Synchrotron/crystal sample preparation

Science.gov (United States)

Johnson, R. Barry

1993-01-01

The Center for Applied Optics (CAO) of the University of Alabama in Huntsville (UAH) prepared this final report entitled 'Synchrotron/Crystal Sample Preparation' in completion of contract NAS8-38609, Delivery Order No. 53. Hughes Danbury Optical Systems (HDOS) is manufacturing the Advanced X-ray Astrophysics Facility (AXAF) mirrors. These thin-walled, grazing incidence, Wolter Type-1 mirrors, varying in diameter from 1.2 to 0.68 meters, must be ground and polished using state-of-the-art techniques in order to prevent undue stress due to damage or the presence of crystals and inclusions. The effect of crystals on the polishing and grinding process must also be understood. This involves coating special samples of Zerodur and measuring the reflectivity of the coatings in a synchrotron system. In order to gain the understanding needed on the effect of the Zerodur crystals by the grinding and polishing process, UAH prepared glass samples by cutting, grinding, etching, and polishing as required to meet specifications for witness bars for synchrotron measurements and for investigations of crystals embedded in Zerodur. UAH then characterized these samples for subsurface damage and surface roughness and figure.

Standard methods for sampling and sample preparation for gamma spectroscopy

International Nuclear Information System (INIS)

Taskaeva, M.; Taskaev, E.; Nikolov, P.

1993-01-01

The strategy for sampling and sample preparation is outlined: necessary number of samples; analysis and treatment of the results received; quantity of the analysed material according to the radionuclide concentrations and analytical methods; the minimal quantity and kind of the data needed for making final conclusions and decisions on the base of the results received. This strategy was tested in gamma spectroscopic analysis of radionuclide contamination of the region of Eleshnitsa Uranium Mines. The water samples was taken and stored according to the ASTM D 3370-82. The general sampling procedures were in conformity with the recommendations of ISO 5667. The radionuclides was concentrated by coprecipitation with iron hydroxide and ion exchange. The sampling of soil samples complied with the rules of ASTM C 998, and their sample preparation - with ASTM C 999. After preparation the samples were sealed hermetically and measured. (author)

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.

[Sample preparation and bioanalysis in mass spectrometry].

Science.gov (United States)

Bourgogne, Emmanuel; Wagner, Michel

2015-01-01

The quantitative analysis of compounds of clinical interest of low molecular weight (sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

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.

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.

Preparation and Characterization of Hybrid Nanocomposite of Polyacrylamide/Silica-Nanoparticles

Directory of Open Access Journals (Sweden)

Ahmad Rabiee

2013-01-01

Full Text Available Polyacrylamides are water soluble macromolecules. These polymers are widely used for flocculation, separation and treatment of solid-liquid phase materials. In this research, organic-inorganic hybrid of polyacrylamide/silica nanoparticle is prepared via radical polymerization. First, the silica nanoparticle surfaces were modified by 3-methacryloxypropyltrimethoxysilane as coupling agent using a sol-gel technique in aqueous media in acidic condition. Afterwards, the modified nanoparticles are copolymerized by acrylamide monomer in presence of a peroxide initiator during a free radical polymerization. The chemical structure of the prepared modified nano-silica as well as polyacrylamide nanocomposite was studied and confirmed by FTIR spectroscopy technique. The morphology of nanocomposite was investigated by scanning electron microscopy. The SEM micrograph showed that the surface of the composite did not display any phase separation. Nanoparticles distribution was investigated by SEM-EDX technique. The results showed a uniform distribution of particles throughout the polymer bulk. TEM analysis showed the presence of silica nanoparticles in bulk of polymer which is an indicative of suitable dispersion of nanoparticles. The thermal stability of hybrid nanocomosite with that of polyacrylamide was compared by TGA technique. The higher thermal stability of hybrid nanocomposite with respect to homopolymer is indicative of a reaction between the modified nanoparticles and polyacrylamide chain. The presence of silica particles in copolymer was also confirmed with EDX analysis in ash content of hybrid nanocomposite.

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.

Sample preparation guidelines for two-dimensional electrophoresis.

Science.gov (United States)

Posch, Anton

2014-12-01

Sample preparation is one of the key technologies for successful two-dimensional electrophoresis (2DE). Due to the great diversity of protein sample types and sources, no single sample preparation method works with all proteins; for any sample the optimum procedure must be determined empirically. This review is meant to provide a broad overview of the most important principles in sample preparation in order to avoid a multitude of possible pitfalls. Sample preparation protocols from the expert in the field were screened and evaluated. On the basis of these protocols and my own comprehensive practical experience important guidelines are given in this review. The presented guidelines will facilitate straightforward protocol development for researchers new to gel-based proteomics. In addition the available choices are rationalized in order to successfully prepare a protein sample for 2DE separations. The strategies described here are not limited to 2DE and can also be applied to other protein separation techniques.

Preparation and magnetic properties of anisotropic bulk MnBi/NdFeB hybrid magnets

International Nuclear Information System (INIS)

Ma, Y.L.; Liu, X.B.; Nguyen, V.V.; Poudyal, N.; Yue, M.; Liu, J.P.

2016-01-01

Anisotropic hybrid bulk magnets of MnBi/NdFeB with different composition ratio have been prepared with starting MnBi and Nd 2 Fe 14 B powders as well as epoxy resin as a binder in case it is needed to form bulk samples. It has been found that the ratio between the two phases in content has a remarkable influence on the magnetic properties, the thermal stability and the density of the bulk magnets. With increasing MnBi content the binder addition can be reduced. When the MnBi content is larger than 30 wt%, no binder is needed. On the other hand, the coercivity and saturation magnetization were increased significantly with increasing NdFeB content. When the NdFeB content was increased from 0% to 50%, the maximum energy product was enhanced from 4.7 to 10.0 MGOe, respectively. The energy product then decreased gradually with the NdFeB content due to the reduced density of the hybrid magnet. The thermal stability measurements showed that the temperature coefficient of coercivity grew with the MnBi content and became positive with MnBi=80 wt%. - Highlights: • Anisotropic bulk hybrid MnBi/NdFeB magnets were prepared. • MnBi content affected the density and coercivity temperature coefficient positively. • An energy product (BH) max of 10 MGOe was obtained at NdFeB content of 50 wt%.

Preparation and magnetic properties of anisotropic bulk MnBi/NdFeB hybrid magnets

Energy Technology Data Exchange (ETDEWEB)

Ma, Y.L. [Department of Physics, University of Texas at Arlington, Arlington, TX 76019 (United States); College of Metallurgical and Materials Engineering, Chongqing University of Science and Technology, Chongqing 401331 (China); Liu, X.B.; Nguyen, V.V.; Poudyal, N. [Department of Physics, University of Texas at Arlington, Arlington, TX 76019 (United States); Yue, M. [College of Materials Science and Engineering, Beijing University of Technology, Beijing 100124 (China); Liu, J.P., E-mail: pliu@uta.edu [Department of Physics, University of Texas at Arlington, Arlington, TX 76019 (United States)

2016-08-01

Anisotropic hybrid bulk magnets of MnBi/NdFeB with different composition ratio have been prepared with starting MnBi and Nd{sub 2}Fe{sub 14}B powders as well as epoxy resin as a binder in case it is needed to form bulk samples. It has been found that the ratio between the two phases in content has a remarkable influence on the magnetic properties, the thermal stability and the density of the bulk magnets. With increasing MnBi content the binder addition can be reduced. When the MnBi content is larger than 30 wt%, no binder is needed. On the other hand, the coercivity and saturation magnetization were increased significantly with increasing NdFeB content. When the NdFeB content was increased from 0% to 50%, the maximum energy product was enhanced from 4.7 to 10.0 MGOe, respectively. The energy product then decreased gradually with the NdFeB content due to the reduced density of the hybrid magnet. The thermal stability measurements showed that the temperature coefficient of coercivity grew with the MnBi content and became positive with MnBi=80 wt%. - Highlights: • Anisotropic bulk hybrid MnBi/NdFeB magnets were prepared. • MnBi content affected the density and coercivity temperature coefficient positively. • An energy product (BH){sub max} of 10 MGOe was obtained at NdFeB content of 50 wt%.

Preparation of dye waste-barium sulfate hybrid adsorbent and application in organic wastewater treatment.

Science.gov (United States)

Hu, Zhang-Jun; Xiao, Yan; Zhao, Dan-Hua; Shen, Yu-Lin; Gao, Hong-Wen

2010-03-15

A new hybrid material was developed by the template-free hybridization of weak acidic pink red B (APRB, C.I. 18073) with BaSO(4). The composition and structure of the material were determined and characterized. In contrast to conventional sorbents, the hybrid material has a specific surface area of 0.89 m(2)/g, but it contains lots of negative charges and lipophilic groups as the basis of specific adsorption. The efficient removal of cationic dyes and persistent organic pollutants (POPs) indicates that it has an improved adsorption capacity and selectivity with a short removal time less than 2 min; while the hybrid sorbents fit the Langmuir isotherm model, and follow the octanol-water partition law. Instead of using APRB reagent, an APRB-producing wastewater was reused to prepare the cost-effective sorbent, and the equilibrium adsorption capacities of which reached 222 and 160 mg/g for EV and BPR, respectively. The sorbents was then used to treat three wastewater samples with satisfactory results of over 97% decolonization and 88% COD-decreasing. In addition, the hybrid sorbent was regenerated from sludge over five cycles, and its adsorption capacity was not appreciably changed. This work has developed a simple and eco-friendly method for synthesizing a practical and efficient sorbent. (c) 2009 Elsevier B.V. All rights reserved.

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

International Nuclear Information System (INIS)

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

2015-01-01

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.

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.

Inorganic-organic hybrid polymer for preparation of affiliating material using electron beam irradiation

International Nuclear Information System (INIS)

Chung, Jaeseung; Kim, Seongeun; Kim, Byounggak; Lee, Jongchan; Park, Jihyun; Lee, Byeongcheol

2011-01-01

Recently, silver nano materials have gained a lot of attentions in a variety of applications due to the unique biological, optical, and electrical properties. Especially, the antifouling property of these material is considered to be an important character for biomedical field, marine coatings industry, biosensor, and drug delivery. In this study, we design and synthesize the inorganic-organic hybrid polymer for preparation of affiliating materials. Silver nano materials having antifouling property with different shapes are prepared by control the electron beam irradiation conditions. Inorganic-organic hybrid polymer was synthesized and characterized. → Morphology and size controlled nano materials are prepared using electron beam irradiation. → Silver nano materials having various shapes can be used for antifouling material

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

International Nuclear Information System (INIS)

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

2011-01-01

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.

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. Copyright © 2011 Elsevier B.V. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

Yang, Jiazhi; Yu, Junwei [Key Laboratory of Soft Chemistry and Functional Materials (Ministry of Education), Nanjing University of Science and Technology, Nanjing 210094 (China); Fan, Jun [School of Environment, Nanjing University, Nanjing 210093 (China); Sun, Dongping [Key Laboratory of Soft Chemistry and Functional Materials (Ministry of Education), Nanjing University of Science and Technology, Nanjing 210094 (China); Tang, Weihua [Key Laboratory of Soft Chemistry and Functional Materials (Ministry of Education), Nanjing University of Science and Technology, Nanjing 210094 (China); Yang, Xuejie [Key Laboratory of Soft Chemistry and Functional Materials (Ministry of Education), Nanjing University of Science and Technology, Nanjing 210094 (China)

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{sub 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.

Collection and preparation of samples for gamma spectrometry

International Nuclear Information System (INIS)

Pan Jingquan

1994-01-01

The paper presents the basic principles of sample collection and preparation: setting up unified sampling program, methods and procedures, sample packing, transportation and storage, determination of sample quantity, sample pretreatment and preparation of samples to be analysed, etc. for gamma spectrometry. And the paper also describes briefly the main methods and special issues of sampling and preparation for the same environmental and biological samples, such as, air, water, grass, soil and foods

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.

Microfluidic Sample Preparation for Diagnostic Cytopathology

Science.gov (United States)

Mach, Albert J.; Adeyiga, Oladunni B.; Di Carlo, Dino

2014-01-01

The cellular components of body fluids are routinely analyzed to identify disease and treatment approaches. While significant focus has been placed on developing cell analysis technologies, tools to automate the preparation of cellular specimens have been more limited, especially for body fluids beyond blood. Preparation steps include separating, concentrating, and exposing cells to reagents. Sample preparation continues to be routinely performed off-chip by technicians, preventing cell-based point-of-care diagnostics, increasing the cost of tests, and reducing the consistency of the final analysis following multiple manually-performed steps. Here, we review the assortment of biofluids for which suspended cells are analyzed, along with their characteristics and diagnostic value. We present an overview of the conventional sample preparation processes for cytological diagnosis. We finally discuss the challenges and opportunities in developing microfluidic devices for the purpose of automating or miniaturizing these processes, with particular emphases on preparing large or small volume samples, working with samples of high cellularity, automating multi-step processes, and obtaining high purity subpopulations of cells. We hope to convey the importance of and help identify new research directions addressing the vast biological and clinical applications in preparing and analyzing the array of available biological fluids. Successfully addressing the challenges described in this review can lead to inexpensive systems to improve diagnostic accuracy while simultaneously reducing overall systemic healthcare costs. PMID:23380972

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.

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.

Matrix removal in state of the art sample preparation methods for serum by charged aerosol detection and metabolomics-based LC-MS.

Science.gov (United States)

Schimek, Denise; Francesconi, Kevin A; Mautner, Anton; Libiseller, Gunnar; Raml, Reingard; Magnes, Christoph

2016-04-07

Investigations into sample preparation procedures usually focus on analyte recovery with no information provided about the fate of other components of the sample (matrix). For many analyses, however, and particularly those using liquid chromatography-mass spectrometry (LC-MS), quantitative measurements are greatly influenced by sample matrix. Using the example of the drug amitriptyline and three of its metabolites in serum, we performed a comprehensive investigation of nine commonly used sample clean-up procedures in terms of their suitability for preparing serum samples. We were monitoring the undesired matrix compounds using a combination of charged aerosol detection (CAD), LC-CAD, and a metabolomics-based LC-MS/MS approach. In this way, we compared analyte recovery of protein precipitation-, liquid-liquid-, solid-phase- and hybrid solid-phase extraction methods. Although all methods provided acceptable recoveries, the highest recovery was obtained by protein precipitation with acetonitrile/formic acid (amitriptyline 113%, nortriptyline 92%, 10-hydroxyamitriptyline 89%, and amitriptyline N-oxide 96%). The quantification of matrix removal by LC-CAD showed that the solid phase extraction method (SPE) provided the lowest remaining matrix load (48-123 μg mL(-1)), which is a 10-40 fold better matrix clean-up than the precipitation- or hybrid solid phase extraction methods. The metabolomics profiles of eleven compound classes, comprising 70 matrix compounds showed the trends of compound class removal for each sample preparation strategy. The collective data set of analyte recovery, matrix removal and matrix compound profile was used to assess the effectiveness of each sample preparation method. The best performance in matrix clean-up and practical handling of small sample volumes was showed by the SPE techniques, particularly HLB SPE. CAD proved to be an effective tool for revealing the considerable differences between the sample preparation methods. This detector can

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

OpenAIRE

Chiku, Masanobu; Tomita, Shoji; Higuchi, Eiji; Inoue, Hiroshi

2011-01-01

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.

Sequencing of real-world samples using a microfabricated hybrid device having unconstrained straight separation channels.

Science.gov (United States)

Liu, Shaorong; Elkin, Christopher; Kapur, Hitesh

2003-11-01

We describe a microfabricated hybrid device that consists of a microfabricated chip containing multiple twin-T injectors attached to an array of capillaries that serve as the separation channels. A new fabrication process was employed to create two differently sized round channels in a chip. Twin-T injectors were formed by the smaller round channels that match the bore of the separation capillaries and separation capillaries were incorporated to the injectors through the larger round channels that match the outer diameter of the capillaries. This allows for a minimum dead volume and provides a robust chip/capillary interface. This hybrid design takes full advantage, such as sample stacking and purification and uniform signal intensity profile, of the unique chip injection scheme for DNA sequencing while employing long straight capillaries for the separations. In essence, the separation channel length is optimized for both speed and resolution since it is unconstrained by chip size. To demonstrate the reliability and practicality of this hybrid device, we sequenced over 1000 real-world samples from Human Chromosome 5 and Ciona intestinalis, prepared at Joint Genome Institute. We achieved average Phred20 read of 675 bases in about 70 min with a success rate of 91%. For the similar type of samples on MegaBACE 1000, the average Phred20 read is about 550-600 bases in 120 min separation time with a success rate of about 80-90%.

Innovative methods for inorganic sample preparation

Energy Technology Data Exchange (ETDEWEB)

Essling, A.M.; Huff, E.A.; Graczyk, D.G.

1992-04-01

Procedures and guidelines are given for the dissolution of a variety of selected materials using fusion, microwave, and Parr bomb techniques. These materials include germanium glass, corium-concrete mixtures, and zeolites. Emphasis is placed on sample-preparation approaches that produce a single master solution suitable for complete multielement characterization of the sample. In addition, data are presented on the soil microwave digestion method approved by the Environmental Protection Agency (EPA). Advantages and disadvantages of each sample-preparation technique are summarized.

Innovative methods for inorganic sample preparation

International Nuclear Information System (INIS)

Essling, A.M.; Huff, E.A.; Graczyk, D.G.

1992-04-01

Procedures and guidelines are given for the dissolution of a variety of selected materials using fusion, microwave, and Parr bomb techniques. These materials include germanium glass, corium-concrete mixtures, and zeolites. Emphasis is placed on sample-preparation approaches that produce a single master solution suitable for complete multielement characterization of the sample. In addition, data are presented on the soil microwave digestion method approved by the Environmental Protection Agency (EPA). Advantages and disadvantages of each sample-preparation technique are summarized

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

Science.gov (United States)

Yu, Liang; Gong, Jie; Zeng, Changfeng; Zhang, Lixiong

2013-10-01

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(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(+)-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(2+)-exchanged hybrid composites was observed with the highest weight gain of 51.4% in 30 days. The 35 wt.% Ag(+)-exchanged hybrid composite showed the highest antimicrobial activity, which could reduce the 9×10(6) CFU mL(-1)E. coli concentration to zero within 4h of incubation time with the Ag(+)-exchanged hybrid composite amount of 0.4 g L(-1). The bioactivity and antimicrobial activity could be combined by ion-exchanging the composites first with Ca(2+) and then with Ag(+). These zeolite-A/chitosan hybrid composites have potential applications on tissue engineering and antimicrobial food packaging. Copyright © 2013 Elsevier B.V. All rights reserved.

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

Science.gov (United States)

Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

2004-01-01

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

Newly introduced sample preparation techniques: towards miniaturization.

Science.gov (United States)

Costa, Rosaria

2014-01-01

Sampling and sample preparation are of crucial importance in an analytical procedure, representing quite often a source of errors. The technique chosen for the isolation of analytes greatly affects the success of a chemical determination. On the other hand, growing concerns about environmental and human safety, along with the introduction of international regulations for quality control, have moved the interest of scientists towards specific needs. Newly introduced sample preparation techniques are challenged to meet new criteria: (i) miniaturization, (ii) higher sensitivity and selectivity, and (iii) automation. In this survey, the most recent techniques introduced in the field of sample preparation will be described and discussed, along with many examples of applications.

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.

Preparation and Characterization of Graphene-Based Magnetic Hybrid Nano composite

International Nuclear Information System (INIS)

Jashiela Wani Jusin; Madzlan Aziz

2016-01-01

Graphene-based magnetic hybrid nano composite has the advantage of exhibiting better performance as platform or supporting materials to develop novel properties of composite by increasing selectivity of the targeted adsorbate. The hybrid nano material was prepared by mixing and hydrolysing iron (II) and iron (III) salt precursors in the presence of GO dispersion through coprecipitation method followed by in situ chemical reduction of GO. The effect of weight loading ratio of Fe to GO (4:1, 2.5:1, 1:1 and 1:4) on structural properties of the hybrid nano materials was investigated. The presence of characteristic peaks in FTIR spectra indicated that GO has been successfully oxidized from graphite while the decrease in oxygenated functional groups and peaks intensity evidenced the formation of hybrid nano materials through the subsequent reduction process. The presence of characteristic peaks in XRD pattern denoted that magnetite nanoparticles disappeared at higher loading of GO. TEM micrograph showed that the best distribution of iron oxide particles on the surface of hybrid nano material occurred when the loading ratio of Fe to GO was fixed at 2:5 to 1. The reduced graphene oxide (RGO) sheets in the hybrid materials showed less wrinkled sheet like structure compared to GO due to exfoliation and reduction process during the synthesis. The layered morphology of GO degrades at higher concentrations of iron oxide. (author)

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.

Mechanochemical preparation of polydiphenylamine and its electrochemical performance in hybrid supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Palaniappan, SP. [Department of Industrial Chemistry, School of Chemistry, Alagappa University, Alagappapuram, Karaikudi 630003, Tamil Nadu (India); Manisankar, P., E-mail: pms11@rediffmail.com [Department of Industrial Chemistry, School of Chemistry, Alagappa University, Alagappapuram, Karaikudi 630003, Tamil Nadu (India)

2011-07-01

Highlights: > For the first time, a simple to adopt, greener, rapid and efficient alternative route was successfully developed for preparing different PDPA salts. > For the first time, a judicial attempt was made to evaluate the performance of mechanochemically prepared PDPA-H{sub 2}SO{sub 4} as cathode material in asymmetric hybrid supercapacitors. > The results obtained are highly promising and the physicochemical properties of PDPA salts could be fine-tuned in the future for large scale applications in energy storage devices. - Abstract: A simple mechanochemical route for the synthesis of high quality inorganic anion doped polydiphenylamines (PDPAs) is reported in this article. Elemental analysis performed for the PDPAs indicated the presence of dopant anions in the polymeric chain. PDPA prepared in the presence of 96 wt% H{sub 2}SO{sub 4} (PDPA-H{sub 2}SO{sub 4}) was found to be better doped than the other polymeric salts. Spectroscopic profiles of the polymers showed that the PDPAs were in a doped conducting state. The X-ray diffraction (XRD) pattern of the as-prepared polymeric powders revealed the presence of more crystalline phases in PDPA-H{sub 2}SO{sub 4}. Field emission scanning electron microscopic (FESEM) images highlighted the formation of inorganic anion doped PDPA particles with different sizes (80-100 nm). Electrochemical studies performed for the polymeric particles depicted the redox behavior and good electrochemical activity of PDPA salts. Thermogravimetric analysis (TGA)/differential thermal analysis (DTA) proved that all the PDPA salts were thermally stable up to 300 deg. C. The electrochemical performance of PDPA-H{sub 2}SO{sub 4} in hybrid supercapacitors was evaluated due to its superior physicochemical properties. The maximum specific capacitance of the hybrid supercapacitor constructed out of PDPA-H{sub 2}SO{sub 4} powder was found to be 108 F g{sup -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.

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.

Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis.

Science.gov (United States)

Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

2017-02-01

Sample preparation is considered to be the most challenging step of the analytical procedure, since it has an effect on the whole analytical methodology, therefore it contributes significantly to the greenness or lack of it of the entire process. The elimination of the sample treatment steps, pursuing at the same time the reduction of the amount of the sample, strong reductions in consumption of hazardous reagents and energy also maximizing safety for operators and environment, the avoidance of the use of big amount of organic solvents, form the basis for greening sample preparation and analytical methods. In the last decade, the development and utilization of greener and sustainable microextraction techniques is an alternative to classical sample preparation procedures. In this review, the main green microextraction techniques (solid phase microextraction, stir bar sorptive extraction, hollow-fiber liquid phase microextraction, dispersive liquid - liquid microextraction, etc.) will be presented, with special attention to bioanalytical applications of these environment-friendly sample preparation techniques which comply with the green analytical chemistry principles. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation of environmental samples using benzene synthesis followed by high-performance LSC

International Nuclear Information System (INIS)

Filippis, S. De; Noakes, J.E.

1991-01-01

Liquid scintillation counting (LSC) techniques have been widely employed as the detection method for determining environmental levels of tritium and 14 C. Since anthropogenic and nonanthropogenic inputs to the environment are a concern, sampling the environment surrounding a nuclear power facility or fuel reprocessing operation requires the collection of many different sample types, including agriculture products, water, biota, aquatic life, soil, and vegetation. These sample types are not suitable for the direct detection of tritium of 14 C for liquid scintillation techniques. Each sample type must be initially prepared in order to obtain the carbon or hydrogen component of interest and present this in a chemical form that is compatible with common chemicals used in scintillation counting applications. Converting the sample of interest to chemically pure benzene as a sample preparation technique has been widely accepted for processing samples for radiocarbon age-dating applications. The synthesized benzene is composed of the carbon or hydrogen atoms from the original sample and is ideal as a solvent for LSC with excellent photo-optical properties. Benzene synthesis followed by low-background scintillation counting can be applied to the preparation and measurement of environmental samples yielding good detection sensitivities, high radionuclide counting efficiency, and shorter preparation time. The method of benzene synthesis provides a unique approach to the preparation of a wide variety of environmental sample types using similar chemistry for all samples

Quantitative sample preparation of some heavy elements

International Nuclear Information System (INIS)

Jaffey, A.H.

1977-01-01

A discussion is given of some techniques that have been useful in quantitatively preparing and analyzing samples used in the half-life determinations of some plutonium and uranium isotopes. Application of these methods to the preparation of uranium and plutonium samples used in neutron experiments is discussed

7 CFR 27.21 - Preparation of samples of cotton.

Science.gov (United States)

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

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

KAUST Repository

Elsheikh, Ahmed H.; Wheeler, Mary Fanett; Hoteit, Ibrahim

2014-01-01

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

Sample preparation in alkaline media

International Nuclear Information System (INIS)

Nobrega, Joaquim A.; Santos, Mirian C.; Sousa, Rafael A. de; Cadore, Solange; Barnes, Ramon M.; Tatro, Mark

2006-01-01

The use of tetramethylammonium hydroxide, tertiary amines and strongly alkaline reagents for sample treatment involving extraction and digestion procedures is discussed in this review. The preparation of slurries is also discussed. Based on literature data, alkaline media offer a good alternative for sample preparation involving an appreciable group of analytes in different types of samples. These reagents are also successfully employed in tailored speciation procedures wherein there is a critical dependence on maintenance of chemical forms. The effects of these reagents on measurements performed using spectroanalytical techniques are discussed. Several undesirable effects on transport and atomization processes necessitate use of the method of standard additions to obtain accurate results. It is also evident that alkaline media can improve the performance of techniques such as inductively coupled plasma mass spectrometry and accessories, such as autosamplers coupled to graphite furnace atomic absorption spectrometers

Urine sample preparation for proteomic analysis.

Science.gov (United States)

Olszowy, Pawel; Buszewski, Boguslaw

2014-10-01

Sample preparation for both environmental and more importantly biological matrices is a bottleneck of all kinds of analytical processes. In the case of proteomic analysis this element is even more important due to the amount of cross-reactions that should be taken into consideration. The incorporation of new post-translational modifications, protein hydrolysis, or even its degradation is possible as side effects of proteins sample processing. If protocols are evaluated appropriately, then identification of such proteins does not bring difficulties. However, if structural changes are provided without sufficient attention then protein sequence coverage will be reduced or even identification of such proteins could be impossible. This review summarizes obstacles and achievements in protein sample preparation of urine for proteome analysis using different tools for mass spectrometry analysis. The main aim is to present comprehensively the idea of urine application as a valuable matrix. This article is dedicated to sample preparation and application of urine mainly in novel cancer biomarkers discovery. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthetic Strategies in the Preparation of Polymer/Inorganic Hybrid Nanoparticles

Science.gov (United States)

Hood, Matthew A.; Mari, Margherita; Muñoz-Espí, Rafael

2014-01-01

This article reviews the recent advances and challenges in the preparation of polymer/inorganic hybrid nanoparticles. We mainly focus on synthetic strategies, basing our classification on whether the inorganic and the polymer components have been formed in situ or ex situ, of the hybrid material. Accordingly, four types of strategies are identified and described, referring to recent examples: (i) ex situ formation of the components and subsequent attachment or integration, either by covalent or noncovalent bonding; (ii) in situ polymerization in the presence of ex situ formed inorganic nanoparticles; (iii) in situ precipitation of the inorganic components on or in polymer structures; and (iv) strategies in which both polymer and inorganic component are simultaneously formed in situ. PMID:28788665

Recent advances in applications of nanomaterials for sample preparation.

Science.gov (United States)

Xu, Linnan; Qi, Xiaoyue; Li, Xianjiang; Bai, Yu; Liu, Huwei

2016-01-01

Sample preparation is a key step for qualitative and quantitative analysis of trace analytes in complicated matrix. Along with the rapid development of nanotechnology in material science, numerous nanomaterials have been developed with particularly useful applications in analytical chemistry. Benefitting from their high specific areas, increased surface activities, and unprecedented physical/chemical properties, the potentials of nanomaterials for rapid and efficient sample preparation have been exploited extensively. In this review, recent progress of novel nanomaterials applied in sample preparation has been summarized and discussed. Both nanoparticles and nanoporous materials are evaluated for their unusual performance in sample preparation. Various compositions and functionalizations extended the applications of nanomaterials in sample preparations, and distinct size and shape selectivity was generated from the diversified pore structures of nanoporous materials. Such great variety make nanomaterials a kind of versatile tools in sample preparation for almost all categories of analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

Liquid scintillation: Sample preparation and counting atypical emissions

International Nuclear Information System (INIS)

Anon.

1991-01-01

Liquid scintillation sample preparation has the most published information but the least amount of definitive technical direction because the chemical and physical nature of the samples from biological investigations varies widely. This chapter discusses the following related topics: Aqueous Samples; Tissue Solubilizers; Absorption of 14 CO 2 ; Sample Combustion Methods; Heterogeneous Systems; Sample Preparation Problems (colored samples, chemiluminescence, photoluminescence, static electricity); Counting Various Types of Emitters; Counting Atypical Emissions. 2 refs., 2 figs

Recent advances in column switching sample preparation in bioanalysis.

Science.gov (United States)

Kataoka, Hiroyuki; Saito, Keita

2012-04-01

Column switching techniques, using two or more stationary phase columns, are useful for trace enrichment and online automated sample preparation. Target fractions from the first column are transferred online to a second column with different properties for further separation. Column switching techniques can be used to determine the analytes in a complex matrix by direct sample injection or by simple sample treatment. Online column switching sample preparation is usually performed in combination with HPLC or capillary electrophoresis. SPE or turbulent flow chromatography using a cartridge column and in-tube solid-phase microextraction using a capillary column have been developed for convenient column switching sample preparation. Furthermore, various micro-/nano-sample preparation devices using new polymer-coating materials have been developed to improve extraction efficiency. This review describes current developments and future trends in novel column switching sample preparation in bioanalysis, focusing on innovative column switching techniques using new extraction devices and materials.

Glycan characterization of the NIST RM monoclonal antibody using a total analytical solution: From sample preparation to data analysis.

Science.gov (United States)

Hilliard, Mark; Alley, William R; McManus, Ciara A; Yu, Ying Qing; Hallinan, Sinead; Gebler, John; Rudd, Pauline M

Glycosylation is an important attribute of biopharmaceutical products to monitor from development through production. However, glycosylation analysis has traditionally been a time-consuming process with long sample preparation protocols and manual interpretation of the data. To address the challenges associated with glycan analysis, we developed a streamlined analytical solution that covers the entire process from sample preparation to data analysis. In this communication, we describe the complete analytical solution that begins with a simplified and fast N-linked glycan sample preparation protocol that can be completed in less than 1 hr. The sample preparation includes labelling with RapiFluor-MS tag to improve both fluorescence (FLR) and mass spectral (MS) sensitivities. Following HILIC-UPLC/FLR/MS analyses, the data are processed and a library search based on glucose units has been included to expedite the task of structural assignment. We then applied this total analytical solution to characterize the glycosylation of the NIST Reference Material mAb 8761. For this glycoprotein, we confidently identified 35 N-linked glycans and all three major classes, high mannose, complex, and hybrid, were present. The majority of the glycans were neutral and fucosylated; glycans featuring N-glycolylneuraminic acid and those with two galactoses connected via an α1,3-linkage were also identified.

Modular microfluidic system for biological sample preparation

Science.gov (United States)

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.

Development of Syringe/Bottle Hybrids for Sampling Slurries

International Nuclear Information System (INIS)

Coleman, C.J.

1998-01-01

A convenient and effective sample bottle system based on simple modifications of disposable plastic syringes and bottles has been devised and tested for slurry samples. Syringe/ bottle hybrids (hereafter referred to as syringe bottles) have the convenience of regular flat-bottom bottles with screw cap closures. In addition, the syringe imparts a sliding and adjustable bottom to the bottle that forces the entire contents from the bottle. The system was designed especially to collect samples for high temperature work-ups of DWPF slurry samples. The syringe bottles together with fixed-bottom sample vial inserts would provide the DWPF with convenient and reliable methods for dealing with slurry samples

Automated sample preparation station for studying self-diffusion in porous solids with NMR spectroscopy

Science.gov (United States)

Hedin, Niklas; DeMartin, Gregory J.; Reyes, Sebastián C.

2006-03-01

In studies of gas diffusion in porous solids with nuclear magnetic resonance (NMR) spectroscopy the sample preparation procedure becomes very important. An apparatus is presented here that pretreats the sample ex situ and accurately sets the desired pressure and temperature within the NMR tube prior to its introduction in the spectrometer. The gas manifold that supplies the NMR tube is also connected to a microbalance containing another portion of the same sample, which is kept at the same temperature as the sample in the NMR tube. This arrangement permits the simultaneous measurement of the adsorption loading on the sample, which is required for the interpretation of the NMR diffusion experiments. Furthermore, to ensure a good seal of the NMR tube, a hybrid valve design composed of titanium, a Teflon® seat, and Kalrez® O-rings is utilized. A computer controlled algorithm ensures the accuracy and reproducibility of all the procedures, enabling the NMR diffusion experiments to be performed at well controlled conditions of pressure, temperature, and amount of gas adsorbed on the porous sample.

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

Directory of Open Access Journals (Sweden)

Helena Prosen

2014-05-01

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

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

Science.gov (United States)

Prosen, Helena

2014-05-23

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

Importance of sample preparation for molecular diagnosis of lyme borreliosis from urine.

Science.gov (United States)

Bergmann, A R; Schmidt, B L; Derler, A-M; Aberer, E

2002-12-01

Urine PCR has been used for the diagnosis of Borrelia burgdorferi infection in recent years but has been abandoned because of its low sensitivity and the irreproducibility of the results. Our study aimed to analyze technical details related to sample preparation and detection methods. Crucial for a successful urine PCR were (i) avoidance of the first morning urine sample; (ii) centrifugation at 36,000 x g; and (iii) the extraction method, with only DNAzol of the seven different extraction methods used yielding positive results with patient urine specimens. Furthermore, storage of frozen urine samples at -80 degrees C reduced the sensitivity of a positive urine PCR result obtained with samples from 72 untreated erythema migrans (EM) patients from 85% in the first 3 months to samples was proven by hybridization with a GEN-ETI-K-DEIA kit and for a 10 further positive amplicons by sequencing. By using all of these steps to optimize the urine PCR technique, B. burgdorferi infection could be diagnosed by using urine samples from EM patients with a sensitivity (85%) substantially better than that of serological methods (50%). This improved method could be of future importance as an additional laboratory technique for the diagnosis of unclear, unrecognized borrelia infections and diseases possibly related to Lyme borreliosis.

Indigenous development of automated metallographic sample preparation system

International Nuclear Information System (INIS)

Kulkarni, A.P.; Pandit, K.M.; Deshmukh, A.G.; Sahoo, K.C.

2005-01-01

Surface preparation of specimens for Metallographic studies on irradiated material involves a lot of remote handling of radioactive material by skilled manpower. These are laborious and man-rem intensive activities and put limitations on number of samples that can be prepared for the metallographic studies. To overcome these limitations, automated systems have been developed for surface preparation of specimens in PIE division. The system includes (i) Grinding and polishing stations (ii) Water jet cleaning station (iii) Ultrasonic cleaning stations (iv) Drying station (v) Sample loading and unloading station (vi) Dispenser for slurries and diluents and (vii) Automated head for movement of the sample holder disc from one station to other. System facilities the operator for programming/changing sequence of the sample preparations including remote changing of grinding/polishing discs from the stations. Two such systems have been installed and commissioned in Hot Cell for PIE Division. These are being used for preparation of irradiated samples from nuclear fuels and structural components. This development has increased the throughput of metallography work and savings in terms of (man-severts) radiation exposure to operators. This presentation will provide details of the challenges in undertaking this developmental work. (author)

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

OpenAIRE

Helena Prosen

2014-01-01

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...

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.

Sample Preparation for Electron Probe Microanalysis-Pushing the Limits.

Science.gov (United States)

Geller, Joseph D; Engle, Paul D

2002-01-01

There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the "k-ratios," to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very

Preparation of honey sample for tritium monitoring

International Nuclear Information System (INIS)

Chen Bingru; Wang Chenlian; Wang Weihua

1989-01-01

The method of preparation of honey sample for tritium monitoring was described. The equipments consist of an air and honey supply system, a quartz combustor with CM-type monolithic combustion catalyst and a condensation system. In the equipments, honey sample was converted into cooling water by the distilling, cracking and carbonizing procedures for tritium counting. The recovery ratio is 99.0 ± 4.5 percent for tritiated water and 96.0 ± 2.0 for tritiated organic compounds. It is a feasible preparing method for the total tritium monitoring in honey sample

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

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......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......, 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...

Platelet-rich fibrin prepared from stored whole-blood samples.

Science.gov (United States)

Isobe, Kazushige; Suzuki, Masashi; Watanabe, Taisuke; Kitamura, Yutaka; Suzuki, Taiji; Kawabata, Hideo; Nakamura, Masayuki; Okudera, Toshimitsu; Okudera, Hajime; Uematsu, Kohya; Nakata, Koh; Tanaka, Takaaki; Kawase, Tomoyuki

2017-12-01

In regenerative therapy, self-clotted platelet concentrates, such as platelet-rich fibrin (PRF), are generally prepared on-site and are immediately used for treatment. If blood samples or prepared clots can be preserved for several days, their clinical applicability will expand. Here, we prepared PRF from stored whole-blood samples and examined their characteristics. Blood samples were collected from non-smoking, healthy male donors (aged 27-67 years, N = 6), and PRF clots were prepared immediately or after storage for 1-2 days. Fibrin fiber was examined by scanning electron microscopy. Bioactivity was evaluated by means of a bioassay system involving human periosteal cells, whereas PDGF-BB concentrations were determined by an enzyme-linked immunosorbent assay. Addition of optimal amounts of a 10% CaCl 2 solution restored the coagulative ability of whole-blood samples that contained an anticoagulant (acid citrate dextrose) and were stored for up to 2 days at ambient temperature. In PRF clots prepared from the stored whole-blood samples, the thickness and cross-links of fibrin fibers were almost identical to those of freshly prepared PRF clots. PDGF-BB concentrations in the PRF extract were significantly lower in stored whole-blood samples than in fresh samples; however, both extracts had similar stimulatory effects on periosteal-cell proliferation. Quality of PRF clots prepared from stored whole-blood samples is not reduced significantly and can be ensured for use in regenerative therapy. Therefore, the proposed method enables a more flexible treatment schedule and choice of a more suitable platelet concentrate immediately before treatment, not after blood collection.

The effect of sample preparation on uranium hydriding

International Nuclear Information System (INIS)

Banos, A.; Stitt, C.A.; Scott, T.B.

2016-01-01

Highlights: • Distinct differences in uranium hydride growth rates and characteristics between different surface preparation methods. • The primary difference between the categories of sample preparations is the level of strain present in the surface. • Greater surface-strain, leads to higher nucleation number density, implying a preferred attack of strained vs unstrained metal. • As strain is reduced, surface features such as carbides and grain boundaries become more important in controlling the UH3 location. - Abstract: The influence of sample cleaning preparation on the early stages of uranium hydriding has been examined, by using four identical samples but concurrently prepared using four different methods. The samples were reacted together in the same corrosion cell to ensure identical exposure conditions. From the analysis, it was found that the hydride nucleation rate was proportional to the level of strain exhibiting higher number density for the more strained surfaces. Additionally, microstructure of the metal plays a secondary role regarding initial hydrogen attack on the highly strained surfaces yet starts to dominate the system while moving to more pristine samples.

Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

Science.gov (United States)

Casavant, Benjamin P; Guckenberger, David J; Beebe, David J; Berry, Scott M

2014-07-01

Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

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

International Nuclear Information System (INIS)

Azócar, Ignacio; Vargas, Esteban; Duran, Nicole; Arrieta, Abel; González, Evelyn

2012-01-01

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 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: ► Antibacterial activity of films (zirconia–polyether glycol) modified with silver nanoparticles. ► Biofilm formation is prevented. ► High sensibility against gram positive bacteria.

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.

Preparation and Physicochemical Properties of Functionalized Silica/Octamethacryl-Silsesquioxane Hybrid Systems

Directory of Open Access Journals (Sweden)

Karolina Szwarc-Rzepka

2013-01-01

Full Text Available Alkoxysilane-grafted silica/polyhedral oligomeric silsesquioxane with methacryl substituents (SiO2/silane/POSS hybrid material was synthesized according to hydrolyzation and condensation reactions in the so-called “bifunctionalization process.” It is a new attractive system because of its physicochemical, especially thermal and structural, properties. This innovative method of preparation as well as specific physicochemical and useful properties determine the potential applications of such products in many industries. The structure and physicochemical parameters of obtained hybrid systems were characterized using infrared spectroscopy (FTIR, 13C and 29Si solid-state nuclear magnetic resonance (CP MAS NMR, and thermal analysis. The mechanism of bifunctionalization reaction was proposed. The chemical immobilization of silane coupling agent and Methacryl POSS onto silica support surface was noted during the study. Those changes caused a significant increase in the hydrophobic character of fillers obtained. Moreover, changes in thermal stability of SiO2/silane/POSS hybrid systems in comparison to pure POSS modifier were also observed.

On the development of automatic sample preparation devices

International Nuclear Information System (INIS)

Oesselmann, J.

1987-01-01

Modern mass spectrometers for stable isotope analysis offer accurate isotope ratio results from gaseous samples (CO 2 , N 2 , H 2 , SO 2 ) in a completely automated fashion. However, most samples of interest either are associated with contaminant gases or the gas has to be liberated by a chemical procedure prior to measurement. In most laboratories this sample preparation step is performed manually. As a consequence, sample throughput is rather low and - despite skilful operation - the preparation procedure varies slightly from one sample to the next affecting mainly the reproducibility of the data. (author)

Sample Preparation for Electron Probe Microanalysis—Pushing the Limits

Science.gov (United States)

Geller, Joseph D.; Engle, Paul D.

2002-01-01

There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the “k-ratios,” to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very

40 CFR 205.160-2 - Test sample selection and preparation.

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Test sample selection and preparation... sample selection and preparation. (a) Vehicles comprising the sample which are required to be tested... maintained in any manner unless such preparation, tests, modifications, adjustments or maintenance are part...

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 routinely used to process samples (for culture, arrest and fixation of cells) and/or to expand limited amount of samples (in case of prenatal diagnostics). Arguably, this expansion and other sample pretreatments form the longest part of the entire diagnostic protocols spanning over 3–4 days. We present here...... with minimal handling for metaphase FISH slide preparation....

Preparation and magnetic properties of anisotropic bulk MnBi/NdFeB hybrid magnets

Science.gov (United States)

Ma, Y. L.; Liu, X. B.; Nguyen, V. V.; Poudyal, N.; Yue, M.; Liu, J. P.

2016-08-01

Anisotropic hybrid bulk magnets of MnBi/NdFeB with different composition ratio have been prepared with starting MnBi and Nd2Fe14B powders as well as epoxy resin as a binder in case it is needed to form bulk samples. It has been found that the ratio between the two phases in content has a remarkable influence on the magnetic properties, the thermal stability and the density of the bulk magnets. With increasing MnBi content the binder addition can be reduced. When the MnBi content is larger than 30 wt%, no binder is needed. On the other hand, the coercivity and saturation magnetization were increased significantly with increasing NdFeB content. When the NdFeB content was increased from 0% to 50%, the maximum energy product was enhanced from 4.7 to 10.0 MGOe, respectively. The energy product then decreased gradually with the NdFeB content due to the reduced density of the hybrid magnet. The thermal stability measurements showed that the temperature coefficient of coercivity grew with the MnBi content and became positive with MnBi=80 wt%.

Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality: Effect of sample preparation on MALDI-MS of synthetic polymers.

Science.gov (United States)

Kooijman, Pieter C; Kok, Sander; Honing, Maarten

2017-02-28

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) provides detailed and in-depth information about the molecular characteristics of synthetic polymers. To obtain the most accurate results the sample preparation parameters should be chosen to suit the sample and the aim of the experiment. Because the underlying principles of MALDI are still not fully known, a priori determination of optimal sample preparation protocols is often not possible. Employing an automated sample preparation quality assessment method recently presented by us we quantified the sample preparation quality obtained using various sample preparation protocols. Six conventional matrices with and without added potassium as a cationization agent and six ionic liquid matrices (ILMs) were assessed using poly(ethylene glycol) (PEG), polytetrahydrofuran (PTHF) and poly(methyl methacrylate) (PMMA) as samples. All sample preparation protocols were scored and ranked based on predefined quality parameters and spot-to-spot repeatability. Clearly distinctive preferences were observed in matrix identity and cationization agent for PEG, PTHF and PMMA, as the addition of an excess of potassium cationization agent results in an increased score for PMMA and a contrasting matrix-dependent effect for PTHF and PEG. The addition of excess cationization agent to sample mixtures dissipates any overrepresentation of high molecular weight polymer species. Our results show reduced ionization efficiency and similar sample deposit homogeneity for all tested ILMs, compared with well-performing conventional MALDI matrices. The results published here represent a start in the unsupervised quantification of sample preparation quality for MALDI samples. This method can select the best sample preparation parameters for any synthetic polymer sample and the results can be used to formulate hypotheses on MALDI principles. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Excellent electrochemical performance of graphene-silver nanoparticle hybrids prepared using a microwave spark assistance process

International Nuclear Information System (INIS)

Shanmugharaj, A.M.; Ryu, Sung Hun

2012-01-01

Highlights: ► A simple synthesis route is explored in preparing graphene-metal nanoparticle hybrids using cost effective microwave radiation process. ► Electrochemical performance of the synthesized graphene-silver nanoparticle hybrids have been compared with graphite and silver nanoparticle based anode materials. ► Graphene-silver nanoparticle hybrid exhibits stable charge/discharge characteristics of 714 mAh g −1 and it is significantly higher compared to natural graphite and silver based electrodes. - Abstract: A simple method is described for the synthesis of graphene-silver nanoparticle hybrids from graphite and silver precursors using microwave spark ignition process. Adding ecofriendly free radical initiators, in the presence of hydrogen peroxide solution leads to the expansion of graphite to graphene nanosheets. Simultaneously, silver ions intercalated between the graphene layers are reduced to silver nanocrystals leading to the development of graphene-silver nanoparticle hybrids. Transmission electron microscopic (TEM) studies reveal the successful formation of graphene-silver nanoparticle hybrids. X-ray diffraction (XRD) shows that the silver nanoparticles formed on the graphene surfaces are face centered cubic crystals. The surface composition and functional groups present on the graphene-silver nanoparticle hybrids are corroborated using X-ray photoelectron spectroscopy (XPS) and Fourier Transform Infrared Spectroscopy (FT-IR). The lithium storage capacity of the synthesized material, when used as an anode material for rechargeable lithium secondary batteries is investigated. Its first specific discharge capacity is observed to be 580 mAh g −1 and this has been increased to 827 mAh g −1 , by incorporating the silver nanoparticles between the graphene platelets. The reversible capacity of the graphene-silver nanoparticle hybrids is observed to be 714 mAh g −1 , which is significantly higher compared to that of graphene (420 mAh g −1

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...

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...

Trends in sample preparation 2002. Development and application. Book of abstracts

International Nuclear Information System (INIS)

Wenzl, T.; Eberl, M.; Zischka, M.; Knapp, G.

2002-01-01

This conference comprised topics dealing with sample preparation such as: sample decomposition, solvent extraction, derivatization techniques and uncertainty in sample preparation. In particular microwave assisted sample preparation techniques and equipment were discussed. The papers were organized under the general topics: trace element analysis, trace analysis of organic compounds, high performance instrumentation in sample preparation, speciation analysis and posters session. Those papers of INIS interest are cited individually. (nevyjel)

Trends in sample preparation 2002. Development and application. Book of abstracts

Energy Technology Data Exchange (ETDEWEB)

Wenzl, T; Eberl, M; Zischka, M; Knapp, G [eds.

2002-07-01

This conference comprised topics dealing with sample preparation such as: sample decomposition, solvent extraction, derivatization techniques and uncertainty in sample preparation. In particular microwave assisted sample preparation techniques and equipment were discussed. The papers were organized under the general topics: trace element analysis, trace analysis of organic compounds, high performance instrumentation in sample preparation, speciation analysis and posters session. Those papers of INIS interest are cited individually. (nevyjel)

Thermal stability of octadecylsilane hybrid silicas prepared by grafting and sol-gel methods

International Nuclear Information System (INIS)

Brambilla, Rodrigo; Santos, Joao H.Z. dos; Miranda, Marcia S.L.; Frost, Ray L.

2008-01-01

Hybrid silicas bearing octadecylsilane groups were prepared by grafting and sol-gel (SG) methods. The effect of the preparative route on the thermal stability was evaluated by means of thermal gravimetric analysis (TGA), infrared emission spectroscopy (IRES) and, complementary, by 13 C solid-state nuclear magnetic resonance ( 13 C NMR) and matrix assisted laser deionization time of flight mass spectroscopy (MALDI-TOF-MS). Silicas prepared by the grafting route seem to be slightly more stable than those produced by the sol-gel method. This behavior seems to be associated to the preparative route, since grafting affords a liquid-like conformation, while in the case of sol-gel a highly organized crystalline chain conformation was observed

Hybrids of ethylene vinyl acetate with Na-montmorillonite and titania: preparation and characterization

International Nuclear Information System (INIS)

Ashfaq, M.

2010-01-01

Hybrids of Ethylene vinyl acetate (EVA) with Na-montmorillonite and titania were formed. Montmorillonite was organically modified by two different modifiers: Pyridinium ions and 4. 4-oxydianilinium ions. X-ray diffraction results revealed that Pyridinium ions increased the .interlayer spacing by 0.33 nm and 4, 4-oxydianilinium by 0.55 nm approximately. These modified organo-clays were successfully exfoliated in EVA using melt blending. These hybrids showed improvement in mechanical and thermal properties. 4, 4-oxydianilinium ions were degraded at higher temperature due to which thermal degradation was enhanced in EVA. In addition to this, EVA/titania hybrids were also prepared using sot-gel technique and modified by triethoxy vinyl silane and (3-aminopropyI)- triethoxy silane to increase their compatibility with EVA. Some portion of unmodified titania was heat treated to 600 degree C to obtain particulate titania. The hybrid of particulate titania and modified titania improved the mechanical properties and thermal properties. Especially in case of modified titania toughness was almost doubled. (author)

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)

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.

On-line Automated Sample Preparation-Capillary Gas Chromatography for the Analysis of Plasma Samples.

NARCIS (Netherlands)

Louter, A.J.H.; van der Wagt, R.A.C.A.; Brinkman, U.A.T.

1995-01-01

An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up

Cr(VI) generation during sample preparation of solid samples – A ...

African Journals Online (AJOL)

Cr(VI) generation during sample preparation of solid samples – A chromite ore case study. R.I Glastonbury, W van der Merwe, J.P Beukes, P.G van Zyl, G Lachmann, C.J.H Steenkamp, N.F Dawson, M.H Stewart ...

In situ hybridization; principles and applications: review article

Directory of Open Access Journals (Sweden)

Zahra Nozhat

2015-06-01

Full Text Available In situ hybridization (ISH is a method that uses labeled complementary single strand DNA or RNA to localize specific DNA or RNA sequences in an intact cell or in a fixed tissue section. The main steps of ISH consist of: probe selection, tissue or sample preparation, pre-hybridization treatment, hybridization and washing, detection and control procedure. Probe selection is one of the important aspects of successful hybridization. ISH sensitivity and specificity can be influenced by: probe construct, efficiency of labeling, percentage of GC, probe length and signal detection systems. Different methods such as nick translation, random priming, end tailing and T4 DNA polymerase replacement are used for probe generation. Both radioactive and non-radioactive labels can be used in order to probe labeling. Nucleic acid maintenance in samples, prevention of morphological changes of samples and probe penetration into tissue section are the main aims of sample preparation step. Then, a small amount of solution containing probe, is added on slides containing tissue sections for hybridization process, then slides are incubated overnight. Next day, washes are carried out to remove the probes which are not bound to target DNA or RNA. Finally, in order to be sure that the observed labeling is specific to the target sequence, using several control procedures is very important. Various techniques based on ISH consist of: Fluorescence in situ hybridization (FISH, chromogenic in situ hybridization (CISH, genomic in situ hybridization (GISH, comparative genomic hybridization (CGH, spectral karyotyping (SKY and multiplex fluorescence in situ hybridization (MFISH. One of the most common techniques of ISH is fluorescence in situ hybridization. FISH can be used to: 1 detect small deletions and duplications that are not visible using microscope analysis, 2 detect how many chromosomes of a certain type are present in each cell and 3 confirm rearrangements that are

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

Energy Technology Data Exchange (ETDEWEB)

Castricum, H.L.; Sah, A; Blank, D.H.A.; Ten Elshof, J.E. [Inorganic Materials Science, MESA Institute for Nanotechnology, University of Twente, P.O. Box 217, 7500 AE Enschede (Netherlands); Geenevasen, J.A.J. [Van ' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018 WV Amsterdam (Netherlands); Kreiter, R.; Vente, J.F. [ECN Energy Efficiency in the Industry, Petten (Netherlands)

2008-06-15

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 methyltriethoxysilane (MTES), or bis(triethoxysilyl)ethane (BTESE) and MTES. Early-stage hydrolysis and condensation rates of the individual silane precursors were followed with 29Si liquid NMR and structural characteristics of more developed sols were studied with Dynamic Light Scattering. Condensation was found to proceed at more or less similar rates for the different precursors. Homogeneously mixed hybrid colloids can therefore be formed from precursor mixtures. The conditions of preparation under which clear sols with low viscosity could be formed from BTESE/MTES were determined. These sols were synthesised at moderate water/silane and acid/silane ratios and could be applied for the coating of defect-free microporous membranes for molecular separations under hydrothermal conditions.

A hybrid approach to device integration on a genetic analysis platform

International Nuclear Information System (INIS)

Brennan, Des; Justice, John; Aherne, Margaret; Galvin, Paul; Jary, Dorothee; Kurg, Ants; Berik, Evgeny; Macek, Milan

2012-01-01

Point-of-care (POC) systems require significant component integration to implement biochemical protocols associated with molecular diagnostic assays. Hybrid platforms where discrete components are combined in a single platform are a suitable approach to integration, where combining multiple device fabrication steps on a single substrate is not possible due to incompatible or costly fabrication steps. We integrate three devices each with a specific system functionality: (i) a silicon electro-wetting-on-dielectric (EWOD) device to move and mix sample and reagent droplets in an oil phase, (ii) a polymer microfluidic chip containing channels and reservoirs and (iii) an aqueous phase glass microarray for fluorescence microarray hybridization detection. The EWOD device offers the possibility of fully integrating on-chip sample preparation using nanolitre sample and reagent volumes. A key challenge is sample transfer from the oil phase EWOD device to the aqueous phase microarray for hybridization detection. The EWOD device, waveguide performance and functionality are maintained during the integration process. An on-chip biochemical protocol for arrayed primer extension (APEX) was implemented for single nucleotide polymorphism (SNiP) analysis. The prepared sample is aspirated from the EWOD oil phase to the aqueous phase microarray for hybridization. A bench-top instrumentation system was also developed around the integrated platform to drive the EWOD electrodes, implement APEX sample heating and image the microarray after hybridization. (paper)

Current trends in sample preparation for cosmetic analysis.

Science.gov (United States)

Zhong, Zhixiong; Li, Gongke

2017-01-01

The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Recent Developments in Sample Preparation for Mass Spectrometry-Based Metabolomics.

Science.gov (United States)

Gong, Zhi-Gang; Hu, Jing; Wu, Xi; Xu, Yong-Jiang

2017-07-04

Metabolomics is a critical member in systems biology. Although great progress has been achieved in metabolomics, there are still some problems in sample preparation, data processing and data interpretation. In this review, we intend to explore the roles, challenges and trends in sample preparation for mass spectrometry- (MS-) based metabolomics. The newly emerged sample preparation methods were also critically examined, including laser microdissection, in vivo sampling, dried blood spot, microwave, ultrasound and enzyme-assisted extraction, as well as microextraction techniques. Finally, we provide some conclusions and perspectives for sample preparation in MS-based metabolomics.

Synthesis, characterization and antibacterial activity of hybrid chitosan-cerium oxide nanoparticles: As a bionanomaterials.

Science.gov (United States)

Senthilkumar, R P; Bhuvaneshwari, V; Ranjithkumar, R; Sathiyavimal, S; Malayaman, V; Chandarshekar, B

2017-11-01

The hybrid chitosan cerium oxide nanoparticles were prepared for the first time by green chemistry approach using plant leaf extract. The intense peak observed around 292nm in the UV-vis spectrum indicate the formation of cerium oxide nanoparticles. The XRD pattern revealed that the hybrid chitosan-cerium oxide nanoparticles have a polycrystalline structure with cubic fluorite phase. The FTIR spectrum of prepared samples showed the formation of Ce-O bonds and chitosan main chains COC and CO. The FESEM image of hybrid chitosan cerium oxide nanoparticles revealed that the particles are spherical in shape with grains size varying from 23.12nm to 89.91nm. EDAX analysis confirmed the presence of Ce, O, C and N elements in the prepared sample. TEM images showed that the prepared hybrid chitosan-cerium oxide nanoparticles are predominantly uniform in size and most of the particles are spherical in shape with less agglomeration and the particles size varies from 3.61nm to 24.40nm. The prepared chitosan cerium oxide nanoparticles of 50μL concentration showed good antibacterial properties against test pathogens, which was confirmed by the FESEM analysis. The prepared small particle size facilitate that these hybrid ChiCO 2 NPs could effectively be used in biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Carbon nanotubes/magnetite hybrids prepared by a facile synthesis process and their magnetic properties

International Nuclear Information System (INIS)

Zhang Li; Ni, Qing-Qing; Natsuki, Toshiaki; Fu Yaqin

2009-01-01

In this paper, a facile synthesis process is proposed to prepare multiwalled carbon nanotubes/magnetite (MWCNTs/Fe 3 O 4 ) hybrids. The process involves two steps: (1) water-soluble CNTs are synthesized by one-pot modification using potassium persulfate (KPS) as oxidant. (2) Fe 3 O 4 is assembled along the treated CNTs by employing a facile hydrothermal process with the presence of hydrazine hydrate as the mineralizer. The treated CNTs can be easily dispersed in aqueous solvent. Moreover, X-ray photoelectron spectroscopy (XPS) analysis reveals that several functional groups such as potassium carboxylate (-COOK), carbonyl (-C=O) and hydroxyl (-C-OH) groups are formed on the nanotube surfaces. The MWCNTs/Fe 3 O 4 hybrids are characterized with respect to crystal structure, morphology, element composition and magnetic property by X-ray diffraction (XRD), transmission electron microscopy (TEM), XPS and superconducting quantum interference device (SQUID) magnetometer. XRD and TEM results show that the Fe 3 O 4 nanoparticles with diameter in the range of 20-60 nm were firmly assembled on the nanotube surface. The magnetic property investigation indicated that the CNTs/Fe 3 O 4 hybrids exhibit a ferromagnetic behavior and possess a saturation magnetization of 32.2 emu/g. Further investigation indicates that the size of assembled Fe 3 O 4 nanoparticles can be turned by varying experiment factors. Moreover, a probable growth mechanism for the preparation of CNTs/Fe 3 O 4 hybrids was discussed.

Facile and controllable preparation of glucose biosensor based on Prussian blue nanoparticles hybrid composites.

Science.gov (United States)

Li, Lei; Sheng, Qinglin; Zheng, Jianbin; Zhang, Hongfang

2008-11-01

A glucose biosensor based on polyvinylpyrrolidone (PVP) protected Prussian blue nanoparticles (PBNPs)-polyaniline/multi-walled carbon nanotubes hybrid composites was fabricated by electrochemical method. A novel route for PBNPs preparation was applied in the fabrication with the help of PVP, and from scanning electron microscope images, Prussian blue particles on the electrode were found nanoscaled. The biosensor exhibits fast current response (<6 s) and a linearity in the range from 6.7x10(-6) to 1.9x10(-3) M with a high sensitivity of 6.28 microA mM(-1) and a detection limit of 6x10(-7) M (S/N=3) for the detection of glucose. The apparent activation energy of enzyme-catalyzed reaction and the apparent Michaelis-Menten constant are 23.9 kJ mol(-1) and 1.9 mM respectively, which suggests a high affinity of the enzyme-substrate. This easy and controllable construction method of glucose biosensor combines the characteristics of the components of the hybrid composites, which favors the fast and sensitive detection of glucose with improved analytical capabilities. In addition, the biosensor was examined in human serum samples for glucose determination with a recovery between 95.0 and 104.5%.

A novel chitosan 3-amino-1,2,4-triazole hybrid: Preparation and its effects on cotton fabric properties

Directory of Open Access Journals (Sweden)

Asmaa Aboelnaga

2017-09-01

Full Text Available A hybrid of chitosan and 3-amino-1,2,4-triazole was prepared using the semi-wet method, which allows for the adsorption of the triazole molecules on the chitosan surface. Moreover, an easy method for applying this hybrid to cotton fabric was established. The tensional strength, uniformity and compatibility of the hybrid components in forming of a strong film were studied using different variables, including the chitosan 3-amino-1,2,4-triazole ratio, fixation temperature and time. The loading of the hybrid onto the fabric in the absence and presence of cross linker (butane tetra carboxylic acid was also studied. The best conditions for preparing the hybrid was a 1:4 molar ratio of chitosan to 3-amino-1,2,4-triazole at 60 °C for 240 min, and those for the application of the hybrid to cotton fabric were a 1:1 molar ratio at 150 °C with a 5 min curing time. Both hybrid and treated cotton fabrics were characterized using FTIR, SEM, TGA, and DSC as well as the nitrogen content and tensional strength of the treated cotton. Finally, the antibacterial activities of the treated cotton fabric display 100% activity and excellent effects against gram-positive bacteria, Staphylococcus aureus and gram-negative Escherichia coli.

Enhanced configurational sampling with hybrid non-equilibrium molecular dynamics-Monte Carlo propagator

Science.gov (United States)

Suh, Donghyuk; Radak, Brian K.; Chipot, Christophe; Roux, Benoît

2018-01-01

Molecular dynamics (MD) trajectories based on classical equations of motion can be used to sample the configurational space of complex molecular systems. However, brute-force MD often converges slowly due to the ruggedness of the underlying potential energy surface. Several schemes have been proposed to address this problem by effectively smoothing the potential energy surface. However, in order to recover the proper Boltzmann equilibrium probability distribution, these approaches must then rely on statistical reweighting techniques or generate the simulations within a Hamiltonian tempering replica-exchange scheme. The present work puts forth a novel hybrid sampling propagator combining Metropolis-Hastings Monte Carlo (MC) with proposed moves generated by non-equilibrium MD (neMD). This hybrid neMD-MC propagator comprises three elementary elements: (i) an atomic system is dynamically propagated for some period of time using standard equilibrium MD on the correct potential energy surface; (ii) the system is then propagated for a brief period of time during what is referred to as a "boosting phase," via a time-dependent Hamiltonian that is evolved toward the perturbed potential energy surface and then back to the correct potential energy surface; (iii) the resulting configuration at the end of the neMD trajectory is then accepted or rejected according to a Metropolis criterion before returning to step 1. A symmetric two-end momentum reversal prescription is used at the end of the neMD trajectories to guarantee that the hybrid neMD-MC sampling propagator obeys microscopic detailed balance and rigorously yields the equilibrium Boltzmann distribution. The hybrid neMD-MC sampling propagator is designed and implemented to enhance the sampling by relying on the accelerated MD and solute tempering schemes. It is also combined with the adaptive biased force sampling algorithm to examine. Illustrative tests with specific biomolecular systems indicate that the method can yield

Soil sample preparation using microwave digestion for uranium analysis

International Nuclear Information System (INIS)

Mohagheghi, Amir H.; Preston, Rose; Akbarzadeh, Mansoor; Bakthiar, Steven

2000-01-01

A new sample preparation procedure has been developed for digestion of soil samples for uranium analysis. The technique employs a microwave oven digestion system to digest the sample and to prepare it for separation chemistry and analysis. The method significantly reduces the volume of acids used, eliminates a large fraction of acid vapor emissions, and speeds up the analysis time. The samples are analyzed by four separate techniques: Gamma Spectrometry, Alpha Spectroscopy using the open digestion method, Kinetic Phosphorescence Analysis (KPA) using open digestion, and KPA by Microwave digestion technique. The results for various analytical methods are compared and used to confirm the validity of the new procedure. The details of the preparation technique along with its benefits are discussed

ProTaper rotary instrument fracture during root canal preparation: a comparison between rotary and hybrid techniques.

Science.gov (United States)

Farid, Huma; Khan, Farhan Raza; Rahman, Munawar

2013-03-01

This study aimed to compare the frequency of ProTaper rotary instrument fracture with rotary (conventional) and hybrid (rotary and hand files) canal preparation techniques. Secondary objectives were to determine whether there was an association of ProTaper file fracture with the canal curvature and to compare the mean time required for canal preparation in the two techniques. An in vitro experiment was conducted on 216 buccal canals of extracted maxillary and mandibular first molars. After creating an access cavity and a glide path for each canal, a periapical radiograph was taken and the canal curvature was measured with Schneider's technique. The canals were then randomly divided into Group A (rotary technique) and Group B (hybrid technique). The length of ProTaper files were measured before and after each canal preparation. Time taken for each canal preparation was recorded. A total of seven ProTaper files fractured in Group A (P=0.014) in canals with a curvature >25 degrees (PProTaper rotary files, although time consuming, was safer in canals having a curvature greater than 25 degrees.

7 CFR 61.34 - Drawing and preparation of sample.

Science.gov (United States)

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Drawing and preparation of sample. 61.34 Section 61.34 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards... Cottonseed Samplers § 61.34 Drawing and preparation of sample. Each licensed cottonseed sampler shall draw...

New trends in sample preparation techniques for environmental analysis.

Science.gov (United States)

Ribeiro, Cláudia; Ribeiro, Ana Rita; Maia, Alexandra S; Gonçalves, Virgínia M F; Tiritan, Maria Elizabeth

2014-01-01

Environmental samples include a wide variety of complex matrices, with low concentrations of analytes and presence of several interferences. Sample preparation is a critical step and the main source of uncertainties in the analysis of environmental samples, and it is usually laborious, high cost, time consuming, and polluting. In this context, there is increasing interest in developing faster, cost-effective, and environmentally friendly sample preparation techniques. Recently, new methods have been developed and optimized in order to miniaturize extraction steps, to reduce solvent consumption or become solventless, and to automate systems. This review attempts to present an overview of the fundamentals, procedure, and application of the most recently developed sample preparation techniques for the extraction, cleanup, and concentration of organic pollutants from environmental samples. These techniques include: solid phase microextraction, on-line solid phase extraction, microextraction by packed sorbent, dispersive liquid-liquid microextraction, and QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe).

Tooth enamel sample preparation using alkaline treatment in ESR dosimetry

International Nuclear Information System (INIS)

Yongzeng, Zhou; Jiadong, Wang; Xiaomei, Jia; Ke, Wu; Jianbo, Cong

2002-01-01

Tooth enamel sample preparation using alkaline treatment was studied and compared with traditional mechanical method in this paper. 20 adult teeth were used. Samples were placed into NaOH solution. This method requires 4-5 weeks and the enamel was separated from dentin. Experimental results show that 8M NaOH was appropriate for separating enamel from dentin and that there is no difference in background signal relative intensity between samples prepared by mechanical and by chemical methods. There is also no difference in radiosensitivity between samples prepared by two methods mentioned above. Dose response curve for tooth enamel samples isolated by 8M NaOH solution was obtained

Sample preparation for special PIE-techniques at ITU

International Nuclear Information System (INIS)

Toscano, E.H.; Manzel, R.

2002-01-01

Several sample preparation techniques were developed and installed in hot cells. The techniques were conceived to evaluate the performance of highly burnt fuel rods and include: (a) a device for the removal of the fuel, (b) a method for the preparation of the specimen ends for the welding of new end caps and for the careful cleaning of samples for Transmission Electron Microscopy and Glow Discharge Mass Spectroscopy, (c) a sample pressurisation device for long term creep tests, and (d) a diameter measuring device for creep or burst samples. Examples of the determination of the mechanical properties, the behaviour under transient conditions and for the assessment of the corrosion behaviour of high burnup cladding materials are presented. (author)

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

2017-01-27

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.

Facile preparation of well-combined lignin-based carbon/ZnO hybrid composite with excellent photocatalytic activity

Science.gov (United States)

Wang, Huan; Qiu, Xueqing; Liu, Weifeng; Yang, Dongjie

2017-12-01

In this work, a novel lignin-based carbon/ZnO (LC/ZnO) hybrid composite with excellent photocatalytic performance was prepared through a convenient and environment friendly method using alkali lignin (AL) as carbon source. The morphological, microstructure and optical properties of the as-prepared LC/ZnO hybrid composite was characterized with scanning electron microscope (SEM), X-ray diffraction (XRD), Raman and UV-vis. The resulting LC/ZnO hybrid is composed of highly dispersed ZnO nanoparticles embedded on a lignin-based carbon nanosheet, showing excellent photogenerated electrons and holes separation and migration efficiency. The photocatalytic activity of LC/ZnO was much higher than the pure ZnO. The LC/ZnO hybrid composite showed different photocatalytic mechanism for degradation of negative methyl orange (MO) and positive Rhodamine B (RhB). It showed that h+ was the main photocatalytic active group during the degradation of MO, ·O2- and ·OH were the photocatalytic active groups during degradation of RhB. This reported photocatalyst with selective degradation of positive and negative organic dyes may have a great application prospect for photoelectric conversion and catalytic materials. Results of this work were of practical importance for high-valued utilization of lignin for carbon materials.

Hybrid manganese oxide films for supercapacitor application prepared by sol-gel technique

International Nuclear Information System (INIS)

Chen, Chin-Yi; Wang, Sheng-Chang; Tien, Yue-Han; Tsai, Wen-Ta; Lin, Chung-Kwei

2009-01-01

Hybrid films were prepared by adding various concentrations of meso-carbon microbeads (MCMB) during sol-gel processing of manganese oxide films. The heat-treated films were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). In addition, electrochemical performance of the MCMB-added Mn-oxide hybrid coatings was evaluated by cyclic voltammetry (CV) and compared with its unadded counterpart. Experimental results showed that Mn-oxide films exhibited a mixture of Mn 2 O 3 and Mn 3 O 4 phases. The higher the heat-treatment temperature, the more Mn 2 O 3 can be observed. The specific capacitance of the unadded Mn-oxide electrodes is 209 F/g. Because the MCMB particles provide more interfacial surface area for electrochemical reactions, a significant improvement can be noticed by adding MCMB in Mn-oxide coatings. The 300 o C heat-treated hybrid Mn-oxide coating with a Mn/MCMB ratio of 10/1 exhibits the highest value of 350 F/g, showing a ∼ 170% increase in specific capacitance.

Sample preparations for spark source mass spectrography

International Nuclear Information System (INIS)

Catlett, C.W.; Rollins, M.B.; Griffin, E.B.; Dorsey, J.G.

1977-10-01

Methods have been developed for the preparation of various materials for spark source mass spectrography. The essential features of these preparations (all which can provide adequate precision in a cost-effective manner) consist in obtaining spark-stable electrode sample pieces, a common matrix, a reduction of anomolous effects in the spark, the incorporation of a suitable internal standard for plate response normalization, and a reduction in time

Present status of NMCC and sample preparation method for bio-samples

International Nuclear Information System (INIS)

Futatsugawa, S.; Hatakeyama, S.; Saitou, S.; Sera, K.

1993-01-01

In NMCC(Nishina Memorial Cyclotron Center) we are doing researches on PET of nuclear medicine (Positron Emission Computed Tomography) and PIXE analysis (Particle Induced X-ray Emission) using a small cyclotron of compactly designed. The NMCC facilities have been opened to researchers of other institutions since April 1993. The present status of NMCC is described. Bio-samples (medical samples, plants, animals and environmental samples) have mainly been analyzed by PIXE in NMCC. Small amounts of bio-samples for PIXE are decomposed quickly and easily in a sealed PTFE (polytetrafluoroethylene) vessel with a microwave oven. This sample preparation method of bio-samples also is described. (author)

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.

Finding even more anthropogenic indicators in mildly prepared sediment samples

DEFF Research Database (Denmark)

Enevold, Renée; Odgaard, Bent Vad

2016-01-01

be worth the effort to prepare the NPP samples with as mild a preparation method as possible. We have mildly prepared NPP samples from a small forest hollow, Tårup Lund, Denmark. From the recovered NPP assemblages we attempt identifying anthropogenic indicators by comparing to the environmental information......NPPs in anthropogenic soils and archaeological samples are often numerous in types as well as in abundance. Preparing these soil samples with methods based on acid digestion holds the potential of severe bias leaving the NPP assemblages devoid of acid vulnerable NPPs. In many cases it might...... derived from sediment, pollen and macrofossil analyses. The sediment from the forest hollow encompasses environmental information from the last 6000 years, including a period of locally intense pastoral and/or agricultural activity during the Iron Age. Keywords: NPP diversity, forest hollow, anthropogenic...

Sampling, storage and sample preparation procedures for X ray fluorescence analysis of environmental materials

International Nuclear Information System (INIS)

1997-06-01

X ray fluorescence (XRF) method is one of the most commonly used nuclear analytical technique because of its multielement and non-destructive character, speed, economy and ease of operation. From the point of view of quality assurance practices, sampling and sample preparation procedures are the most crucial steps in all analytical techniques, (including X ray fluorescence) applied for the analysis of heterogeneous materials. This technical document covers recent modes of the X ray fluorescence method and recent developments in sample preparation techniques for the analysis of environmental materials. Refs, figs, tabs

Optimal Design for Hybrid Ratio of Carbon/Basalt Hybrid Fiber Reinforced Resin Matrix Composites

Directory of Open Access Journals (Sweden)

XU Hong

2017-08-01

Full Text Available The optimum hybrid ratio range of carbon/basalt hybrid fiber reinforced resin composites was studied. Hybrid fiber composites with nine different hybrid ratios were prepared before tensile test.According to the structural features of plain weave, the unit cell's performance parameters were calculated. Finite element model was established by using SHELL181 in ANSYS. The simulated values of the sample stiffness in the model were approximately similar to the experimental ones. The stress nephogram shows that there is a critical hybrid ratio which divides the failure mechanism of HFRP into single failure state and multiple failure state. The tensile modulus, strength and limit tensile strain of HFRP with 45% resin are simulated by finite element method. The result shows that the tensile modulus of HFRP with 60% hybrid ratio increases by 93.4% compared with basalt fiber composites (BFRP, and the limit tensile strain increases by 11.3% compared with carbon fiber composites(CFRP.

A Chip-Capillary Hybrid Device for Automated Transfer of Sample Pre-Separated by Capillary Isoelectric Focusing to Parallel Capillary Gel Electrophoresis for Two-Dimensional Protein Separation

Science.gov (United States)

Lu, Joann J.; Wang, Shili; Li, Guanbin; Wang, Wei; Pu, Qiaosheng; Liu, Shaorong

2012-01-01

In this report, we introduce a chip-capillary hybrid device to integrate capillary isoelectric focusing (CIEF) with parallel capillary sodium dodecyl sulfate – polyacrylamide gel electrophoresis (SDS-PAGE) or capillary gel electrophoresis (CGE) toward automating two-dimensional (2D) protein separations. The hybrid device consists of three chips that are butted together. The middle chip can be moved between two positions to re-route the fluidic paths, which enables the performance of CIEF and injection of proteins partially resolved by CIEF to CGE capillaries for parallel CGE separations in a continuous and automated fashion. Capillaries are attached to the other two chips to facilitate CIEF and CGE separations and to extend the effective lengths of CGE columns. Specifically, we illustrate the working principle of the hybrid device, develop protocols for producing and preparing the hybrid device, and demonstrate the feasibility of using this hybrid device for automated injection of CIEF-separated sample to parallel CGE for 2D protein separations. Potentials and problems associated with the hybrid device are also discussed. PMID:22830584

Influences of different sample preparation methods on tooth enamel ESR signals

International Nuclear Information System (INIS)

Zhang Wenyi; Jiao Ling; Zhang Liang'an; Pan Zhihong; Zeng Hongyu

2005-01-01

Objective: To study the influences of different sample preparation methods on tooth enamel ESR signals in order to reduce the effect of dentine on their sensitivities to radiation. Methods: The enamel was separated from dentine of non-irradiated adult teeth by mechanical, chemical, or both methods. The samples of different preparations were scanned by an ESR spectrometer before and after irradiation. Results: The response of ESR signals of samples prepared with different methods to radiation dose was significantly different. Conclusion: The selection of sample preparation method is very important for dose reconstruction by tooth enamel ESR dosimetry, especially in the low dose range. (authors)

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

International Nuclear Information System (INIS)

Ferreira, Sidney A.; Ituassu, Leonardo T.; Melo, Maria N.

2009-01-01

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 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)

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.

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

Sample preparation is considered one of the limiting steps in microbial metabolome analysis. Eukaryotes and prokaryotes behave very differently during the several steps of classical sample preparation methods for analysis of metabolites. Even within the eukaryote kingdom there is a vast diversity...

Fluidics platform and method for sample preparation and analysis

Science.gov (United States)

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.

Combining Electrochemical Sensors with Miniaturized Sample Preparation for Rapid Detection in Clinical Samples

Science.gov (United States)

Bunyakul, Natinan; Baeumner, Antje J.

2015-01-01

Clinical analyses benefit world-wide from rapid and reliable diagnostics tests. New tests are sought with greatest demand not only for new analytes, but also to reduce costs, complexity and lengthy analysis times of current techniques. Among the myriad of possibilities available today to develop new test systems, amperometric biosensors are prominent players—best represented by the ubiquitous amperometric-based glucose sensors. Electrochemical approaches in general require little and often enough only simple hardware components, are rugged and yet provide low limits of detection. They thus offer many of the desirable attributes for point-of-care/point-of-need tests. This review focuses on investigating the important integration of sample preparation with (primarily electrochemical) biosensors. Sample clean up requirements, miniaturized sample preparation strategies, and their potential integration with sensors will be discussed, focusing on clinical sample analyses. PMID:25558994

A hybrid reliability algorithm using PSO-optimized Kriging model and adaptive importance sampling

Science.gov (United States)

Tong, Cao; Gong, Haili

2018-03-01

This paper aims to reduce the computational cost of reliability analysis. A new hybrid algorithm is proposed based on PSO-optimized Kriging model and adaptive importance sampling method. Firstly, the particle swarm optimization algorithm (PSO) is used to optimize the parameters of Kriging model. A typical function is fitted to validate improvement by comparing results of PSO-optimized Kriging model with those of the original Kriging model. Secondly, a hybrid algorithm for reliability analysis combined optimized Kriging model and adaptive importance sampling is proposed. Two cases from literatures are given to validate the efficiency and correctness. The proposed method is proved to be more efficient due to its application of small number of sample points according to comparison results.

Hybrid Warfare: Preparing for Future Conflict

Science.gov (United States)

2015-02-17

ciceromagazine.com/?s=getting+behind+hybrid+warfare. Brown , Col Leslie F. “Twenty-First Century Warfare Will be Hybrid.” Carlisle Barracks, PA...Lebanon and Gaza.” Rand Corporation Occasional Paper. Santa Monica, CA: Rand Corporation, 2010. Jones, Gareth and Darya Korsunskaya. “U.S., EU

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.

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

Directory of Open Access Journals (Sweden)

Kecheng Yang

Full Text Available 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.

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.

Sample preparation techniques in trace element analysis by X-ray emission spectroscopy

International Nuclear Information System (INIS)

Valkovic, V.

1983-11-01

The report, written under a research contract with the IAEA, contains a detailed presentation of the most difficult problem encountered in the trace element analysis by methods of the X-ray emission spectroscopy, namely the sample preparation techniques. The following items are covered. Sampling - with specific consideration of aerosols, water, soil, biological materials, petroleum and its products, storage of samples and their handling. Pretreatment of samples - preconcentration, ashing, solvent extraction, ion exchange and electrodeposition. Sample preparations for PIXE - analysis - backings, target uniformity and homogeneity, effects of irradiation, internal standards and specific examples of preparation (aqueous, biological, blood serum and solid samples). Sample preparations for radioactive sources or tube excitation - with specific examples (water, liquid and solid samples, soil, geological, plants and tissue samples). Finally, the problem of standards and reference materials, as well as that of interlaboratory comparisons, is discussed

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)

Preparation and morphological and optical characterization of azo-polymer-based SiO2 sonogel hybrid composites

International Nuclear Information System (INIS)

Morales-Saavedra, Omar G; Ontiveros-Barrera, Fernando G; Torres-Zúñiga, Vicente; Guadalupe-Bañuelos, José; Ortega-Martínez, Roberto; Rivera, Ernesto; García, Tonatiuh

2009-01-01

The well-established catalyst-free sonogel route was successfully implemented to fabricate highly pure, optically active, solid state polymeric azo- dye/SiO 2 -based hybrid composites. Bulk samples exhibit controllable geometrical shapes and monolithic structure with variable dopant concentrations. Since the implemented azo-dye chromophores exhibit a push–pull structure, hybrid film samples were spin-coated on ITO-covered glass substrates; molecular alignment was then performed via electrical poling in order to explore the quadratic nonlinear optical performance of this kind of composite. Comprehensive morphological, spectroscopic and optical characterization of the samples were performed with several experimental techniques: atomic force microscopy, x-ray diffraction and infrared, Raman, photoluminescent and ultraviolet–visible spectroscopies. The linear refractive indices of both bulk and thin film samples were measured according to the Brewster angle technique and a numerical analysis of the transmission spectral data, respectively. Regardless of the low glass transition temperatures of the studied polymers, some hybrid film samples were able to display stable nonlinear optical activity such as second harmonic generation. Results show that the chromophores were satisfactorily embedded into the highly pure SiO 2 sonogel network without significant guest–host molecular interactions, thus preserving their optical properties and producing sol–gel hybrid glasses suitable for optical applications

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.

Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review

Science.gov (United States)

Dong, Yonghui; Li, Bin; Malitsky, Sergey; Rogachev, Ilana; Aharoni, Asaph; Kaftan, Filip; Svatoš, Aleš; Franceschi, Pietro

2016-01-01

Mass spectrometry imaging (MSI) is a mass spectrometry based molecular ion imaging technique. It provides the means for ascertaining the spatial distribution of a large variety of analytes directly on tissue sample surfaces without any labeling or staining agents. These advantages make it an attractive molecular histology tool in medical, pharmaceutical, and biological research. Likewise, MSI has started gaining popularity in plant sciences; yet, information regarding sample preparation methods for plant tissues is still limited. Sample preparation is a crucial step that is directly associated with the quality and authenticity of the imaging results, it therefore demands in-depth studies based on the characteristics of plant samples. In this review, a sample preparation pipeline is discussed in detail and illustrated through selected practical examples. In particular, special concerns regarding sample preparation for plant imaging are critically evaluated. Finally, the applications of MSI techniques in plants are reviewed according to different classes of plant metabolites. PMID:26904042

Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review.

Science.gov (United States)

Dong, Yonghui; Li, Bin; Malitsky, Sergey; Rogachev, Ilana; Aharoni, Asaph; Kaftan, Filip; Svatoš, Aleš; Franceschi, Pietro

2016-01-01

Mass spectrometry imaging (MSI) is a mass spectrometry based molecular ion imaging technique. It provides the means for ascertaining the spatial distribution of a large variety of analytes directly on tissue sample surfaces without any labeling or staining agents. These advantages make it an attractive molecular histology tool in medical, pharmaceutical, and biological research. Likewise, MSI has started gaining popularity in plant sciences; yet, information regarding sample preparation methods for plant tissues is still limited. Sample preparation is a crucial step that is directly associated with the quality and authenticity of the imaging results, it therefore demands in-depth studies based on the characteristics of plant samples. In this review, a sample preparation pipeline is discussed in detail and illustrated through selected practical examples. In particular, special concerns regarding sample preparation for plant imaging are critically evaluated. Finally, the applications of MSI techniques in plants are reviewed according to different classes of plant metabolites.

15N sample preparation for mass spectroscopy analysis

International Nuclear Information System (INIS)

Trivelin, P.C.O.; Salati, E.; Matsui, E.

1973-01-01

Technics for preparing 15 N samples to be analised is presented. Dumas method and oxidation by sodium hypobromite method are described in order to get the appropriate sample. Method to calculate 15 N ratio from mass spectrometry dates is also discussed [pt

Preparation of archaeological samples for its dating by thermoluminescence

International Nuclear Information System (INIS)

Mejia F, D.

2000-01-01

The present work shows the results of the preparation of archaeological samples for their dating by thermoluminescence (Tl) using the Fine grain technique established by Zimmerman but with the varying of such preparation was realized in normal daylight conditions, only the taking of the Tl readings were realized in dark room and red light. In the chapter 1 basic concepts are described about: matter constitution, radioactivity, units and radiation magnitudes, and thermoluminescence. In the chapter 2 some theoretical aspects on dating are showed. It is described how realizing the samples collection, the fine grain method, the determination of the accumulated dose through the years or paleodoses (P=Q+I) by mean of the increasing to obtain the dose equivalent dose (Q) and the signal regeneration method to obtain the correction factor by supra linearity (1), the determination of the annual dose rate to apply the age equation and the evaluation of the age uncertainty with the error limits. The development of experimental part with samples from the archaeological site named Edzna in Campeche, Mexico is described in the chapter 3. The results are presented in the chapter 4. It was obtained an age for the sample named CH7 it was obtained an age of 389 ± years. In conclusion the preparation of the archaeological samples for their dating by Tl in the conditions before mentioned is reliable, but they must be realized more studies with samples of well known age, preparing them in normal daylight conditions and simultaneously in dark room with red light. In order to observe how respond the minerals present in the sample at different dose rapidity, the same samples must be radiated with radiation sources with different dose rate. (Author)

Deterministic joint remote preparation of an equatorial hybrid state via high-dimensional Einstein-Podolsky-Rosen pairs: active versus passive receiver

Science.gov (United States)

Bich, Cao Thi; Dat, Le Thanh; Van Hop, Nguyen; An, Nguyen Ba

2018-04-01

Entanglement plays a vital and in many cases non-replaceable role in the quantum network communication. Here, we propose two new protocols to jointly and remotely prepare a special so-called bipartite equatorial state which is hybrid in the sense that it entangles two Hilbert spaces with arbitrary different dimensions D and N (i.e., a type of entanglement between a quDit and a quNit). The quantum channels required to do that are however not necessarily hybrid. In fact, we utilize four high-dimensional Einstein-Podolsky-Rosen pairs, two of which are quDit-quDit entanglements, while the other two are quNit-quNit ones. In the first protocol the receiver has to be involved actively in the process of remote state preparation, while in the second protocol the receiver is passive as he/she needs to participate only in the final step for reconstructing the target hybrid state. Each protocol meets a specific circumstance that may be encountered in practice and both can be performed with unit success probability. Moreover, the concerned equatorial hybrid entangled state can also be jointly prepared for two receivers at two separated locations by slightly modifying the initial particles' distribution, thereby establishing between them an entangled channel ready for a later use.

Preparation of thermally stable microcapsules with a chitosan-silica hybrid.

Science.gov (United States)

Kang, Hong-Yi; Chen, Hui-Huang

2014-09-01

Addition of microcapsules with a high dielectric constant and low specific heat capacity to a battered layer was designed to create a higher temperature in the crust than in the prefried fish nuggets to prevent the water vapor in the fish nuggets from migrating to the crust during microwave heating. Therefore, chitosan-silica hybrids and soybean oil were utilized to prepare the shell and core of the thermally stable microcapsules (MC(CS)), respectively. The MC(CS) were prepared by sol-gel coacervation from an oil-in-water emulsion. The sodium silicate was hydrolyzed and coacervated through polymerization for 24 h at pH 5. The zeta potential analysis indicated that chitosan with a positive charge and silica with a negative charge interacted through electrostatic attraction to form a hybrid shell. The volume mean particle size and encapsulation efficiency of the MC(CS) were 9.6 ± 0.2 μm and 75.6% ± 1.3%, respectively, when oil/chitosan = 0.2 and chitosan/silica = 0.5 (w/w). In addition to H-bonding and electrostatic attraction, Si-O-N bonds were formed between chitosan and silica. Dehydration of the bound water in the MC(CS) was observed in the range of 25 to 250 °C in the differential scanning calorimetry thermal analysis, with the lack of apparent thermal peaks indicating its high thermal stability. The decrease of force to cut the crust observed by texture analysis as well as the increase of hedonic score by consumer acceptance test revealed the addition of 1% MC(CS) significantly improved the crispness of the crust in the microwave-reheated nuggets. © 2014 Institute of Food Technologists®

Preparation and unique electrical behaviors of monodispersed hybrid nanorattles of metal nanocores with hairy electroactive polymer shells.

Science.gov (United States)

Cai, Tao; Zhang, Bin; Chen, Yu; Wang, Cheng; Zhu, Chun Xiang; Neoh, Koon-Gee; Kang, En-Tang

2014-03-03

A versatile template-assisted strategy for the preparation of monodispersed rattle-type hybrid nanospheres, encapsulating a movable Au nanocore in the hollow cavity of a hairy electroactive polymer shell (Au@air@PTEMA-g-P3HT hybrid nanorattles; PTEMA: poly(2-(thiophen-3-yl)ethyl methacrylate; P3HT: poly(3-hexylthiophene), was reported. The Au@silica core-shell nanoparticles, prepared by the modified Stöber sol-gel process on Au nanoparticle seeds, were used as templates for the synthesis of Au@silica@PTEMA core-double shell nanospheres. Subsequent oxidative graft polymerization of 3-hexylthiophene from the exterior surface of the Au@silica@PTEMA core-double shell nanospheres allowed the tailoring of surface functionality with electroactive P3HT brushes (Au@silica@PTEMA-g-P3HT nanospheres). The Au@air@ PTEMA-g-P3HT hybrid nanorattles were obtained after etching of the silica interlayer by HF. The as-prepared nanorattles were dispersed into an electrically insulating polystyrene matrix and for the first time used to fabricate nonvolatile memory devices. As a result, unique electrical behaviors, including insulator behavior, write-once-read-many-times and rewritable memory effects, and conductor behavior as well, were observed in the Al/Au@air@PTEMA-g-P3HT+PS/ITO (ITO: indium-tin oxide) sandwich thin-film devices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Real-time imaging of spin-to-orbital angular momentum hybrid remote state preparation

Science.gov (United States)

Erhard, Manuel; Qassim, Hammam; Mand, Harjaspreet; Karimi, Ebrahim; Boyd, Robert W.

2015-08-01

There exists two prominent methods to transfer information between two spatially separated parties, namely Alice (A) and Bob (B): quantum teleportation and remote state preparation. However, the difference between these methods is, in the teleportation scheme, the state to be transferred is completely unknown, whereas in state preparation it should be known to the sender. In addition, photonic state teleportation is probabilistic due to the impossibility of performing a two-particle complete Bell-state analysis with linear optics, while remote state preparation can be performed deterministically. Here we report the first realization of photonic hybrid remote state preparation from spin to orbital angular momentum degrees of freedom. In our scheme, the polarization state of photon A is transferred to orbital angular momentum of photon B. The prepared states are visualized in real time by means of an intensified CCD camera. The quality of the prepared states is verified by performing quantum state tomography, which confirms an average fidelity higher than 99.4%. We believe that this experiment paves the way towards a novel means of quantum communication in which encryption and decryption are carried out in naturally different Hilbert spaces, and therefore may provide a means for enhancing security.

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

International Nuclear Information System (INIS)

Lari, L; Dudkiewicz, A

2014-01-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

Science.gov (United States)

Lari, L.; Dudkiewicz, A.

2014-06-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility.

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.

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

Science.gov (United States)

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

2016-01-05

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

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

Science.gov (United States)

Harrington, Brent; Nickerson, Beverly; Guo, Michele Xuemei; Barber, Marc; Giamalva, David; Lee, Carlos; Scrivens, Garry

2014-12-16

In pharmaceutical analysis, the results of drug product assay testing are used to make decisions regarding the quality, efficacy, and stability of the drug product. In order to make sound risk-based decisions concerning drug product potency, an understanding of the uncertainty of the reportable assay value is required. Utilizing the most restrictive criteria in current regulatory documentation, a maximum variability attributed to method repeatability is defined for a drug product potency assay. A sampling strategy that reduces the repeatability component of the assay variability below this predefined maximum is demonstrated. The sampling strategy consists of determining the number of dosage units (k) to be prepared in a composite sample of which there may be a number of equivalent replicate (r) sample preparations. The variability, as measured by the standard error (SE), of a potency assay consists of several sources such as sample preparation and dosage unit variability. A sampling scheme that increases the number of sample preparations (r) and/or number of dosage units (k) per sample preparation will reduce the assay variability and thus decrease the uncertainty around decisions made concerning the potency of the drug product. A maximum allowable repeatability component of the standard error (SE) for the potency assay is derived using material in current regulatory documents. A table of solutions for the number of dosage units per sample preparation (r) and number of replicate sample preparations (k) is presented for any ratio of sample preparation and dosage unit variability.

Use of robotic systems for radiochemical sample changing and for analytical sample preparation

International Nuclear Information System (INIS)

Delmastro, J.R.; Hartenstein, S.D.; Wade, M.A.

1989-01-01

Two uses of the Perkin-Elmer (PE) robotic system will be presented. In the first, a PE robot functions as an automatic sample changer for up to five low energy photon spectrometry (LEPS) detectors operated with a Nuclear Data ND 6700 system. The entire system, including the robot, is controlled by an IBM PC-AT using software written in compiled BASIC. Problems associated with the development of the system and modifications to the robot will be presented. In the second, an evaluation study was performed to assess the abilities of the PE robotic system for performing complex analytical sample preparation procedures. For this study, a robotic system based upon the PE robot and auxiliary devices was constructed and programmed to perform the preparation of final product samples (UO 3 ) for accountability and impurity specification analyses. These procedures require sample dissolution, dilution, and liquid-liquid extraction steps. The results of an in-depth evaluation of all system components will be presented

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

International Nuclear Information System (INIS)

Elsheikh, Ahmed H.; Wheeler, Mary F.; Hoteit, Ibrahim

2014-01-01

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

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.

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.

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.

Sample preparation of energy materials for X-ray nanotomography with micromanipulation.

Science.gov (United States)

Chen-Wiegart, Yu-chen Karen; Camino, Fernando E; Wang, Jun

2014-06-06

X-ray nanotomography presents an unprecedented opportunity to study energy storage/conversion materials at nanometer scales in three dimensions, with both elemental and chemical sensitivity. A critical step in obtaining high-quality X-ray nanotomography data is reliable sample preparation to ensure that the entire sample fits within the field of view of the X-ray microscope. Although focused-ion-beam lift-out has previously been used for large sample (few to tens of microns) preparation, a difficult undercut and lift-out procedure results in a time-consuming sample preparation process. Herein, we propose a much simpler and direct sample preparation method to resolve the issues that block the view of the sample base after milling and during the lift-out process. This method is applied on a solid-oxide fuel cell and a lithium-ion battery electrode, before numerous critical 3D morphological parameters are extracted, which are highly relevant to their electrochemical performance. A broad application of this method for microstructure study with X-ray nanotomography is discussed and presented. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sample preparation optimization in fecal metabolic profiling.

Science.gov (United States)

Deda, Olga; Chatziioannou, Anastasia Chrysovalantou; Fasoula, Stella; Palachanis, Dimitris; Raikos, Νicolaos; Theodoridis, Georgios A; Gika, Helen G

2017-03-15

Metabolomic analysis of feces can provide useful insight on the metabolic status, the health/disease state of the human/animal and the symbiosis with the gut microbiome. As a result, recently there is increased interest on the application of holistic analysis of feces for biomarker discovery. For metabolomics applications, the sample preparation process used prior to the analysis of fecal samples is of high importance, as it greatly affects the obtained metabolic profile, especially since feces, as matrix are diversifying in their physicochemical characteristics and molecular content. However there is still little information in the literature and lack of a universal approach on sample treatment for fecal metabolic profiling. The scope of the present work was to study the conditions for sample preparation of rat feces with the ultimate goal of the acquisition of comprehensive metabolic profiles either untargeted by NMR spectroscopy and GC-MS or targeted by HILIC-MS/MS. A fecal sample pooled from male and female Wistar rats was extracted under various conditions by modifying the pH value, the nature of the organic solvent and the sample weight to solvent volume ratio. It was found that the 1/2 (w f /v s ) ratio provided the highest number of metabolites under neutral and basic conditions in both untargeted profiling techniques. Concerning LC-MS profiles, neutral acetonitrile and propanol provided higher signals and wide metabolite coverage, though extraction efficiency is metabolite dependent. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of sample preparation procedures on metal(loid) fractionation patterns in lichens.

Science.gov (United States)

Kroukamp, E M; Godeto, T W; Forbes, P B C

2017-08-13

The effects of different sample preparation strategies and storage on metal(loid) fractionation trends in plant material is largely underresearched. In this study, a bulk sample of lichen Parmotrema austrosinense (Zahlbr.) Hale was analysed for its total extractable metal(loid) content by ICP-MS, and was determined to be adequately homogenous (sample were prepared utilising a range of sample preservation techniques and subjected to a modified sequential extraction procedure or to total metal extraction. Both experiments were repeated after 1-month storage at 4 °C. Cryogenic freezing gave the best reproducibility for total extractable elemental concentrations between months, indicating this to be the most suitable method of sample preparation in such studies. The combined extraction efficiencies were >82% for As, Cu, Mn, Pb, Sr and Zn but poor for other elements, where sample preparation strategies 'no sample preparation' and 'dried in a desiccator' had the best extraction recoveries. Cryogenic freezing procedures had a significantly (p sample cleaning and preservation when species fractionation patterns are of interest. This study also shows that the assumption that species stability can be ensured through cryopreservation and freeze drying techniques needs to be revisited.

Preparation of polyhedral oligomeric silsesquioxane based hybrid monoliths by ring-opening polymerization for capillary LC and CEC.

Science.gov (United States)

Lin, Hui; Zhang, Zhenbin; Dong, Jing; Liu, Zhongshan; Ou, Junjie; Zou, Hanfa

2013-09-01

A new organic-inorganic hybrid monolith was prepared by the ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxane (POSS) with 1,4-butanediamine (BDA) using 1-propanol, 1,4-butanediol, and PEG 10,000 as a porogenic system. Benefiting from the moderate phase separation process, the resulting poly(POSS-co-BDA) hybrid monolith possessed a uniform microstructure and exhibited excellent performance in chromatographic applications. Neutral, acidic, and basic compounds were successfully separated on the hybrid monolith in capillary LC (cLC), and high column efficiencies were achieved in all of the separations. In addition, as the amino groups could generate a strong EOF, the hybrid monolith was also applied in CEC for the separation of neutral and polar compounds, and a satisfactory performance was obtained. These results demonstrate that the poly(POSS-co-BDA) hybrid monolith is a good separation media in chromatographic separations of various types of compounds by both cLC and CEC. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In-situ preparation of NaA zeolite/chitosan porous hybrid beads for removal of ammonium from aqueous solution.

Science.gov (United States)

Yang, Kai; Zhang, Xiang; Chao, Cong; Zhang, Bing; Liu, Jindun

2014-07-17

Inorganic/organic hybrid materials play important roles in removal of contaminants from wastewater. Herein, we used the natural materials of halloysite and chitosan to prepare a new adsorbent of NaA zeolite/chitosan porous hybrid beads by in-situ hydrothermal synthesis method. SEM indicated that the porous hybrid beads were composed of 6-8 μm sized cubic NaA zeolite particles congregated together with chitosan. The adsorption behavior of NH4(+) from aqueous solution onto hybrid beads was investigated at different conditions. The Langmuir and Freundlich adsorption models were applied to describe the equilibrium isotherms. A maximum adsorption capacity of 47.62 mg/g at 298 K was achieved according to Langmuir model. The regenerated or reused experiments indicated that the adsorption capacity of the hybrid beads could maintain in 90% above after 10 successive adsorption-desorption cycles. The high adsorption and reusable ability implied potential application of the hybrid beads for removing NH4(+) pollutants from wastewater. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

2018-01-01

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.

Field Sample Preparation Method Development for Isotope Ratio Mass Spectrometry

International Nuclear Information System (INIS)

Leibman, C.; Weisbrod, K.; Yoshida, T.

2015-01-01

Non-proliferation and International Security (NA-241) established a working group of researchers from Los Alamos National Laboratory (LANL), Pacific Northwest National Laboratory (PNNL) and Savannah River National Laboratory (SRNL) to evaluate the utilization of in-field mass spectrometry for safeguards applications. The survey of commercial off-the-shelf (COTS) mass spectrometers (MS) revealed no instrumentation existed capable of meeting all the potential safeguards requirements for performance, portability, and ease of use. Additionally, fieldable instruments are unlikely to meet the International Target Values (ITVs) for accuracy and precision for isotope ratio measurements achieved with laboratory methods. The major gaps identified for in-field actinide isotope ratio analysis were in the areas of: 1. sample preparation and/or sample introduction, 2. size reduction of mass analyzers and ionization sources, 3. system automation, and 4. decreased system cost. Development work in 2 through 4, numerated above continues, in the private and public sector. LANL is focusing on developing sample preparation/sample introduction methods for use with the different sample types anticipated for safeguard applications. Addressing sample handling and sample preparation methods for MS analysis will enable use of new MS instrumentation as it becomes commercially available. As one example, we have developed a rapid, sample preparation method for dissolution of uranium and plutonium oxides using ammonium bifluoride (ABF). ABF is a significantly safer and faster alternative to digestion with boiling combinations of highly concentrated mineral acids. Actinides digested with ABF yield fluorides, which can then be analyzed directly or chemically converted and separated using established column chromatography techniques as needed prior to isotope analysis. The reagent volumes and the sample processing steps associated with ABF sample digestion lend themselves to automation and field

Sample Preparation Strategies for the Effective Quantitation of Hydrophilic Metabolites in Serum by Multi-Targeted HILIC-MS/MS

Directory of Open Access Journals (Sweden)

Elisavet Tsakelidou

2017-03-01

Full Text Available The effect of endogenous interferences of serum in multi-targeted metabolite profiling HILIC-MS/MS analysis was investigated by studying different sample preparation procedures. A modified QuEChERS dispersive SPE protocol, a HybridSPE protocol, and a combination of liquid extraction with protein precipitation were compared to a simple protein precipitation. Evaluation of extraction efficiency and sample clean-up was performed for all methods. SPE sorbent materials tested were found to retain hydrophilic analytes together with endogenous interferences, thus additional elution steps were needed. Liquid extraction was not shown to minimise matrix effects. In general, it was observed that a balance should be reached in terms of recovery, efficient clean-up, and sample treatment time when a wide range of metabolites are analysed. A quick step for removing phospholipids prior to the determination of hydrophilic endogenous metabolites is required, however, based on the results from the applied methods, further studies are needed to achieve high recoveries for all metabolites.

Choice and preparation of standard samples for X-ray spectral microanalysis

International Nuclear Information System (INIS)

Gavrilenko, I.S.; Surzhko, V.F.

1989-01-01

Choice, preparation and certification of standard samples for X-ray spectral microanalysis are considered. Requirements for standard samples in terms of concentration and volume, porosity, corrosion, conductivity distribution are formulated. Stages of sample preparation process, including composition choice, heat treatment, section production, certification, are considered in detail. The choice of composition is based on studying phase equilibrium diagrams, subdivided into 6 types

Novel strategies for sample preparation in forensic toxicology.

Science.gov (United States)

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

2011-09-01

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

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.

TEM sample preparation by FIB for carbon nanotube interconnects

International Nuclear Information System (INIS)

Ke, Xiaoxing; Bals, Sara; Romo Negreira, Ainhoa; Hantschel, Thomas; Bender, Hugo; Van Tendeloo, Gustaaf

2009-01-01

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

TEM sample preparation by FIB for carbon nanotube interconnects

Energy Technology Data Exchange (ETDEWEB)

Ke, Xiaoxing, E-mail: xiaoxing.ke@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Bals, Sara [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Romo Negreira, Ainhoa [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Metallurgy and Materials Engineering Department, KU Leuven, Kasteelpark Arenberg 44, Leuven B-3001 (Belgium); Hantschel, Thomas; Bender, Hugo [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Van Tendeloo, Gustaaf [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium)

2009-10-15

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

Supporting Sampling and Sample Preparation Tools for Isotope and Nuclear Analysis

International Nuclear Information System (INIS)

2016-03-01

Nuclear and related techniques can help develop climate-smart agricultural practices by optimizing water and nutrient use efficiency, assessing organic carbon sequestration in soil, and assisting in the evaluation of soil erosion control measures. Knowledge on the behaviour of radioactive materials in soil, water and foodstuffs is also essential in enhancing nuclear emergency preparedness and response. Appropriate sampling and sample preparation are the first steps to ensure the quality and effective use of the measurements and this publication provides comprehensive detail on the necessary steps

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

Science.gov (United States)

Hernandez-Valladares, Maria; Aasebø, Elise; Selheim, Frode; Berven, Frode S; Bruserud, Øystein

2016-08-22

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.

Development of sample preparation method for honey analysis using PIXE

International Nuclear Information System (INIS)

Saitoh, Katsumi; Chiba, Keiko; Sera, Koichiro

2008-01-01

We developed an original preparation method for honey samples (samples in paste-like state) specifically designed for PIXE analysis. The results of PIXE analysis of thin targets prepared by adding a standard containing nine elements to honey samples demonstrated that the preparation method bestowed sufficient accuracy on quantitative values. PIXE analysis of 13 kinds of honey was performed, and eight mineral components (Si, P, S, K, Ca, Mn, Cu and Zn) were detected in all honey samples. The principal mineral components were K and Ca, and the quantitative value for K accounted for the majority of the total value for mineral components. K content in honey varies greatly depending on the plant source. Chestnuts had the highest K content. In fact, it was 2-3 times that of Manuka, which is known as a high quality honey. K content of false-acacia, which is produced in the greatest abundance, was 1/20 that of chestnuts. (author)

Witness sample preparation for measuring antireflection coatings.

Science.gov (United States)

Willey, Ronald R

2014-02-01

Measurement of antireflection coating of witness samples from across the worldwide industry has been shown to have excess variability from a sampling taken for the OSA Topical Meeting on Optical Interference Coatings: Measurement Problem. Various sample preparation techniques have been discussed with their limitations, and a preferred technique is recommended with its justification, calibration procedures, and limitations. The common practice of grinding the second side to reduce its reflection is less than satisfactory. One recommended practice is to paint the polished second side, which reduces its reflection to almost zero. A method to evaluate the suitability of given paints is also described.

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.

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.

Hybrid Organometallic-Inorganic Nanomaterial: Acetyl Ferrocene Schiff base Immobilized on Silica Coated Magnetite Nanoparticles

Directory of Open Access Journals (Sweden)

M. Masteri-Farahani

2015-10-01

Full Text Available In  this  work,  a  new  hybrid  organometallic-inorganic  hybrid nanomaterial was prepared by immobilization of acetyl ferrocene on the  surface  of magnetite  nanoparticles. Covalent  grafting of silica coated magnetite nanoparticles (SCMNPs with 3-aminopropyl triethoxysilane gave aminopropyl-modified magnetite nanoparticles (AmpSCMNPs. Then, Schiff base condensation  of AmpSCMNPs with acetyl  ferrocene resulted in the preparation of acferro-SCMNPs hybrid nanomaterial. Characterization of the prepared nanomaterial was performed with different physicochemical methods such as Fourier transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, vibrating sample magnetometry (VSM, thermogravimetric analysis (TGA, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. VSM analysis showed superparamagnetic properties of the prepared nanomaterial and TEM and SEM analyses indicated the relatively spherical nanoparticles with 15 nm average size.

Sample preparation techniques of biological material for isotope analysis

International Nuclear Information System (INIS)

Axmann, H.; Sebastianelli, A.; Arrillaga, J.L.

1990-01-01

Sample preparation is an essential step in all isotope-aided experiments but often it is not given enough attention. The methods of sample preparation are very important to obtain reliable and precise analytical data and for further interpretation of results. The size of a sample required for chemical analysis is usually very small (10mg-1500mg). On the other hand the amount of harvested plant material from plots in a field experiment is often bulky (several kilograms) and the entire sample is too large for processing. In addition, while approaching maturity many crops show not only differences in physical consistency but also a non-uniformity in 15 N content among plant parts, requiring a plant fractionation or separation into parts (vegetative and reproductive) e.g. shoots and spikes, in case of small grain cereals, shoots and pods in case of grain legumes and tops and roots or beets (including crown) in case of sugar beet, etc. In any case the ultimate goal of these procedures is to obtain representative subsample harvested from greenhouse or field experiments for chemical analysis. Before harvesting an isotopic-aided experiment the method of sampling has to be selected. It should be based on the type of information required in relation to the objectives of the research and the availability of resources (staff, sample preparation equipment, analytical facilities, chemicals and supplies, etc.). 10 refs, 3 figs, 3 tabs

Preparation of polyethersulfone-organophilic montmorillonite hybrid particles for the removal of bisphenol A

International Nuclear Information System (INIS)

Cao Fuming; Bai Pengli; Li Haocheng; Ma Yunli; Deng Xiaopei; Zhao Changsheng

2009-01-01

Polyethersulfone (PES)-organophilic montmorillonite (OMMT) hybrid particles, with various proportions of OMMT, were prepared by using a liquid-liquid phase separation technique, and then were used for the removal of bisphenol A (BPA) from aqueous solution. The adsorbed BPA amounts increased significantly when the OMMT were embedded into the particles. The structure of the particle was characterized by using scanning electron microscopy (SEM); and these particles hardly release small molecules below 250 deg. C which was testified by using thermogravimetric analysis (TGA). The experimental data of BPA adsorption were adequately fitted with Langmuir equations. Three simplified kinetics model including the pseudo-first-order (Lagergren equation), the pseudo-second-order, and the intraparticle diffusion model were used to describe the adsorption process. Kinetic studies showed that the adsorbed BPA amount reached an equilibrium value after 300 min, and the experimental data could be expressed by the intraparticular mass transfer diffusion model. Furthermore, the adsorbed BPA could be effectively removed by ethanol, which indicated that the hybrid particles could be reused. These results showed that the PES-OMMT hybrid particles have the potential to be used in the environmental application

[Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

Science.gov (United States)

Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

2015-09-01

Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

Considerations for Sample Preparation Using Size-Exclusion Chromatography for Home and Synchrotron Sources.

Science.gov (United States)

Rambo, Robert P

2017-01-01

The success of a SAXS experiment for structural investigations depends on two precise measurements, the sample and the buffer background. Buffer matching between the sample and background can be achieved using dialysis methods but in biological SAXS of monodisperse systems, sample preparation is routinely being performed with size exclusion chromatography (SEC). SEC is the most reliable method for SAXS sample preparation as the method not only purifies the sample for SAXS but also almost guarantees ideal buffer matching. Here, I will highlight the use of SEC for SAXS sample preparation and demonstrate using example proteins that SEC purification does not always provide for ideal samples. Scrutiny of the SEC elution peak using quasi-elastic and multi-angle light scattering techniques can reveal hidden features (heterogeneity) of the sample that should be considered during SAXS data analysis. In some cases, sample heterogeneity can be controlled using a small molecule additive and I outline a simple additive screening method for sample preparation.

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 C 12 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 (IC 50  = 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 C 12 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.

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.

A Method for Microalgae Proteomics Analysis Based on Modified Filter-Aided Sample Preparation.

Science.gov (United States)

Li, Song; Cao, Xupeng; Wang, Yan; Zhu, Zhen; Zhang, Haowei; Xue, Song; Tian, Jing

2017-11-01

With the fast development of microalgal biofuel researches, the proteomics studies of microalgae increased quickly. A filter-aided sample preparation (FASP) method is widely used proteomics sample preparation method since 2009. Here, a method of microalgae proteomics analysis based on modified filter-aided sample preparation (mFASP) was described to meet the characteristics of microalgae cells and eliminate the error caused by over-alkylation. Using Chlamydomonas reinhardtii as the model, the prepared sample was tested by standard LC-MS/MS and compared with the previous reports. The results showed mFASP is suitable for most of occasions of microalgae proteomics studies.

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.

Final Report for X-ray Diffraction Sample Preparation Method Development

Energy Technology Data Exchange (ETDEWEB)

Ely, T. M. [Hanford Site (HNF), Richland, WA (United States); Meznarich, H. K. [Hanford Site (HNF), Richland, WA (United States); Valero, T. [Hanford Site (HNF), Richland, WA (United States)

2018-01-30

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Ring-Opening Polymerization of N-Carboxyanhydrides for Preparation of Polypeptides and Polypeptide-Based Hybrid Materials with Various Molecular Architectures

KAUST Repository

Pahovnik, David; Hadjichristidis, Nikolaos

2015-01-01

Different synthetic approaches utilizing ring-opening polymerization of N-carboxyanhydrides for preparation of polypeptide and polypeptide-based hybrid materials with various molecular architectures are described. An overview of polymerization

Protocol for Cohesionless Sample Preparation for Physical Experimentation

Science.gov (United States)

2016-05-01

Standard test method for consolidated drained triaxial compression test for soils . In Annual book of ASTM standards. West Conshohocken, PA: ASTM...derived wherein uncertainties and laboratory scatter associated with soil fabric-behavior variance during sample preparation are mitigated. Samples of...wherein comparable analysis between different laboratory tests’ results can be made by ensuring a comparable soil fabric prior to laboratory testing

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

Structure and Optical Properties of Titania-PDMS Hybrid Nanocomposites Prepared by In Situ Non-Aqueous Synthesis

Directory of Open Access Journals (Sweden)

Antoine R. M. Dalod

2017-12-01

Full Text Available Organic-inorganic hybrid materials are attractive due to the combination of properties from the two distinct types of materials. In this work, transparent titania-polydimethylsiloxane hybrid materials with up to 15.5 vol. % TiO2 content were prepared by an in situ non-aqueous method using titanium (IV isopropoxide and hydroxy-terminated polydimethylsiloxane as precursors. Spectroscopy (Fourier transform infrared, Raman, Ultraviolet-visible, ellipsometry and small-angle X-ray scattering analysis allowed to describe in detail the structure and the optical properties of the nanocomposites. Titanium alkoxide was successfully used as a cross-linker and titania-like nanodomains with an average size of approximately 4 nm were shown to form during the process. The resulting hybrid nanocomposites exhibit high transparency and tunable refractive index from 1.42 up to 1.56, depending on the titania content.

Preparation and characterization of carbon nanotube-hybridized carbon fiber to reinforce epoxy composite

International Nuclear Information System (INIS)

An, Feng; Lu, Chunxiang; Li, Yonghong; Guo, Jinhai; Lu, Xiaoxuan; Lu, Huibin; He, Shuqing; Yang, Yu

2012-01-01

Highlights: → CNTs were uniformly grown onto the carbon fibers. → No obvious mechanical properties of carbon fiber were observed after CNT growth. → The IFSS of multiscale epoxy composite was measured by single fiber pull-out tests. → Observing fractography of composite, the fracture modes of CNTs were discussed. -- Abstract: The multiscale carbon nanotube-hybridized carbon fiber was prepared by a newly developed aerosol-assisted chemical vapour deposition. Scanning electron microscopy and transmission electron microscope were carried out to characterize this multiscale material. Compared with the original carbon fibers, the fabrication of this hybrid fiber resulted in an almost threefold increase of BET surface area to reach 2.22 m 2 /g. Meanwhile, there was a slight degradation of fiber tensile strength within 10%, while the fiber modulus was not significantly affected. The interfacial shearing strength of a carbon fiber-reinforced polymer composite with carbon nanotube-hybridized carbon fiber and an epoxy matrix was determined from the single fiber pull-out tests of microdroplet composite. Due to an efficient increase of load transfer at the fiber/matrix interfaces, the interracial shear strength of composite reinforced by carbon nanotube-hybridized carbon fiber is almost 94% higher than that of one reinforced by the original carbon fiber. Based on the fractured morphologies of the composites, the interfacial reinforcing mechanisms were discussed through proposing different types of carbon nanotube fracture modes along with fiber pulling out from epoxy composites.

Challenges in TEM sample preparation of solvothermally grown CuInS2 films.

Science.gov (United States)

Frank, Anna; Changizi, Rasa; Scheu, Christina

2018-06-01

Transmission electron microscopy (TEM) is a widely used tool to characterize materials. The required samples need to be electron transparent which should be achieved without changing the microstructure. This work describes different TEM sample preparation techniques of nanostructured CuInS 2 thin films on fluorine-doped tin oxide substrates, synthesized solvothermally using l-cysteine as sulfur source. Focused ion beam lamellae, conventional cross section samples and scratch samples have been prepared and investigated. It was possible to prepare appropriate samples with each technique, however, each technique brings with it certain advantages and disadvantages. FIB preparation of solvothermally synthesized CuInS 2 suffers from two main drawbacks. First, the whole CuInS 2 layer displays a strongly increased Cu content caused by Cu migration and preferential removal of In. Further, electron diffraction shows the formation of an additional CuS phase after Ga + bombardment. Second, diffraction analysis is complicated by a strong contribution of crystalline Pt introduced during the FIB preparation and penetrating into the porous film surface. The conventional cross sectional CuInS 2 sample also shows a Cu signal enhancement which is caused by contribution of the brass tube material used for embedding. Additionally, Cu particles have been observed inside the CuInS 2 which have been sputtered on the film during preparation. Only the scratch samples allow an almost artefact-free and reliable elemental quantification using energy-dispersive X-ray spectroscopy. However, scratch samples suffer from the drawback that it is not possible to determine the layer thickness, which is possible for both cross sectional preparation techniques. Consequently, it is concluded that the type of sample preparation should be chosen dependent on the required information. A full characterization can only be achieved when the different techniques are combined. Copyright © 2018 Elsevier Ltd. All

Perspectives of an acoustic–electrostatic/electrodynamic hybrid levitator for small fluid and solid samples

International Nuclear Information System (INIS)

Lierke, E G; Holitzner, L

2008-01-01

The feasibility of an acoustic–electrostatic hybrid levitator for small fluid and solid samples is evaluated. A proposed design and its theoretical assessment are based on the optional implementation of simple hardware components (ring electrodes) and standard laboratory equipment into typical commercial ultrasonic standing wave levitators. These levitators allow precise electrical charging of drops during syringe- or ink-jet-type deployment. The homogeneous electric 'Millikan field' between the grounded ultrasonic transducer and the electrically charged reflector provide an axial compensation of the sample weight in an indifferent equilibrium, which can be balanced by using commercial optical position sensors in combination with standard electronic PID position control. Radial electrostatic repulsion forces between the charged sample and concentric ring electrodes of the same polarity provide stable positioning at the centre of the levitator. The levitator can be used in a pure acoustic or electrostatic mode or in a hybrid combination of both subsystems. Analytical evaluations of the radial–axial force profiles are verified with detailed numerical finite element calculations under consideration of alternative boundary conditions. The simple hardware modification with implemented double-ring electrodes in ac/dc operation is also feasible for an electrodynamic/acoustic hybrid levitator

Automated SEM and TEM sample preparation applied to copper/low k materials

Science.gov (United States)

Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

2001-01-01

We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

Polymeric ionic liquid-based portable tip microextraction device for on-site sample preparation of water samples.

Science.gov (United States)

Chen, Lei; Pei, Junxian; Huang, Xiaojia; Lu, Min

2018-06-05

On-site sample preparation is highly desired because it avoids the transportation of large-volume samples and ensures the accuracy of the analytical results. In this work, a portable prototype of tip microextraction device (TMD) was designed and developed for on-site sample pretreatment. The assembly procedure of TMD is quite simple. Firstly, polymeric ionic liquid (PIL)-based adsorbent was in-situ prepared in a pipette tip. After that, the tip was connected with a syringe which was driven by a bidirectional motor. The flow rates in adsorption and desorption steps were controlled accurately by the motor. To evaluate the practicability of the developed device, the TMD was used to on-site sample preparation of waters and combined with high-performance liquid chromatography with diode array detection to measure trace estrogens in water samples. Under the most favorable conditions, the limits of detection (LODs, S/N = 3) for the target analytes were in the range of 4.9-22 ng/L, with good coefficients of determination. Confirmatory study well evidences that the extraction performance of TMD is comparable to that of the traditional laboratory solid-phase extraction process, but the proposed TMD is more simple and convenient. At the same time, the TMD avoids complicated sampling and transferring steps of large-volume water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Optimization of Sample Preparation processes of Bone Material for Raman Spectroscopy.

Science.gov (United States)

Chikhani, Madelen; Wuhrer, Richard; Green, Hayley

2018-03-30

Raman spectroscopy has recently been investigated for use in the calculation of postmortem interval from skeletal material. The fluorescence generated by samples, which affects the interpretation of Raman data, is a major limitation. This study compares the effectiveness of two sample preparation techniques, chemical bleaching and scraping, in the reduction of fluorescence from bone samples during testing with Raman spectroscopy. Visual assessment of Raman spectra obtained at 1064 nm excitation following the preparation protocols indicates an overall reduction in fluorescence. Results demonstrate that scraping is more effective at resolving fluorescence than chemical bleaching. The scraping of skeletonized remains prior to Raman analysis is a less destructive method and allows for the preservation of a bone sample in a state closest to its original form, which is beneficial in forensic investigations. It is recommended that bone scraping supersedes chemical bleaching as the preferred method for sample preparation prior to Raman spectroscopy. © 2018 American Academy of Forensic Sciences.

Magnetic separation techniques in sample preparation for biological analysis: a review.

Science.gov (United States)

He, Jincan; Huang, Meiying; Wang, Dongmei; Zhang, Zhuomin; Li, Gongke

2014-12-01

Sample preparation is a fundamental and essential step in almost all the analytical procedures, especially for the analysis of complex samples like biological and environmental samples. In past decades, with advantages of superparamagnetic property, good biocompatibility and high binding capacity, functionalized magnetic materials have been widely applied in various processes of sample preparation for biological analysis. In this paper, the recent advancements of magnetic separation techniques based on magnetic materials in the field of sample preparation for biological analysis were reviewed. The strategy of magnetic separation techniques was summarized. The synthesis, stabilization and bio-functionalization of magnetic nanoparticles were reviewed in detail. Characterization of magnetic materials was also summarized. Moreover, the applications of magnetic separation techniques for the enrichment of protein, nucleic acid, cell, bioactive compound and immobilization of enzyme were described. Finally, the existed problems and possible trends of magnetic separation techniques for biological analysis in the future were proposed. Copyright © 2014 Elsevier B.V. All rights reserved.

State of the art in sample preparation for trace element analysis (M1)

International Nuclear Information System (INIS)

Barnes, R.M.

2002-01-01

Full text: The accelerated capabilities of modern trace element analysis techniques, especially inductively coupled plasma mass spectrometry (ICP-MS), have challenged the sample preparation competence of most laboratories. Exceptional analytical sensitivity, remarkable analysis speed, automated sample presentation, and intelligent sample sequencing of modern spectroscopic instrumentation have lead to demanding requirements for appropriate sample preparation steps needed for ultra trace concentration and speciation measurements. Contamination control, reliable digestion and extraction techniques, presentation of chemical forms, sample matrix management, and intelligent sample processing available today are often inadequate for the most demanding measurements. Some commercial instrumentation provides convenient implementation of well-established contamination control measures, and reagent and container purity are steadily being improved. Direct sample introduction approaches offer alternatives to conventional solution samples, but achieving calibration reliability is difficult. Developing new sample preparation chemistry is especially arduous and rare, yet progress exists in characterizing microwave-assisted reactions. This presentation will describe contemporary targets for modern sample preparation approaches for ultra trace elemental analysis and the likelihood that they can be reasonably achieved. (author)

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.

The effect of sample preparation methods on glass performance

International Nuclear Information System (INIS)

Oh, M.S.; Oversby, V.M.

1990-01-01

A series of experiments was conducted using SRL 165 synthetic waste glass to investigate the effects of surface preparation and leaching solution composition on the alteration of the glass. Samples of glass with as-cast surfaces produced smooth reaction layers and some evidence for precipitation of secondary phases from solution. Secondary phases were more abundant in samples reacted in deionized water than for those reacted in a silicate solution. Samples with saw-cut surfaces showed a large reduction in surface roughness after 7 days of reaction in either solution. Reaction in silicate solution for up to 91 days produced no further change in surface morphology, while reaction in DIW produced a spongy surface that formed the substrate for further surface layer development. The differences in the surface morphology of the samples may create microclimates that control the details of development of alteration layers on the glass; however, the concentrations of elements in leaching solutions show differences of 50% or less between samples prepared with different surface conditions for tests of a few months duration. 6 refs., 7 figs., 1 tab

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.

Sample preparation procedures utilized in microbial metabolomics: An overview.

Science.gov (United States)

Patejko, Małgorzata; Jacyna, Julia; Markuszewski, Michał J

2017-02-01

Bacteria are remarkably diverse in terms of their size, structure and biochemical properties. Due to this fact, it is hard to develop a universal method for handling bacteria cultures during metabolomic analysis. The choice of suitable processing methods constitutes a key element in any analysis, because only appropriate selection of procedures may provide accurate results, leading to reliable conclusions. Because of that, every analytical experiment concerning bacteria requires individually and very carefully planned research methodology. Although every study varies in terms of sample preparation, there are few general steps to follow while planning experiment, like sampling, separation of cells from growth medium, stopping their metabolism and extraction. As a result of extraction, all intracellular metabolites should be washed out from cell environment. What is more, extraction method utilized cannot cause any chemical decomposition or degradation of the metabolome. Furthermore, chosen extraction method should correlate with analytical technique, so it will not disturb or prolong following sample preparation steps. For those reasons, we observe a need to summarize sample preparation procedures currently utilized in microbial metabolomic studies. In the presented overview, papers concerning analysis of extra- and intracellular metabolites, published over the last decade, have been discussed. Presented work gives some basic guidelines that might be useful while planning experiments in microbial metabolomics. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation techniques for (p, X) spectrometry

International Nuclear Information System (INIS)

Whitehead, N.E.

1985-01-01

Samples are ashed at low temperature, using oxygen plasma; a rotary evaporator, and freeze drying speeded up the ashing. The new design of apparatus manufactured was only 10 watt but was as efficient as a 200 watt commercial machine; a circuit diagram is included. Samples of hair and biopsy samples of skin were analysed by the technique. A wool standard was prepared for interlaboratory comparison exercises. It was based on New Zealand merino sheep wool and was 2.9 kg in weight. A washing protocol was developed, which preserves most of the trace element content. The wool was ground in liquid nitrogen using a plastic pestle and beaker, driven by a rotary drill press. (author)

Report: Optimization study of the preparation factors for argan oil microcapsule based on hybrid-level orthogonal array design via SPSS modeling.

Science.gov (United States)

Zhao, Xi; Wu, Xiaoli; Zhou, Hui; Jiang, Tao; Chen, Chun; Liu, Mingshi; Jin, Yuanbao; Yang, Dongsheng

2014-11-01

To optimize the preparation factors for argan oil microcapsule using complex coacervation of chitosan cross-linked with gelatin based on hybrid-level orthogonal array design via SPSS modeling. Eight relatively significant factors were firstly investigated and selected as calculative factors for the orthogonal array design from the total of ten factors effecting the preparation of argan oil microcapsule by utilizing the single factor variable method. The modeling of hybrid-level orthogonal array design was built in these eight factors with the relevant levels (9, 9, 9, 9, 7, 6, 2 and 2 respectively). The preparation factors for argan oil microcapsule were investigated and optimized according to the results of hybrid-level orthogonal array design. The priorities order and relevant optimum levels of preparation factors standard to base on the percentage of microcapsule with the diameter of 30~40 μm via SPSS. Experimental data showed that the optimum factors were controlling the chitosan/gelatin ratio, the systemic concentration and the core/shell ratio at 1:2, 1.5% and 1:7 respectively, presetting complex coacervation pH at 6.4, setting cross-linking time and complex coacervation at 75 min and 30 min, using the glucose-delta lactone as the type of cross-linking agent, and selecting chitosan with the molecular weight of 2000～3000.

Luminescent Eosin Y–SiO2 hybrid nano and microrods prepared by sol–gel template method

International Nuclear Information System (INIS)

Secu, M.; Secu, C.E.; Sima, M.; Negrea, R.F.; Bartha, C.; Dinescu, M.; Damian, V.

2013-01-01

Sol–gel chemistry within the pores of a polycarbonate template membrane was used for the preparation of Eosin Y–SiO 2 hybrid nano- and microrods, using tetraethylorthosilicate [TEOS, Si(OC 2 H 5 ) 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 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 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

Preparation and photocatalytic properties of hybrid core–shell reusable CoFe2O4–ZnO nanospheres

International Nuclear Information System (INIS)

Wilson, A.; Mishra, S.R.; Gupta, R.; Ghosh, K.

2012-01-01

Magnetically separable and reusable core–shell CoFe 2 O 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 2 O 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: ► Synthesis of novel hybrid magnetic-ZnO core–shell composite nanospheres. ► High photocatalytic activity of hybrid nanospheres was noted as compared to that of pure ZnO nanoparticles. ► The hybrid nanospheres could be easily retrieved using an external magnet for repeated use. ► Repeated use of hybrid nanospheres did not show any degradation in the photocatalytic activity. ► The photocatalysis rate was observed to be ZnO shell thickness dependent.

Traceability and measurement uncertainty in sample preparation (W5)

International Nuclear Information System (INIS)

Wegscheider, W.; Walner, U.; Moser, J.

2002-01-01

Full text: Very few chemical measurements are being made directly on the object of interest and sample preparation is thus the rule rather than the exception in daily practice. Unfortunately the operations undertaken in the course of sample preparation are prone to rendering a sample useless for the purpose of interpreting a measurement performed on it, as it might not represent the original and relevant status any longer. Sample preparation along with sampling itself constitutes therefore a procedure that leads to a loss of representation of the original specimen or population. On the other hand it is also not sufficient to confine aspects of traceability and measurement uncertainty to the ultimate measurement, as the key purpose of measuring is to supply adequate data for some kind of decision, be it in production, in health, in the environment, or indeed in any other circumstance. These considerations have led to severe confusion in the community as to what traceability really means in chemistry. CITAC and EURACHEM have only recently issued a preliminary document that clarifies these issues and gives a firm handle on the future development of quality assurance in analytical chemistry. In this talk it will be attempted to outline the general ideas and procedures that lead to traceability of analytical chemical results accompanied by valid statements of their uncertainty. It will be argued that the central element in achieving these goals is a well-designed validation study that frequently goes beyond those requirements currently laid out in official documents. (author)

Preparation and optical and electrical evaluation of bulk SiO2 sonogel hybrid composites and vacuum thermal evaporated thin films prepared from molecular materials derived from (Fe, Co) metallic phthalocyanines and 1,8 dihydroxiantraquinone compounds

International Nuclear Information System (INIS)

Sanchez Vergara, Maria Elena; Morales-Saavedra, Omar G.; Ontiveros-Barrera, Fernando G.; Torres-Zuniga, Vicente; Ortega-Martinez, Roberto; Ortiz Rebollo, Armando

2009-01-01

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 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 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

Mechanical Conversion for High-Throughput TEM Sample Preparation

International Nuclear Information System (INIS)

Kendrick, Anthony B; Moore, Thomas M; Zaykova-Feldman, Lyudmila

2006-01-01

This paper presents a novel method of direct mechanical conversion from lift-out sample to TEM sample holder. The lift-out sample is prepared in the FIB using the in-situ liftout Total Release TM method. The mechanical conversion is conducted using a mechanical press and one of a variety of TEM coupons, including coupons for both top-side and back-side thinning. The press joins a probe tip point with attached TEM sample to the sample coupon and separates the complete assembly as a 3mm diameter TEM grid, compatible with commercially available TEM sample holder rods. This mechanical conversion process lends itself well to the high through-put requirements of in-line process control and to materials characterization labs where instrument utilization and sample security are critically important

40 CFR 205.171-2 - Test exhaust system sample selection and preparation.

Science.gov (United States)

2010-07-01

... Systems § 205.171-2 Test exhaust system sample selection and preparation. (a)(1) Exhaust systems... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Test exhaust system sample selection and preparation. 205.171-2 Section 205.171-2 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY...

Droplet Size-Aware and Error-Correcting Sample Preparation Using Micro-Electrode-Dot-Array Digital Microfluidic Biochips.

Science.gov (United States)

Li, Zipeng; Lai, Kelvin Yi-Tse; Chakrabarty, Krishnendu; Ho, Tsung-Yi; Lee, Chen-Yi

2017-12-01

Sample preparation in digital microfluidics refers to the generation of droplets with target concentrations for on-chip biochemical applications. In recent years, digital microfluidic biochips (DMFBs) have been adopted as a platform for sample preparation. However, there remain two major problems associated with sample preparation on a conventional DMFB. First, only a (1:1) mixing/splitting model can be used, leading to an increase in the number of fluidic operations required for sample preparation. Second, only a limited number of sensors can be integrated on a conventional DMFB; as a result, the latency for error detection during sample preparation is significant. To overcome these drawbacks, we adopt a next generation DMFB platform, referred to as micro-electrode-dot-array (MEDA), for sample preparation. We propose the first sample-preparation method that exploits the MEDA-specific advantages of fine-grained control of droplet sizes and real-time droplet sensing. Experimental demonstration using a fabricated MEDA biochip and simulation results highlight the effectiveness of the proposed sample-preparation method.

Identification of a novel interspecific hybrid yeast from a metagenomic spontaneously inoculated beer sample using Hi-C.

Science.gov (United States)

Smukowski Heil, Caiti; Burton, Joshua N; Liachko, Ivan; Friedrich, Anne; Hanson, Noah A; Morris, Cody L; Schacherer, Joseph; Shendure, Jay; Thomas, James H; Dunham, Maitreya J

2018-01-01

Interspecific hybridization is a common mechanism enabling genetic diversification and adaptation; however, the detection of hybrid species has been quite difficult. The identification of microbial hybrids is made even more complicated, as most environmental microbes are resistant to culturing and must be studied in their native mixed communities. We have previously adapted the chromosome conformation capture method Hi-C to the assembly of genomes from mixed populations. Here, we show the method's application in assembling genomes directly from an uncultured, mixed population from a spontaneously inoculated beer sample. Our assembly method has enabled us to de-convolute four bacterial and four yeast genomes from this sample, including a putative yeast hybrid. Downstream isolation and analysis of this hybrid confirmed its genome to consist of Pichia membranifaciens and that of another related, but undescribed, yeast. Our work shows that Hi-C-based metagenomic methods can overcome the limitation of traditional sequencing methods in studying complex mixtures of genomes. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

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 (ZrO 2 -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 ZrCl 4 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 ZrO 2 -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. Copyright © 2016 Elsevier B.V. All rights reserved.

Automated Blood Sample Preparation Unit (ABSPU) for Portable Microfluidic Flow Cytometry.

Science.gov (United States)

Chaturvedi, Akhil; Gorthi, Sai Siva

2017-02-01

Portable microfluidic diagnostic devices, including flow cytometers, are being developed for point-of-care settings, especially in conjunction with inexpensive imaging devices such as mobile phone cameras. However, two pervasive drawbacks of these have been the lack of automated sample preparation processes and cells settling out of sample suspensions, leading to inaccurate results. We report an automated blood sample preparation unit (ABSPU) to prevent blood samples from settling in a reservoir during loading of samples in flow cytometers. This apparatus automates the preanalytical steps of dilution and staining of blood cells prior to microfluidic loading. It employs an assembly with a miniature vibration motor to drive turbulence in a sample reservoir. To validate performance of this system, we present experimental evidence demonstrating prevention of blood cell settling, cell integrity, and staining of cells prior to flow cytometric analysis. This setup is further integrated with a microfluidic imaging flow cytometer to investigate cell count variability. With no need for prior sample preparation, a drop of whole blood can be directly introduced to the setup without premixing with buffers manually. Our results show that integration of this assembly with microfluidic analysis provides a competent automation tool for low-cost point-of-care blood-based diagnostics.

Error Analysis of Ceramographic Sample Preparation for Coating Thickness Measurement of Coated Fuel Particles

International Nuclear Information System (INIS)

Liu Xiaoxue; Li Ziqiang; Zhao Hongsheng; Zhang Kaihong; Tang Chunhe

2014-01-01

The thicknesses of four coatings of HTR coated fuel particle are very important parameters. It is indispensable to control the thickness of four coatings of coated fuel particles for the safety of HTR. A measurement method, ceramographic sample-microanalysis method, to analyze the thickness of coatings was developed. During the process of ceramographic sample-microanalysis, there are two main errors, including ceramographic sample preparation error and thickness measurement error. With the development of microscopic techniques, thickness measurement error can be easily controlled to meet the design requirements. While, due to the coated particles are spherical particles of different diameters ranged from 850 to 1000μm, the sample preparation process will introduce an error. And this error is different from one sample to another. It’s also different from one particle to another in the same sample. In this article, the error of the ceramographic sample preparation was calculated and analyzed. Results show that the error introduced by sample preparation is minor. The minor error of sample preparation guarantees the high accuracy of the mentioned method, which indicates this method is a proper method to measure the thickness of four coatings of coated particles. (author)

Miniaturizing EM Sample Preparation: Opportunities, Challenges, and "Visual Proteomics".

Science.gov (United States)

Arnold, Stefan A; Müller, Shirley A; Schmidli, Claudio; Syntychaki, Anastasia; Rima, Luca; Chami, Mohamed; Stahlberg, Henning; Goldie, Kenneth N; Braun, Thomas

2018-03-01

This review compares and discusses conventional versus miniaturized specimen preparation methods for transmission electron microscopy (TEM). The progress brought by direct electron detector cameras, software developments and automation have transformed transmission cryo-electron microscopy (cryo-EM) and made it an invaluable high-resolution structural analysis tool. In contrast, EM specimen preparation has seen very little progress in the last decades and is now one of the main bottlenecks in cryo-EM. Here, we discuss the challenges faced by specimen preparation for single particle EM, highlight current developments, and show the opportunities resulting from the advanced miniaturized and microfluidic sample grid preparation methods described, such as visual proteomics and time-resolved cryo-EM studies. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimized preparation of urine samples for two-dimensional electrophoresis and initial application to patient samples

DEFF Research Database (Denmark)

Lafitte, Daniel; Dussol, Bertrand; Andersen, Søren

2002-01-01

OBJECTIVE: We optimized of the preparation of urinary samples to obtain a comprehensive map of urinary proteins of healthy subjects and then compared this map with the ones obtained with patient samples to show that the pattern was specific of their kidney disease. DESIGN AND METHODS: The urinary...

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.

Ring-Opening Polymerization of N-Carboxyanhydrides for Preparation of Polypeptides and Polypeptide-Based Hybrid Materials with Various Molecular Architectures

KAUST Repository

Pahovnik, David

2015-09-01

Different synthetic approaches utilizing ring-opening polymerization of N-carboxyanhydrides for preparation of polypeptide and polypeptide-based hybrid materials with various molecular architectures are described. An overview of polymerization mechanisms using conventional (various amines) as well as some recently developed initiators (hexamethyldisilazane, N-heterocyclic persistent carbenes, etc.) is presented, and their benefits and drawbacks for preparation of polypeptides with well-defined chain lengths and chain-end functionality are discussed. Recent examples from literature are used to illustrate different possibilities for synthesis of pure polypeptide materials with different molecular architectures bearing various functional groups, which are introduced either by modification of amino acids, before they are transformed into corresponding Ncarboxyanhydrides, or by post-polymerization modifications using protective groups and/or orthogonal functional groups. Different approaches for preparation of polypeptide-based hybrid materials are discussed as well using examples from recent literature. Syntheses of simple block copolymers or copolymers with more complex molecular architectures (graft and star copolymers) as well as modifications of nanoparticles and other surfaces with polypeptides are described.

Analytical characterization of high-level mixed wastes using multiple sample preparation treatments

International Nuclear Information System (INIS)

King, A.G.; Baldwin, D.L.; Urie, M.W.; McKinley, S.G.

1994-01-01

The Analytical Chemistry Laboratory at the Pacific Northwest Laboratory in Richland, Washington, is actively involved in performing analytical characterization of high-level mixed waste from Hanford's single shell and double shell tank characterization programs. A full suite of analyses is typically performed on homogenized tank core samples. These analytical techniques include inductively-coupled plasma-atomic emission spectroscopy, total organic carbon methods and radiochemistry methods, as well as many others, all requiring some type of remote sample-preparation treatment to solubilize the tank sludge material for analysis. Most of these analytical methods typically use a single sample-preparation treatment, inherently providing elemental information only. To better understand and interpret tank chemistry and assist in identifying chemical compounds, selected analytical methods are performed using multiple sample-preparation treatments. The sample preparation treatments used at Pacific Northwest Laboratory for this work with high-level mixed waste include caustic fusion, acid digestion, and water leach. The type of information available by comparing results from different sample-prep treatments includes evidence for the presence of refractory compounds, acid-soluble compounds, or water-soluble compounds. Problems unique to the analysis of Hanford tank wastes are discussed. Selected results from the Hanford single shell ferrocyanide tank, 241-C-109, are presented, and the resulting conclusions are discussed

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.

Novel sample preparation for operando TEM of catalysts

International Nuclear Information System (INIS)

Miller, Benjamin K.; Barker, Trevor M.; Crozier, Peter A.

2015-01-01

A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. - Highlights: • High in-situ conversion of CO to CO 2 achieved by a novel TEM sample preparation method. • A 3 mm fiber pellet increases the TEM sample surface area by 50×. • Operando atomic resolution is maintained by also including a 3 mm grid in the sample. • Evidence for a well-mixed gas composition inside the ETEM cell is given

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.

Extraordinary Hall effect in Co implanted GaAs hybrid magnetic semiconductors

International Nuclear Information System (INIS)

Honda, S.; Tateishi, K.; Nawate, M.; Sakamoto, I.

2004-01-01

Hybrid Co/GaAs ferromagnetic semiconductors have been prepared by implantation method. In these samples, sheet resistance shows weak temperature dependence, and the extraordinary Hall effect with positive coefficient is observed. In small Co content samples, Hall resistance increases with decreasing temperature and maximum value of 3.6x10 -2 Ω is obtained at 150 K

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

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......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...... weather conditions. The results show that radiated heat loss from the front surface and the convective heat loss due to the wind speed are the most critical parameters on performance of the hybrid panel performance. The results also indicate that, with existing thermoelectric materials, the power...

Effective Enrichment and Detection of Trace Polycyclic Aromatic Hydrocarbons in Food Samples based on Magnetic Covalent Organic Framework Hybrid Microspheres.

Science.gov (United States)

Li, Ning; Wu, Di; Hu, Na; Fan, Guangsen; Li, Xiuting; Sun, Jing; Chen, Xuefeng; Suo, Yourui; Li, Guoliang; Wu, Yongning

2018-04-04

The present study reported a facile, sensitive, and efficient method for enrichment and determination of trace polycyclic aromatic hydrocarbons (PAHs) in food samples by employing new core-shell nanostructure magnetic covalent organic framework hybrid microspheres (Fe 3 O 4 @COF-(TpBD)) as the sorbent followed by HPLC-DAD. Under mild synthetic conditions, the Fe 3 O 4 @COF-(TpBD) were prepared with the retention of colloidal nanosize, larger specific surface area, higher porosity, uniform morphology, and supermagnetism. The as-prepared materials showed an excellent adsorption ability for PAHs, and the enrichment efficiency of the Fe 3 O 4 @COF-(TpBD) could reach 99.95%. The obtained materials also had fast adsorption kinetics and realized adsorption equilibrium within 12 min. The eluent was further analyzed by HPLC-DAD, and good linearity was observed in the range of 1-100 ng/mL with the linear correlation being above 0.9990. The limits of detection (S/N = 3) and limits of quantitation (S/N = 10) for 15 PAHs were in the range of 0.83-11.7 ng/L and 2.76-39.0 ng/L, respectively. For the application, the obtained materials were employed for the enrichment of trace PAHs in food samples and exhibited superior enrichment capacity and excellent applicability.

Modern methods of sample preparation for GC analysis

NARCIS (Netherlands)

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

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

Collection and preparation of wet and dry stream-sediment samples

International Nuclear Information System (INIS)

Puchlik, K.

1977-03-01

Lawrence Livermore Laboratory is responsible for the Hydrogeochemistry and Stream Sediment Reconnaissance (HSSR) program for uranium in the seven far western states. The work thus far has concentrated on the arid to semi-arid regions of the West and this paper discusses the collection and preparation of sediment samples in the Basin and Range province. The sample collection and preparation procedures described here may not be applicable to other parts of the far western states or other areas. These procedures also differ somewhat from those used by the other three laboratories involved in the HSSR program

Sampling and sample preparation methods for the analysis of trace elements in biological material

International Nuclear Information System (INIS)

Sansoni, B.; Iyengar, V.

1978-05-01

The authors attempt to give a most systamtic possible treatment of the sample taking and sample preparation of biological material (particularly in human medicine) for trace analysis (e.g. neutron activation analysis, atomic absorption spectrometry). Contamination and loss problems are discussed as well as the manifold problems of the different consistency of solid and liquid biological materials, as well as the stabilization of the sample material. The process of dry and wet ashing is particularly dealt with, where new methods are also described. (RB) [de

Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

Science.gov (United States)

Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

2015-05-11

In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

Automated dried blood spots standard and QC sample preparation using a robotic liquid handler.

Science.gov (United States)

Yuan, Long; Zhang, Duxi; Aubry, Anne-Francoise; Arnold, Mark E

2012-12-01

A dried blood spot (DBS) bioanalysis assay involves many steps, such as the preparation of standard (STD) and QC samples in blood, the spotting onto DBS cards, and the cutting-out of the spots. These steps are labor intensive and time consuming if done manually, which, therefore, makes automation very desirable in DBS bioanalysis. A robotic liquid handler was successfully applied to the preparation of STD and QC samples in blood and to spot the blood samples onto DBS cards using buspirone as the model compound. This automated preparation was demonstrated to be accurate and consistent. However the accuracy and precision of automated preparation were similar to those from manual preparation. The effect of spotting volume on accuracy was evaluated and a trend of increasing concentrations of buspirone with increasing spotting volumes was observed. The automated STD and QC sample preparation process significantly improved the efficiency, robustness and safety of DBS bioanalysis.

Green sample preparation for liquid chromatography and capillary electrophoresis of anionic and cationic analytes.

Science.gov (United States)

Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

2015-04-21

A sample preparation device for the simultaneous enrichment and separation of cationic and anionic analytes was designed and implemented in an eight-channel configuration. The device is based on the use of an electric field to transfer the analytes from a large volume of sample into small volumes of electrolyte that was suspended into two glass micropipettes using a conductive hydrogel. This simple, economical, fast, and green (no organic solvent required) sample preparation scheme was evaluated using cationic and anionic herbicides as test analytes in water. The analytical figures of merit and ecological aspects were evaluated against the state-of-the-art sample preparation, solid-phase extraction. A drastic reduction in both sample preparation time (94% faster) and resources (99% less consumables used) was observed. Finally, the technique in combination with high-performance liquid chromatography and capillary electrophoresis was applied to analysis of quaternary ammonium and phenoxypropionic acid herbicides in fortified river water as well as drinking water (at levels relevant to Australian guidelines). The presented sustainable sample preparation approach could easily be applied to other charged analytes or adopted by other laboratories.

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.

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.

Preparation and characterization of organic-inorganic hybrid perovskite (C4H9NH3)2CuCl4

International Nuclear Information System (INIS)

Xiao Zelong; Chen Hongzheng; Shi Minmin; Wu Gang; Zhou Renjia; Yang Zhisheng; Wang Mang; Tang Benzhong

2005-01-01

Organic-inorganic hybrid perovskite (C 4 H 9 NH 3 ) 2 CuCl 4 was prepared via the reaction between copper chloride and butylammonium chloride. Its chemical structure was characterized by FT-IR and elemental analysis. Its thin film was obtained by spin-coating, and X-ray diffraction (XRD) measurements indicated the formation of two-dimensional layered perovskites structure, with the c-axis perpendicular to the substrate surface. The electronic structure, thermal properties and electrical properties of the hybrid perovskite (C 4 H 9 NH 3 ) 2 CuCl 4 were also studied by UV-vis, photoluminescience (PL), TGA, DSC, and Hall measurement

Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality : Effect of sample preparation on MALDI-MS of synthetic polymers

NARCIS (Netherlands)

Kooijman, Pieter C.; Kok, Sander; Honing, Maarten

2017-01-01

Rationale: Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) provides detailed and in-depth information about the molecular characteristics of synthetic polymers. To obtain the most accurate results the sample preparation parameters should be chosen to suit the sample and the

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.

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. Graphical Abstract ᅟ.

Universal Sample Preparation Module for Molecular Analysis in Space, Phase I

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...

Diagnosis of visceral Leishmaniasis in asymptomatic dogs by the KDNA PCR-hybridization assay using noninvasive samples

International Nuclear Information System (INIS)

Leite, Rodrigo Souza; Andrade, Antero Silva Ribeiro de; Ferreira, Sydney de Almeida; Ituassu, Leonardo Trindade; Melo, Maria Norma de

2009-01-01

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 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)

Preparation and properties of recycled HDPE/clay hybrids

Science.gov (United States)

Yong Lei; Qinglin Wu; Craig M. Clemons

2007-01-01

Hybrids based on recycled high density polyethylene (RHDPE) and organic clay were made by melt compounding. The influence of blending method, compatibilizers, and clay content on clay intercalation and exfoliation, RHDPE crystallization behavior, and the mechanical properties of RHDPE/clay hybrids were investigated. Both maleated polyethylene (MAPE) and titanate could...

Recent developments in sample preparation and data pre-treatment in metabonomics research.

Science.gov (United States)

Li, Ning; Song, Yi peng; Tang, Huiru; Wang, Yulan

2016-01-01

Metabonomics is a powerful approach for biomarker discovery and an effective tool for pinpointing endpoint metabolic effects of external stimuli, such as pathogens and disease development. Due to its wide applications, metabonomics is required to deal with various biological samples of different properties. Hence sample preparation and corresponding data pre-treatment become important factors in ensuring validity of an investigation. In this review, we summarize some recent developments in metabonomics sample preparation and data-pretreatment procedures. Copyright © 2015 Elsevier Inc. All rights reserved.

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.

Thermal and Mechanical Properties of Novolac-Silica Hybrid Aerogels Prepared by Sol-Gel Polymerization in Solvent-Saturated Vapor Atmosphere

Directory of Open Access Journals (Sweden)

Mohamad Mehdi Seraji1, Seraji

2015-05-01

Full Text Available Nowadays organic–inorganic hybrid aerogel materials have attracted increasing interests due to improved thermal and mechanical properties. In the present research, initially, novolac type phenolic resin-silica hybrid gels with different solid concentrations were synthesized using sol-gel polymerization in solvent-saturatedvapor atmosphere. The hybrid gels were dried at air atmosphere through ambient drying process. This method removed the need for costly and risky supercritical drying process. The yields of the obtained hybrid aerogels increased with less shrinkage in comparison with conventional sol-gel process. The precursor of silica phase in this study was tetraethoxysilane and inexpensive novolac resin was used as a reinforcing phase. The results of FTIR analysis confirmed the simultaneous formation of silica and novolac gels in the hybrid systems. The resultant hybrid aerogels showed a nanostructure hybrid network with high porosity (above 80% and low density (below 0.25 g/cm3. Nonetheless, higher content of silica resulted in more shrinkage in the hybrid aerogel structure due to the tendency of the silica network to shrink more during gelation and drying process. The SEM images of samples exhibited a continuous network of interconnected colloidal particles formed during sol-gel polymerization with mean particle size of less than 100 nanometers. Si mapping analysis showed good distribution of silica phase throughout the hybrid structure. The results demonstrated improvements in insulation properties and thermal stability of novolac-silica aerogel with increasing the silica content. The results of compressive strength showed that the mechanical properties of samples declined with increasing the silica content.

Synthesis and application of magnetic molecularly imprinted polymers in sample preparation.

Science.gov (United States)

Huang, Shuyao; Xu, Jianqiao; Zheng, Jiating; Zhu, Fang; Xie, Lijun; Ouyang, Gangfeng

2018-04-12

Magnetic molecularly imprinted polymers (MMIPs) have superior advantages in sample pretreatment because of their high selectivity for target analytes and the fast and easy isolation from samples. To meet the demand of both good magnetic property and good extraction performance, MMIPs with various structures, from traditional core-shell structures to novel composite structures with a larger specific surface area and more accessible binding sites, are fabricated by different preparation technologies. Moreover, as the molecularly imprinted polymer (MIP) layers determine the affinity, selectivity, and saturated adsorption amount of MMIPs, the development and innovation of the MIP layer are attracting attention and are reviewed here. Many studies that used MMIPs as sorbents in dispersive solid-phase extraction of complex samples, including environmental, food, and biofluid samples, are summarized. Graphical abstract The application of magnetic molecularly imprinted polymers (MIPs) in the sample preparation procedure improves the analytical performances for complex samples. MITs molecular imprinting technologies.

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.

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.

Sample preparation and detection device for infectious agents

Science.gov (United States)

Miles, Robin R.; Wang, Amy W.; Fuller, Christopher K.; Lemoff, Asuncion V.; Bettencourt, Kerry A.; Yu, June

2003-06-10

A sample preparation and analysis device which incorporates both immunoassays and PCR assays in one compact, field-portable microchip. The device provides new capabilities in fluid and particle control which allows the building of a fluidic chip with no moving parts, thus decreasing fabrication cost and increasing the robustness of the device. The device can operate in a true continuous (not batch) mode. The device incorporates magnetohydrodynamic (MHD) pumps to move the fluid through the system, acoustic mixing and fractionation, dielectropheretic (DEP) sample concentration and purification, and on-chip optical detection capabilities.

Facile Preparation of Hybrid Zinc Porphyrin Dendrimer Using Coordination Complex

Energy Technology Data Exchange (ETDEWEB)

Choi, Go-Eun; Shin, Eun Ju [Sunchon National University, Suncheon (Korea, Republic of)

2016-03-15

Porphyrins and metalloporphyrins have been investigated extensively due to their important role in natural photosynthesis, strong absorption in visible region, good light-harvesting properties, unique photophysical and electrochemical properties, and the development of simple synthetic routes for various derivatives. Dendrimers have globular structure with branches of repeating units and wide diversity of the architecture because their size, shape, and functionalities can be tailored. Numerous dendrimers have been designed and synthesized for various applications ranging from catalyst to drug delivery. Both pyridine dendrons Py-PD and Py-AD were successfully coordinated at axial position on central zinc metal cation in zinc porphyrin dendrimers ZnP-AD, ZnP-AD2, or ZnP-AD4. Therefore, it was proven that the formation of axial coordination complex between metal-centered dendrimer and ligand-containing dendron provides another facile method for the preparation of new hybrid dendrimer.

Microstructure and properties of TiAlSiN coatings prepared by hybrid PVD technology

International Nuclear Information System (INIS)

Yu Donghai; Wang Chengyong; Cheng Xiaoling; Zhang Fenglin

2009-01-01

TiAlSiN coatings with different Si content were prepared by hollow cathode discharge (HCD) and mid-frequency magnetron sputtering (MFMS) hybrid coating deposition technology. The chemical composition, microstructure, mechanical properties of these coatings were systematically investigated by means of energy dispersive spectrometry (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), nanoindentation measurement, scratch and high speed milling hardened steel tests. The coatings prepared by this method showed the structure of crystalline phase was corresponding to that of TiAlN, however, different preferred orientation with addition of Si. Proper content of Si into TiAlN led to increase of microhardness and adhesion. TiAlSiN coated end mill with Si content of 4.78 at.% had the least flank wear, which was improved about 20% milling distance than TiAlN coated end mill.

Microstructure and properties of TiAlSiN coatings prepared by hybrid PVD technology

Energy Technology Data Exchange (ETDEWEB)

Yu Donghai [Faculty of Electromechanical Engineering, Guangdong University of Technology, Guangzhou 510006 (China); Wang Chengyong, E-mail: cywang@gdut.edu.c [Faculty of Electromechanical Engineering, Guangdong University of Technology, Guangzhou 510006 (China); Cheng Xiaoling; Zhang Fenglin [Faculty of Electromechanical Engineering, Guangdong University of Technology, Guangzhou 510006 (China)

2009-07-01

TiAlSiN coatings with different Si content were prepared by hollow cathode discharge (HCD) and mid-frequency magnetron sputtering (MFMS) hybrid coating deposition technology. The chemical composition, microstructure, mechanical properties of these coatings were systematically investigated by means of energy dispersive spectrometry (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), nanoindentation measurement, scratch and high speed milling hardened steel tests. The coatings prepared by this method showed the structure of crystalline phase was corresponding to that of TiAlN, however, different preferred orientation with addition of Si. Proper content of Si into TiAlN led to increase of microhardness and adhesion. TiAlSiN coated end mill with Si content of 4.78 at.% had the least flank wear, which was improved about 20% milling distance than TiAlN coated end mill.

Mechanical properties of hybrid SiC/CNT filled toughened epoxy nanocomposite

Science.gov (United States)

Ratim, S.; Ahmad, S.; Bonnia, N. N.; Yahaya, Sabrina M.

2018-01-01

Mechanical properties of epoxy nanocomposites filled single filler have been extensively studied by various researchers. However, there are not much discovery on the behavior of hybrid nanocomposite. In this study, single and hybrid nanocomposites of toughened epoxy filled CNT/SiC nanoparticles were investigated. The hybrid nanocomposites samples were prepared by combining CNT and SiC nanoparticles in toughened epoxy matrix via mechanical stirring method assisted with ultrasonic cavitations. Epoxy resin and liquid epoxidized natural rubber (LENR) mixture were first blend prior to the addition of nanofillers. Then, the curing process of the nanocomposite samples were conducted by compression molding technique at 130°C for 2 hours. The purpose of this study is to investigate the hybridization effect of CNT and SiC nanoparticles on mechanical properties toughened epoxy matrix. The total loading of single and hybrid nanofillers were fixed to 4% volume are 0, 4C, 4S, 3S1C, 2S2C, and 1S3C. Mechanical properties of hybrid composites show that the highest value of tensile strength achieved by 3S1C sample at about 7% increment and falls between their single composite values. Meanwhile, the stiffness of the same sample is significantly increased at about 31% of the matrix. On the other hand, a highest flexural property is obtained by 1S3C sample at about 20% increment dominated by CNT content. However, the impact strength shows reduction trend with the addition of SiC and CNT into the matrix. The hybridization of SiC and CNT show highest value in sample 1S3C at about 3.37 kJ/m2 of impact energy absorbed. FESEM micrograph have confirmed that better distributions and interaction observed between SiC nanoparticles and matrix compared to CNT, which contributed to higher tensile strength and modulus.

One-step electrochemical approach for the preparation of graphene wrapped-phosphotungstic acid hybrid and its application for simultaneous determination of sunset yellow and tartrazine

International Nuclear Information System (INIS)

Gan Tian; Sun Junyong; Cao Shuqin; Gao Fuxing; Zhang Yuxia; Yang Yingqin

2012-01-01

Highlights: ► Graphene layer–wrapped PTA hybrid is one–step electropolymerized onto GCE surface. ► Graphene–PTA/GCE is used for simultaneous detection of sunset yellow and tartrazine. ► The oxidation mechanisms of sunset yellow and tartrazine were studied. ► Sunset yellow and tartrazine contents in soft drink samples are successfully determined. - Abstract: We have demonstrated a one-step and effective electrochemical method to prepare graphene (GN) layer-wrapped phosphotungstic acid (PTA) hybrid on the surface of glassy carbon electrode (GCE) using graphene as an electron transfer mediator. The PTA coupled with graphene provides good selectivity and high sensitivity for the simultaneous determination of two synthetic food colorants, sunset yellow and tartrazine, exhibiting as well-defined oxidation peaks in differential pulse voltammetry with a peak potential separation of ca. 260 mV. The detection limit was found to be 0.5 μg L −1 for sunset yellow and 30.0 μg L −1 for tartrazine. The interference of some common food additives was studied and it was concluded that application of this method for the determination of sunset yellow and tartrazine in several commercial soft drink samples led to satisfactory results. This study provides useful further evidences for the development of portable sensors for food additives.

High-resolution X-ray diffraction with no sample preparation.

Science.gov (United States)

Hansford, G M; Turner, S M R; Degryse, P; Shortland, A J

2017-07-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions.

Application of immunoaffinity columns for different food item samples preparation in micotoxins determination

Directory of Open Access Journals (Sweden)

Ćurčić Marijana

2016-01-01

Full Text Available In analytical methods used for monitoring of what special attention is paid to sample preparation. Therefore, the objective of this study was testing the efficiency of immunoaffinity columns (IAC that are based on solid phase extraction principles used for samples preparation in determining aflatoxins and ochratoxins. Aflatoxins and ochratoxins concentrations were determined in totally 56 samples of food items: wheat, corn, rice, barley and other grains (19 samples, flour and flour products from grain and additives for the bakery industry (7 samples, fruits and vegetables (3 samples, hazelnut, walnut, almond, coconut flour (4 samples, roasted cocoa beans, peanuts, tea, coffee (16 samples, spices (4 samples and meat and meat products (4 samples. Obtained results indicate advantage of IAC use for sample preparation based on enhanced specificity due to binding of extracted molecules to incorporated specific antibodies and rinsing the rest molecules from sample which could interfere with further analysis. Additional advantage is the usage of small amount of organic solvents and consequently decreased exposure of staff who conduct micotoxins determination. Of special interest is increase in method sensitivity since limit of quantification for aflatoxins and ochratoxins determination method is lower than maximal allowed concentration of these toxines prescribed by national rule book.

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.

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.

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)

A Proteomics Sample Preparation Method for Mature, Recalcitrant Leaves of Perennial Plants

Science.gov (United States)

Na, Zhang; Chengying, Lao; Bo, Wang; Dingxiang, Peng; Lijun, Liu

2014-01-01

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. PMID:25028960

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.

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

2016-01-01

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.…

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

International Nuclear Information System (INIS)

Ponard, O.F.X.

2002-01-01

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

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

2017-03-01

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.

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

Energy Technology Data Exchange (ETDEWEB)

Mandal, Abhishek; Boatz, Jennifer C. [University of Pittsburgh School of Medicine, Department of Structural Biology (United States); Wheeler, Travis B. [University of Pittsburgh School of Medicine, Department of Cell Biology (United States); Wel, Patrick C. A. van der, E-mail: vanderwel@pitt.edu [University of Pittsburgh School of Medicine, Department of Structural Biology (United States)

2017-03-15

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.

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.

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.

Difficulties in preparing a standard sample of uranium metal having traces of nitrogen

International Nuclear Information System (INIS)

Toteja, R.S.D.; Jangida, B.L.; Sundaresan, M.

1991-01-01

Normally in the analysis of uranium for nitrogen, the nitrides are hydrolysed to give NH 3 and that for standardisation purposes to approximate the closest conditions of analysis of ammonia, NH 4 Cl is added to the sample and the recovery is tested. An appropriate method will be to have a standard sample of uranium with known amounts of nitrogen to be used as reference sample. The present work describes the efforts made in the preparation of such a reference sample and a general assessment of such methods available. In present work, known microamounts of nitrogen in an enclosed volume were allowed to react at a temperature of 773 K with a fixed amount of uranium metal of nitrogen content determined chemically. As the reaction of nitrogen with uranium is essentially a surface reaction, a sample had to be homogenised by allowing the nitrided sample to melt at about 1500 K and allow the nitrogen to diffuse through so that the concentration gradient along the profile will disappear. Attempts were made to prepare such samples in the range to 40 to 100 ppm of nitrogen. The density differences of uranium nitride and uranium metal made this diffusion and homogenisation process difficult. The prepared samples were analysed by the micro-kjeldahl's method and the recoveries tested. The equipment used for the preparation of the nitrided samples, for homogenisation and analysis of the results obtained are detailed in the paper together with the assessment of the general methods. (author). 2 refs., 1 fig., 1 tab

Skin sample preparation by collagenase digestion for diclofenac quantification using LC-MS/MS after topical application.

Science.gov (United States)

Nirogi, Ramakrishna; Padala, Naga Surya Prakash; Boggavarapu, Rajesh Kumar; Kalaikadhiban, Ilayaraja; Ajjala, Devender Reddy; Bhyrapuneni, Gopinadh; Muddana, Nageswara Rao

2016-06-01

Skin is the target site to evaluate the pharmacokinetic parameters of topical applications. Sample preparation is one of the influential steps in the bioanalysis of drugs in the skin. Evaluation of dermatopharmacokinetics at preclinical stage is challenging due to lack of proper sample preparation method. There is a need for an efficient sample preparation procedure for quantification of drugs in the skin using LC-MS/MS. The skin samples treated with collagenase followed by homogenization using a bead beater represents a best-fit method resulting in uniform homogenate for reproducible results. A new approach involving enzymatic treatment and mechanical homogenization techniques were evaluated for efficient sample preparation of skin samples in the bioanalysis.

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.

Durable flame retardant finish for silk fabric using boron hybrid silica sol

Energy Technology Data Exchange (ETDEWEB)

Zhang, Qiang-hua; Gu, Jiali; Chen, Guo-qiang [National Engineering Laboratory for Modern Silk, Soochow University (China); Xing, Tie-ling, E-mail: xingtieling@suda.edu.cn [National Engineering Laboratory for Modern Silk, Soochow University (China); Jiangsu HuaJia Group (China)

2016-11-30

Highlights: • Highly homogeneous boron hybrid silica sol flame retardant system was prepared through sol-gel method. • The silk samples treated and cross-linked by this hybrid sol and BTCA solution showed a higher limiting oxygen index (LOI) more than 31.0% and a better washing durability for more than 30 times washing. • The smoke suppression, combustion performance and thermal stability properties of the treated samples have a significant improvement. - Abstract: A hybrid silica sol was prepared via sol gel method using tetraethoxysilane (TEOS) as a precursor and boric acid (H{sub 3}BO{sub 3}) as flame retardant additive and then applied to silk fabric. In order to endow silk fabric with durable flame retardancy, 1,2,3,4-butanetetracarboxylic acid (BTCA) was used as cross-linking agent for the sake of strong linkage formation between the hybrid silica sol and silk fabric. The FT-IR and XPS analysis demonstrated the Si-O-B formation in the sol system, as well as the linkage between the sol and silk after the treatment. The limiting oxygen index (LOI) and smoke density test indicated good flame retardancy and smoke suppression of the treated silk fabrics. The micro calorimeter combustion (MCC) test and thermo gravimetric (TG) analysis showed that the treated samples had less weight loss in the high temperature and lower heat release rate when burning. The washing durability evaluation results indicated that there was a distinct improvement for the silk samples treated with BTCA even after 30 times washing. In addition, the influence of the processing order of BTCA and silica sol treatment on the limiting oxygen index (LOI) of the finished silk fabric was also investigated. And the results demonstrated that the sample treated with BTCA first and then with the silica sol exhibited better LOI value (32.3%) than that of the sample by the conversed treatment order. Moreover the tensile property of treated samples was nearly unchanged, but the handle of sol treated

imFASP: An integrated approach combining in-situ filter-aided sample pretreatment with microwave-assisted protein digestion for fast and efficient proteome sample preparation.

Science.gov (United States)

Zhao, Qun; Fang, Fei; Wu, Ci; Wu, Qi; Liang, Yu; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2016-03-17

An integrated sample preparation method, termed "imFASP", which combined in-situ filter-aided sample pretreatment and microwave-assisted trypsin digestion, was developed for preparation of microgram and even nanogram amounts of complex protein samples with high efficiency in 1 h. For imFASP method, proteins dissolved in 8 M urea were loaded onto a filter device with molecular weight cut off (MWCO) as 10 kDa, followed by in-situ protein preconcentration, denaturation, reduction, alkylation, and microwave-assisted tryptic digestion. Compared with traditional in-solution sample preparation method, imFASP method generated more protein and peptide identifications (IDs) from preparation of 45 μg Escherichia coli protein sample due to the higher efficiency, and the sample preparation throughput was significantly improved by 14 times (1 h vs. 15 h). More importantly, when the starting amounts of E. coli cell lysate decreased to nanogram level (50-500 ng), the protein and peptide identified by imFASP method were improved at least 30% and 44%, compared with traditional in-solution preparation method, suggesting dramatically higher peptide recovery of imFASP method for trace amounts of complex proteome samples. All these results demonstrate that the imFASP method developed here is of high potential for high efficient and high throughput preparation of trace amounts of complex proteome samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A review of sample preparation and its influence on pH determination in concrete samples

International Nuclear Information System (INIS)

Manso, S.; Aguado, A.

2017-01-01

If we are to monitor the chemical processes in cementitious materials, then pH assays in the pore solutions of cement pastes, mortars, and concretes are of key importance. However, there is no standard method that regulates the sample-preparation method for pH determination. The state-of-the-art of different methods for pH determination in cementitious materials is presented in this paper and the influence of sample preparation in each case. Moreover, an experimental campaign compares three different techniques for pH determination. Its results contribute to establishing a basic criterion to help researchers select the most suitable method, depending on the purpose of the research. A simple tool is described for selecting the easiest and the most economic pH determination method, depending on the objective; especially for researchers and those with limited experience in this field.

A user-friendly robotic sample preparation program for fully automated biological sample pipetting and dilution to benefit the regulated bioanalysis.

Science.gov (United States)

Jiang, Hao; Ouyang, Zheng; Zeng, Jianing; Yuan, Long; Zheng, Naiyu; Jemal, Mohammed; Arnold, Mark E

2012-06-01

Biological sample dilution is a rate-limiting step in bioanalytical sample preparation when the concentrations of samples are beyond standard curve ranges, especially when multiple dilution factors are needed in an analytical run. We have developed and validated a Microsoft Excel-based robotic sample preparation program (RSPP) that automatically transforms Watson worklist sample information (identification, sequence and dilution factor) to comma-separated value (CSV) files. The Freedom EVO liquid handler software imports and transforms the CSV files to executable worklists (.gwl files), allowing the robot to perform sample dilutions at variable dilution factors. The dynamic dilution range is 1- to 1000-fold and divided into three dilution steps: 1- to 10-, 11- to 100-, and 101- to 1000-fold. The whole process, including pipetting samples, diluting samples, and adding internal standard(s), is accomplished within 1 h for two racks of samples (96 samples/rack). This platform also supports online sample extraction (liquid-liquid extraction, solid-phase extraction, protein precipitation, etc.) using 96 multichannel arms. This fully automated and validated sample dilution and preparation process has been applied to several drug development programs. The results demonstrate that application of the RSPP for fully automated sample processing is efficient and rugged. The RSPP not only saved more than 50% of the time in sample pipetting and dilution but also reduced human errors. The generated bioanalytical data are accurate and precise; therefore, this application can be used in regulated bioanalysis.

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

Energy Technology Data Exchange (ETDEWEB)

Kim, Jungdae [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Department of Physics and EHSRC, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Nam, Hyoungdo; Schroeder, Allan; Shih, Chih-Kang, E-mail: shih@physics.utexas.edu [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Qin, Shengyong [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Department of Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China); ICQD, Hefei National Laboratory for Physical Sciences at the Microscale, University of Science and Technology of China, Hefei, Anhui 230026 (China); Kim, Sang-ui [Department of Physics and EHSRC, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Eom, Daejin [Korea Research Institute of Standards and Science, Daejeon 305-340 (Korea, Republic of)

2015-09-15

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.

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.

Automated cellular sample preparation using a Centrifuge-on-a-Chip.

Science.gov (United States)

Mach, Albert J; Kim, Jae Hyun; Arshi, Armin; Hur, Soojung Claire; Di Carlo, Dino

2011-09-07

The standard centrifuge is a laboratory instrument widely used by biologists and medical technicians for preparing cell samples. Efforts to automate the operations of concentration, cell separation, and solution exchange that a centrifuge performs in a simpler and smaller platform have had limited success. Here, we present a microfluidic chip that replicates the functions of a centrifuge without moving parts or external forces. The device operates using a purely fluid dynamic phenomenon in which cells selectively enter and are maintained in microscale vortices. Continuous and sequential operation allows enrichment of cancer cells from spiked blood samples at the mL min(-1) scale, followed by fluorescent labeling of intra- and extra-cellular antigens on the cells without the need for manual pipetting and washing steps. A versatile centrifuge-analogue may open opportunities in automated, low-cost and high-throughput sample preparation as an alternative to the standard benchtop centrifuge in standardized clinical diagnostics or resource poor settings.

Ultra-High-Throughput Sample Preparation System for Lymphocyte Immunophenotyping Point-of-Care Diagnostics.

Science.gov (United States)

Walsh, David I; Murthy, Shashi K; Russom, Aman

2016-10-01

Point-of-care (POC) microfluidic devices often lack the integration of common sample preparation steps, such as preconcentration, which can limit their utility in the field. In this technology brief, we describe a system that combines the necessary sample preparation methods to perform sample-to-result analysis of large-volume (20 mL) biopsy model samples with staining of captured cells. Our platform combines centrifugal-paper microfluidic filtration and an analysis system to process large, dilute biological samples. Utilizing commercialization-friendly manufacturing methods and materials, yielding a sample throughput of 20 mL/min, and allowing for on-chip staining and imaging bring together a practical, yet powerful approach to microfluidic diagnostics of large, dilute samples. © 2016 Society for Laboratory Automation and Screening.

Highly Reproducible Automated Proteomics Sample Preparation Workflow for Quantitative Mass Spectrometry.

Science.gov (United States)

Fu, Qin; Kowalski, Michael P; Mastali, Mitra; Parker, Sarah J; Sobhani, Kimia; van den Broek, Irene; Hunter, Christie L; Van Eyk, Jennifer E

2018-01-05

Sample preparation for protein quantification by mass spectrometry requires multiple processing steps including denaturation, reduction, alkylation, protease digestion, and peptide cleanup. Scaling these procedures for the analysis of numerous complex biological samples can be tedious and time-consuming, as there are many liquid transfer steps and timed reactions where technical variations can be introduced and propagated. We established an automated sample preparation workflow with a total processing time for 96 samples of 5 h, including a 2 h incubation with trypsin. Peptide cleanup is accomplished by online diversion during the LC/MS/MS analysis. In a selected reaction monitoring (SRM) assay targeting 6 plasma biomarkers and spiked β-galactosidase, mean intraday and interday cyclic voltammograms (CVs) for 5 serum and 5 plasma samples over 5 days were samples repeated on 3 separate days had total CVs below 20%. Similar results were obtained when the workflow was transferred to a second site: 93% of peptides had CVs below 20%. An automated trypsin digestion workflow yields uniformly processed samples in less than 5 h. Reproducible quantification of peptides was observed across replicates, days, instruments, and laboratory sites, demonstrating the broad applicability of this approach.

Biomimetic synthesis and characterization of semiconducting hybrid

Indian Academy of Sciences (India)

Triple hybrid materials based on polyaniline-polyethylene glycol and cadmium sulphide have been prepared by the duffusion–limited biomimetic route and characterized by a number of spectroscopic, XRD, SEM, thermal and electrical measurements. These hybrid materials have been prepared by controlled precipitation of ...

Focused-microwave-assisted sample preparation (M8)

International Nuclear Information System (INIS)

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

2002-01-01

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

Radiation preparation of graphene/carbon nanotubes hybrid fillers for mechanical reinforcement of poly(vinyl alcohol) films

Science.gov (United States)

Ma, Hui-Ling; Zhang, Long; Zhang, Youwei; Wang, Shuojue; Sun, Chao; Yu, Hongyan; Zeng, Xinmiao; Zhai, Maolin

2016-01-01

Graphene/carbon nanotubes (G/CNTs) hybrid fillers were synthesized by γ-ray radiation reduction of graphene oxide (GO) in presence of CNTs. The obtained hybrid fillers with three-dimensional (3D) interconnected network structure were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Poly(vinyl alcohol) (PVA) composite films with enhanced mechanical properties and thermal stability were subsequently prepared by solution blending of G/CNTs with PVA matrix. The tensile strength and Young's modulus of PVA composite films containing 1 wt% G/CNTs were measured to be 81.9 MPa and 3.9 GPa respectively, which were 56% and 33.6% higher than those of pure PVA. These substantial improvements could be attributed to the interconnected 3D structure of G/CNTs, homogeneous dispersion as well as the strong hydrogen-bonding interaction between G/CNTs and PVA macromolecular chains.

Ionic liquids: solvents and sorbents in sample preparation.

Science.gov (United States)

Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

2018-01-01

The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Glucose aided preparation of tungsten sulfide/multi-wall carbon nanotube hybrid and use as counter electrode in dye-sensitized solar cells.

Science.gov (United States)

Wu, Jihuai; Yue, Gentian; Xiao, Yaoming; Huang, Miaoliang; Lin, Jianming; Fan, Leqing; Lan, Zhang; Lin, Jeng-Yu

2012-12-01

The tungsten sulfide/multi-wall carbon nanotube (WS(2)/MWCNT) hybrid was prepared in the presence of glucose by the hydrothermal route. The hybrid materials were used as counter electrode in the dye-sensitized solar cell (DSSC). The results of cyclic voltammetry measurement and electrochemical impedance spectroscopy indicated that the glucose aided prepared (G-A) WS(2)/MWCNT electrode had low charge-transfer resistance (R(ct)) and high electrocatalytic activity for triiodide reduction. The excellent electrochemical properties for (G-A) WS(2)/MWCNT electrode is due to the synergistic effects of WS(2) and MWCNTs, as well as amorphous carbon introduced by glucose. The DSSC based on the G-A WS(2)/MWCNT counter electrode achieved a high power conversion efficiency of 7.36%, which is comparable with the performance of the DSSC using Pt counter electrode (7.54%).

Development of a sample preparation system for AMS radiocarbon dating at CRICH, Korea

Energy Technology Data Exchange (ETDEWEB)

Kim, Myung-Jin; Lee, Byeong-Cheol; Lim, Eun-Soo [Cultural Research Institute of Chungcheong Heritage, Gongju (Korea, Republic of); Hong, Duk-Geun [Kangwon National University, Chuncheon (Korea, Republic of); Park, Soon-Bal [Chungnam National University, Daejeon (Korea, Republic of); Youn, Min-Young [Seoul National University, Seoul (Korea, Republic of)

2010-01-15

We developed a sample preparation system for radiocarbon dating by using AMS measurement at Cultural Research Institute of Chungcheong Heritage, Korea. From the investigation of the reduction process, the optimum graphitization temperature was chosen as 625 .deg. C. Using Aldrich graphite powder of 0.75 {+-} 0.023 pMC, the background value of our preparation system was controlled at a low level. The robustness against chemical treatment and contamination was also observed from samples of Oxalic acid II and IAEA-C4. The resultant values, 134.04 {+-} 0.99 pMC and 0.38 {+-} 0.043 pMC, were in good agreement with the consensus values. Based on comparison, our conventional ages agreed very well with those of Beta Analytic Co. and SNU-AMS. No memory effect existed in the preparation system. Therefore, we concluded that the sample preparation system was operated in a stable manner and that the basic radiocarbon dating procedures were completely verified.

TCLP Preparation and Analysis of K East Basin Composite Sludge Samples

International Nuclear Information System (INIS)

Silvers, K.L.; Wagner, J.J.; Steele, R.T.

2000-01-01

Sludge samples from the Hanford K East Basin were analyzed by the Toxicity Characterization Leaching Procedure (TCLP) to assist in the appropriate Resource Conservation and Recovery Act (RCIL4) designation of this material. Sludge samples were collected by Fluor Hanford, Inc. using the consolidated sludge sampling system (system that allows collection of a single sample from multiple sample locations). These samples were shipped to the Postirradiation Testing Laboratory (PTL, 327 Building) and then transferred to the Pacific Northwest National Laboratory (PNNL) Radiochemical Processing Laboratory (RPL, 325 Building) for recovery and testing. Two sludge composites were prepared, using the consolidated sludge samples, to represent K East canister sludge (sample KC Can Comp) and K East floor sludge (sample KC Floor Comp). Each composite was extracted in duplicate and analyzed in duplicate following pre-approved(a) TCLP extraction and analyses procedures. In addition, these samples and duplicates were analyzed for total RCRA metals (via acid digestion preparation). The work was conducted in accordance with the requirements of the Hanford Analytical Quality Assurance Requirements Document (HASQARD). A PNNL Quality Assurance Program compliant with J HASQARD was implemented for this effort. The results from the TCLP analyses showed that all RCRA metal concentrations were less than the TCLP limits for both the canister and floor composite samples and their respective duplicates

Capacitive deionization on-chip as a method for microfluidic sample preparation

NARCIS (Netherlands)

Roelofs, Susan Helena; Kim, Bumjoo; Eijkel, Jan C.T.; Han, Jongyoon; van den Berg, Albert; Odijk, Mathieu

2015-01-01

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

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

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...... 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...

Sb(III)-Imprinted Organic-Inorganic Hybrid Sorbent Prepared by Hydrothermal-Assisted Surface Imprinting Technique for Selective Adsorption of Sb(III)

Science.gov (United States)

Zhang, Dan; Zhao, Yue; Xu, Hong-Bo

2018-03-01

Sb(III)-imprinted organic-inorganic hybrid sorbent was prepared by hydrothermal-assisted surface imprinting technique and was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy coupled to an energy dispersive spectrometer and N2 adsorption/desorption isotherms. Hydrothermal-assisted process can improve the selectivity of the Sb(III)-imprinted hybrid sorbent for Sb(III) due to stable control of temperature and pressure. The Sb(III)-imprinted hybrid sorbent IIS indicated higher selectivity for Sb(III), had high static adsorption capacity of 37.3 mg g-1 for Sb(III), displayed stable adsorption capacity in pH range from 4 to 8, reached an rapid adsorption equilibrium within 30 min. According to the correlation coefficient ( r 2 > 0.99), the experimental data fitted better the pseudo-second-order kinetic model and Langmuir equilibrium isotherm.

[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.

A review of sample preparation and its influence on pH determination in concrete samples

Directory of Open Access Journals (Sweden)

S. Manso

2017-01-01

Full Text Available If we are to monitor the chemical processes in cementitious materials, then pH assays in the pore solutions of cement pastes, mortars, and concretes are of key importance. However, there is no standard method that regulates the sample-preparation method for pH determination. The state-of-the-art of different methods for pH determination in cementitious materials is presented in this paper and the influence of sample preparation in each case. Moreover, an experimental campaign compares three different techniques for pH determination. Its results contribute to establishing a basic criterion to help researchers select the most suitable method, depending on the purpose of the research. A simple tool is described for selecting the easiest and the most economic pH determination method, depending on the objective; especially for researchers and those with limited experience in this field.

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.

Study in electron microscopy of the formation of the hybrid layer using adhesive systems One Coat and Experimental (EXL 759), at the Facultad de Odontologia of the Universidad de Costa Rica

International Nuclear Information System (INIS)

Santamaria Guzman, S. Marcela; Guevara Lopez, Rodrigo

2012-01-01

The formation of the hybrid layer is observed in dental pieces in vitro, utilizing conventional adhesives systems and of self etching with different times of acid etching, by applying of electron microscopy. Samples of dental pieces are prepared utilizing conventional adhesive systems as Single Bond 2 of 3M, One Coat of Coltene and the adhesive self etching Experimental (EXL 759) of 3M. Samples of dental pieces collected have been molars recently extracted and later stored in jars with water. Samples prepared with the adhesive systems are observed in the electron microscope to obtain images of the hybrid layers formed. The hybrid layers formed are compared observing the photographs of the images obtained in the electron microscope. The adhesive system that has allowed the formation of a hybrid layer more convenient is determined. The time of acid etching is determined and has interfered in the formation of a hybrid layer more stable [es

Automated injection of a radioactive sample for preparative HPLC with feedback control

International Nuclear Information System (INIS)

Iwata, Ren; Yamazaki, Shigeki

1990-01-01

The injection of a radioactive reaction mixture into a preparative HPLC column has been automated with computer control for rapid purification of routinely prepared positron emitting radiopharmaceuticals. Using pneumatic valves, a motor-driven pump and a liquid level sensor, two intelligent injection methods for the automation were compared with regard to efficient and rapid sample loading into a 2 mL loop of the 6-way valve. One, a precise but rather slow method, was demonstrated to be suitable for purification of 18 F-radiopharmaceuticals, while the other, due to its rapid operation, was more suitable for 11 C-radiopharmaceuticals. A sample volume of approx 0.5 mL can be injected onto a preparative HPLC column with over 90% efficiency with the present automated system. (author)

Inorganic-organic hybrid polyoxometalate containing supramolecular helical chains: Preparation, characterization and application in chemically bulk-modified electrode

International Nuclear Information System (INIS)

Han Zhangang; Zhao Yulong; Peng Jun; Liu Qun; Wang Enbo

2005-01-01

An inorganic-organic hybrid polyoxometalate (POM) (Hbpy) 4 [SiMo 12 O 40 ] (1) (bpy = 2,4-bipyridine), has been prepared and characterized. X-ray diffraction study reveals that compound 1 contains interesting organic double helical chains. The hybrid nanoparticles was used as a solid bulkmodifier to fabricate a three-dimensional chemically modified carbon paste electrode (1-CPE) by direct mixing. The electrochemical behavior and electrocatalysis of 1-CPE has been studied in detail. The results indicate that 1-CPE has a good electrocatalytic activity toward the reduction of nitrite in 1 M H 2 SO 4 aqueous solution. 1-CPE shows remarkable stability that can be ascribed to the interactions existed between POM anions and organic double helical bpy chains, which are very important for practical applications in electrode modification

Sample preparation and fractionation for proteome analysis and cancer biomarker discovery by mass spectrometry.

Science.gov (United States)

Ahmed, Farid E

2009-03-01

Sample preparation and fractionation technologies are one of the most crucial processes in proteomic analysis and biomarker discovery in solubilized samples. Chromatographic or electrophoretic proteomic technologies are also available for separation of cellular protein components. There are, however, considerable limitations in currently available proteomic technologies as none of them allows for the analysis of the entire proteome in a simple step because of the large number of peptides, and because of the wide concentration dynamic range of the proteome in clinical blood samples. The results of any undertaken experiment depend on the condition of the starting material. Therefore, proper experimental design and pertinent sample preparation is essential to obtain meaningful results, particularly in comparative clinical proteomics in which one is looking for minor differences between experimental (diseased) and control (nondiseased) samples. This review discusses problems associated with general and specialized strategies of sample preparation and fractionation, dealing with samples that are solution or suspension, in a frozen tissue state, or formalin-preserved tissue archival samples, and illustrates how sample processing might influence detection with mass spectrometric techniques. Strategies that dramatically improve the potential for cancer biomarker discovery in minimally invasive, blood-collected human samples are also presented.

Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS

Energy Technology Data Exchange (ETDEWEB)

Adamic, M.L., E-mail: Mary.Adamic@inl.gov [Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID 83402 (United States); Lister, T.E.; Dufek, E.J.; Jenson, D.D.; Olson, J.E. [Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID 83402 (United States); Vockenhuber, C. [Laboratory of Ion Beam Physics, ETH Zurich, Otto-Stern-Weg 5, 8093 Zurich (Switzerland); Watrous, M.G. [Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID 83402 (United States)

2015-10-15

This paper presents an evaluation of an alternate method for preparing environmental samples for {sup 129}I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Precipitated silver iodide samples are usually mixed with niobium or silver powder prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.

Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS

International Nuclear Information System (INIS)

Adamic, M.L.; Lister, T.E.; Dufek, E.J.; Jenson, D.D.; Olson, J.E.; Vockenhuber, C.; Watrous, M.G.

2015-01-01

This paper presents an evaluation of an alternate method for preparing environmental samples for "1"2"9I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Precipitated silver iodide samples are usually mixed with niobium or silver powder prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.

A high-throughput sample preparation method for cellular proteomics using 96-well filter plates.

Science.gov (United States)

Switzar, Linda; van Angeren, Jordy; Pinkse, Martijn; Kool, Jeroen; Niessen, Wilfried M A

2013-10-01

A high-throughput sample preparation protocol based on the use of 96-well molecular weight cutoff (MWCO) filter plates was developed for shotgun proteomics of cell lysates. All sample preparation steps, including cell lysis, buffer exchange, protein denaturation, reduction, alkylation and proteolytic digestion are performed in a 96-well plate format, making the platform extremely well suited for processing large numbers of samples and directly compatible with functional assays for cellular proteomics. In addition, the usage of a single plate for all sample preparation steps following cell lysis reduces potential samples losses and allows for automation. The MWCO filter also enables sample concentration, thereby increasing the overall sensitivity, and implementation of washing steps involving organic solvents, for example, to remove cell membranes constituents. The optimized protocol allowed for higher throughput with improved sensitivity in terms of the number of identified cellular proteins when compared to an established protocol employing gel-filtration columns. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Review of sample preparation techniques for the analysis of pesticide residues in soil.

Science.gov (United States)

Tadeo, José L; Pérez, Rosa Ana; Albero, Beatriz; García-Valcárcel, Ana I; Sánchez-Brunete, Consuelo

2012-01-01

This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination. The optimization of sample preparation is a very important part of the method development that can reduce the analysis time, the amount of solvent, and the size of samples. This review considers all aspects of sample preparation, including extraction and cleanup. Classical extraction techniques, such as shaking, Soxhlet, and ultrasonic-assisted extraction, and modern techniques like pressurized liquid extraction, microwave-assisted extraction, solid-phase microextraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are reviewed. The different cleanup strategies applied for the purification of soil extracts are also discussed. In addition, the application of these techniques to environmental studies is considered.

Corrosion Testing of Hybrid Welded Stainless Steel Pot

DEFF Research Database (Denmark)

Sondrup, Lars de Caldas; Bagger, Claus; Olsen, Flemming Ove

2004-01-01

Investigation of the use of hybrid welding by preparation of tailored blanks for the manufacturing of a deep drawn pot.......Investigation of the use of hybrid welding by preparation of tailored blanks for the manufacturing of a deep drawn pot....

Ergonomic analysis of radiopharmaceuticals samples preparation process

International Nuclear Information System (INIS)

Gomes, Luciene Betzler C.; Santos, Isaac Luquetti dos; Fonseca, Antonio Carlos C. da; Pellini, Marcos Pinto; Rebelo, Ana Maria

2005-01-01

The doses of radioisotopes to be administrated in patients for diagnostic effect or therapy are prepared in the radiopharmacological sector. The preparation process adopts techniques that are aimed to reduce the exposition time of the professionals and the absorption of excessive doses for patients. The ergonomic analysis of this process contributes in the prevention of occupational illnesses and to prevent risks of accidents during the routines, providing welfare and security to the involved users and conferring to the process an adequate working standard. In this context it is perceived relevance of studies that deal with the analysis of factors that point with respect to the solution of problems and for establishing proposals that minimize risks in the exercise of the activities. Through a methodology that considers the application of the concepts of Ergonomics, it is searched the improvement of the effectiveness or the quality and reduction of the difficulties lived for the workers. The work prescribed, established through norms and procedures codified will be faced with the work effectively carried through, the real work, shaped to break the correct appreciation, with focus in the activities. This work has as objective to argue an ergonomic analysis of samples preparation process of radioisotopes in the Setor de Radiofarmacia do Hospital Universitario Clementino Fraga Filho da Universidade Federal do Rio de Janeiro (UFRJ). (author)

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 testing in the 1960's. We are developing sample preparation methods coupled to direct counting of T via ultra-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

Preparation and application of radioactive soil samples for intercomparison

International Nuclear Information System (INIS)

Gao Zequan; Li Zhou; Li Pengxiang; Wang Ruijun; Ren Xiaona

2014-01-01

This article summarized the preparation process and intercomparison results of the simulated environmental radioactive soil samples. The components of the matrix were: SiO 2 , Al 2 O 3 , Fe 2 O 3 , MgO, CaO, NaCl, KCl and TiO 2 . All of the components were milled, oven-dried, sieved and then blended together. The homogeneity test was according to GB 15000. 5-1994, and no significant differences were observed. The 3 H analysis soils were spiked natural soils with the moisture content of 15%. Eight laboratories attended this intercomparison. The results proves that the preparation of the simulated soils were suitable for the inter-laboratories comparison. (authors)

Preparation of rock samples for measurement of the thermal neutron macroscopic absorption cross-section

International Nuclear Information System (INIS)

Czubek, J.A.; Burda, J.; Drozdowicz, K.; Igielski, A.; Kowalik, W.; Krynicka-Drozdowicz, E.; Woznicka, U.

1986-03-01

Preparation of rock samples for the measurement of the thermal neutron macroscopic absorption cross-section in small cylindrical two-region systems by a pulsed technique is presented. Requirements which should be fulfilled during the preparation of the samples due to physical assumptions of the method are given. A cylindrical vessel is filled with crushed rock and saturated with a medium strongly absorbing thermal neutrons. Water solutions of boric acid of well-known macroscopic absorption cross-section are used. Mass contributions of the components in the sample are specified. This is necessary for the calculation of the thermal neutron macroscopic absorption cross-section of the rock matrix. The conditions necessary for assuring the required accuracy of the measurement are given and the detailed procedure of preparation of the rock sample is described. (author)

Application of DNA-DNA colony hybridization to the detection of catabolic genotypes in environmental samples

International Nuclear Information System (INIS)

Sayler, G.S.; Shields, M.S.; Tedford, E.T.; Breen, A.; Hooper, S.W.; Sirotkin, K.M.; Davis, J.W.

1985-01-01

The application of preexisting DNA hybridization techniques was investigated for potential in determining populations of specific gene sequences in environmental samples. Cross-hybridizations among two degradative plasmids, TOL and NAH, and two cloning vehicles, pLAFR1 and RSF1010, were determined. The detection limits for the TOL plasmid against a nonhomologous plasmid-bearing bacterial background was ascertained. The colony hybridization technique allowed detection of one colony containing TOL plasmid among 10(6) Escherichia coli colonies of nonhomologous DNA. Comparisons between population estimates derived from growth on selective substrates and from hybridizations were examined. Findings indicated that standard sole carbon source enumeration procedures for degradative populations lead to overestimations due to nonspecific growth of other bacteria on the microcontaminant carbon sources present in the media. Population estimates based on the selective growth of a microcosm population on two aromatic substrates (toluene and naphthalene) and estimates derived from DNA-DNA colony hybridizations, using the TOL or NAH plasmid as a probe, corresponded with estimates of substrate mineralization rates and past exposure to environmental contaminants. The applications of such techniques are hoped to eventually allow enumeration of any specific gene sequences in the environment, including both anabolic and catabolic genes. In addition, this procedure should prove useful in monitoring recombinant DNA clones released into environmental situations

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

Energy Technology Data Exchange (ETDEWEB)

Wahba, Adel Maher, E-mail: adel.mousa@f-eng.tanta.edu.eg [Department of Engineering Physics and Mathematics, Faculty of Engineering, Tanta University (Egypt); Mohamed, Mohamed Bakr [Ain shams University, Faculty of Science, Physics Department, Cairo (Egypt)

2017-02-15

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. - Highlights: • Samples with different masses of CoFe{sub 2}O{sub 4} were prepared by autocombustion method. • XRD and IR data confirmed a pure spinel cubic structure for all samples. • Structural and magnetic properties show detectable changes with the mass prepared. • Cation distribution was suggested from experimental data of XRD, IR, and M-H loops.

Controllable preparation of multi-dimensional hybrid materials of nickel-cobalt layered double hydroxide nanorods/nanosheets on electrospun carbon nanofibers for high-performance supercapacitors

International Nuclear Information System (INIS)

Lai, Feili; Huang, Yunpeng; Miao, Yue-E; Liu, Tianxi

2015-01-01

Graphical Abstract: Multi-dimensional hybrid materials of nickel-cobalt layered double hydroxide nanorods/nanosheets grown on electrospun carbon nanofiber membranes were prepared via electrospinning combined with solution co-deposition for high-performance supercapacitor electrodes. - Highlights: • Ni-Co LDH@CNFhybridswerepreparedbyelectrospinningandsolutionco-deposition. • Ni-Co LDH@CNF hybrids show high electrochemical performance for supercapacitors. • This method can be extended to other bimetallic@CNF hybrids for electrode materials. - Abstract: Hybrid nanomaterials with hierarchical structures have been considered as one kind of the most promising electrode materials for high-performance supercapacitors with high capacity and long cycle lifetime. In this work, multi-dimensional hybrid materials of nickel-cobalt layered double hydroxide (Ni-Co LDH) nanorods/nanosheets on carbon nanofibers (CNFs) were prepared by electrospinning technique combined with one-step solution co-deposition method. Carbon nanofiber membranes were obtained by electrospinning of polyacrylonitrile (PAN) followed by pre-oxidation and carbonization. The successful growth of Ni-Co LDH with different morphologies on CNF membrane by using two kinds of auxiliary agents reveals the simplicity and universality of this method. The uniform and immense growth of Ni-Co LDH on CNFs significantly improves its dispersion and distribution. Meanwhile the hierarchical structure of carbon nanofiber@nickel-cobalt layered double hydroxide nanorods/nanosheets (CNF@Ni-Co LDH NR/NS) hybrid membranes provide not only more active sites for electrochemical reaction but also more efficient pathways for electron transport. Galvanostatic charge-discharge measurements reveal high specific capacitances of 1378.2 F g −1 and 1195.4 F g −1 (based on Ni-Co LDH mass) at 1 A g −1 for CNF@Ni-Co LDH NR and CNF@Ni-Co LDH NS hybrid membranes, respectively. Moreover, cycling stabilities for both hybrid membranes are

Experiences from Refurbishment of Metallography Hot Cells and Application of a New Preparation Concept for Materialography Samples

International Nuclear Information System (INIS)

Oberlander, B. C.; Espeland, M.; Solum, N. O.

2001-01-01

After more than 30 years of operation the lead shielded metallography hot cells needed a basic renewal and modernisation not least of the specimen preparation equipment. Preparation in hot cells of radioactive samples for metallography and ceramography is challenging and time consuming. It demands a special design and quality of all in-cell equipment and skill and patience from the operator. Essentials in the preparation process are: simplicity and reliability of the machines, and a good quality, reproducibility and efficiency in performance. Desirable is process automation, flexibility and an alara amounto of radioactive waste produced per sample prepared. State of the art preparation equipment for materialography seems to meet most of the demands, however, it cannot be used in hot cells without modifications. Therefore. IFE and Struers in Copenhagen modified a standard model of a Strues precision cutting machine and a microprocessor controlled grinding and polishing machine for Hot Cell application. Hot cell utilisation of the microcomputer controlled grinding and polishing machine and the existing automatic dosing equipment made the task of preparing radioactive samples more attractive. The new grinding and polishing system for hot cells provides good sample preparation quality and reproductibility at reduced preparation time and reduced amount of contaminated waste produced per sample prepared. the sample materials examined were irradiated cladding materials and fuels

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

International Nuclear Information System (INIS)

Macario, Kita D.; Gomes, Paulo R. S.; Anjos, Roberto M. dos; Linares, Roberto; Queiroz, Eduardo; Oliveira, Fabiana M. de; Cardozo, Laio; Carvalho, Carla R.A.

2011-01-01

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 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)

Effect of measurement error budgets and hybrid metrology on qualification metrology sampling

Science.gov (United States)

Sendelbach, Matthew; Sarig, Niv; Wakamoto, Koichi; Kim, Hyang Kyun (Helen); Isbester, Paul; Asano, Masafumi; Matsuki, Kazuto; Osorio, Carmen; Archie, Chas

2014-10-01

Until now, metrologists had no statistics-based method to determine the sampling needed for an experiment before the start that accuracy experiment. We show a solution to this problem called inverse total measurement uncertainty (TMU) analysis, by presenting statistically based equations that allow the user to estimate the needed sampling after providing appropriate inputs, allowing him to make important "risk versus reward" sampling, cost, and equipment decisions. Application examples using experimental data from scatterometry and critical dimension scanning electron microscope tools are used first to demonstrate how the inverse TMU analysis methodology can be used to make intelligent sampling decisions and then to reveal why low sampling can lead to unstable and misleading results. One model is developed that can help experimenters minimize sampling costs. A second cost model reveals the inadequacy of some current sampling practices-and the enormous costs associated with sampling that provides reasonable levels of certainty in the result. We introduce the strategies on how to manage and mitigate these costs and begin the discussion on how fabs are able to manufacture devices using minimal reference sampling when qualifying metrology steps. Finally, the relationship between inverse TMU analysis and hybrid metrology is explored.

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.

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

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

International Nuclear Information System (INIS)

Kreuzpaintner, Wolfgang

2010-01-01

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

Infrared biospectroscopy for a fast qualitative evaluation of sample preparation in metabolomics.

Science.gov (United States)

Kuligowski, Julia; Pérez-Guaita, David; Escobar, Javier; Lliso, Isabel; de la Guardia, Miguel; Lendl, Bernhard; Vento, Máximo; Quintás, Guillermo

2014-09-01

Liquid chromatography-mass spectrometry (LC-MS) has been increasingly used in biomedicine to study the dynamic metabolomic responses of biological systems under different physiological or pathological conditions. To obtain an integrated snapshot of the system, metabolomic methods in biomedicine typically analyze biofluids (e.g. plasma) that require clean-up before being injected into LC-MS systems. However, high resolution LC-MS is costly in terms of resources required for sample and data analysis and care must be taken to prevent chemical (e.g. ion suppression) or statistical artifacts. Because of that, the effect of sample preparation on the metabolomic profile during metabolomic method development is often overlooked. This work combines an Attenuated Total Reflectance-Fourier transform infrared (ATR-FTIR) and a multivariate exploratory data analysis for a cost-effective qualitative evaluation of major changes in sample composition during sample preparation. ATR-FTIR and LC-time of flight mass spectrometry (TOFMS) data from the analysis of a set of plasma samples precipitated using acetonitrile, methanol and acetone performed in parallel were used as a model example. Biochemical information obtained from the analysis of the ATR-FTIR and LC-TOFMS data was thoroughly compared to evaluate the strengths and shortcomings of FTIR biospectroscopy for assessing sample preparation in metabolomics studies. Results obtained show the feasibility of ATR-FTIR for the evaluation of major trends in the plasma composition changes among different sample pretreatments, providing information in terms of e.g., amino acids, proteins, lipids and carbohydrates overall contents comparable to those found by LC-TOFMS. Copyright © 2014 Elsevier B.V. All rights reserved.

Highly oriented Bi-system bulk sample prepared by a decomposition-crystallization process

International Nuclear Information System (INIS)

Xi Zhengping; Zhou Lian; Ji Chunlin

1992-01-01

A decomposition-crystallization method, preparing highly oriented Bi-system bulk sample is reported. The effects of processing parameter, decomposition temperature, cooling rate and post-treatment condition on texture and superconductivity are investigated. The method has successfully prepared highly textured Bi-system bulk samples. High temperature annealing does not destroy the growing texture, but the cooling rate has some effect on texture and superconductivity. Annealing in N 2 /O 2 atmosphere can improve superconductivity of the textured sample. The study on the superconductivity of the Bi(Pb)-Sr-Ca-Cu-O bulk material has been reported in numerous papers. The research on J c concentrates on the tape containing the 2223 phase, with very few studies on the J c of bulk sample. The reason for the lack of studies is that the change of superconducting phases at high temperatures has not been known. The authors have reported that the 2212 phase incongruently melted at about 875 degrees C and proceeded to orient the c-axis perpendicular to the surface in the process of crystallization of the 2212 phase. Based on that result, a decomposition-crystallization method was proposed to prepare highly oriented Bi-system bulk sample. In this paper, the process is described in detail and the effects of processing parameters on texture and superconductivity are reported

X-ray diffraction without sample preparation: Proof-of-principle experiments

International Nuclear Information System (INIS)

Hansford, Graeme M.

2013-01-01

The properties of a novel X-ray diffraction (XRD) technique having very low sensitivity to the sample morphology were previously elucidated through theoretical considerations and model simulations (Hansford, 2011). This technique opens up the possibility of mineralogical analysis by XRD without sample preparation. Here, the results of proof-of-principle experimental tests are presented. Two sets of experiments were performed using a vacuum chamber equipped with an X-ray tube source, sample holder and charge-coupled detector. Firstly, a pressed-powder pellet of α-quartz was placed in three different positions relative to the X-ray source and detector. The changes in position represent gross sample movements which would be inconceivable in conventional XRD analysis. The resulting back-reflection energy-dispersive spectra show a very high degree of correspondence other than an overall intensity factor dependent on the distance between the sample and detector. Secondly, the back-reflection spectrum of an unprepared limestone hand specimen, having mm-scale surface morphology, was compared to the spectrum of a calcite pressed-powder pellet. The correspondence of the diffraction peaks in the spectra demonstrate that the limestone is comprised dominantly of calcite. In both cases, the claims of the earlier paper are fully supported by the results of these experimental tests. -- Highlights: • Proof-of-principle tests of a novel X-ray diffraction (XRD) method were conducted. • Very low sensitivity to sample position and orientation was demonstrated. • Insensitivity to sample morphology is inferred. • A simple analysis of an unprepared limestone hand specimen was performed. • This technique enables mineralogical analysis by XRD without sample preparation

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

The role of graphene-based sorbents in modern sample preparation techniques.

Science.gov (United States)

de Toffoli, Ana Lúcia; Maciel, Edvaldo Vasconcelos Soares; Fumes, Bruno Henrique; Lanças, Fernando Mauro

2018-01-01

The application of graphene-based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene-based material, their properties, synthesis routes, and the most important applications in both off-line and on-line sample preparation techniques. The discussion of the off-line approaches includes methods derived from conventional solid-phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on-line approaches focus on the use of graphene-based material mainly in on-line solid phase extraction, its variation called in-tube solid-phase microextraction, and on-line microdialysis systems. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation and validation of gross alpha/beta samples used in EML's quality assessment program

International Nuclear Information System (INIS)

Scarpitta, S.C.

1997-10-01

A set of water and filter samples have been incorporated into the existing Environmental Measurements Laboratory's (EML) Quality Assessment Program (QAP) for gross alpha/beta determinations by participating DOE laboratories. The participating laboratories are evaluated by comparing their results with the EML value. The preferred EML method for measuring water and filter samples, described in this report, uses gas flow proportional counters with 2 in. detectors. Procedures for sample preparation, quality control and instrument calibration are presented. Liquid scintillation (LS) counting is an alternative technique that is suitable for quantifying both the alpha ( 241 Am, 230 Th and 238 Pu) and beta ( 90 Sr/ 90 Y) activity concentrations in the solutions used to prepare the QAP water and air filter samples. Three LS counting techniques (Cerenkov, dual dpm and full spectrum analysis) are compared. These techniques may be used to validate the activity concentrations of each component in the alpha/beta solution before the QAP samples are actually prepared

Sample preparation and characterization of technetium metal

International Nuclear Information System (INIS)

Minato, Kazuo; Serizawa, Hiroyuki; Fukuda, Kousaku; Itoh, Mitsuo

1997-10-01

Technetium-99 is a long-lived fission product with a half-life of about 2.1 x 10 5 years, which decays by β-emission. For the transmutation of 99 Tc, research on solid technetium was started. Technetium metal powder purchased was analyzed by X-ray diffraction, γ-ray spectrometry, and inductively coupled plasma-atomic emission spectrometry and -mass spectrometry. The lattice parameters obtained were agreed with the reported values. The metallic impurity was about 15 ppm, where aluminum and iron contributed mainly. No impurity nuclide with γ-emission was found. Using the technetium metal powder, button-, rod-, and disk-shaped samples of technetium metal were prepared by arc-melting technique. Thermal diffusivity of technetium metal was measured on a disk sample from room temperature to 1173 K by laser flash method. The thermal diffusivity decreased with increasing temperature though it was almost constant above 600 K. (author)

Fabrication and Characteristics of ZnO/OAD-InN/PbPc Hybrid Solar Cells Prepared by Oblique-Angle Deposition

Directory of Open Access Journals (Sweden)

Lung-Chien Chen

2012-08-01

Full Text Available In this work, lead phthalocyanine (PbPc and ZnO/InN inorganic semiconductor films prepared by oblique-angle deposition (OAD were layered to form heterojunction organic/inorganic hybrid photovoltaic solar cells. Among the available organic materials, phthalocyanines, particularly the non-planar ones such as PbPc, are notable for their absorption in the visible and near infrared regions. The organic/inorganic hybrid solar cells fabricated on ZnO/OAD-InN/PbPc showed short-circuit current density (J_SC, open-circuit voltage (V_OC, and power conversion efficiencies (η of 1.2 mA/cm², 0.6 V and 0.144%, respectively.

Comparison of leach results from field and laboratory prepared samples

International Nuclear Information System (INIS)

Oblath, S.B.; Langton, C.A.

1985-01-01

The leach behavior of saltstone prepared in the laboratory agrees well with that from samples mixed in the field using the Littleford mixer. Leach rates of nitrates and cesium from the current reference formulation saltstone were compared. The laboratory samples were prepared using simulated salt solution; those in the field used Tank 50 decontaminated supernate. For both nitrate and cesium, the field and laboratory samples showed nearly identical leach rates for the first 30 to 50 days. For the remaining period of the test, the field samples showed higher leach rates with the maximum difference being less than a factor of three. Ruthenium and antimony were present in the Tank 50 supernate in known amounts. Antimony-125 was observed in the leachate and a fractional leach rate was calculated to be at least a factor of ten less than that of 137 Cs. No 106 Ru was observed in the leachate, and the release rate was not calculated. However, based on the detection limits for the analysis, the ruthenium leach rate must also be at least a factor of ten less than cesium. These data are the first measurements of the leach rates of Ru and Sb from saltstone. The nitrate leach rates for these samples were 5 x 10 -5 grams of nitrate per square cm per day after 100 days for the laboratory samples and after 200 days for the field samples. These values are consistent with the previously measured leach rates for reference formulation saltstone. The relative standard deviation in the leach rate is about 15% for the field samples, which all were produced from one batch of saltstone, and about 35% for the laboratory samples, which came from different batches. These are the first recorded estimates of the error in leach rates for saltstone

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

International Nuclear Information System (INIS)

Gagnon, Alan R.; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; Reden, Karl von

2000-01-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS 14 C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts ( 14 C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC)

Collection and preparation of bottom sediment samples for analysis of radionuclides and trace elements

International Nuclear Information System (INIS)

2003-07-01

The publication is the first in a series of TECDOCs on sampling and sample handling as part of the IAEA support to improve reliability of nuclear analytical techniques (NATs) in Member State laboratories. The purpose of the document is to provide information on the methods for collecting sediments, the equipment used, and the sample preparation techniques for radionuclide and elemental analysis. The most appropriate procedures for defining the strategies and criteria for selecting sampling locations, for sample storage and transportation are also given. Elements of QA/QC and documentation needs for sampling and sediment analysis are discussed. Collection and preparation of stream and river bottom sediments, lake bottom sediments, estuary bottom sediments, and marine (shallow) bottom sediments are covered. The document is intended to be a comprehensive manual for the collection and preparation of bottom sediments as a prerequisite to obtain representative and meaningful results using NATs. Quality assurance and quality control (QA/QC) is emphasized as an important aspect to ensure proper collection, transportation, preservation, and analysis since it forms the basis for interpretation and legislation. Although there are many approaches and methods available for sediment analyses, the scope of the report is limited to sample preparation for (1) analysis of radionuclides (including sediment dating using radionuclides such as Pb-210 and Cs-137) and (2) analysis of trace, minor and major elements using nuclear and related analytical techniques such as NAA, XRF and PIXE

Collection and preparation of bottom sediment samples for analysis of radionuclides and trace elements

Energy Technology Data Exchange (ETDEWEB)

NONE

2003-07-01

The publication is the first in a series of TECDOCs on sampling and sample handling as part of the IAEA support to improve reliability of nuclear analytical techniques (NATs) in Member State laboratories. The purpose of the document is to provide information on the methods for collecting sediments, the equipment used, and the sample preparation techniques for radionuclide and elemental analysis. The most appropriate procedures for defining the strategies and criteria for selecting sampling locations, for sample storage and transportation are also given. Elements of QA/QC and documentation needs for sampling and sediment analysis are discussed. Collection and preparation of stream and river bottom sediments, lake bottom sediments, estuary bottom sediments, and marine (shallow) bottom sediments are covered. The document is intended to be a comprehensive manual for the collection and preparation of bottom sediments as a prerequisite to obtain representative and meaningful results using NATs. Quality assurance and quality control (QA/QC) is emphasized as an important aspect to ensure proper collection, transportation, preservation, and analysis since it forms the basis for interpretation and legislation. Although there are many approaches and methods available for sediment analyses, the scope of the report is limited to sample preparation for (1) analysis of radionuclides (including sediment dating using radionuclides such as Pb-210 and Cs-137) and (2) analysis of trace, minor and major elements using nuclear and related analytical techniques such as NAA, XRF and PIXE.

Microfluidic devices for sample preparation and rapid detection of foodborne pathogens.

Science.gov (United States)

Kant, Krishna; Shahbazi, Mohammad-Ali; Dave, Vivek Priy; Ngo, Tien Anh; Chidambara, Vinayaka Aaydha; Than, Linh Quyen; Bang, Dang Duong; Wolff, Anders

2018-03-10

Rapid detection of foodborne pathogens at an early stage is imperative for preventing the outbreak of foodborne diseases, known as serious threats to human health. Conventional bacterial culturing methods for foodborne pathogen detection are time consuming, laborious, and with poor pathogen diagnosis competences. This has prompted researchers to call the current status of detection approaches into question and leverage new technologies for superior pathogen sensing outcomes. Novel strategies mainly rely on incorporating all the steps from sample preparation to detection in miniaturized devices for online monitoring of pathogens with high accuracy and sensitivity in a time-saving and cost effective manner. Lab on chip is a blooming area in diagnosis, which exploits different mechanical and biological techniques to detect very low concentrations of pathogens in food samples. This is achieved through streamlining the sample handling and concentrating procedures, which will subsequently reduce human errors and enhance the accuracy of the sensing methods. Integration of sample preparation techniques into these devices can effectively minimize the impact of complex food matrix on pathogen diagnosis and improve the limit of detections. Integration of pathogen capturing bio-receptors on microfluidic devices is a crucial step, which can facilitate recognition abilities in harsh chemical and physical conditions, offering a great commercial benefit to the food-manufacturing sector. This article reviews recent advances in current state-of-the-art of sample preparation and concentration from food matrices with focus on bacterial capturing methods and sensing technologies, along with their advantages and limitations when integrated into microfluidic devices for online rapid detection of pathogens in foods and food production line. Copyright © 2018. Published by Elsevier Inc.

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

Science.gov (United States)

Zellnig, Günther; Möstl, Stefan; Zechmann, Bernd

2013-01-01

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

Protocols for the analytical characterization of therapeutic monoclonal antibodies. II - Enzymatic and chemical sample preparation.

Science.gov (United States)

Bobaly, Balazs; D'Atri, Valentina; Goyon, Alexandre; Colas, Olivier; Beck, Alain; Fekete, Szabolcs; Guillarme, Davy

2017-08-15

The analytical characterization of therapeutic monoclonal antibodies and related proteins usually incorporates various sample preparation methodologies. Indeed, quantitative and qualitative information can be enhanced by simplifying the sample, thanks to the removal of sources of heterogeneity (e.g. N-glycans) and/or by decreasing the molecular size of the tested protein by enzymatic or chemical fragmentation. These approaches make the sample more suitable for chromatographic and mass spectrometric analysis. Structural elucidation and quality control (QC) analysis of biopharmaceutics are usually performed at intact, subunit and peptide levels. In this paper, general sample preparation approaches used to attain peptide, subunit and glycan level analysis are overviewed. Protocols are described to perform tryptic proteolysis, IdeS and papain digestion, reduction as well as deglycosylation by PNGase F and EndoS2 enzymes. Both historical and modern sample preparation methods were compared and evaluated using rituximab and trastuzumab, two reference therapeutic mAb products approved by Food and Drug Administration (FDA) and European Medicines Agency (EMA). The described protocols may help analysts to develop sample preparation methods in the field of therapeutic protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Morphology and properties of silica/novolac hybrid xerogels synthesized using sol–gel polymerization at solvent vapor-saturated atmosphere

International Nuclear Information System (INIS)

Seraji, Mohamad Mehdi; Seifi, Azadeh; Bahramian, Ahmad Reza

2015-01-01

Highlights: • Sol–gel polymerization in vapor of solvent saturated atmosphere is developed. • Highly porous novolac–silica hybrid xerogels are successfully synthesized. • Novolac–silica hybrid gel was dried in ambient condition with low shrinkage. • Required time for preparation of gel reduced from 5 days to about 5 h. • By incorporation of silica into the novolac xerogel structure, the pore size decreases. - Abstract: Highly porous novolac–silica hybrid xerogels were successfully synthesized via the novel method of sol–gel polymerization in solvent vapor-saturated atmosphere. This method removes the need for supercritical drying and yields the hybrid xerogels with reduced shrinkage in comparison with conventional sol–gel process. Tetraethoxysilane (TEOS) was used as the precursor of silica-based inorganic phase. The chemical and structural characterization of the prepared hybrid xerogels were performed by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) analysis, respectively. Thermal and mechanical properties of the hybrid samples were investigated by differential scanning calorimetry (DSC), and compressive strength analysis. The resultant hybrid xerogels show a nanostructured colloidal hybrid network with high porosity (above 80%) and low density (below 0.25 g cm −3 ). Si mapping images shows the good distribution of silica phase throughout the hybrid structure

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

Energy Technology Data Exchange (ETDEWEB)

Gagnon, Alan R. E-mail: agagnon@whoi.edu; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; Reden, Karl von

2000-10-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS {sup 14}C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts (<100 {mu}g) of carbon. The capability to mass-produce small samples for {sup 14}C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC)

Sample preparation method for induced mutation on orchid

International Nuclear Information System (INIS)

Suhaimi Musa; Sakinah Ariffin

2005-01-01

Studies on the induction of mutation in Dendrobium orchid at MINT has produced a number of new orchid mutant cultivars. Tissue culture techniques on orchid seeds and meristem cloning are employed in preparing the samples for the mutation induction. Solid medium based on the Murashige and Skoog (1962) and liquid medium based on Vacin and Went (1949) were found to be suitable in producing protocorm like bodies (PLBs) that are required for the irradiation treatment. (Author)

[Standard sample preparation method for quick determination of trace elements in plastic].

Science.gov (United States)

Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

2011-08-01

Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

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

Directory of Open Access Journals (Sweden)

Myung-Jin Lee

2017-03-01

Full Text Available 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 < 0.05. In the MTT assay, cell viability increased significantly in every group as the concentration of the extracts decreased (p < 0.05. Extracts from post-cured and removed unreacted layer samples of bonding resin were less toxic than post-cured and removed unreacted layer samples of composite resin. Removal of the oxygen-inhibition layer resulted in the lowest cytotoxicity. Clinicians should remove unreacted monomers on the resin surface immediately after restoring teeth with light-curing resin to improve the restoration biocompatibility.

Sample preparation prior to the LC-MS-based metabolomics/metabonomics of blood-derived samples.

Science.gov (United States)

Gika, Helen; Theodoridis, Georgios

2011-07-01

Blood represents a very important biological fluid and has been the target of continuous and extensive research for diagnostic, or health and drug monitoring reasons. Recently, metabonomics/metabolomics have emerged as a new and promising 'omics' platform that shows potential in biomarker discovery, especially in areas such as disease diagnosis, assessment of drug efficacy or toxicity. Blood is collected in various establishments in conditions that are not standardized. Next, the samples are prepared and analyzed using different methodologies or tools. When targeted analysis of key molecules (e.g., a drug or its metabolite[s]) is the aim, enforcement of certain measures or additional analyses may correct and harmonize these discrepancies. In omics fields such as those performed by holistic analytical approaches, no such rules or tools are available. As a result, comparison or correlation of results or data fusion becomes impractical. However, it becomes evident that such obstacles should be overcome in the near future to allow for large-scale studies that involve the assaying of samples from hundreds of individuals. In this case the effect of sample handling and preparation becomes very serious, in order to avoid wasting months of work from experts and expensive instrument time. The present review aims to cover the different methodologies applied to the pretreatment of blood prior to LC-MS metabolomic/metabonomic studies. The article tries to critically compare the methods and highlight issues that need to be addressed.

Fast preparation of hybrid monolithic columns via photo-initiated thiol-yne polymerization for capillary liquid chromatography.

Science.gov (United States)

Ma, Shujuan; Zhang, Haiyang; Li, Ya; Li, Yanan; Zhang, Na; Ou, Junjie; Ye, Mingliang; Wei, Yinmao

2018-02-23

Although several approaches have been developed to fabricate hybrid monoliths, it would still take a few hours to finish the formation of monoliths. Herein, photo-initiated thiol-yne polymerization was first adopted to in situ fabricate hybrid monoliths within the confines of UV-transparent fused-silica capillary. A silicon-containing diyne (1,3-diethynyltetramethyl-disiloxane, DYDS) was copolymerized with three multithiols, 1,6-hexanedithiol, trimethylolpropane tris(3-mercaptopropionate) and pentaerythriol tetrakis(3-mercaptopropionate), by using a binary porogenic system of diethylene glycol diethyl ether (DEGDE)/poly(ethylene glycol) (PEG200) within 10 min. Several characterizations of three hybrid monoliths (assigned as I, II and III, respectively) were performed. The results showed that these hybrid monoliths possessed bicontinuous porous structure, which was remarkably different from that via typical free-radical polymerization. The highest column efficiency of 76,000 plates per meter for butylbenzene was obtained on the column I in reversed-phase liquid chromatography (RPLC). It was observed that the efficiencies for strong-retained butylbenzene were almost close to those of weak-retained benzene, indicating a retention-independent efficient performance of small molecules on hybrid column I. The surface area of this hybrid monolith was very small in the dry state (less than 10.0 m 2 /g), and the chromatographic behavior of hybrid monolithic columns would be possibly explained by radical-mediated step-growth process of thiol-yne polymerization. Finally, the column I was applied for separation of BSA tryptic digest by cLC-MS/MS, indicating satisfactory separation ability for complicated samples. Copyright © 2018 Elsevier B.V. All rights reserved.

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Monolith Chromatography as Sample Preparation Step in Virome Studies of Water Samples.

Science.gov (United States)

Gutiérrez-Aguirre, Ion; Kutnjak, Denis; Rački, Nejc; Rupar, Matevž; Ravnikar, Maja

2018-01-01

Viruses exist in aquatic media and many of them use this media as transmission route. Next-generation sequencing (NGS) technologies have opened new doors in virus research, allowing also to reveal a hidden diversity of viral species in aquatic environments. Not surprisingly, many of the newly discovered viruses are found in environmental fresh and marine waters. One of the problems in virome research can be the low amount of viral nucleic acids present in the sample in contrast to the background ones (host, eukaryotic, prokaryotic, environmental). Therefore, virus enrichment prior to NGS is necessary in many cases. In water samples, an added problem resides in the low concentration of viruses typically present in aquatic media. Different concentration strategies have been used to overcome such limitations. CIM monoliths are a new generation of chromatographic supports that due to their particular structural characteristics are very efficient in concentration and purification of viruses. In this chapter, we describe the use of CIM monolithic chromatography for sample preparation step in NGS studies targeting viruses in fresh or marine water. The step-by-step protocol will include a case study where CIM concentration was used to study the virome of a wastewater sample using NGS.

Electrodeposition as a sample preparation technique for TXRF analysis

International Nuclear Information System (INIS)

Griesel, S.; Reus, U.; Prange, A.

2000-01-01

TXRF analysis of trace elements at concentrations in the μg/L range and below in high salt matrices normally requires a number of sample preparation steps that include separation of the salt matrix and preconcentration of the trace elements. A neat approach which allows samples to be prepared straightforwardly in a single step involves the application of electrochemical deposition using the TXRF sample support itself as an electrode. For this work a common three-electrode arrangement (radiometer analytical) with a rotating disc electrode as the working electrode, as is frequently employed in voltametric analysis, has been used. A special electrode tip has been constructed as a holder for the sample carrier which consists of polished glassy carbon. This material has been proven to be suitable for both its electrical and chemical properties. Measurements of the trace elements were performed using the ATOMIKA 8030C TXRF spectrometer, with the option of variable incident angles. In first experiments an artificial sea water matrix containing various trace elements in the μg/L range has been used. Elements such as Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Cd, Hg, and Pb deposited on glassy carbon carriers. The deposition can be optimized by controlling the potential of the working electrode with respect to the reference electrode. Metal ions with a suitable standard potential are reduced to the metallic state and plated onto the electrode surface. When deposition is finished the sample carrier is demounted, rinsed with ultra-pure water and measured directly. Deposition yields for the elements under investigation are quite similar, and with an appropriate choice of the reference element, quantification can be achieved directly by internal standardization. The influence of parameters such as time, pH value, and trace element concentration on the deposition yield has been examined, and the results will be presented along with reproducibility studies. (author)

Guidance document for preparing water sampling and analysis plans for UMTRA Project sites. Revision 1

International Nuclear Information System (INIS)

1995-09-01

A water sampling and analysis plan (WSAP) is prepared for each Uranium Mill Tailings Remedial Action (UMTRA) Project site to provide the rationale for routine ground water sampling at disposal sites and former processing sites. The WSAP identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the routine ground water monitoring stations at each site. This guidance document has been prepared by the Technical Assistance Contractor (TAC) for the US Department of Energy (DOE). Its purpose is to provide a consistent technical approach for sampling and monitoring activities performed under the WSAP and to provide a consistent format for the WSAP documents. It is designed for use by the TAC in preparing WSAPs and by the DOE, US Nuclear Regulatory Commission, state and tribal agencies, other regulatory agencies, and the public in evaluating the content of WSAPS

Sample preparation for large-scale bioanalytical studies based on liquid chromatographic techniques.

Science.gov (United States)

Medvedovici, Andrei; Bacalum, Elena; David, Victor

2018-01-01

Quality of the analytical data obtained for large-scale and long term bioanalytical studies based on liquid chromatography depends on a number of experimental factors including the choice of sample preparation method. This review discusses this tedious part of bioanalytical studies, applied to large-scale samples and using liquid chromatography coupled with different detector types as core analytical technique. The main sample preparation methods included in this paper are protein precipitation, liquid-liquid extraction, solid-phase extraction, derivatization and their versions. They are discussed by analytical performances, fields of applications, advantages and disadvantages. The cited literature covers mainly the analytical achievements during the last decade, although several previous papers became more valuable in time and they are included in this review. Copyright © 2017 John Wiley & Sons, Ltd.

Sample Preparation and Identification of Biological, Chemical and Mid-Spectrum Agents

National Research Council Canada - National Science Library

Hancock, J. R; Dragon, D. C

2005-01-01

A general survey of sample preparation and identification techniques for biological, chemical and mid-spectrum agents was conducted as part of Canada's contribution to a joint NATO Allied Engineering Publication (AEP) handbook...

Bi-functional properties of Fe3O4@YPO4:Eu hybrid nanoparticles: hyperthermia application.

Science.gov (United States)

Prasad, A I; Parchur, A K; Juluri, R R; Jadhav, N; Pandey, B N; Ningthoujam, R S; Vatsa, R K

2013-04-14

Magnetic nanoparticles based hyperthermia therapy is a possible low cost and effective technique for killing cancer tissues in the human body. Fe3O4 and Fe3O4@YPO4:5Eu hybrid magnetic nanoparticles are prepared by co-precipitation method and their average particle sizes are found to be ∼10 and 25 nm, respectively. The particles are spherical, non-agglomerated and highly dispersible in water. The crystallinity of as-prepared YPO4:5Eu sample is more than Fe3O4@YPO4:5Eu hybrid magnetic nanoparticles. The chemical bonds interaction between Fe3O4 and YPO4:5Eu is confirmed through FeO-P. The magnetization of hybrid nanocomposite shows magnetization Ms = 11.1 emu g(-1) with zero coercivity (measured at 2 × 10(-4) Oe) at room temperature indicating superparamagnetic behaviour. They attain hyperthermia temperature (~42 °C) under AC magnetic field showing characteristic induction heating of the prepared nanohybrid and they will be potential material for biological application. Samples produce the red emission peaks at 618 nm and 695 nm, which are in range of biological window. The quantum yield of YPO4:5Eu sample is found to be 12%. Eu(3+) present on surface and core could be distinguished from luminescence decay study. Very high specific absorption rate up to 100 W g(-1) could be achieved. The intracellular uptake of nanocomposites is found in mouse fibrosarcoma (Wehi 164) tumor cells by Prussian blue staining.

Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Nomura, Cassiana S.; Silva, Cintia S.; Nogueira, Ana R.A.; Oliveira, Pedro V.

2005-01-01

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 μg of W + 200 μg 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 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1 , respectively. The relative standard deviations were lower than 6% (n = 5). The

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. Copyright © 2013 Elsevier Ltd. All rights reserved.

Carbon nanotube TiO2 hybrid films for detecting traces of O2

Science.gov (United States)

Llobet, E.; Espinosa, E. H.; Sotter, E.; Ionescu, R.; Vilanova, X.; Torres, J.; Felten, A.; Pireaux, J. J.; Ke, X.; Van Tendeloo, G.; Renaux, F.; Paint, Y.; Hecq, M.; Bittencourt, C.

2008-09-01

Hybrid titania films have been prepared using an adapted sol-gel method for obtaining well-dispersed hydrogen plasma-treated multiwall carbon nanotubes in either pure titania or Nb-doped titania. The drop-coating method has been used to fabricate resistive oxygen sensors based on titania or on titania and carbon nanotube hybrids. Morphology and composition studies have revealed that the dispersion of low amounts of carbon nanotubes within the titania matrix does not significantly alter its crystallization behaviour. The gas sensitivity studies performed on the different samples have shown that the hybrid layers based on titania and carbon nanotubes possess an unprecedented responsiveness towards oxygen (i.e. more than four times higher than that shown by optimized Nb-doped TiO2 films). Furthermore, hybrid sensors containing carbon nanotubes respond at significantly lower operating temperatures than their non-hybrid counterparts. These new hybrid sensors show a strong potential for monitoring traces of oxygen (i.e. beverage industry.

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...

Microfluidic devices for sample preparation and rapid detection of foodborne pathogens

DEFF Research Database (Denmark)

Kant, Krishna; Shahbazi, Mohammad-Ali; Dave, Vivek Priy

2018-01-01

and improve the limit of detections. Integration of pathogen capturing bio-receptors on microfluidic devices is a crucial step, which can facilitate recognition abilities in harsh chemical and physical conditions, offering a great commercial benefit to the food-manufacturing sector. This article reviews...... diagnosis competences. This has prompted researchers to call the current status of detection approaches into question and leverage new technologies for superior pathogen sensing outcomes. Novel strategies mainly rely on incorporating all the steps from sample preparation to detection in miniaturized devices...... recent advances in current state-of-the-art of sample preparation and concentration from food matrices with focus on bacterial capturing methods and sensing technologies, along with their advantages and limitations when integrated into microfluidic devices for online rapid detection of pathogens in foods...

Ballistic Impact Response of Woven Hybrid Coir/Kevlar Laminated Composites

Directory of Open Access Journals (Sweden)

Azrin Hani A.R

2016-01-01

Full Text Available The effects of different laminated hybrid composites stacking configuration subjected to ballistic impact were investigated. The hybrid composites consist of woven coir (C and woven Kevlar (K layers laminated together. The samples of woven coir were prepared using handloom device. The composites were produced by stacking the laminated woven coir and Kevlar alternately with the presence of the binder. The samples were tested under ballistic impact with different stacking configuration. The results obtained had successfully achieved the National Institute of Justice (NIJ standard level IIA with energy absorption of 435.6 kJ and 412.2 kJ under the projectile speed of between 330 m/s and 321 m/s respectively. Samples that having Kevlar layer at the front face and woven coir layer as back face achieved partial penetration during projectile impact. This orientation is proven to have good impact energy absorption and able to stop projectile at the second panel of the composites.

Sample preparation method for the combined extraction of ethyl glucuronide and drugs of abuse in hair.

Science.gov (United States)

Meier, Ulf; Briellmann, Thomas; Scheurer, Eva; Dussy, Franz

2018-04-01

Often in hair analysis, a small hair sample is available while the analysis of a multitude of structurally diverse substances with different concentration ranges is demanded. The analysis of the different substances often requires different sample preparation methods, increasing the amount of required hair sample. When segmental hair analysis is necessary, the amount of hair sample needed is further increased. Therefore, the required sample amount for a full analysis can quickly exceed what is available. To combat this problem, a method for the combined hair sample preparation using a single extraction procedure for analysis of ethyl glucuronide with liquid chromatography-multistage fragmentation mass spectrometry/multiple reaction monitoring (LC-MS 3 /MRM) and common drugs of abuse with LC-MRM was developed. The combined sample preparation is achieved by separating ethyl glucuronide from the drugs of abuse into separate extracts by fractionation in the solid-phase extraction step during sample clean-up. A full validation for all substances for the parameters selectivity, linearity, limit of detection, limit of quantification, accuracy, precision, matrix effects, and recovery was successfully completed. The following drugs of abuse were included in the method: Amphetamine; methamphetamine; 3,4-methylenedioxy-N-methylamphetamine (MDMA); 3,4-methylenedioxyamphetamine (MDA); 3,4-methylenedioxy-N-ethylamphetamine (MDE); morphine; 6-monoacetylmorphine; codeine; acetylcodeine; cocaine; benzoylecgonine; norcocaine; cocaethylene; methadone; 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) and methylphenidate. In conclusion, as only 1 sample preparation is needed with 1 aliquot of hair, the presented sample preparation allows an optimal analysis of both ethyl glucuronide and of the drugs of abuse, even when the sample amount is a limiting factor. Copyright © 2017 John Wiley & Sons, Ltd.

Study of sample preparation in the measurement of 36Ar(n, p)36Cl reaction cross section

International Nuclear Information System (INIS)

Jiang Songsheng; Hemick, T.K.

1992-01-01

The preparation of enriched 36 Ar gas samples and 36 Cl samples for the use in the AMS measurement of 36 Ar(n, p) 36 Cl reaction cross section was described. The 36 Ar samples prepared had the volumes of about 0.4 ml and the weights of about 0.5 mg. The uncertainty in atomic numbers of 36 Ar was (0.3∼0.4)%. The reaction product, 36 Cl, in the 36 Ar was collected and the AgCl samples were prepared

Dynamic Headspace Sampling as an Initial Step for Sample Preparation in Chromatographic Analysis.

Science.gov (United States)

Wojnowski, Wojciech; Majchrzak, Tomasz; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

2017-11-01

This work represents a brief summary of the use of dynamic headspace (DHS) as a technique for sample preparation in chromatographic analysis. Despite numerous developments in the area of analyte isolation and enrichment, DHS remains one of the fundamental methods used with GC. In our opinion, interest in this technique will not diminish significantly because it conforms to stipulations of green analytical chemistry. Moreover, DHS fulfills the need for methods that facilitate detection and determination of analytes present at ultratrace levels in complex matrixes. The main focus of this work was placed on the theoretical fundamentals of this method. Also described herein were DHS development, the advantages and disadvantages of this technique compared with other headspace sampling techniques, and selected examples of its applications in food and environmental analyses.

Chitosan-nanosilica hybrid materials: Preparation and properties

International Nuclear Information System (INIS)

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

2014-01-01

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 2 , TiO 2 /SiO 2 and Al 2 O 3 /SiO 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 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

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.

Ultrasonic assisted extraction - an alternative for sample preparation (M4)

International Nuclear Information System (INIS)

Santos Junior, P.; Barbosa Junior, F.; Krug, F.J.; Trevizan, L.C.; Nobrega, J.A.

2002-01-01

Full text: In the last years the ultrasound assisted metal extraction has been frequency proposed as a simple and inexpensive alternative for sample preparation of biological and inorganic samples. The extraction effect is considered as being caused by acoustic cavitation, that is, bubble formation and subsequent disruptive action. The collapse of bubbles created by sonication of solutions results in the generation of extremely high local temperature and pressure gradients, which may be regarded as localized 'hot spots'. On a timescale of about 10 -10 s, effective local pressures and temperature of about 10 5 atm and about 5000 K, respectively, are generated under sonochemical conditions. Usually, this method uses a diluted acid medium decreasing blank values and reducing both reagents and time consumption compared to traditional wet digestion systems using conductive or microwave-assisted heating. Furthermore, sonication can also allow the preparation of samples directly within the sample container, thereby preventing sample losses and minimizing sample contamination. Although some controversial results concerning metals extraction behavior have been reported, they could be explained by analyte-matrix interaction and the ability of the ultrasonic processor to generate ultrasound (i.e. the use of an ultrasonic bath or an ultrasonic probe at different power, frequency, and amplitude). This contribution presents a review of ultrasound assisted metal extraction and recent performance data obtained in our laboratory for determination of elements in biological materials, soils and sediments by ICP-OES and ETAAS. The effect of extraction parameters, such as type and concentration of the leaching solution, sonication time and performance of ultrasonic processor (bath or probe) will be presented. (author)

Homogeneous immunosubtraction integrated with sample preparation is enabled by a microfluidic format

Science.gov (United States)

Apori, Akwasi A.; Herr, Amy E.

2011-01-01

Immunosubtraction is a powerful and resource-intensive laboratory medicine assay that reports both protein mobility and binding specificity. To expedite and automate this electrophoretic assay, we report on advances to the electrophoretic immunosubtraction assay by introducing a homogeneous, not heterogeneous, format with integrated sample preparation. To accomplish homogeneous immunosubtraction, a step-decrease in separation matrix pore-size at the head of a polyacrylamide gel electrophoresis (PAGE) separation channel enables ‘subtraction’ of target analyte when capture antibody is present (as the large immune-complex is excluded from PAGE), but no subtraction when capture antibody is absent. Inclusion of sample preparation functionality via small pore size polyacrylamide membranes is also key to automated operation (i.e., sample enrichment, fluorescence sample labeling, and mixing of sample with free capture antibody). Homogenous sample preparation and assay operation allows on-the-fly, integrated subtraction of one to multiple protein targets and reuse of each device. Optimization of the assay is detailed which allowed for ~95% subtraction of target with 20% non-specific extraction of large species at the optimal antibody-antigen ratio, providing conditions needed for selective target identification. We demonstrate the assay on putative markers of injury and inflammation in cerebrospinal fluid (CSF), an emerging area of diagnostics research, by rapidly reporting protein mobility and binding specificity within the sample matrix. We simultaneously detect S100B and C-reactive protein, suspected biomarkers for traumatic brain injury (TBI), in ~2 min. Lastly, we demonstrate S100B detection (65 nM) in raw human CSF with a lower limit of detection of ~3.25 nM, within the clinically relevant concentration range for detecting TBI in CSF. Beyond the novel CSF assay introduced here, a fully automated immunosubtraction assay would impact a spectrum of routine but labor

Over-Sampling Codebook-Based Hybrid Minimum Sum-Mean-Square-Error Precoding for Millimeter-Wave 3D-MIMO

KAUST Repository

Mao, Jiening

2018-05-23

Abstract: Hybrid precoding design is challenging for millimeter-wave (mmWave) massive MIMO. Most prior hybrid precoding schemes are designed to maximize the sum spectral efficiency (SSE), while seldom investigate the bit-error-rate (BER). Therefore, this letter designs an over-sampling codebook (OSC)-based hybrid minimum sum-mean-square-error (min-SMSE) precoding to optimize the BER. Specifically, given the effective baseband channel consisting of the real channel and analog precoding, we first design the digital precoder/combiner based on min-SMSE criterion to optimize the BER. To further reduce the SMSE between the transmit and receive signals, we propose an OSC-based joint analog precoder/combiner (JAPC) design. Simulation results show that the proposed scheme can achieve the better performance than its conventional counterparts.

Over-Sampling Codebook-Based Hybrid Minimum Sum-Mean-Square-Error Precoding for Millimeter-Wave 3D-MIMO

KAUST Repository

Mao, Jiening; Gao, Zhen; Wu, Yongpeng; Alouini, Mohamed-Slim

2018-01-01

Hybrid precoding design is challenging for millimeter-wave (mmWave) massive MIMO. Most prior hybrid precoding schemes are designed to maximize the sum spectral efficiency (SSE), while seldom investigate the bit-error-rate (BER). Therefore, this letter designs an over-sampling codebook (OSC)-based hybrid minimum sum-mean-square-error (min-SMSE) precoding to optimize the BER. Specifically, given the effective baseband channel consisting of the real channel and analog precoding, we first design the digital precoder/combiner based on min-SMSE criterion to optimize the BER. To further reduce the SMSE between the transmit and receive signals, we propose an OSC-based joint analog precoder/combiner (JAPC) design. Simulation results show that the proposed scheme can achieve the better performance than its conventional counterparts.

Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

Directory of Open Access Journals (Sweden)

Abuzar Kabir

2017-12-01

Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

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.

Robotic sample preparation for radiochemical plutonium and americium analyses

International Nuclear Information System (INIS)

Stalnaker, N.; Beugelsdijk, T.; Thurston, A.; Quintana, J.

1985-01-01

A Zymate robotic system has been assembled and programmed to prepare samples for plutonium and americium analyses by radioactivity counting. The system performs two procedures: a simple dilution procedure and a TTA (xylene) extraction of plutonium. To perform the procedures, the robotic system executes 11 unit operations such as weighing, pipetting, mixing, etc. Approximately 150 programs, which require 64 kilobytes of memory, control the system. The system is now being tested with high-purity plutonium metal and plutonium oxide samples. Our studies indicate that the system can give results that agree within 5% at the 95% confidence level with determinations performed manually. 1 ref., 1 fig., 1 tab

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

2017-11-30

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 Elsevier B.V. All rights reserved.

Ultrafast preparation of a polyhedral oligomeric silsesquioxane-based ionic liquid hybrid monolith via photoinitiated polymerization, and its application to capillary electrochromatography of aromatic compounds.

Science.gov (United States)

Zhang, Bingyu; Lei, Xiaoyun; Deng, Lijun; Li, Minsheng; Yao, Sicong; Wu, Xiaoping

2018-06-06

An ionic liquid hybrid monolithic capillary column was prepared within 7 min via photoinitiated free-radical polymerization of an ionic liquid monomer (1-butyl-3-vinylimidazolium-bis[(trifluoromethyl)sulfonyl]imide); VBIMNTF 2 ) and a methacryl substituted polyhedral oligomeric silsesquioxane (POSS-MA) acting as a cross-linker. The effects of composition of prepolymerization solution and initiation time on the porous structure and electroosmotic flow (EOF) of monolithic column were investigated. The hybrid monolith was characterized by scanning electron microscopy and FTIR. Owing to the introduction of a rigid nanosized POSS silica core and ionic liquids with multiple interaction sites, the monolithic column has a well-defined 3D skeleton morphology, good mechanical stability, and a stable anodic electroosmotic flow. The hybrid monolithic stationary phase was applied to the capillary electrochromatographic separation of various alkylbenzenes, phenols, anilines and polycyclic aromatic hydrocarbons (PAHs). The column efficiency is highest (98,000 plates/m) in case of alkylbenzenes. Mixed-mode retention mechanisms including hydrophobic interactions, π-π stacking, electrostatic interaction and electrophoretic mobility can be observed. This indicates the potential of this material in terms of efficient separation of analytes of different structural type. Graphical Abstract Preparation of a mixed-mode ionic liquid hybrid monolithic column via photoinitiated polymerization of methacryl substituted polyhedral oligomeric silsesquioxane (POSS-MA) and 1-butyl-3-vinylimidazolium-bis[(trifluoromethyl)sulfonyl]imide (VBIMNTF 2 ) ionic liquid for use in capillary electrochromatography.

Integrated Automation of High-Throughput Screening and Reverse Phase Protein Array Sample Preparation

DEFF Research Database (Denmark)

Pedersen, Marlene Lemvig; Block, Ines; List, Markus

into automated robotic high-throughput screens, which allows subsequent protein quantification. In this integrated solution, samples are directly forwarded to automated cell lysate preparation and preparation of dilution series, including reformatting to a protein spotter-compatible format after the high......-throughput screening. Tracking of huge sample numbers and data analysis from a high-content screen to RPPAs is accomplished via MIRACLE, a custom made software suite developed by us. To this end, we demonstrate that the RPPAs generated in this manner deliver reliable protein readouts and that GAPDH and TFR levels can...

Influence of rice sample preparation and milling procedures on milling quality appraisals

Science.gov (United States)

The objective of this research was to investigate the effect of sample preparation and milling procedure on milling quality appraisals of rough rice. Samples of freshly harvested medium-grain rice (M202) with different initial moisture contents (MCs) ranging from 20.2% to 25.1% (w.b.) were used for...

Microextraction sample preparation techniques in biomedical analysis.

Science.gov (United States)

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

2014-11-01

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

Notes on sample preparation of food: food of plant and animal origins, and daily meals

International Nuclear Information System (INIS)

Heilgeist, M.

1992-01-01

The procedure of food sample preparation to determine their specific radioactivity, analogous to chemical residue analysis, is laid down in the relevant sets of regulations. Several procedural steps of sample preparation of single food and composite food are dealt with. The sample size necessary for gamma spectroscopy and Sr-89/Sr-90 analysis, and the incineration step to enrich radionuclides are explained. Finally, enrichment by freeze drying of the high-volatile radionuclide I-131 is considered. (orig.) [de

Hyper-cross-linked, hybrid membranes via interfacial polymerization

NARCIS (Netherlands)

Raaijmakers, Michiel

2015-01-01

Hyper-cross-linked, hybrid membranes consist of covalent networks of alternating organic and inorganic, or biological groups. This thesis reports on the preparation of such hybrid networks via interfacial polymerization. The structure-property relationships of the hybrid networks depend strongly on

Sample collection and preparation of biofluids and extracts for gas chromatography-mass spectrometry.

Science.gov (United States)

Emwas, Abdul-Hamid M; Al-Talla, Zeyad A; Kharbatia, Najeh M

2015-01-01

To maximize the utility of gas chromatography-mass spectrometry (GC-MS) in metabonomics research, all stages of the experimental design should be standardized, including sample collection, storage, preparation, and sample separation. Moreover, the prerequisite for any GC-MS analysis is that a compound must be volatile and thermally stable if it is to be analyzed using this technique. Since many metabolites are nonvolatile and polar in nature, they are not readily amenable to analysis by GC-MS and require initial chemical derivatization of the polar functional groups in order to reduce the polarity and to increase the thermal stability and volatility of the analytes. In this chapter, an overview is presented of the optimum approach to sample collection, storage, and preparation for gas chromatography-mass spectrometry-based metabonomics with particular focus on urine samples as example of biofluids.

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

OpenAIRE

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

1998-01-01

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

COED Transactions, Vol. X, No. 10, October 1978. Simulation of a Sampled-Data System on a Hybrid Computer.

Science.gov (United States)

Mitchell, Eugene E., Ed.

The simulation of a sampled-data system is described that uses a full parallel hybrid computer. The sampled data system simulated illustrates the proportional-integral-derivative (PID) discrete control of a continuous second-order process representing a stirred-tank. The stirred-tank is simulated using continuous analog components, while PID…

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

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...... AFFF-ICP-MS fractograms, which corresponded to the enzymatic digests, showed a major nano-peak (about 80 % recovery of AgNPs spiked to the meat) plus new smaller peaks that eluted close to the void volume of the fractograms. Small, but significant shifts in retention time of AFFF peaks were observed...... for the meat sample extracts and the corresponding neat AgNP suspension, and rendered sizing by way of calibration with AgNPs as sizing standards inaccurate. In order to gain further insight into the sizes of the separated AgNPs, or their possible dissolved state, fractions of the AFFF eluate were collected...

Effect of method of sample preparation on ruminal in situ ...

African Journals Online (AJOL)

Midmar) was harvested at three and four weeks after cutting and fertilizing with 200 kg nitrogen (N)/ha. Freshly cut herbage was used to investigate the following four sample preparation methods. In trial 1, herbage was (1) chopped with a paper-cutting guillotine into 5-10 mm lengths, representing fresh (FR) herbage; ...

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.

Gold nanoparticle-embedded silk protein-ZnO nanorod hybrids for flexible bio-photonic devices

Science.gov (United States)

Gogurla, Narendar; Kundu, Subhas C.; Ray, Samit K.

2017-04-01

Silk protein has been used as a biopolymer substrate for flexible photonic devices. Here, we demonstrate ZnO nanorod array hybrid photodetectors on Au nanoparticle-embedded silk protein for flexible optoelectronics. Hybrid samples exhibit optical absorption at the band edge of ZnO as well as plasmonic energy due to Au nanoparticles, making them attractive for selective UV and visible wavelength detection. The device prepared on Au-silk protein shows a much lower dark current and a higher photo to dark-current ratio of ∼105 as compared to the control sample without Au nanoparticles. The hybrid device also exhibits a higher specific detectivity due to higher responsivity arising from the photo-generated hole trapping by Au nanoparticles. Sharp pulses in the transient photocurrent have been observed in devices prepared on glass and Au-silk protein substrates due to the light induced pyroelectric effect of ZnO, enabling the demonstration of self-powered photodetectors at zero bias. Flexible hybrid detectors have been demonstrated on Au-silk/polyethylene terephthalate substrates, exhibiting characteristics similar to those fabricated on rigid glass substrates. A study of the performance of photodetectors with different bending angles indicates very good mechanical stability of silk protein based flexible devices. This novel concept of ZnO nanorod array photodetectors on a natural silk protein platform provides an opportunity to realize integrated flexible and self-powered bio-photonic devices for medical applications in near future.

Influence of sample preparation on the microstructure of tooth enamel apatite

Czech Academy of Sciences Publication Activity Database

Kallistová, Anna; Skála, Roman; Horáček, I.; Miyajima, N.; Malíková, R.

2015-01-01

Roč. 48, č. 3 (2015), s. 763-768 ISSN 0021-8898 Institutional support: RVO:67985831 Keywords : X-ray powder diffraction * sample preparation * microstructure * dental hydroxyapatite Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.720, year: 2014

THE EFFECT OF TWO - ELEMNETED PROBIOTIC PREPARATE ON BASIC FATTENING PARAMETERS OF HYBRID HUBBARD JV

Directory of Open Access Journals (Sweden)

J. WEIS

2007-05-01

Full Text Available Growth stimulators on basic of probiotics are preparations biological character with correctly defined strains live micro organisms. Most important signification their used consisted in positive stimulation natural micro flora of digestive tract therefore fortified mechanisms of autoimmunity system of organism, what very narrowly relate with achieved utility animal parameters. Healthy and vital individuals marking better nutrient utilisation, equally growth intensity consistent higher slaughter yield. Propoul is two - elemental probiotic preparate designated for poultry, which include special selected strain of genus Lactobacillus. Results their affect is improve of immunity, metabolism and also favourable effect on utility.In 42- days experiment we tested effect of probiotic preparate Propoul on basic fattening parameters of hybrid Hubbard JV. We divided broiler chickens into three groups - control (C without probiotic, experimental 1(E1 with decreased probiotic amount during fattening period and experimental 2 (E2 with constant concentration of testing preparate. Propoul in fluid form we was applicating in drinking water. Effect of probiotic positive manifested in all observed parameters. With exception organic growth and growth index, where we founded favourable effect his application especially in first two weeks in all other both experimentals by expressive rate dominated in achieved values in compared with control. Mostly, from aspect average live weight, where we recorded from 2. week to end of fattening period statistically high significant (P<0.01 and statistically very high significant difference (P<0.001 in benefit of E1 and E2 groups.

Stochastic Primal-Dual Hybrid Gradient Algorithm with Arbitrary Sampling and Imaging Application

KAUST Repository

Chambolle, Antonin; Ehrhardt, Matthias J.; Richtarik, Peter; Schö nlieb, Carola-Bibiane

2017-01-01

We propose a stochastic extension of the primal-dual hybrid gradient algorithm studied by Chambolle and Pock in 2011 to solve saddle point problems that are separable in the dual variable. The analysis is carried out for general convex-concave saddle point problems and problems that are either partially smooth / strongly convex or fully smooth / strongly convex. We perform the analysis for arbitrary samplings of dual variables, and obtain known deterministic results as a special case. Several variants of our stochastic method significantly outperform the deterministic variant on a variety of imaging tasks.

Stochastic Primal-Dual Hybrid Gradient Algorithm with Arbitrary Sampling and Imaging Application

KAUST Repository

Chambolle, Antonin

2017-06-15

We propose a stochastic extension of the primal-dual hybrid gradient algorithm studied by Chambolle and Pock in 2011 to solve saddle point problems that are separable in the dual variable. The analysis is carried out for general convex-concave saddle point problems and problems that are either partially smooth / strongly convex or fully smooth / strongly convex. We perform the analysis for arbitrary samplings of dual variables, and obtain known deterministic results as a special case. Several variants of our stochastic method significantly outperform the deterministic variant on a variety of imaging tasks.

Investigation of mechanical properties of hemp/glass fiber reinforced nano clay hybrid composites

Science.gov (United States)

Unki, Hanamantappa Ningappa; Shivanand, H. K.; Vidyasagar, H. N.

2018-04-01

Over the last twenty to thirty years composite materials have been used in engineering field. Composite materials possess high strength, high strength to weight ratio due to these facts composite materials are becoming popular among researchers and scientists. The major proportion of engineering materials consists of composite materials. Composite materials are used in vast applications ranging from day-to-day household articles to highly sophisticated applications. In this paper an attempt is made to prepare three different composite materials using e-glass and Hemp. In this present investigation hybrid composite of Hemp, Glass fiber and Nano clay will be prepared by Hand-layup technique. The glass fiber used in this present investigation is E-glass fiber bi-directional: 90˚ orientation. The composite samples will be made in the form of a Laminates. The wt% of nanoclay added in the preparation of sample is 20 gm constant. The fabricated composite Laminate will be cut into corresponding profiles as per ASTM standards for Mechanical Testing. The effect of addition of Nano clay and variation of Hemp/glass fibers will be studied. In the present work, a new Hybrid composite is developed in which Hemp, E glass fibers is reinforced with epoxy resin and with Nano clay.

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.

Effects of the LiFePO4 content and the preparation method on the properties of (LiFePO4+AC/Li4Ti5O12 hybrid battery–capacitors

Directory of Open Access Journals (Sweden)

XUE BU HU

2010-09-01

Full Text Available Two composite cathode materials containing LiFePO4 and activated carbon (AC were synthesized by an in-situ method and a direct mixing technique, which are abbreviated as LAC and DMLAC, respectively. Hybrid battery–capacitors LAC/Li4Ti5O12 and DMLAC/Li4Ti5O12 were then assembled. The effects of the content of LiFePO4 and the preparation method on the cyclic voltammograms, the rate of charge–discharge and the cycle performance of the hybrid battery–capacitors were investigated. The results showed the overall electrochemical performance of the hybrid battery–capacitors was the best when the content of LiFePO4 in the composite cathode materials was in the range from 11.8 to 28.5 wt. %, while the preparation method had almost no impact on the electrochemical performance of the composite cathodes and hybrid battery–capacitors. Moreover, the hybrid battery–capacitor devices had a good cycle life performance at high rates. After 1000 cycles, the capacity loss of the DMLAC/Li4Ti5O12 hybrid battery–capacitor device at 4C was no more than 4.8 %. Moreover, the capacity loss would be no more than 9.6 % after 2000 cycles at 8C.

An electrodeposition method for the preparation of actinides and Ra samples for α spectrometry

International Nuclear Information System (INIS)

Garcia-Tenorio, R.; Garcia-Leon, M.; Madurga, G.; Piazza, C.

1986-01-01

As it is confirmed in this work, electrodeposition of α radionuclides gives a simple method for preparing α samples of high spectrometric quality, compared to those prepared by evaporation. Then we give the methods for electrodepositon or α emitters use in our Department. Actinides α emitters are electroplated from a 1% H 2 SO 4 medium with a recovery of about 90%. The samples of Ra are prepared by electrodeposition from a HCl + CH 3 -COONH 4 medium at pH approx.= 5. In this case the recovery reaches a value that ranges from 70 to 90%. For these measurements a Si surface barrier detector has been used. Some of its features are discussed in the text. (author)

On the preparation of as-produced and purified single-walled carbon nanotube samples for standardized X-ray diffraction characterization

International Nuclear Information System (INIS)

Allaf, Rula M.; Rivero, Iris V.; Spearman, Shayla S.; Hope-Weeks, Louisa J.

2011-01-01

The aim of this research was to specify proper sample conditioning for acquiring representative X-ray diffraction (XRD) profiles for single-walled carbon nanotube (SWCNT) samples. In doing so, a specimen preparation method for quantitative XRD characterization of as-produced and purified arc-discharge SWCNT samples has been identified. Series of powder XRD profiles were collected at different temperatures, states, and points of time to establish appropriate conditions for acquiring XRD profiles without inducing much change to the specimen. It was concluded that heating in the 300-450 deg. C range for 20 minutes, preferably vacuum-assisted, and then sealing the sample is an appropriate XRD specimen preparation technique for purified arc-discharge SWCNT samples, while raw samples do not require preconditioning for characterization. - Graphical Abstract: A sample preparation method for XRD characterization of as-produced and purified arc-discharge SWCNT samples is identified. The preparation technique seeks to acquire representative XRD profiles without inducing changes to the samples. Purified samples required 20 minutes of heating at (300-450)deg. C, while raw samples did not require preconditioning for characterization. Highlights: → Purification routines may induce adsorption onto the SWCNT samples. → Heating a SWCNT sample may result in material loss, desorption, and SWCNTs closing. → Raw arc-discharge samples do not require preparation for XRD characterization. → Heating is appropriate specimen preparation for purified and heat-treated samples. → XRD data fitting is required for structural analysis of SWCNT bundles.

Inexpensive sol-gel synthesis of multiwalled carbon nanotube-TiO{sub 2} hybrids for high performance antibacterial materials

Energy Technology Data Exchange (ETDEWEB)

Abbas, Nadir; Shao, Godlisten N. [Department of Fusion Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of); Haider, M. Salman [Department of Civil and Environmental System Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of); Imran, Syed Muhammad; Park, Sung Soo; Jeon, Sun-Jeong [Department of Fusion Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of); Kim, Hee Taik, E-mail: khtaik@hanyang.ac.kr [Department of Fusion Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do 426-791 (Korea, Republic of)

2016-11-01

This study reports an inexpensive sol-gel method to synthesize TiO{sub 2}-CNT hybrid materials. Synthesized TiO{sub 2}-CNT materials show strong antibacterial activity in the absence of light. Cheap TiO{sub 2} source TiOCl{sub 2} is used during synthesis in the absence of high temperatures, high pressures and organic solvents. TiO{sub 2}-CNT materials with 0, 2, 5, 10, 15 and 20 wt% of CNT were synthesized and compared for antibacterial activity, surface area, porosity, crystalline structure, chemical state, and HaCaT cell proliferation. The antibacterial strength of hybrid materials increased significantly with the increase in CNT loading amount, and the TiO{sub 2}-CNT samples with a CNT loading of 10 wt% or more nearly removed all of the E.coli bacteria. HaCaT cell proliferation studies of synthesized hybrid materials illustrated that prepared TiO{sub 2}-CNT systems exhibit minimum cytotoxicity. The characteristics of prepared materials were analyzed by means of XRD, FTIR, Raman spectroscopy, XPS, TEM, and nitrogen gas physisorption studies, compared and discussed. - Highlights: • An inexpensive scheme of preparing TiO{sub 2}-CNT hybrids is presented. • Significant increase in the antibacterial properties of TiO{sub 2} in absence of light • Effects of CNT addition on the physicochemical properties of hybrids are studied. • Antibacterial activity increases with increase in CNT content. • Hybrids show no toxicity towards HaCaT skin cell line.

Novel high dielectric constant hybrid elastomers based on glycerol-insilicone emulsions

DEFF Research Database (Denmark)

Mazurek, Piotr Stanislaw; Skov, Anne Ladegaard

2016-01-01

Novel hybrid elastomers were prepared by speedmixing of two virtually immiscible liquids – glycerol and polydimethylsiloxane (PDMS) prepolymer. Upon crosslinking ofthe PDMS phase of the resulting glycerol-in-silicone emulsion freestanding films were obtained. In this way glycerol became uniformly...... elastomeractuators. Conductivities of samples based on various PDMS compositions with different loadings of embedded glycerol were thoroughly investigated providing useful information about the dielectric behavior....

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

DEFF Research Database (Denmark)