaces of the panel. The model is developed for three sample cities in Europe with different...

  8. Facile Preparation of Phosphotungstic Acid-Impregnated Yeast Hybrid Microspheres and Their Photocatalytic Performance for Decolorization of Azo Dye

    Directory of Open Access Journals (Sweden)

    Lan Chen

    2013-01-01

    Full Text Available Phosphotungstic acid (HPW-impregnated yeast hybrid microspheres were prepared by impregnation-adsorption technique through tuning pH of the aqueous yeast suspensions. The obtained products were characterized by field emission scanning electron microscopy (FE-SEM, energy dispersive spectrometry (EDS, X-ray diffraction (XRD, thermogravimetry-differential scanning calorimetry (TG-DSC, and ultraviolet-visible spectrophotometry (UV-Vis, respectively. FE-SEM and EDS ascertain that the HPW has been effectively introduced onto the surface of yeast, and the resulting samples retain ellipsoid shape, with the uniform size (length 4.5 ± 0.2 μm, width 3.0 ± 0.3 μm and good monodispersion. XRD pattern indicates that the main crystal structure of as-synthesized HPW@yeast microsphere is Keggin structure. TG-DTA states that the HPW in composites has better thermal stability than pure HPW. Fourier transform infrared spectroscopy (FT-IR elucidates that the functional groups or chemical bonds inherited from the pristine yeast cell were critical to the assembling of the composites. UV-Vis shows that the obtained samples have a good responding to UV light. The settling ability indicates that the hybrid microspheres possess an excellent suspension performance. In the test of catalytic activity, the HPW@yeast microsphere exhibits a high photocatalytic activity for the decoloration of Methylene blue and Congo red dye aqueous solutions, and there are a few activity losses after four cycles of uses.

  9. Porous polylactic acid-silica hybrids: preparation, characterization, and study of mesenchymal stem cell osteogenic differentiation.

    Science.gov (United States)

    Pandis, Christos; Trujillo, Sara; Matos, Joana; Madeira, Sara; Ródenas-Rochina, Joaquín; Kripotou, Sotiria; Kyritsis, Apostolos; Mano, João F; Gómez Ribelles, José Luis

    2015-02-01

    A novel approach to reinforce polymer porous membranes is presented. In the prepared hybrid materials, the inorganic phase of silica is synthesized in-situ and inside the pores of aminolyzed polylactic acid (PLA) membranes by sol-gel reactions using tetraethylorthosilicate (TEOS) and glycidoxypropyltrimethoxysilane (GPTMS) as precursors. The hybrid materials present a porous structure with a silica layer covering the walls of the pores while GPTMS serves also as coupling agent between the organic and inorganic phase. The adjustment of silica precursors ratio allows the modulation of the thermomechanical properties. Culture of mesenchymal stem cells on these supports in osteogenic medium shows the expression of characteristic osteoblastic markers and the mineralization of the extracellular matrix.

  10. Zirconium oxocluster/polymer hybrid nanoparticles prepared by photoactivated miniemulsion copolymerization

    Science.gov (United States)

    Benedetti, Cesare; Flouda, Paraskevi; Antonello, Alice; Rosenauer, Christine; Pérez-Pla, Francisco F.; Landfester, Katharina; Gross, Silvia; Muñoz-Espí, Rafael

    2017-09-01

    The photoactivated free radical miniemulsion copolymerization of methyl methacrylate (MMA) and the zirconium oxocluster Zr4O2(methacrylate)12 is used as an effective and fast preparation method for polymer/inorganic hybrid nanoparticles. The oxoclusters, covalently anchored to the polymer network, act as metal-organic cross-linkers, thus improving the thermomechanical properties of the resulting hybrid nanoparticles. Benzoin carbonyl organic compounds were used as photoinitiators. The obtained materials are compared in terms of cross-linking, effectiveness of cluster incorporation, and size distribution with the analogous nanoparticles produced by using conventional thermally induced free radical miniemulsion copolymerization. The kinetics of the polymerization process in the absence and in the presence of the oxocluster is also investigated.

  11. Preparation and characterization of gold nanoparticles capped by peptide-biphenyl hybrids.

    Science.gov (United States)

    Pérez, Yolanda; Mann, Enrique; Herradón, Bernardo

    2011-07-15

    Gold nanoparticles were prepared using peptide-biphenyl hybrids (PBHs) as capping agents. AuNPs were characterized by different techniques including UV-Vis, TEM, EDX, FT-IR, elemental analysis, (1)H NMR and (13)C CP/MAS NMR spectroscopy. TEM analysis showed that AuNPs present diameters in the range of 1.8-3.7 nm, depending on the structure and the amount of the capping PBH used. FT-IR spectroscopy and solid-state (13)C NMR revealed that the carboxylic group of PBHs, especially in the case of the acid ligands, interacts with the gold surface (in the form of carboxylate). The results confirm that PBHs are excellent stabilizers of AuNPs, being one of the first examples on the use of peptidomimetics-gold hybrid materials.

  12. Sample Preparation (SS): SE55_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available 80℃ until analysis. The frozen tissues were homogenized in five volumes of 80% aqueous methanol containing 0...SE55_SS01 Metabolic profiling Collected sample tissues were weighed and stored at -

  13. Sample Preparation for Monolithic Refractories Part 1: Refractory Castables

    Institute of Scientific and Technical Information of China (English)

    Zhang Xiaohui; Peng Xigao

    2010-01-01

    @@ 1 Scope This standard specifies the definition and test methods of flowability of dense and insulating refractory castables,and moulding equipment,moulding methods,curing and drying conditions of castables samples.

  14. Sample Preparation (SS): SE52_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available Tokyo, Japan) using a mixer mill (MM 300, Retsch) with a zirconia bead for 6 min... at 20 Hz. Next, the samples were centrifuged at 15,000 g for 10 min and filtered (Ultrafree-MC filter, 0.2 μm; Mil...lipore, Bedford, MA, USA). The sample extracts were then applied to an HLB μElution plate (Waters, Mil

  15. PREPARATION AND PROPERTIES OF SPAES-TiO_2 HYBRID MEMBRANES FOR DIRECT METHANOL FUEL CELL

    Institute of Scientific and Technical Information of China (English)

    Ni Zhang; Hui-ling Liu; Jun-jing Li; Zhi Xia

    2009-01-01

    Sulfonated poly(arylene ether sulfone) (SPAES) copolymer with degree of sulfonation of 1.0 was synthesized and characterized. A series of SPAES-TiO_2 hybrid membranes with various contents of nano-sized TiO_2 particles were prepared and characterized through sol-gel reactions. Scanning electron microscopy (SEM) images indicated the TiO_2 particles were well dispersed within polymer matrix. These composite membranes were evaluated for proton exchange membranes (PEMs) in direct methanol fuel cell (DMFC). These membranes showed good thermal stability and mechanical properties. It was found that the water uptake of these membranes increased with the increase of the TiO_2 contents in the hybrid membranes. Meanwhile, the introduction of inorganic particles increased the proton conductivity and reduced the methanol permeability. The proton conductivities (0.118-0.162 S/cm) of SPAES-TiO_2 hybrid membranes with 8% TiO_2 particles are much higher than those of Nation 117 membrane (0.095-0.117 S/cm) and pure SPAES membrane (0.100-0.124 S/cm) with degree of sulfonation of 1.0 at all temperatures (25-100℃). Especially, the methanol diffusion coefficient (8.4×10~(-7) cm~2/s) of SPAES-TiO_2 hybrid membranes with 8% TiO_2 is much lower than that of Nation 117 membrane (2.1 ×10~(-6) cm~2/s). SPAES-TiO_2 hybrid membranes were therefore proposed as candidates of material for PEM in DMFC.

  16. One-pot preparation of Ni-graphene hybrids with enhanced catalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Guiqiang, E-mail: chengphnu@126.com [College of Information Science and Engineering, Hebei North University, Zhangjiakou 075000, Hebei (China); Wang, Fengli [College of Information Science and Engineering, Hebei North University, Zhangjiakou 075000, Hebei (China); Liu, Fei [Department of Electrical Engineering, Zhangjiakou Vocational College of Technology, Zhangjiakou 075000, Hebei (China); Zhang, Xiao, E-mail: Zhangxiao83690@163.com [College of Information Science and Engineering, Hebei North University, Zhangjiakou 075000, Hebei (China)

    2014-10-15

    Highlights: • Ni-rGO hybrids were synthesized by a microwave-assisted method. • NaBH4 was used as a reducing agent to fabricate Ni-rGO hybrids. • Ni-rGO was used as catalyst for the reduction of p-nitrophenol. • Ni-rGO showed higher catalytic ability than pure Ni nanoparticles. • Ni-rGO showed good recyclability and stability. - Abstract: A facile one-pot method was developed to synthesize magnetic nickel nanoparticles (Ni NPs) decorated on reduced graphene oxide (rGO) with NaHB{sub 4} as a reductant under microwave irradiation. The morphologies and structures of the Ni-rGO hybrids were investigated by electron microscopy, thermal gravimetric analysis, X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectroscopy and magnetic measurements. The results showed that Ni-rGO hybrids composed of the well-dispersed Ni NPs with an average diameter of 12 nm were successfully prepared. To demonstrate one potential application, the catalytic ability of Ni-rGO was evaluated and it was found that Ni-rGO showed much enhanced catalytic ability, good recyclability and stability toward the catalytic reduction of p-nitrophenol to p-aminophenol. The excellent catalytic activity of Ni-rGO hybrids was due possibly to the synergistic effect of Ni NPs and rGO, including the uniform distribution of Ni NPs onto rGO, enhanced electrons separation and transport, as well as the fast adsorption of p-nitrophenol by rGO.

  17. Hybrid nested sampling algorithm for Bayesian model selection applied to inverse subsurface flow problems

    KAUST Repository

    Elsheikh, Ahmed H.

    2014-02-01

    A Hybrid Nested Sampling (HNS) algorithm is proposed for efficient Bayesian model calibration and prior model selection. The proposed algorithm combines, Nested Sampling (NS) algorithm, Hybrid Monte Carlo (HMC) sampling and gradient estimation using Stochastic Ensemble Method (SEM). NS is an efficient sampling algorithm that can be used for Bayesian calibration and estimating the Bayesian evidence for prior model selection. Nested sampling has the advantage of computational feasibility. Within the nested sampling algorithm, a constrained sampling step is performed. For this step, we utilize HMC to reduce the correlation between successive sampled states. HMC relies on the gradient of the logarithm of the posterior distribution, which we estimate using a stochastic ensemble method based on an ensemble of directional derivatives. SEM only requires forward model runs and the simulator is then used as a black box and no adjoint code is needed. The developed HNS algorithm is successfully applied for Bayesian calibration and prior model selection of several nonlinear subsurface flow problems. © 2013 Elsevier Inc.

  18. Quantitating morphological changes in biological samples during scanning electron microscopy sample preparation with correlative super-resolution microscopy.

    Science.gov (United States)

    Zhang, Ying; Huang, Tao; Jorgens, Danielle M; Nickerson, Andrew; Lin, Li-Jung; Pelz, Joshua; Gray, Joe W; López, Claudia S; Nan, Xiaolin

    2017-01-01

    Sample preparation is critical to biological electron microscopy (EM), and there have been continuous efforts on optimizing the procedures to best preserve structures of interest in the sample. However, a quantitative characterization of the morphological changes associated with each step in EM sample preparation is currently lacking. Using correlative EM and superresolution microscopy (SRM), we have examined the effects of different drying methods as well as osmium tetroxide (OsO4) post-fixation on cell morphology during scanning electron microscopy (SEM) sample preparation. Here, SRM images of the sample acquired under hydrated conditions were used as a baseline for evaluating morphological changes as the sample went through SEM sample processing. We found that both chemical drying and critical point drying lead to a mild cellular boundary retraction of ~60 nm. Post-fixation by OsO4 causes at least 40 nm additional boundary retraction. We also found that coating coverslips with adhesion molecules such as fibronectin prior to cell plating helps reduce cell distortion from OsO4 post-fixation. These quantitative measurements offer useful information for identifying causes of cell distortions in SEM sample preparation and improving current procedures.

  19. PREPARATION AND PROPERTIES OF SPAES-TiO_2 HYBRID MEMBRANES FOR DIRECT METHANOL FUEL CELL

    Institute of Scientific and Technical Information of China (English)

    刘惠玲

    2009-01-01

    Sulfonated poly(arylene ether sulfone)(SPAES) copolymer with degree of sulfonation of 1.0 was synthesized and characterized.A series of SPAES-TiO_2 hybrid membranes with various contents of nano-sized TiO_2 particles were prepared and characterized through sol-gel reactions.Scanning electron microscopy(SEM) images indicated the TiO_2 particles were well dispersed within polymer matrix.These composite membranes were evaluated for proton exchange membranes(PEMs) in direct methanol fuel cell(DMFC).These mem...

  20. Hybrid Materials Prepared from Polymers and Self-assembled Systems by Physical Processes

    Institute of Scientific and Technical Information of China (English)

    Jean-Michel; Guenet

    2007-01-01

    1 Results A new type of hybrid materails prepared from ternary systems polymer/bicopper organic complex/solvent is presented.Each binary system displays differing types of behaviour: The polymer solutions produce thermoreversible gels while the bicopper organic complex (designated as CuS8) forms randomly-dispersed,self-assembling threads in organic solvents (See Fig.1(a),(b)).Fig.1 The CuS8 and ips thermoreversible gels Thermoreversible gels possess a fibrillar morphology with a typical mesh size ra...

  1. Microfluidic desalination. Capacitive deionization on chip for microfluidic sample preparation

    NARCIS (Netherlands)

    Roelofs, Susan Helena

    2015-01-01

    The main aim of the work described in this thesis is to implement the desalination technique capacitive deionization (CDI) on a microfluidic chip to improve the reproducibility in the analysis of biological samples for drug development. Secondly, microfluidic CDI allows for the in situ study of ion

  2. Microsystem strategies for sample preparation in biological detection.

    Energy Technology Data Exchange (ETDEWEB)

    James, Conrad D.; Galambos, Paul C.; Bennett, Dawn Jonita (University of Maryland Baltimore County, Baltimore, MD); Manginell, Monica; Okandan, Murat; Acrivos, Andreas (The City College of New York, NY); Brozik, Susan Marie; Khusid, Boris (New Jersey Institute of Technology, Newark, NJ)

    2005-03-01

    The objective of this LDRD was to develop microdevice strategies for dealing with samples to be examined in biological detection systems. This includes three sub-components: namely, microdevice fabrication, sample delivery to the microdevice, and sample processing within the microdevice. The first component of this work focused on utilizing Sandia's surface micromachining technology to fabricate small volume (nanoliter) fluidic systems for processing small quantities of biological samples. The next component was to develop interfaces for the surface-micromachined silicon devices. We partnered with Micronics, a commercial company, to produce fluidic manifolds for sample delivery to our silicon devices. Pressure testing was completed to examine the strength of the bond between the pressure-sensitive adhesive layer and the silicon chip. We are also pursuing several other methods, both in house and external, to develop polymer-based fluidic manifolds for packaging silicon-based microfluidic devices. The second component, sample processing, is divided into two sub-tasks: cell collection and cell lysis. Cell collection was achieved using dielectrophoresis, which employs AC fields to collect cells at energized microelectrodes, while rejecting non-cellular particles. Both live and dead Staph. aureus bacteria have been collected using RF frequency dielectrophoresis. Bacteria have been separated from polystyrene microspheres using frequency-shifting dielectrophoresis. Computational modeling was performed to optimize device separation performance, and to predict particle response to the dielectrophoretic traps. Cell lysis is continuing to be pursued using microactuators to mechanically disrupt cell membranes. Novel thermal actuators, which can generate larger forces than previously tested electrostatic actuators, have been incorporated with and tested with cell lysis devices. Significant cell membrane distortion has been observed, but more experiments need to be

  3. Effects of Sample Preparation on the Infrared Reflectance Spectra of Powders

    Energy Technology Data Exchange (ETDEWEB)

    Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.; Su, Yin-Fong; Blake, Thomas A.; Forland, Brenda M.

    2015-05-22

    While reflectance spectroscopy is a useful tool in identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-packed as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.

  4. Preparation and characterization of humic acid-carbon hybrid materials as adsorbents for organic micro-pollutants.

    Science.gov (United States)

    Radwan, Emad K; Abdel Ghafar, Hany H; Moursy, Ahmed S; Langford, Cooper H; Bedair, Ahmed H; Achari, Gopal

    2015-08-01

    The present work involves the preparation of novel adsorbent materials by the insolubilization and hybridization of humic acid (HA) with carbon. The prepared materials were characterized by N2 adsorption, elemental analysis, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, solid-state (13)C cross polarization magic angle spinning nuclear magnetic resonance, and low-field nuclear magnetic resonance (NMR) relaxometry on wetted samples. The water solubility of these materials and the lack of effect of oxidants were also confirmed. With this background, the adsorption capacities toward phenol, 2,4,6-tricholrophenol, and atrazine were evaluated, using these as model compounds for organic micropollutants of concern in water. Experimental results show that the prepared materials are mesoporous and have a higher surface area than humic acid and even than the porous carbon in the case of carbon coating. They retain the basic features of the starting materials with lowered functional group content. Moreover, there are interesting new features. NMR relaxometry shows that equilibration of water uptake is very fast, making use in water simple. They have higher adsorption capacities than the pure materials, and they can be applied under a wide range of environmental conditions.

  5. Sample preparation and assay refinements for pathogen detection platforms

    Science.gov (United States)

    Lim, Daniel V.; Kearns, Elizabeth A.; Leskinen, Stephaney D.; Magaña, Sonia; Stroot, Joyce M.; Hunter, Dawn M.; Schlemmer, Sarah M.

    2009-02-01

    Food-borne and waterborne microbial pathogens are a potential problem in biowarfare and public health. Such pathogens can affect the health, combat readiness, and effectiveness of the warfighter in a battlefield environment and present potential threats to the civilian population through intentional or natural contamination of food and water. Conventional procedures to detect and identify microbial pathogens in food, water, and other materials can take days to perform and may provide inconclusive information. Research at the University of South Florida's Advanced Biosensors Laboratory (ABL) focuses on development of sample processing procedures and biosensor-based assays for rapid detection of biothreat agents. Rapid processing methods, including use of an automated concentrator of microorganisms in water, have been developed for complex matrix samples including ground beef, apple juice, produce, potable water and recreational water, enabling such samples to be directly tested by biosensor assays for target analytes. Bacillus atrophaeus spores and other bacteria can be concentrated from potable and recreational water at low levels with a dead-end hollow-fiber ultrafiltration concentration system. Target bacteria recovered by these processing procedures can be identified by evanescent wave, fiber optic biosensors or other detection platforms. Fiber optic biosensor assays have been improved to include subsequent PCR analysis and viability determination of captured target bacteria using broth enrichment and/or ATP luminescence.

  6. Quantitative analysis of intermediately and infinitely thick samples with thin sample approach without sample preparation using confocal X-ray fluorescence

    CERN Document Server

    Sun, Xue-Peng; Sun, Tian-Xi; Peng, Song; Sun, Wei-Yuan; Li, Fang-Zuo; Jiang, Bo-Wen; Ma, Yong-Zhong; Ding, Xun-Liang

    2015-01-01

    In order to validate that the confocal X-ray fluorescence had potential applications in analyzing the intermediately and infinitely thick samples with thin sample approach without sample preparations, as an example, the confocal X-ray fluorescence based on polycapillary X-ray optics was used to analyze multi elements solutions.

  7. Sampling Enrichment toward Target Structures Using Hybrid Molecular Dynamics-Monte Carlo Simulations.

    Science.gov (United States)

    Yang, Kecheng; Różycki, Bartosz; Cui, Fengchao; Shi, Ce; Chen, Wenduo; Li, Yunqi

    2016-01-01

    Sampling enrichment toward a target state, an analogue of the improvement of sampling efficiency (SE), is critical in both the refinement of protein structures and the generation of near-native structure ensembles for the exploration of structure-function relationships. We developed a hybrid molecular dynamics (MD)-Monte Carlo (MC) approach to enrich the sampling toward the target structures. In this approach, the higher SE is achieved by perturbing the conventional MD simulations with a MC structure-acceptance judgment, which is based on the coincidence degree of small angle x-ray scattering (SAXS) intensity profiles between the simulation structures and the target structure. We found that the hybrid simulations could significantly improve SE by making the top-ranked models much closer to the target structures both in the secondary and tertiary structures. Specifically, for the 20 mono-residue peptides, when the initial structures had the root-mean-squared deviation (RMSD) from the target structure smaller than 7 Å, the hybrid MD-MC simulations afforded, on average, 0.83 Å and 1.73 Å in RMSD closer to the target than the parallel MD simulations at 310K and 370K, respectively. Meanwhile, the average SE values are also increased by 13.2% and 15.7%. The enrichment of sampling becomes more significant when the target states are gradually detectable in the MD-MC simulations in comparison with the parallel MD simulations, and provide >200% improvement in SE. We also performed a test of the hybrid MD-MC approach in the real protein system, the results showed that the SE for 3 out of 5 real proteins are improved. Overall, this work presents an efficient way of utilizing solution SAXS to improve protein structure prediction and refinement, as well as the generation of near native structures for function annotation.

  8. Preparation and characterization of TiO 2-cationic hybrid nanoparticles as electrophoretic particles

    Science.gov (United States)

    Li, Jingjing; Deng, Liandong; Xing, Jinfeng; Dong, Anjie; Li, Xianggao

    2012-01-01

    The hybrid nanoparticles (TiO2-HNPs) with TiO2 nanoparticles as core and with poly(N,N-dimethylaminoethyl methacrylate-co-methyl methacrylate) by using triallylamine as cross-linking agent as shell were firstly prepared via atom transfer radical polymerization (ATRP) in methanol. Then the hybrid nanoparticles with positive charge were produced by the quaternization with methyl iodide as quaternization reagent so as to endow them with greater electrophoretic mobility. The cationic hybrid nanoparticles (TiO2-CHNPs) were studied by means of transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy and dynamic light scattering (DLS) measurements. The results indicate that the cationic polymer is successfully grafted on the surface of the TiO2 nanoparticles. The particle size of TiO2-CHNPs is about 150 nm and the polydispersity index (PDI) is 0.307. The zeta potential, the contrast ratio of white state to dark state and response time of TiO2-CHNPs are +16.8 mV, 30 and 3 s, respectively, which show the potential application prospect in the development of electrophoretic ink.

  9. Preparation, photophysical characterization, and modeling of LDS722/Laponite 2D-ordered hybrid films.

    Science.gov (United States)

    Epelde-Elezcano, Nerea; Duque-Redondo, Eduardo; Martínez-Martínez, Virginia; Manzano, Hegoi; López-Arbeloa, Iñigo

    2014-08-26

    A novel hybrid material with promising optical properties for nonlinear optical applications is presented, as formed by LDS 722 organic dye confined in Laponite clay. Thin films of the hybrid material with different dye loadings have been prepared. The film thickness, the dye and water content, and the clay swelling due to guest molecule incorporation have been characterized. Then, the photophysical properties of the thin films have been studied in detail using experimental methods and molecular simulation. As the dye load increases, the hybrid films present a hypsochromic shift in absorption and a bathochromic shift in emission. The former is attributed to the increasing strength of solvation of the dye donor group, while the latter is ascribed to a switch from an intramolecular to an intermolecular charge-transfer process as the dye load increases. The LDS 722 molecules are preferentially oriented in the host clay almost in parallel to the platelet surfaces, inducing macroscopic order that makes the material responsive to polarized light.

  10. Preparation and gas sensing properties of novel CdS-supramolecular organogel hybrid films

    Energy Technology Data Exchange (ETDEWEB)

    Xia Huiyun; Peng Junxia; Liu Kaiqiang; Li Chen; Fang Yu [Key Laboratory of Applied Surface and Colloid Chemistry of Ministry of Education, School of Chemistry and Materials Science, Shaanxi Normal University, Xi' an 710062 (China)], E-mail: yfang@snnu.edu.cn

    2008-05-21

    A novel CdS-supramolecular organogel hybrid film with unusual morphology has been fabricated by exposing a supramolecular organogel film containing Cd(Ac){sub 2} in an H{sub 2}S atmosphere at room temperature. The organogel film was prepared by spin-coating a LMOG (low-molecular weight organic gelator) gel of dmethyl sulfoxide onto a glass plate substrate. XRD, SEM, EDS, TG-DTA, UV-vis, PL (photoluminescence) spectroscopy and PL lifetime measurements were employed to characterize the film. It was shown that the organogel film had functioned as a template to control the morphology of the final hybrid film. The quantities and sizes of the CdS particles embedded in the organogel films can be easily altered by varying the initial concentration of Cd(Ac){sub 2}. Importantly, the PL of the hybrid film is sensitive to the presence of some volatile organic monoamines and diamines. The selectivity and reversibility of the sensing process were investigated.

  11. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance

    Directory of Open Access Journals (Sweden)

    Xiaoli Zhang

    2016-05-01

    Full Text Available Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  12. Global metabolite analysis of yeast: evaluation of sample preparation methods

    DEFF Research Database (Denmark)

    Villas-Bôas, Silas Granato; Højer-Pedersen, Jesper; Åkesson, Mats Fredrik;

    2005-01-01

    , which is the analysis of a large number of metabolites with very diverse chemical and physical properties. This work reports the leakage of intracellular metabolites observed during quenching yeast cells with cold methanol solution, the efficacy of six different methods for the extraction...... of intracellular metabolites, and the losses noticed during sample concentration by lyophilization and solvent evaporation. A more reliable procedure is suggested for quenching yeast cells with cold methanol solution, followed by extraction of intracellular metabolites by pure methanol. The method can be combined...

  13. Sample preparation of metal alloys by electric discharge machining

    Science.gov (United States)

    Chapman, G. B., II; Gordon, W. A.

    1976-01-01

    Electric discharge machining was investigated as a noncontaminating method of comminuting alloys for subsequent chemical analysis. Particulate dispersions in water were produced from bulk alloys at a rate of about 5 mg/min by using a commercially available machining instrument. The utility of this approach was demonstrated by results obtained when acidified dispersions were substituted for true acid solutions in an established spectrochemical method. The analysis results were not significantly different for the two sample forms. Particle size measurements and preliminary results from other spectrochemical methods which require direct aspiration of liquid into flame or plasma sources are reported.

  14. Preparation of Al-Ce hybrid adsorbent and its application for defluoridation of drinking water

    Energy Technology Data Exchange (ETDEWEB)

    Liu Han [Department of Environmental Science and Engineering, Tsinghua University, Beijing 100084 (China); Deng Shubo, E-mail: dengshubo@tsinghua.edu.cn [Department of Environmental Science and Engineering, Tsinghua University, Beijing 100084 (China); POPs Research Center, Tsinghua University, Beijing 100084 (China); Li Zhijian; Yu Gang; Huang Jun [Department of Environmental Science and Engineering, Tsinghua University, Beijing 100084 (China); POPs Research Center, Tsinghua University, Beijing 100084 (China)

    2010-07-15

    A novel Al-Ce hybrid adsorbent with high sorption capacity for fluoride was prepared through the coprecipitation method in this study, and its preparation conditions were optimized. X-ray diffraction (XRD) and scanning electron microscope (SEM) results showed that the hybrid adsorbent was of amorphous structure and constituted by some aggregated nanoparticles. As the adsorbent had the zero point of {zeta} potential at pH 9.6, it was very effective in fluoride removal from aqueous solution via electrostatic interaction. The results of sorption experiments including sorption kinetics, isotherms, and the effect of solution pH showed that the sorption of fluoride on the Al-Ce adsorbent was fast and pH-dependent. Especially, the adsorbent had high sorption capacity up to 27.5 mg g{sup -1} for fluoride at the equilibrium fluoride concentration of 1 mg L{sup -1}, much higher than that of the conventional adsorbents. Fourier transform infrared (FTIR) analysis and zeta potential measurement showed that the hydroxyl groups and the protonated hydroxyl groups on the adsorbent surface were involved in the fluoride adsorption.

  15. Current advances and strategies towards fully automated sample preparation for regulated LC-MS/MS bioanalysis.

    Science.gov (United States)

    Zheng, Naiyu; Jiang, Hao; Zeng, Jianing

    2014-09-01

    Robotic liquid handlers (RLHs) have been widely used in automated sample preparation for liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalysis. Automated sample preparation for regulated bioanalysis offers significantly higher assay efficiency, better data quality and potential bioanalytical cost-savings. For RLHs that are used for regulated bioanalysis, there are additional requirements, including 21 CFR Part 11 compliance, software validation, system qualification, calibration verification and proper maintenance. This article reviews recent advances in automated sample preparation for regulated bioanalysis in the last 5 years. Specifically, it covers the following aspects: regulated bioanalysis requirements, recent advances in automation hardware and software development, sample extraction workflow simplification, strategies towards fully automated sample extraction, and best practices in automated sample preparation for regulated bioanalysis.

  16. Organic/hybrid nanoparticles and single-walled carbon nanotubes: preparation methods and chiral applications.

    Science.gov (United States)

    Alhassen, Haysem; Antony, Vijy; Ghanem, Ashraf; Yajadda, Mir Massoud Aghili; Han, Zhao Jun; Ostrikov, Kostya Ken

    2014-11-01

    Nanoparticles are molecular-sized solids with at least one dimension measuring between 1-100 nm or 10-1000 nm depending on the individual discipline's perspective. They are aggregates of anywhere from a few hundreds to tens of thousands of atoms which render them larger than molecules but smaller than bulk solids. Consequently, they frequently exhibit physical and chemical properties somewhere between. On the other hand, nanocrystals are a special class of nanoparticles which have started gaining attention recently owing to their unique crystalline structures which provide a larger surface area and promising applications including chiral separations. Hybrid nanoparticles are supported by the growing interest of chemists, physicists, and biologists, who are researching to fully exploit them. These materials can be defined as molecular or nano-composites with mixed (organic or bio) and inorganic components, where at least one of the component domain has a dimension ranging from a few Å to several nanometers. Similarly, and due to their extraordinary physical, chemical, and electrical properties, single-walled carbon nanotubes have been the subject of intense research. In this short review, the focus is mainly on the current well-established simple preparation techniques of chiral organic and hybrid nanoparticles as well as single-walled carbon nanotubes and their applications in separation science. Of particular interest, cinchonidine, chitosan, and β-CD-modified gold nanoparticles (GNPs) are discussed as model examples for organic and hybrid nanoparticles. Likewise, the chemical vapor deposition method, used in the preparation of single-walled carbon nanotubes, is discussed. The enantioseparation applications of these model nanomaterials is also presented.

  17. Status report of AMS sample preparation laboratory at GADAM Centre, Gliwice, Poland

    Energy Technology Data Exchange (ETDEWEB)

    Piotrowska, N., E-mail: natalia.piotrowska@polsl.pl [GADAM Centre of Excellence, Department of Radioisotopes, Institute of Physics, Silesian University of Technology, Gliwice (Poland)

    2013-01-15

    The laboratory for {sup 14}C AMS sample preparation in the Gliwice Radiocarbon Laboratory has gradually evolved since its start in 1999 to cater for an increase in volume and variety of radiocarbon dating samples. To date, nearly 2000 graphite targets have been produced from materials such as plant macrofossils, charcoal, peat, bones, shells and wood. The equipment comprises a station for chemical preparation and high vacuum lines for production, purification and graphitization of sample carbon dioxide. The present capacity allows preparation of up to 400 targets annually for the needs of scientific projects and external orders for radiocarbon dating continuously received by the GADAM Centre of Excellence. The laboratory's sample preparation protocols and recent improvements are described and its performance during the 10 years of activity is discussed in terms of parameters obtained from reference materials prepared in this laboratory and demonstrated with a few science applications.

  18. Recent trends in preparation and application of carbon nanotube-graphene hybrid thin films

    Science.gov (United States)

    Thanh Dang, Van; Dung Nguyen, Duc; Thanh Cao, Thi; Le, Phuoc Huu; Tran, Dai Lam; Phan, Ngoc Minh; Chuc Nguyen, Van

    2016-09-01

    The combination of one-dimensional (1D) carbon nanotubes (CNTs) and two-dimensional (2D) graphene materials to generate three-dimensional (3D) carbon nanotube-graphene hybrid thin films (CNGHTFs) has attracted great attention owing to their intriguing properties via the synergistic effects of these two materials on their electrical, optical, and electrochemical properties in comparison with their individual components. This review aims to provide a brief introduction of recent trends in preparation methodologies and some outstanding applications of CNGHTFs. It contains two main scientific subjects. The first of these is the research on preparation techniques of CNGHTFs, including reduction agent-assisted mechanical blending of reduced graphene oxide (rGO) and CNTs, hybridization methods for layer-by-layer (LBL) assembly of CNTs and rGO sheets, multi-step methods using combinations of a solution and chemical vapor deposition (CVD) processing, one-step growth of CNGHTFs by the CVD method, and modified CVD methods via thermal deposition of carbon source on catalyst surfaces. The advantages and disadvantages of the preparation methods of CNGHTFs are presented and discussed in detail. The second scientific subject of the review is the research on some outstanding applications of CNGHTFs in various research fields, including transparent conductors, electron field emitters, field-effect transistors, biosensors and supercapacitors. In most cases, the CNGHTFs showed superior performances than those of the pristine GO/graphene or CNT materials. Therefore, the CNGHTFs exhibit as high-potential materials for various practical applications. Opportunites and challenges in the fields are also presented.

  19. PNA-based fluorescence in situ hybridization for identification of bacteria in clinical samples

    DEFF Research Database (Denmark)

    Fazli, Mustafa; Bjarnsholt, Thomas; Høiby, Niels;

    2014-01-01

    Fluorescence in situ hybridization with PNA probes (PNA-FISH) that target specific bacterial ribosomal RNA sequences is a powerful and rapid tool for identification of bacteria in clinical samples. PNA can diffuse readily through the bacterial cell wall due to its uncharged backbone, and PNA-FISH....... In all these cases, bacteria can be identified in biofilm aggregates, which may explain their recalcitrance to antibiotic treatment.......Fluorescence in situ hybridization with PNA probes (PNA-FISH) that target specific bacterial ribosomal RNA sequences is a powerful and rapid tool for identification of bacteria in clinical samples. PNA can diffuse readily through the bacterial cell wall due to its uncharged backbone, and PNA......-FISH can be performed with high specificity due to the extraordinary thermal stability of RNA-PNA hybrid complexes. We describe a PNA-FISH procedure and provide examples of the application of PNA-FISH for the identification of bacteria in chronic wounds, cystic fibrosis lungs, and soft tissue fillers...

  20. Field Emission Properties of the Graphene Double-Walled Carbon Nanotube Hybrid Films Prepared by Vacuum Filtration and Screen Printing

    OpenAIRE

    Jinzhuo Xu; Tao Feng; Yiwei Chen; Zhuo Sun

    2013-01-01

    The graphene double-walled carbon nanotube (DWCNT) hybrid films were prepared by vacuum filtration and screen printing. Their electron field emission properties have been studied systematically. The electron emission properties of the hybrid films are much better than those of pure DWCNT films and pure graphene films. Comparing with the screen printed films, the vacuum filtered films have many advantages, such as lower turn-on field, higher emission current density, better uniformity, better ...

  1. Preparation of AgBr@SiO{sub 2} core@shell hybrid nanoparticles and their bactericidal activity

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yuanyuan [Key Laboratory for Special Functional Materials of Ministry of Education, Henan University, Kaifeng 475004 (China); Yang, Lisu [Key Laboratory for Special Functional Materials of Ministry of Education, Henan University, Kaifeng 475004 (China); Henna Sports School, Zhengzhou 450045 (China); Zhao, Yanbao, E-mail: yanbaozhao@126.com [Key Laboratory for Special Functional Materials of Ministry of Education, Henan University, Kaifeng 475004 (China); Li, Binjie; Sun, Lei; Luo, Huajuan [Key Laboratory for Special Functional Materials of Ministry of Education, Henan University, Kaifeng 475004 (China)

    2013-04-01

    AgBr@SiO{sub 2} core@shell hybrid nanoparticles (NPs) were successfully prepared by sol-gel method. Their morphology and structure were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The hybrid NPs are predominantly spherical in shape, with an average diameter of 180–200 nm, and each NP contains one inorganic core. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of the hybrid NPs were examined against Staphylococcus aureus (S. aureus), Pseudomonas aeruginosa (P. aeruginosa) and Escherichia coli (E. coli), respectively. Results indicated that the AgBr@SiO{sub 2} NPs had excellent antibacterial activity. - Highlights: ► Presents a novel antibacterial agent “AgBr@ SiO{sub 2} NPs”. ► AgBr@SiO{sub 2} hybrid NPs could provide long-term antimicrobial effect. ► AgBr@SiO{sub 2} hybrid NPs have excellent antibacterial activity.

  2. Sample preparation for atomic-resolution STEM at low voltages by FIB

    Energy Technology Data Exchange (ETDEWEB)

    Schaffer, Miroslava, E-mail: mschaffer@SuperSTEM.org [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Department of Engineering, George Holt Building, Ashton Street, Liverpool L69 3BX (United Kingdom); Schaffer, Bernhard [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Kelvin Nanocharacterisation Centre, SUPA School of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ, Scotland (United Kingdom); Ramasse, Quentin [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Department of Engineering, George Holt Building, Ashton Street, Liverpool L69 3BX (United Kingdom)

    2012-03-15

    While FIB sample preparation for transmission electron microscopy is a well established technique, few examples exist of samples of sufficient quality for atomic resolution imaging by aberration corrected (scanning) transmission electron microscopy (STEM). In this work we demonstrate the successful preparation of such samples from five different materials and present the refined lift-out preparation technique, which was applied here. Samples with parallel surfaces and a general thickness between 20 and 40 nm over a range of several {mu}m were repeatedly prepared and analyzed by Cs-corrected STEM at 60 and 100 kV. Here, a novel 'wedge pre-milling' step helps to keep the protective surface layers intact during the whole milling process, allowing features close to or at the sample surface to be analyzed without preparation damage. Another example shows the cross-sectional preparation of a working thin film solar cell device to a final thickness of 10 to 20 nm over {mu}m sized areas in the region of interest, enabling atomic resolution imaging and elemental mapping across general grain boundaries without projection artefacts. All sample preparation has been carried out in modern Dual-Beam FIB microscopes capable of low-kV Ga{sup +} ion milling, but without additional preparation steps after the FIB lift-out procedure. -- Highlights: Black-Right-Pointing-Pointer Suitability of stand-alone FIB preparation for atomic resolution STEM is shown. Black-Right-Pointing-Pointer Reproducible preparation of 10-40 nm thick samples from 5 different materials. Black-Right-Pointing-Pointer Low-kV milling and adjusted procedure for crystalline, homogeneously thin specimen. Black-Right-Pointing-Pointer Wedge pre-milling to protect surface-near features.

  3. Preparation and characterization of inorganic-organic trilayer core-shell polysilsesquioxane/polyacrylate/polydimethylsiloxane hybrid latex particles

    Science.gov (United States)

    Bai, Ruiqin; Qiu, Teng; Han, Feng; He, Lifan; Li, Xiaoyu

    2012-07-01

    The inorganic-organic trilayer core-shell polysilsesquioxane/polyacrylate/polydimethylsiloxane hybrid latex particles have been successfully prepared via seeded emulsion polymerization of acrylate monomers and octamethylcyclotetrasiloxane (D4) gradually, using functional polymethacryloxypropylsilsesquioxane (PSQ) latex particles with reactive methacryloxypropyl groups synthesized by the hydrolysis and polycondensation of (3-methacryloxypropyl)trimethoxysilane in the presence of mixed emulsifiers as seeds. The FTIR spectra show that acrylate monomers and D4 are effectively involved in the emulsion copolymerization and formed the polydimethylsiloxane-containing hybrid latex particles. Transmission electron microscopy (TEM) and dynamic light scattering (DLS) confirm that the resultant hybrid latex particles have evident trilayer core-shell structure and a narrow size distribution. XPS analysis also indicates that polysilsesquioxane/polyacrylate/polydimethylsiloxane hybrid latex particles have been successfully prepared and PDMS is rich in the surface of the hybrid latex film. Additionally, compared with the hybrid latex film without PDMS, the hybrid latex film containing PDMS shows higher hydrophobicity (water contact angle) and lower water absorption.

  4. Preparation and characterization of inorganic-organic trilayer core-shell polysilsesquioxane/polyacrylate/polydimethylsiloxane hybrid latex particles

    Energy Technology Data Exchange (ETDEWEB)

    Bai Ruiqin [College of Materials Science and Engineering, State Key Laboratory of Organic-Inorganic Composite, Key Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Qiu Teng, E-mail: qiuteng@mail.buct.edu.cn [College of Materials Science and Engineering, State Key Laboratory of Organic-Inorganic Composite, Key Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Han Feng; He Lifan [College of Materials Science and Engineering, State Key Laboratory of Organic-Inorganic Composite, Key Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Li Xiaoyu, E-mail: lixy@mail.buct.edu.cn [College of Materials Science and Engineering, State Key Laboratory of Organic-Inorganic Composite, Key Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China)

    2012-07-15

    The inorganic-organic trilayer core-shell polysilsesquioxane/polyacrylate/polydimethylsiloxane hybrid latex particles have been successfully prepared via seeded emulsion polymerization of acrylate monomers and octamethylcyclotetrasiloxane (D{sub 4}) gradually, using functional polymethacryloxypropylsilsesquioxane (PSQ) latex particles with reactive methacryloxypropyl groups synthesized by the hydrolysis and polycondensation of (3-methacryloxypropyl)trimethoxysilane in the presence of mixed emulsifiers as seeds. The FTIR spectra show that acrylate monomers and D{sub 4} are effectively involved in the emulsion copolymerization and formed the polydimethylsiloxane-containing hybrid latex particles. Transmission electron microscopy (TEM) and dynamic light scattering (DLS) confirm that the resultant hybrid latex particles have evident trilayer core-shell structure and a narrow size distribution. XPS analysis also indicates that polysilsesquioxane/polyacrylate/polydimethylsiloxane hybrid latex particles have been successfully prepared and PDMS is rich in the surface of the hybrid latex film. Additionally, compared with the hybrid latex film without PDMS, the hybrid latex film containing PDMS shows higher hydrophobicity (water contact angle) and lower water absorption.

  5. pH adjustment of human blood plasma prior to bioanalytical sample preparation

    NARCIS (Netherlands)

    Hendriks, G.; Uges, D. R. A.; Franke, J. P.

    2008-01-01

    pH adjustment in bioanalytical sample preparation concerning ionisable compounds is one of the most common sample treatments. This is often done by mixing an aliquot of the sample with a proper buffer adjusted to the proposed pH. The pH of the resulting mixture however, does not necessarily have to

  6. Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

    Science.gov (United States)

    Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

    2017-08-01

    Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

  7. Effect of sample preparation methods on photometric determination of the tellurium and cobalt content in the samples of copper concentrates

    Directory of Open Access Journals (Sweden)

    Viktoriya Butenko

    2016-03-01

    Full Text Available Methods of determination of cobalt and nickel in copper concentrates currently used in factory laboratories are very labor intensive and time consuming. The limiting stage of the analysis is preliminary chemical sample preparation. Carrying out the decomposition process of industrial samples with concentrated mineral acids in open systems does not allow to improve the metrological characteristics of the methods, for this reason improvement the methods of sample preparation is quite relevant and has a practical interest. The work was dedicated to the determination of the optimal conditions of preliminary chemical preparation of copper concentrate samples for the subsequent determination of cobalt and tellurium in the obtained solution using tellurium-spectrophotometric method. Decomposition of the samples was carried out by acid dissolving in individual mineral acids and their mixtures by heating in an open system as well as by using ultrasonification and microwave radiation in a closed system. In order to select the optimal conditions for the decomposition of the samples in a closed system the phase contact time and ultrasonic generator’s power were varied. Intensification of the processes of decomposition of copper concentrates with nitric acid (1:1, ultrasound and microwave radiation allowed to transfer quantitatively cobalt and tellurium into solution spending 20 and 30 min respectively. This reduced the amount of reactants used and improved the accuracy of determination by running the process in strictly identical conditions.

  8. Fluorescence in situ hybridization rapidly detects three different pathogenic bacteria in urinary tract infection samples.

    Science.gov (United States)

    Wu, Qing; Li, Yan; Wang, Ming; Pan, Xiao P; Tang, Yong F

    2010-11-01

    The detection of pathogenic bacteria in urine is an important criterion for diagnosing urinary tract infections (UTIs). By using fluorescence in situ hybridization (FISH) with rRNA-targeted, fluorescently labeled oligonucleotide probes, bacterial pathogens present in urine samples were identified within 3-4 h. In this study, three probes that are specific for Escherichia coli, Enterococcus faecalis and Staphylococcus aureus were designed based on the conserved 16S RNA sequences, whereas probe Eub338 broadly recognizes all bacteria. We collected a total of 1000 urine samples, and 325 of these samples tested positive for a UTI via traditional culturing techniques; additionally, all 325 of these samples tested positive with the Eub338 probe in FISH analysis. FISH analyses with species-specific probes were performed in parallel to the test the ability to differentiate among several pathogenic bacteria. The samples for these experiments included 76 E. coli infected samples, 32 E. faecalis infected samples and 9 S. aureus infected samples. Compared to conventional methods of bacterial identification, the FISH method produced positive results for >90% of the samples tested. FISH has the potential to become an extremely useful diagnostic tool for UTIs because it has a quick turnaround time and high accuracy.

  9. Preparation and investigation of bulk and thin film samples of strontium ferrite

    Directory of Open Access Journals (Sweden)

    A Poorbafrani

    2008-07-01

    Full Text Available   In this article, bulk and thin film samples of strontium ferrite have been studied. Due to the high electrical resistivity in strontium ferrite, energy loss due to eddy currents reduces and because of this, it can be used in high frequency magnetic circuits. On the other hand, strontium ferrite has attracted much attention as a permanent magnet. At first, we study the preparation process of bulk samples of strontium ferrite by a solid state reaction technique. In preparation of samples, to optimize the magnetic properties, we have used the stoichiometry factor (n = Fe2O3 / SrO of 5.25. In addition, we have used additives such as CaO and SiO2 to control grain growth. The samples have been prepared in two series: Isotropic and Anisotropic. For preparation of anisotropic samples, the magnetic field of 1T has been used for orientation of the grains during the press. Then, X-ray diffraction, Scanning Electron Microscopy (SEM, EDAX analysis and Magnetometer, was used for analyzing and comparing of structural and magnetic properties of isotropic and anisotropic samples. The results indicate that, due to the applied magnetic field, the structural and Magnetic properties of anisotropic samples improved efficiently because of the orientation of the grains during the press. In the next stage, we used bulk samples to prepare strontium ferrite thin films by Pulsed Laser Deposition technique (PLD. The Si (111 substrate has been used to prepare the thin films. Then we have studied the microstructure of thin films by X-ray diffraction, SEM and EDAX analysis. These studies on different samples show that for the preparation of crystalline phase of strontium ferrite thin films, the substrate temperature must be higher than 800˚C. The optimum conditions for preparation of strontium, ferrite thin films have been achieved on the substrate temperature of 840˚C and oxygen pressure of 75 mtorr.

  10. Preparation and characterization of phosphorylated Zr-doped hybrid silica/PSF composite membrane.

    Science.gov (United States)

    Zhang, Yuqing; Jin, Zhenhua; Shan, Xing; Sunarso, Jaka; Cui, Ping

    2011-02-15

    Polysulfone (PSF) membranes are broadly applied in many fields owing to good physicochemical stability, resistance to oxidation and chlorine. But when treated with wastewater containing oil, PSF membranes are easy to be contaminated for its hydrophobicity, which can result in the declining of flux and lifespan of the membrane and limit their application in large scale. To enhance the capability of PSF membrane in the above circumstances, phosphorylated Zr-doped hybrid silica particles (SZP particles) were firstly prepared. SZP particles have various point defects inside their structure and lots of hydroxide radicals on their surface. SZP particles were added to the porous matrix of PSF to prepare a novel composite membrane (SZP/PSF) through a phase inversion process. Finally, the optimum preparation conditions of SZP/PSF composite membranes were determined. The optimum conditions are: the mass ratio of PSF, PEG400 and SZP is 12:10:10; ultrasound 10 min inside each 30 min; the pre-evaporating time is 10s. Optimized SZP/PSF composite membrane was characterized by scanning electron microscope (SEM) and ultrafiltration experiment. The results indicate that SZP particles can be uniformly dispersed in SZP/PSF composite membranes with excellent hydrophilic property, antifouling capability and tensile strength. Therefore, it can be concluded that the optimized SZP/PSF composite membrane is desirable in the treatment of wastewater containing oil and wastewater.

  11. Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared Detector Samples

    Science.gov (United States)

    2015-11-13

    Approved for Public Release; Distribution Unlimited Final Report: Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared...Final Report: Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared Detector Samples Report Title A used calibrated...camera will reinitialize and the video settings have to be reset. 6 Figure 4. This will open the both video overlay and the Dektak

  12. Preparation, characterization and application of organic-inorganic hybrid caffeine imprinted monolith.

    Science.gov (United States)

    Liu, Xiaofang; Sun, Na; Zhu, Quanfei; Wu, Mei; Ye, Yong; Chen, Huaixia

    2013-08-23

    The present work aims to synthesize an organic-inorganic hybrid caffeine imprinted monolith using one-step method. The synthesis conditions such as the type of inorganic precursor and porogenic solvent, the molar ratios of the monomer and cross-linker, the volume ratio of the inorganic alcoholysate and organic part were optimized. The morphology of the monolith was studied by scanning electron microscopy and Fourier transform infrared spectra. The imprinted factor of the monolith for caffeine reached 3.02. A simple, rapid and sensitive method for the determination of caffeine in children's milk using the organic-inorganic hybrid caffeine imprinted polymer monolith microextraction combined with high-performance liquid chromatography-photodiodes array detector was developed. Several parameters affecting the sample pretreatment were investigated, including the type, flow rate and volume of eluent, the flow rate and volume of sample solution. The assay exhibited a linear dynamic range of 8-500μgL(-1) with the correlation coefficient above 0.9987. Lower limits of detection (LOD, at S/N=3) and quantification (LOQ, at S/N=10) in children's milk samples were 2.7 and 8μgL(-1). Recoveries of caffeine from spiked children's milk ranged from 85 to 104% with relative standard deviations of less than 8.9%.

  13. Advanced Curation Activities at NASA: Preparing for the Next Waves of Astromaterials Sample Return

    Science.gov (United States)

    Zeigler, R. A.; Allton, J. H.; Evans, C. A.; Fries, M. D.; McCubbin, F. M.; Nakamura-Messenger, K.; Righter, K.; Zolensky, M.; Stansbery, E. K.

    2017-02-01

    We discuss the current curatorial efforts for NASA's astromaterials collections, as well as efforts that are underway (or need to be undertaken) to prepare for the challenging curation conditions required by future sample return missions.

  14. Simple and Reproducible Sample Preparation for Single-Shot Phosphoproteomics with High Sensitivity

    DEFF Research Database (Denmark)

    Jersie-Christensen, Rosa R.; Sultan, Abida; Olsen, Jesper V

    2016-01-01

    The traditional sample preparation workflow for mass spectrometry (MS)-based phosphoproteomics is time consuming and usually requires multiple steps, e.g., lysis, protein precipitation, reduction, alkylation, digestion, fractionation, and phosphopeptide enrichment. Each step can introduce chemica...

  15. Robotic, MEMS-based Multi Utility Sample Preparation Instrument for ISS Biological Workstation Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This project will develop a multi-functional, automated sample preparation instrument for biological wet-lab workstations on the ISS. The instrument is based on a...

  16. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 2, Sample preparation methods

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOC and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.

  17. Preparation of Cu2ZnSnS4 thin films by hybrid sputtering

    Science.gov (United States)

    Tanaka, Tooru; Nagatomo, Takeshi; Kawasaki, Daisuke; Nishio, Mitsuhiro; Guo, Qixin; Wakahara, Akihiro; Yoshida, Akira; Ogawa, Hiroshi

    2005-11-01

    In order to fabricate Cu2ZnSnS4 thin films, hybrid sputtering system with two sputter sources and two effusion cells is used. The Cu2ZnSnS4 films are fabricated by the sequential deposition of metal elements and annealing in S flux, varying the substrate temperature. The Cu2ZnSnS4 films with stoichiometric composition are obtained at the substrate temperature up to 400 °C, whereas the film composition becomes quite Zn-pool at the substrate temperature above 450 °C. The Cu2ZnSnS4 film shows p-type conductivity, and the optical absorption coefficient and the band gap of the Cu2ZnSnS4 film prepared in this experiment are suitable for fabricating a thin film solar cell.

  18. Preparation of P(DVB-co-MPS) inorganic-organic hybrid polymer microspheres

    Science.gov (United States)

    Wu, Chunrong; Zhang, Jimei; Dai, Zhao; Chen, Xiaoyu

    2010-07-01

    A novel inorganic-organic hybrid polymer microspheres were facilely synthesised by distillation-precipitation polymerization in absence of any stabilizer or surfcant. The process were conducted with [3-(Methacryloyloxy) propyl] trimethoxysilan (MPS) as monomer, divinyl benzene (DVB) as cross linking agent and azobisisobutyronitrile (AIBN) as initator in acetonitrile. A series of silica nanoparticles were prepared in accordance with the volume ratio of MPS, which was varied in the range of 10% to 50%. However, there is no microspheres obtained while the ratio up to 50%. Products were charactered by transmission electron micrograph (TEM) and fourier transform infrared spectroscopy (FTIR). We may infer it from the constructional formular and FTIR graph that there were silicon hydroxyl remained in the microsphere surface.

  19. [Preparation, characterization and surface-enhanced Raman properties of agarose gel/gold nanoparticles hybrid].

    Science.gov (United States)

    Ma, Xiao-yuan; Liu, Ying; Wang, Zhou-ping

    2014-08-01

    Agarose gel/gold nanoparticles hybrid was prepared by adding gold nanoparticles to preformed agarose gel. Naniocomposite structures and properties were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and UV-Vis-NIR absorption spectroscopy. Experimental data indicated a uniform distribution of gold nanoparticles adsorbed on agarose gel network And the excellent optical absorption properties were shown. Based on the swelling-contraction characteristics of agarose gel and the adjustable localized surface plasmon resonance (LSPR) of the gold nanoparticles, the nano-composites were used as surface enhanced Raman scattering (SERS) substrate to detect the Raman signal molecules Nile blue A. Results revealed that the porous structure of the agarose gel provided a good carrier for the enrichment of the gold nanoparticles. The gold nanoparticles dynamic hot-spot effect arising from the agarose gel contraction loss of water in the air greatly enhanced the Raman signal.

  20. Synthesis of organic-inorganic hybrid azobenzene materials for the preparation of nanofibers by electrospinning

    Science.gov (United States)

    Bućko, Aleksandra; Zielińska, Sonia; Ortyl, Ewelina; Larkowska, Maria; Barille, Regis

    2014-12-01

    The new photochromic hybrid materials containing different mole fractions of highly photoactive 4-[(E)-[4-[ethyl(2-hydroxyethyl)amino]phenyl]azo]-N-(4-methylpyrimidin-2-yl)benzenesulfonamide (SMERe) were prepared by a low temperature sol-gel process. The guest-host systems with triethoxyphenylsilane matrix were obtained. These materials were used to form thin transparent films by a spin-coating technique. Then the ability of thin hybrid films to reversible trans-cis photoisomerization under illumination was investigated using ellipsometry and UV-Vis spectroscopy. The reversible changes of refractive index of the films under illumination were in the range of 0.005-0.056. The maximum absorption of these materials was located at 462-486 nm. Moreover, the organic-inorganic azobenzene materials were used to form nanofibers by electrospinning using various parameters of the process. The microstructure of electrospun fibers depended on sols properties (e.g. concentration and viscosity of the sols) and process conditions (e.g. the applied voltage, temperature or type of the collector) at ambient conditions. The morphology of obtained nanofibers was analyzed by an optical microscopy and scanning electron microscopy. In most instances, the beadless fibers were obtained. The wettability of the surface of electrospun fibers deposited on glass substrates was investigated.

  1. New Inorganic-organic Hybrid Tetravanadate:Preparation, Characterization and Application in Chemically Modified Electrode

    Institute of Scientific and Technical Information of China (English)

    SUN Ying-hua; LI Xiao-ping; MEI Ze-min; ZHU Yu; NIU Li

    2011-01-01

    A new inorganic-organic hybrid tetravanadate [Co(2,2'-bpy)3]2V4O12.llH2O(l) has been prepared and characterized. X-Ray diffraction study reveals that compound 1 contains classical cluster anions [V4O12]4-, coordi nated cations [Co(2,2'-bpy)3]2+ and eleven water molecules, in which an interesting decamer water cluster is formed.The hybrid nanoparticles were firstly used as a bulk-modifier to fabricate a chemically modified paste electrode (1-CPE). The electrochemical behavior and electrocatalysis of 1-CPE have been studied in detail. The results indicate that 1-CPE has a good electrocatalytic activity toward the reduction of bromate in a 0.5 mol/L H2SO4 aqueous solu tion. I-CPE shows remarkable stability that be ascribed to the hydrogen bonding interactions between V4O12 cluster and water cluster, which are very important for practical application in electrode modification.

  2. Preparation of testate amoebae samples affects water table depth reconstructions in peatland palaeoecological studies

    Directory of Open Access Journals (Sweden)

    Eve Avel

    2013-05-01

    Full Text Available In peatland palaeoecological studies, the preparation of peat samples for testate amoebae (TA analysis involves boiling of samples and microsieving them through a 15-μm sieve. We studied the effect of these preparation stages on the estimation of TA assemblages and on the reconstruction of water table depths (WTD. Our results indicate that the TA assemblages of boiled and unboiled samples are not significantly different, while microsieving reduces the concentration of small TA taxa and results in significantly different TA assemblages. The differences between microsieved and unsieved TA assemblages were reflected also in predicted values of WTD, which indicated drier conditions in case of unsieved samples than in microsieved samples. We conclude that the boiling of samples might be omitted if TA are extracted from the fresh peat samples. Microsieving may lead to erroneous palaeoecological WTD reconstructions and should be avoided if small TA taxa are present in samples.

  3. On radiation damage in FIB-prepared softwood samples measured by scanning X-ray diffraction.

    Science.gov (United States)

    Storm, Selina; Ogurreck, Malte; Laipple, Daniel; Krywka, Christina; Burghammer, Manfred; Di Cola, Emanuela; Müller, Martin

    2015-03-01

    The high flux density encountered in scanning X-ray nanodiffraction experiments can lead to severe radiation damage to biological samples. However, this technique is a suitable tool for investigating samples to high spatial resolution. The layered cell wall structure of softwood tracheids is an interesting system which has been extensively studied using this method. The tracheid cell has a complex geometry, which requires the sample to be prepared by cutting it perpendicularly to the cell wall axis. Focused ion beam (FIB) milling in combination with scanning electron microscopy allows precise alignment and cutting without splintering. Here, results of a scanning X-ray diffraction experiment performed on a biological sample prepared with a focused ion beam of gallium atoms are reported for the first time. It is shown that samples prepared and measured in this way suffer from the incorporation of gallium atoms up to a surprisingly large depth of 1 µm.

  4. 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.

  5. Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel.

    Science.gov (United States)

    Robinson, T; Bronson, B; Gogolek, P; Mehrani, P

    2016-02-01

    Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF.

  6. Expanding the application of the tablet processing workstation to support the sample preparation of oral suspensions.

    Science.gov (United States)

    Opio, Alex Manuel; Nickerson, Beverly; Xue, Gang; Warzeka, John; Norris, Ken

    2011-06-01

    Sample preparation is the most time-consuming part of the analytical method for powder for oral suspension (POS) assay, purity, and preservative analysis, as this involves multiple dilution and filtration steps. The Tablet Processing Workstation (TPW) was used to automate the sample preparation of a POS formulation. Although the TPW is typically used to automate the preparation of solid oral dosage forms and powders, it contains all of the necessary components to perform POS sample preparation. The TPW exhibited acceptable repeatability in testing 3 lots using 10 replicate preparations per lot. Acceptable linearity of the drug and preservative in the presence of excipients was demonstrated over the range corresponding to 50-150% of intent. Accuracy showed suitable recoveries for all points evaluated. TPW results were shown to correlate to results obtained with the manual method. The TPW method was used to prepare samples in support of manufacturing scale-up efforts. With the efficiencies gained using the TPW, it was possible to analyze a large number of samples generated during process development activities for the POS formulation with minimal human intervention. The extensive data enabled trending of the manufacturing development runs and helped to identify optimization strategies for the process.

  7. Dummy molecularly imprinted mesoporous silica prepared by hybrid imprinting method for solid-phase extraction of bisphenol A.

    Science.gov (United States)

    Yu, Dan; Hu, Xiaolei; Wei, Shoutai; Wang, Qiang; He, Chiyang; Liu, Shaorong

    2015-05-29

    A novel hybrid dummy imprinting strategy was developed to prepare a mesoporous silica for the solid-phase extraction (SPE) of bisphenol A (BPA). A new covalent template-monomer complex (BPAF-Si) was first synthesized with 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BPAF) as the template. The imprinted silica was obtained through the gelation of BPAF-Si with tetraethoxysilane and the subsequent removal of template by thermal cleavage, and then it was characterized by FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption-desorption isotherms. Results showed that the new silica had micron-level particle size and ordered mesoporous structure. The static binding test verified that the imprinted silica had much higher recognition ability for BPA than the non-imprinted silica. The imprinted silica also showed high extraction efficiencies and high enrichment factor for SPE of BPA. Using the imprinted silica, a SPE-HPLC-UV method was developed and successfully applied for detecting BPA in BPA-spiked tap water and lake water samples with a recovery of 99-105%, a RSD of 2.7-5.0% and a limit of detection (S/N=3) of 0.3ng/mL. The new imprinted silica avoided the interference of the residual template molecules and reduced the non-specific binding sites, and therefore it can be utilized as a good sorbent for SPE of BPA in environmental water samples.

  8. Cytotoxicity of Light-Cured Dental Materials according to Different Sample Preparation Methods

    Science.gov (United States)

    Lee, Myung-Jin; Kim, Mi-Joo; Kwon, Jae-Sung; Lee, Sang-Bae; Kim, Kwang-Mahn

    2017-01-01

    Dental light-cured resins can undergo different degrees of polymerization when applied in vivo. When polymerization is incomplete, toxic monomers may be released into the oral cavity. The present study assessed the cytotoxicity of different materials, using sample preparation methods that mirror clinical conditions. Composite and bonding resins were used and divided into four groups according to sample preparation method: uncured; directly cured samples, which were cured after being placed on solidified agar; post-cured samples were polymerized before being placed on agar; and “removed unreacted layer” samples had their oxygen-inhibition layer removed after polymerization. Cytotoxicity was evaluated using an agar diffusion test, MTT assay, and confocal microscopy. Uncured samples were the most cytotoxic, while removed unreacted layer samples were the least cytotoxic (p cytotoxicity. Clinicians should remove unreacted monomers on the resin surface immediately after restoring teeth with light-curing resin to improve the restoration biocompatibility. PMID:28772647

  9. Preparation and characterization of microporous fibers for sample preparation and LC-MS determination of drugs.

    Science.gov (United States)

    Buszewski, Boguslaw; Nowaczyk, Jacek; Ligor, Tomasz; Olszowy, Pawel; Ligor, Magdalena; Wasiniak, Bartlomiej; Miekisch, Wolfram; Schubert, Jochen K; Amann, Anton

    2009-07-01

    The aim of this study was the preparation of polypyrrole (PPy) fibers for solid phase microextraction (SPME). PPy coatings were obtained during the electrochemical polymerization process. The utility of various metal wires (Fe, Cu, Ag, Cu/Ag, kanthal and medical stainless steel) as a support for polymers was compared. Various experimental conditions of the synthesis process such as scan rate, voltage limits and number of scans and deposition time were applied. The average polymer thickness was in the range of 7-125 microm and its weight was in the scope of 0.65-5.6 mg. Different techniques, mainly elemental analysis, Fourier transform infrared spectroscopy, microscopy, and chromatography were performed for the characterization of obtained fibers with microporous structure. The extraction efficiency of cardiovascular drugs (metoprolol, propranolol, oxprenolol, propafenone and mexiletine) by means of fibers was tested. The concentration of mentioned compounds in standard solution was in the span of 10-150 ng/mL. LC-MS was employed for determination of drugs in desorption solution. LODs varied from 0.013 to 1.51 ng/mL for metoprolol and mexiletine respectively. The repeatability of extraction was obtained with the RSD values lower than 10%.

  10. Preparing Teachers to Use GIS: The Impact of a Hybrid Professional Development Program on Teachers' Use of GIS

    Science.gov (United States)

    Moore, Steven; Haviland, Don; Moore, William; Tran, Michael

    2016-08-01

    This article reports the findings of a 3-year study of a hybrid professional development program designed to prepare science and mathematics teachers to implement GIS in their classrooms. The study was conducted as part of the CoastLines Innovative Technology Experiences for Students and Teachers project funded by the National Science Foundation. Three cohorts of teachers participated in the program, with each participant receiving 40 h of synchronous online instruction and 80 h of in-person instruction and support over an 8-month period. Data from surveys of participants both before and after the program were analyzed using correlation, ordinary least squares, and ordered logit regression analyses. The analyses revealed increases in the self-reported frequency of GIS use and enhanced feelings of preparation, competence, community, and comfort with respect to using GIS for instruction. A composite index of all impact variables was positively influenced as well. The statistical analyses found a strong relationship between self-reported feelings of preparation and use of GIS. Some support was found for the idea that feelings of competence, community, and comfort were related to the teachers' sense of preparation. The findings suggest that a robust hybrid model of teacher professional development can prepare teachers to use GIS in their classrooms. More research is needed to understand how hybrid models influence the sociopsychological and other dimensions that support teachers' feelings of preparation to implement GIS.

  11. Preparing Teachers to Use GIS: The Impact of a Hybrid Professional Development Program on Teachers' Use of GIS

    Science.gov (United States)

    Moore, Steven; Haviland, Don; Moore, William; Tran, Michael

    2016-12-01

    This article reports the findings of a 3-year study of a hybrid professional development program designed to prepare science and mathematics teachers to implement GIS in their classrooms. The study was conducted as part of the CoastLines Innovative Technology Experiences for Students and Teachers project funded by the National Science Foundation. Three cohorts of teachers participated in the program, with each participant receiving 40 h of synchronous online instruction and 80 h of in-person instruction and support over an 8-month period. Data from surveys of participants both before and after the program were analyzed using correlation, ordinary least squares, and ordered logit regression analyses. The analyses revealed increases in the self-reported frequency of GIS use and enhanced feelings of preparation, competence, community, and comfort with respect to using GIS for instruction. A composite index of all impact variables was positively influenced as well. The statistical analyses found a strong relationship between self-reported feelings of preparation and use of GIS. Some support was found for the idea that feelings of competence, community, and comfort were related to the teachers' sense of preparation. The findings suggest that a robust hybrid model of teacher professional development can prepare teachers to use GIS in their classrooms. More research is needed to understand how hybrid models influence the sociopsychological and other dimensions that support teachers' feelings of preparation to implement GIS.

  12. Reagent preparation and storage for amplification of microarray hybridization targets with a fully automated system.

    Science.gov (United States)

    Zhou, Mingjie; Marlowe, Jon; Graves, Jaime; Dahl, Jason; Riley, Zackery; Tian, Lena; Duenwald, Sven; Tokiwa, George; Fare, Thomas L

    2007-08-01

    The advent of automated systems for gene expression profiling has accentuated the need for the development of convenient and cost-effective methods for reagent preparation. We have developed a method for the preparation and storage of pre-aliquoted cocktail plates that contain all reagents required for amplification of nucleic acid by reverse transcription and in vitro transcription reactions. Plates can be stored at -80 degrees C for at least 1 month and kept in a hotel at 4 degrees C for at least 24 h prior to use. Microarray data quality generated from these pre-aliquoted reagent plates is not statistically different between cRNA amplified with stored cocktails and cRNA amplified with freshly prepared cocktails. Deployment of pre-aliquoted, stored cocktail plates in a fully automated system not only increases the throughput of amplifying cRNA targets from thousands of RNA samples, but could also considerably reduce reagent costs and potentially improve process robustness.

  13. Preparation of Pd/Bacterial Cellulose Hybrid Nanofibers for Dopamine Detection

    Directory of Open Access Journals (Sweden)

    Dawei Li

    2016-05-01

    Full Text Available Palladium nanoparticle-bacterial cellulose (PdBC hybrid nanofibers were synthesized by in-situ chemical reduction method. The obtained PdBC nanofibers were characterized by a series of analytical techniques. The results revealed that Pd nanoparticles were evenly dispersed on the surfaces of BC nanofibers. Then, the as-prepared PdBC nanofibers were mixed with laccase (Lac and Nafion to obtain mixture suspension, which was further modified on electrode surface to construct novel biosensing platform. Finally, the prepared electrochemical biosensor was employed to detect dopamine. The analysis result was satisfactory, the sensor showed excellent electrocatalysis towards dopamine with high sensitivity (38.4 µA·mM−1, low detection limit (1.26 µM, and wide linear range (5–167 µM. Moreover, the biosensor also showed good repeatability, reproducibility, selectivity and stability and was successfully used in the detection of dopamine in human urine, thus providing a promising method for dopamine analysis in clinical application.

  14. Reducing Spatial Heterogeneity of MALDI Samples with Marangoni Flows During Sample Preparation

    Science.gov (United States)

    Lai, Yin-Hung; Cai, Yi-Hong; Lee, Hsun; Ou, Yu-Meng; Hsiao, Chih-Hao; Tsao, Chien-Wei; Chang, Huan-Tsung; Wang, Yi-Sheng

    2016-08-01

    This work demonstrates a method to prepare homogeneous distributions of analytes to improve data reproducibility in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). Natural-air drying processes normally result in unwanted heterogeneous spatial distributions of analytes in MALDI crystals and make quantitative analysis difficult. This study demonstrates that inducing Marangoni flows within drying droplets can significantly reduce the heterogeneity problem. The Marangoni flows are accelerated by changing substrate temperatures to create temperature gradients across droplets. Such hydrodynamic flows are analyzed semi-empirically. Using imaging mass spectrometry, changes of heterogeneity of molecules with the change of substrate temperature during drying processes are demonstrated. The observed heterogeneities of the biomolecules reduce as predicted Marangoni velocities increase. In comparison to conventional methods, drying droplets on a 5 °C substrate while keeping the surroundings at ambient conditions typically reduces the heterogeneity of biomolecular ions by 65%-80%. The observation suggests that decreasing substrate temperature during droplet drying processes is a simple and effective means to reduce analyte heterogeneity for quantitative applications.

  15. Preparation of ZnO/CdS/BC Photocatalyst Hybrid Fiber and Research of Its Photocatalytic Properties

    Directory of Open Access Journals (Sweden)

    Beibei Dai

    2015-01-01

    Full Text Available An environment-friendly biomaterial bacterial cellulose (BC is introduced to substitute general organic polymers to assist the preparation of ZnO/CdS/BC photocatalyst hybrid nanofiber through coprecipitation method under the low-temperature condition. The XRD, XPS, and SEM results show that high load of ZnO/CdS/BC ternary hybrid fiber can be produced. TGA curves scan shows that ZnO/CdS/BC hybrid fiber has better thermal properties than bacterial cellulose. The UV-Vis spectra of the ZnO/CdS/BC hybrid nanofiber (0, 10, 20, and 50 wt%, resp. show that photocatalytic activities of ZnO/CdS/BC are influenced by the added amount of CdS. The degradation curve of methyl shows that ZnO/CdS/BC nanohybrid fibers exhibit excellent photocatalytic efficiency.

  16. Durable antibacterial Ag/polyacrylonitrile (Ag/PAN) hybrid nanofibers prepared by atmospheric plasma treatment and electrospinning

    Science.gov (United States)

    Durable antibacterial Ag/polyacrylonitrile (Ag/PAN) hybrid nanofibers were prepared by atmospheric plasma treatment and electrospinning. Atmospheric helium plasma treatment was first used to reduce the silver nitrate precursor in pre-electrospinning solutions into metallic silver nanoparticles, foll...

  17. Retrospective study of trisomy 18 in chorionic villi with fluorescent in situ hybridization on archival direct preparations

    NARCIS (Netherlands)

    A.R.M. van Opstal (Diane); C.D.F. van den Berg (Cardi); M.G. Jahoda (M.); H. Brandenburg (Helen); F.J. Los; P.A. In't Veld (Peter)

    1995-01-01

    textabstractTrisomy 18 in direct chorionic villus preparations needs further investigation since the chromosome abnormality may be confined to the placenta and may not represent the actual fetal karyotype. We performed, retrospectively, fluorescent in situ hybridization (FISH) with the chromosome 18

  18. Repeating cytological preparations on liquid-based cytology samples: A methodological advantage?

    Science.gov (United States)

    Pinto, Alvaro P; Maia, Henrique Felde; di Loretto, Celso; Krunn, Patrícia; Túlio, Siumara; Collaço, Luis Martins

    2007-10-01

    This study investigates the rule that repeating cytological preparations on liquid-based cytology improves sample adequacy, diagnosis, microbiological, and hormonal evaluations. We reviewed 156 cases of pap-stained preparations of exfoliated cervical cells in two slides processed by DNA-Cytoliq System. After sample repeat/dilution, limiting factors affecting sample adequacy were removed in nine cases and three unsatisfactory cases were reclassified as satisfactory. Diagnosis was altered in 24 cases. Of these, the original diagnosis in 15 was atypical squamous cells of undetermined significance; after the second slide examination, diagnosis in 5 of the 15 cases changed to low-grade squamous intraepithelial lesion, 3 to high-grade squamous intraepithelial lesion, and 7 to absence of lesion. Microbiological evaluation was altered, with Candida sp. detected in two repeated slides. Repeat slide preparation or dilution of residual samples enhances cytological diagnosis and decreases effects of limiting factors in manually processed DIGENE DCS LBC.

  19. Development of a high vacuum sample preparation system for helium mass spectrometer

    Science.gov (United States)

    Kumar, P.; Das, N. K.; Mallik, C.; Bhandari, R. K.

    2012-11-01

    A high vacuum sample preparation system for the 3He/4He ratio mass spectrometer (Helix SFT) has been developed to remove all the gaseous constituents excluding helium from the field gases. The sample preparation system comprises of turbo molecular pump, ion pump, zirconium getter, pipettes and vacuum gauges with controller. All these are fitted with cylindrical SS chamber using all metal valves. The field samples are initially treated with activated charcoal trap immersed in liquid nitrogen to cutoff major impurities and moisture present in the sample gas. A sample of 5 ml is collected out of this stage at a pressure of 10-2 mbar. This sample is subsequently purified at a reduced pressure of 10-7 mbar before it is injected into the ion source of the mass spectrometer. The sample pressure was maintained below 10-7 mbar with turbo molecular vacuum pumps and ion pumps. The sample gas passes through several getter elements and a cold finger with the help of manual high vacuum valves before it is fed to the mass spectrometer. Thus the high vacuum sample preparation system introduces completely clean, dry and refined helium sample to the mass spectrometer for best possible analysis of isotopic ratio of helium.

  20. Preparation of electrochemically reduced graphene oxide/multi-wall carbon nanotubes hybrid film modified electrode, and its application to amperometric sensing of rutin

    Indian Academy of Sciences (India)

    Uling Yang; Gang Li; Meifang Hu; Lingbo Qu

    2014-07-01

    Through a facile electrochemical method, we prepared an electrochemically reduced graphene oxide (ERGO)/multi-wall carbon nanotubes (MWNTs) hybrid film modified glassy carbon electrode (GCE), and characterized it by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and x-ray diffraction (XRD) The experimental results demonstrated that ERGO-MWNTs/GCE exhibited excellent electrocatalytic activity toward rutin as evidenced by the significant enhancement of redox peak currents in comparison with a bare GCE, ERGO/GCE and MWNTs/GCE. This method has been applied for the direct determination of rutin in real samples with satisfactory results.

  1. Electromembrane extraction as a rapid and selective miniaturized sample preparation technique for biological fluids

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Pedersen-Bjergaard, Stig; Seip, Knut Fredrik

    2015-01-01

    This special report discusses the sample preparation method electromembrane extraction, which was introduced in 2006 as a rapid and selective miniaturized extraction method. The extraction principle is based on isolation of charged analytes extracted from an aqueous sample, across a thin film....... Technical aspects of electromembrane extraction, important extraction parameters as well as a handful of examples of applications from different biological samples and bioanalytical areas are discussed in the paper....

  2. TruSeq Stranded mRNA and Total RNA Sample Preparation Kits

    Science.gov (United States)

    Total RNA-Seq enabled by ribosomal RNA (rRNA) reduction is compatible with formalin-fixed paraffin embedded (FFPE) samples, which contain potentially critical biological information. The family of TruSeq Stranded Total RNA sample preparation kits provides a unique combination of unmatched data quality for both mRNA and whole-transcriptome analyses, robust interrogation of both standard and low-quality samples and workflows compatible with a wide range of study designs.

  3. Real-time assessment of hybridization between wolves and dogs: combining noninvasive samples with ancestry informative markers.

    Science.gov (United States)

    Godinho, Raquel; López-Bao, José Vicente; Castro, Diana; Llaneza, Luís; Lopes, Susana; Silva, Pedro; Ferrand, Nuno

    2015-03-01

    Wolves and dogs provide a paradigmatic example of the ecological and conservation implications of hybridization events between wild and domesticated forms. However, our understanding of such implications has been traditionally hampered by both high genetic similarity and the difficulties in obtaining tissue samples (TS), which limit our ability to assess ongoing hybridization events. To assess the occurrence and extension of hybridization in a pack of wolf-dog hybrids in northwestern Iberia, we compared the power of 52 nuclear markers implemented on TS with a subset of 13 ancestry informative markers (AIMs) typed in noninvasive samples (NIS). We demonstrate that the 13 AIMs are as accurate as the 52 markers that were chosen without regard to the power to differentiate between wolves and dogs, also having the advantage of being rapidly screened on NIS. The efficiency of AIMs significantly outperformed ten random sets of similar size and an additional commercial set of 18 markers. Bayesian clustering analysis implemented on AIMs and NIS identified nine hybrids, two wolves and two dogs. Four hybrids were unambiguously assigned to F1xWolf backcrosses. Our approach (AIMs + NIS) overcomes previous difficulties related to sample availability and informative power of markers, allowing a quick identification of wolf-dog hybrids in the first phases of hybridization episodes. This provides managers with a reliable tool to evaluate hybridization and estimate the success of their actions. This approach may be easily adapted for other pairs of wild/domesticated species, thus improving our understanding of the introgression of domestication genes into natural populations. © 2014 John Wiley & Sons Ltd.

  4. Hybrid micro-/nano-structures derived from metal-organic frameworks: preparation and applications in energy storage and conversion.

    Science.gov (United States)

    Cao, Xiehong; Tan, Chaoliang; Sindoro, Melinda; Zhang, Hua

    2017-05-22

    Metal-organic frameworks (MOFs), an important class of inorganic-organic hybrid crystals with intrinsic porous structures, can be used as versatile precursors or sacrificial templates for preparation of numerous functional nanomaterials for various applications. Recent developments of MOF-derived hybrid micro-/nano-structures, constructed by more than two components with varied functionalities, have revealed their extensive capabilities to overcome the weaknesses of the individual counterparts and thus give enhanced performance for energy storage and conversion. In this tutorial review, we summarize the recent advances in MOF-derived hybrid micro-/nano-structures. The synthetic strategies for preparing MOF-derived hybrid micro-/nano-structures are first introduced. Focusing on energy storage and conversion, we then discuss their potential applications in lithium-ion batteries, lithium-sulfur batteries, supercapacitors, lithium-oxygen batteries and fuel cells. Finally, we give our personal insights into the challenges and opportunities for the future research of MOF-derived hybrid micro-/nano-structures.

  5. High-throughput automated microfluidic sample preparation for accurate microbial genomics

    Science.gov (United States)

    Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B.; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P.; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C.

    2017-01-01

    Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications. PMID:28128213

  6. Superconductivity in LiTi2O4 Prepared by Hybrid Microwave Method

    Institute of Scientific and Technical Information of China (English)

    YANG Li-Hong; DONG Cheng; SONG Hui-Hua; GUO Juan; FU Guang-Cai

    2005-01-01

    @@ The well-known superconducting oxide LiTi2 O4 has a structural phase transition from spinel to ramsdellite around 900 ℃. We have successfully obtained the superconducting spinel phase and the non-superconducting ramsdellite phase of LiTi2O4 using a hybrid microwave method. The samples are characterized by x-ray powder diffraction, scanning electron microscopy, and measurements of resistivity and magnetic susceptibility. The results show that the low-temperature spinel phase is a superconductor with Tc = 13 K, while the high-temperature ramsdellite phase is a semiconductor. By comparison between the crystal structures of the spinel and the ramsdellite phases, it is suggested that the geometrical frustration plays an important role in the superconductivity of the spinel LiTi2 O4.

  7. A proteomics sample preparation method for mature, recalcitrant leaves of perennial plants.

    Directory of Open Access Journals (Sweden)

    Deng Gang

    Full Text Available Sample preparation is key to the success of proteomics studies. In the present study, two sample preparation methods were tested for their suitability on the mature, recalcitrant leaves of six representative perennial plants (grape, plum, pear, peach, orange, and ramie. An improved sample preparation method was obtained: Tris and Triton X-100 were added together instead of CHAPS to the lysis buffer, and a 20% TCA-water solution and 100% precooled acetone were added after the protein extraction for the further purification of protein. This method effectively eliminates nonprotein impurities and obtains a clear two-dimensional gel electrophoresis array. The method facilitates the separation of high-molecular-weight proteins and increases the resolution of low-abundance proteins. This method provides a widely applicable and economically feasible technology for the proteomic study of the mature, recalcitrant leaves of perennial plants.

  8. LC-MS analysis of the plasma metabolome–a novel sample preparation strategy

    DEFF Research Database (Denmark)

    Skov, Kasper; Hadrup, Niels; Smedsgaard, Jørn

    2015-01-01

    of plasma samples: The first is protein precipitation; the second is protein precipitation followed by solid phase extraction with sub-fractionation into three sub-samples; a phospholipid, a lipid and a polar sub-fraction. Molecular feature extraction of the data files from LC-qTOF analysis of the samples......Blood plasma is a well-known body fluid often analyzed in studies on the effects of toxic compounds as physiological or chemical induced changes in the mammalian body are reflected in the plasma metabolome. Sample preparation prior to LC-MS based analysis of the plasma metabolome is a challenge...... as plasma contains compounds with very different properties. Besides, proteins, which usually are precipitated with organic solvent, phospholipids, are known to cause ion suppression in electrospray mass spectrometry. We have compared two different sample preparation techniques prior to LC-qTOF analysis...

  9. A Hybrid Monte Carlo Sampling Filter for Non-Gaussian Data Assimilation

    Directory of Open Access Journals (Sweden)

    Adrian Sandu

    2015-12-01

    Full Text Available Data assimilation combines information from models, measurements, and priors to obtain improved estimates of the state of a dynamical system such as the atmosphere. Ensemble-based data assimilation approaches such as the Ensemble Kalman filter (EnKF have gained wide popularity due to their simple formulation, ease of implementation, and good practical results. Many of these methods are derived under the assumption that the underlying probability distributions are Gaussian. It is well accepted, however, that the Gaussianity assumption is too restrictive when applied to large nonlinear models, nonlinear observation operators, and large levels of uncertainty. When the Gaussianity assumptions are severely violated, the performance of EnKF variations degrades. This paper proposes a new ensemble-based data assimilation method, named the sampling filter, which obtains the analysis by sampling directly from the posterior distribution. The sampling strategy is based on a Hybrid Monte Carlo (HMC approach that can handle non-Gaussian probability distributions. Numerical experiments are carried out using the Lorenz-96 model and observation operators with different levels of non-linearity and differentiability. The proposed filter is also tested with shallow water model on a sphere with linear observation operator. Numerical results show that the sampling filter performs well even in highly nonlinear situations where the traditional filters diverge.

  10. Automatic coal sample preparation system%煤炭自动制样系统

    Institute of Scientific and Technical Information of China (English)

    王兴无

    2015-01-01

    To solve the problems occurred during manual coal sample preparation,such as low work efficien-cy,high labor intensity,poor working environment,harmful to human beings and poor representativeness of the sample due to large error,the auto coal sample preparation system was designed.Performance tests like residue sample mass,fuel size,residue sample precision and sample preparation bias verified this system has met the requirements of GB/T 1 9494.3-2004 and GB 474-2008 on precision and bias.Its application not only improves the automation degree of sample preparation,but also reduces human disturbance factors in the sample preparation process.%为了解决电厂燃煤人工制样存在的工作效率低,劳动强度大,工作环境差,有害人体健康,误差大影响样品的代表性等问题,设计了煤炭自动制样系统.通过留样质量、出料粒径、留样精密度及制样偏倚等性能试验,证明该系统精密度和偏倚达到了 GB 474—2008和 GB/T 19494.3—2004规定的要求,其应用提高了样品制备的自动化程度,减少了制样过程人为因素的干扰.

  11. Electric transport measurements on bulk, polycrystalline MgB2 samples prepared at various reaction temperatures

    Science.gov (United States)

    Wiederhold, A.; Koblischka, M. R.; Inoue, K.; Muralidhar, M.; Murakami, M.; Hartmann, U.

    2016-03-01

    A series of disk-shaped, bulk MgB2 superconductors (sample diameter up to 4 cm) was prepared in order to improve the performance for superconducting super-magnets. Several samples were fabricated using a solid state reaction in pure Ar atmosphere from 750 to 950oC in order to determine the optimum processing parameters to obtain the highest critical current density as well as large trapped field values. Additional samples were prepared with added silver (up to 10 wt.-%) to the Mg and B powder. Magneto-resistance data and I/V-characteristics were recorded using an Oxford Instruments Teslatron system. From Arrhenius plots, we determine the TAFF pinning potential, U 0. The I/V-characteristics yield detailed information on the current flow through the polycrystalline samples. The current flow is influenced by the presence of pores in the samples. Our analysis of the achieved critical currents together with a thorough microstructure investigation reveals that the samples prepared at temperatures between 775°C and 805°C exhibit the smallest grains and the best connectivity between them, while the samples fabricated at higher reaction temperatures show a reduced connectivity and lower pinning potential. Doping the samples with silver leads to a considerable increase of the pinning potential and hence, the critical current densities.

  12. [Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter].

    Science.gov (United States)

    Hao, Liang; Wu, Dapeng; Guan, Yafeng

    2014-09-01

    The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

  13. Preparation and thermal shock resistance of high emissivity molybdenum disilicide- aluminoborosilicate glass hybrid coating on fiber reinforced aerogel composite

    Science.gov (United States)

    Shao, Gaofeng; Lu, Yucao; Wu, Xiaodong; Wu, Jun; Cui, Sheng; Jiao, Jian; Shen, Xiaodong

    2017-09-01

    To develop a flexible reusable surface insulation for thermal protection system, MoSi2-aluminoborosilicate glass hybrid coatings have been prepared on Al2O3 fiber reinforced Al2O3-SiO2 aerogel composite by slurry dipping and rapid sintering method. The effect of MoSi2 content on radiative property and thermal shock behavior was investigated. The total emissivity values of all the coatings exceeded 0.85 in the wavelength of 0.8-2.5 μm. The M10 and M50 coatings were up to 0.9, which was due to the highest amorphous glass content of the M10 coating and the largest surface roughness of the M50 coating. The M30 coated composite showed the best thermal shock resistance with only 0.023% weight loss after 20 thermal shock cycles between 1473 K and room temperature, which was attributed to the similar thermal expansion coefficients between the coating and the substrate and the appropriate viscosity of aluminoborosilicate glass at 1473 K. The cracks resulted from CTE mismatch stress with different sizes formed and grew on the surface of M10, M40 and M50 coated samples, leading to the failure of the composites.

  14. Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives

    DEFF Research Database (Denmark)

    Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna

    2017-01-01

    Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high...... the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given....

  15. Analysis of aroma compounds of Roselle by Dynamic Headspace Sampling using different preparation methods

    DEFF Research Database (Denmark)

    Juhari, Nurul Hanisah Binti; Varming, Camilla; Petersen, Mikael Agerlin

    2015-01-01

    The influence of different methods of sample preparation on the aroma profiles of dried Roselle (Hibiscus sabdariffa) was studied. Least amounts of aroma compounds were recovered by analysis of whole dry calyxes (WD) followed by ground dry (GD), blended together with water (BTW), and ground...... and then mixed with water (GMW). The highest number of aroma compounds was found in Roselle treated in water bath (2hr/40°C) (GMWKB). GMW was chosen as the preparation method because it was shown to be an efficient extraction method without the possibility of excessive chemical changes of the sample....

  16. A polynomial hybrid reflection model and measurement of its parameters based on images of sample

    Institute of Scientific and Technical Information of China (English)

    Lei Yang; Jiuqiang Han

    2007-01-01

    Reflectance model is a basic concept in computer vision. Some existing models combining the classical diffuse reflectance model and those for surfaces containing specular components can approximately describe real reflectance. But the ratio of diffuse and specular reflection decided manually has no clear meaning.We propose a new polynomial hybrid reflectance model. The reflectance map equation with a known shape (for example cylinder) as a sample is used to estimate parameters of the proposed reflectance model by least square regression algorithm. Then the reflectance parameters for surfaces of the same class of materials can be determined. Experiments are performed for a metal surface. The synthesis images produced by the proposed method and existing ones are compared with the real acquired image, and the results show that the proposed reflectance model is suitable for describing real reflectance.

  17. HPLC analysis of oxindole alkaloids in Uncaria tomentosa: sample preparation and analysis optimisation by factorial design.

    Science.gov (United States)

    Bertol, Gustavo; Franco, Luzia; Oliveira, Brás Heleno de

    2012-01-01

    Uncaria tomentosa ("cat's claw") is widely used for the treatment of some infectious and inflammatory diseases. Oxindole alkaloids are regarded as the most important components responsible for the biological activities attributed to the plant. Their analysis require efficient sample preparation and suitable reference standards but few are commercially available. To develop and validate a HPLC analytical method for oxindole alkaloids in Uncaria tomentosa with emphasis on sample preparation. Factorial experimental designs were used for the optimisation of both sample preparation and chromatographic separation. The optimised sample preparation involved extraction with aqueous ethanol, and the granulometry of the powdered plant material significantly influenced extraction yields. Mitraphylline was used as a calibration reference for the determination of total alkaloids. The method was fully validated and showed good selectivity, linearity (r²  ≥ 0.9996), accuracy (≥ 96%) and precision (RSD < 2.4%). Detection and quantification limits for mitraphylline were 0.8 and 2.4 ppm, respectively. The optimised chromatographic method, using organic buffer in the mobile phase, provided baseline separation of tetracyclic and pentacyclic alkaloids in the samples. Calibration using mitraphylline provided more accurate estimates of total alkaloid content when compared to other available reference alkaloids. Copyright © 2011 John Wiley & Sons, Ltd.

  18. Large 2D-arrays of size-controllable silver nanoparticles prepared by hybrid deposition

    Science.gov (United States)

    Dieu Thuy Ung, Thi; Hoa Nguyen, Thi; Liem Nguyen, Quang

    2016-09-01

    Two main results are presented in this paper. (i) Silver nanoparticles (AgNPs) with uniform size-distribution and controllability in the range of 20-50 nm were synthesized by seeding and growing at ambient conditions. The single-crystal Ag nano-seeds were created by reduction of AgNO3 in presence of citrate surfactant at 70 °C. Then, importantly, the fresh AgCl precursor was used in the presence of polyvinylpyrrolidone to adjust the reaction rate with ascorbic acid to generate Ag for growing on the surface of single-crystal Ag nano-seeds. The AgNPs size could be well-controlled by varying the amount of Ag nano-seeds while keeping the AgCl precursor concentration to be constant. (ii) The large 2D-arrays with homogeneous and dense monolayers of AgNPs were prepared on ITO substrates by hybrid method, in which the key technological point is the surface functionalization of AgNPs using mixed alkanethiols (dodecanethiol:octadecanethiol = 6:1). We have used the fabricated 2D-arrays from the 50 nm AgNPs as a surface enhanced Raman scattering substrate to take the Raman scattering spectra of rhodamine B (RhB), glucose and viral pathogen (H5N1) at very low concentrations of 10-10 M, 10-12 M and 4 ng μl-1, respectively.

  19. Synthesis, characterization, and mercury adsorption properties of hybrid mesoporous aluminosilicate sieve prepared with fly ash.

    Science.gov (United States)

    Liu, Minmin; Hou, Li-An; Xi, Beidou; Zhao, Ying; Xia, Xunfeng

    2013-05-15

    A novel hybrid mesoporous aluminosilicate sieve (HMAS) was prepared with fly ash and impregnated with zeolite A precursors. This improved the mercury adsorption of HMAS compared to original MCM-41. The HMAS was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier transform infrared (FTIR) analysis, transmission electron microscopy (TEM) images and (29)Si and (27)Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectra. These showed that the HMAS structure was still retained after impregnated with zeolite A. But the surface area and pore diameter of HMAS decreased due to pore blockage. Adsorption of mercury from aqueous solution was studied on untreated MCM-41and HMAS. The mercury adsorption rate of HMAS was higher than that of origin MCM-41. The adsorption of mercury was investigated on HMAS regarding the pH of mercury solution, initial mercury concentration, and the reaction temperature. The experimental data fit well to Langmuir and Freundlich isotherm models. The Dublin-Radushkevich isotherm and the characterization show that the mercury adsorption on HMAS involved the ion-exchange mechanisms. In addition, the thermodynamic parameters suggest that the adsorption process was endothermic in nature. The adsorption of mercury on HMAS followed the first order kinetics.

  20. Synthesis, characterization, and mercury adsorption properties of hybrid mesoporous aluminosilicate sieve prepared with fly ash

    Science.gov (United States)

    Liu, Minmin; Hou, Li-an; Xi, Beidou; Zhao, Ying; Xia, Xunfeng

    2013-05-01

    A novel hybrid mesoporous aluminosilicate sieve (HMAS) was prepared with fly ash and impregnated with zeolite A precursors. This improved the mercury adsorption of HMAS compared to original MCM-41. The HMAS was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier transform infrared (FTIR) analysis, transmission electron microscopy (TEM) images and 29Si and 27Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectra. These showed that the HMAS structure was still retained after impregnated with zeolite A. But the surface area and pore diameter of HMAS decreased due to pore blockage. Adsorption of mercury from aqueous solution was studied on untreated MCM-41and HMAS. The mercury adsorption rate of HMAS was higher than that of origin MCM-41. The adsorption of mercury was investigated on HMAS regarding the pH of mercury solution, initial mercury concentration, and the reaction temperature. The experimental data fit well to Langmuir and Freundlich isotherm models. The Dublin-Radushkevich isotherm and the characterization show that the mercury adsorption on HMAS involved the ion-exchange mechanisms. In addition, the thermodynamic parameters suggest that the adsorption process was endothermic in nature. The adsorption of mercury on HMAS followed the first order kinetics.

  1. Synthesis, characterization, and mercury adsorption properties of hybrid mesoporous aluminosilicate sieve prepared with fly ash

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Minmin [School of Environmental Science and Engineering, Tongji University, 1239 Siping Road, Shanghai 200092 (China); Hou, Li-an, E-mail: 11liuminmin@tongji.edu.cn [School of Environmental Science and Engineering, Tongji University, 1239 Siping Road, Shanghai 200092 (China); Xi, Beidou; Zhao, Ying; Xia, Xunfeng [China Research Academy of Environmental Science, Beijing 200012 (China)

    2013-05-15

    A novel hybrid mesoporous aluminosilicate sieve (HMAS) was prepared with fly ash and impregnated with zeolite A precursors. This improved the mercury adsorption of HMAS compared to original MCM-41. The HMAS was characterized by X-ray diffraction (XRD), nitrogen adsorption–desorption, Fourier transform infrared (FTIR) analysis, transmission electron microscopy (TEM) images and {sup 29}Si and {sup 27}Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectra. These showed that the HMAS structure was still retained after impregnated with zeolite A. But the surface area and pore diameter of HMAS decreased due to pore blockage. Adsorption of mercury from aqueous solution was studied on untreated MCM-41and HMAS. The mercury adsorption rate of HMAS was higher than that of origin MCM-41. The adsorption of mercury was investigated on HMAS regarding the pH of mercury solution, initial mercury concentration, and the reaction temperature. The experimental data fit well to Langmuir and Freundlich isotherm models. The Dublin–Radushkevich isotherm and the characterization show that the mercury adsorption on HMAS involved the ion-exchange mechanisms. In addition, the thermodynamic parameters suggest that the adsorption process was endothermic in nature. The adsorption of mercury on HMAS followed the first order kinetics.

  2. Optically active substituted polyacetylene@carbon nanotube hybrids: Preparation, characterization and infrared emissivity property study

    Energy Technology Data Exchange (ETDEWEB)

    Bu, Xiaohai; Zhou, Yuming, E-mail: ymzhou@seu.edu.cn; Zhang, Tao; Wang, Yongjuan; Zhang, Zewu; He, Man

    2014-08-15

    Optically active substituted polyacetylene@multiwalled carbon nanotubes (SPA@MWCNTs) nanohybrids were fabricated by wrapping helical SPA copolymers onto the surface of modified nanotubes through ester bonding linkage. SPA copolymer based on chiral phenylalanine and serine was pre-polymerized by a rhodium zwitterion catalyst in THF, and evidently proved to possess strong optical activity and adopt a predominately one-handed helical conformation. Various characterizations including Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and transmission electron microscopy (TEM) demonstrated that the SPA had been covalently grafted onto the nanotubes without destroying their original graphite structure. The wrapped SPA was found to exhibit an enhancement in thermal stability and still maintained considerable optical activity after grafting. The infrared emissivity property of the nanohybrids at 8–14 μm was investigated in addition. The results indicated that the SPA@MWCNTs hybrid matrix could possess a much lower infrared emissivity value (ε=0.707) than raw MWCNTs, which might be due to synergistic effect of the unique helical conformation of optically active SPA and strengthened interfacial interaction between the organic polymers and inorganic nanoparticles. - Graphical abstract: Optically active SPA@MWCNTs nanohybrids with low infrared emissivity. - Highlights: • Synthesis of optically active SPA copolymer derived from serine and phenylalanine. • Preparation and characterization of optically active SPA@MWCNTs nanohybrids. • Application study of the SPA@MWCNTs nanohybrids (ε=0.707) in lowering the infrared emissivity.

  3. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    Science.gov (United States)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  4. Validation of a fully automated robotic setup for preparation of whole blood samples for LC-MS toxicology analysis

    DEFF Research Database (Denmark)

    Andersen, David Wederkinck; Rasmussen, Brian; Linnet, Kristian

    2012-01-01

    A fully automated setup was developed for preparing whole blood samples using a Tecan Evo workstation. By integrating several add-ons to the robotic platform, the flexible setup was able to prepare samples from sample tubes to a 96-well sample plate ready for injection on liquid chromatography...

  5. Recent advances in sample preparation techniques and methods of sulfonamides detection - A review.

    Science.gov (United States)

    Dmitrienko, Stanislava G; Kochuk, Elena V; Apyari, Vladimir V; Tolmacheva, Veronika V; Zolotov, Yury A

    2014-11-19

    Sulfonamides (SAs) have been the most widely used antimicrobial drugs for more than 70 years, and their residues in foodstuffs and environmental samples pose serious health hazards. For this reason, sensitive and specific methods for the quantification of these compounds in numerous matrices have been developed. This review intends to provide an updated overview of the recent trends over the past five years in sample preparation techniques and methods for detecting SAs. Examples of the sample preparation techniques, including liquid-liquid and solid-phase extraction, dispersive liquid-liquid microextraction and QuEChERS, are given. Different methods of detecting the SAs present in food and feed and in environmental, pharmaceutical and biological samples are discussed.

  6. A Novel Hybrid Ultramicrotomy/FIB-SEM Technique: Preparation of Serial Electron-Transparent Thin Sections of a Hayabusa Grain

    Science.gov (United States)

    Berger, Eve L.; Keller, Lindsay P.

    2014-01-01

    The Japanese space agency's (JAXA) Hayabusa mission returned the first particulate samples (typically SEM). Using a diamond trim knife, the epoxy surrounding the grain is removed on 3 sides (to within a few microns of the grain); the depth of material removed extends well below the bottom of the particle. The sample is attached to an SEM pin mount, the epoxy coated with conductive paint, and the entire assembly coated with approx. 40nm of carbon to eliminate sample charging during FIB work. A protective carbon cap is placed according to the plan for the 15 FIB sections. The central 'spine' of the cap runs perpendicular to the front of the sample, and the 'ribs' protruding from either side run parallel. Each rib indicates the location of a planned FIB section, and the spine contains the final two planned sections. We use a cap with a 4 micron-wide spine and 2micron-wide ribs that have ?3.5 micron of space between them (narrower cuts result in too much re-deposition of material inside the trenches). Using a 30kV, 3nA ion-beam we expose the front surface of the grain and commence milling trenches between sections. Rather than using the typical C-cut to prepare the sample for lift-out, an L-cut is used instead, leaving the sample connected by an interior tab. tab. Sections are lifted out, attached to TEM grids and thinned to electron transparency. TEM analyses show that our hybrid technique preserves both interior and edge features, including surface modifications from exposure to the space environment, such as damaged rims that form in response to solar wind implantation effects and adhering grains. In addition, the FIB sections provide larger areas that are free of fractures and chatter effects in comparison to the microtome thin sections, thus enabling more accurate measurements of solar flare particle track densities that are used to determine the surface exposure age of the particles.

  7. Author Contribution to the Pu Handbook II: Chapter 37 LLNL Integrated Sample Preparation Glovebox (TEM) Section

    Energy Technology Data Exchange (ETDEWEB)

    Wall, Mark A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2016-10-25

    The development of our Integrated Actinide Sample Preparation Laboratory (IASPL) commenced in 1998 driven by the need to perform transmission electron microscopy studies on naturally aged plutonium and it’s alloys looking for the microstructural effects of the radiological decay process (1). Remodeling and construction of a laboratory within the Chemistry and Materials Science Directorate facilities at LLNL was required to turn a standard radiological laboratory into a Radiological Materials Area (RMA) and Radiological Buffer Area (RBA) containing type I, II and III workplaces. Two inert atmosphere dry-train glove boxes with antechambers and entry/exit fumehoods (Figure 1), having a baseline atmosphere of 1 ppm oxygen and 1 ppm water vapor, a utility fumehood and a portable, and a third double-walled enclosure have been installed and commissioned. These capabilities, along with highly trained technical staff, facilitate the safe operation of sample preparation processes and instrumentation, and sample handling while minimizing oxidation or corrosion of the plutonium. In addition, we are currently developing the capability to safely transfer small metallographically prepared samples to a mini-SEM for microstructural imaging and chemical analysis. The gloveboxes continue to be the most crucial element of the laboratory allowing nearly oxide-free sample preparation for a wide variety of LLNL-based characterization experiments, which includes transmission electron microscopy, electron energy loss spectroscopy, optical microscopy, electrical resistivity, ion implantation, X-ray diffraction and absorption, magnetometry, metrological surface measurements, highpressure diamond anvil cell equation-of-state, phonon dispersion measurements, X-ray absorption and emission spectroscopy, and differential scanning calorimetry. The sample preparation and materials processing capabilities in the IASPL have also facilitated experimentation at world-class facilities such as the

  8. Preparing to Receive and Handle Martian Samples When They Arrive on Earth

    Science.gov (United States)

    McCubbin, Francis M.

    2017-01-01

    The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F+ derivative NPR 'Curation of Extraterrestrial Materials', JSC is charged with 'The curation of all extraterrestrial material under NASA control, including future NASA missions. 'The Directive goes on to define Curation as including'...documentation, preservation, preparation, and distribution of samples for research, education, and public outreach."

  9. High Refractive Organic–Inorganic Hybrid Films Prepared by Low Water Sol-Gel and UV-Irradiation Processes

    Directory of Open Access Journals (Sweden)

    Hsiao-Yuan Ma

    2016-03-01

    Full Text Available Organic-inorganic hybrid sols (Ti–O–Si precursor were first synthesized by the sol-gel method at low addition of water, and were then employed to prepare a highly refractive hybrid optical film. This film was obtained by blending the Ti–O–Si precursor with 2-phenylphenoxyethyl acrylate (OPPEA to perform photo-polymerization by ultraviolet (UV irradiation. Results show that the film transparency of poly(Ti–O–Si precursor-co-OPPEA film is higher than that of a pure poly(Ti–O–Si precursor film, and that this poly(Ti–O–Si precursor-co-OPPEA hybrid film exhibits a high transparency of ~93.7% coupled with a high refractive index (n of 1.83 corresponding to a thickness of 2.59 μm.

  10. Field Emission Properties of the Graphene Double-Walled Carbon Nanotube Hybrid Films Prepared by Vacuum Filtration and Screen Printing

    Directory of Open Access Journals (Sweden)

    Jinzhuo Xu

    2013-01-01

    Full Text Available The graphene double-walled carbon nanotube (DWCNT hybrid films were prepared by vacuum filtration and screen printing. Their electron field emission properties have been studied systematically. The electron emission properties of the hybrid films are much better than those of pure DWCNT films and pure graphene films. Comparing with the screen printed films, the vacuum filtered films have many advantages, such as lower turn-on field, higher emission current density, better uniformity, better long-term stability, and stronger adhesive strength with conductive substrates. The optimized hybrid films with 20% weight ratio of graphene, which were fabricated by vacuum filtration, show the best electron emission performances with a low turn-on field of 0.50 Vμm−1 (at 1 μAcm−2 and a high field enhancement factor β of 27000.

  11. PREPARATION OF POLYIMIDE-BaTiO3 HYBRID FILMS BY A DISPERSION PROCESS AND THEIR MICROSTRUCTURE

    Institute of Scientific and Technical Information of China (English)

    Yue-sheng Li; Yue-jin Tong; Kai Jing; Meng-xian Ding

    2001-01-01

    Barium titanate (BaTiO3) powders with particle sizes of 30~50 nm were prepared from barium stearate, titanium alkoxides and stearic acid by stearic acid-gel method. Dispersing the agglomerate of BaTiO3 nanoparticles into poly(amic acid) solution followed by curing led to the formation of polyimide hybrid films. The hybrid films were transparent and well distributed with BaTiO3 nanoparticles when the BaTiO3 content was less than 1 wt%. Highly loaded hybrid film containing 30 wt % BaTiO3 was tough, had a smooth surface and possessed much higher dielectric and piezoelectric constants than the parent polyimide.

  12. Optimization of sample preparation for accurate results in quantitative NMR spectroscopy

    Science.gov (United States)

    Yamazaki, Taichi; Nakamura, Satoe; Saito, Takeshi

    2017-04-01

    Quantitative nuclear magnetic resonance (qNMR) spectroscopy has received high marks as an excellent measurement tool that does not require the same reference standard as the analyte. Measurement parameters have been discussed in detail and high-resolution balances have been used for sample preparation. However, the high-resolution balances, such as an ultra-microbalance, are not general-purpose analytical tools and many analysts may find those balances difficult to use, thereby hindering accurate sample preparation for qNMR measurement. In this study, we examined the relationship between the resolution of the balance and the amount of sample weighed during sample preparation. We were able to confirm the accuracy of the assay results for samples weighed on a high-resolution balance, such as the ultra-microbalance. Furthermore, when an appropriate tare and amount of sample was weighed on a given balance, accurate assay results were obtained with another high-resolution balance. Although this is a fundamental result, it offers important evidence that would enhance the versatility of the qNMR method.

  13. Soil and Water – What is Detectable through Microbiological Sample Preparation Techniques

    Science.gov (United States)

    The concerns of a potential terrorist’s use of biological agents in soil and ground water are articulated by comparisons to major illnesses in this Country involving contaminated drinking water sources. Objectives are focused on the importance of sample preparation in the rapid, ...

  14. Analysis of biopharmaceutical proteins in biological matrices by LC-MS/MS I. Sample preparation

    NARCIS (Netherlands)

    Bischoff, Rainer; Bronsema, Kees J.; van de Merbel, Nico C.

    2013-01-01

    Part I of this review discusses sample-preparation aspects of quantifying biopharmaceutical proteins in complex biological matrices by LC-MS/MS with a focus on blood-derived body fluids. We conclude Part I with a short overview over options for automating the entire analytical procedure, which is

  15. Analysis of biopharmaceutical proteins in biological matrices by LC-MS/MS I. Sample preparation

    NARCIS (Netherlands)

    Bischoff, Rainer; Bronsema, Kees J.; van de Merbel, Nico C.

    2013-01-01

    Part I of this review discusses sample-preparation aspects of quantifying biopharmaceutical proteins in complex biological matrices by LC-MS/MS with a focus on blood-derived body fluids. We conclude Part I with a short overview over options for automating the entire analytical procedure, which is in

  16. Challenges of sample preparation for cross sectional EBSD analysis of electrodeposited nickel films

    DEFF Research Database (Denmark)

    Alimadadi, Hossein; Pantleon, Karen

    2009-01-01

    . Different procedures for sample preparation including mechanical grinding and polishing, electropolishing and focused ion beam milling have been applied to a nickel film electrodeposited on top of an amorphous Ni-P layer on a Cu-substrate. Reliable EBSD analysis of the whole cross section can be obtained...

  17. Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

    Directory of Open Access Journals (Sweden)

    Paul M. Pellegrino

    2013-05-01

    Full Text Available Hazard detection systems must be evaluated with appropriate test material concentrations under controlled conditions in order to accurately identify and quantify unknown residues commonly utilized in theater. The existing assortment of hazard reference sample preparation methods/techniques presents a range of variability and reproducibility concerns, making it increasingly difficult to accurately assess optically- based detection technologies. To overcome these challenges, we examined the optimization, characterization, and calibration of microdroplets from a drop-on-demand microdispenser that has a proven capability for the preparation of energetic reference materials. Research presented herein focuses on the development of a simplistic instrument calibration technique and sample preparation protocol for explosive materials testing based on drop-on-demand technology. Droplet mass and reproducibility were measured using ultraviolet-visible (UV-Vis absorption spectroscopy. The results presented here demonstrate the operational factors that influence droplet dispensing for specific materials (e.g., energetic and interferents. Understanding these parameters permits the determination of droplet and sample uniformity and reproducibility (typical R2 values of 0.991, relative standard deviation or RSD ≤ 5%, and thus the demonstrated maturation of a successful and robust methodology for energetic sample preparation.

  18. Sample preparation composite and replicate strategy case studies for assay of solid oral drug products.

    Science.gov (United States)

    Nickerson, Beverly; Harrington, Brent; Li, Fasheng; Guo, Michele Xuemei

    2017-08-16

    Drug product assay is one of several tests required for new drug products to ensure the quality of the product at release and throughout the life cycle of the product. Drug product assay testing is typically performed by preparing a composite sample of multiple dosage units to obtain an assay value representative of the batch. In some cases replicate composite samples may be prepared and the reportable assay value is the average value of all the replicates. In previously published work by Harrington et al. (2014) [5], a sample preparation composite and replicate strategy for assay was developed to provide a systematic approach which accounts for variability due to the analytical method and dosage form with a standard error of the potency assay criteria based on compendia and regulatory requirements. In this work, this sample preparation composite and replicate strategy for assay is applied to several case studies to demonstrate the utility of this approach and its application at various stages of pharmaceutical drug product development. Copyright © 2017. Published by Elsevier B.V.

  19. A novel sample preparation method to avoid influence of embedding medium during nano-indentation

    Science.gov (United States)

    Yujie Meng; Siqun Wang; Zhiyong Cai; Timothy M. Young; Guanben Du; Yanjun Li

    2012-01-01

    The effect of the embedding medium on the nano-indentation measurements of lignocellulosic materials was investigated experimentally using nano-indentation. Both the reduced elastic modulus and the hardness of nonembedded cell walls were found to be lower than those of the embedded samples, proving that the embedding medium used for specimen preparation on cellulosic...

  20. Sample preparation for combined chemical analysis and bioassay application in water quality assessment

    NARCIS (Netherlands)

    Kolkman, A.; Schriks, M.; Brand, W; Bäuerlein, P.S.; van der Kooi, M.M.E.; van Doorn, R.H.; Emke, E.; Reus, A.; van der Linden, S.; de Voogt, P.; Heringa, M.B.

    2013-01-01

    The combination of in vitro bioassays and chemical screening can provide a powerful toolbox to determine biologically relevant compounds in water extracts. In this study, a sample preparation method is evaluated for the suitability for both chemical analysis and in vitro bioassays. A set of 39 chemi

  1. A novel IgY-Aptamer hybrid system for cost-effective detection of SEB and its evaluation on food and clinical samples.

    Science.gov (United States)

    Mudili, Venkataramana; Makam, Shivakiran S; Sundararaj, Naveen; Siddaiah, Chandranayaka; Gupta, Vijai Kumar; Rao, Putcha V Lakshmana

    2015-10-19

    In the present study, we introduce a novel hybrid sandwich-ALISA employing chicken IgY and ssDNA aptamers for the detection of staphylococcal enterotoxin B (SEB). Cloning, expression and purification of the full length recombinant SEB was carried out. Anti-SEB IgY antibodies generated by immunizing white leg-horn chickens with purified recombinant SEB protein and were purified from the immunized egg yolk. Simultaneously, ssDNA aptamers specific to the toxin were prepared by SELEX method on microtiter well plates. The sensitivity levels of both probe molecules i.e., IgY and ssDNA aptamers were evaluated. We observed that the aptamer at 250 ngmL(-1) concentration could detect the target antigen at 50 ngmL(-1) and the IgY antibodies at 250 ngmL(-1), could able to detect 100 ngmL(-1) antigen. We further combined both the probes to prepare a hybrid sandwich aptamer linked immune sorbent assay (ALISA) wherein the IgY as capturing molecule and biotinylated aptamer as revealing probe. Limit of detection (LOD) for the developed method was determined as 50 ngmL(-1). Further, developed method was evaluated with artificially SEB spiked milk and natural samples and obtained results were validated with PCR. In conclusion, developed ALISA method may provide cost-effective and robust detection of SEB from food and environmental samples.

  2. Preparation of poly(ethylene glycol/polylactide hybrid fibrous scaffolds for bone tissue engineering

    Directory of Open Access Journals (Sweden)

    Ni P

    2011-11-01

    Full Text Available PeiYan Ni, ShaoZhi Fu, Min Fan, Gang Guo, Shuai Shi, JinRong Peng, Feng Luo, ZhiYong QianState Key Laboratory of Biotherapy and Cancer Center, West China Hospital, West China Medical School, Sichuan University, Chengdu, Sichuan, People's Republic of ChinaAbstract: Polylactide (PLA electrospun fibers have been reported as a scaffold for bone tissue engineering application, however, the great hydrophobicity limits its broad application. In this study, the hybrid amphiphilic poly(ethylene glycol (PEG/hydrophobic PLA fibrous scaffolds exhibited improved morphology with regular and continuous fibers compared to corresponding blank PLA fiber mats. The prepared PEG/PLA fibrous scaffolds favored mesenchymal stem cell (MSC attachment and proliferation by providing an interconnected porous extracellular environment. Meanwhile, MSCs can penetrate into the fibrous scaffold through the interstitial pores and integrate well with the surrounding fibers, which is very important for favorable application in tissue engineering. More importantly, the electrospun hybrid PEG/PLA fibrous scaffolds can enhance MSCs to differentiate into bone-associated cells by comprehensively evaluating the representative markers of the osteogenic procedure with messenger ribonucleic acid quantitation and protein analysis. MSCs on the PEG/PLA fibrous scaffolds presented better differentiation potential with higher messenger ribonucleic acid expression of the earliest osteogenic marker Cbfa-1 and mid-stage osteogenic marker Col I. The significantly higher alkaline phosphatase activity of the PEG/PLA fibrous scaffolds indicated that these can enhance the differentiation of MSCs into osteoblast-like cells. Furthermore, the higher messenger ribonucleic acid level of the late osteogenic differentiation markers OCN (osteocalcin and OPN (osteopontin, accompanied by the positive Alizarin red S staining, showed better maturation of osteogenic induction on the PEG/PLA fibrous scaffolds at the

  3. The role of sample preparation in interpretation of trace element concentration variability in moss bioindication studies

    Science.gov (United States)

    Migaszewski, Z.M.; Lamothe, P.J.; Crock, J.G.; Galuszka, A.; Dolegowska, S.

    2011-01-01

    Trace element concentrations in plant bioindicators are often determined to assess the quality of the environment. Instrumental methods used for trace element determination require digestion of samples. There are different methods of sample preparation for trace element analysis, and the selection of the best method should be fitted for the purpose of a study. Our hypothesis is that the method of sample preparation is important for interpretation of the results. Here we compare the results of 36 element determinations performed by ICP-MS on ashed and on acid-digested (HNO3, H2O2) samples of two moss species (Hylocomium splendens and Pleurozium schreberi) collected in Alaska and in south-central Poland. We found that dry ashing of the moss samples prior to analysis resulted in considerably lower detection limits of all the elements examined. We also show that this sample preparation technique facilitated the determination of interregional and interspecies differences in the chemistry of trace elements. Compared to the Polish mosses, the Alaskan mosses displayed more positive correlations of the major rock-forming elements with ash content, reflecting those elements' geogenic origin. Of the two moss species, P. schreberi from both Alaska and Poland was also highlighted by a larger number of positive element pair correlations. The cluster analysis suggests that the more uniform element distribution pattern of the Polish mosses primarily reflects regional air pollution sources. Our study has shown that the method of sample preparation is an important factor in statistical interpretation of the results of trace element determinations. ?? 2010 Springer-Verlag.

  4. Preparation and characterisation of magnetic nanostructured samples for inelastic neutron scattering experiments

    Energy Technology Data Exchange (ETDEWEB)

    Kreuzpaintner, Wolfgang

    2010-06-22

    Recent advances in thin-film structuring techniques have generated significant interest in the dynamics of spin waves in magnetic nanostructures and the possible use of inelastic neutron scattering (INS) for their investigation. This thesis describes the design and implementation, at GKSS Research Centre, of equipment for preparation of large and laterally submicron and nanometre structured magnetic samples for such future INS experiments. After a brief resume on spin waves in nanostructures, the development work on new purpose-designed equipment, including high vacuum (HV) argon ion beam milling and ultra high vacuum (UHV) e-beam evaporation setups, is described. Ni nanodot as well as Ni and novel Gd nanowire samples were prepared using combinations of sputter deposition, laser interference lithography, argon ion beam milling, e-beam evaporation and self organisation techniques. With reference to sample preparation, epitaxial growth studies for Ni on Si(100) substrate were performed, resulting in the development of a new deposition process, which by thermal tuning allows for the direct epitaxial growth of Ni on Si with unprecedented crystalline quality. The results of various characterisation experiments on the prepared nanostructured samples, including Scanning Electron Microscopy (SEM), microprobe analysis, Atomic and Magnetic Force Microscopy (AFM/MFM), Vibrating Sample Magnetometry (VSM), X-ray Diffraction (XRD) and Reflectivity (XRR), unpolarised and Polarised Neutron Scattering (PNR) and off-specular scattering by X-rays and neutrons using rocking scans and Time-Of-Flight Grazing Incidence Small Angle Neutron Scattering (TOF-GISANS), together with various analysis procedures such as Distorted-Wave Born Approximation (DWBA), are reported. The analysis of a Gd nanowire sample by TOF-GISANS led to a novel evaluation technique which in comparison with single wavelength methods allows portions of reciprocal space to be scanned without changing the angle of

  5. Aptamer-based organic-silica hybrid affinity monolith prepared via "thiol-ene" click reaction for extraction of thrombin.

    Science.gov (United States)

    Wang, Zheng; Zhao, Jin-cheng; Lian, Hong-zhen; Chen, Hong-yuan

    2015-06-01

    A novel strategy for preparing aptamer-based organic-silica hybrid monolithic column was developed via "thiol-ene" click chemistry. Due to the large specific surface area of the hybrid matrix and the simplicity, rapidness and high efficiency of "thiol-ene" click reaction, the average coverage density of aptamer on the organic-silica hybrid monolith reached 420 pmol μL(-1). Human α-thrombin can be captured on the prepared affinity monolithic column with high specificity and eluted by NaClO4 solution. N-p-tosyl-Gly-Pro-Arg p-nitroanilide acetate was used as the sensitive chromogenic substrate of thrombin. The thrombin enriched by this affinity column was detected with a detection of limit of 0.01 μM by spectrophotometry. Furthermore, the extraction recovery of thrombin at 0.15 μM in human serum was 91.8% with a relative standard deviation of 4.0%. These results indicated that "thiol-ene" click chemistry provided a promising technique to immobilize aptamer on organic-inorganic hybrid monolith and the easily-assembled affinity monolithic material could be used to realize highly selective recognition of trace proteins.

  6. Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

    Energy Technology Data Exchange (ETDEWEB)

    Chandra, Subhash [Cornell SIMS Laboratory, Department of Earth and Atmospheric Sciences, Snee Hall, Cornell University, Ithaca, NY 14853 (United States)], E-mail: sc40@cornell.edu

    2008-12-15

    Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O{sub 2}{sup +}) revealed local secondary ion signal enhancements correlated with the water image signals of {sup 19}(H{sub 3}O){sup +}. A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K{sup +} and Na{sup +} in physiologically relevant concentrations. The high K

  7. A simple and rapid method for the preparation of homologous DNA oligonucleotide hybridization probes from heterologous gene sequences and probes.

    Science.gov (United States)

    Maxwell, E S; Sarge, K D

    1988-11-30

    We describe a simple and rapid method for the preparation of homologous DNA oligonucleotide probes for hybridization analysis and/or cDNA/genomic library screening. With this method, a synthetic DNA oligonucleotide derived from a known heterologous DNA/RNA/protein sequence is annealed to an RNA preparation containing the gene transcript of interest. Any unpaired 3'-terminal oligonucleotides of the heterologous DNA primer are then removed using the 3' exonuclease activity of the DNA Polymerase I Klenow fragment before primer extension/dideoxynucleotide sequencing of the annealed RNA species with AMV reverse transcriptase. From the determined RNA sequence, a completely homologous DNA oligonucleotide probe is then prepared. This approach has been used to prepare a homologous DNA oligonucleotide probe for the successful library screening of the yeast hybRNA gene starting with a heterologous mouse hybRNA DNA oligonucleotide probe.

  8. A simple sample preparation method for measuring amoxicillin in human plasma by hollow fiber centrifugal ultrafiltration.

    Science.gov (United States)

    Dong, Wei-Chong; Hou, Zi-Li; Jiang, Xin-Hui; Jiang, Ye

    2013-02-01

    A simple sample preparation method has been developed for the determination of amoxicillin in human plasma by hollow fiber centrifugal ultrafiltration (HF-CF-UF). A 400-μL plasma sample was placed directly into the HF-CF-UF device, which consisited of a slim glass tube and a U-shaped hollow fiber. After centrifugation at 1.25 × 10(3) g for 10 min, the filtrate was withdrawn from the hollow fiber and 20 µL was directly injected into the high-performance liquid chromatography (HPLC) for analysis. The calibration curve was linear over the range of 0.1-20 µg/mL (r = 0.9996) and the limit of detection was as low as 0.025 µg/mL. The average recovery and absolute recovery were 99.9% and 84.5%, respectively. Both the intra-day and inter-day precisions (relative standard deviation) were less than 3.1% for three concentrations (0.25, 2.5 and 10 µg/mL). The sample preparation process was simplified. Only after a single centrifugal ultrafiltration can the filtrate be injected directly into HPLC. The present method is simple, sensitive and accurate. It could be effective for the analysis of biological samples with high protein contents, especially for the biopharmaceutical analysis of drugs that use traditional isolation techniques for sample preparation such as the protein precipitation method.

  9. Community-Level Physiological Profiling of Microbial Communities in Constructed Wetlands: Effects of Sample Preparation.

    Science.gov (United States)

    Button, Mark; Weber, Kela; Nivala, Jaime; Aubron, Thomas; Müller, Roland Arno

    2016-03-01

    Community-level physiological profiling (CLPP) using BIOLOG® EcoPlates™ has become a popular method for characterizing and comparing the functional diversity, functional potential, and metabolic activity of heterotrophic microbial communities. The method was originally developed for profiling soil communities; however, its usage has expanded into the fields of ecotoxicology, agronomy, and the monitoring and profiling of microbial communities in various wastewater treatment systems, including constructed wetlands for water pollution control. When performing CLPP on aqueous samples from constructed wetlands, a wide variety of sample characteristics can be encountered and challenges may arise due to excessive solids, color, or turbidity. The aim of this study was to investigate the impacts of different sample preparation methods on CLPP performed on a variety of aqueous samples covering a broad range of physical and chemical characteristics. The results show that using filter paper, centrifugation, or settling helped clarify samples for subsequent CLPP analysis, however did not do so as effectively as dilution for the darkest samples. Dilution was able to provide suitable clarity for the darkest samples; however, 100-fold dilution significantly affected the carbon source utilization patterns (CSUPs), particularly with samples that were already partially or fully clear. Ten-fold dilution also had some effect on the CSUPs of samples which were originally clear; however, the effect was minimal. Based on these findings, for this specific set of samples, a 10-fold dilution provided a good balance between ease of use, sufficient clarity (for dark samples), and limited effect on CSUPs. The process and findings outlined here can hopefully serve future studies looking to utilize CLPP for functional analysis of microbial communities and also assist in comparing data from studies where different sample preparation methods were utilized.

  10. Isolation and purification of heroin from heroin street samples by preparative high performance liquid chromatography.

    Science.gov (United States)

    Guo, Zhen; Zheng, Hui; Lu, Yanzhen; Wei, Yun

    2012-09-10

    The present study established a novel method using preparative high performance liquid chromatography to isolate and purify heroin·HCl from heroin street samples to be used as a reference standard. Different kinds of mobile phases and columns were used, ultimately the mobile phase consisting of hexane-isopropanol-methanol (65:28:7, v/v) and the SIL preparative column prepared in laboratory were selected as the final condition. Heroin was further purified by the drowning-out crystallization method using isopropanol-methanol (50:1, v/v) and hexane as drowning-out anti-solvents and salting-out agents, respectively. The purity was assessed by analytical high performance liquid chromatography and the confirmation of the chemical structure was performed by IR and NMR. About 110.7mg of heroin·HCl at a purity of over 99.52% was obtained from 180mg of heroin street samples which contained 156.15mg of heroin·HCl component by preparative high performance liquid chromatography. This method is suitable for preparing heroin standards in forensic science area.

  11. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community

    KAUST Repository

    Xue, Zheng

    2014-07-15

    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community. © 2014 © 2014 Taylor & Francis.

  12. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community.

    Science.gov (United States)

    Xue, Zheng; Lu, Huijie; Liu, Wen-Tso

    2014-01-01

    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community.

  13. An enzyme-based DNA preparation method for application to forensic biological samples and degraded stains.

    Science.gov (United States)

    Lounsbury, Jenny A; Coult, Natalie; Miranian, Daniel C; Cronk, Stephen M; Haverstick, Doris M; Kinnon, Paul; Saul, David J; Landers, James P

    2012-09-01

    Extraction of DNA from forensic samples typically uses either an organic extraction protocol or solid phase extraction (SPE) and these methods generally involve numerous sample transfer, wash and centrifugation steps. Although SPE has been successfully adapted to the microdevice, it can be problematic because of lengthy load times and uneven packing of the solid phase. A closed-tube enzyme-based DNA preparation method has recently been developed which uses a neutral proteinase to lyse cells and degrade proteins and nucleases [14]. Following a 20 min incubation of the buccal or whole blood sample with this proteinase, DNA is polymerase chain reaction (PCR)-ready. This paper describes the optimization and quantitation of DNA yield using this method, and application to forensic biological samples, including UV- and heat-degraded whole blood samples on cotton or blue denim substrates. Results demonstrate that DNA yield can be increased from 1.42 (±0.21)ng/μL to 7.78 (±1.40)ng/μL by increasing the quantity of enzyme per reaction by 3-fold. Additionally, there is a linear relationship between the amount of starting cellular material added and the concentration of DNA in the solution, thereby allowing DNA yield estimations to be made. In addition, short tandem repeat (STR) profile results obtained using DNA prepared with the enzyme method were comparable to those obtained with a conventional SPE method, resulting in full STR profiles (16 of 16 loci) from liquid samples (buccal swab eluate and whole blood), dried buccal swabs and bloodstains and partial profiles from UV or heat-degraded bloodstains on cotton or blue denim substrates. Finally, the DNA preparation method is shown to be adaptable to glass or poly(methyl methacrylate) (PMMA) microdevices with little impact on STR peak height but providing a 20-fold reduction in incubation time (as little as 60 s), leading to a ≥1 h reduction in DNA preparation time.

  14. MALDI MS sample preparation by using paraffin wax film: systematic study and application for peptide analysis.

    Science.gov (United States)

    Wang, Junhua; Chen, Ruibing; Ma, Mingming; Li, Lingjun

    2008-01-15

    Recently developed sample preparation techniques employing hydrophobic sample support have improved the detection sensitivity and mass spectral quality of matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). These methods concentrate the samples on target by minimizing the sample area via the solvent repellent effect of the target surface. In the current study, we employed the use of paraffin wax film (Parafilm M) for improved MALDI MS analysis of low-abundance peptide mixtures, including neuronal tissue releasate and protein tryptic digests. This thin film was found to strongly repel polar solvents including water, methanol, and acetonitrile, which enabled the application of a wide range of sample preparation protocols that involved the use of various organic solvents. A "nanoliter-volume deposition" technique employing a capillary column has been used to produce tiny ( approximately 400 microm) matrix spots of 2,5-dihydroxybenzoic acid on the film. By systematically optimizing the sample volume, solvent composition, and film treatment, the Parafilm M substrate in combination with the nanoliter-volume matrix deposition method allowed dilute sample to be concentrated on the film for MALDI MS analysis. Peptide mixtures with nanomolar concentrations have been detected by MALDI time-of-flight and MALDI Fourier transform ion cyclotron resonance mass spectrometers. Overall, the use of Parafilm M enabled improved sensitivity and spectral quality for the analysis of complex peptide mixtures.

  15. Preparation and Conducting Behavior of Amphibious Organic/Inorganic Hybrid Proton Exchange Membranes Based on Benzyltetrazole

    Institute of Scientific and Technical Information of China (English)

    QIAO Li-gen; SHI Wen-fang

    2012-01-01

    A series of novel amphibious organic/inorganic hybrid proton exchange membranes with H3PO4 doped which could be used under both wet and dry conditions was prepared through a sol-gel process based on acrylated triethoxysilane(A-TES)and benzyltetrazole-modified triethoxysilane(BT-TES).The dual-curing approach including UV-curing and thermal curing was used to obtain the crosslinked membranes.Polyethylene glycol(400)diacrylate(PEGDA)was used as an oligomer to form the polymeric matrix.The molecular structures of precursors were characterized by 1H,13C and 29Si NMR spectra.The thermogravimetric analysis(TGA)results show that the membranes exhibit acceptable thermal stability for their application at above 200 ℃.The differential scanning calorimeter(DSC)determination indicates that the crosslinked membranes with the mass ratios of below 1.6 of BT-TES to A-TES and the same mass of H3PO4 doped as that of A-TES possess the-Tgs,and the lowest Tg(-28.9 ℃)exists for the membrane with double mass of H3PO4 doped as well.The high proton conductivity in a range of 9.4-17.3 mS/cm with the corresponding water uptake of 19.1%-32.8% of the membranes was detected at 90 ℃ under wet conditions.Meanwhile,the proton conductivity in a dry environment for the membrane with a mass ratio of 2.4 of BT-TES to A-TES and double H3PO4 loading increases from 4.89× 10-2 mS/cm at 30 ℃ to 25.7 mS/cm at 140 ℃.The excellent proton transport ability under both hydrous and anhydrous conditions demonstrates a potential application in the polymer electrolyte membrane fuel cells.

  16. Charge Density Wave and Crystal Structure of KxWO3 (x=0.20 and 0.22) Prepared by Hybrid Microwave Method

    Science.gov (United States)

    Chen, Runze; Gao, Chaojun; Bu, Kun; Hao, Xiaoyu; Wang, Zichen; Wen, Lianjun; Guo, Juan; Chao, Mingju; Liang, Erjun; Yang, Lihong; Dong, Cheng

    2017-02-01

    Potassium tungsten bronzes KxWO3 (x=0.20 and 0.22) with the coexistence of charge density wave (CDW) and superconductivity (SC) were prepared from K2WO4, WO3 and W powders using a hybrid microwave method. The structure refinement confirmed that all samples had a pure hexagonal phase with the space group of P63 /mcm. The distortion degree of W-O octahedron declines with x and is independent of synthesis condition for the same x (=0.20). The CDW transition is studied as a function of residual resistivity ratio. By increasing the crystallinity of sample, this transition can be suppressed, which is probably attributed to the interaction between CDW and defects in crystallites. The CDW transition temperature increases with x, which may be related to the decline of the distortion degree of W-O octahedron. The competition between CDW and SC is observed according to the resistivity and magnetization measurements.

  17. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability

    Science.gov (United States)

    Kim, Jungdae; Nam, Hyoungdo; Qin, Shengyong; Kim, Sang-ui; Schroeder, Allan; Eom, Daejin; Shih, Chih-Kang

    2015-09-01

    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  18. Experimental improvements in sample preparation for the track registration technique from dry and solution media

    Energy Technology Data Exchange (ETDEWEB)

    Suarez-Navarro, M.J. [Universidad Politecnica de Madrid (UPM), E.T.S.I de Caminos, Canales y Puertos, Profesor Aranguren s/n, 28040 Madrid (Spain)]. E-mail: he04@caminos.upm.es; Pujol, Ll. [Centro de Estudios y Experimentacion de Obras Publicas (CEDEX), Alfonso XII, 3, 28014 Madrid (Spain); Gonzalez-Gonzalez, J.A. [Universidad Politecnica de Madrid (UPM), E.T.S.I de Caminos, Canales y Puertos, Profesor Aranguren s/n, 28040 Madrid (Spain)

    2006-04-15

    This paper describes the sample preparation studies carried out to determine gross alpha activities in waste materials by means of alpha-particle track counting using CR-39 detector. Sample preparation for the track registration technique using evaporation or electroplating methods (also known as conventional 'dry methods') has a number of drawbacks. The distribution of tracks in different areas of the detector surface is non-uniform, so accurate quantitative determinations depend on tedious and time-consuming counting of tracks under an optical microscope. In this paper, we propose the use of tensioactives in sample preparation to achieve uniform track distribution over the entire detector surface, which enables track density to be evaluated by scanning a small representative area. Under our counting conditions, uniform distribution was achieved with 0.2 ml of Teg from a planchetted source. Furthermore, track registration techniques using solution media (also known as the 'wet methods') and conventional 'dry methods' were analysed and compared with the proposed method. The reproducibility of the procedure described in the study was tested by analysing gross alpha activity in two low-level nuclear waste samples at two different laboratories.

  19. Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives.

    Science.gov (United States)

    Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna; Chidambara, Vinayaka Aaydha; Wolff, Anders; Bang, Dang Duong; Sun, Yi

    2017-05-15

    Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high loading capacity. MIPs have been intensively employed in classical solid-phase extraction and solid-phase microextraction. More recently, MIPs have been combined with magnetic bead extraction, which greatly simplifies sample handling procedures. Studies have consistently shown that MIPs can effectively minimize complex food matrix effects, and improve recoveries and detection limits. In addition to sample preparation, MIPs have also been viewed as promising alternatives to bio-receptors due to the inherent molecular recognition abilities and the high stability in harsh chemical and physical conditions. MIPs have been utilized as receptors in biosensing platforms such as electrochemical, optical and mass biosensors to detect various analytes in food. In this review, we will discuss the current state-of-the-art of MIP synthesis and applications in the context of food analysis. We will highlight the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given.

  20. Comparison of sample preparation methods for the recovery of foodborne pathogens from fresh produce.

    Science.gov (United States)

    Kim, Se-Ri; Yoon, Yohan; Kim, Won-Il; Park, Kyeong-Hun; Yun, Hye-Jeong; Chung, Duck Hwa; Yun, Jong Chul; Ryu, Kyoung Yul

    2012-07-01

    Sample preparation methods (pummeling, pulsifying, sonication, and shaking by hand) were compared for achieving maximum recovery of foodborne pathogens from iceberg lettuce, perilla leaves, cucumber, green pepper, and cherry tomato. Antimicrobial and dehydration effects also were examined to investigate causes of poor recovery of pathogens. Each produce type was inoculated with Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, Staphylococcus aureus, and Bacillus cereus at 6.0 log CFU/cm(2), and samples were prepared using the four methods. Bacterial populations recovered from the five types of produce were significantly different (P cucumber, and green pepper had no antimicrobial activity, the populations of E. coli O157:H7, Salmonella Typhimurium, B. cereus, and L. monocytogenes in cherry tomato extract were slightly reduced after these treatments (P 2 log CFU/cm(2) after exposure to 40% relative humidity for 1 h. No reduction was observed when the five pathogens were exposed to 90% relative humidity. These data suggest that pummeling and pulsifying are optimal sample preparation methods for detection of microorganisms. Acidic produce such as cherry tomato should be treated with a method that does not cause sample breakdown so that acid stress on the bacteria can be minimized. Dehydration stress also affects recovery of pathogens from produce.

  1. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    Energy Technology Data Exchange (ETDEWEB)

    Hou Aiqin, E-mail: aiqinhou@dhu.edu.c [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China); Chen Huawei [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China)

    2010-03-15

    The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

  2. Should the mass of a nanoferrite sample prepared by autocombustion method be considered as a realistic preparation parameter?

    Science.gov (United States)

    Wahba, Adel Maher; Mohamed, Mohamed Bakr

    2017-02-01

    Detectable variations in structural, elastic and magnetic properties have been reported depending on the mass of the cobalt nanoferrite sample prepared by citrate autocombustion method. Heat released during the autocombustion process and its duration are directly proportional to the mass to be prepared, and is thus expected to affect both the crystallite size and the cation distribution giving rise to the reported variations in microstrain, magnetization, and coercivity. Formation of a pure spinel phase has been validated using X-ray diffraction patterns (XRD) and Fourier-transform infrared (FTIR) spectra. Crystallite sizes obtained from Williamson-Hall (W-H) method range from 28-87 nm, being further supported by images of high-resolution transmission electron microscope (HRTEM). Saturation magnetization and coercivity deduced from M-H hysteresis loops show a clear correlation with the cation distribution, which was proposed on the basis of experimentally obtained data of XRD, VSM, and IR. Elastic parameters have been estimated using the cation distribution and FTIR data, with a resulting trend quite opposite to that of the lattice parameter.

  3. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina B. de [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Oliveira, Bras H. de, E-mail: bho@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica

    2013-01-15

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C{sub 18} column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min-1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 {+-} 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  4. Advances in organic-inorganic hybrid sorbents for the extraction of organic and inorganic pollutants in different types of food and environmental samples.

    Science.gov (United States)

    Ng, Nyuk-Ting; Kamaruddin, Amirah Farhan; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Abdul Keyon, Aemi S

    2017-08-21

    The efficiency of the extraction and removal of pollutants from food and the environment has been an important issue in analytical science. By incorporating inorganic species into an organic matrix, a new material known as an organic-inorganic hybrid material is formed. As it possesses high selectivity, permeability, and mechanical and chemical stabilities, organic-inorganic hybrid materials constitute an emerging research field and have become popular to serve as sorbents in various separaton science methods. Here, we review recent significant advances in analytical solid-phase extraction employing organic-inorganic composite/nanocomposite sorbents for the extraction of organic and inorganic pollutants from various types of food and environmental matrices. The physicochemical characteristics, extraction properties, and analytical performances of sorbents are discussed; including morphology and surface characteristics, types of functional groups, interaction mechanism, selectivity and sensitivity, accuracy, and regeneration abilities. Organic-inorganic hybrid sorbents combined with extraction techniques are highly promising for sample preparation of various food and environmental matrixes with analytes at trace levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Comparative genomic hybridization of microdissected samples from different stages in the development of a seminoma and a non-seminoma

    NARCIS (Netherlands)

    Looijenga, LHJ; Rosenberg, C; van Gurp, RJHLM; Geelen, E; van Echten-Arends, J; de Jong, B; Mostert, M

    2000-01-01

    Human testicular germ cell tumours (TGCTs) of adolescents and adults, both seminomas and non-seminomas, originate from intratubular germ cell neoplasia (IGCN). Comparative genomic hybridization (CGH) was applied to microdissected samples from different stages of the development of a seminoma and a m

  6. Comparative genomic hybridization of microdissected samples from different stages in the development of a seminoma and a non-seminoma

    NARCIS (Netherlands)

    Looijenga, LHJ; Rosenberg, C; van Gurp, RJHLM; Geelen, E; van Echten-Arends, J; de Jong, B; Mostert, M

    Human testicular germ cell tumours (TGCTs) of adolescents and adults, both seminomas and non-seminomas, originate from intratubular germ cell neoplasia (IGCN). Comparative genomic hybridization (CGH) was applied to microdissected samples from different stages of the development of a seminoma and a

  7. Hybrid Capture 2 and cobas human papillomavirus assays perform similarly on SurePath samples from women with abnormalities

    DEFF Research Database (Denmark)

    Fornari, D; Rebolj, M; Bjerregaard, B

    2016-01-01

    OBJECTIVE: In two laboratories (Departments of Pathology, Copenhagen University Hospitals of Herlev and Hvidovre), we compared cobas and Hybrid Capture 2 (HC2) human papillomavirus (HPV) assays using SurePath® samples from women with atypical squamous cells of undetermined significance (ASCUS) at...

  8. A hybrid design-based and model-based sampling approach to estimate the temporal trend of spatial means

    NARCIS (Netherlands)

    Brus, D.J.; Gruijter, de J.J.

    2012-01-01

    This paper launches a hybrid sampling approach, entailing a design-based approach in space followed by a model-based approach in time, for estimating temporal trends of spatial means or totals. The underlying space–time process that generated the soil data is only partly described, viz. by a linear

  9. Preparation and electrochemical performance of hyper-networked Li4Ti5O12/carbon hybrid nanofiber sheets for a battery-supercapacitor hybrid system.

    Science.gov (United States)

    Choi, Hong Soo; Kim, TaeHoon; Im, Ji Hyuk; Park, Chong Rae

    2011-10-07

    Hyper-networked Li(4)Ti(5)O(12)/carbon hybrid nanofiber sheets that contain both a faradaically rechargeable battery-type component, namely Li(4)Ti(5)O(12), and a non-faradaically rechargeable supercapacitor-type component, namely N-enriched carbon, are prepared by electrospinning and their dual function as a negative electrode of lithium-ion batteries (LIBs) and a capacitor is tested for a new class of hybrid energy storage (denoted BatCap). An aqueous solution composed of polyvinylpyrrolidone, lithium hydroxide, titanium(IV) bis(ammonium-lactato)dihydroxide and ammonium persulfate is electrospun to obtain hyper-networked nanofiber sheets. Next, the sheets are exposed to pyrrole monomer vapor to prepare the polypyrrole-coated nanofiber sheets (PPy-HNS). The hyper-networked Li(4)Ti(5)O(12)/N-enriched carbon hybrid nanofiber sheets (LTO/C-HNS) are then obtained by a stepwise heat treatment of the PPy-HNS. The LTO/C-HNS deliver a specific capacity of 135 mAh g(-1) at 4000 mA g(-1) as a negative electrode for LIBs. In addition, potentiodynamic experiments are performed using a full cell with activated carbon (AC) as the positive electrode and LTO/C-HNS as the negative electrode to estimate the capacitance properties. This new asymmetric electrode system exhibits a high energy density of 91 W kg(-1) and 22 W kg(-1) at power densities of 50 W kg(-1) and 4000 W kg(-1), respectively, which are superior to the values observed for the AC [symbol: see text] AC symmetric electrode system.

  10. Preparation and electrochemical performance of hyper-networked Li4Ti5O12/carbon hybrid nanofiber sheets for a battery-supercapacitor hybrid system

    Science.gov (United States)

    Choi, Hong Soo; Kim, TaeHoon; Im, Ji Hyuk; Park, Chong Rae

    2011-10-01

    Hyper-networked Li4Ti5O12/carbon hybrid nanofiber sheets that contain both a faradaically rechargeable battery-type component, namely Li4Ti5O12, and a non-faradaically rechargeable supercapacitor-type component, namely N-enriched carbon, are prepared by electrospinning and their dual function as a negative electrode of lithium-ion batteries (LIBs) and a capacitor is tested for a new class of hybrid energy storage (denoted BatCap). An aqueous solution composed of polyvinylpyrrolidone, lithium hydroxide, titanium(IV) bis(ammonium-lactato)dihydroxide and ammonium persulfate is electrospun to obtain hyper-networked nanofiber sheets. Next, the sheets are exposed to pyrrole monomer vapor to prepare the polypyrrole-coated nanofiber sheets (PPy-HNS). The hyper-networked Li4Ti5O12/N-enriched carbon hybrid nanofiber sheets (LTO/C-HNS) are then obtained by a stepwise heat treatment of the PPy-HNS. The LTO/C-HNS deliver a specific capacity of 135 mAh g - 1 at 4000 mA g - 1 as a negative electrode for LIBs. In addition, potentiodynamic experiments are performed using a full cell with activated carbon (AC) as the positive electrode and LTO/C-HNS as the negative electrode to estimate the capacitance properties. This new asymmetric electrode system exhibits a high energy density of 91 W kg - 1 and 22 W kg - 1 at power densities of 50 W kg - 1 and 4000 W kg - 1, respectively, which are superior to the values observed for the {AC} \\parallel {AC} symmetric electrode system.

  11. All-atom/coarse-grained hybrid predictions of distribution coefficients in SAMPL5

    Science.gov (United States)

    Genheden, Samuel; Essex, Jonathan W.

    2016-11-01

    We present blind predictions submitted to the SAMPL5 challenge on calculating distribution coefficients. The predictions were based on estimating the solvation free energies in water and cyclohexane of the 53 compounds in the challenge. These free energies were computed using alchemical free energy simulations based on a hybrid all-atom/coarse-grained model. The compounds were treated with the general Amber force field, whereas the solvent molecules were treated with the Elba coarse-grained model. Considering the simplicity of the solvent model and that we approximate the distribution coefficient with the partition coefficient of the neutral species, the predictions are of good accuracy. The correlation coefficient, R is 0.64, 82 % of the predictions have the correct sign and the mean absolute deviation is 1.8 log units. This is on a par with or better than the other simulation-based predictions in the challenge. We present an analysis of the deviations to experiments and compare the predictions to another submission that used all-atom solvent.

  12. New hybrid materials as Zn(II) sorbents in water samples

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Quintanilla, Damian, E-mail: damian.perez@urjc.es [Departamento de Quimica Inorganica y Analitica, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid (Spain); Sanchez, Alfredo; Hierro, Isabel del; Fajardo, Mariano [Departamento de Quimica Inorganica y Analitica, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid (Spain); Sierra, Isabel, E-mail: isabel.sierra@urjc.es [Departamento de Quimica Inorganica y Analitica, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid (Spain)

    2010-09-15

    Mesoporous silicas have been chemically modified with 5-mercapto-1-methyltetrazole (MTTZ) obtaining hybrid materials denominated MTTZ-MSU-2 and MTTZ-HMS. These materials were employed as Zn(II) sorbents from aqueous media at room temperature. The effect of several variables (stirring time, pH, presence of other metals) has been studied using batch and column techniques. Flame atomic absorption spectrometry (FAAS) was used to determinate Zn(II) concentration in the filtrate or in the eluted solution after the adsorption process. The results indicate that under pH 8, the maximum adsorption value was 0.94 {+-} 0.01 and 0.72 {+-} 0.01 mmol Zn(II)/g for MTTZ-MSU-2 and MTTZ-HMS, respectively. In tap water samples, a preconcentration factor of 200 was obtained. On the basis of these results, it can be concluded that it is possible to modify chemically MSU-2 and HMS with 5-mercapto-1-methyltetrazole and to use the resulting modified mesoporous silica as an effective adsorbent for Zn(II) in aqueous media.

  13. Flat mount preparation for observation and analysis of zebrafish embryo specimens stained by whole mount in situ hybridization.

    Science.gov (United States)

    Cheng, Christina N; Li, Yue; Marra, Amanda N; Verdun, Valerie; Wingert, Rebecca A

    2014-07-17

    The zebrafish embryo is now commonly used for basic and biomedical research to investigate the genetic control of developmental processes and to model congenital abnormalities. During the first day of life, the zebrafish embryo progresses through many developmental stages including fertilization, cleavage, gastrulation, segmentation, and the organogenesis of structures such as the kidney, heart, and central nervous system. The anatomy of a young zebrafish embryo presents several challenges for the visualization and analysis of the tissues involved in many of these events because the embryo develops in association with a round yolk mass. Thus, for accurate analysis and imaging of experimental phenotypes in fixed embryonic specimens between the tailbud and 20 somite stage (10 and 19 hours post fertilization (hpf), respectively), such as those stained using whole mount in situ hybridization (WISH), it is often desirable to remove the embryo from the yolk ball and to position it flat on a glass slide. However, performing a flat mount procedure can be tedious. Therefore, successful and efficient flat mount preparation is greatly facilitated through the visual demonstration of the dissection technique, and also helped by using reagents that assist in optimal tissue handling. Here, we provide our WISH protocol for one or two-color detection of gene expression in the zebrafish embryo, and demonstrate how the flat mounting procedure can be performed on this example of a stained fixed specimen. This flat mounting protocol is broadly applicable to the study of many embryonic structures that emerge during early zebrafish development, and can be implemented in conjunction with other staining methods performed on fixed embryo samples.

  14. Bio-sample preparation and gas chromatographic determination of benzodiazepines--a review.

    Science.gov (United States)

    Uddin, Mohammad Nasir; Samanidou, Victoria F; Papadoyannis, Ioannis N

    2013-08-01

    Benzodiazepines have become commonly prescribed medicines worldwide in the therapy of anxiety, sleep disorders and convulsive attacks because they are relatively safe, with mild side effects. The availability of rapid, sensitive and selective analytical methods is essential for the determination of these drugs in clinical and forensic cases. Benzodiazepines are usually present at trace levels (μg/mL or ng/mL) in a complex biological matrix, and the potentially interfering compounds need to be removed before analysis. Therefore, a sample preparation technique is often mandatory, both to extract the drugs of interest from the matrices and to increase their concentration. An extended and comprehensive review is presented herein, focusing on bio-sample preparation (pretreatment, extraction and derivatization) and gas chromatographic methods applied for the quantification of 1,4-benzodiazepines.

  15. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR.

    Science.gov (United States)

    Mandal, Abhishek; Boatz, Jennifer C; Wheeler, Travis B; van der Wel, Patrick C A

    2017-02-22

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  16. Sample preparation for the analysis of flavors and off-flavors in foods.

    Science.gov (United States)

    Wilkes, J G; Conte, E D; Kim, Y; Holcomb, M; Sutherland, J B; Miller, D W

    2000-06-01

    Off-flavors in foods may originate from environmental pollutants, the growth of microorganisms, oxidation of lipids, or endogenous enzymatic decomposition in the foods. The chromatographic analysis of flavors and off-flavors in foods usually requires that the samples first be processed to remove as many interfering compounds as possible. For analysis of foods by gas chromatography (GC), sample preparation may include mincing, homogenation, centrifugation, distillation, simple solvent extraction, supercritical fluid extraction, pressurized-fluid extraction, microwave-assisted extraction, Soxhlet extraction, or methylation. For high-performance liquid chromatography of amines in fish, cheese, sausage and olive oil or aldehydes in fruit juice, sample preparation may include solvent extraction and derivatization. Headspace GC analysis of orange juice, fish, dehydrated potatoes, and milk requires almost no sample preparation. Purge-and-trap GC analysis of dairy products, seafoods, and garlic may require heating, microwave-mediated distillation, purging the sample with inert gases and trapping the analytes with Tenax or C18, thermal desorption, cryofocusing, or elution with ethyl acetate. Solid-phase microextraction GC analysis of spices, milk and fish can involve microwave-mediated distillation, and usually requires adsorption on poly(dimethyl)siloxane or electrodeposition on fibers followed by thermal desorption. For short-path thermal desorption GC analysis of spices, herbs, coffee, peanuts, candy, mushrooms, beverages, olive oil, honey, and milk, samples are placed in a glass-lined stainless steel thermal desorption tube, which is purged with helium and then heated gradually to desorb the volatiles for analysis. Few of the methods that are available for analysis of food flavors and off-flavors can be described simultaneously as cheap, easy and good.

  17. Fast detection of Noroviruses using a real-time PCR assay and automated sample preparation

    Directory of Open Access Journals (Sweden)

    Schmid Michael

    2004-06-01

    Full Text Available Abstract Background Noroviruses (NoV have become one of the most commonly reported causative agents of large outbreaks of non-bacterial acute gastroenteritis worldwide as well as sporadic gastroenteritis in the community. Currently, reverse transcriptase polymerase chain reaction (RT-PCR assays have been implemented in NoV diagnosis, but improvements that simplify and standardize sample preparation, amplification, and detection will be further needed. The combination of automated sample preparation and real-time PCR offers such refinements. Methods We have designed a new real-time RT-PCR assay on the LightCycler (LC with SYBR Green detection and melting curve analysis (Tm to detect NoV RNA in patient stool samples. The performance of the real-time PCR assay was compared with that obtained in parallel with a commercially available enzyme immunoassay (ELISA for antigen detection by testing a panel of 52 stool samples. Additionally, in a collaborative study with the Baden-Wuerttemberg State Health office, Stuttgart (Germany the real-time PCR results were blindly assessed using a previously well-established nested PCR (nPCR as the reference method, since PCR-based techniques are now considered as the "gold standard" for NoV detection in stool specimens. Results Analysis of 52 clinical stool samples by real-time PCR yielded results that were consistent with reference nPCR results, while marked differences between the two PCR-based methods and antigen ELISA were observed. Our results indicate that PCR-based procedures are more sensitive and specific than antigen ELISA for detecting NoV in stool specimens. Conclusions The combination of automated sample preparation and real-time PCR provided reliable diagnostic results in less time than conventional RT-PCR assays. These benefits make it a valuable tool for routine laboratory practice especially in terms of rapid and appropriate outbreak-control measures in health-care facilities and other settings.

  18. Development of an automated sample preparation module for environmental monitoring of biowarfare agents.

    Science.gov (United States)

    Hindson, Benjamin J; Brown, Steve B; Marshall, Graham D; McBride, Mary T; Makarewicz, Anthony J; Gutierrez, Dora M; Wolcott, Duane K; Metz, Thomas R; Madabhushi, Ramakrishna S; Dzenitis, John M; Colston, Billy W

    2004-07-01

    An automated sample preparation module, based upon sequential injection analysis (SIA), has been developed for use within an autonomous pathogen detection system. The SIA system interfaced aerosol sampling with multiplexed microsphere immunoassay-flow cytometric detection. Metering and sequestering of microspheres using SIA was found to be reproducible and reliable, over 24-h periods of autonomous operation. Four inbuilt immunoassay controls showed excellent immunoassay and system stability over five days of unattended continuous operation. Titration curves for two biological warfare agents, Bacillus anthracis and Yersinia pestis, obtained using the automated SIA procedure were shown to be similar to those generated using a manual microtiter plate procedure.

  19. Optimization of Proteomic Sample Preparation Procedures for Comprehensive Protein Characterization of Pathogenic Systems

    Science.gov (United States)

    Mottaz-Brewer, Heather M.; Norbeck, Angela D.; Adkins, Joshua N.; Manes, Nathan P.; Ansong, Charles; Shi, Liang; Rikihisa, Yasuko; Kikuchi, Takane; Wong, Scott W.; Estep, Ryan D.; Heffron, Fred; Pasa-Tolic, Ljiljana; Smith, Richard D.

    2008-01-01

    Mass spectrometry-based proteomics is a powerful analytical tool for investigating pathogens and their interactions within a host. The sensitivity of such analyses provides broad proteome characterization, but the sample-handling procedures must first be optimized to ensure compatibility with the technique and to maximize the dynamic range of detection. The decision-making process for determining optimal growth conditions, preparation methods, sample analysis methods, and data analysis techniques in our laboratory is discussed herein with consideration of the balance in sensitivity, specificity, and biomass losses during analysis of host-pathogen systems. PMID:19183792

  20. Preparation and property of a novel soluble electron transport POSS-based hybrid material

    Institute of Scientific and Technical Information of China (English)

    Xin Wang; Juan Shen; Jin Cui Wu; Min Fang; Hong Yao Xu

    2008-01-01

    A novel POSS-based organic/inorganic hybrid covalently attached at molecular level, 2-(4-(allyloxy)phenyl)-5-(4-(octyloxy)phenyl)-1,3,4-oxadiazole-POSS (6) (abbreviated as oxadiazole-POSS) was synthesized by Pt (dcp) catalyst. The hybrid was soluble in common organic solvents such as CHCl3, toluene, C2H4Cl2, and THF. Its structures and properties were characterized and evaluated with FTIR, 1H NMR, 13C NMR, 29Si NMR, EA, TGA, DSC, GPC, and CV, respectively. The results show that the novel hybrid possesses high thermal stability and good electron injection ability.

  1. Preparation of Plant 41Ca Tracer Samples for Accelerator Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    ZHAO Qing-zhang1;JANG Ping-ping3;LIN De-yu4;YANG Xian-lin1;DOU Liang1;PANG Yi-jun1;WANG Xiao-ming1;ZHANG Hui1,5;YANG Xu-ran1;WU Shao-yong1;GAO Dong-sheng2;LI Ling2;WANG Lei2;SUN Ke-peng2;ZHOU Jun2;DONG Ke-jun1;HE Ming1

    2016-11-01

    Full Text Available Calcium plays an important role in the metabolism of plants and animals. In this paper, the preparation method of plant 41Ca for accelerator mass spectrometry (AMS measurement was developed for the first time in China. AMS, with its advantages of high sensitivity, small dose of radioactivity, high accuracy, large measuring range, and long tracer cycle, can be used to measure cosmogenic nuclide 41Ca , which has long half-life. The intensity of the beam in ion source is an important parameter for the sensitivity of AMS measurement. The high beam current can improve the sensitivity of AMS. The preparation methods of plant samples of 41Ca tracer were systematically studied to obtain high beam current using wet, dry and a combining method with wet and dry re-fluoride. A reliable preparation procedure of plant samples for 41Ca tracer and its optimization parameters were determined by testing beam currents of various samples and lay a foundation for the 41Ca-AMS technology at plant tracer applications.

  2. Sample preparation: a critical step in the analysis of cholesterol oxidation products.

    Science.gov (United States)

    Georgiou, Christiana A; Constantinou, Michalis S; Kapnissi-Christodoulou, Constantina P

    2014-02-15

    In recent years, cholesterol oxidation products (COPs) have drawn scientific interest, particularly due to their implications on human health. A big number of these compounds have been demonstrated to be cytotoxic, mutagenic, and carcinogenic. The main source of COPs is through diet, and particularly from the consumption of cholesterol-rich foods. This raises questions about the safety of consumers, and it suggests the necessity for the development of a sensitive and a reliable analytical method in order to identify and quantify these components in food samples. Sample preparation is a necessary step in the analysis of COPs in order to eliminate interferences and increase sensitivity. Numerous publications have, over the years, reported the use of different methods for the extraction and purification of COPs. However, no method has, so far, been established as a routine method for the analysis of COPs in foods. Therefore, it was considered important to overview different sample preparation procedures and evaluate the different preparative parameters, such as time of saponification, the type of organic solvents for fat extraction, the stationary phase in solid phase extraction, etc., according to recovery, precision and simplicity.

  3. DNA isolation and sample preparation for quantification of adduct levels by accelerator mass spectrometry.

    Science.gov (United States)

    Dingley, Karen H; Ubick, Esther A; Vogel, John S; Ognibene, Ted J; Malfatti, Michael A; Kulp, Kristen; Haack, Kurt W

    2014-01-01

    Accelerator mass spectrometry (AMS) is a highly sensitive technique used for the quantification of adducts following exposure to carbon-14- or tritium-labeled chemicals, with detection limits in the range of one adduct per 10(11)-10(12) nucleotides. The protocol described in this chapter provides an optimal method for isolating and preparing DNA samples to measure isotope-labeled DNA adducts by AMS. When preparing samples, special precautions must be taken to avoid cross-contamination of isotope among samples and produce a sample that is compatible with AMS. The DNA isolation method described is based upon digestion of tissue with proteinase K, followed by extraction of DNA using Qiagen isolation columns. The extracted DNA is precipitated with isopropanol, washed repeatedly with 70 % ethanol to remove salt, and then dissolved in water. DNA samples are then converted to graphite or titanium hydride and the isotope content measured by AMS to quantify adduct levels. This method has been used to reliably generate good yields of uncontaminated, pure DNA from animal and human tissues for analysis of adduct levels.

  4. On-chip sample preparation for complete blood count from raw blood.

    Science.gov (United States)

    Nguyen, John; Wei, Yuan; Zheng, Yi; Wang, Chen; Sun, Yu

    2015-03-21

    This paper describes a monolithic microfluidic device capable of on-chip sample preparation for both RBC and WBC measurements from whole blood. For the first time, on-chip sample processing (e.g. dilution, lysis, and filtration) and downstream single cell measurement were fully integrated to enable sample preparation and single cell analysis from whole blood on a single device. The device consists of two parallel sub-systems that perform sample processing and electrical measurements for measuring RBC and WBC parameters. The system provides a modular environment capable of handling solutions of various viscosities by adjusting the length of channels and precisely controlling mixing ratios, and features a new 'offset' filter configuration for increased duration of device operation. RBC concentration, mean corpuscular volume (MCV), cell distribution width, WBC concentration and differential are determined by electrical impedance measurement. Experimental characterization of over 100,000 cells from 10 patient blood samples validated the system's capability for performing on-chip raw blood processing and measurement.

  5. Preparation and optical and electrical evaluation of bulk SiO{sub 2} sonogel hybrid composites and vacuum thermal evaporated thin films prepared from molecular materials derived from (Fe, Co) metallic phthalocyanines and 1,8 dihydroxiantraquinone compounds

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez Vergara, Maria Elena [Coordinacion de Ingenieria Mecatronica, Facultad de Ingenieria, Universidad Anahuac Mexico Norte. Avenida Universidad Anahuac 46, Col. Lomas Anahuac, 52786 Huixquilucan, Estado de Mexico (Mexico); Morales-Saavedra, Omar G. [Universidad Nacional Autonoma de Mexico, Centro de Ciencias Aplicadas y Desarrollo Tecnologico, CCADET-UNAM, A.P. 70-186, Coyoacan, 04510 Mexico, D.F. (Mexico)], E-mail: omar.morales@ccadet.unam.mx; Ontiveros-Barrera, Fernando G.; Torres-Zuniga, Vicente; Ortega-Martinez, Roberto [Universidad Nacional Autonoma de Mexico, Centro de Ciencias Aplicadas y Desarrollo Tecnologico, CCADET-UNAM, A.P. 70-186, Coyoacan, 04510 Mexico, D.F. (Mexico); Ortiz Rebollo, Armando [Universidad Nacional Autonoma de Mexico, Instituto de Investigaciones en Materiales, IIM-UNAM, A.P. 70-360, Coyoacan, 04510 Mexico, D.F. (Mexico)

    2009-02-25

    Semiconducting molecular material of PcFe(CN)L1 and PcCo(CN)L1 (L1 = 1,8 dihydroxianthraquinone), PcFe(CN)L2 and PcCo(CN)L2 (L2 = double potassium salt of 1,8 dihydroxianthraquinone) have been successfully used to prepare thin film and bulk sol-gel hybrid optical materials. These samples were developed according to the vacuum thermal evaporation technique and the catalyst-free sonogel route, respectively. Thin films samples were deposited on Corning glass substrates and crystalline silicon wafers and were characterized by infrared (FTIR), Raman and ultraviolet-visible (UV-vis) spectroscopies. IR-spectroscopy and Raman studies unambiguously confirmed that the molecular material thin films exhibit the same intra-molecular bonds, which suggests that the thermal evaporation process does not alter these bonds significantly. These results show that it is possible to deposit molecular materials of PcFe(CN)L2 and PcCo(CN)L2 on Corning glass substrates and silicon wafers. From the UV-vis studies the optical band gap (E{sub g}) was evaluated. The effect of temperature on conductivity was also evaluated in these samples. Finally, the studied molecular systems dissolved at different concentrations in tetrahydrofuran (THF) were successfully embedded into a highly pure SiO{sub 2} sonogel network generated via sonochemical reactions to form several solid state, optically active sol-gel hybrid glasses. By this method, homogeneous and stable hybrid monoliths suitable for optical characterization can be produced. The linear optical properties of these amorphous bulk structures were determined by the Brewster angle method and by absorption-, Raman- and photoluminescent (PL)-spectroscopies, respectively.

  6. On a novel method to synthesize POSS-based hybrids: An example of the preparation of TPU based system

    Directory of Open Access Journals (Sweden)

    O. Monticelli

    2013-12-01

    Full Text Available A novel method to prepare polymer/polyhedral oligomeric silsesquioxanes (POSS hybrids by melt reactive blending is proposed in this paper, by the controlled polymer chain scission and reaction of chain ends with functional silsesquioxanes. Application to thermoplastic polyurethanes (TPU is addressed, taking advantage of the polyurethane chain scission equilibrium reaction, leading to the formation of highly reactive isocyanate and hydroxyl chain ends. Despite the isocyanate chemistry has been widely studied for the preparation of polymer/POSS hybrids by in situ copolymerisation, the exploitation of similar chemical processes in an industrially viable and environmental friendly melt blending process is currently an open research field. In this work, the reaction in the molten state of dihydroxyl-functionalised POSS with the polyurethane chain is demonstrated to produce a TPU/POSS hybrids. The effect of POSS concentration on nanomorphology, thermal properties and surface properties is studied, showing significant changes compared to pristine TPU. In particular, an increase of glass transition temperature is observed in the presence of reactive POSS (ΔT up to about 10°C in the presence of 10 wt% loading. Furthermore, an increase of surface water wettability, evidenced by the decrease of water contact angle from 95° for pristine TPU to 70° in TPU containing 10"wt% of reactive POSS, is found.

  7. Investigation of Tribological Behavior of a Novel Hybrid Composite Prepared with Al-Coconut Shell Ash Mixed with Graphite

    Science.gov (United States)

    Siva Sankara Raju, R.; Panigrahi, M. K.; Ganguly, R. I.; Srinivasa Rao, G.

    2017-08-01

    The present investigation develops a next-generation hybrid Al metal matrix composite using coconut shell ash (CSA) and graphite (Gr) reinforcement. Stir-casting is adapted to prepare an Al-1100-based composite. Three other composites of Al-Al2O3, Al-Al2O3-Gr, and Al-CSA are prepared that contain equivalent volume fractions of Al2O3, CSA, and Gr. These assist in comparisons among the three composites and the developed hybrid Al-CSA-Gr composite. The study reveals that the addition of 3 pct Gr improves the specific strength, toughness, and tribological properties. The Al-CSA composite shows better mechanical properties, such as tensile strength and hardness, than the other three composites. Gr addition helps the hybrid Al-CSA-Gr composite to attain better tribological properties with a slightly lower specific strength. Scanning electron microscopy studies of the worn material surfaces corroborate the findings of the abrasion testing. Elemental analyses by energy-dispersive X-ray spectroscopy of the debris from the counter-face of the tribo surface confirm the presence of Al, O, Si, Fe, Mn, and C.

  8. Improved sample preparation and counting techniques for enhanced tritium measurement sensitivity

    Science.gov (United States)

    Moran, J.; Aalseth, C.; Bailey, V. L.; Mace, E. K.; Overman, C.; Seifert, A.; Wilcox Freeburg, E. D.

    2015-12-01

    Tritium (T) measurements offer insight to a wealth of environmental applications including hydrologic tracking, discerning ocean circulation patterns, and aging ice formations. However, the relatively short half-life of T (12.3 years) limits its effective age dating range. Compounding this limitation is the decrease in atmospheric T content by over two orders of magnitude (from 1000-2000 TU in 1962 to low background proportional counters which, when combined, offer improved T measurement sensitivity (~4.5 mmoles of H2 equivalent) and will help expand the application of T age dating to smaller sample sizes linked to persistent environmental questions despite the limitations above. For instance, this approach can be used to T date ~ 2.2 mmoles of CH4 collected from sample-limited systems including microbial communities, soils, or subsurface aquifers and can be combined with radiocarbon dating to distinguish the methane's formation age from C age in a system. This approach can also expand investigations into soil organic C where the improved sensitivity will permit resolution of soil C into more descriptive fractions and provide direct assessments of the stability of specific classes of organic matter in soils environments. We are employing a multiple step sample preparation system whereby organic samples are first combusted with resulting CO2 and H2O being used as a feedstock to synthesize CH4. This CH4 is mixed with Ar and loaded directly into an ultra-low background proportional counter for measurement of T β decay in a shallow underground laboratory. Analysis of water samples requires only the addition of geologic CO2 feedstock with the sample for methane synthesis. The chemical nature of the preparation techniques enable high sample throughput with only the final measurement requiring T decay with total sample analysis time ranging from 2 -5 weeks depending on T content.

  9. Preparation and characterization of biodegradable aliphatic-aromatic copolyesters/nano-SiO_2 hybrids via in situ melt polycondensation

    Institute of Scientific and Technical Information of China (English)

    Yan Zhang; Bing Tao Wang; Zheng Hong Guo; Jie Chen; Zheng Ping Fang

    2009-01-01

    In situ melt polycondensation was proposed to prepare biodegradable aliphatic-aromatic copolyesters/nano-SiO_2 hybrids based on terephthalic acid (TPA), poly(L-lactic acid) oligomer (OLLA), 1,4-butanediol (BDO) and nano-SiO_2. TEM and FT-IR characterizations confirmed that TPA, OLLA and BDO copolymerized to obtain biodegradable copolyesters, poly(butylene terephthalate-co-lactate) (PBTL), and the abundant hydroxyl groups on the surface of nano-SiO_2 provided potential sites for in situ grafting with the simultaneous resulted PBTL. The nano-SiO_2 particles were chemically wrapped with PBTL to form PBTL/nano-SiO2 hybrids. Due to the good dispersion and interfacial adhesion of nano-SiO_2 particles with the copolyester matrix, the tensile strength and the Young's modulus increased from 5.4 and 5.6 Mpa for neat PBTL to 16 and 390 Mpa for PBTL/nano-SiO_2 hybrids with 5 wt.% nano-SiO_2, respectively. The mechanical properties of PBTL/nano-SiO_2 hybrids were substantially improved.

  10. Preparation of Graphene/Gold Nano-Hybrid Using Diamine Linker as Effective Surface-Enhanced Raman Scattering Platforms.

    Science.gov (United States)

    Yoon, Sang Su; Lee, Wonoh; Byun, Joon Hyung; Lee, Jea Uk

    2015-11-01

    Development of simple and efficient method for the large-scale production of gaphene/metal nanoparticle hybrids is highly desirable for practical applications, such as catalyst, energy generation and storage, optoelectronics, and sensors. Here, we present a facile approach for the preparation of graphene/gold nanoparticle (AuNP) hybrids by simply mixing the functionalized graphene oxide and AuNPs in aqueous media. Among various functionalized graphene sheets, amine-functionalized graphene oxide (GO-NH2) is used as the hybrid platform due to its synthetic convenience, good dispersity, scalable production with low cost, and positive charge on the surfacce, which could immobilize the AuNPs on the graphene sheets via electrostatic interaction. The synthesized graphene/AgNP hybrids show high surface-enhanced Raman scattering (SERS) sensitivity due to the combined effects of the high contents of amine functional groups on the GO-NH2 surface to adsorb more AgNPs and the electromagnetic enhancement of AgNPs.

  11. Reducing time and increasing sensitivity in sample preparation for adherent mammalian cell metabolomics.

    Science.gov (United States)

    Lorenz, Matthew A; Burant, Charles F; Kennedy, Robert T

    2011-05-01

    A simple, fast, and reproducible sample preparation procedure was developed for relative quantification of metabolites in adherent mammalian cells using the clonal β-cell line INS-1 as a model sample. The method was developed by evaluating the effect of different sample preparation procedures on high performance liquid chromatography- mass spectrometry quantification of 27 metabolites involved in glycolysis and the tricarboxylic acid cycle on a directed basis as well as for all detectable chromatographic features on an undirected basis. We demonstrate that a rapid water rinse step prior to quenching of metabolism reduces components that suppress electrospray ionization thereby increasing signal for 26 of 27 targeted metabolites and increasing total number of detected features from 237 to 452 with no detectable change of metabolite content. A novel quenching technique is employed which involves addition of liquid nitrogen directly to the culture dish and allows for samples to be stored at -80 °C for at least 7 d before extraction. Separation of quenching and extraction steps provides the benefit of increased experimental convenience and sample stability while maintaining metabolite content similar to techniques that employ simultaneous quenching and extraction with cold organic solvent. The extraction solvent 9:1 methanol: chloroform was found to provide superior performance over acetonitrile, ethanol, and methanol with respect to metabolite recovery and extract stability. Maximal recovery was achieved using a single rapid (∼1 min) extraction step. The utility of this rapid preparation method (∼5 min) was demonstrated through precise metabolite measurements (11% average relative standard deviation without internal standards) associated with step changes in glucose concentration that evoke insulin secretion in the clonal β-cell line INS-1.

  12. Increasing the sampling efficiency of protein conformational transition using velocity-scaling optimized hybrid explicit/implicit solvent REMD simulation

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Yuqi; Wang, Jinan; Shao, Qiang, E-mail: qshao@mail.shcnc.ac.cn, E-mail: Jiye.Shi@ucb.com, E-mail: wlzhu@mail.shcnc.ac.cn; Zhu, Weiliang, E-mail: qshao@mail.shcnc.ac.cn, E-mail: Jiye.Shi@ucb.com, E-mail: wlzhu@mail.shcnc.ac.cn [ACS Key Laboratory of Receptor Research, Drug Discovery and Design Center, Shanghai Institute of Materia Medica, Chinese Academy of Sciences, 555 Zuchongzhi Road, Shanghai 201203 (China); Shi, Jiye, E-mail: qshao@mail.shcnc.ac.cn, E-mail: Jiye.Shi@ucb.com, E-mail: wlzhu@mail.shcnc.ac.cn [UCB Pharma, 216 Bath Road, Slough SL1 4EN (United Kingdom)

    2015-03-28

    The application of temperature replica exchange molecular dynamics (REMD) simulation on protein motion is limited by its huge requirement of computational resource, particularly when explicit solvent model is implemented. In the previous study, we developed a velocity-scaling optimized hybrid explicit/implicit solvent REMD method with the hope to reduce the temperature (replica) number on the premise of maintaining high sampling efficiency. In this study, we utilized this method to characterize and energetically identify the conformational transition pathway of a protein model, the N-terminal domain of calmodulin. In comparison to the standard explicit solvent REMD simulation, the hybrid REMD is much less computationally expensive but, meanwhile, gives accurate evaluation of the structural and thermodynamic properties of the conformational transition which are in well agreement with the standard REMD simulation. Therefore, the hybrid REMD could highly increase the computational efficiency and thus expand the application of REMD simulation to larger-size protein systems.

  13. Soybean and lactose in meat products and preparations sampled at retail

    Directory of Open Access Journals (Sweden)

    Filomena Piccolo

    2016-06-01

    Full Text Available Food allergies and intolerances have increased during the last decades and regulatory authorities have taken different measures to prevent and manage consumers’ adverse reactions, including correct labelling of foods. Aim of this work was to search for soybean and lactose in meat products and meat preparations taken from retail in some provinces of Campania Region (Southern Italy and to evaluate the food labels compliance with Regulation (EU n.1169/2011. Soybean and lactose were searched using commercial kits in n. 58 samples of meat products produced in or distributed by 19 establishments, and in n. 55 samples of meat products and n. 8 of meat preparations produced in 21 plants. All samples were selected on the basis of the absence of any information on the labels about the presence of the two searched allergens, with the exception of n. 5 samples tested for lactose. Traces of soybean were detected in 50 out of the 58 examined samples, at concentrations up to 0.93 mg kg–1. Only two samples contained levels above the detection limit of 0.31 mg kg–1. Lactose levels ranging from 0.11 to 2.95 g/100 g, i.e. above the detection limit, were found in all the tested samples (n. 63. The results of the present research underline the need for careful controls and planning by operators as part of the self-control plans, and deserve attention from the competent authorities considering not only the consumers’ health but also the great attention media pay to regulations providing consumers with information on food.

  14. Preparation and Photocatalytic Application of High Temperature Stabilized ZrSiO4@TiO2 Hybrid Nanostructure

    Institute of Scientific and Technical Information of China (English)

    PENG Cheng; FANG Peiyu; ZENG Zhichao; Lü Ming; WU Jianqing

    2014-01-01

    A new ZrSiO4@TiO2 hybrid nanostructure was prepared by a heterogeneous flocculation method. Phytic acid was introduced to modify the surface charging of the components for hybrid assembly. The obtained powder was coated on ceramic tiles and fired at 900 ℃ to fabricate photocatalytic ceramic. Experimental results show that anatase TiO2 in the composite powder has high thermal stability until 1 200℃. ZrSiO4 matrix prevents the mass transfer of anatase TiO2 at high temperature and greatly retards the phase transition of anatase to rutile. Besides, the photocatalytic ceramic shows apparent activities for the degradation of methyl orange under ultra-violet irradiation.

  15. Coordination-driven in situ self-assembly strategy for the preparation of metal-organic framework hybrid membranes.

    Science.gov (United States)

    Zhang, Rong; Ji, Shulan; Wang, Naixin; Wang, Lin; Zhang, Guojun; Li, Jian-Rong

    2014-09-08

    Metal-organic frameworks (MOFs) have emerged as porous solids of a superior type for the fabrication of membranes. However, it is still challenging to prepare a uniformly dispersed robust MOF hybrid membrane. Herein, we propose a simple and powerful strategy, namely, coordination-driven in situ self-assembly, for the fabrication of MOF hybrid membranes. On the basis of the coordination interactions between metal ions and ligands and/or the functional groups of the organic polymer, this method was confirmed to be feasible for the production of a stable membrane with greatly improved MOF-particle dispersion in and compatibility with the polymer, thus providing outstanding separation ability. As an experimental proof of concept, a high-quality ZIF-8/PSS membrane was fabricated that showed excellent performance in the nanofiltration and separation of dyes from water.

  16. A hybrid DNA extraction method for the qualitative and quantitative assessment of bacterial communities from poultry production samples.

    Science.gov (United States)

    Rothrock, Michael J; Hiett, Kelli L; Gamble, John; Caudill, Andrew C; Cicconi-Hogan, Kellie M; Caporaso, J Gregory

    2014-12-10

    The efficacy of DNA extraction protocols can be highly dependent upon both the type of sample being investigated and the types of downstream analyses performed. Considering that the use of new bacterial community analysis techniques (e.g., microbiomics, metagenomics) is becoming more prevalent in the agricultural and environmental sciences and many environmental samples within these disciplines can be physiochemically and microbiologically unique (e.g., fecal and litter/bedding samples from the poultry production spectrum), appropriate and effective DNA extraction methods need to be carefully chosen. Therefore, a novel semi-automated hybrid DNA extraction method was developed specifically for use with environmental poultry production samples. This method is a combination of the two major types of DNA extraction: mechanical and enzymatic. A two-step intense mechanical homogenization step (using bead-beating specifically formulated for environmental samples) was added to the beginning of the "gold standard" enzymatic DNA extraction method for fecal samples to enhance the removal of bacteria and DNA from the sample matrix and improve the recovery of Gram-positive bacterial community members. Once the enzymatic extraction portion of the hybrid method was initiated, the remaining purification process was automated using a robotic workstation to increase sample throughput and decrease sample processing error. In comparison to the strict mechanical and enzymatic DNA extraction methods, this novel hybrid method provided the best overall combined performance when considering quantitative (using 16S rRNA qPCR) and qualitative (using microbiomics) estimates of the total bacterial communities when processing poultry feces and litter samples.

  17. Rapid Measurement of Food Adulteration with Minimal Sample Preparation and No Chromatography Using Ambient Ionization Mass Spectrometry.

    Science.gov (United States)

    Dalmia, Avinash

    2017-03-01

    A rapid method, with minimal sample preparation and no chromatography, was developed for analyzing food samples such as olive oil and pomegranate juice to measure adulteration with cheaper ingredients using the novel Direct Sample Analysis™ (DSA) ion source in conjunction with a time-of-flight (TOF)-MS. In less than 30 s, with minimal sample preparation and method development, adulteration of olive oil and pomegranate juice with cheaper seed oils and fruit juices, respectively, was measured with DSA/TOF-MS.

  18. Membrane-based sample preparation for ion chromatography-Techniques, instrumental configurations and applications.

    Science.gov (United States)

    Frenzel, Wolfgang; Markeviciute, Inga

    2017-01-06

    Sample preparation is the bottleneck of many analytical methods, including ion chromatography (IC). Procedures based on the application of membranes are important, yet not well appreciated means for clean-up and analyte preconcentration of liquid samples. Filtration, ultrafiltration, the variety of dialysis techniques, i.e. passive dialysis, Donnan dialysis and electrodialysis, as well as gas-diffusion are being reviewed here with respect to their application in combination with IC. Instrumental aspects including hardware requirements, configuration of membrane separation units and membrane characteristics are presented. Operation in batch and flow-through mode is described with emphasis on the latter to in-line coupling with IC, permitting fully automated operation. Attention is also drawn to dialysis probes and microdialysis both providing options for in-situ measurements with inherent selective sampling of analytes and sample preparation. The respective features of the various techniques are outlined with respect to the possibilities of matrix removal and selectivity enhancement. In this article, we provide examples of application of the diverse membrane separation techniques and discuss the benefits and limitations thereof.

  19. Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

    Directory of Open Access Journals (Sweden)

    Vuković Gorica L.

    2009-01-01

    Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

  20. Preparation of highly stable fullerene C60 decorated graphene oxide nanocomposite and its sensitive electrochemical detection of dopamine in rat brain and pharmaceutical samples.

    Science.gov (United States)

    Thirumalraj, Balamurugan; Palanisamy, Selvakumar; Chen, Shen-Ming; Lou, Bih-Show

    2016-01-15

    The research community has continuously paid much attention on the preparation of hybrid of carbon nanomaterials owing to combine their unique properties. Herein, we report the preparation of highly stable fullerene C60 (C60) wrapped graphene oxide (GO) nanocomposite by using a simple sonication method. The fabricated GO-C60 nanocomposite modified glassy carbon electrode shows a good sensitivity and lower oxidation overpotential towards dopamine (DA) than that of pristine GO and C60. The fabricated sensor detects the DA in the linear response range of 0.02-73.5μM. The limit of detection is estimated to be 0.008μM based on 3σ with a sensitivity of 4.23μAμM(-1)cm(-2). The fabricated sensor also exhibits other features such as good selectivity, stability, reproducibility and repeatability. The proposed sensor exhibits good practicality towards the detection of DA in rat brain and commercial DA injection samples.

  1. Removal of interfering substances in samples prepared for two-dimensional (2-D) electrophoresis.

    Science.gov (United States)

    Berkelman, Tom

    2008-01-01

    Biological samples may contain contaminants that interfere with analysis by two-dimensional (2-D) electrophoresis. Lysates or biological fluids are complex mixtures that contain a wide variety of nonprotein substances in addition to the proteins to be analyzed. These substances often interfere with the resolution of the electrophoretic separation or the visualization of the result. Macromolecules (e.g., polysaccharides and DNA) can interfere with electrophoretic separation by clogging gel pores. Small ionic molecules can impair isoelectric focusing (IEF) separation by rendering the sample too conductive. Other substances (e.g., phenolics and lipids) can bind to proteins, influencing their electrophoretic properties or solubility. In many cases, measures to remove interfering substances can result in significantly clearer 2-D patterns with more visible spots and better resolution. It should be borne in mind, however, that analysis of samples by 2-D electrophoresis is usually most successful and informative when performed with minimally processed samples, so it is important that any steps taken to remove interfering substance be appropriate to the sample and only performed when necessary. Procedures for the removal of interfering substances therefore represent a compromise between removing nonprotein contaminants, and minimizing interference with the integrity and relative abundances of the sample proteins. This chapter presents a number of illustrative examples of optimized sample preparation methods in which specific interfering substances are removed by a variety of different strategies.

  2. Design and Preparation of RF System for the Lower Hybrid Fast Wave Heating and Current Drive Research on VEST

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Sun Ho; Jeong, Seung Ho [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Lee, Hyun Woo; Lee, Byung Je [Kwang Woon University, Chuncheon (Korea, Republic of); Jo, Jong Gab; Lee, Hyun Young; Hwang, Yong Seok [Seoul National University, Seoul (Korea, Republic of)

    2015-10-15

    Continuous current drive is one of the key issues for tokamak to be a commercial fusion reactor. As a part of new and efficient current drive concept research by using a Lower Hybrid Fast Wave (LHFW), the experimental study is planned on Versatile Experiment Spherical Torus (VEST) and a RF system is being developed in collaboration with Kwang Woon University (KWU), Korea Accelerator Plasma Research Association (KAPRA) and Seoul National University (SNU). The LHFW RF system includes UHF band klystron, inter-digital antenna, RF diagnostics and power transmission sub components such as circulator, DC breaker, vacuum feed-thru. The design and preparation status of the RF system will be presented in the meeting in detail. A RF system has been designed and prepared for the experimental study of efficient current drive by using Lower Hybrid Fast Wave. Overall LHFW RF system including diagnostics is designed to deliver about 10 kW in UHF band. And the key hardware components including klystron and antenna are being prepared and designed through the collaboration with KWU, KAPRA and SNU.

  3. A developed wedge fixtures assisted high precision TEM samples pre-thinning method: Towards the batch lamella preparation

    Directory of Open Access Journals (Sweden)

    Dandan Wang

    2017-04-01

    Full Text Available Ion milling, wedge cutting or polishing, and focused ion beam (FIB milling are widely-used techniques for the transmission electron microscope (TEM sample preparation. Especially, the FIB milling provides a site-specific analysis, deposition, and ablation of materials in the micrometer and nanometer scale. However, the cost of FIB tools has been always a significant concern. Since it is inevitable to use the FIB technique, the improvement of efficiency is a key point. Traditional TEM sample preparation with FIB was routinely implemented on a single sample each time. Aiming at cost efficiency, a new pre-thinning technique for batch sample preparation was developed in this paper. The present proposal combines the sample preparation techniques with multi-samples thinning, cross-section scanning electron microscopy (SEM, wedge cutting, FIB and other sample pre-thinning techniques. The new pre-thinning technique is to prepare an edge TEM sample on a grinding and polishing fixture with a slant surface. The thickness of the wedges sample can be measured to 1∼2 μm under optical microscope. Therefore, this fixture is superior to the traditional optical method of estimating the membrane thickness. Moreover, by utilizing a multi-sample holding fixture, more samples can be pre-thinned simultaneously, which significantly improved the productivity of TEM sample preparation.

  4. Evaluation of neon focused ion beam milling for TEM sample preparation.

    Science.gov (United States)

    Pekin, T C; Allen, F I; Minor, A M

    2016-10-01

    Gallium-based focused ion beams generated from liquid-metal sources are widely used in micromachining and sample preparation for transmission electron microscopy, with well-known drawbacks such as sample damage and contamination. In this work, an alternative (neon) focused ion beam generated by a gas field-ionization source is evaluated for the preparation of electron-transparent specimens. To do so, electron-transparent sections of Si and an Al alloy are prepared with both Ga and Ne ion beams for direct comparison. Diffraction-contrast imaging and energy dispersive x-ray spectroscopy are used to evaluate the relative damage induced by the two beams, and cross-sections of milled trenches are examined to compare the implantation depth with theoretical predictions from Monte Carlo simulations. Our results show that for the beam voltages and materials systems investigated, Ne ion beam milling does not significantly reduce the focused ion beam induced artefacts. However, the Ne ion beam does enable more precise milling and may be of interest in cases where Ga contamination cannot be tolerated.

  5. A Novel Sample Preparation for Shotgun Proteomics Characterization of HCPs in Antibodies.

    Science.gov (United States)

    Huang, Lihua; Wang, Ning; Mitchell, Charles E; Brownlee, Tammy; Maple, Steven R; De Felippis, Michael R

    2017-05-16

    Residual host cell proteins (HCPs) in biopharmaceuticals derived from recombinant DNA technology can present potential safety risks to patients or compromise product stability. Thus, the downstream purification process is designed to demonstrate robust removal of these impurities. ELISA using polyclonal anti-HCP antibodies as reagents for capture, detection, and quantitation purposes is most commonly used to monitor HCP removal during process development, but this technique has limitations. More recently, LC-MS for residual HCP characterization has emerged as a powerful tool to support purification process development. However, mass spectrometry needs to overcome the enormous dynamic range to detect low ppm levels of residual HCPs in biopharmaceutical samples. We describe a simple and powerful methodology to characterize residual HCPs in (monoclonal) antibodies by combining a novel sample preparation procedure using trypsin digestion and a shotgun proteomics approach. Differing from the traditional methodology, the sample preparation approach maintains nearly intact antibody while HCPs are digested. Thus, the dynamic range for HCP detection by MS is 1 to 2 orders of magnitude less than the traditional trypsin digestion sample preparation procedure. HCP spiking experiments demonstrated that our method could detect 0.5 ppm of HCP with molecular weight >60 kDa, such as rPLBL2. Application of our method to analyze a high-purity NIST monoclonal antibody standard RM 8670 derived from a murine cell line expression system resulted in detection of 60 mouse HCPs; twice as many as previously reported with 2D-UPLC/IM/MS(E) method. A control monoclonal antibody used for 70 analyses over 450 days demonstrated that our method is robust.

  6. Novel sample preparation method for surfactant containing suppositories: effect of micelle formation on drug recovery.

    Science.gov (United States)

    Kalmár, Éva; Ueno, Konomi; Forgó, Péter; Szakonyi, Gerda; Dombi, György

    2013-09-01

    Rectal drug delivery is currently at the focus of attention. Surfactants promote drug release from the suppository bases and enhance the formulation properties. The aim of our work was to develop a sample preparation method for HPLC analysis for a suppository base containing 95% hard fat, 2.5% Tween 20 and 2.5% Tween 60. A conventional sample preparation method did not provide successful results as the recovery of the drug failed to fulfil the validation criterion 95-105%. This was caused by the non-ionic surfactants in the suppository base incorporating some of the drug, preventing its release. As guidance for the formulation from an analytical aspect, we suggest a well defined surfactant content based on the turbidimetric determination of the CMC (critical micelle formation concentration) in the applied methanol-water solvent. Our CMC data correlate well with the results of previous studies. As regards the sample preparation procedure, a study was performed of the effects of ionic strength and pH on the drug recovery with the avoidance of degradation of the drug during the procedure. Aminophenazone and paracetamol were used as model drugs. The optimum conditions for drug release from the molten suppository base were found to be 100 mM NaCl, 20-40 mM NaOH and a 30 min ultrasonic treatment of the final sample solution. As these conditions could cause the degradation of the drugs in the solution, this was followed by NMR spectroscopy, and the results indicated that degradation did not take place. The determined CMCs were 0.08 mM for Tween 20, 0.06 mM for Tween 60 and 0.04 mM for a combined Tween 20, Tween 60 system. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Sample preparation methods for beeswax characterization by gas chromatography with flame ionization detection.

    Science.gov (United States)

    Jiménez, J J; Bernal, J L; del Nozal, M A J; Martín, M A T; Bernal, J

    2006-10-06

    New and simpler methods of sample preparation to determine several families of compounds in beeswax by conventional and high temperature gas chromatography are proposed. To analyze hydrocarbons and palmitates, a dilution of sample is enough whereas for the total acid content, a hydrolysis and simultaneous methylation with BF3-methanol results more effective than the usual methods; for the total content of alcohols, a further acetylation with acetic anhydride is necessary. Free alcohols are directly acetylated in a sample dissolution but for free acids and monoesterified 1,2,3-propanetriols analysis, a previous extraction with acetonitrile is required. The concentrations of all the compounds studied are expressed in weight percentage referred only to one standard: octadecyl octadecanoate. The precision of the analytical methods has been evaluated showing its importance in the analysis of beeswaxes used in apiculture.

  8. Multifunctional Fe{sub 3}O{sub 4}@C@Ag hybrid nanoparticles: Aqueous solution preparation, characterization and photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Hongxia [School of Chemistry and Chemical Engineering, Anhui University, Hefei 230039 (China); Niu, Helin, E-mail: niuhelin@ahu.edu.cn [School of Chemistry and Chemical Engineering, Anhui University, Hefei 230039 (China); Li, Ping; Tao, Zhiyin; Mao, Changjie; Song, Jiming; Zhang, Shengyi [School of Chemistry and Chemical Engineering, Anhui University, Hefei 230039 (China)

    2013-07-15

    Highlights: ► Ag-loaded Fe{sub 3}O{sub 4}@C magnetic-optical bifunctional materials have been investigated. ► The magnetism was studied at the room temperature. ► The photocatalytic activity was evaluated under visible light irradiation. ► Ag-loaded Fe{sub 3}O{sub 4}@C nanocomposites show superior magnetism and photocatalytic activity. ► A simple synthetic process was discussed. - Abstract: The paper describes a kind of multifunctional Fe{sub 3}O{sub 4}@C@Ag hybrid nanoparticles, which can be successfully synthesized using a simple route based on directly adsorption and spontaneous reduction of silver ions onto the surface shell of carbon-coated magnetic nanoparticles. The as-prepared samples have been characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), Fourier transform infrared (FT-IR) spectrum, vibrating sample magnetometer (VSM) and UV–vis spectrum (UV–vis). The Ag nanocrystals loaded on the surface shell of carbon-coated magnetic nanoparticles are nearly spherical with an average diameter of 10 nm. And the carbonaceous polysaccharides shell obtained using an glucose hydrothermal reaction act as a role of a bridge between magnetic Fe{sub 3}O{sub 4} core and noble metallic Ag nanocrystals. The as-prepared samples can be used as an effective catalyst for the photodegradation of organic dyes (neutral red) under the exposure of visible light. Results show that the as-prepared samples have a degradation rate of 93.7% for dyes within 30 min, which indicates their high-efficiency and rapid photocatalytic activity.

  9. Practical Guide to Using Cryoprotectants in Biological Sample Preparation at Cryogenic temperature for Electron Microscopic Studies

    Directory of Open Access Journals (Sweden)

    A-Reum Je

    2011-10-01

    Full Text Available Cryo-fixation enables the preservation of the fine structures of intracellular organelles in a condition that is as close to their native state as possible compared with chemical fixation and room temperature processing. Fixation is the initial step for biological sample preparation in electron microscopy. This step is critically important because the goals of electron microscopic observation are fundamentally dependent on well-preserved specimens resulting from this fixation. In the present work, key components of cryo-fixation, cryoprotectants, are tested with various cell types of interest. The results show that dextran can be easily adapted for use with animal cells and cyanobacteria, whereas 1-hexadecene is applicable to plant and yeast cells. The current report provides useful information on the preparation of cryo-fixed biological specimens using high pressure freezing and freeze-substitution aimed at electron microscopic observation.

  10. Laboratory Investigation of Rivers State Clay Samples for Drilling Mud Preparation

    Directory of Open Access Journals (Sweden)

    Nmegbu, Chukwuma Godwin Jacob

    2014-06-01

    Full Text Available Drilling fluids are an integral part of any oil and gas industry, providing the ease to which wells are drilled to access subsurface reservoir fluids. Certain rheology and mineralogical properties of the clay material used for drilling mud preparation must be critically investigated since clay deposits in different location exhibits different characteristics. Clay samples were collected from three different geographical locations namely; Egbamini (Emolga, Afam Street (Port Harcourt and Oboboru (onelga local government areas in Rivers state. Their rheological and wall building properties were measured in the laboratory to determine their suitability for drilling mud formulation. Results showed that in their respective native states, they proved unsuitable for drilling mud preparation when compared to standard Bentonite because they were observed to show responses far below the required API standards for mud formulation.

  11. Preparation of carbon-nitride bulk samples in the presence of seed carbon-nitride films

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J. I. [Korea University of Technology and Education, Chonan (Korea, Republic of); Zorov, N. B. [Moscow State University, Moscow (Russian Federation)

    2004-05-15

    A procedure was developed for preparing bulk carbon-nitride crystals from polymeric alpha-C{sub 3}N{sub 4.2} at high pressure and high temperature in the presence of seeds of crystalline carbon-nitride films prepared by using a high-voltage discharge plasma combined with pulsed laser ablation of a graphite target. The samples were evaluated by using X-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, Auger electron spectroscopy (AES), secondary-ion mass spectrometry (SIMS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Notably, XPS studies of the film composition before and after thermobaric treatments demonstrated that the nitrogen composition in the alpha-C{sub 3}N{sub 4.2} material, which initially contained more than 58 % nitrogen, decreased during the annealing process and reached a common, stable composition of approx 45 %. The thermobaric experiments were performed at 10 - 77 kbar and 350 - 1200 .deg. C.

  12. Improved sample preparation for CE-LIF analysis of plant N-glycans.

    Science.gov (United States)

    Nagels, Bieke; Santens, Francis; Weterings, Koen; Van Damme, Els J M; Callewaert, Nico

    2011-12-01

    In view of glycomics studies in plants, it is important to have sensitive tools that allow one to analyze and characterize the N-glycans present on plant proteins in different species. Earlier methods combined plant-based sample preparations with CE-LIF N-glycan analysis but suffered from background contaminations, often resulting in non-reproducible results. This publication describes a reproducible and sensitive protocol for the preparation and analysis of plant N-glycans, based on a combination of the 'in-gel release method' and N-glycan analysis on a multicapillary DNA sequencer. Our protocol makes it possible to analyze plant N-glycans starting from low amounts of plant material with highly reproducible results. The developed protocol was validated for different plant species and plant cells.

  13. Preparation of novel ferrocene-based shell cross-linked thermoresponsive hybrid micelles with antitumor efficacy.

    Science.gov (United States)

    Wei, Hua; Quan, Chang-Yun; Chang, Cong; Zhang, Xian-Zheng; Zhuo, Ren-Xi

    2010-04-29

    The shell cross-linked (SCL) thermoresponsive hybrid poly(N-isopropylacrylamide-co-aminoethyl methacrylate)-b-polymethyl methacrylate (P(NIPAAm-co-AMA)-b-PMMA) micelle consisting of a cross-linked thermoresponsive hybrid shell and a hydrophobic core domain was fabricated via a two-step process: micellization of P(NIPAAm-co-AMA)-b-PMMA in aqueous solution followed by cross-linking of the hydrophilic shell layer via the amidation reaction between the amine groups of AMA units and the carboxylic acid functions of 1,1'-ferrocenedicarboxylic acid. The SCL micelle showed reversible dispersion/aggregation in response to the temperature cycles through the lower critical solution temperature (LCST) of the thermoresponsive hybrid shell at around 36 degrees C, observed by turbidity measurements and dynamic light scattering (DLS). Besides the usage as an inorganic difunctional cross-linker, the inorganic ferrocene segment further endowed the SCL hybrid micelle with the antitumor efficacy, namely, the resulting SCL micelle exhibited a remarkable cytotoxic effect for HeLa cells with a very low IC50. The results showed that the SCL hybrid micelle developed in this study could be potentially used as an antitumor agent, which is unique compared to the conventional tumor therapy by using the antitumor drug loaded in the micellar core.

  14. A home-made hybrid system for the simultaneous determination of ergotamine, dipyrone and caffeine in pharmaceutical preparations

    OpenAIRE

    2007-01-01

    A novel home-made hybrid detection system was designed for simultaneous determination of caffeine (CAF), dipyrone (DIP) and ergotamine (ERG) in pharmaceutical preparations. Thus, ERG was determined by a fluorimetric signal and PLS-1 method for resolving DIP and CAF UV-Vis spectral data was used. The calibration curve for ERG was linear over the range 2.5-10 mg L-1. The calibration set consisted of 18 mixtures with 0.5 to 4 mg L-1 for CAF, 5 to 20 mg L-1 for DIP and 2.5 and 10 mg L-1 for ERG. ...

  15. Dopamine/TiO{sub 2} hybrid thin films prepared by the liquid phase deposition method

    Energy Technology Data Exchange (ETDEWEB)

    Gutierrez-Tauste, David [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain)], E-mail: davidg@qf.uab.es; Domenech, Xavier [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain); Domingo, Concepcion [Instituto de Ciencia de Materiales (CSIC), Campus UAB, 08290 Cerdanyola del Valles, Barcelona (Spain); Ayllon, Jose A. [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain)

    2008-04-30

    Liquid phase deposition method is applied to one-step production of a hybrid material composed by dopamine(DA) and TiO{sub 2} anatase. An optimized amount of the enediol derivative is added to a fluoride titania precursor aqueous solution in order to entrap this modifier within the growing TiO{sub 2}, yielding a DA/TiO{sub 2} nanocomposite material. Uniform, well-adhered and brown-colored thin films are deposited on indium tin oxide covered glass substrate. The DA/TiO{sub 2} hybrid material has been characterized by infrared spectroscopy, electronic microscopy, X-ray diffraction and UV-vis spectroscopy. The formation of the hybrid material seems to be reasonably explained by linkage of different TiO{sub 2} nanocrystallites taking advantage of both enediol and amine groups of DA.

  16. Human genomic DNA analysis using a semi-automated sample preparation, amplification, and electrophoresis separation platform.

    Science.gov (United States)

    Raisi, Fariba; Blizard, Benjamin A; Raissi Shabari, Akbar; Ching, Jesus; Kintz, Gregory J; Mitchell, Jim; Lemoff, Asuncion; Taylor, Mike T; Weir, Fred; Western, Linda; Wong, Wendy; Joshi, Rekha; Howland, Pamela; Chauhan, Avinash; Nguyen, Peter; Petersen, Kurt E

    2004-03-01

    The growing importance of analyzing the human genome to detect hereditary and infectious diseases associated with specific DNA sequences has motivated us to develop automated devices to integrate sample preparation, real-time PCR, and microchannel electrophoresis (MCE). In this report, we present results from an optimized compact system capable of processing a raw sample of blood, extracting the DNA, and performing a multiplexed PCR reaction. Finally, an innovative electrophoretic separation was performed on the post-PCR products using a unique MCE system. The sample preparation system extracted and lysed white blood cells (WBC) from whole blood, producing DNA of sufficient quantity and quality for a polymerase chain reaction (PCR). Separation of multiple amplicons was achieved in a microfabricated channel 30 microm x 100 microm in cross section and 85 mm in length filled with a replaceable methyl cellulose matrix operated under denaturing conditions at 50 degrees C. By incorporating fluorescent-labeled primers in the PCR, the amplicons were identified by a two-color (multiplexed) fluorescence detection system. Two base-pair resolution of single-stranded DNA (PCR products) was achieved. We believe that this integrated system provides a unique solution for DNA analysis.

  17. Sample preparation for laser-microdissection of soybean shoot apical meristem

    Directory of Open Access Journals (Sweden)

    Chui E. Wong

    2012-10-01

    Full Text Available The shoot apical meristem houses stem cells responsible for the continuous formation of aerial plant organs including leaves and stems throughout the life of plants. Laser-microdissection in combination with high-throughput technology such as next generation sequencing permits an in-depth analysis of molecular events associated with specific cell type of interest. Sample preparation is the most critical step in ensuring good quality RNA to be extracted from samples following laser-microdissection. Here, we optimized the sample preparation for a major legume crop, soybean. We used Farmer’s solution as a fixative and paraffin as the embedding medium for soybean shoot apical meristem tissue without the use of any specialized equipment. Shorter time for tissue fixation (two days was found to be critical for the preservation of RNA in soybean shoot apical meristem. We further demonstrated the utility of this method for different tissues derived from soybean and rice. The method outlined here shall facilitate studies on crop plants involving laser-microdissection.

  18. Application of a Dual-Arm Robot in Complex Sample Preparation and Measurement Processes.

    Science.gov (United States)

    Fleischer, Heidi; Drews, Robert Ralf; Janson, Jessica; Chinna Patlolla, Bharath Reddy; Chu, Xianghua; Klos, Michael; Thurow, Kerstin

    2016-10-01

    Automation systems with applied robotics have already been established in industrial applications for many years. In the field of life sciences, a comparable high level of automation can be found in the areas of bioscreening and high-throughput screening. Strong deficits still exist in the development of flexible and universal fully automated systems in the field of analytical measurement. Reasons are the heterogeneous processes with complex structures, which include sample preparation and transport, analytical measurements using complex sensor systems, and suitable data analysis and evaluation. Furthermore, the use of nonstandard sample vessels with various shapes and volumes results in an increased complexity. The direct use of existing automation solutions from bioscreening applications is not possible. A flexible automation system for sample preparation, analysis, and data evaluation is presented in this article. It is applied for the determination of cholesterol in biliary endoprosthesis using gas chromatography-mass spectrometry (GC-MS). A dual-arm robot performs both transport and active manipulation tasks to ensure human-like operation. This general robotic concept also enables the use of manual laboratory devices and equipment and is thus suitable in areas with a high standardization grade.

  19. Gel-aided sample preparation (GASP)--a simplified method for gel-assisted proteomic sample generation from protein extracts and intact cells.

    Science.gov (United States)

    Fischer, Roman; Kessler, Benedikt M

    2015-04-01

    We describe a "gel-assisted" proteomic sample preparation method for MS analysis. Solubilized protein extracts or intact cells are copolymerized with acrylamide, facilitating denaturation, reduction, quantitative cysteine alkylation, and matrix formation. Gel-aided sample preparation has been optimized to be highly flexible, scalable, and to allow reproducible sample generation from 50 cells to milligrams of protein extracts. This methodology is fast, sensitive, easy-to-use on a wide range of sample types, and accessible to nonspecialists. © 2014 The Authors. PROTEOMICS published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Error baseline rates of five sample preparation methods used to characterize RNA virus populations

    Science.gov (United States)

    Kugelman, Jeffrey R.; Wiley, Michael R.; Nagle, Elyse R.; Reyes, Daniel; Pfeffer, Brad P.; Kuhn, Jens H.; Sanchez-Lockhart, Mariano; Palacios, Gustavo F.

    2017-01-01

    Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic “no amplification” method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a “targeted” amplification method, sequence-independent single-primer amplification (SISPA) as a “random” amplification method, rolling circle reverse transcription sequencing (CirSeq) as an advanced “no amplification” method, and Illumina TruSeq RNA Access as a “targeted” enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4−5) of all compared methods. PMID:28182717

  1. Simple, Expendable, 3D-Printed Microfluidic Systems for Sample Preparation of Petroleum.

    Science.gov (United States)

    Kataoka, Érica M; Murer, Rui C; Santos, Jandyson M; Carvalho, Rogério M; Eberlin, Marcos N; Augusto, Fabio; Poppi, Ronei J; Gobbi, Angelo L; Hantao, Leandro W

    2017-03-21

    In this study, we introduce a simple protocol to manufacture disposable, 3D-printed microfluidic systems for sample preparation of petroleum. This platform is produced with a consumer-grade 3D-printer, using fused deposition modeling. Successful incorporation of solid-phase extraction (SPE) to microchip was ensured by facile 3D element integration using proposed approach. This 3D-printed μSPE device was applied to challenging matrices in oil and gas industry, such as crude oil and oil-brine emulsions. Case studies investigated important limitations of nonsilicon and nonglass microchips, namely, resistance to nonpolar solvents and conservation of sample integrity. Microfluidic features remained fully functional even after prolonged exposure to nonpolar solvents (20 min). Also, 3D-printed μSPE devices enabled fast emulsion breaking and solvent deasphalting of petroleum, yielding high recovery values (98%) without compromising maltene integrity. Such finding was ascertained by high-resolution molecular analyses using comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry by monitoring important biomarker classes, such as C10 demethylated terpanes, ααα-steranes, and monoaromatic steroids. 3D-Printed chips enabled faster and reliable preparation of maltenes by exhibiting a 10-fold reduction in sample processing time, compared to the reference method. Furthermore, polar (oxygen-, nitrogen-, and sulfur-containing) analytes found in low-concentrations were analyzed by Fourier transform ion cyclotron resonance mass spectrometry. Analysis results demonstrated that accurate characterization may be accomplished for most classes of polar compounds, except for asphaltenes, which exhibited lower recoveries (82%) due to irreversible adsorption to sorbent phase. Therefore, 3D-printing is a compelling alternative to existing microfabrication solutions, as robust devices were easy to prepare and operate.

  2. Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology.

    Science.gov (United States)

    Causon, Tim J; Hann, Stephan

    2016-09-28

    Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid

  3. Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

    Energy Technology Data Exchange (ETDEWEB)

    Jakeman, David L.; Mitchell, Dan J.; Shuttleworth, Wendy A.; Evans, Jeremy N.S. [Washington State University, Department of Biochemistry and Biophysics (United States)

    1998-10-15

    Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of {sup 13}P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 {+-} 12 Hz and 125 {+-} 7 Hz respectively, by a variety of methods involving additives and freezing techniques.

  4. Preconcentration of Zn(II) in water samples using a new hybrid SBA-15-based material

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Quintanilla, Damian; Sanchez, Alfredo; Hierro, Isabel del; Fajardo, Mariano [Departamento de Quimica Inorganica y Analitica, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid (Spain); Sierra, Isabel, E-mail: isabel.sierra@urjc.es [Departamento de Quimica Inorganica y Analitica, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid (Spain)

    2009-07-30

    A SBA-15 mesoporous silica has been chemically modified with 5-mercapto-1-methyltetrazole. The newly synthesized material (MTTZ-SBA-15) has been characterized, by powder X-ray diffraction, N{sub 2} adsorption, FT-IR, {sup 13}C NMR spectroscopy and elemental analysis, and used to preconcentrate Zn(II) in water samples. The effect of some variables on the adsorption capacity has been studied using the column techniques. The adsorption capacity of the prepared material followed the order: Zn >> Cu > Cd >> Mn, and under optimized conditions the maximum adsorption value for Zn(II) was 0.96 {+-} 0.01 mmol/g with the adsorption efficiency of 0.76. In column experiments, adsorption was quantitative for 1000 mL of 7.65 x 10{sup -4} mM of Zn(II) solution and adsorbed ions were eluted out by 5 mL of 1 M HCl (preconcentration factor of 200). Spiked tap water and mineral water were used for the preconcentration and determination of Zn(II) by flame atomic absorption spectrometry (FAAS), and a 102 {+-} 2 and 98 {+-} 3% recoveries were obtained. The LOD and LOQ values of the proposed method were found to be 8.0 x 10{sup -6} and 1.23 x 10{sup -5} mM, respectively. The relative standard deviation for four preconcentration experiments was found to be {<=}4% in all cases.

  5. Preparation and Characterization of a Novel Hybrid Hydrogel Composed of Bombyx mori Fibroin and Poly(N-isopropylacrylamide

    Directory of Open Access Journals (Sweden)

    Ting Wang

    2013-01-01

    Full Text Available A novel hybrid hydrogel was prepared and investigated based on silkworm silk fibroin and poly(N-isopropylacrylamide (PNIPAAm. PNIPAAm was introduced to silk fibroin, the resultant composite hydrogel was examined, and freeze-dried SF/PNIPAAm scaffold was analyzed using LB-550 dynamic light scattering particle-size analyzer, circular dichroism (CD, and scanning electron microscopy (SEM. Our results suggested that the hybrid hydrogels owned the porous sponge-like structures, and the gelation time of SF/PNIPAAm hybrids decreased with an increase in temperature and concentration of each polymer. Results of rheological analysis suggested that the rheological property of resultant SF/PNIPAAm gel depended on the concentration combinations as well as the aging time, which elapsed after mixing the two polymers. Results of CD spectra demonstrated that pH showed little influence on the secondary structure of silk fibroin, and significant changes of , , and G* as surrounding increase temperature above the lower critical solution temperature (LCST.

  6. Preparation and characterization of uniformly sized sub-micrometer spherical silica/organic polymer hybrid particles

    Energy Technology Data Exchange (ETDEWEB)

    Xing, X.-S.; Li, R.K.Y.; Shek, C.-H. [Department of Physics and Materials Science, City University of Hong Kong, Tak Chee Avenue, Kowloon, Hong Kong (China)

    2003-09-01

    Hybrid particles with a core-shell structure, consisting of a silica core and a polyvinyl alcohol (PVA) shell were fabricated via a two-step sol-gel process. The PVA molecular chains are probably physically adsorbed onto the surface of silica cores by hydrogen bonds and van der Waals forces. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  7. Surface morphology of PMMA/boehmite hybrid nanostructures prepared via facile one-pot process

    Science.gov (United States)

    Ghamari, Misagh; Farzi, Gholamali

    2017-08-01

    In this study, we developed the novel aqueous-based PMMA/AlOOH hybrid by a one-pot process starting from their relevant precursors in a controlled manner. Starting chemical reactions directly from precursors and the sequence of adding reactants provide the possibility towards enhancing the homogeneity of the final product. Inorganic and organic segments were made compatible by means of oleic acid as a coupling agent. Boehmite to PMMA weight ratio as the main parameter was varied from 0 to 18% and the morphology, particle size, size distribution, and topography map of hybrids was shown to be composition dependent. Final PMMA/Bo nanohybrids were characterized using FTIR to confirm the chemical interactions between inorganic and organic segments. TEM analysis showed that nanohybrid particles with irregular shapes containing inorganic particles dispersed in the organic matrix are formed with an average diameter which depends on boehmite content. The presence of phase transformation of Bo makes PMMA/Bo hybrids significantly thermally stable. According to AFM topography map analysis and relevant Gaussian fit function, the roughness of nanocomposite, the size of hybrid nanoparticles and deviation from the mean value (size) were increased as Bo increases from 0 to 18.

  8. Sample preparation and separation techniques for bioanalysis of morphine and related substances.

    Science.gov (United States)

    Hansen, Steen Honoré

    2009-03-01

    In present time the use or misuse of morphine and its derivatives are monitored by assaying the presence of the drug and its metabolites in biofluids. In the present review, focus is placed on the sample preparation and on the separation techniques used in the current best practices of bioanalysis of morphine and its major metabolites. However, as methods for testing the misuse of heroin, a morphine derivative, often involve bioanalytical methods that cover a number of other illicit drug substances, such methods are also included in the review. Furthermore, the review also includes bioanalysis in a broader perspective as analysis of plant materials, cell cultures and environmental samples. The review is not intended to cover all publications that include bioanalysis of morphine but is more to be considered a view into the current best practices of bioanalysis of morphine, its metabolites and other related substances.

  9. Capacitive deionization on-chip as a method for microfluidic sample preparation.

    Science.gov (United States)

    Roelofs, Susan H; Kim, Bumjoo; Eijkel, Jan C T; Han, Jongyoon; van den Berg, Albert; Odijk, Mathieu

    2015-03-21

    Desalination as a sample preparation step is essential for noise reduction and reproducibility of mass spectrometry measurements. A specific example is the analysis of proteins for medical research and clinical applications. Salts and buffers that are present in samples need to be removed before analysis to improve the signal-to-noise ratio. Capacitive deionization is an electrostatic desalination (CDI) technique which uses two porous electrodes facing each other to remove ions from a solution. Upon the application of a potential of 0.5 V ions migrate to the electrodes and are stored in the electrical double layer. In this article we demonstrate CDI on a chip, and desalinate a solution by the removal of 23% of Na(+) and Cl(-) ions, while the concentration of a larger molecule (FITC-dextran) remains unchanged. For the first time impedance spectroscopy is introduced to monitor the salt concentration in situ in real-time in between the two desalination electrodes.

  10. Hybrid monolith sorbent of polypyrrole-coated graphene oxide incorporated into a polyvinyl alcohol cryogel for extraction and enrichment of sulfonamides from water samples.

    Science.gov (United States)

    Chullasat, Kochaporn; Nurerk, Piyaluk; Kanatharana, Proespichaya; Kueseng, Pamornrat; Sukchuay, Thanyaporn; Bunkoed, Opas

    2017-04-08

    A hybrid monolith sorbent of polypyrrole-coated graphene oxide embedded in polyvinyl alcohol cryogel was prepared and used as an effective solid phase extraction sorbent for the determination of trace sulfonamides. The large surface areas with many adsorption sites of polypyrrole and graphene oxide facilitated the high adsorption of sulfonamides via hydrogen bonding, π-π and hydrophobic interactions. The high porosity of the polyvinyl alcohol cryogel helped to reduce the back pressure that occurs in a conventional packed solid phase extraction cartridge. The effecting parameters on the extraction efficiency including the type of sorbent, the polymerization time, desorption conditions, the sample pH, the sample volume, the sample flow rate, and ionic strength were investigated and optimized. Under the optimum conditions, the developed method provided a wide linear range from 0.20 to 100.0 μg L(-1) for sulfadiazine, sulfathiazole and sulfamerazine; and from 0.10 to 100 μg L(-1) for sulfamethazine, sulfamonomethoxine and sulfadimethoxine. The limits of detection were 0.20 μg L(-1) for sulfadiazine, sulfathiazole and sulfamerazine; and 0.10 μg L(-1) for sulfamethazine, sulfamonomethoxine and sulfadimethoxine. The developed hybrid monolith polypyrrole-coated graphene oxide embedded in the polyvinyl alcohol cryogel sorbent provided good recoveries in the range of 85.5-99.0% with RSDs of less than 5.0%. The sorbent offered a good reproducibility, was robust and can be reused at least 10 times. It was successfully applied for the extraction and enrichment of sulfonamides from normal and supplemented water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

    Science.gov (United States)

    Yokochi, Reika

    2016-09-01

    Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

  12. Luminescent Eosin Y–SiO{sub 2} hybrid nano and microrods prepared by sol–gel template method

    Energy Technology Data Exchange (ETDEWEB)

    Secu, M., E-mail: msecu@infim.ro [National Institute for Materials Physics, P.O. Box MG-7, Bucharest–Magurele, 077125 (Romania); Secu, C.E.; Sima, M.; Negrea, R.F.; Bartha, C. [National Institute for Materials Physics, P.O. Box MG-7, Bucharest–Magurele, 077125 (Romania); Dinescu, M.; Damian, V. [National Institute for Laser, Plasma and Radiation, P.O. Box MG-36, Bucharest–Magurele 077125 (Romania)

    2013-11-15

    Sol–gel chemistry within the pores of a polycarbonate template membrane was used for the preparation of Eosin Y–SiO{sub 2} hybrid nano- and microrods, using tetraethylorthosilicate [TEOS, Si(OC{sub 2}H{sub 5}){sub 4}] as the precursor in the presence of trifluoroacetic acid (TFA) catalyst. The ethanolic solution of Eosin-Y was added to the silica sol to trap dye molecules inside the SiO{sub 2} gel network during the gelation. Structural and morphological characterization using scanning electron microscopy (SEM) and luminescence microscopy have shown the formation of rods with 200 nm and 1.2 μm diameter and about 30 μm length, exhibiting luminescence properties. Spectroscopic characterization has shown that the luminescence is due to Eosin-Y molecule in the xerogel porous network, surrounded by a solvation shell given mainly by the water. -- Highlights: • Sol–gel template method was used to prepare Eosin Y–SiO{sub 2} hybrid rods-type structures. • Morphological characterization has shown nano- and microrods with luminescent properties. • Luminescence is due to Eosin-Y molecule surrounded by a solvation shell given by water.

  13. Electroless Sliver-Plating Process in the Preparation of 103Pd-125I Hybrid Brachytherapy Seed Cores

    Directory of Open Access Journals (Sweden)

    LI Zhong-yong1,2;CHEN Bin-da1;Lv Xiao-zhou1;LU Jin-hui1;CUI Hai-ping1,2

    2014-02-01

    Full Text Available Electroless 103Pd plating and electroless Ag plating and chemical 125I depositing were took place on the surface of carbon rods in turn, which was a reliable method for the preparation of 103Pd-125I hybrid brachytherapy seed cores. 103Pd and 125I were deposited on the same substrate effectively through silver coating as a bridge. The process of electroless Ag plating was a novel and important step in the preparation of 103Pd-125I hybrid seed. In this work, the process of electroless Ag plating was studied using 0.5×3.0 mm carbon rods with palladium coating as substrate, silver-ammino complex as precursor, 110mAg as radioactive tracer, and hydrazine as reductant. The optimum conditions were AgNO3 2g/L,Na2EDTA 40 g/L,NH3•H2O 16.25%,H4N2•H2O 5‰,pH=10,t=60 min,and T=35 ℃. Sliver deposited on each carbon rod was uniform, and sliver-coating was white and smooth.

  14. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices.

    Science.gov (United States)

    Naccarato, Attilio; Pawliszyn, Janusz

    2016-09-01

    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future.

  15. Performance Evaluation of Fast Microfluidic Thermal Lysis of Bacteria for Diagnostic Sample Preparation

    Directory of Open Access Journals (Sweden)

    Evangelyn C. Alocilja

    2013-01-01

    Full Text Available Development of new diagnostic platforms that incorporate lab-on-a-chip technologies for portable assays is driving the need for rapid, simple, low cost methods to prepare samples for downstream processing or detection. An important component of the sample preparation process is cell lysis. In this work, a simple microfluidic thermal lysis device is used to quickly release intracellular nucleic acids and proteins without the need for additional reagents or beads used in traditional chemical or mechanical methods (e.g., chaotropic salts or bead beating. On-chip lysis is demonstrated in a multi-turn serpentine microchannel with external temperature control via an attached resistive heater. Lysis was confirmed for Escherichia coli by fluorescent viability assay, release of ATP measured with bioluminescent assay, release of DNA measured by fluorometry and qPCR, as well as bacterial culture. Results comparable to standard lysis techniques were achievable at temperatures greater than 65 °C and heating durations between 1 and 60 s.

  16. Semiautomated Sample Preparation for Protein Stability and Formulation Screening via Buffer Exchange.

    Science.gov (United States)

    Ying, William; Levons, Jaquan K; Carney, Andrea; Gandhi, Rajesh; Vydra, Vicky; Rubin, A Erik

    2016-06-01

    A novel semiautomated buffer exchange process workflow was developed to enable efficient early protein formulation screening. An antibody fragment protein, BMSdab, was used to demonstrate the workflow. The process afforded 60% to 80% cycle time and scientist time savings and significant material efficiencies. These efficiencies ultimately facilitated execution of this stability work earlier in the drug development process, allowing this tool to inform the developability of potential candidates for development from a formulation perspective. To overcome the key technical challenges, the protein solution was buffer-exchanged by centrifuge filtration into formulations for stability screening in a 96-well plate with an ultrafiltration membrane, leveraging automated liquid handling and acoustic volume measurements to allow several cycles of exchanges. The formulations were transferred into a vacuum manifold and sterile filtered into a rack holding 96 glass vials. The vials were sealed with a capmat of individual caps and placed in stability stations. Stability of the samples prepared by this process and by the standard process was demonstrated to be comparable. This process enabled screening a number of formulations of a protein at an early pharmaceutical development stage with a short sample preparation time.

  17. Transformation from Ag@Ag3PO4 to Ag@Ag2SO4 hybrid at room temperature: preparation and its visible light photocatalytic activity

    Science.gov (United States)

    Wei, Ting; Gao, Shanmin; Wang, Qingyao; Xu, Hui; Wang, Zeyan; Huang, Baibiao; Dai, Ying

    2017-02-01

    In the present study, Ag/Ag2SO4 hybrid photocatalysts were obtained via a facile redox-precipitation reaction approach by using Ag@Ag3PO4 nanocomposite as the precursor and KMnO4 as the oxidant. Multiple techniques, such as X-ray diffraction pattern (XRD), transmission electron microscope (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS) and Brunauer-Emmett-Teller (BET), photocurrent and electrochemical impedance spectroscopy (EIS), were applied to investigate the structures, morphologies, optical, and electronic properties of as-prepared samples. The photocatalytic activities were evaluated by photodegradation of organic rhodamine B (RhB) and methyl orange (MO) under visible light irradiation. It was found that pure Ag2SO4 can partially transform into metallic Ag during the photocatalytic degradation of organic pollutants, but the Ag/Ag2SO4 hybrids can maintain its structure stability and show enhanced visible light photocatalytic activity because of the surface plasma resonance effect of the metallic Ag.

  18. Diagnosis of visceral Leishmaniasis in asymptomatic dogs by the KDNA PCR-hybridization assay using noninvasive samples

    Energy Technology Data Exchange (ETDEWEB)

    Leite, Rodrigo Souza; Andrade, Antero Silva Ribeiro de [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Lab. de Radiobiologia], e-mail: rleite2005@gmail.com; Ferreira, Sydney de Almeida; Ituassu, Leonardo Trindade; Melo, Maria Norma de [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Centro de Ciencias Biologicas. Dept. de Parasitologia], e-mail: saninoalmeida@gmail.com

    2009-07-01

    The visceral leishmaniasis (VL) in Brazil is caused by Leishmania (Leishmania) chagasi and the asymptomatic dogs may transmit the parasite to sand flies vectors. The VL epidemiological control in Brazil involves the elimination of seropositive dogs, insecticide treatment and systematic treatment of human cases. Therefore, the accurate diagnosis is important in order to avoid the disease transmission or unnecessary culling of dogs. Serological tests are used for screening of dogs. However, these techniques present limitations. The Polymerase Chain Reaction (PCR) is an attractive alternative to the diagnosis in this context; but non-invasive samplings have great importance because they are simpler, painless and less resisted by dog-owners. This study aimed at evaluating conjunctival swab (CS) for canine VL diagnosis. In this methodology a sterile cotton swab is used to sampling the dog conjunctiva in both eyes. Thirty asymptomatic seropositive dogs were used. The samples were analyzed by the kDNA PCR-hybridization procedure in which the PCR products are hybridized with cloned kDNA mini-circles labeled with {sup 32}P[]dCTP. In addition, blood (B) was collected from each animal. L. chagasi was identified in 90% of CS samples and 13,6% of B samples. The high sensitivity obtained with asymptomatic dogs, in which the diagnosis is more difficult due the low number of parasites in the samples, allow concluding that the conjunctival swab associated to the kDNA PCR-hybridization assay provides a valuable alternative tool for the direct diagnosis of canine leishmaniasis. (author)

  19. Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

    CERN Document Server

    Crotti, C; Celestino, T; Fontana, S

    2003-01-01

    The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

  20. Evaluation of sample preparation methods and optimization of nickel determination in vegetable tissues

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar

    2011-02-01

    Full Text Available Nickel, although essential to plants, may be toxic to plants and animals. It is mainly assimilated by food ingestion. However, information about the average levels of elements (including Ni in edible vegetables from different regions is still scarce in Brazil. The objectives of this study were to: (a evaluate and optimize a method for preparation of vegetable tissue samples for Ni determination; (b optimize the analytical procedures for determination by Flame Atomic Absorption Spectrometry (FAAS and by Electrothermal Atomic Absorption (ETAAS in vegetable samples and (c determine the Ni concentration in vegetables consumed in the cities of Lorena and Taubaté in the Vale do Paraíba, State of São Paulo, Brazil. By means of the analytical technique for determination by ETAAS or FAAS, the results were validated by the test of analyte addition and recovery. The most viable method tested for quantification of this element was HClO4-HNO3 wet digestion. All samples but carrot tissue collected in Lorena contained Ni levels above the permitted by the Brazilian Ministry of Health. The most disturbing results, requiring more detailed studies, were the Ni concentrations measured in carrot samples from Taubaté, where levels were five times higher than permitted by Brazilian regulations.

  1. Preparation of Magnetic Hollow Molecularly Imprinted Polymers for Detection of Triazines in Food Samples.

    Science.gov (United States)

    Wang, Aixiang; Lu, Hongzhi; Xu, Shoufang

    2016-06-22

    Novel magnetic hollow molecularly imprinted polymers (M-H-MIPs) were proposed for highly selective recognition and fast enrichment of triazines in food samples. M-H-MIPs were prepared on the basis of multi-step swelling polymerization, followed by in situ growth of magnetic Fe3O4 nanoparticles on the surface of hollow molecularly imprinted polymers (H-MIPs). Transmission electron microscopy and scanning electron microscopy confirmed the successful immobilization of Fe3O4 nanoparticles on the surface of H-MIPs. M-H-MIPs could be separated simply using an external magnet. The binding adsorption results indicated that M-H-MIPs displayed high binding capacity and fast mass transfer property and class selective property for triazines. Langmuir isotherm and pseudo-second-order kinetic models fitted the best adsorption models for M-H-MIPs. M-H-MIPs were used to analyze atrazine, simazine, propazine, and terbuthylazine in corn, wheat, and soybean samples. Satisfactory recoveries were in the range of 80.62-101.69%, and relative standard deviation was lower than 5.2%. Limits of detection from 0.16 to 0.39 μg L(-1) were obtained. When the method was applied to test positive samples that were contaminated with triazines, the results agree well with those obtained from an accredited method. Thus, the M-H-MIP-based dispersive solid-phase extraction method proved to be a convenient and practical platform for detection of triazines in food samples.

  2. Optimized sample preparation of endoscopic collected pancreatic fluid for SDS-PAGE analysis.

    Science.gov (United States)

    Paulo, Joao A; Lee, Linda S; Wu, Bechien; Repas, Kathryn; Banks, Peter A; Conwell, Darwin L; Steen, Hanno

    2010-07-01

    The standardization of methods for human body fluid protein isolation is a critical initial step for proteomic analyses aimed to discover clinically relevant biomarkers. Several caveats have hindered pancreatic fluid proteomics, including the heterogeneity of samples and protein degradation. We aim to optimize sample handling of pancreatic fluid that has been collected using a safe and effective endoscopic collection method (endoscopic pancreatic function test). Using SDS-PAGE protein profiling, we investigate (i) precipitation techniques to maximize protein extraction, (ii) auto-digestion of pancreatic fluid following prolonged exposure to a range of temperatures, (iii) effects of multiple freeze-thaw cycles on protein stability, and (iv) the utility of protease inhibitors. Our experiments revealed that TCA precipitation resulted in the most efficient extraction of protein from pancreatic fluid of the eight methods we investigated. In addition, our data reveal that although auto-digestion of proteins is prevalent at 23 and 37 degrees C, incubation on ice significantly slows such degradation. Similarly, when the sample is maintained on ice, proteolysis is minimal during multiple freeze-thaw cycles. We have also determined the addition of protease inhibitors to be assay-dependent. Our optimized sample preparation strategy can be applied to future proteomic analyses of pancreatic fluid.

  3. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Corina Mahu Ştefania

    2015-12-01

    Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

  4. Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Taflik, Ticiane; Antes, Fabiane G.; Paniz, Jose N.G.; Flores, Erico M.M.; Dressler, Valderi L., E-mail: valdres@quimica.ufsm.br [Departamento de Quimica, Universidade Federal de Santa Maria, RS (Brazil); Duarte, Fabio A. [Escola de Quimica e Alimentos, Universidade Federal do Rio Grande, Rio Grande, RS (Brazil); Flores, Eder L.M. [Coordenacao de Engenharia de Alimentos, Universidade Tecnologica Federal do Parana, Medianeira, PR (Brazil)

    2012-03-15

    Pyrohydrolysis was employed for mineral supplements decomposition prior to F, Br and I determination. Fluoride determination was carried out by potentiometry using a fluoride-ion selective electrode, whereas Br and I were determined by inductively coupled plasma mass spectrometry. The main parameters that influence on pyrohydrolysis were investigated. After evaluation, the following conditions were established: reactor temperature of 1000 deg C during 10 min; sample plus accelerator mass ratio of 1 + 5 and carrier gas (air) flow rate of 200 mL min{sup -1} . The accuracy of the proposed method was evaluated by analyte recovery tests and analysis of certified reference materials of phosphate rock and soil. Commercial mineral supplement samples were analyzed. The limits of quantification were 16, 0.3 and 0.07 {mu}g g{sup -1} for F, Br and I, respectively. By using a relatively simple and low cost pyrohydrolysis system up to 5 samples can be processed per hour. The developed sample preparation procedure can be routinely employed for F, Br and I determination in mineral supplements. (author)

  5. Preparative divergent flow IEF without carrier ampholytes for separation of complex biological samples.

    Science.gov (United States)

    Stastna, Miroslava; Slais, Karel

    2010-01-01

    Efficient separation method is a crucial part of the process in which components of highly complex biological sample are identified and characterized. Based on the principles of recently newly established electrophoretic method called divergent flow IEF (DF IEF), we have tested the DF IEF instrument which is able to operate without the use of background carrier ampholytes. We have verified that during separation and focusing of sample consisting of high numbers of proteins (yeast lysate and wheat flour extract), the pH gradient of preparative DF IEF can be created by autofocusing of the sample components themselves without any addition of carrier ampholytes. In DF IEF, the proteins are separated, desalted and concentrated in one step. The fractions of yeast lysate sample, collected at the DF IEF output and subjected to gel IEF, contained the zones of proteins gradually covering the pI values from 3.7 to 8.5. In our experimental arrangement, the highest number of proteins has been found in fractions with pI values around 5.3 as detected by polyacrylamide gel IEF with CBB staining. During DF IEF, the selected protein bands have been concentrated up to 16.8-fold.

  6. Sample preparation for scanning electron microscopy of plant surfaces--horses for courses.

    Science.gov (United States)

    Pathan, A K; Bond, J; Gaskin, R E

    2008-12-01

    Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniques on different leaf types are discussed. Comparative examples are depicted from our lab using similar techniques; the pros and cons for specific techniques are discussed. New promising techniques and microscopes, which can alleviate some of the problems encountered in conventional methods of leaf sample processing and visualisation, are also discussed. It is concluded that the choice of technique for a specific leaf sample is dictated by the surface features that need to be preserved (such as trichomes, epidermal cells or wax microstructure), the resolution to be achieved, availability of the appropriate processing equipment and the technical capabilities of the available electron microscope.

  7. RNA SAMPLE PREPARATION APPLIED TO GENE EXPRESSION PROFILING FOR THE HORSE BIOLOGICAL PASSPORT.

    Science.gov (United States)

    Bailly-Chouriberry, Ludovic; Baudoin, Florent; Cormant, Florence; Glavieux, Yohan; Loup, Benoit; Garcia, Patrice; Popot, Marie-Agnès; Bonnaire, Yves

    2017-04-05

    The improvement of doping control is an on-going race. Techniques to fight against doping are usually based on the direct detection of drugs or their metabolites by analytical methods such as chromatography hyphenated to mass spectrometry after ad hoc sample preparation. Nowadays, omic methods constitute an attractive development and advances have been achieved particularly by application of molecular biology tools for detection of anabolic androgenic steroids (AAS), erythropoiesis-stimulating agent (ESA) or to control human growth hormone misuses. These interesting results across different animal species have suggested that modification of gene expression offers promising new methods of improving the window of detection of banned substances by targeting their effects on blood cell gene expression. In this context, the present study describes the possibility of using a modified version of the dedicated Human IVD (in vitro Diagnostics) PAXgene® Blood RNA Kit for horse gene expression analysis in blood collected on PAXgene® tubes applied to the Horse Biological Passport. The commercial kit was only approved for human blood samples and has required an optimization of specific technical requirements for equine blood samples. Improvements and recommendations were achieved for sample collection, storage and RNA extraction procedure. Following these developments, RNA yield and quality were demonstrated to be suitable for downstream gene expression analysis by qPCR techniques.

  8. Preparation and analysis of dust samples for medical examinations; Praeparation und Analytik der Staubproben fuer medizinische Untersuchungen

    Energy Technology Data Exchange (ETDEWEB)

    Armbruster, L. [Deutsche Montan Technologie GmbH, Essen (Germany). Gas and Fire Div.

    2004-07-01

    For medical research within this project three respirable dust samples have been prepared and analysed. The original bulk material came from three different stratigraphic horizons, for the preparation a multiplex classifier was used. The respirable samples showed the same size distribution as the samples used in former projects. The quartz content was rather low, but within the normal variability. Pure quartz particles without surface contamination are not present in the three samples. Nickel, lead, cobalt, and arsenic are the most significant trace elements in the samples. (orig.)

  9. Preparing and measuring ultra-small radiocarbon samples with the ARTEMIS AMS facility in Saclay, France

    Energy Technology Data Exchange (ETDEWEB)

    Delque-Kolic, E., E-mail: emmanuelle.delque-kolic@cea.fr [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France); Comby-Zerbino, C.; Ferkane, S.; Moreau, C.; Dumoulin, J.P.; Caffy, I.; Souprayen, C.; Quiles, A.; Bavay, D.; Hain, S.; Setti, V. [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France)

    2013-01-15

    The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18 ml for the first line and 12 ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10 {mu}g of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5 mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring {sup 14}C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1 {+-} 0.8 and 0.2 {+-} 0.1 {mu}g, respectively. The results presented here were obtained for IAEA-C1, {sup 14}C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

  10. Automation of sample preparation for mass cytometry barcoding in support of clinical research: protocol optimization.

    Science.gov (United States)

    Nassar, Ala F; Wisnewski, Adam V; Raddassi, Khadir

    2017-03-01

    Analysis of multiplexed assays is highly important for clinical diagnostics and other analytical applications. Mass cytometry enables multi-dimensional, single-cell analysis of cell type and state. In mass cytometry, the rare earth metals used as reporters on antibodies allow determination of marker expression in individual cells. Barcode-based bioassays for CyTOF are able to encode and decode for different experimental conditions or samples within the same experiment, facilitating progress in producing straightforward and consistent results. Herein, an integrated protocol for automated sample preparation for barcoding used in conjunction with mass cytometry for clinical bioanalysis samples is described; we offer results of our work with barcoding protocol optimization. In addition, we present some points to be considered in order to minimize the variability of quantitative mass cytometry measurements. For example, we discuss the importance of having multiple populations during titration of the antibodies and effect of storage and shipping of labelled samples on the stability of staining for purposes of CyTOF analysis. Data quality is not affected when labelled samples are stored either frozen or at 4 °C and used within 10 days; we observed that cell loss is greater if cells are washed with deionized water prior to shipment or are shipped in lower concentration. Once the labelled samples for CyTOF are suspended in deionized water, the analysis should be performed expeditiously, preferably within the first hour. Damage can be minimized if the cells are resuspended in phosphate-buffered saline (PBS) rather than deionized water while waiting for data acquisition.

  11. Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

    Energy Technology Data Exchange (ETDEWEB)

    Pietrzyńska, Monika, E-mail: monikapietrzynska@gmail.com; Voelkel, Adam; Bielicka-Daszkiewicz, Katarzyna

    2013-05-07

    Graphical abstract: -- Highlights: •MINE device for isolation of analytes from water samples. •Nine polymer poly(styrene-divinylbenzene) monoliths prepared in stainless steel needles. •High efficiency of in-needle extraction systems based on monolithic materials. •New possibilities in sample preparation area. -- Abstract: Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg.

  12. High-Throughput Serum 25-Hydroxy Vitamin D Testing with Automated Sample Preparation.

    Science.gov (United States)

    Stone, Judy

    2016-01-01

    Serum from bar-coded tubes, and then internal standard, are pipetted to 96-well plates with an 8-channel automated liquid handler (ALH). The first precipitation reagent (methanol:ZnSO4) is added and mixed with the 8-channel ALH. A second protein precipitating agent, 1 % formic acid in acetonitrile, is added and mixed with a 96-channel ALH. After a 4-min delay for larger precipitates to settle to the bottom of the plate, the upper 36 % of the precipitate/supernatant mix is transferred with the 96-channel ALH to a Sigma Hybrid SPE(®) plate and vacuumed through for removal of phospholipids and precipitated proteins. The filtrate is collected in a second 96-well plate (collection plate) which is foil-sealed, placed in the autosampler (ALS), and injected into a multiplexed LC-MS/MS system running AB Sciex Cliquid(®) and MPX(®) software. Two Shimadzu LC stacks, with multiplex timing controlled by MPX(®) software, inject alternately to one AB Sciex API-5000 MS/MS using positive atmospheric pressure chemical ionization (APCI) and a 1.87 min water/acetonitrile LC gradient with a 2.1 × 20 mm, 2.7 μm, C18 fused core particle column (Sigma Ascentis Express). LC-MS/MS through put is ~44 samples/h/LC-MS/MS system with dual-LC channel multiplexing. Plate maps are transferred electronically from the ALH and reformatted into LC-MS/MS sample table format using the Data Innovations LLC (DI) Instrument Manager middleware application. Before collection plates are loaded into the ALS, the plate bar code is manually scanned to download the sample table from the DI middleware to the LC-MS/MS. After acquisition-LC-MS/MS data is analyzed with AB Sciex Multiquant(®) software using customized queries, and then results are transferred electronically via a DI interface to the LIS. 2500 samples/day can be extracted by two analysts using four ALHs in 4-6 h. LC-MS/MS analysis of those samples on three dual-channel LC multiplexed LC-MS/MS systems requires 19-21 h and data analysis can be

  13. In-situ polymerized nanosilica/acrylic/epoxy hybrid coating:Preparation,microstructure and properties

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    An in-situ polymerization method was employed to synthesize the nanosilica/acrylic/epoxy (SAE) hybrid coating on AISI 430 stainless steel (430SS), as compared with a traditional blending method. Mi- crostructures of the blending SAE hybrid coating (BC) and in-situ SAE hybrid coating (ISC) were characterized by transmission electron microscopy (TEM). Corrosion resistance of BC and ISC on 430SS was evaluated by the neutral salt spray test and potentiodynamic polarization technique. Failure mechanism of the BC on 430SS was suggested by the microstructures and corrosion behaviors. Serious aggregation of nanosilica particles in the BC impairs its structural uniformity and induces the flaws formation. These flaws in the BC initiates the failures of pitting, filiform corrosion and peeling which are accelerated by the O2 concentration cell and H+ self-catalysis in chlorine-containing moist environments. The ISC-coated 430SS shows a more advantageous corrosion resistance than that of the BC-coated. The ISC-coated 430SS can suffer the salt spray over 1000 h. Besides, it exhibits a high corrosion potential beyond 0.925 V and good passivation characteristics during the potentiodynamic polarization.

  14. Preparation and characterization of SMA/S-POSS hybrid membranes for direct methanol fuel cell applications

    Institute of Scientific and Technical Information of China (English)

    WANG Erdong; SHI Pengfei; CHANG Young-wook

    2006-01-01

    A novel sulfonated polyhedral oligomeric silsesquioxane(S-POSS) monomer was synthesized successfully in this article. S-POSS acted as a donor of sulfonic acid group and reacted with poly(styrene-co-maleic anhydride) (SMA). FT-IR spectroscopy confirmed the modification through introduction of peaks characteristic of ester linkages and carboxylic groups. The SMA/S-POSS hybrid membranes were fabricated from different S-POSS contents. The proton conductivity and methanol permeability of the hybrid membranes were studied with changing S-POSS content from 5wt.% to 30wt.%. It was found that the proton conductivity and the methanol permeability were dependent on the S-POSS content. Both of proton conductivity and methanol permeability properties improve with increasing S-POSS content. The proton conductivities of the hybrid membranes are in the range of 10-3-10-2 S·cm-1,and the range of methanol permeabilities was between 10-8 and 10-7 cm2·s-1. The membranes show good thermal properties characterized by thermogravimetric analysis (TGA).

  15. ORGANIC-INORGANIC HYBRIDS PREPARED FROM ALKYL PHOSPHONIUM SALTS INTERCALATED MONTMORILLONITES

    Directory of Open Access Journals (Sweden)

    SAHELI GANGULY

    2012-12-01

    Full Text Available Present investigation is focused on systematic and detailed characterization of alkyl phosphonium intercalated montmorillonite (MMT. The objective of the work is to provide a better understanding of the specific changes in properties of the hybrid material with changes in structure of incoming organic cations. In the present work, Na-MMT was intercalated with phosphonium salts of two different cationic head compositions namely alkyl triphenyl and alkyl tributyl groups. Length of alkyl chain was also varied. Resultant organic-inorganic hybrids were characterized by X-ray diffraction (XRD, Transmission electron microscopy (TEM, Thermogravimetry (TG and Fourier transformed infrared spectroscopy (FTIR. Effective volume occupied by the cationic heads influenced interlayer arrangements. Intercalated MMT with two different cationic heads behaved differently in relation to thermal decomposition patterns. Possible explanation was given based on hybridization of bonds. Van der Waals attachment of alkyl chains influenced the interlayer stacking and organic loading. Attempts were made to correlate the changes in properties of intercalated MMT with the structural aspects of incoming organic cations.

  16. Performance of hybrid programming models for multiscale cardiac simulations: preparing for petascale computation.

    Science.gov (United States)

    Pope, Bernard J; Fitch, Blake G; Pitman, Michael C; Rice, John J; Reumann, Matthias

    2011-10-01

    Future multiscale and multiphysics models that support research into human disease, translational medical science, and treatment can utilize the power of high-performance computing (HPC) systems. We anticipate that computationally efficient multiscale models will require the use of sophisticated hybrid programming models, mixing distributed message-passing processes [e.g., the message-passing interface (MPI)] with multithreading (e.g., OpenMP, Pthreads). The objective of this study is to compare the performance of such hybrid programming models when applied to the simulation of a realistic physiological multiscale model of the heart. Our results show that the hybrid models perform favorably when compared to an implementation using only the MPI and, furthermore, that OpenMP in combination with the MPI provides a satisfactory compromise between performance and code complexity. Having the ability to use threads within MPI processes enables the sophisticated use of all processor cores for both computation and communication phases. Considering that HPC systems in 2012 will have two orders of magnitude more cores than what was used in this study, we believe that faster than real-time multiscale cardiac simulations can be achieved on these systems.

  17. Hybrid aerogel preparations as drug delivery matrices for low water-solubility drugs.

    Science.gov (United States)

    Veres, Peter; López-Periago, Ana M; Lázár, István; Saurina, Javier; Domingo, Concepción

    2015-12-30

    A comprehensive study of 14 hybrid aerogels of different composition with applications in drug delivery has been carried out. The overall objective was to modulate the release behavior of drug-impregnated aerogels, from an almost instantaneous release to a semi-retarded delivery prolonged during several hours, through internal surface functionalization. The designed hybrid aerogels were composed of silica and gelatin and functionalized with either phenyl, long (16) hydrocarbon chain or methyl moiety. As model systems, three class II active agents (pKaaerogels. The work relied on the use of supercritical fluid technology for both the synthesis and functionalization of the hybrid aerogels, as well as for the impregnation with an active agent using supercritical CO2 as a solvent. For the impregnated aerogels, in vitro release profiles were recorded under gastric and intestinal pH-conditions using HPLC techniques. The release behavior observed for the three studied drugs was explained considering the measured dissolution profiles of the crystalline drugs, the aerogel composition and its functionalization. Such features are considered of great interest to tailor the bioavailability of drugs with low water solubility.

  18. Preparation and evaluation of a novel hybrid monolithic column based on pentafluorobenzyl imidazolium bromide ionic liquid.

    Science.gov (United States)

    Shan, Yuanhong; Qiao, Lizhen; Shi, Xianzhe; Xu, Guowang

    2015-01-02

    To develop a novel hybrid monolithic column based on pentafluorobenzyl imidazolium bromide ionic liquid, a new ionic liquid monomer was synthesized from 1-vinylimidazole and pentafluorobenzyl bromide. By employing a facile one-step copolymerization of polyhedral-oligomeric-silsesquioxane-type (POSS) cross-linking agent and the home-made ionic liquid monomer, the hybrid monolithic columns were in situ fabricated in fused-silica capillary. The morphology of monolithic column was characterized by scanning electron microscope (SEM) and the chemical composition was confirmed by Fourier-transform infrared spectroscopy (FT-IR) and elemental analysis. Excellent mechanical stability and slight swelling propensity were exhibited which was ascribed to the rigid hybrid monolithic skeleton. Reproducibility results of run-to-run, column-to-column, batch-to-batch and day-to-day were investigated and the RSDs were less than 0.46%, 1.84%, 3.96% and 3.17%, respectively. The mixed-mode retention mechanism with hydrophobic interaction, π-π stacking, ion-exchange, electrostatic interaction and dipole-dipole interaction was explored systematically using analytes with different structure types. Satisfied separation capability and column efficiency were achieved for the analysis of small molecular compounds such as alkylbenzenes, polycyclic aromatic hydrocarbons, nucleosides and halogenated compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Preparation of patterned graphene-ZnO hybrid nanoflower and nanorods on ITO surface

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Sin Tee; Umar, Marjoni Imamora Ali; Ginting, Riski Titian; Yahaya, Muhammad; Yap, Chi Chin [School of Applied Physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Umar, Akrajas Ali; Salleh, Muhamad Mat; Majlis, Burhanuddin Yeop; Naumar, Fitri Yenni [Institute of Microengineering and Nanoelectronics (IMEN), Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia)

    2013-11-27

    Hybrid ZnO nanostructure with controlled morphology have been proved to enhance the physical and chemical properties of the material and used as photodiode and sensor. In this paper, hybrid graphene-ZnO nanoflower and nanorods have been successfully synthesized via a seed mediated method with micropatterned ZnO nanoseed treated with multilayer graphene (MLG) in a hydrothermal process. In typical process, the ZnO nanoseeds with and without resists were spin coated with a multilayer graphene prior to the growth process. The treated seed was then used to grow the ZnO nanostructures in the growth solution that contained equimolar (0.04 M) of zinc nitrate hexahydrate and hexamethylenetetramine. The growth process was carried out inside an autoclave at temperature 70 °C. The growth time was 4 h. It was proved that the MLG treatment on micropatterning substrate may induce new morphology formation of ZnO nanostructure. It is expected that the heteroepitaxy reaction occurred between the MLG and ZnO interface. This presence method can be used as an alternative approach to control the morphology of hybrid ZnO nanostructure growth.

  20. Spectrum of Cytogenomic Abnormalities Revealed by Array Comparative Genomic Hybridization on Products of Conception Culture Failure and Normal Karyotype Samples.

    Science.gov (United States)

    Zhou, Qinghua; Wu, Shen-Yin; Amato, Katherine; DiAdamo, Autumn; Li, Peining

    2016-03-20

    Approximately 30% of pregnancies after implantation end up in spontaneous abortions, and 50% of them are caused by chromosomal abnormalities. However, the spectrum of genomic copy number variants (CNVs) in products of conception (POC) and the underlying gene-dosage-sensitive mechanisms causing spontaneous abortions remain largely unknown. In this study, array comparative genomic hybridization (aCGH) analysis was performed as a salvage procedure for 128 POC culture failure (POC-CF) samples and as a supplemental procedure for 106 POC normal karyotype (POC-NK) samples. Chromosomal abnormalities were detected in 10% of POC-CF and pathogenic CNVs were detected in 3.9% of POC-CF and 5.7% of POC-NK samples. Compiled results from this study and relevant case series through a literature review demonstrated an abnormality detection rate (ADR) of 35% for chromosomal abnormalities in POC-CF samples, 3.7% for pathogenic CNVs in POC-CF samples, and 4.6% for pathogenic CNVs in POC-NK samples. Ingenuity Pathway Analysis (IPA) was performed on the genes from pathogenic CNVs found in POC samples. The denoted primary gene networks suggested that apoptosis and cell proliferation pathways are involved in miscarriage. In summary, a similar spectrum of cytogenomic abnormalities was observed in POC culture success and POC-CF samples. A threshold effect correlating the number of dosage-sensitive genes in a chromosome with the observed frequency of autosomal trisomy is proposed. A rationalized approach using firstly fluorescence in situ hybridization (FISH) testing with probes of chromosomes X/Y/18, 13/21, and 15/16/22 for common aneuploidies and polyploidies and secondly aCGH for other cytogenomic abnormalities is recommended for POC-CF samples.

  1. Preparation of Pt Ag alloy nanoisland/graphene hybrid composites and its high stability and catalytic activity in methanol electro-oxidation

    Directory of Open Access Journals (Sweden)

    Feng Lili

    2011-01-01

    Full Text Available Abstract In this article, PtAg alloy nanoislands/graphene hybrid composites were prepared based on the self-organization of Au@PtAg nanorods on graphene sheets. Graphite oxides (GO were prepared and separated to individual sheets using Hummer's method. Graphene nano-sheets were prepared by chemical reduction with hydrazine. The prepared PtAg alloy nanomaterial and the hybrid composites with graphene were characterized by SEM, TEM, and zeta potential measurements. It is confirmed that the prepared Au@PtAg alloy nanorods/graphene hybrid composites own good catalytic function for methanol electro-oxidation by cyclic voltammograms measurements, and exhibited higher catalytic activity and more stability than pure Au@Pt nanorods and Au@AgPt alloy nanorods. In conclusion, the prepared PtAg alloy nanoislands/graphene hybrid composites own high stability and catalytic activity in methanol electro-oxidation, so that it is one kind of high-performance catalyst, and has great potential in applications such as methanol fuel cells in near future.

  2. A 96-well screen filter plate for high-throughput biological sample preparation and LC-MS/MS analysis.

    Science.gov (United States)

    Peng, Sean X; Cousineau, Martin; Juzwin, Stephen J; Ritchie, David M

    2006-01-01

    A novel 96-well screen filter plate (patent pending) has been invented to eliminate a time-consuming and labor-intensive step in preparation of in vivo study samples--to remove blood or plasma clots. These clots plug the pipet tips during a manual or automated sample-transfer step causing inaccurate pipetting or total pipetting failure. Traditionally, these blood and plasma clots are removed by picking them out manually one by one from each sample tube before any sample transfer can be made. This has significantly slowed the sample preparation process and has become a bottleneck for automated high-throughput sample preparation using robotic liquid handlers. Our novel screen filter plate was developed to solve this problem. The 96-well screen filter plate consists of 96 stainless steel wire-mesh screen tubes connected to the 96 openings of a top plate so that the screen filter plate can be readily inserted into a 96-well sample storage plate. Upon insertion, the blood and plasma clots are excluded from entering the screen tube while clear sample solutions flow freely into it. In this way, sample transfer can be easily completed by either manual or automated pipetting methods. In this report, three structurally diverse compounds were selected to evaluate and validate the use of the screen filter plate. The plasma samples of these compounds were transferred and processed in the presence and absence of the screen filter plate and then analyzed by LC-MS/MS methods. Our results showed a good agreement between the samples prepared with and without the screen filter plate, demonstrating the utility and efficiency of this novel device for preparation of blood and plasma samples. The device is simple, easy to use, and reusable. It can be employed for sample preparation of other biological fluids that contain floating particulates or aggregates.

  3. Magnetic solid phase extraction of gemfibrozil from human serum and pharmaceutical wastewater samples utilizing a β-cyclodextrin grafted graphene oxide-magnetite nano-hybrid.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Talleb, Zeynab

    2015-03-01

    A magnetic solid phase extraction method based on β-cyclodextrin (β-CD) grafted graphene oxide (GO)/magnetite (Fe3O4) nano-hybrid as an innovative adsorbent was developed for the separation and pre-concentration of gemfibrozil prior to its determination by spectrofluorometry. The as-prepared β-CD/GO/Fe3O4 nano-hybrid possesses the magnetism property of Fe3O4 nano-particles that makes it easily manipulated by an external magnetic field. On the other hand, the surface modification of GO by β-CD leads to selective separation of the target analyte from sample matrices. The structure and morphology of the synthesized adsorbent were characterized using powder X-ray diffraction, Fourier transform infrared spectroscopy, and field emission scanning electron microscopy. The experimental factors affecting the extraction/pre-concentration and determination of the analyte were investigated and optimized. Under the optimized experimental conditions, the calibration graph was linear in the range between 10 and 5000 pg mL(-1) with a correlation coefficient of 0.9989. The limit of detection and enrichment factor for gemfibrozil were 3 pg mL(-1) and 100, respectively. The maximum sorption capacity of the adsorbent for gemfibrozil was 49.8 mg g(-1). The method was successfully applied to monitoring gemfibrozil in human serum and pharmaceutical wastewaters samples with recoveries in the range of 96.0-104.0% for the spiked samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Microwave processing for sample preparation to evaluate mitochondrial ultrastructural damage in hemorrhagic shock.

    Science.gov (United States)

    Josephsen, Gary D; Josephsen, Kelly A; Beilman, Greg J; Taylor, Jodie H; Muiler, Kristine E

    2005-12-01

    This is a report of the adaptation of microwave processing in the preparation of liver biopsies for transmission electron microscopy (TEM) to examine ultrastructural damage of mitochondria in the setting of metabolic stress. Hemorrhagic shock was induced in pigs via 35% total blood volume bleed and a 90-min period of shock followed by resuscitation. Hepatic biopsies were collected before shock and after resuscitation. Following collection, biopsies were processed for TEM by a rapid method involving microwave irradiation (Giberson, 2001). Samples pre- and postshock of each of two animals were viewed and scored using the mitochondrial ultrastructure scoring system (Crouser et al., 2002), a system used to quantify the severity of ultrastructural damage during shock. Results showed evidence of increased ultrastructural damage in the postshock samples, which scored 4.00 and 3.42, versus their preshock controls, which scored 1.18 and 1.27. The results of this analysis were similar to those obtained in another model of shock (Crouser et al., 2002). However, the amount of time used to process the samples was significantly shortened with methods involving microwave irradiation.

  5. Using Exclusion-Based Sample Preparation (ESP to Reduce Viral Load Assay Cost.

    Directory of Open Access Journals (Sweden)

    Scott M Berry

    Full Text Available Viral load (VL measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD, accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1 and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP.71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL and high accuracy (average difference between methods of 0.08 log, R2 = 0.97. Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  6. Using Exclusion-Based Sample Preparation (ESP) to Reduce Viral Load Assay Cost.

    Science.gov (United States)

    Berry, Scott M; Pezzi, Hannah M; Williams, Eram D; Loeb, Jennifer M; Guckenberger, David J; Lavanway, Alex J; Puchalski, Alice A; Kityo, Cissy M; Mugyenyi, Peter N; Graziano, Franklin M; Beebe, David J

    2015-01-01

    Viral load (VL) measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD), accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1) and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP).71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL) and high accuracy (average difference between methods of 0.08 log, R2 = 0.97). Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  7. Modular approach to customise sample preparation procedures for viral metagenomics: a reproducible protocol for virome analysis.

    Science.gov (United States)

    Conceição-Neto, Nádia; Zeller, Mark; Lefrère, Hanne; De Bruyn, Pieter; Beller, Leen; Deboutte, Ward; Yinda, Claude Kwe; Lavigne, Rob; Maes, Piet; Van Ranst, Marc; Heylen, Elisabeth; Matthijnssens, Jelle

    2015-11-12

    A major limitation for better understanding the role of the human gut virome in health and disease is the lack of validated methods that allow high throughput virome analysis. To overcome this, we evaluated the quantitative effect of homogenisation, centrifugation, filtration, chloroform treatment and random amplification on a mock-virome (containing nine highly diverse viruses) and a bacterial mock-community (containing four faecal bacterial species) using quantitative PCR and next-generation sequencing. This resulted in an optimised protocol that was able to recover all viruses present in the mock-virome and strongly alters the ratio of viral versus bacterial and 16S rRNA genetic material in favour of viruses (from 43.2% to 96.7% viral reads and from 47.6% to 0.19% bacterial reads). Furthermore, our study indicated that most of the currently used virome protocols, using small filter pores and/or stringent centrifugation conditions may have largely overlooked large viruses present in viromes. We propose NetoVIR (Novel enrichment technique of VIRomes), which allows for a fast, reproducible and high throughput sample preparation for viral metagenomics studies, introducing minimal bias. This procedure is optimised mainly for faecal samples, but with appropriate concentration steps can also be used for other sample types with lower initial viral loads.

  8. Preparation of polyhedral oligomeric silsesquioxane-based hybrid monolith by ring-opening polymerization and post-functionalization via thiol-ene click reaction.

    Science.gov (United States)

    Liu, Zhongshan; Ou, Junjie; Lin, Hui; Wang, Hongwei; Dong, Jing; Zou, Hanfa

    2014-05-16

    A polyhedral oligomeric silsesquioxane (POSS) hybrid monolith was simply prepared by using octaglycidyldimethylsilyl POSS (POSS-epoxy) and cystamine dihydrochloride as monomers via ring-opening polymerization. The effects of composition of prepolymerization solution and polycondensation temperature on the morphology and permeability of monolithic column were investigated in detail. The obtained POSS hybrid monolithic column showed 3D skeleton morphology and exhibited high column efficiency of ∼71,000 plates per meter in reversed-phase mechanism. Owing to this POSS hybrid monolith essentially possessing a great number of disulfide bonds, the monolith surface would expose thiol groups after reduction with dithiothreitol (DTT), which supplied active sites to functionalize with various alkene monomers via thiol-ene click reaction. The results indicated that the reduction with DTT could not destroy the 3D skeleton of hybrid monolith. Both stearyl methylacrylate (SMA) and benzyl methacrylate (BMA) were selected to functionalize the hybrid monolithic columns for reversed-phase liquid chromatography (RPLC), while [2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl)-ammonium hydroxide (MSA) was used to modify the hybrid monolithic column in hydrophilic interaction chromatography (HILIC). These modified hybrid monolithic columns could be successfully applied for separation of small molecules with high efficiency. It is demonstrated that thiol-ene click reaction supplies a facile way to introduce various functional groups to the hybrid monolith possessing thiol groups. Furthermore, due to good permeability of the resulting hybrid monoliths, we also prepared long hybrid monolithic columns in narrow-bore capillaries. The highest column efficiency reached to ∼70,000 plates using a 1-m-long column of 75μm i.d. with a peak capacity of 147 for isocratic chromatography, indicating potential application in separation and analysis of complex biosamples. Copyright © 2014

  9. Preparations of meiotic pachytene chromosomes and extended DNA fibers from cotton suitable for fluorescence in situ hybridization.

    Directory of Open Access Journals (Sweden)

    Renhai Peng

    Full Text Available Fluorescence in situ hybridization (FISH has become one of the most important techniques applied in plant molecular cytogenetics. However, the application of this technique in cotton has lagged behind because of difficulties in chromosome preparation. The focus of this article was FISH performed not only on cotton pachytene chromosomes, but also on cotton extended DNA fibers. The cotton pollen mother cells (PMCs instead of buds or anthers were directly digested in enzyme to completely breakdown the cell wall. Before the routine acetic acid treatment, PMCs were incubated in acetic acid and enzyme mixture to remove the cytoplasm and clear the background. The method of ice-cold Carnoy's solution spreading chromosome was adopted instead of nitrogen removed method to avoid chromosomes losing and fully stretch chromosome. With the above-improved steps, the high-quality well-differentiated pachytene chromosomes with clear background were obtained. FISH results demonstrated that a mature protocol of cotton pachytene chromosomes preparation was presented. Intact and no debris cotton nuclei were obtained by chopping from etiolation cotyledons instead of the conventional liquid nitrogen grinding method. After incubating the nuclei with nucleus lysis buffer on slide, the parallel and clear background DNA fibers were acquired along the slide. This method overcomes the twist, accumulation and fracture of DNA fibers compared with other methods. The entire process of DNA fibers preparation requires only 30 min, in contrast, it takes 3 h with routine nitrogen grinding method. The poisonous mercaptoethanol in nucleus lysis buffer is replaced by nonpoisonous dithiothreitol. PVP40 in nucleus isolation buffer is used to prevent oxidation. The probability of success in isolating nuclei for DNA fiber preparation is almost 100% tested with this method in cotton. So a rapid, safe, and efficient method for the preparation of cotton extended DNA fibers suitable for FISH

  10. Effects of sample preparation on the optical properties of breast tissue

    Science.gov (United States)

    Marks, Fay A.

    1996-04-01

    The optical properties of biological tissue should be determined in vivo whenever possible. However, for those instances when in vivo studies are impractical, too expensive or inappropriate, and when blood flow is not an issue, the ability to perform in vitro studies then becomes invaluable. Optical absorption spectroscopy shows that it may be possible to obtain meaningful information about the optical properties of human breast tissue from in vitro samples if strict preparation and measuring protocols are used. That a strict protocol for storing and handling tissue is critical can be seen from our observations of changes in the optical absorption spectra that occur in response to formalin fixation, the passage of time, application of stains and dyes, and storage in growth medium of the excised tissue. In vivo optical absorption spectroscopy measurements have been made on human breast cancer xenografts and compared with in vitro measurements on breast biopsies prepared according to precise collection and treatment protocols. There is a 'window of opportunity' before time dependent changes in the UV optical absorption spectra of the excised tissue specimens occur. This time window of opportunity widens at longer wavelengths with the least changes occurring in the optical spectra in the NIR.

  11. Lights Will Guide You : Sample Preparation and Applications for Integrated Laser and Electron Microscopy

    Science.gov (United States)

    Karreman, M. A.

    2013-03-01

    Correlative microscopy is the combined use of two different forms of microscopy in the study of a specimen, allowing for the exploitation of the advantages of both imaging tools. The integrated Laser and Electron Microscope (iLEM), developed at Utrecht University, combines a fluorescence microscope (FM) and a transmission electron microscope (TEM) in a single set-up. The region of interest in the specimen is labeled or tagged with a fluorescent probe and can easily be identified within a large field of view with the FM. Next, this same area is retraced in the TEM and can be studied at high resolution. The iLEM demands samples that can be imaged with both FM and TEM. Biological specimen, typically composed of light elements, generate low image contrast in the TEM. Therefore, these samples are often ‘contrasted’ with heavy metal stains. FM, on the other hand, images fluorescent samples. Sample preparation for correlative microscopy, and iLEM in particular, is complicated by the fact that the heavy metals stains employed for TEM quench the fluorescent signal of the probe that is imaged with FM. The first part of this thesis outlines preparation procedures for biological material yielding specimen that can be imaged with the iLEM. Here, approaches for the contrasting of thin sections of cells and tissue are introduced that do not affect the fluorescence signal of the probe that marks the region of interest. Furthermore, two novel procedures, VIS2FIXH and VIS2FIX­FS are described that allow for the chemical fixation of thin sections of cryo-immobilized material. These procedures greatly expedite the sample preparation process, and open up novel possibilities for the immuno-labeling of difficult antigens, eg. proteins and lipids that are challenging to preserve. The second part of this thesis describes applications of iLEM in research in the field of life and material science. The iLEM was employed in the study of UVC induced apoptosis (programmed cell death) of

  12. Sample Preparation for Headspace GC Analysis of Residual Solvents in Hyaluronic Acid Derivative Fiber

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hoon Joo; Kim, Dong Min; Yang, Jeong Soo [LG life Sciences, Ltd./R and D Park, Daejeon (Korea, Republic of); Kim, Chan Wha [Korea University, Seoul (Korea, Republic of)

    2006-02-15

    The aim of this study is to develop efficient sample preparation method for HS-GC analysis of residual solvents in HA derivative fiber. Compared to direct extraction of residual solvents from HA derivative fiber, the extraction through the hydrolysis of HA derivative fiber by HAse gave more complete and higher reproducible quantification of residual solvent. To validate HS-GC analysis method of residual solvents, specificity, limits of detection and quantification, linearity, accuracy and precision are investigated in the study. HA derivative fiber was hydrolyzed using HAse for headspace gas chromatographic analysis of residual solvents of ethanol, acetone and isopropanol in HA derivative fiber. This study showed that the developed method had specificity, linearity, accuracy and precision. In addition, it demonstrated that HS-GC coupled with matrix-breaking method such as hydrolysis was available for the determination of residual solvents in a matrix like HA derivative fiber.

  13. Applied Study on Magnetic Nanometer Beads in Preparation of Genechip Samples

    Institute of Scientific and Technical Information of China (English)

    陈慧; 高华方; 谢欣; 马雪梅; 杨渝珍

    2004-01-01

    Summary: A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid-phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads with karyocyte as template directly and the PCR products were applied on an oligonucleotide array to do gene typing. The HLA-A PCR amplification system and a small HLA-A oligonucleotide microarray were applied as the platform and an experiment protocol of separating karyocyte from whole blood using the magnetic nanometer beads (Fe2O3) were set up.The experimental conditions were also discussed. It showed that pH level of PBS eluent, Taq enzyme quantity and fragment length of products could influent the amplification results, and the magnetic nano-beads could succeed in sample preparation in microarray to provide a promising way in automatic detection and lab-on-a-chip.

  14. NGSI FY15 Final Report. Innovative Sample Preparation for in-Field Uranium Isotopic Determinations

    Energy Technology Data Exchange (ETDEWEB)

    Yoshida, Thomas M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Meyers, Lisa [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-11-10

    Our FY14 Final Report included an introduction to the project, background, literature search of uranium dissolution methods, assessment of commercial off the shelf (COTS) automated sample preparation systems, as well as data and results for dissolution of bulk quantities of uranium oxides, and dissolution of uranium oxides from swipe filter materials using ammonium bifluoride (ABF). Also, discussed were reaction studies of solid ABF with uranium oxide that provided a basis for determining the ABF/uranium oxide dissolution mechanism. This report details the final experiments for optimizing dissolution of U3O8 and UO2 using ABF and steps leading to development of a Standard Operating Procedure (SOP) for dissolution of uranium oxides on swipe filters.

  15. Agarose- and alginate-based biopolymers for sample preparation: Excellent green extraction tools for this century.

    Science.gov (United States)

    Sanagi, Mohd Marsin; Loh, Saw Hong; Wan Ibrahim, Wan Nazihah; Pourmand, Neda; Salisu, Ahmed; Wan Ibrahim, Wan Aini; Ali, Imran

    2016-03-01

    Recently, there has been considerable interest in the use of miniaturized sample preparation techniques before the chromatographic monitoring of the analytes in unknown complex compositions. The use of biopolymer-based sorbents in solid-phase microextraction techniques has achieved a good reputation. A great variety of polysaccharides can be extracted from marine plants or microorganisms. Seaweeds are the major sources of polysaccharides such as alginate, agar, agarose, as well as carrageenans. Agarose and alginate (green biopolymers) have been manipulated for different microextraction approaches. The present review is focused on the classification of biopolymer and their applications in multidisciplinary research. Besides, efforts have been made to discuss the state-of-the-art of the new microextraction techniques that utilize commercial biopolymer interfaces such as agarose in liquid-phase microextraction and solid-phase microextraction.

  16. METHODOLOGICAL ASPECTS OF MOLASSES SAMPLE PREPARATION IN SULFUR DIOXIDE CONTENT DETERMINING

    Directory of Open Access Journals (Sweden)

    M. I. Egorova

    2015-01-01

    Full Text Available Summary. Molasses is characterized as sugar production by-product from primary or secondary sacchariferous raw materials. The features of the appearance, the chemical composition, molasses and exit directions of its use, depending on the type of production, in which it is formed. The value of molasses is demonstrated according to its total composition as well as its use directions. Statistics on beet molasses amounts in Russia is presented. Described consumer market molasses in Russia and abroad with its exports. Shown regulations contain requirements for the quality and safety of molasses, including sulfur dioxide. The data on sulfur allergenic properties are presented. Showing source of the sulfur dioxide in the residual molasses number of processing aids and the impact of its level in the value of raw molasses for use in biotechnological processes and fodder production. The necessity to develop methodology for determining the sulfur dioxide content in the molasses to control its security. The iodometric method, which is used in practice for determination of sulphur dioxide in foods are characterized. Differences molasses and sugar as objects of iodometric determination of sulfur dioxide, which leads to the inability to ascertain the equivalence point. The variants eliminate interfering background of dark-colored foods common in analytical chemistry. Advantages and disadvantages of the background masking and stripping the determination of sulfur dioxide in the darkcolored products. It was characterized by clarifying sugar solutions in optical control methods. The hypothesis about preferability of its use in sample molasses preparation for equivalence point fixation in iodometric titration is suggested. The tasks of experimental research for the development of sample preparation algorithm molasses in determining the content of sulphurous acid.

  17. ALGORITHM OF PREPARATION OF THE TRAINING SAMPLE USING 3D-FACE MODELING

    Directory of Open Access Journals (Sweden)

    D. I. Samal

    2016-01-01

    Full Text Available The algorithm of preparation and sampling for training of the multiclass qualifier of support vector machines (SVM is provided. The described approach based on the modeling of possible changes of the face features of recognized person. Additional features like perspectives of shooting, conditions of lighting, tilt angles were introduced to get improved identification results. These synthetic generated changes have some impact on the classifier learning expanding the range of possible variations of the initial image. The classifier learned with such extended example is ready to recognize unknown objects better. The age, emotional looks, turns of the head, various conditions of lighting, noise, and also some combinations of the listed parameters are chosen as the key considered parameters for modeling. The third-party software ‘FaceGen’ allowing to model up to 150 parameters and available in a demoversion for free downloading is used for 3D-modeling.The SVM classifier was chosen to test the impact of the introduced modifications of training sample. The preparation and preliminary processing of images contains the following constituents like detection and localization of area of the person on the image, assessment of an angle of rotation and an inclination, extension of the range of brightness of pixels and an equalization of the histogram to smooth the brightness and contrast characteristics of the processed images, scaling of the localized and processed area of the person, creation of a vector of features of the scaled and processed image of the person by a Principal component analysis (algorithm NIPALS, training of the multiclass SVM-classifier.The provided algorithm of expansion of the training selection is oriented to be used in practice and allows to expand using 3D-models the processed range of 2D – photographs of persons that positively affects results of identification in system of face recognition. This approach allows to compensate

  18. Preparation and properties of poly(vinylidene fluoride nanocomposites blended with graphene oxide coated silica hybrids

    Directory of Open Access Journals (Sweden)

    Q. Fu

    2012-04-01

    Full Text Available Graphene oxide coated silica hybirds (SiO2-GO were fabricated through electrostatic assembly in this work, then blended with poly(vinylidene fluoride (PVDF by solution mixing to make PVDF nanocomposites. The interfacial interaction was investigated by scanning electron microscopy (SEM, polarized optical microscopy (POM and Fourier transform infrared spectroscopy (FTIR. The results showed that the interfacial interaction was enhanced by adding of SiO2-GO and strong hydrogen bonds were observed. The as-made nanocomposites were investigated using standard tensile test and dynamic mechanical analysis (DMA measurements, mechanical properties of PVDF with SiO2-GO hybrids showed limited improvement.

  19. Bonelike/PLGA hybrid materials for bone regeneration : preparation route and physicochemical characterisation

    OpenAIRE

    Oliveira, Joaquim M.; Miyazaki, T; Lopes, M A; Ohtsuki, C.; Santos,J.D.

    2005-01-01

    Bonelike R /PLGA hybrid materials have been developed using γ -MPS as silane-coupling agent between the inorganic and organic phases for controlled drug delivery applications. Silanization showed to be more effective when cyclohexane was used as a non-polar solvent (nP method) due to a chemical interaction between Bonelike R and the silane film, while by using a 95/5 (V/V) methanol/water as a polar solvent (P method), a much thinner film was achieved. Functional groups of PL...

  20. Preparation of well-defined polystyrene/silica hybrid nanoparticles by ATRP

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Immobilization of the atom transfer radical polymerization(ATRP)macroinitiators at the silica nanoparticle surfaces was achieved through surface modification with excess toluene-2,4-diisocynate(TDI),after which the residual isocyanate groups were converted into ATRP macroinitiators.Structurally well-defined polystyrene chains were grown from the nanoparticle surfaces to yield individual particles composed of a silica core and a well-defined,densely grafted outer polystyrene by ATRP,which was initiated by the as-synthesized silica-based macroinitiator.FTIR,NMR and gel permeation chromatography(GPC)were used to characterize the polystyrene/silica hybrid particles.

  1. Preparation of well-defined polystyrene/silica hybrid nanoparticles by ATRP

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Immobilization of the atom transfer radical polymerization (ATRP) macroinitiators at the silica nanoparticle surfaces was achieved through surface modification with excess toluene-2,4-diisocynate (TDI), after which the residual isocyanate groups were converted into ATRP macroinitiators. Structurally well-defined polystyrene chains were grown from the nanoparticle surfaces to yield individual particles composed of a silica core and a well-defined, densely grafted outer polystyrene by ATRP, which was initiated by the as-synthesized silica-based macroinitiator. FTIR, NMR and gel permeation chro-matography (GPC) were used to characterize the polystyrene/silica hybrid particles.

  2. Advanced sample preparation for the molecular quantification of Staphylococcus aureus in artificially and naturally contaminated milk.

    Science.gov (United States)

    Aprodu, Iuliana; Walcher, Georg; Schelin, Jenny; Hein, Ingeborg; Norling, Börje; Rådström, Peter; Nicolau, Anca; Wagner, Martin

    2011-03-01

    Sample treatment is an essential element when using real-time PCR for quantification of pathogens directly on food samples. This study comparatively evaluated three different principles of sample treatment, i.e. immunomagnetic separation based on phage-derived cell wall binding molecules, matrix solubilization and flotation, in order to establish their suitability for quantifying low numbers of Staphylococcus aureus in milk. All three procedures succeeded to remove S. aureus from the milk matrix, either raw or pasteurized, and, as a result of the concentration of the target cells, minimized the effect of milk associated PCR inhibitors. Sample preparation based on immunomagnetic separation albeit of being user friendly, specific and rapid, failed to allow quantification of low and medium numbers (<10(4)CFU) of S. aureus. In a mastitic milk model cell wall binding domain (CBD)-based target cell extraction revealed results most closely matching those derived from culture-based quantification. Both matrix lysis and flotation allowed quantification of S. aureus at a level of 1-10 cells per ml. Both methods resulted in higher numbers of bacterial cell equivalents (bce) than plating could reveal. Since both methods harvest cells that have been subjected to either mechanical and chemical stresses before quantification, we concluded that the higher bce numbers resulted from a disaggregation of S. aureus clusters initially present in the inoculum. Conclusively, since likely each S. aureus cell of a toxigenic strain contributes to enterotoxin production, molecular quantification could provide an even more realistic impact assessment in outbreak investigations than plating does.

  3. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

    Science.gov (United States)

    Yang, Bin; Smith, A. M.; Long, S.

    2015-10-01

    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0-3 bar) and so has the capacity to graphitise CO2 samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a 'budget' fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  4. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Bin; Smith, A.M.; Long, S.

    2015-10-15

    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0–3 bar) and so has the capacity to graphitise CO{sub 2} samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a ‘budget’ fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  5. Porphyrinosilica and metalloporphyrinosilica: hybrid organic-inorganic materials prepared by sol-gel processing

    Directory of Open Access Journals (Sweden)

    YASSUKO IAMAMOTO

    2000-03-01

    Full Text Available New materials porphyrinosilica and metalloporphyrinosilica template have been obtained by a sol-gel processing where functionalyzed porphyrins and metalloporphyrins "building blocks" were assembled into a three-dimensional silicate network. The optimized conditions for preparation of these materials are revised. The monomer precursors porphyrinopropylsilyl and metalloporphyrinopropylsilyl preparation reactions and subsequent one pot sol-gel processing with tetraethoxysilane are discussed. In the case of metalloporphyrins the nitrogen base coordinates to the central metal and acts as a template in the molecular imprinting technique. UV-visible absorption spectroscopy, thermogravimetric analysis, electron paramagnetic resonance, nuclear magnetic spectra, infrared spectra, luminescence spectra, surface area and electron spectroscopy imaging of the materials are used to characterize the prepared materials. The catalytic activities of these metalloporphyrinosilica- template are compared.

  6. Preparation and characterization of hybrid nanoparticles based on chitosan and poly(methacryloylglycylglycine)

    Science.gov (United States)

    Ferri, Marcella; Dash, Mamoni; Cometa, Stefania; De Giglio, Elvira; Sabbatini, Luigia; Chiellini, Federica

    2014-05-01

    The present work investigated the possibility of preparing nanoparticles based on methacryloylglycylglycine (MAGG) and chitosan (CS) by in situ polymerization. The study revealed that nanoparticle formation was strictly dependent on ionic interactions between NH3 + groups from CS and COO- groups arising from the anionic monomer MAGG. The subsequent in situ polymerizations of MAGG in the presence of CS led to the formation of nanoparticles with homogeneous morphology, a uniform particle size distribution, and a good spherical shape as confirmed by laser diffraction granulometry and scanning electron microscopy analyses. Nanoparticle formulations with different amounts of CS and MAGG were prepared, and their chemical compositions were investigated by X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The obtained results showed that the polymerization of MAGG in the presence of CS appears to be a very promising approach in the preparation of nanoparticles for drug delivery applications.

  7. Preparation and characteristics of nanotetrapods CdSe-polymer hybrid solar cells

    Indian Academy of Sciences (India)

    Qi Pang; Li Juan Zhao; Jun He; Chun Jie Liang; Ai Miao Qin; Jian Nong Wang

    2013-12-01

    Tetrapod-shaped CdSe nanocrystals were obtained using a simple method. HRTEM shows that the average size of the tetrapod core are about 4 nm, widths of the tetrapod arms are about 4 nm and lengths of the arms are about 20 nm. XRD patterns reveal that the OA-capped CdSe tetrapod nanocrystals have a hexagonal wurtzite structure. A hybrid solar cell fabricated based on an 8:1 (w/w) blend of CdSe tetrapod nanocrystals and MEH–PPV showed a maximum power conversion efficiency of 0.46% under an air mass 1.5 global condition. The effects of nanocrystal composition on the photovoltaic properties of hybrid solar cells based on nanotetrapods CdSe/MEH–PPV were investigated. The power conversion efficiency values initially increased and then decreased, but the OC values linearly decreased from 1.1 to 0.25 V with increased CdSe nanotetrapod in the blend film. The significant quenching of PL with increased nanotetrapod concentration indicated photo-induced charge transfer between MEH–PPV and CdSe.

  8. Preparation of Luminol-doped Nanoparticle and Its Application in DNA Hybridization Analysis

    Institute of Scientific and Technical Information of China (English)

    QIAN,Ke-Jun(钱柯君); ZHANG,Ling(张玲); YANG,Min-Li(杨敏丽); HE,Pin-Gang(何品刚); FANG,Yu-Zhi(方禹之)

    2004-01-01

    The dye-doped silica nanoparticles can be used as nanobiosensors that are able to recognize and detect specific DNA sequence. In this paper, spherical nanosized luminol/SiO2 composite particles have been synthesized with reverse micells via hydrolysis of tetraethyl orthosilicate (TEOS) in the microemulsion. The nanoparticles were modified with chitosan and used to label DNA, forming the DNA probe which was used to hybridize with target DNA immobilized on a PPy modified Pt electrode. The hybridization events were evaluated by electrogenerated chemiluminescence (ECL) measurements and only the complementary sequence could form a double-stranded DNA (dsDNA) with DNA probe and give strong ECL signals. A three base mismatch sequence and a non-complementary sequence had almost negligible responses. Due to the large number of luminol molecules inside silica nanoparticles, the assay allows detection at levels as low as 2.0 × 10- 12 mol/L of the target DNA. The intensity of ECL was linearly related to the concentration of the complementary sequence in the range of 5.0 × 10-12-1.0 ×10-9 mol/L.

  9. Preparation and Properties of Polymer/Vermiculite Hybrid Superabsorbent Reinforced by Fiber for Enhanced Oil Recovery

    Directory of Open Access Journals (Sweden)

    Fayang Jin

    2014-01-01

    Full Text Available A series of polymer/clay hybrid superabsorbent composites (SACFs comprising acrylamide, acrylic acid, sodium 2-acrylamido-tetradecyl sulfonate, fiber, and vermiculite by in situ intercalation and exfoliated method was successfully synthesized. The structure of SACFs was characterized by IR, SXRD, and SEM measurements. Much notable absorbency for SACF-2 was observed compared to that for SACF-1 in the absence of hydrophobic group in the high cationic solution due to the alkyl carbon chain and sulfonic acid group of hydrophobic moistures protecting the cations from attacking the carboxylate groups. What is more, high temperature fiber which acts as bridge connection for the polymeric network structure enhanced both toughness and strength for SACF-4 in the harsh conditions. At the total dissolved substance of 212000 mg/L for Tarim Basin injected water and the temperature of 120°C, desired absorbency as well as water retaining property for SACF-4 was observed during the long period of thermal ageing. Core flooding experiments demonstrated that SACFs could migrate as amoeba in the porous medium and accumulated in the narrow channel to adjust injection profile, promoting the subsequent water diverting into the unswept zones. Finally, characteristic parameters for SACFs calculated from flooding experiment further confirmed these polymer/clay hybrid composites reinforced by fiber would have robust application in the mature oilfield for profile control.

  10. A simple nanostructured polymer/ZnO hybrid solar cell - preparation and operation in air

    DEFF Research Database (Denmark)

    Krebs, Frederik C; Thomann, Yi; Thomann, Ralf

    2008-01-01

    without notable loss in efficiency. The devices do not require any form of encapsulation to gain stability, while a barrier for mechanical protection may be useful. The devices are based on soluble zinc oxide nanoparticles mixed with the thermocleavable conjugated polymer poly-(3-(2-methylhexan-2-yl......A detailed description is given of the preparation of a polymer solar cell and its characterization. The solar cell can be prepared entirely in the ambient atmosphere by solution processing without the use of vacuum coating steps, and it can be operated in the ambient atmosphere with good...

  11. The solvothermal synthesis of magnetic iron oxide nanocrystals and the preparation of hybrid poly(L-lactide)-polyethyleneimine magnetic particles.

    Science.gov (United States)

    Stojanović, Zoran; Otoničar, Mojca; Lee, Jongwook; Stevanović, Magdalena M; Hwang, Mintai P; Lee, Kwan Hyi; Choi, Jonghoon; Uskoković, Dragan

    2013-09-01

    We report a simple and green procedure for the preparation of magnetic iron oxide nanocrystals via solvothermal synthesis. The nanocrystal synthesis was carried out under mild conditions in the water-ethanol-oleic acid solvent system with the use of the oleate anion as a surface modifier of nanocrystals and glucose as a reducing agent. Specific conditions for homogenous precipitation achieved in such a reaction system lead to the formation of uniform high-quality nanocrystals down to 5 nm in diameter. The obtained hydrophobic nanocrystals can easily be converted to hydrophilic magnetic nanoparticles by being immobilized in a poly(L-lactide)-polyethyleneimine polymeric matrix. These hybrid nano-constructs may find various biomedical applications, such as magnetic separation, gene transfection and/or magnetic resonance imaging. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Optical biosensor system with integrated microfluidic sample preparation and TIRF based detection

    Science.gov (United States)

    Gilli, Eduard; Scheicher, Sylvia R.; Suppan, Michael; Pichler, Heinz; Rumpler, Markus; Satzinger, Valentin; Palfinger, Christian; Reil, Frank; Hajnsek, Martin; Köstler, Stefan

    2013-05-01

    There is a steadily growing demand for miniaturized bioanalytical devices allowing for on-site or point-of-care detection of biomolecules or pathogens in applications like diagnostics, food testing, or environmental monitoring. These, so called labs-on-a-chip or micro-total analysis systems (μ-TAS) should ideally enable convenient sample-in - result-out type operation. Therefore, the entire process from sample preparation, metering, reagent incubation, etc. to detection should be performed on a single disposable device (on-chip). In the early days such devices were mainly fabricated using glass or silicon substrates and adapting established fabrication technologies from the electronics and semiconductor industry. More recently, the development focuses on the use of thermoplastic polymers as they allow for low-cost high volume fabrication of disposables. One of the most promising materials for the development of plastic based lab-on-achip systems are cyclic olefin polymers and copolymers (COP/COC) due to their excellent optical properties (high transparency and low autofluorescence) and ease of processing. We present a bioanalytical system for whole blood samples comprising a disposable plastic chip based on TIRF (total internal reflection fluorescence) optical detection. The chips were fabricated by compression moulding of COP and microfluidic channels were structured by hot embossing. These microfluidic structures integrate several sample pretreatment steps. These are the separation of erythrocytes, metering of sample volume using passive valves, and reagent incubation for competitive bioassays. The surface of the following optical detection zone is functionalized with specific capture probes in an array format. The plastic chips comprise dedicated structures for simple and effective coupling of excitation light from low-cost laser diodes. This enables TIRF excitation of fluorescently labeled probes selectively bound to detection spots at the microchannel surface

  13. Sample preparation for metalloprotein analysis: A case study using horse chestnuts.

    Science.gov (United States)

    de Magalhães, Cristiana Schmidt; Arruda, Marco Aurélio Zezzi

    2007-03-30

    In the present work, 11 different procedures for protein and metalloprotein extraction from horse chestnuts (Aescullus hippocastanum L.) in natura were tested. After each extraction, total protein was determined and, after protein separation through sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), those metals belonging to the protein structure were mapped by synchrotron radiation X-ray fluorescence (SRXRF). After mapping the elements (Cr, Fe and Mn) in the protein bands (ca. 33 and 23.7kDa), their concentrations were determined using atomic absorption spectrometry (ET AAS). Good results were obtained for protein extraction using a combination of grinding and sonication. However, this strategy was not suitable to preserve metal ions in the protein structure. In fact, there was 42% decrease on Mn concentration using this procedure, compared to that performed with sample agitation in water (taken as reference). On the other hand, when grinding and agitation with an extracting buffer was used, there was a 530% increase of Mn concentration, when compared to the reference procedure. These results indicate agreement between metal identification and determination in proteins as well as the great influence of the extraction procedure (i.e., the sample preparation step) for preserving metals in the protein structures.

  14. Suspension trapping (STrap) sample preparation method for bottom-up proteomics analysis.

    Science.gov (United States)

    Zougman, Alexandre; Selby, Peter J; Banks, Rosamonde E

    2014-05-01

    Despite recent developments in bottom-up proteomics, the need still exists in a fast, uncomplicated, and robust method for comprehensive sample processing especially when applied to low protein amounts. The suspension trapping method combines the advantage of efficient SDS-based protein extraction with rapid detergent removal, reactor-type protein digestion, and peptide cleanup. Proteins are solubilized in SDS. The sample is acidified and introduced into the suspension trapping tip incorporating the depth filter and hydrophobic compartments, filled with the neutral pH methanolic solution. The instantly formed fine protein suspension is trapped in the depth filter stack-this crucial step is aimed at separating the particulate matter in space. SDS and other contaminants are removed in the flow-through, and a protease is introduced. Following the digestion, the peptides are cleaned up using the tip's hydrophobic part. The methodology allows processing of protein loads down to the low microgram/submicrogram levels. The detergent removal takes about 5 min, whereas the tryptic proteolysis of a cellular lysate is complete in as little as 30 min. We have successfully utilized the method for analysis of cellular lysates, enriched membrane preparations, and immunoprecipitates. We expect that due to its robustness and simplicity, the method will become an essential proteomics tool.

  15. Layered Ni(OH)2-Co(OH)2 films prepared by electrodeposition as charge storage electrodes for hybrid supercapacitors

    Science.gov (United States)

    Nguyen, Tuyen; Boudard, Michel; Carmezim, M. João; Montemor, M. Fátima

    2017-01-01

    Consecutive layers of Ni(OH)2 and Co(OH)2 were electrodeposited on stainless steel current collectors for preparing charge storage electrodes of high specific capacity with potential application in hybrid supercapacitors. Different electrodes were prepared consisting on films of Ni(OH)2, Co(OH)2, Ni1/2Co1/2(OH)2 and layered films of Ni(OH)2 on Co(OH)2 and Co(OH)2 on Ni(OH)2 to highlight the advantages of the new architecture. The microscopy studies revealed the formation of nanosheets in the Co(OH)2 films and of particles agglomerates in the Ni(OH)2 films. Important morphological changes were observed in the double hydroxides films and layered films. Film growth by electrodeposition was governed by instantaneous nucleation mechanism. The new architecture composed of Ni(OH)2 on Co(OH)2 displayed a redox response characterized by the presence of two peaks in the cyclic voltammograms, arising from redox reactions of the metallic species present in the layered film. These electrodes revealed a specific capacity of 762 C g−1 at the specific current of 1 A g−1. The hybrid cell using Ni(OH)2 on Co(OH)2 as positive electrode and carbon nanofoam paper as negative electrode display specific energies of 101.3 W h g−1 and 37.8 W h g−1 at specific powers of 0.2 W g−1 and 2.45 W g−1, respectively. PMID:28051143

  16. Layered Ni(OH)2-Co(OH)2 films prepared by electrodeposition as charge storage electrodes for hybrid supercapacitors.

    Science.gov (United States)

    Nguyen, Tuyen; Boudard, Michel; Carmezim, M João; Montemor, M Fátima

    2017-01-04

    Consecutive layers of Ni(OH)2 and Co(OH)2 were electrodeposited on stainless steel current collectors for preparing charge storage electrodes of high specific capacity with potential application in hybrid supercapacitors. Different electrodes were prepared consisting on films of Ni(OH)2, Co(OH)2, Ni1/2Co1/2(OH)2 and layered films of Ni(OH)2 on Co(OH)2 and Co(OH)2 on Ni(OH)2 to highlight the advantages of the new architecture. The microscopy studies revealed the formation of nanosheets in the Co(OH)2 films and of particles agglomerates in the Ni(OH)2 films. Important morphological changes were observed in the double hydroxides films and layered films. Film growth by electrodeposition was governed by instantaneous nucleation mechanism. The new architecture composed of Ni(OH)2 on Co(OH)2 displayed a redox response characterized by the presence of two peaks in the cyclic voltammograms, arising from redox reactions of the metallic species present in the layered film. These electrodes revealed a specific capacity of 762 C g(-1) at the specific current of 1 A g(-1). The hybrid cell using Ni(OH)2 on Co(OH)2 as positive electrode and carbon nanofoam paper as negative electrode display specific energies of 101.3 W h g(-1) and 37.8 W h g(-1) at specific powers of 0.2 W g(-1) and 2.45 W g(-1), respectively.

  17. Investigation into Alternative Sample Preparation Techniques for the Determination of Heavy Metals in Stationary Source Emission Samples Collected on Quartz Filters

    Directory of Open Access Journals (Sweden)

    Sharon L. Goddard

    2014-11-01

    Full Text Available Monitoring stationary source emissions for heavy metals generally requires the use of quartz filters to collect samples because of the high temperature and high moisture sampling environment. The documentary standard method sample preparation technique in Europe, EN 14385, uses digestion in hydrofluoric acid and nitric acid (HF/HNO3 followed by complexing with boric acid (H3BO3 prior to analysis. However, the use of this method presents a number of problems, including significant instrumental drift during analysis caused by the matrix components, often leading to instrument breakdown and downtime for repairs, as well as posing significant health and safety risks. The aim of this work was to develop an alternative sample preparation technique for emissions samples on quartz filters. The alternative techniques considered were: (i acid digestion in a fluoroboric acid (HBF4 and HNO3 mixture and (ii acid extraction in an aqua regia (AR mixture (HCl and HNO3. Assessment of the effectiveness of these options included determination of interferences and signal drift, as well as validating the different methods by measurement of matrix certified reference materials (CRMs, and comparing the results obtained from real test samples and sample blanks to determine limits of detection. The results showed that the HBF4/HNO3 mixture provides the most viable alternative to the documentary standard preparation technique.

  18. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

    Science.gov (United States)

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

    2016-01-28

    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed.

  19. Red-blood-cell-like BSA/Zn3(PO4)2 hybrid particles: Preparation and application to adsorption of heavy metal ions

    Science.gov (United States)

    Zhang, Baoliang; Li, Peitao; Zhang, Hepeng; Li, Xiangjie; Tian, Lei; Wang, Hai; Chen, Xin; Ali, Nisar; Ali, Zafar; Zhang, Qiuyu

    2016-03-01

    A novel kind of red-blood-cell-like bovine serum albumin (BSA)/Zn3(PO4)2 hybrid particle is prepared at room temperature by a facile and rapid one-step method based on coordination between BSA and zinc ion. The morphology of the monodisperse hybrid particle shows oblate spheroidal type with a one sided single hole on the surface. The hybrid particle is constructed with BSA/Zn3(PO4)2 nanoplates of 35 nm thick. The average particle size of hybrid particle is 2.3 μm, and its BET specific surface area is 146.64 cm2/g. To clarify the evolution of BSA/Zn3(PO4)2 hybrid particle, SEM and elemental analysis as a function of particle growth time are investigated. The formation mechanism of BSA/Zn3(PO4)2 hybrid particle, which can be described as crystallization, coordination and self-assembly process, is illustrated in detail. The as-prepared BSA/Zn3(PO4)2 hybrid particle is used for adsorption of Cu2+. The hybrid particle displayed excellent adsorption properties on Cu2+. The adsorption efficiency of BSA/Zn3(PO4)2 hybrid particles at 5 min and 30 min are 86.33% and 98.9%, respectively. The maximum adsorption capacity is 6.85 mg/g. Thus, this kind of novel adsorbent shows potential application value in ultra-fast and highly efficient removal of Cu2+.

  20. Preparation of new hybrid organic/inorganic polymeric chiral stationary phases for ligand-exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Three new hybrid organic/inorganic polymeric ligand-exchange chiral stationary phases were developed by radical chain transfer reaction and surface grafting on silica gel, and successfully used for the enantioseparations of DL-amino acids and DL-hydroxyl acids. The resolutions were achieved by using water containing 2.0 × 10-4 mol/L of CuAc2 as a mobile phase, column temperature of 40 ℃, flow rate of 1.0 mL/min and detection at UV 254 mn. The elution order of D-isomer before L-isomer was observed for all DL-amino acids resolved except DL-Pro.

  1. Nanostructured Wood Hybrids for Fire-Retardancy Prepared by Clay Impregnation into the Cell Wall.

    Science.gov (United States)

    Fu, Qiliang; Medina, Lilian; Li, Yuanyuan; Carosio, Federico; Hajian, Alireza; Berglund, Lars A

    2017-09-14

    Eco-friendly materials need "green" fire-retardancy treatments, which offer opportunity for new wood nanotechnologies. Balsa wood (Ochroma pyramidale) was delignified to form a hierarchically structured and nanoporous scaffold mainly composed of cellulose nanofibrils. This nanocellulosic wood scaffold was impregnated with colloidal montmorillonite clay to form a nanostructured wood hybrid with high flame-retardancy. The nanoporous scaffold was characterized by scanning electron microscopy and gas adsorption. Flame-retardancy was evaluated by cone calorimetry, whereas thermal and thermo-oxidative stabilities were assessed by thermogravimetry. The location of well-distributed clay nanoplatelets inside the cell walls was confirmed by energy-dispersive X-ray analysis. This unique nanostructure dramatically increased the thermal stability because of thermal insulation, oxygen depletion, and catalytic charring effects. A coherent organic/inorganic charred residue was formed during combustion, leading to a strongly reduced heat release rate peak and reduced smoke generation.

  2. Preparation and mechanical properties of TLCP/UP/GF in-situ hybrid composites

    Institute of Scientific and Technical Information of China (English)

    YU Xian-bao; WEI Chun; LU Shao-rong; YU Jing-hong; XU Deng; LU Chi-hua

    2006-01-01

    One kind of novel reactive thermotropic liquid crystalline polymer-methacryloyl copolymer (LCMC) containing polyester mesogenic units was synthesized. Its structure,morphology and properties were investigated systemically by Ubbelohde viscometer,differential scanning calorimetry (DSC),Fourier transform infrared spectroscopy (FTIR),wide-angle X-ray diffractometry (WAXD) and polarizing optical microscopy (POM). The results indicate that it is one kind of nematic thermotropic liquid crystal polymer (TLCP). The impact strength,bending strength and the morphologies of impact fracture surface of LCMC,unsaturated polyester (UP) and glass fiber (GF) in-situ hybrid composites were studied by Izod impact tester,universal testing machine and scanning electron microscopy (SEM),respectively. The results show that the impact and bending strength of composites containing LCMC are improved,especially the composites containing 5% LCMC increases most obviously. These results with SEM results reveal that LCMC plays an important role in the improvement of interfacial adhesive between matrix and fiber.

  3. Investigation of hybrid molecular material prepared by ionic liquid and polyoxometalate anion

    Indian Academy of Sciences (India)

    T Rajkumar; G Ranga Rao

    2008-11-01

    A solid hybrid molecular material containing 1-butyl 3-methyl imidazolium cations and Keggin anions of phosphotungstic acid has been synthesized. It is fully characterized by CHN analysis, FTIR, XRD, UV-Vis-NIR DRS, 31P MAS NMR, TGA and SEM. The FTIR spectrum of the compound shows the fingerprint vibrational bands of both Keggin molecular anions and imidazolium cations. The aromatic C-H stretch region (2700-3250 cm-1) of imidazolium cation is split due to the interaction between the ring C-H and bulky Keggin anion. The red-shift in the UV-Vis spectra and the downfield 31P MAS NMR chemical shift also confirm the electrostatic interaction between the ions in the compound. Near IR spectral region (1000-2500 nm) shows the elimination of water in the compound which is hydrophobic.

  4. Toward a Fieldable Atomic Mass Spectrometer for Safeguards Applications: Sample Preparation and Ionization

    Energy Technology Data Exchange (ETDEWEB)

    Barinaga, Charles J.; Hager, George J.; Hart, Garret L.; Koppenaal, David W.; Marcus, R. Kenneth; Jones, Sarah MH; Manard, Benjamin T.

    2014-10-31

    The International Atomic Energy Agency’s (IAEA’s) long-term research and development plan calls for the development of new methods to detect misuse at nuclear fuel cycle facilities such as reprocessing and enrichment plants. At enrichment plants, for example, the IAEA’s contemporary safeguards approaches are based on a combination of routine and random inspections that include collection of UF6 samples from in-process material and selected cylinders for subsequent analyses. These analyses include destructive analysis (DA) in a laboratory (typically by mass spectrometry [MS]) for isotopic characterization, and environmental sampling (ES) for subsequent laboratory elemental and isotopic analysis (also both typically by MS). One area of new method development includes moving this kind of isotope ratio analytical capability for DA and ES activities into the field. Some of the reasons for these developments include timeliness of results, avoidance of hazardous material shipments, and guidance for additional sample collecting. However, this capability does not already exist for several reasons, such as that most lab-based chemical and instrumental methods rely on laboratory infrastructure (highly trained staff, power, space, hazardous material handling, etc.) and require significant amounts of consumables (power, compressed gases, etc.). In addition, there are no currently available, fieldable instruments for atomic or isotope ratio analysis. To address these issues, Pacific Northwest National Laboratory (PNNL) and collaborator, Clemson University, are studying key areas that limit the fieldability of isotope ratio mass spectrometry for atomic ions: sample preparation and ionization, and reducing the physical size of a fieldable mass spectrometer. PNNL is seeking simple and robust techniques that could be effectively used by inspectors who may have no expertise in analytical MS. In this report, we present and describe the preliminary findings for three candidate

  5. A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS.

    Science.gov (United States)

    Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas

    2017-03-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

  6. Core-shell hybrid liposomal vesicles loaded with panax notoginsenoside: preparation, characterization and protective effects on global cerebral ischemia/reperfusion injury and acute myocardial ischemia in rats

    OpenAIRE

    Zhang J.; Han XZ; Li X.; Luo Y; Zhao HP; Yang M.; Ni B; Liao ZG

    2012-01-01

    Jing Zhang,1,* Xizhen Han,1,* Xiang Li,2 Yun Luo,1 Haiping Zhao,1 Ming Yang,1 Bin Ni,1 Zhenggen Liao11Key Laboratory of Modern Preparation of TCM, Ministry of Education, 2National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine, Jiangxi University of Traditional Chinese Medicine, Nanchang, People's Republic of China*These authors contributed equally to this workPurpose: Novel panax notoginsenoside-loaded core-shell hybrid liposomal vesicles (PNS-HLV)...

  7. Preparation of edible wild fruit and plant samples for analysis and some difficulties encountered in such analyses

    CSIR Research Space (South Africa)

    Strydom, ESP

    1969-12-01

    Full Text Available Freeze-dried samples are used for analysis and the methods of preparation of samples for freeze-drying are discussed. Freeze-drying has obvious advantages but has also a few minor disadvantages. Difficulties encountered in the determination of some...

  8. Selectivity in the sample preparation for the analysis of drug residues in products of animal origin using LC-MS

    NARCIS (Netherlands)

    Berendsen, B.J.A.; Stolker, A.A.M.; Nielen, M.W.F.

    2013-01-01

    Sample preparation is critical in relation to analysis time, sample throughput and therefore analysis costs. Due to recent advances in liquid chromatography-mass spectrometry (LC-MS) instrumentation, the detection of many compounds within one run became possible, and methods for the simultaneous ana

  9. New Sample Preparation Method for Quantification of Phenolic Compounds of Tea (Camellia sinensis L. Kuntze: A Polyphenol Rich Plant

    Directory of Open Access Journals (Sweden)

    P. A. Nimal Punyasiri

    2015-01-01

    Full Text Available Chemical analysis of the Sri Lankan tea (Camellia sinensis, L. germplasm would immensely contribute to the success of the tea breeding programme. However, the polyphenols, particularly catechins (flavan-3-ols, are readily prone to oxidation in the conventional method of sample preparation. Therefore, optimization of the present sample preparation methodology for the profiling of metabolites is much important. Two sample preparation methodologies were compared, fresh leaves (as in the conventional procedures and freeze-dried leaves (a new procedure, for quantification of major metabolites by employing two cultivars, one is known to be high quality black tea and the other low quality black tea. The amounts of major metabolites such as catechins, caffeine, gallic acid, and theobromine, recorded in the new sampling procedure via freeze-dried leaves, were significantly higher than those recorded in the conventional sample preparation procedure. Additionally new method required less amount of leaf sample for analysis of major metabolites and facilitates storage of samples until analysis. The freeze-dried method would be useful for high throughput analysis of large number of samples in shorter period without chemical deterioration starting from the point of harvest until usage. Hence, this method is more suitable for metabolite profiling of tea as well as other phenol rich plants.

  10. CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.13)

    Science.gov (United States)

    The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

  11. CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.13)

    Science.gov (United States)

    The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

  12. Evaluation of PCR, DNA hybridization and immunomagnetic separation - PCR for detection of Burkholderia mallei in artificially inoculated environmental samples.

    Science.gov (United States)

    Merwyn, S; Kumar, S; Agarwal, G S; Rai, G P

    2010-06-01

    Glanders is highly contagious disease of equines, caused by Burkholderia mallei. The disease though rare, can be transmitted to humans. Here, we report a strategy for rapid detection of B. mallei from environmental samples. Different bacteriological media were evaluated and brain heart infusion broth medium with selective supplements (BHIB-SS) of penicillin (200 U/ml) and crystal violet (1:10,00000) was found to support the maximum growth of B. mallei even in the presence of other bacteria like Escherichia coli and Staphylococcus aureus. A polymerase chain reaction (PCR) and a DNA hybridization method was standardized for 823 bp specific dNA sequence of B. mallei. To enable the quicker and direct enrichment of B. mallei bacteria from environmental samples, an immunomagnetic separation (IMS) method was also standardized. Water, husk, grass and gram samples were artificially contaminated by B. mallei bacteria and after enrichment of B. mallei in BHIB-SS, detection was carried out by PCR and DNA hybridization. PCR was found to be a better method of the two with a detection limit of 10(4)-10(6) CFU/ml (6 h enrichment in BHIB-SS) in water and other particulate matrices. Detection by PCR in the above samples without enrichment in BHIBSS was carried out following IMS where the detection limit was about 1-2 log higher than PCR following enrichment in BHIB-SS. We recommend PCR for 823 bp for detection of B. mallei from environmental samples either following enrichment in BHIB-SS or IMS. IMS-PCR method may be preferred in situations where numbers of B. mallei bacteria are expected to be high and results are required in short time.

  13. A hybrid solution using computational prediction and measured data to accurately determine process corrections with reduced overlay sampling

    Science.gov (United States)

    Noyes, Ben F.; Mokaberi, Babak; Mandoy, Ram; Pate, Alex; Huijgen, Ralph; McBurney, Mike; Chen, Owen

    2017-03-01

    Reducing overlay error via an accurate APC feedback system is one of the main challenges in high volume production of the current and future nodes in the semiconductor industry. The overlay feedback system directly affects the number of dies meeting overlay specification and the number of layers requiring dedicated exposure tools through the fabrication flow. Increasing the former number and reducing the latter number is beneficial for the overall efficiency and yield of the fabrication process. An overlay feedback system requires accurate determination of the overlay error, or fingerprint, on exposed wafers in order to determine corrections to be automatically and dynamically applied to the exposure of future wafers. Since current and future nodes require correction per exposure (CPE), the resolution of the overlay fingerprint must be high enough to accommodate CPE in the overlay feedback system, or overlay control module (OCM). Determining a high resolution fingerprint from measured data requires extremely dense overlay sampling that takes a significant amount of measurement time. For static corrections this is acceptable, but in an automated dynamic correction system this method creates extreme bottlenecks for the throughput of said system as new lots have to wait until the previous lot is measured. One solution is using a less dense overlay sampling scheme and employing computationally up-sampled data to a dense fingerprint. That method uses a global fingerprint model over the entire wafer; measured localized overlay errors are therefore not always represented in its up-sampled output. This paper will discuss a hybrid system shown in Fig. 1 that combines a computationally up-sampled fingerprint with the measured data to more accurately capture the actual fingerprint, including local overlay errors. Such a hybrid system is shown to result in reduced modelled residuals while determining the fingerprint, and better on-product overlay performance.

  14. A lab-on-a-chip system with integrated sample preparation and loop-mediated isothermal amplification for rapid and quantitative detection of Salmonella spp. in food samples

    DEFF Research Database (Denmark)

    Sun, Yi; Than Linh, Quyen; Hung, Tran Quang

    2015-01-01

    and usually take a few hours to days to complete. In response to the demand for rapid on line or at site detection of pathogens, in this study, we describe for the first time an eight-chamber lab-on-a-chip (LOC) system with integrated magnetic beads-based sample preparation and loop-mediated isothermal...

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

    Science.gov (United States)

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

    2002-03-01

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

  16. Demonstration of a frozen sample aliquotter to prepare plasma and serum aliquots without thawing frozen parent samples.

    Science.gov (United States)

    Ellis, Helena Judge; Venturini, Deborah S

    2013-06-01

    Human biospecimens represent invaluable resources to advance molecular medicine, epidemiology, and biomarker discovery/validation, among other biomedical research. Biobanks typically cryopreserve biospecimens to safeguard their biochemical composition. However, exposing specimens repeatedly to freeze/thaw cycles can degrade their integrity in unforeseen ways. Those biobanks storing liquid samples, thus, regularly make a fundamental compromise at collection time between freezing samples in many small volumes (e.g., 0.5 mL or smaller) or in fewer, larger volumes (e.g., 1.8 mL). The former eliminates the need to expose samples to repeated freeze/thaw cycling, although increasing up-front labor costs, consumables used, and cold storage space requirements. The latter decreases up-front labor costs, consumables, and cold storage requirements, yet exposes samples repeatedly to damaging freeze/thaw cycles when smaller aliquots are needed for analysis. The Rhode Island BioBank at Brown University (RIBB) thoroughly evaluated the performance of an original technology that minimizes a sample's exposure to freeze/thaw cycling by enabling the automated extraction of frozen aliquots from one single frozen parent sample without thawing it. A technology that eliminates unnecessary sample exposures to freeze/thaw cycles could help protect sample integrity, extend its useful life, and effectively rectify and eliminate the aforementioned need to compromise. This report presents the results of the evaluation, and conclusively demonstrates the technology's ability to extract multiple uniform frozen aliquots from a single cryotube of never-thawed frozen human plasma, which faithfully represent the parent sample when analyzed for typical biochemical analytes, showing a coefficient of variability lower than 5.5%.

  17. Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Takayama, Yuki; Nakasako, Masayoshi [Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Mikaduki, Sayo, Hyogo 679-5148 (Japan)

    2012-05-15

    Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

  18. Rapid Preparation Methods of Biological Samples for Ionic Compounds Using Ion Exchange Type Monolithic Silica Spin Column

    OpenAIRE

    宮崎, 将太; 山田, 智子; 太田, 茂徳; 斉藤, 剛; 奈女良, 昭; 大平, 真義

    2010-01-01

    We developed a device comprising a spin column packed with ion exchange type (SCX and SAX) monolithic silica for extracting ionic compounds from biological samples. The methods involving the use of these spin column are not useful for the extraction of ionic analytes, but are highly reproducible for the analysis in serum and urine. This spin column enabled sample preparation in less than 10 min. Handling such as sample loading, washing, and elution of analytes, was exhibited by the centrifuga...

  19. Quality analysis of salmon calcitonin in a polymeric bioadhesive pharmaceutical formulation: sample preparation optimization by DOE.

    Science.gov (United States)

    D'Hondt, Matthias; Van Dorpe, Sylvia; Mehuys, Els; Deforce, Dieter; DeSpiegeleer, Bart

    2010-12-01

    A sensitive and selective HPLC method for the assay and degradation of salmon calcitonin, a 32-amino acid peptide drug, formulated at low concentrations (400 ppm m/m) in a bioadhesive nasal powder containing polymers, was developed and validated. The sample preparation step was optimized using Plackett-Burman and Onion experimental designs. The response functions evaluated were calcitonin recovery and analytical stability. The best results were obtained by treating the sample with 0.45% (v/v) trifluoroacetic acid at 60 degrees C for 40 min. These extraction conditions did not yield any observable degradation, while a maximum recovery for salmon calcitonin of 99.6% was obtained. The HPLC-UV/MS methods used a reversed-phase C(18) Vydac Everest column, with a gradient system based on aqueous acid and acetonitrile. UV detection, using trifluoroacetic acid in the mobile phase, was used for the assay of calcitonin and related degradants. Electrospray ionization (ESI) ion trap mass spectrometry, using formic acid in the mobile phase, was implemented for the confirmatory identification of degradation products. Validation results showed that the methodology was fit for the intended use, with accuracy of 97.4+/-4.3% for the assay and detection limits for degradants ranging between 0.5 and 2.4%. Pilot stability tests of the bioadhesive powder under different storage conditions showed a temperature-dependent decrease in salmon calcitonin assay value, with no equivalent increase in degradation products, explained by the chemical interaction between salmon calcitonin and the carbomer polymer.

  20. Use of hybrid composite particles prepared using alkoxysilane-functionalized amphiphilic polymer precursors for simultaneous removal of various pollutants from water.

    Science.gov (United States)

    Cho, Seulki; Kim, Nahae; Lee, Soonjae; Lee, Hoseok; Lee, Sang-Hyup; Kim, Juyoung; Choi, Jae-Woo

    2016-08-01

    In this study, we present new inorganic-organic hybrid particles and their possible application as an adsorbent for simultaneous removal of hydrophobic and hydrophilic pollutants from water. These hybrid particles were prepared using tailor-made alkoxysilane-functionalized amphiphilic polymer precursors (M-APAS), which have amphiphilic polymers and reactive alkoxysilane groups attached to the same backbone. Through a single conventional sol-gel process, the polymerization of M-APAS and the chemical conjugation of M-APAS onto silica nanoparticles was simultaneous, resulting in the formation of hybrid particles (M-APAS-SiO2) comprised of hyperbranch-like amphiphilic polymers bonded onto silica nanoparticles with a relatively high grafting efficiency. A test for the adsorption of water-soluble dye (organe-16) and water insoluble dye (solvent blue-35) onto the hybrid particles was performed to evaluate the possibility of adsorbing hydrophilic and hydrophobic compound within the same particle. The hybrid particle was also evaluated as an adsorbent for the removal of contaminated water containing various pollutants by wastewater treatment test. The hybrid particle could remove phenolic compounds from wastewater and the azo dye reactive orange-16 from aqueous solutions, and it was easily separated from the treated wastewater because of the different densities involved. These results demonstrate that the hybrid particles are a promising sorbent for hydrophilic and/or hydrophobic pollutants in water.

  1. Preparation and photocatalytic properties of hybrid core-shell reusable CoFe{sub 2}O{sub 4}-ZnO nanospheres

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, A. [Department of Physics, University of Memphis, Memphis, TN 38152 (United States); Mishra, S.R., E-mail: srmishra@memphis.edu [Department of Physics, University of Memphis, Memphis, TN 38152 (United States); Gupta, R.; Ghosh, K. [Department of Physics, Materials Science, and Astronomy, Missouri State University, Springfield, MO (United States)

    2012-08-15

    Magnetically separable and reusable core-shell CoFe{sub 2}O{sub 4}-ZnO photocatalyst nanospheres were prepared by the hydrothermal synthesis technique using glucose derived carbon nanospheres as the template. The morphology and the phase of core-shell hybrid structure of CoFe{sub 2}O{sub 4}-ZnO were assessed via TEM, SEM and XRD. The magnetic composite showed high UV photocatalytic activity for the degradation of methylene blue in water. The photocatalytic activity was found to be ZnO shell thickness dependent. Thicker ZnO shells lead to higher rate of photocatalytic activity. Hybrid nanospheres recovered using an external magnetic field demonstrated good repeatability of photocatalytic activity. These results promise the reusability of the hybrid nanospheres for photocatalytic activity. - Highlights: Black-Right-Pointing-Pointer Synthesis of novel hybrid magnetic-ZnO core-shell composite nanospheres. Black-Right-Pointing-Pointer High photocatalytic activity of hybrid nanospheres was noted as compared to that of pure ZnO nanoparticles. Black-Right-Pointing-Pointer The hybrid nanospheres could be easily retrieved using an external magnet for repeated use. Black-Right-Pointing-Pointer Repeated use of hybrid nanospheres did not show any degradation in the photocatalytic activity. Black-Right-Pointing-Pointer The photocatalysis rate was observed to be ZnO shell thickness dependent.

  2. Adjustable virtual pore-size filter for automated sample preparation using acoustic radiation force

    Energy Technology Data Exchange (ETDEWEB)

    Jung, B; Fisher, K; Ness, K; Rose, K; Mariella, R

    2008-05-22

    We present a rapid and robust size-based separation method for high throughput microfluidic devices using acoustic radiation force. We developed a finite element modeling tool to predict the two-dimensional acoustic radiation force field perpendicular to the flow direction in microfluidic devices. Here we compare the results from this model with experimental parametric studies including variations of the PZT driving frequencies and voltages as well as various particle sizes and compressidensities. These experimental parametric studies also provide insight into the development of an adjustable 'virtual' pore-size filter as well as optimal operating conditions for various microparticle sizes. We demonstrated the separation of Saccharomyces cerevisiae and MS2 bacteriophage using acoustic focusing. The acoustic radiation force did not affect the MS2 viruses, and their concentration profile remained unchanged. With optimized design of our microfluidic flow system we were able to achieve yields of > 90% for the MS2 with > 80% of the S. cerevisiae being removed in this continuous-flow sample preparation device.

  3. Dynamic simulation tools for the analysis and optimization of novel collection, filtration and sample preparation systems

    Energy Technology Data Exchange (ETDEWEB)

    Clague, D; Weisgraber, T; Rockway, J; McBride, K

    2006-02-12

    The focus of research effort described here is to develop novel simulation tools to address design and optimization needs in the general class of problems that involve species and fluid (liquid and gas phases) transport through sieving media. This was primarily motivated by the heightened attention on Chem/Bio early detection systems, which among other needs, have a need for high efficiency filtration, collection and sample preparation systems. Hence, the said goal was to develop the computational analysis tools necessary to optimize these critical operations. This new capability is designed to characterize system efficiencies based on the details of the microstructure and environmental effects. To accomplish this, new lattice Boltzmann simulation capabilities where developed to include detailed microstructure descriptions, the relevant surface forces that mediate species capture and release, and temperature effects for both liquid and gas phase systems. While developing the capability, actual demonstration and model systems (and subsystems) of national and programmatic interest were targeted to demonstrate the capability. As a result, where possible, experimental verification of the computational capability was performed either directly using Digital Particle Image Velocimetry or published results.

  4. Methodologies and perspectives of proteomics applied to filamentous fungi: from sample preparation to secretome analysis.

    Science.gov (United States)

    Bianco, Linda; Perrotta, Gaetano

    2015-03-12

    Filamentous fungi possess the extraordinary ability to digest complex biomasses and mineralize numerous xenobiotics, as consequence of their aptitude to sensing the environment and regulating their intra and extra cellular proteins, producing drastic changes in proteome and secretome composition. Recent advancement in proteomic technologies offers an exciting opportunity to reveal the fluctuations of fungal proteins and enzymes, responsible for their metabolic adaptation to a large variety of environmental conditions. Here, an overview of the most commonly used proteomic strategies will be provided; this paper will range from sample preparation to gel-free and gel-based proteomics, discussing pros and cons of each mentioned state-of-the-art technique. The main focus will be kept on filamentous fungi. Due to the biotechnological relevance of lignocellulose degrading fungi, special attention will be finally given to their extracellular proteome, or secretome. Secreted proteins and enzymes will be discussed in relation to their involvement in bio-based processes, such as biomass deconstruction and mycoremediation.

  5. Atmospheric pressure microwave sample preparation procedure for the combined analysis of total phosphorus and kjeldahl nitrogen.

    Science.gov (United States)

    Collins, L W; Chalk, S J; Kingston, H M

    1996-08-01

    An atmospheric pressure microwave digestion method has been developed for the combined analysis of total phosphorus and Kjeldahl nitrogen in complex matrices. In comparison to the digestion steps in EPA Methods 365.4 (total phosphorus) and 351.x (Kjeldahl nitrogen), this method requires less time, eliminates the need for a catalyst, and reduces the toxicity of the waste significantly. It employs a microwave-assisted digestion step, using refluxing borosilicate glass vessels at atmospheric pressure. Traditionally, this method has a time-consuming sample preparation step and generates toxic waste through the use of heavy metal catalysts. These advantages are gained by the combination of a high boiling point acid (sulfuric acid) and the application of focused microwave irradiation, which enhances the digestion process by direct energy coupling. NIST standard reference materials 1572 (citrus leaves), 1577a (bovine liver), and 1566 (oyster tissue) and tryptophan were analyzed to validate the method. Phosphorus concentrations were determined by the colorimetric ascorbic acid method outlined in EPA Method 365.3. Kjeldahl nitrogen concentrations were determined using EPA Method 351.1. The results of the analyses showed good precision and are in excellent agreement with the NIST published values for both elements.

  6. Preparation and characterization of functional material based on hybrid polymer composites

    Science.gov (United States)

    Agusu, La; Amiruddin; Taswito, Chen Chen; Herdianto; Zamrun, Muh.

    2016-08-01

    The microstructures and properties of hybrid polymer composites based on polyaniline (PANi)/γ-Fe2O3 nanoparticles/TiO2/carbon have been investigated for multifunctional applications such as heavy metal removal and initial study for radar absorbing material application. γ-Fe2O3 nanoparticles with spherical shape were synthetized by a coprecipitation method from iron sand. By activating the polyethylene glycol (PEG-400) coated carbon of coconut shell, the homogenous shape and size of carbon was achieved. Then, γ- Fe2O3, TiO2, and carbon were mixed with PANi by an in situ polymerization method at low temperature 0-5 oC. Characterization process involved XRD, SEM, FTIR, VSM, and DC conductivity measurements. For radar absorber application, the functionalized polymer composites showed good electrical conductivity 0.45 S/cm to absorb the incoming electromagnetic energy. An efficient and effective reduction of Pb2+ ion from the water has been achieved by using this material.

  7. Preparation and toxicological assessment of functionalized carbon nanotube-polymer hybrids.

    Directory of Open Access Journals (Sweden)

    Nikos D Koromilas

    Full Text Available Novel Carbon Nanotube-Polymer Hybrids were synthesized as potential materials for the development of membranes for water treatment applications in the field of Membrane Bioreactors (MBRs. Due to the toxicological concerns regarding the use of nanomaterials in water treatment as well as the rising demand for safe drinking water to protect public health, we studied the functionalization of MWCNTs and Thin-MWCNTs as to control their properties and increase their ability of embedment into porous anisotropic polymeric membranes. Following the growth of the hydrophilic monomer on the surface of the properly functionalized CNTs, that act as initiator for the controlled radical polymerization (ATRP of sodium styrene sulfonate (SSNa, the antimicrobial quaternized phosphonium and ammonium salts were attached on CNTs-g-PSSNa through non-covalent bonding. In another approach the covalent attachment of quaternized ammonium polymeric moieties of acrylic acid-vinyl benzyl chloride copolymers with N,N-dimethylhexadecylamine (P(AA12-co-VBCHAM on functionalized CNTs has also been attempted. Finally, the toxicological assessment in terms of cell viability and cell morphological changes revealed that surface characteristics play a major role in the biological response of functionalized CNTs.

  8. Spectral characterization of Compact Toroidal Hybrid plasmas in preparation for Thomson scattering measurements

    Science.gov (United States)

    Goforth, M. M.; Loch, S. D.; Maurer, D. A.; Pearce, A. J.; Traverso, P. J.

    2014-10-01

    A Thomson scattering system is in development for the Compact Toroidal Hybrid (CTH) experiment to provide localized, internal electron temperature and density measurements. Thomson scattering yields accurate information on the internal plasma electron pressure profile, which will aid in the equilibrium reconstruction of CTH plasmas using the V3FIT code. The expected Thomson scattered signal is approximately 1015 times less than the incident laser light, and can be overwhelmed by stray laser light, background plasma emission, and intrinsic detector noise. Background plasma emission measurements in the visible spectral region near the planned laser wavelength of 532 nm are underway using a Holospec f/1.8 spectrometer and an And or iStar image intensified CCD camera to quantify line and continuum background levels. In addition, impurity line identification and plans for a separate line-of-sight averaged impurity temperature and density measurement capability employing the Thomson spectrometer are in progress. This work is supported by US DOE Grant DE-FG-02-00ER54610 and by the Auburn University Undergraduate Research Fellowship.

  9. Preparation and Photochromic Behavior of Novel Hybrid Inorganic-Organic Thin Film

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A novel photochromic complex comprising of Keggin type tungstophosphate acid (PW12) and polyacrylamide (PAM) was prepared. FT-IR results showed that the Keggin geometry of PW12 was still preserved inside the composite, and a charge-transfer bridge was built between PW12 and PAM via hydrogen bond. AFM images indicated that surface topography of polymer matrix changed after adding PW12. Under UV irradiation, the film was reduced photochemically to yield a blue species, which was reversible in the present of oxygen in polymeric network.

  10. Preparation of Poly (ethylene oxide) (PEO) Modified Tungsten Oxide Hybrid Films via Sol-Gel Processing

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Poly (ethylene axide) (PEO) modified WO3 thin films were prepared on glass substrates with special temperature.The sol-gel transition proess was investigated by using DTA-TG,SEM and XRD.The electrochemical characteristic of the films was studied by cyclic voltmmetry measurement.The results show that PEO has heavy effects on the crystallization of WO3 during structure evolution because of the interaction between PEO and WO3.It increases the crystallization temperature of the gels and thus improves the electrochemical properties and cyclic life of WO3 film as electrochromic materials.

  11. A green method for the preparation of fluorescent hybrid structures of gold and corrole

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Ângela S., E-mail: aspereira@ua.pt; Barata, Joana F. B. [University of Aveiro, CICECO – Chemistry Department, Aveiro Institute of Materials (Portugal); Vaz Serra, Vanda I. R. C. [University of Aveiro, QOPNA Chemistry Department (Portugal); Pereira, Sérgio; Trindade, Tito [University of Aveiro, CICECO – Chemistry Department, Aveiro Institute of Materials (Portugal)

    2015-10-15

    Gold/soap nanostructures were prepared by a green methodology using saponified household sunflower oil, as reducing and organic dispersing agent of auric acid. The incorporation of hydrophobic molecules on the novel water-soluble gold nanoparticles was followed by fluorescence lifetime imaging microscopy, using as model hydrophobic compound 5,10,15-tris-(pentafluorophenyl)corrolatogallium(III)(pyridine) (GaPFC), a highly fluorescent corrole. The results showed the hydrophobic GaPFC located between the organic bilayer surrounding several Au nanoparticles, which in turn were coated with fatty acids salts anchored by the double bond at the gold’s surface.

  12. Preparation of hydroxyapatite/poly(lactic acid) hybrid microparticles for local drug delivery

    Science.gov (United States)

    Loca, D.; Locs, J.; Berzina-Cimdina, L.

    2013-12-01

    Calcium phosphate (CaP) bioceramic is well known as bioactive and biocompatible material in bone tissue regeneration applications. Apatitic CaP, especially nano sized hydroxyapatite (NHAp), is more similar to the natural apatite presented in the bone tissue than CaP bioceramics. In the current research NHAp was modified using biodegradable polymer - poly(lactic acid) (PLA) to develop composites providing bone regeneration and local drug delivery. NHAp/PLA microcapsules were prepared using solid-in-water-in-oil-in-water (s/w1/o/w2) encapsulation technology. The impact of primary and secondary emulsion stability on the emulsion droplet and microparticle properties was evaluated. The stability of final emulsion can be increased by varying the process parameters. Stable s/w1/o/w2 emulsion using 3ml of NHAp suspension, not less than 100ml of 4% PVA water solution and 10ml of 10% PLA solution in dichloromethane can be obtained. S/w1/o/w2 microencapuslation method can be effectively used for the preparation of multi-domain microcapsules achieving high NHAp encapsulation efficacy (93%).

  13. Organic-inorganic Hybrids Towards the Preparation of Nanoporous Composite Thin Films for Microelectronic Application

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Silicon containing materials have traditionally been used in microelectronic fabrication. Semiconductor devices often have one or more arrays of patterned interconnect levels that serve to electrically couple the individual circuit elements forming an integrated circuit. These interconnect levels are typically separated by an insulating or dielectric film. Previously, a silicon oxide film was the most commonly used material for such dielectric films having dielectric constants(k) near 4. 0. However, as the feature size is continuously scaling down, the relatively high k of such silicon oxide films became inadequate to provide efficient electrical insulation. As such, there has been an increasing market demand for materials with even lower dielectric constant for Interlayer Dielectric (ILD) applications, yet retaining thermal and mechanical integrity. We wish to report here our investigations on the preparation of ultra-low k ILD materials using a sacrificial approach whereby organic groups are burnt out to generate low k porous ORMOSIL films. We have been able to prepare a variety of organically modified silicone resins leading to highly microporous thin films, exhibiting ultra-low k from 1.80 to 2.87, and good to high modulus, 1.5 to 5.5 Gpa. Structure property influences on porosity, dielectric constant and modulus will be discussed.

  14. Development of a sample preparation procedure for the simultaneous determination of Np and Pu in clay samples

    Energy Technology Data Exchange (ETDEWEB)

    Renz, Tobias; Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Bauer, Andreas; Geckeis, Horst [INE, KIT, Eggenstein-Leopoldshafen (Germany); Taubald, Heinrich [Eberhard Karls Universitaet, Tuebingen (Germany)

    2015-07-01

    Neptunium (Np) and plutonium (Pu) are two key radionuclides for the long-term disposal of nuclear waste. Within this context Opalinus Clay formations are considered as a potential location for disposal of high-level radioactive waste. In the framework of experiments studying the diffusion behavior and retention of actinides under repository conditions, the present work focuses on the development of an analytical-chemical procedure for the determination of Np and Pu in clay (or clay-rich soil) samples. The procedure aims at the simultaneous determination of Np and Pu at femto- to attogram levels with AMS. Fields of application are the investigation of global fallout actinides in environmental clay-rich samples or the diffusion behavior of actinides in compacted clay liners used as technical barriers in nuclear waste repositories. Clay samples are spiked with certified standards of Pu-242 and Np-237. The analytical method, including a) leaching of the spiked clay samples, b) redox adjustments of Np and Pu, c) chromatographic separation of Np and Pu from the sample matrix and d) measurement of the actinides with Sector Field (SF)-ICP-MS will be presented. The suitability of a Pu isotope as non-isotopic tracer for determination of Np-237 is evaluated by determining the chemical yield using SF-ICP-MS.

  15. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Directory of Open Access Journals (Sweden)

    Christina Schreier

    2013-01-01

    Full Text Available Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after 1H NMR spectroscopy. Results. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at −20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Conclusion. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  16. Reproducibility of NMR analysis of urine samples: impact of sample preparation, storage conditions, and animal health status.

    Science.gov (United States)

    Schreier, Christina; Kremer, Werner; Huber, Fritz; Neumann, Sindy; Pagel, Philipp; Lienemann, Kai; Pestel, Sabine

    2013-01-01

    Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining (1)H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after (1)H NMR spectroscopy. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at -20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  17. Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

    Science.gov (United States)

    Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

    2014-05-01

    MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

  18. Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

    Science.gov (United States)

    Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

    2016-04-01

    We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents.

  19. Automated Gel Size Selection to Improve the Quality of Next-generation Sequencing Libraries Prepared from Environmental Water Samples.

    Science.gov (United States)

    Uyaguari-Diaz, Miguel I; Slobodan, Jared R; Nesbitt, Matthew J; Croxen, Matthew A; Isaac-Renton, Judith; Prystajecky, Natalie A; Tang, Patrick

    2015-04-17

    Next-generation sequencing of environmental samples can be challenging because of the variable DNA quantity and quality in these samples. High quality DNA libraries are needed for optimal results from next-generation sequencing. Environmental samples such as water may have low quality and quantities of DNA as well as contaminants that co-precipitate with DNA. The mechanical and enzymatic processes involved in extraction and library preparation may further damage the DNA. Gel size selection enables purification and recovery of DNA fragments of a defined size for sequencing applications. Nevertheless, this task is one of the most time-consuming steps in the DNA library preparation workflow. The protocol described here enables complete automation of agarose gel loading, electrophoretic analysis, and recovery of targeted DNA fragments. In this study, we describe a high-throughput approach to prepare high quality DNA libraries from freshwater samples that can be applied also to other environmental samples. We used an indirect approach to concentrate bacterial cells from environmental freshwater samples; DNA was extracted using a commercially available DNA extraction kit, and DNA libraries were prepared using a commercial transposon-based protocol. DNA fragments of 500 to 800 bp were gel size selected using Ranger Technology, an automated electrophoresis workstation. Sequencing of the size-selected DNA libraries demonstrated significant improvements to read length and quality of the sequencing reads.

  20. Synthesis and structural characterization of polyoxometalates incorporating with anilinium cations and facile preparation of hybrid film

    Science.gov (United States)

    Fukaya, Keisuke; Srifa, Atthapon; Isikawa, Eri; Naruke, Haruo

    2010-08-01

    The self-assembly reaction of tungstate and copper(II) in the presence of aniline (ANI) and phosphoric acid led to the formation of an anilinium (ANIH +) salt of mono-substituted Keggin-type polyoxotungstophosphate (ANIH) 5[PCu(H 2O)W 11O 39](ANI)·8H 2O ( 1), while the reaction of heptamolybdate in the coexistence of copper(II), phosphoric acid and ANI yielded an ANIH + salt of Strandberg-type pentamolybdodiphosphate, (ANIH) 2[(PO 4) 2Mo 5O 15{Cu(ANI) 2(H 2O)} 2](ANI)·2H 2O ( 2). These compounds were characterized by elemental analysis, infrared spectroscopy and X-ray single-crystal analysis. The compound 1, crystallizing in trigonal, P3¯,a = 13.883(4), c = 10.187(3) Å, Z = 1, consists of copper mono-substituted Keggin-typed [PCu(H 2O)W 11O 39] 5- anion surrounded by six ANI molecules, of which five are protonated (ANIH +). The compound 2, crystallizing in triclinic, P1¯,a = 13.98(2), b = 14.73(1), c = 16.24(1) Å, α = 111.27(3), β = 97.42(3), γ = 99.54(4)°, Z = 2, consists of Strandberg-type pentamolybdodiphospate [(PO 4) 2Mo 5O 15] 6- anions interconnected by two Cu(ANI) 2(H 2O) linkers to form a 1D-chain structure. A potentiostatic electrolysis of 1 in aqueous solution gave rise to electropolymerization of the ANIH + cations (and ANI) and deposition with the [PCu(H 2O)W 11O 39] 5- anion on an ITO electrode, forming a nano-structured polyaniline/[PCu(H 2O)W 11O 39] 5- hybrid thin film.

  1. Preparation of lactoperoxidase incorporated hybrid nanoflower and its excellent activity and stability.

    Science.gov (United States)

    Altinkaynak, Cevahir; Yilmaz, Ismail; Koksal, Zeynep; Özdemir, Hasan; Ocsoy, Ismail; Özdemir, Nalan

    2016-03-01

    We report a green approach to synthesize lactoperoxidase (LPO) enzyme and metal ions hybrid nanoflowers (HNFs) and investigate mechanism underlying formation and enhanced catalytic activity and stability under different experimental parameters. The HNFs formed of LPO enzyme purified from bovine milk and copper ions (Cu(2+)) were synthesized at two different temperatures (+4 °C and 20 °C) in PBS (pH 7.4). The effects of experimental conditions, pH and storage temperatures, on the activity and stability of LPO-copper phosphate HNFs were evaluated using guaiacol as a substrate in the presence of hydrogen peroxide (H2O2). Optimum pHs were determined as pH 8 and pH 6 for LPO-copper phosphate HNF and free LPO, respectively. LPO-copper phosphate HNF has higher activity than free LPO at each pHs. Activities of LPO-copper phosphate HNF at pH 6 and pH 8 were calculated as 70.48 EU/mg, 107.23 EU/mg, respectively while free LPO shows 45.78 EU/mg and 30.12 EU/mg, respectively. Compared with free LPO, LPO-copper phosphate HNFs exhibited ∼160% and ∼360% increase in activities at pH 6 and pH 8, respectively. Additionally, LPO-copper phosphate HNFs displayed perfect reusability after six cycles. Finally, we demonstrated that LPO-copper phosphate HNFs can be utilized as a nanosensor for detection of dopamine and epinephrine.

  2. Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

    Science.gov (United States)

    Wang, Xuan; Ye, Nengsheng

    2017-09-04

    In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  3. An On-Target Desalting and Concentration Sample Preparation Protocol for MALDI-MS and MS/MS Analysis

    DEFF Research Database (Denmark)

    Zhang, Xumin; Wang, Quanhui; Lou, Xiaomin;

    2012-01-01

    2DE coupled with MALDI-MS is one of the most widely used and powerful analytic technologies in proteomics study. The MALDI sample preparation method has been developed and optimized towards the combination of simplicity, sample-cleaning, and sample concentration since its introduction. Here we...... present a protocol of the so-called Sample loading, Matrix loading, and on-target Wash (SMW) method which fulfills the three criteria by taking advantage of the AnchorChip™ targets. Our method is extremely simple and no pre-desalting or concentration is needed when dealing with samples prepared from 2DE....... The protocol is amendable for automation and would pave the road for high-throughput MALDI-MS or MS/MS-based proteomics studies with guaranteed sensitivity and high identification rate. The method has been successfully applied to mouse liver proteome study and so far has been employed in other proteome studies...

  4. Preparation, characterization and luminescent properties of dense nano-silica hybrids loaded with 1,8-naphthalic anhydride.

    Science.gov (United States)

    Wang, Jinpeng; Sun, Jihong; Li, Yuzhen; Wang, Feng

    2014-03-01

    Novel luminescent dense nano-silica hybrid materials (DNSS) modified with different amounts of (3-aminopropyl)triethoxysilane (APTES) and 1,8-naphthalic anhydride (NA) were successfully synthesized via two steps combined with post-grafting methods. Powder X-ray diffraction (XRD), N2-sorption analysis, Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), thermogravimetric analysis (TGA), photoluminescence (PL) spectroscopy and elemental analysis, as well as time-resolved decays were employed to characterize the resultant hybrid materials. The results revealed that luminescent organic molecules had been successfully loaded onto the amine-modified surface of nano-silica spheres. In addition, their fluorescence intensity and characteristic peak of emission spectra changed with increasing amount of APTES and NA additive. In particular, the characteristic peak showed a red shift from 390 to 450 nm, however, this was inconsistent with results calculated on the basis of the elemental analysis data, most probably because of the dispersion behaviors of NA molecules from the aggregating to the monolayer state. These observations demonstrated the existence of a quantum confinement effectiveness of NA-DNSS samples, and therefore a possible mechanism was put forward.

  5. Hybrid Ant Bee Algorithm for Fuzzy Expert System Based Sample Classification.

    Science.gov (United States)

    GaneshKumar, Pugalendhi; Rani, Chellasamy; Devaraj, Durairaj; Victoire, T Aruldoss Albert

    2014-01-01

    Accuracy maximization and complexity minimization are the two main goals of a fuzzy expert system based microarray data classification. Our previous Genetic Swarm Algorithm (GSA) approach has improved the classification accuracy of the fuzzy expert system at the cost of their interpretability. The if-then rules produced by the GSA are lengthy and complex which is difficult for the physician to understand. To address this interpretability-accuracy tradeoff, the rule set is represented using integer numbers and the task of rule generation is treated as a combinatorial optimization task. Ant colony optimization (ACO) with local and global pheromone updations are applied to find out the fuzzy partition based on the gene expression values for generating simpler rule set. In order to address the formless and continuous expression values of a gene, this paper employs artificial bee colony (ABC) algorithm to evolve the points of membership function. Mutual Information is used for idenfication of informative genes. The performance of the proposed hybrid Ant Bee Algorithm (ABA) is evaluated using six gene expression data sets. From the simulation study, it is found that the proposed approach generated an accurate fuzzy system with highly interpretable and compact rules for all the data sets when compared with other approaches.

  6. Preparation

    Directory of Open Access Journals (Sweden)

    M.M. Dardir

    2014-03-01

    Full Text Available Some hexanamide-mono and di-linoleniate esters were prepared by the reaction of linolenic acid and hexanamide (derived from the reaction of hexanoic acid and diethanolamine. The chemical structure for the newly prepared hexanamide-mono and di-linoleniate esters were elucidated using elemental analysis, (FTIR, H 1NMR and chemical ionization mass spectra (CI/Ms spectroscopic techniques. The results of the spectroscopic analysis indicated that they were prepared through the right method and they have high purity. The new prepared esters have high biodegradability and lower toxicity (environmentally friendly so they were evaluated as a synthetic-based mud (ester-based mud for oil-well drilling fluids. The evaluation included study of the rheological properties, filtration and thermal properties of the ester based-muds formulated with the newly prepared esters compared to the reference commercial synthetic-based mud.

  7. Preparation and antifrictional properties of surface modified hybrid fluorine-containing silica particles

    Science.gov (United States)

    Gorbunova, T. I.; Zapevalov, A. Ya.; Beketov, I. V.; Demina, T. M.; Timoshenkova, O. R.; Murzakaev, A. M.; Gaviko, V. S.; Safronov, A. P.; Saloutin, V. I.

    2015-01-01

    Modified SiO2 particles were successfully prepared via [(perfluorobutyl)methyl]oxirane and [(perfluorobutyl)methyl]thiirane in sol-gel conditions using basic catalysis. As a result of acid catalysis non-modified nano-sized SiO2 particles were formed. Chemically modified SiO2 particles were characterized by means of FT-IR, BET, TEM, XRD- and XPS-analyses. Friction coefficients were determined at steel surface for base oil with modified SiO2 additives (5, 10 and 15 wt.%) at 10, 20, 30 and 60 N loads. Friction was reduced most strongly in the oil mix with the lowest content of the additive. A possible mechanism of antifrictional improvement is the formation of boundary lubrication layers containing iron salts.

  8. Preparation of hydrazine functionalized polymer brushes hybrid magnetic nanoparticles for highly specific enrichment of glycopeptides.

    Science.gov (United States)

    Huang, Guang; Sun, Zhen; Qin, Hongqiang; Zhao, Liang; Xiong, Zhichao; Peng, Xiaojun; Ou, Junjie; Zou, Hanfa

    2014-05-07

    Hydrazide chemistry is a powerful technique in glycopeptides enrichment. However, the low density of the monolayer hydrazine groups on the conventional hydrazine-functionalized magnetic nanoparticles limits the efficiency of glycopeptides enrichment. Herein, a novel magnetic nanoparticle grafted with poly(glycidyl methacrylate) (GMA) brushes was fabricated via reversible addition-fragmentation chain transfer (RAFT) polymerization, and a large amount of hydrazine groups were further introduced to the GMA brushes by ring-opening the epoxy groups with hydrazine hydrate. The resulting magnetic nanoparticles (denoted as Fe3O4@SiO2@GMA-NHNH2) demonstrated the high specificity of capturing glycopeptides from a tryptic digest of the sample comprising a standard non-glycosylated protein bovine serum albumin (BSA) and four standard glycoproteins with a weight ratio of 50 : 1, and the detection limit was as low as 130 fmol. In the analysis of a real complex biological sample, the tryptic digest of hepatocellular carcinoma, 179 glycosites were identified by the Fe3O4@SiO2@GMA-NHNH2 nanoparticles, surpassing that of 68 glycosites by Fe3O4@SiO2-single-NHNH2 (with monolayer hydrazine groups on the surface). It can be expected that the magnetic nanoparticles modified with hydrazine functionalized polymer brushes via RAFT technique will improve the specificity and the binding capacity of glycopeptides from complex samples, and show great potential in the analysis of protein glycosylation in biological samples.

  9. Effect of the preparation procedure on the morphology of thin TiO₂ films and their device performance in small-molecule bilayer hybrid solar cells.

    Science.gov (United States)

    Unger, Eva L; Spadavecchia, Francesca; Nonomura, Kazuteru; Palmgren, Pål; Cappelletti, Giuseppe; Hagfeldt, Anders; Johansson, Erik M J; Boschloo, Gerrit

    2012-11-01

    Flat titanium dioxide films, to be used as the acceptor layer in bilayer hybrid solar cell devices, were prepared by spray-pyrolysis and by spin-casting. Both preparation methods resulted in anatase titania films with similar optical and electronic properties but considerably different film morphologies. Spray pyrolysis resulted in dense TiO₂ films grown onto and affected by the surface roughness of the underlying conducting glass substrates. The spin-casting preparation procedure resulted in nanoporous titania films. Hybrid solar cell devices with varying layer thickness of the small-molecule semiconducting dye TDCV-TPA were investigated. Devices built with spray-pyrolyzed titania substrates yielded conversion efficiencies up to 0.47%. Spin-cast titania substrates exhibited short circuits for thin dye layer thickness. For thicker dye layers the performance of these devices was up to 0.6% due to the higher interfacial area for charge separation of these nanoporous TiO₂ substrates.

  10. Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

    Science.gov (United States)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

    2012-01-01

    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  11. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nomura, Cassiana S. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil); Silva, Cintia S. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil); Nogueira, Ana R.A. [Embrapa Pecuaria Sudeste, CP 339, Sao Carlos, SP 13560-970 (Brazil); Oliveira, Pedro V. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil)]. E-mail: pvolivei@iq.usp.br

    2005-06-30

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 {mu}g of W + 200 {mu}g of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 {mu}g for Cu and 30 {mu}g for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg{sup -} {sup 1} and 128 mg kg{sup -} {sup 1}, respectively. The relative standard deviations were lower

  12. Evaluation of Electrospray as a Sample Preparation Tool for Electron Microscopic Investigations: Toward Quantitative Evaluation of Nanoparticles.

    Science.gov (United States)

    Mielke, Johannes; Dohányosová, Pavla; Müller, Philipp; López-Vidal, Silvia; Hodoroaba, Vasile-Dan

    2017-02-01

    The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension.

  13. Well-defined functional mesoporous silica/polymer hybrids prepared by an ICAR ATRP technique integrated with bio-inspired polydopamine chemistry for lithium isotope separation.

    Science.gov (United States)

    Liu, Yuekun; Liu, Xuegang; Ye, Gang; Song, Yang; Liu, Fei; Huo, Xiaomei; Chen, Jing

    2017-05-09

    Mesoporous silica/polymer hybrids with well-preserved mesoporosity were prepared by integrating the initiators for continuous activator regeneration (ICAR) atom transfer radical polymerization (ATRP) technique with the bio-inspired polydopamine (PDA) chemistry. By manipulating the auto-oxidative polymerization of dopamine, uniform PDA layers were deposited on the surfaces and pore walls of ordered mesoporous silicas (OMSs), thereby promoting the immobilization of ATRP initiators. Poly(glycidyl methacrylate) (PGMA) brushes were then grown from the OMSs by using the ICAR ATRP technique. The evolution of the mesoporous silica/polymer hybrids during synthesis, in terms of morphology, structure, surface and porous properties, was detailed. And, parameters influencing the controlled growth of polymer chains in the ICAR ATRP system were studied. Taking advantage of the abundant epoxy groups in the PGMA platform, post-functionalization of the mesoporous silica/polymer hybrids by the covalent attachment of macrocyclic ligands for the adsorptive separation of lithium isotopes was realized. Adsorption behavior of the functionalized hybrids toward lithium ions was fully investigated, highlighting the good selectivity, and effects of temperature, solvent and counter ions. The ability for lithium isotope separation was evaluated. A higher separation factor could be obtained in systems with softer counter anions and lower polarity solvents. More importantly, due to the versatility of the ICAR ATRP technique, combined with the non-surface specific PDA chemistry, the methodology established in this work would provide new opportunities for the preparation of advanced organic-inorganic porous hybrids for broadened applications.

  14. Metal-conductive polymer hybrid nanostructures: preparation and electrical properties of palladium-polyimidazole nanowires.

    Science.gov (United States)

    Al-Hinai, Mariam; Hassanien, Reda; Watson, Scott M D; Wright, Nicholas G; Houlton, Andrew; Horrocks, Benjamin R

    2016-03-04

    A simple, convenient method for the formation of hybrid metal/conductive polymer nanostructures is described. Polyimidazole (PIm) has been templated on λ-DNA via oxidative polymerisation of imidazole using FeCl3 to produce conductive PIm/DNA nanowires. The PIm/DNA nanowires were decorated with Pd (Pd/PIm/DNA) by electroless reduction of PdCl4(-2) with NaBH4 in the presence of PIm/DNA; the choice of imidazole was motivated by the potential Pd(II) binding site at the pyridinic N atom. The formation of PIm/DNA and the presence of metallic Pd on Pd/PIm/DNA nanowires were verified by FTIR, UV-vis and XPS spectroscopy techniques. AFM studies show that the nanowires have diameters in the range 5-45 nm with a slightly greater mean diameter (17.1 ± 0.75 nm) for the Pd-decorated nanowires than the PIm/DNA nanowires (14.5 ± 0.89 nm). After incubation for 24 h in the polymerisation solution, the PIm/DNA nanowires show a smooth, uniform morphology, which is retained after decoration with Pd. Using a combination of scanned conductance microscopy, conductive AFM and two-terminal measurements we show that both types of nanowire are conductive and that it is possible to discriminate different possible mechanisms of transport. The conductivity of the Pd/PIm/DNA nanowires, (0.1-1.4 S cm(-1)), is comparable to the PIm/DNA nanowires (0.37 ± 0.029 S cm(-1)). In addition, the conductance of Pd/PIm/DNA nanowires exhibits Arrhenius behaviour (E(a )= 0.43 ± 0.02 eV) as a function of temperature in contrast to simple Pd/DNA nanowires. These results indicate that although the Pd crystallites on Pd/PIm/DNA nanowires decorate the PIm polymer, the major current pathway is through the polymer rather than the Pd.

  15. Evaluation of a hybrid sampling train for measuring trace elements and identifying mercury species in combustion flue gas

    Energy Technology Data Exchange (ETDEWEB)

    Miller, S.F.; Wincek, R.T.; Miller, B.G.; Scaroni, A.W.

    1999-07-01

    The Environmental Protection Agency (EPA) initiated an information collection request (ICR) on January 1, 1999 for coal-fired electric utility steam generating units (>25 MW) to document mercury levels in their fuels and emissions. The issuance of an ICR generally precedes the implementation of regulatory action by the EPA. The EPA has designated the Modified Ontario Hydro Method for stack gas sampling to measure total, elemental and oxidized mercury. This recommendation is based on extensive work by the University of North Dakota Energy and Environmental Research Center (UNDEERC) in evaluating a series of methodologies for determining mercury speciation. EPA has also designed the Method 29 sampling train for the sampling and measurement of the other elements identified as HAP's, i.e. As, Be, Cd, Co, Mn, Ni, Pb, Sb, Se, and Hg. Extensive testing has shown that EPA Method 29 may not speciate mercury correctly; however, it may still be used to measure total mercury. Currently there are no emission restrictions on these elements from power plants, however studies are being conducted as to their health risk and environmental impact. The objective of the study is to evaluate a hybrid train consisting of components of both the Modified Ontario Hydro Method and Method 29 sampling trains. Both sampling procedures are very labor intensive and require time to develop sampling expertise. The various sample trains are being tested in a 20 million Btu/hr demonstration boiler and a 2 million Btu/hr research boiler using a variety of fuels and combustion conditions.

  16. Recovery of Salmonella from internally and externally