WorldWideScience

Sample records for prepared sample solution

  1. Solution preparation

    Energy Technology Data Exchange (ETDEWEB)

    Seitz, M.G.

    1982-01-01

    Reviewed in this statement are methods of preparing solutions to be used in laboratory experiments to examine technical issues related to the safe disposal of nuclear waste from power generation. Each approach currently used to prepare solutions has advantages and any one approach may be preferred over the others in particular situations, depending upon the goals of the experimental program. These advantages are highlighted herein for three approaches to solution preparation that are currently used most in studies of nuclear waste disposal. Discussion of the disadvantages of each approach is presented to help a user select a preparation method for his particular studies. Also presented in this statement are general observations regarding solution preparation. These observations are used as examples of the types of concerns that need to be addressed regarding solution preparation. As shown by these examples, prior to experimentation or chemical analyses, laboratory techniques based on scientific knowledge of solutions can be applied to solutions, often resulting in great improvement in the usefulness of results.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-04-15

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

  3. Sample preparation and biopharmaceutical analysis

    OpenAIRE

    Farrelly, Gillian

    1998-01-01

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

  4. Microfluidic Sample Preparation for Immunoassays

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-08-09

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

  5. Preservative solution for skeletal muscle biopsy samples

    Science.gov (United States)

    Kurt, Yasemin Gulcan; Kurt, Bulent; Ozcan, Omer; Topal, Turgut; Kilic, Abdullah; Muftuoglu, Tuba; Acikel, Cengizhan; Sener, Kenan; Sahiner, Fatih; Yigit, Nuri; Aydin, Ibrahim; Alay, Semih; Ekinci, Safak

    2015-01-01

    Context: Muscle biopsy samples must be frozen with liquid nitrogen immediately after excision and maintained at -80°C until analysis. Because of this requirement for tissue processing, patients with neuromuscular diseases often have to travel to centers with on-site muscle pathology laboratories for muscle biopsy sample excision to ensure that samples are properly preserved. Aim: Here, we developed a preservative solution and examined its protectiveness on striated muscle tissues for a minimum of the length of time that would be required to reach a specific muscle pathology laboratory. Materials and Methods: A preservative solution called Kurt-Ozcan (KO) solution was prepared. Eight healthy Sprague-Dawley rats were sacrificed; striated muscle tissue samples were collected and divided into six different groups. Muscle tissue samples were separated into groups for morphological, enzyme histochemical, molecular, and biochemical analysis. Statistical method used: Chi-square and Kruskal Wallis tests. Results: Samples kept in the KO and University of Wisconsin (UW) solutions exhibited very good morphological scores at 3, 6, and 18 hours, but artificial changes were observed at 24 hours. Similar findings were observed for the evaluated enzyme activities. There were no differences between the control group and the samples kept in the KO or UW solution at 3, 6, and 18 hours for morphological, enzyme histochemical, and biochemical features. The messenger ribonucleic acid (mRNA) of β-actin gene was protected up to 6 hours in the KO and UW solutions. Conclusion: The KO solution protects the morphological, enzyme histochemical, and biochemical features of striated muscle tissue of healthy rats for 18 hours and preserves the mRNA for 6 hours. PMID:26019417

  6. Preservative solution for skeletal muscle biopsy samples

    Directory of Open Access Journals (Sweden)

    Yasemin Gulcan Kurt

    2015-01-01

    Full Text Available Context : Muscle biopsy samples must be frozen with liquid nitrogen immediately after excision and maintained at -80 o C until analysis. Because of this requirement for tissue processing, patients with neuromuscular diseases often have to travel to centers with on-site muscle pathology laboratories for muscle biopsy sample excision to ensure that samples are properly preserved. Aim: Here, we developed a preservative solution and examined its protectiveness on striated muscle tissues for a minimum of the length of time that would be required to reach a specific muscle pathology laboratory. Materials and Methods: A preservative solution called Kurt-Ozcan (KO solution was prepared. Eight healthy Sprague-Dawley rats were sacrificed; striated muscle tissue samples were collected and divided into six different groups. Muscle tissue samples were separated into groups for morphological, enzyme histochemical, molecular, and biochemical analysis. Statistical method used: Chi-square and Kruskal Wallis tests. Results: Samples kept in the KO and University of Wisconsin (UW solutions exhibited very good morphological scores at 3, 6, and 18 hours, but artificial changes were observed at 24 hours. Similar findings were observed for the evaluated enzyme activities. There were no differences between the control group and the samples kept in the KO or UW solution at 3, 6, and 18 hours for morphological, enzyme histochemical, and biochemical features. The messenger ribonucleic acid (mRNA of β-actin gene was protected up to 6 hours in the KO and UW solutions. Conclusion: The KO solution protects the morphological, enzyme histochemical, and biochemical features of striated muscle tissue of healthy rats for 18 hours and preserves the mRNA for 6 hours.

  7. Sample Preparation for Bioanalytical and Pharmaceutical Analysis.

    Science.gov (United States)

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

    2016-12-06

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

  8. Alternative sample preparation methods for MALDI-MS

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-12-31

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

  9. METALLOGRAPHIC SAMPLE PREPARATION STATION-CONSTRUCTIVE CONCEPT

    Directory of Open Access Journals (Sweden)

    AVRAM Florin Timotei

    2016-11-01

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

  10. Final Report BW Sample Collection& Preparation Device

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-01-31

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

  11. Modular microfluidic system for biological sample preparation

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-09-29

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

  12. Direct visualization of solute locations in laboratory ice samples

    Science.gov (United States)

    Hullar, Ted; Anastasio, Cort

    2016-09-01

    Many important chemical reactions occur in polar snow, where solutes may be present in several reservoirs, including at the air-ice interface and in liquid-like regions within the ice matrix. Some recent laboratory studies suggest chemical reaction rates may differ in these two reservoirs. While investigations have examined where solutes are found in natural snow and ice, few studies have examined either solute locations in laboratory samples or the possible factors controlling solute segregation. To address this, we used micro-computed tomography (microCT) to examine solute locations in ice samples prepared from either aqueous cesium chloride (CsCl) or rose bengal solutions that were frozen using several different methods. Samples frozen in a laboratory freezer had the largest liquid-like inclusions and air bubbles, while samples frozen in a custom freeze chamber had somewhat smaller air bubbles and inclusions; in contrast, samples frozen in liquid nitrogen showed much smaller concentrated inclusions and air bubbles, only slightly larger than the resolution limit of our images (˜ 2 µm). Freezing solutions in plastic vs. glass vials had significant impacts on the sample structure, perhaps because the poor heat conductivity of plastic vials changes how heat is removed from the sample as it cools. Similarly, the choice of solute had a significant impact on sample structure, with rose bengal solutions yielding smaller inclusions and air bubbles compared to CsCl solutions frozen using the same method. Additional experiments using higher-resolution imaging of an ice sample show that CsCl moves in a thermal gradient, supporting the idea that the solutes in ice are present in mobile liquid-like regions. Our work shows that the structure of laboratory ice samples, including the location of solutes, is sensitive to the freezing method, sample container, and solute characteristics, requiring careful experimental design and interpretation of results.

  13. Automated sample preparation for CE-SDS.

    Science.gov (United States)

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

    2013-05-01

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

  14. Sample preparation in biological mass spectrometry

    CERN Document Server

    Ivanov, Alexander R

    2011-01-01

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

  15. Molecularly imprinted polymers for bioanalytical sample preparation.

    Science.gov (United States)

    Gama, Mariana Roberto; Bottoli, Carla Beatriz Grespan

    2017-02-01

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

  16. Preparation and Preservation of Hypoxia UW Solution

    Institute of Scientific and Technical Information of China (English)

    WAN Chidang; WANG Chunyou; LIU Tan; CHENG Rui; YANG Zhiyong

    2007-01-01

    In order to explore the method to prepare hypoxia UW solution and the stability and preservation of hypoxia UW solution, UW solution was purged by argon or air for 15 min or 60 at a flow rate of 0.8 or 2 L/min, and the oxygen partial pressure of UW solution was detected. The hy-poxia UW solution was exposed to the air or sealed up to preserve by using different methods, and the changes of oxygen partial pressure was tested. The results showed that oxygen partial pressure of 50 mL UW solution, purged by argon for 15 min at a flow rate of 2 L/min, was declined from 242±6 mmHg to 83±10 mmHg. After exposure to the air, oxygen partial pressure of hypoxia UW solution was gradually increased to 160±7 mmHg at 48 h. After sealed up by the centrifuge tube and plastic bad filled with argon, oxygen partial pressure of hypoxia UW solution was stable, about 88±13 mmHg at 72 h. It was concluded that oxygen of UW solution could be purged by argon efficiently. Sealed up by the centrifuge tube and plastic bag filled with argon, oxygen partial pressure of UW so- lution could be stabilized.

  17. Biodiversity optimal sampling: an algorithmic solution

    Directory of Open Access Journals (Sweden)

    Alessandro Ferrarini

    2012-03-01

    Full Text Available Biodiversity sampling is a very serious task. When biodiversity sampling is not representative of the biodiversity spatial pattern due to few data or uncorrected sampling point locations, successive analyses, models and simulations are inevitably biased. In this work, I propose a new solution to the problem of biodiversity sampling. The proposed approach is proficient for habitats, plant and animal species, in addition it is able to answer the two pivotal questions of biodiversity sampling: 1 how many sampling points and 2 where are the sampling points.

  18. OPC Paste Samples Exposed To Aggressive Solutions. Cementitious Barriers Partnership

    Energy Technology Data Exchange (ETDEWEB)

    Langton, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2014-11-01

    The study presented in this report focused on a low-activity wasteform containing a high pH pore solution with a significant level of sulfate. The purpose of the study was to improve understanding of the complex concrete/wasteform reactive transport problem, in particular the role of pH in sulfate attack. Paste samples prepared at three different water-to-cement ratios were tested. The mixtures were prepared with ASTM Type I cement, without additional admixtures. The samples were exposed to two different sodium sulfate contact solutions. The first solution was prepared at 0.15M Na2SO4. The second solution also incorporated 0.5M NaOH, to mimic the high pH conditions found in Saltstone. The data collected indicated that in Na2SO4 solution, damage occurs to the pastes. In the case of the high pH sulfate solution (Na2SO4 + NaOH), no signs of damage was observed on any of the paste mixtures. These results indicate that the high sulfate content found in the wasteform pore solution will not necessarily lead to severe damage to concrete. Good-quality mixtures could thus prove durable over the long term, and act as an effective barrier to prevent radionuclides from reaching the environment.

  19. OPC Paste Samples Exposed To Aggressive Solutions. Cementitious Barriers Partnership

    Energy Technology Data Exchange (ETDEWEB)

    Langton, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2014-11-01

    The study presented in this report focused on a low-activity wasteform containing a high-pH pore solution with a significant level of sulfate. The purpose of the study was to improve understanding of the complex concrete/wasteform reactive transport problem, in particular, the role of pH in sulfate attack. Paste samples prepared at three different water-to-cement ratios were tested. The mixtures were prepared with ASTM Type I cement, without additional admixtures. The samples were exposed to two different sodium sulfate contact solutions. The first solution was prepared at 0.15M Na2SO4. The second solution also incorporated 0.5M NaOH, to mimic the high pH conditions found in Saltstone. The data collected indicated that, in Na2SO4 solution, damage occurs to the pastes. In the case of the high-pH sulfate solution (Na2SO4 + NaOH), no signs of damage were observed on any of the paste mixtures. These results indicate that the high sulfate content found in the wasteform pore solution will not necessarily lead to severe damage to concrete. Good-quality mixtures could thus prove durable over the long term, and act as an effective barrier to prevent radionuclides from reaching the environment.

  20. Sample preparation for SEM of plant surfaces

    OpenAIRE

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

    2010-01-01

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

  1. 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.

  2. Scanning Electron Microscopy Sample Preparation and Imaging.

    Science.gov (United States)

    Nguyen, Jenny Ngoc Tran; Harbison, Amanda M

    2017-01-01

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

  3. 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.

  4. 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.

  5. Sample preparation for SEM of plant surfaces

    Directory of Open Access Journals (Sweden)

    A.K. Pathan

    2010-01-01

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

  6. Preparation and evaluation of veterinary 20% injectable solution of tylosin

    OpenAIRE

    2010-01-01

    A veterinary injectable aqueous solution of the antibiotic tylosin at a concentration of 20% was prepared under aseptic conditions in dark glass bottles each containing 100 ml. The preparation was intended for animal use only. It contained 200 g tylosin tartrate, 500 ml propylene glycol, benzyl alcohol 40 ml as a preservative and water for injection up to 1000 ml. The preparation was clear yellow viscous aqueous solution free from undesired particles. The preparation complied with the require...

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

    DEFF Research Database (Denmark)

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

    2011-01-01

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

  8. Congener Production in Blood Samples During Preparation and Storage

    DEFF Research Database (Denmark)

    Felby, Søren; Nielsen, Erik

    1995-01-01

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

  9. Titania preparation from soda roasted slag using sulfuric acid solution

    Directory of Open Access Journals (Sweden)

    El-Sayed A. Manaa

    2016-11-01

    Full Text Available This work deals with treatment of the sodium titanate cake results from roasted titania slag using 60% sulfuric acid solution. The working sample produced by roasting titania slag with NaCO3 at 850 °C. After roasting V and Cr species as impurities in the roasted sample are converted to water soluble species as NaVO3 and Na2CrO4 before acid treatment however, the insoluble sodium titanate products (NaFeTiO4, Na8Ti5O14, Na6Ti2O7 and Na2TiO4 are then subjected to H2SO4 acid dissolution. The produced sulfate solution is subjected to hydrolysis step in presence of oxalic acid as a reducing agent. The hydrolyzed precipitate after filtration and washing with H2SO4 solution and warm water is dried at 100 °C and calcinated at 850 °C to prepare high pure TiO2 (99.8% besides removing ferrous sulfate (FeSO4 as a byproduct from the sulfate solution.

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

    Science.gov (United States)

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

    2009-12-07

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

  11. Perfect Solutions for Wearing Preparation in India

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    @@ Presentation of KARL MAYER's reorganised warp preparation business unit during a series of symposia held in India on the 19, 21 and 23 January. KARL MAYER's Warp Preparation Section continues to focus on providing an excellent customer service, and has recently been reorganised to make it even more efficient.

  12. Perfect Solutions for Weaving Preparation in india

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Presentation of KARL MAYER’s reorganised warp preparation business unit during a series of symposia held in India on the 19,21 and 23 January. KARL MAYER’s Warp Preparation Section continues to focus on providing an excellent customer service,and has recently been reorganised to make it even more efficient.Its operations were presented during the

  13. Preparation and evaluation of veterinary 20% injectable solution of tylosin

    Directory of Open Access Journals (Sweden)

    Fouad K. Mohammad

    2010-02-01

    Full Text Available A veterinary injectable aqueous solution of the antibiotic tylosin at a concentration of 20% was prepared under aseptic conditions in dark glass bottles each containing 100 ml. The preparation was intended for animal use only. It contained 200 g tylosin tartrate, 500 ml propylene glycol, benzyl alcohol 40 ml as a preservative and water for injection up to 1000 ml. The preparation was clear yellow viscous aqueous solution free from undesired particles. The preparation complied with the requirements for injectable solutions. It was active in vitro against E. coli (JM83. The preparation of 20% tylosin solution was safe under field conditions in treating sheep and cattle suffering from pneumonia at the dose rate of 1 ml/20 kg body weight, intramuscularly/ day for 3 successive days. In conclusion, we presented the know-how of a veterinary formulation of injectable solution of 20% tylosin for clinical use in ruminants. [Vet. World 2010; 3(1.000: 5-7

  14. Method of 14C Sample Preparation for AMS Measurement

    Directory of Open Access Journals (Sweden)

    YANG Xu-ran

    2015-02-01

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

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

    CERN Document Server

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

    2015-01-01

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

  16. 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.

  17. Liquid sample shuffler for gamma active solutions

    Energy Technology Data Exchange (ETDEWEB)

    Crane, T.W.

    1987-02-01

    An instrument is proposed by Los Alamos National Laboratory for measuring low levels of fission-product-contaminated fissile solutions at the Idaho National Engineering Laboratory (INEL). The proposed unit uses neutrons from a /sup 252/Cf neutron source to induce fissions, and delayed neutrons from the induced fissions are counted once the neutron source is withdrawn. Lead is used to shield the neutron detectors from the gamma-ray dose of the fission products found in the solutions at the INEL plant. The designed sensitivity is 5 mg/l of /sup 235/U in 100 s with a 4-standard-deviation confidence.

  18. Effective shelf-life of prepared sodium hypochlorite solution.

    Science.gov (United States)

    Johnson, B R; Remeikis, N A

    1993-01-01

    Although the tissue solvent and bactericidal properties of sodium hypochlorite are well known, the effective shelf-life of prepared sodium hypochlorite solutions is not known. The stability of sodium hypochlorite is adversely affected by exposure to high temperature, light, air, and the presence of organic and inorganic contaminants. The purpose of this study was to investigate the variables of storage conditions and time on the tissue-dissolving capacity of three different concentrations of sodium hypochlorite. Fresh frozen human umbilical cord was used as the tissue sample for this experiment. Tissue samples were dissolved at time intervals ranging from 1 day to 10 wk in 5.25%, 2.62%, and 1.0% solutions of sodium hypochlorite. The tissue-dissolving ability of 5.25% sodium hypochlorite remains stable for at least 10 wk. The tissue-dissolving ability of 2.62% and 1.0% sodium hypochlorite remains relatively stable for 1 wk after mixing, then exhibits a significant decrease in tissue-dissolving ability at 2 wk and beyond.

  19. Solution-based targeted genomic enrichment for precious DNA samples

    Directory of Open Access Journals (Sweden)

    Shearer Aiden

    2012-05-01

    Full Text Available Abstract Background Solution-based targeted genomic enrichment (TGE protocols permit selective sequencing of genomic regions of interest on a massively parallel scale. These protocols could be improved by: 1 modifying or eliminating time consuming steps; 2 increasing yield to reduce input DNA and excessive PCR cycling; and 3 enhancing reproducible. Results We developed a solution-based TGE method for downstream Illumina sequencing in a non-automated workflow, adding standard Illumina barcode indexes during the post-hybridization amplification to allow for sample pooling prior to sequencing. The method utilizes Agilent SureSelect baits, primers and hybridization reagents for the capture, off-the-shelf reagents for the library preparation steps, and adaptor oligonucleotides for Illumina paired-end sequencing purchased directly from an oligonucleotide manufacturing company. Conclusions This solution-based TGE method for Illumina sequencing is optimized for small- or medium-sized laboratories and addresses the weaknesses of standard protocols by reducing the amount of input DNA required, increasing capture yield, optimizing efficiency, and improving reproducibility.

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

    Science.gov (United States)

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

    1995-01-01

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

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

    Data.gov (United States)

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

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

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 等

    2002-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 方维焕

    2002-01-01

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

  4. Development of an online preparation system for multitracer solutions

    Energy Technology Data Exchange (ETDEWEB)

    Kasamatsu, Yoshitaka [Graduate School of Science, Osaka University, Toyonaka, Osaka 560-0043 (Japan); Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan)], E-mail: kasamatsu.yoshitaka@jaea.go.jp; Yatsukawa, Makoto; Sato, Wataru; Ninomiya, Kazuhiko; Ohki, Toshihiro; Takahashi, Naruto [Graduate School of Science, Osaka University, Toyonaka, Osaka 560-0043 (Japan); Yokoyama, Akihiko [Graduate School of Natural Science and Technology, Kanazawa University, Kanazawa, Ishikawa 920-1192 (Japan); Kikunaga, Hidetoshi [Graduate School of Natural Science and Technology, Kanazawa University, Kanazawa, Ishikawa 920-1192 (Japan); RIKEN, Wako, Saitama 351-0198 (Japan); Kinoshita, Norikazu [Graduate School of Natural Science and Technology, Kanazawa University, Kanazawa, Ishikawa 920-1192 (Japan); Shibata, Sadao [Nuclear Safety Technology Center, Rokkasho, Aomori 039-3212 (Japan); Shinohara, Atsushi [Graduate School of Science, Osaka University, Toyonaka, Osaka 560-0043 (Japan)

    2008-03-15

    We have developed a new target-irradiation system for the online preparation of multitracer solutions, where the nuclear-reaction products recoiling out of the target are directly implanted in a solvent as a liquid catcher. A rapid online transportation of the solution has enabled highly efficient recovery of the multitracer solutions having even short-lived radioactive isotopes without any chemical treatments. It has been suggested that the collection efficiency depends on the chemical properties of the recoil elements.

  5. Snow White Trench Prepared for Sample Collection

    Science.gov (United States)

    2008-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Oliveira Elisabeth de

    2003-01-01

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

  7. γ-ray spectrometry results versus sample preparation methods

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2014-01-02

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

  10. Automated acoustic matrix deposition for MALDI sample preparation.

    Science.gov (United States)

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

    2006-02-01

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

  11. Searching for the Optimal Sampling Solution: Variation in Invertebrate Communities, Sample Condition and DNA Quality.

    Directory of Open Access Journals (Sweden)

    Martin M Gossner

    Full Text Available There is a great demand for standardising biodiversity assessments in order to allow optimal comparison across research groups. For invertebrates, pitfall or flight-interception traps are commonly used, but sampling solution differs widely between studies, which could influence the communities collected and affect sample processing (morphological or genetic. We assessed arthropod communities with flight-interception traps using three commonly used sampling solutions across two forest types and two vertical strata. We first considered the effect of sampling solution and its interaction with forest type, vertical stratum, and position of sampling jar at the trap on sample condition and community composition. We found that samples collected in copper sulphate were more mouldy and fragmented relative to other solutions which might impair morphological identification, but condition depended on forest type, trap type and the position of the jar. Community composition, based on order-level identification, did not differ across sampling solutions and only varied with forest type and vertical stratum. Species richness and species-level community composition, however, differed greatly among sampling solutions. Renner solution was highly attractant for beetles and repellent for true bugs. Secondly, we tested whether sampling solution affects subsequent molecular analyses and found that DNA barcoding success was species-specific. Samples from copper sulphate produced the fewest successful DNA sequences for genetic identification, and since DNA yield or quality was not particularly reduced in these samples additional interactions between the solution and DNA must also be occurring. Our results show that the choice of sampling solution should be an important consideration in biodiversity studies. Due to the potential bias towards or against certain species by Ethanol-containing sampling solution we suggest ethylene glycol as a suitable sampling solution when

  12. Searching for the Optimal Sampling Solution: Variation in Invertebrate Communities, Sample Condition and DNA Quality.

    Science.gov (United States)

    Gossner, Martin M; Struwe, Jan-Frederic; Sturm, Sarah; Max, Simeon; McCutcheon, Michelle; Weisser, Wolfgang W; Zytynska, Sharon E

    2016-01-01

    There is a great demand for standardising biodiversity assessments in order to allow optimal comparison across research groups. For invertebrates, pitfall or flight-interception traps are commonly used, but sampling solution differs widely between studies, which could influence the communities collected and affect sample processing (morphological or genetic). We assessed arthropod communities with flight-interception traps using three commonly used sampling solutions across two forest types and two vertical strata. We first considered the effect of sampling solution and its interaction with forest type, vertical stratum, and position of sampling jar at the trap on sample condition and community composition. We found that samples collected in copper sulphate were more mouldy and fragmented relative to other solutions which might impair morphological identification, but condition depended on forest type, trap type and the position of the jar. Community composition, based on order-level identification, did not differ across sampling solutions and only varied with forest type and vertical stratum. Species richness and species-level community composition, however, differed greatly among sampling solutions. Renner solution was highly attractant for beetles and repellent for true bugs. Secondly, we tested whether sampling solution affects subsequent molecular analyses and found that DNA barcoding success was species-specific. Samples from copper sulphate produced the fewest successful DNA sequences for genetic identification, and since DNA yield or quality was not particularly reduced in these samples additional interactions between the solution and DNA must also be occurring. Our results show that the choice of sampling solution should be an important consideration in biodiversity studies. Due to the potential bias towards or against certain species by Ethanol-containing sampling solution we suggest ethylene glycol as a suitable sampling solution when genetic analysis

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

    African Journals Online (AJOL)

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

  14. 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.

  15. Modern methods of sample preparation for GC analysis

    OpenAIRE

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2016-08-01

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

  17. Preparation and characterization of barium titanate stannate solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Horchidan, Nadejda, E-mail: NHorchidan@stoner.phys.uaic.ro [Department of Physics, ' Al. I. Cuza' University, Bv. Carol 11, Iasi 700506 (Romania); Ianculescu, Adelina C. [Department of Oxide Materials Science and Engineering, Polytechnics University, 1-7 Gh. Polizu, P.O. Box 12-134, 011061 Bucharest (Romania); Curecheriu, Lavinia P.; Tudorache, Florin [Department of Physics, ' Al. I. Cuza' University, Bv. Carol 11, Iasi 700506 (Romania); Musteata, Valentina [Institute of Macromolecular Chemistry ' Petru Poni' , Aleea Grigore Ghica Voda 41A, 700487 Iasi (Romania); Stoleriu, Stefania [Department of Oxide Materials Science and Engineering, Polytechnics University, 1-7 Gh. Polizu, P.O. Box 12-134, 011061 Bucharest (Romania); Dragan, Nicolae; Crisan, Dorel [Institute of Physical Chemistry ' Ilie Murgulescu' , Lab. of Oxide Materials Science, 202 Splaiul Independentei, 060021 Bucharest (Romania); Tascu, Sorin; Mitoseriu, Liliana [Department of Physics, ' Al. I. Cuza' University, Bv. Carol 11, Iasi 700506 (Romania)

    2011-04-07

    Research highlights: > BaSnxTi1-xO3 (x = 0; 0.05; 0.1; 0.15; 0.2) ceramics were prepared by solid state reaction and sintered at 13000C for 4h. > The phase purity, structural parameters and microstructural characteristics were investigated. > The dielectric properties were studied as function of temperature and frequency and empirical parameters {eta} and {delta} were calcutate. > The non-linear dielectric properties (tunability) of the samples were studied at room temperature. > By increasing the Sn addition, the {epsilon}(E) dependence tends to reduce its hysteresis behaviour. - Abstract: BaSn{sub x}Ti{sub 1-x}O{sub 3} (x = 0; 0.05; 0.1; 0.15; 0.2) solid solutions were prepared via conventional solid state reaction and sintered at 1300 {sup o}C for 4 h, resulting in dense single phase ceramics with homogeneous microstructures. Tetragonal symmetry for x {<=} 0.1, cubic for x = 0.2 and a superposition of tetragonal and cubic for x = 0.15 compositions were found by X-ray diffraction analysis. The temperature and frequency dependence of the complex dielectric constant and dc tunability were determined. A transformation from normal ferroelectric to relaxor with diffuse phase transition was observed with increasing the Sn concentration. All the investigated compositions show a relative tunability between 0.55 (for x = 0.2) and 0.74 (for x = 0.1), at a field amplitude of E = 20 kV/cm.

  18. A novel cellulose hydrogel prepared from its ionic liquid solution

    Institute of Scientific and Technical Information of China (English)

    LI Lu; LIN ZhangBi; YANG Xiao; WAN ZhenZhen; CUI ShuXun

    2009-01-01

    A novel cellulose hydrogel is prepared by regenerating cellulose from its ionic liquid solution. The transparency cellulose hydrogel presents a good chemical stability and an acceptable mechanical property. This non-toxic cellulose hydrogel should be biocompatibie and may be useful in the future as a biomaterial.

  19. 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

  20. 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.

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    Andrea Adami

    2016-01-01

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

  3. Fluidics platform and method for sample preparation and analysis

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-08-19

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

  4. Metal Nanoparticles Preparation In Supercritical Carbon Dioxide Solutions

    Energy Technology Data Exchange (ETDEWEB)

    Harry W. Rollins

    2004-04-01

    The novel optical, electronic, and/or magnetic properties of metal and semiconductor nanoparticles have resulted in extensive research on new methods for their preparation. An ideal preparation method would allow the particle size, size distribution, crystallinity, and particle shape to be easily controlled, and would be applicable to a wide variety of material systems. Numerous preparation methods have been reported, each with its inherent advantages and disadvantages; however, an ideal method has yet to emerge. The most widely applied methods for nanoparticle preparation include the sonochemical reduction of organometallic reagents,(1&2) the solvothermal method of Alivisatos,(3) reactions in microemulsions,(4-6) the polyol method (reduction by alcohols),(7-9) and the use of polymer and solgel materials as hosts.(10-13) In addition to these methods, there are a variety of methods that take advantage of the unique properties of a supercritical fluid.(14&15) Through simple variations of temperature and pressure, the properties of a supercritical fluid can be continuously tuned from gas-like to liquid-like without undergoing a phase change. Nanoparticle preparation methods that utilize supercritical fluids are briefly reviewed below using the following categories: Rapid Expansion of Supercritical Solutions (RESS), Reactive Supercritical Fluid Processing, and Supercritical Fluid Microemulsions. Because of its easily accessible critical temperature and pressure and environmentally benign nature, carbon dioxide is the most widely used supercritical solvent. Supercritical CO2 is unfortunately a poor solvent for many polar or ionic species, which has impeded its use in the preparation of metal and semiconductor nanoparticles. We have developed a reactive supercritical fluid processing method using supercritical carbon dioxide for the preparation of metal and metal sulfide particles and used it to prepare narrowly distributed nanoparticles of silver (Ag) and silver sulfide

  5. Exploring challenges and solutions in the preparation of surgical patients

    DEFF Research Database (Denmark)

    Møller, Thea Palsgaard; Münter, Kristine Husum; Østergaard, Doris;

    2015-01-01

    guidelines and to identify challenges and solutions for correct preparation through interactive table simulation-based workshops involving the various professions and specialties. METHODS: Firstly, specific tasks in the hospital guidelines were monitored for all surgical procedures during one week. Secondly...... management system tasks, 26% of anaesthesia record tasks, 24% of medication tasks, 14% of blood test tasks and 12% of patient record tasks. In two workshops held for each of four specialties, a total of 21 participants mapped the preoperative patient journey with related responsibilities, tasks and written...... documentation. Furthermore, challenges and suggestions for solutions were identified. CONCLUSIONS: Completion of mandatory tasks for surgical patient preparation was poor. Workshops with table simulations actively involved the stakeholders from various professions and specialties in describing the patient...

  6. Stability of urea in solution and pharmaceutical preparations.

    Science.gov (United States)

    Panyachariwat, Nattakan; Steckel, Hartwig

    2014-01-01

    The stability of urea in solution and pharmaceutical preparations was analyzed as a function of temperature (25°-60°C), pH (3.11-9.67), and initial urea concentration (2.5%-20%). This study was undertaken to (i) obtain more extensive, quantitative information relative to the degradation of urea in both aqueous and non-aqueous solutions and in pharmaceutical preparations, and (ii) test the effects of initial urea concentration, pH, buffer, and temperature values on urea degradation. The stability analysis shows that urea is more stable at the pH range of 4-8 and the stability of urea decreases by increase in temperature for all pH values. Within the experimental range of temperature and initial urea concentration values, the lowest urea degradation was found with lactate buffer pH 6.0. The urea decomposition rate in solution and pharmaceutical preparations shows the dependence of the initial urea concentrations. At higher initial urea concentrations, the rate of degradation is a decreasing function with time. This suggests that the reverse reaction is a factor in the degradation of concentrated urea solution. For non-aqueous solvents, isopropanol showed the best effort in retarding the decomposition of urea. Since the losses in urea is directly influenced by its stability at a given temperature and pH, the stability analysis of urea by the proposed model can be used to prevent the loss and optimize the operating condition for urea-containing pharmaceutical preparations.

  7. Exploring challenges and solutions in the preparation of surgical patients

    DEFF Research Database (Denmark)

    Møller, Thea Palsgaard; Münter, Kristine Husum; Østergaard, Doris;

    2015-01-01

    INTRODUCTION: Handover of surgical patients from ward to operating room is a sensible point for information and communication failures. Guidelines were developed for preparation of surgical patients. Our aim was to explore if patients are sufficiently prepared for surgery according to local......, workshops including table simulations involving the various professions and specialties were held. RESULTS: In total, 314 surgical procedures were performed of which 196 were eligible for analysis. Emergency procedures showed the poorest results with non-completed tasks comprising 58% of electronic patient...... documentation. Furthermore, challenges and suggestions for solutions were identified. CONCLUSIONS: Completion of mandatory tasks for surgical patient preparation was poor. Workshops with table simulations actively involved the stakeholders from various professions and specialties in describing the patient...

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

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

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

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

    Science.gov (United States)

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

    2002-12-15

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

  10. PREPARATION OF MULTIFUNCTIONAL ORGANOLITHIUM INITIATOR IN CYCLOHEXANE SOLUTIONS

    Institute of Scientific and Technical Information of China (English)

    Ming Yao; Hai-yan Zhang; Xing-ying Zhang; Shu-he Zhao

    2011-01-01

    Multifunctional organolithium initiator was prepared in cyclohexane solvent. The process started with adding the cyclohexane solution of butadiene to naphthalene-lithium in batches to produce butadiene oligomer dilithium with 4-8 butadiene repeating units. In the first feeding, the maximum loading of cyclohexane and the minimum concentration of butadiene cyclohexane solution must be controlled under Vcyclohexane ≤ 1.33 VTHnF and p ≥ 40.6cN. Then, SnC14 was added and eventually the multifunctional organolithium initiator containing Sn atom was synthesized through coupling reaction.Experiment results showed that adding the cyclohexane solution in batches was effective in overcoming some difficulties,such as insolubility of naphthalene-lithium in cyclohexane, low efficiency of naphthalene-lithium in initiating butadiene. In practice, benzene can be replaced by cyclohexane completely, which can not only reduce environmental pollution from benzene, but also overcome the difficulty of solvent recovery caused by similar boiling point between benzene and cyclohexane. Prepared with multifunctional organolithium containing Sn atom as initiator, the star-shaped solution polymerized styrene-butadiene rubber (star S-SBR) with better vulcanization performances, lower rolling resistance and higher wet-skid resistance was obtained.

  11. Analysis of fluoride concentration in solutions prepared at dispensing pharmacies

    Directory of Open Access Journals (Sweden)

    Eduardo Pizzatto

    2011-07-01

    Full Text Available Introduction: Fluoride plays an important role in oral health promotion and is considered important in dental caries prevention both in children and adults. Fluoride is widely used at high-risk conditions of caries, when the use of fluoride-containing mouthwashes is recommended, considering that fluoride itself reduces the risk of dental caries. Objective: To evaluate the fluoride concentration in solutions prepared at different dispensing pharmacies in the city of Curitiba – PR, Brazil. Material and methods: The analysis of fluoride concentration was preformed through Ion Chromatography method (DIONEX. Results: The results obtained through this analysis showed that all solutions presented fluoride concentration above that required in the dentist’s prescription, varying between 5.48% and 24.02% more fluoride, at absolute concentration. Conclusion: This finding highlights the increasing risk of fluoride acute intoxication in cases of accidental ingestion of the solution.

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

    Science.gov (United States)

    Lance A. Asherin; Stephen A. Mata

    2001-01-01

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

  13. Preparation of patients submitted to thyroidectomy with oral glucose solutions.

    Science.gov (United States)

    Libiszewski, Michał; Drozda, Rafał; Smigielski, Janusz; Kuzdak, Krzysztof; Kołomecki, Krzysztof

    2012-05-01

    The AIM OF THE STUDY was to determine postoperative insulin-resistance in patients subject to total thyroidectomy, the prevalence of subjective feelings of hunger immediately before surgery, and the incidence of nausea/vomiting after surgery in patients prepared for elective operations by means of oral glucose solutions. The study group comprised 115 patients, including 71 patients prepared for surgery by means of oral glucose solutions (12.5% glucose) administered 12 and 3 hours before the procedure, at a dose of 800 and 400 ml. The control group comprised 44 patients prepared for surgery by means of the traditional manner- the last meal was served before 2pm the day before the surgical procedure, while fluids before 10pm. Considering both groups, we evaluated glucose and insulin levels three times, as well as determined the insulin-resistance ratio (HOMA-IR) 24 before, and 12 hours and 7 days after surgery. The incidence of nausea and vomiting after surgery, and the subjective feeling of hunger before surgery were also evaluated. Statistically significant differences considering insulin level and HOMA-IR values were observed during the II and III measurements. The glucose and insulin values, and the HOMA-IR insulin-resistance ratio, showed no statistically significant differences during measurement I. No statistically significant glucose level differences were observed during measurements II and III. A significantly greater subjective feeling of hunger before surgery and nausea/vomiting afterwards were observed in the control group. The preparation of patients with oral glucose solutions decreases the incidence of postoperative (thyroidectomy) insulin-resistance, and occurrence of nausea/vomiting during the postoperative period.

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

    Science.gov (United States)

    Siegel, David

    2012-12-07

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

  15. 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.

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

    Science.gov (United States)

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

    2014-04-01

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

  17. An ignored variable: solution preparation temperature in protein crystallization.

    Science.gov (United States)

    Chen, Rui-Qing; Lu, Qin-Qin; Cheng, Qing-Di; Ao, Liang-Bo; Zhang, Chen-Yan; Hou, Hai; Liu, Yong-Ming; Li, Da-Wei; Yin, Da-Chuan

    2015-01-19

    Protein crystallization is affected by many parameters, among which certain parameters have not been well controlled. The temperature at which the protein and precipitant solutions are mixed (i.e., the ambient temperature during mixing) is such a parameter that is typically not well controlled and is often ignored. In this paper, we show that this temperature can influence protein crystallization. The experimental results showed that both higher and lower mixing temperatures can enhance the success of crystallization, which follows a parabolic curve with an increasing ambient temperature. This work illustrates that the crystallization solution preparation temperature is also an important parameter for protein crystallization. Uncontrolled or poorly controlled room temperature may yield poor reproducibility in protein crystallization.

  18. Perovskite/polymer solar cells prepared using solution process

    Science.gov (United States)

    Rosa, E. S.; Shobih; Nursam, N. M.; Saputri, D. G.

    2016-11-01

    We report a simple solution-based process to fabricate a perovskite/polymer tandem solar cell using inorganic CH3NH3PM3 as an absorber and organic PCBM (6,6 phenyl C61- butyric acid methyl ester) as an electron transport layer. The absorber solution was prepared by mixing the CH3NH3I (methyl ammonium iodide) with PbI2 (lead iodide) in DMF (N,N- dimethyl formamide) solvent. The absorber and electron transport layer were deposited by spin coating method. The electrical characteristics generated from the cell under 50 mW/cm2 at 25 °C comprised of an open circuit voltage of 0.31 V, a short circuit current density of 2.53 mA/cm2, and a power conversion efficiency of 0.42%.

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

    DEFF Research Database (Denmark)

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

    2005-01-01

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

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

    Science.gov (United States)

    Tolle, Fabian; Mayer, Günter

    2016-01-01

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

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

    Science.gov (United States)

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

    2011-01-01

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

  2. Characterization of Laboratory Prepared Concrete Pastes Exposed to High Alkaline and High Sodium Salt Solutions

    Energy Technology Data Exchange (ETDEWEB)

    Langton, C. A. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-06-30

    The objective of this study was to identify potential chemical degradation mechanisms for the Saltstone Disposal Unit (SDU) concretes, which over the performance life of the structures may be exposed to highly alkaline sodium salt solutions containing sulfate, hydroxide, and other potentially corrosive chemicals in salt solution and saltstone flush water, drain water, leachate and / or pore solution. The samples analyzed in this study were cement pastes prepared in the SIMCO Technologies, Inc. concrete laboratory. They were based on the paste fractions of the concretes used to construct the Saltstone Disposal Units (SDUs). SDU 1 and 4 concrete pastes were represented by the PV1 test specimens. The paste in the SDU 2, 3, 5, and 6 concrete was represented by the PV2 test specimens. SIMCO Technologies, Inc. selected the chemicals and proportions in the aggressive solutions to approximate proportions in the saltstone pore solution [2, 3, 5, and 6]. These test specimens were cured for 56 days in curing chamber before being immersed in aggressive solutions. After exposure, the samples were frozen to prevent additional chemical transport and reaction. Selected archived (retrieved from the freezer) samples were sent to the Savannah River National Laboratory (SRNL) for additional characterization using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive x-ray (EDX) spectroscopy. Characterization results are summarized in this report. In addition, a correlation between the oxide composition of the pastes and their chemical durability in the alkaline salt solutions is provided.

  3. Optimization for Peptide Sample Preparation for Urine Peptidomics

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-02-25

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

  5. Amorphous semiconductor sample preparation for transmission EXAFS measurements

    Energy Technology Data Exchange (ETDEWEB)

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

    1998-12-31

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

  6. Picoliter solution deposition for total reflection X-ray fluorescence analysis of semiconductor samples

    Energy Technology Data Exchange (ETDEWEB)

    Sparks, Chris M., E-mail: chris.sparks@svtc.co [Analytical Services, SVTC Technologies, Austin, TX 78741 (United States); Fittschen, Ursula E.A. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Institute of Inorganic and Applied Chemistry, University of Hamburg, 20146 Hamburg (Germany); Havrilla, George J. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2010-09-15

    A deposition system capable of delivering picoliter quantities of solution in programmable arrays was investigated as a method for sample preparation for total reflection X-ray fluorescence (TXRF) spectroscopy. Arrays of trace metals in solution were deposited on Si wafers. The array deposits provide a capability of depositing closely spaced (100 {mu}m or less), typically 5-20 {mu}m diameter droplets in an area that can be matched to the analysis spot of the TXRF detector. The dried depositions were physically characterized and the effect of deposition type and matrix on the TXRF signal was investigated.

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

    Institute of Scientific and Technical Information of China (English)

    肖化云; 刘丛强

    2001-01-01

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

  8. Preparation of polystyrene–clay nanocomposite by solution intercalation technique

    Indian Academy of Sciences (India)

    P K Paul; S A Hussain; D Bhattacharjee; M Pal

    2013-06-01

    Polymer–clay nanocomposites of commercial polystyrene (PS) and clay laponite were prepared via solution intercalation technique. Laponite was modified suitably with the well known cationic surfactant cetyltrimethyl ammonium bromide by ion-exchange reaction to render laponite miscible with hydrophobic PS. X-ray diffraction analysis in combination with scanning electron microscopy gives an idea of structural and morphological information of PS–laponite nanocomposite for different varying organo-laponite contents. Intercalation of PS chain occurs into the interlayer spacings of laponite for low organo-laponite concentration in the PS–O-laponite mixture. However, aggregation and agglomeration occur at higher clay concentration. The molecular bond vibrational profile of laponite as well as PS–laponite nanocomposite have been explored by Fourier transform infrared spectroscopy. Thermogravimetric analysis along with differential scanning calorimetry results reveal the enhancement of both thermal stability and glass transition temperature of PS due to the incorporation of clay platelets.

  9. Effect of Nb on barium titanate prepared from citrate solutions

    Directory of Open Access Journals (Sweden)

    Stojanović Biljana D.

    2002-01-01

    Full Text Available The influence of the addition of dopants on the microstructure development and electrical properties of BaTiO3 doped with 0.2, 0.4, 0.6, 0.8 mol% of Nb and 0.01 mol% of Mn based compounds was studied. Doped barium titanate was prepared using the polymeric precursor method from citrate solutions. The powders calcined at 700°C for 4 hours were analysed by infrared (IR spectroscopy to verify the presence of carbonates, and by X-ray diffraction (XRD for phase formation. The phase composition, microstructure and dielectric properties show a strong dependence on the amount of added niobium.

  10. Characterization of PAN/ATO nanocomposites prepared by solution blending

    Indian Academy of Sciences (India)

    Wei Pan; Hantao Zou

    2008-10-01

    Conducting nanocomposites of polyacrylonitrile (PAN) and antimony-doped tin oxide (ATO) were prepared by solution blending. Electrical properties of the nanocomposites were characterized by means of electrical conductivity measurements and the phase structures were investigated via scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analyses (TGA) and dynamical mechanical analysis (DMA). This study unveiled a remarkable, interpenetrating network of chainlike nano-ATO within the PAN matrix, consistent with the existence of connected conducting paths at content as low as 4 wt% of the nano-ATO. The storage modulus of the nanocomposites increased with increasing content of ATO, due to formation of immobilized layer between polymer and filler. The interactions between ATO and PAN molecules resulted in high tan for the PAN/ATO nanocomposites. Thermal stability of the nanocomposites was found remarkably enhanced by the incorporation of nano-ATO.

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

    Lifescience Database Archive (English)

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-08-12

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

  13. SCM Paste Samples Exposed To Aggressive Solutions. Cementitious Barriers Partnership

    Energy Technology Data Exchange (ETDEWEB)

    Foster, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2014-12-01

    This report summarizes experimental work performed by SIMCO Technologies Inc. (SIMCO) as part of the Cementitious Barriers Partnership (CBP) project. The test series followed an experimental program dedicated to the study of ordinary Portland cement (OPC) hydrated cement pastes exposed to aggressive solutions. In the present study, the scope is extended to hydrated cement pastes incorporating supplementary cementitious materials (SCM) such as fly ash and ground granulated blast furnace slag (GGBFS). Also, the range of aggressive contact solutions was expanded. The experimental program aimed at testing aggressive contact solutions that more closely mimic the chemical composition of saltstone pore solution. Five different solutions, some of which incorporated high levels of carbonate and nitrate, were placed in contact with four different hydrated cement paste mixes. In all solutions, 150 mmol/L of SO42– (14 400 ppm) were present. The solutions included different pH conditions and different sodium content. Two paste mixes were equivalent to Vault 1/4 and Vault 2 concrete mixes used at SRS in storage structures. Two additional paste mixes, cast at the same water-to-cement ratio and using the same cements but without SCMs, were also tested. The damage evolution in samples was monitored using ultrasonic pulse velocity (UPV) and mass measurements. After three and twelve months of exposure conditions, samples were taken out of solution containers and analyzed to perform migration tests and porosity measurements. Globally, results were in line with the previous study and confirmed that high pH may limit the formation of some deleterious phases like gypsum. In this case, ettringite may form but is not necessarily associated with damage. However, the high concentration of sodium may be associated with the formation of an AFm-like mineral called U-phase. The most significant evidences of damage were all associated with the Vault 2 paste analog. This

  14. SCM Paste Samples Exposed To Aggressive Solutions. Cementitious Barriers Partnership

    Energy Technology Data Exchange (ETDEWEB)

    Foster, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2014-12-01

    This report summarizes experimental work performed by SIMCO Technologies Inc. (SIMCO) as part of the Cementitious Barriers Partnership (CBP) project. The test series followed an experimental program dedicated to the study of ordinary Portland cement (OPC) hydrated cement pastes exposed to aggressive solutions. In the present study, the scope is extended to hydrated cement pastes incorporating supplementary cementitious materials (SCM) such as fly ash and ground granulated blast furnace slag (GGBFS). Also, the range of aggressive contact solutions was expanded. The experimental program aimed at testing aggressive contact solutions that more closely mimic the chemical composition of saltstone pore solution. Five different solutions, some of which incorporated high levels of carbonate and nitrate, were placed in contact with four different hydrated cement paste mixes. In all solutions, 150 mmol/L of SO42– (14 400 ppm) were present. The solutions included different pH conditions and different sodium content. Two paste mixes were equivalent to Vault 1/4 and Vault 2 concrete mixes uses at SRS in storage structures. Two additional paste mixes, cast at the same water-to-cement ratio and using the same cements but without SCMs, were also tested. The damage evolution in samples was monitored using ultrasonic pulse velocity (UPV) and mass measurements. After three and twelve months of exposure conditions, samples were taken out of solution containers and analyzed to perform migration tests and porosity measurements. Globally, results were in line with the previous study and confirmed that high pH may limit the formation of some deleterious phases like gypsum. In this case, ettringite may form but is not necessarily associated with damage. However, the high concentration of sodium may be associated with the formation of an AFm-like mineral called U-phase. The most significant evidences of damage were all associated with the Vault 2 paste analog. This

  15. Sample preparation of metal alloys by electric discharge machining

    Science.gov (United States)

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

    1976-01-01

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

  16. Analytical quality-by-design approach for sample treatment of BSA-containing solutions

    Institute of Scientific and Technical Information of China (English)

    Lien Taevernier; Evelien Wynendaele; Matthias D’Hondt; Bart De Spiegeleer

    2015-01-01

    The sample preparation of samples containing bovine serum albumin (BSA), e.g., as used in transdermal Franz diffusion cell (FDC) solutions, was evaluated using an analytical quality-by-design (QbD) approach. Traditional precipitation of BSA by adding an equal volume of organic solvent, often successfully used with conventional HPLC-PDA, was found insufficiently robust when novel fused-core HPLC and/or UPLC-MS methods were used. In this study, three factors (acetonitrile (%), formic acid (%) and boiling time (min)) were included in the experimental design to determine an optimal and more suitable sample treatment of BSA-containing FDC solutions. Using a QbD and Derringer desirability (D) approach, combining BSA loss, dilution factor and variability, we constructed an optimal working space with the edge of failure defined as Do0.9. The design space is modelled and is confirmed to have an ACN range of 8373%and FA content of 170.25%.

  17. Preparation of fluorescent polyaniline nanoparticles in aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Alves, Kleber G. B. [Universidade Federal de Pernambuco, Departamento de Engenharia Mecanica (Brazil); Melo, Etelino F. de [Universidade Federal de Pernambuco, Departamento de Quimica Fundamental (Brazil); Andrade, Cesar A. S. [Universidade Federal de Pernambuco, Departamento de Bioquimica (Brazil); Melo, Celso P. de, E-mail: celso@df.ufpe.br [Universidade Federal de Pernambuco, Departamento de Fisica (Brazil)

    2013-01-15

    We report the synthesis of stable polyaniline nanoparticles (PANI{sub N}Ps) based on the chemical oxidative polymerization of aniline in aqueous solutions of surfactants. Surfactants of three different types-cationic (dodecyltrimethylammonium bromide-DTAB), anionic (sodium dodecyl sulfate-SDS), and non-ionic (Triton X-405-TX-405)-were used. The resulting PANI{sub N}Ps{sub s}urfactant samples were characterized through UV-Vis, fluorescence and Fourier transform infrared spectroscopies, and scanning electronic microscopy (SEM). We have verified that the color of the PANI{sub N}Ps{sub s}urfactant dispersions is affected by a change in the pH of the solution. The PANI-NPs{sub s}urfactant colloidal suspensions in aqueous solution present a surprising high fluorescence quantum yield value (ranging from 1.9 Multiplication-Sign 10{sup -3} to 6.9 Multiplication-Sign 10{sup -3}) that can be controlled as a function of the pH, a fact that we associate to the corresponding protonation degree of the PANI polymeric chains. We suggest that these fluorescent nanocomposites can find important technological applications in different areas such as organic light emitting devices, biosensors, and pigments for coatings.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-12-15

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

  19. Adsorption of CTAB onto perlite samples from aqueous solutions.

    Science.gov (United States)

    Alkan, Mahir; Karadaş, Mecit; Doğan, Mehmet; Demirbaş, Ozkan

    2005-11-15

    In this study, the adsorption properties of unexpanded and expanded perlite samples in aqueous cetyltrimethylammonium bromide (CTAB) solutions were investigated as a function of ionic strength, pH, and temperature. It was found that the amount of cetyltrimethylammonium bromide adsorbed onto unexpanded perlite was greater than that onto expanded perlite. For both perlite samples, the sorption capacity increased with increasing ionic strength and pH and decreasing temperature. Experimental data were analyzed by Langmuir and Freundlich isotherms and it was found that the experimental data were correlated reasonably well by the Freundlich adsorption isotherm. Furthermore, the isotherm parameters (KF and n) were also calculated. The adsorption enthalpy was determined from experimental data at different temperatures. Results have shown that the interaction between the perlite surface and CTAB is a physical interaction, and the adsorption process is an exothermic one.

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

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Löschner, Katrin

    2014-01-01

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

  1. Lyophilization monophase solution technique for preparation of amorphous flutamide dispersions.

    Science.gov (United States)

    Elgindy, Nazik; Elkhodairy, Kadria; Molokhia, Abdallah; Elzoghby, Ahmed

    2011-07-01

    Flutamide (FLT) is a poorly soluble anticancer drug. Therefore, lyophilized dispersions (LDs) of FLT with polyvinylpyrrolidone (PVP) K30, polyethylene glycol (PEG) 6000, and pluronic F127 were prepared via lyophilization monophase solution technique with the aim of increasing its dissolution rate. FLT showed an A(L)-type phase solubility diagrams with PVP and PEG, whereas A(N)-type diagram was obtained with pluronic. The amount of residual tertiary butyl alcohol, determined by gas chromatography, was 0.015-0.021% w/w. Differential scanning calorimetry and X-ray diffractometry revealed that FLT-polymer 1:1 LDs were partially amorphous, whereas the 1:3 and 1:5 LDs were completely amorphous. After 6 months storage, polymers under study inhibited FLT recrystallization maintaining its amorphous form. The particle size of FLT-polymer LDs was between 0.81 and 2.13 μm, with a high surface area (268.43-510.82 m²/g) and porosity (354.01-676.23 e⁻³ mL/g). Also, the poor flow properties of FLT could be improved but to a limited extent. FLT dissolution was significantly enhanced with the fastest dissolution that was achieved using pluronic. After 30 min, about 66.52%, 78.23%, and 81.64% of FLT was dissolved from 1:5 FLT-PVP, PEG, and pluronic LDs, respectively, compared with only 13.45% of FLT. These data suggest that these polymers might be useful adjuncts in preparation and stabilization of amorphous immediate-release FLT LDs.

  2. 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...

  3. Preparation of nanoparticles of Magnolia bark extract by rapid expansion from supercritical solution into aqueous solutions.

    Science.gov (United States)

    He, Shuai; Zhou, Benjie; Zhang, Shouyao; Lei, Zhengjie; Zhang, Zhongyi

    2011-01-01

    A rapid expansion from supercritical solution into aqueous solution (RESSAS) technology was presented for the micronization of Chinese medicinal material. Magnolia bark extract (MBE) obtained by supercritical carbon dioxide (scCO₂) extraction technology was chosen as the experimental material. RESSAS process produced 303.0 nm nanoparticles (size distribution, 243.6-320.5 nm), which was significantly smaller than the 55.3 µm particles (size distribution, 8.3-102.4 µm) prepared by conventional mechanical milling. The effect of process parameters, including extraction temperature (30 °C, 40 °C, 50 °C), extraction pressure (200, 250, 300 bar) and nozzle size (50, 100, 200 µm), on the size distribution of nanoparticles was investigated. The characteristics of nanoparticles and materials were also studied by scanning electron microscopy (SEM) and laser light scattering (LLS). This study demonstrates that RESSAS is applicable for preparing nanoparticles of MBE at low operating temperature; the process is simple without any residual solvent.

  4. Effects of cardioplegia induced by a Young's solution (YNG solution) on the blood-perfused canine papillary muscle preparation.

    Science.gov (United States)

    Satoh, H; Ohkubo, K; Suzuki, K; Katano, Y; Otorii, T; Kawada, T; Yoshida, S; Imai, S

    1984-03-01

    Experiments were carried out in the blood-perfused canine papillary muscle preparation to evaluate the protective effect of a cardioplegic solution, Young's solution (YNG solution), on the myocardial function. Both in spontaneously contracting preparations and in electrically paced (2 Hz) preparations, the time to the cardiac arrest and the time to the maximum blood flow were found to be significantly shorter when the cardiac arrest was induced with cardioplegic solutions than when it was induced with the cold modified Krebs-Ringer's solution (cold cardioplegia). The maximum blood flow of the paced preparation tended to be greater with cardioplegic solutions. The time to resumption of regular contractions was significantly shorter with YNG solution as compared with cold cardioplegia. The developed tension and the blood flow at the time of resumption of the regular contractions tended to approach the control value more quickly with YNG solution, as compared with other cardioplegic solutions and cold cardioplegia. It is concluded that YNG solution represents an optimal cardioplegic solution.

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

    Science.gov (United States)

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

    2015-03-21

    Desalination as a sample preparation step is essential for noise reduction and reproducibility of mass spectrometry measurements. A specific example is the analysis of proteins for medical research and clinical applications. Salts and buffers that are present in samples need to be removed before analysis to improve the signal-to-noise ratio. Capacitive deionization is an electrostatic desalination (CDI) technique which uses two porous electrodes facing each other to remove ions from a solution. Upon the application of a potential of 0.5 V ions migrate to the electrodes and are stored in the electrical double layer. In this article we demonstrate CDI on a chip, and desalinate a solution by the removal of 23% of Na(+) and Cl(-) ions, while the concentration of a larger molecule (FITC-dextran) remains unchanged. For the first time impedance spectroscopy is introduced to monitor the salt concentration in situ in real-time in between the two desalination electrodes.

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

    Science.gov (United States)

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

    2013-03-01

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

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

    Science.gov (United States)

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

    2004-07-16

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

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

    Science.gov (United States)

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

    2012-09-01

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

  9. Preparing for Remarriage: Anticipating the Issues, Seeking Solutions.

    Science.gov (United States)

    Ganong, Lawrence H.; Coleman, Marilyn

    1989-01-01

    Examined the ways remarried adults with children prepared for remarriage. Asked 100 men and 105 women about their methods of preparing, pre-remarriage concerns, and issues discussed prior to marriage. Primary way subjects prepared for remarriage was by cohabitation. Living together appeared to be more effective for men than for women. (Author/NB)

  10. Preparing for Remarriage: Anticipating the Issues, Seeking Solutions.

    Science.gov (United States)

    Ganong, Lawrence H.; Coleman, Marilyn

    1989-01-01

    Examined the ways remarried adults with children prepared for remarriage. Asked 100 men and 105 women about their methods of preparing, pre-remarriage concerns, and issues discussed prior to marriage. Primary way subjects prepared for remarriage was by cohabitation. Living together appeared to be more effective for men than for women. (Author/NB)

  11. Mask process matching using a model based data preparation solution

    Science.gov (United States)

    Dillon, Brian; Saib, Mohamed; Figueiro, Thiago; Petroni, Paolo; Progler, Chris; Schiavone, Patrick

    2015-10-01

    Process matching is the ability to precisely reproduce the signature of a given fabrication process while using a different one. A process signature is typically described as systematic CD variation driven by feature geometry as a function of feature size, local density or distance to neighboring structures. The interest of performing process matching is usually to address differences in the mask fabrication process without altering the signature of the mask, which is already validated by OPC models and already used in production. The need for such process matching typically arises from the expansion of the production capacity within the same or different mask fabrication facilities, from the introduction of new, perhaps more advanced, equipment to deliver same process of record masks and/or from the re-alignment of processes which have altered over time. For state-of-the-art logic and memory mask processes, such matching requirements can be well below 2nm and are expected to reduce below 1nm in near future. In this paper, a data preparation solution for process matching is presented and discussed. Instead of adapting the physical process itself, a calibrated model is used to modify the data to be exposed by the source process in order to induce the results to match the one obtained while running the target process. This strategy consists in using the differences among measurements from the source and target processes, in the calibration of a single differential model. In this approach, no information other than the metrology results is required from either process. Experimental results were obtained by matching two different processes at Photronics. The standard deviation between both processes was of 2.4nm. After applying the process matching technique, the average absolute difference between the processes was reduced to 1.0nm with a standard deviation of 1.3nm. The methods used to achieve the result will be described along with implementation considerations, to

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

    OpenAIRE

    Itagaki, K.; Lemieux, G.

    1987-01-01

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

  13. Continuous Passive Sampling of Solutes from Agricultural Subsurface Drainage Tubes

    Science.gov (United States)

    Lindblad Vendelboe, Anders; de Jonge, Hubert; Rozemeijer, Joachim; Wollesen de Jonge, Lis

    2015-04-01

    Agricultural subsurface tube drain systems play an important role in water and solute transport. One study, focusing on lowland agricultural catchments, showed that subsurface tube drainage contributed up to 80% of the annual discharge and 90% of the annual NO3 load from agricultural fields to the receiving water bodies. Knowledge of e.g. nutrient loads and drainage volumes, based on measurements and modelling, are important for adequate water quality management. Despite the importance of tube drain transport of solutes, monitoring data are scarce. This scarcity is a result of the existing monitoring techniques for flow and contaminant load from tube drains being expensive and labor-extensive. The study presented here aimed at developing a cheap, simple, and robust method to monitor solute loads from tube drains. The method is based on the newly developed Flowcap, which can be attached to existing tube drain outlets and can measure total flow, contaminant load and flow-averaged concentrations of solutes in the drainage. The Flowcap builds on the existing Sorbicell principle, a passive sampling system that measures average concentrations over longer periods of time (days to months) for various compounds. The Sorbicell consists of two compartments permeable to water. One compartment contains an adsorbent and one contains a tracer. When water passes through the Sorbicell the compound of interest is absorbed while a tracer is released. Using the tracer loss to calculate the volume of water that has passed the Sorbicell it is possible to calculate the average concentration of the compound. When mounting Sorbicells in the Flowcap, a flow-proportional part of the drainage is sampled from the main stream. To accommodate the wide range of drainage flow rates two Flowcaps with different capacities were tested in the laboratory: one with a capacity of 25 L min-1 (Q25) and one with a capacity of 256 L min-1 (Q256). In addition, Sorbicells with two different hydraulic

  14. A new method for preparation of magnetite from iron oxyhydroxide or iron oxide and ferrous salt in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Kahani, S.A. [Department of Chemistry, Faculty of Science, University of Kashan, Kashan 87317-51167 (Iran, Islamic Republic of)], E-mail: Kahani@kashanu.ac.ir; Jafari, M. [Department of Chemistry, Faculty of Science, University of Kashan, Kashan 87317-51167 (Iran, Islamic Republic of)

    2009-07-15

    In this study, a new method is proposed for the preparation of Fe{sub 3}O{sub 4} from iron oxyhydroxides (goethite, akaganeite, lepidocrocite, feroxyhyte and ferrihydrite) or iron oxide (hematite) and ferrous salt in aqueous solution. The product is magnetite with various particle sizes. Products are characterized by X-ray powder diffraction, IR spectra and vibrating sample magnetometery.

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

    Science.gov (United States)

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

    2009-07-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

  17. Levels of carnitine and acylcarnitines in reconstituted red blood cell samples washed with different concentrations of saline solutions

    OpenAIRE

    José Henry Osorio; Morteza Pourfarzam

    2011-01-01

    Objective: To evaluate the percentage of carnitine and acylcarnitines remaining in red blood cells after washing them with different concentrations of saline solution. Materials and methods: Human blood samples were centrifuged and the blood cells were washed with different saline solutions. The final pellet was resuspended in PBS for card preparation and tandem mass spectrometry analysis. Results: It was found that carnitine, as well as short-chain, medium-chain, and long-chain acylca...

  18. Novel sample preparation method for surfactant containing suppositories: effect of micelle formation on drug recovery.

    Science.gov (United States)

    Kalmár, Éva; Ueno, Konomi; Forgó, Péter; Szakonyi, Gerda; Dombi, György

    2013-09-01

    Rectal drug delivery is currently at the focus of attention. Surfactants promote drug release from the suppository bases and enhance the formulation properties. The aim of our work was to develop a sample preparation method for HPLC analysis for a suppository base containing 95% hard fat, 2.5% Tween 20 and 2.5% Tween 60. A conventional sample preparation method did not provide successful results as the recovery of the drug failed to fulfil the validation criterion 95-105%. This was caused by the non-ionic surfactants in the suppository base incorporating some of the drug, preventing its release. As guidance for the formulation from an analytical aspect, we suggest a well defined surfactant content based on the turbidimetric determination of the CMC (critical micelle formation concentration) in the applied methanol-water solvent. Our CMC data correlate well with the results of previous studies. As regards the sample preparation procedure, a study was performed of the effects of ionic strength and pH on the drug recovery with the avoidance of degradation of the drug during the procedure. Aminophenazone and paracetamol were used as model drugs. The optimum conditions for drug release from the molten suppository base were found to be 100 mM NaCl, 20-40 mM NaOH and a 30 min ultrasonic treatment of the final sample solution. As these conditions could cause the degradation of the drugs in the solution, this was followed by NMR spectroscopy, and the results indicated that degradation did not take place. The determined CMCs were 0.08 mM for Tween 20, 0.06 mM for Tween 60 and 0.04 mM for a combined Tween 20, Tween 60 system. Copyright © 2013 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-07-03

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

  20. Red-emitting alkaline-earth rare-earth pentaoxometallates powders prepared by metal carboxylates solution

    Indian Academy of Sciences (India)

    Kyu-Seog Hwang; Sung-Dae Kim; Seung Hwangbo; Jin-Tae Kim

    2013-06-01

    Moisture-insensitive metal carboxylates that are mostly liquids at room temperature have been first applied to the preparation of strontium europium aluminate (Sr2EuAlO5) powders for red-emitting phosphor under near ultraviolet radiation. Strontium naphthenate, aluminium-2-ethylhexanoate and europium-2-ethylhexanoate were dissolved with toluene to prepare starting solution. Precursor pyrolyzed at 500 °C for 240 min was finally annealed at 900–1200 °C for 240 min in Ar. X-ray diffraction analysis, field emission–scanning electron microscope and fluorescent spectrophotometer were used to evaluate structural and optical properties. For the 1000 °C-annealed powders with regular shape and narrow size distribution confirmed by FE–SEM observation, strong red emission at 615nm under the excitation of 395nm maximum was reached, then the higher annealed samples at above 1100 °C gave the lower emission intensities.

  1. 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.

  2. Sampling in Developmental Science: Situations, Shortcomings, Solutions, and Standards

    OpenAIRE

    Bornstein, Marc H.; Jager, Justin; Putnick, Diane L.

    2013-01-01

    Sampling is a key feature of every study in developmental science. Although sampling has far-reaching implications, too little attention is paid to sampling. Here, we describe, discuss, and evaluate four prominent sampling strategies in developmental science: population-based probability sampling, convenience sampling, quota sampling, and homogeneous sampling. We then judge these sampling strategies by five criteria: whether they yield representative and generalizable estimates of a study’s t...

  3. Microfluidic solutions enabling continuous processing and monitoring of biological samples: A review.

    Science.gov (United States)

    Karle, Marc; Vashist, Sandeep Kumar; Zengerle, Roland; von Stetten, Felix

    2016-07-27

    The last decade has witnessed tremendous advances in employing microfluidic solutions enabling Continuous Processing and Monitoring of Biological Samples (CPMBS), which is an essential requirement for the control of bio-processes. The microfluidic systems are superior to the traditional inline sensors due to their ability to implement complex analytical procedures, such as multi-step sample preparation, and enabling the online measurement of parameters. This manuscript provides a backgound review of microfluidic approaches employing laminar flow, hydrodynamic separation, acoustophoresis, electrophoresis, dielectrophoresis, magnetophoresis and segmented flow for the continuous processing and monitoring of biological samples. The principles, advantages and limitations of each microfluidic approach are described along with its potential applications. The challenges in the field and the future directions are also provided.

  4. Preparation of Superhydrophobic ZnO Films on Zinc Substrate by Chemical Solution Method

    Institute of Scientific and Technical Information of China (English)

    XU Wen-guo; LI Ji-hong; LU Shi-xiang; DUAN Ya-qiong; MA Cheng-xiang; SHI Xiao-feng; CHEN Yi-ling; YANG Yan-bo

    2012-01-01

    Superhydrophobic surface was prepared on the zinc substrate by chemical solution method via immersing clean pure zinc substrate into a water solution of zinc nitrate hexahydrate[Zn(NO3)2.6H2O] and hexamethylenetetraamine(C6H12N4) at 95℃ in water bath for 1.5 h,then modified with 18 alkanethiol.The best resulting surface shows superhydrophobic properties with a water contact angle of about 158° and a low water roll-off angle of around 3°.The prepared samples were characterize.d by powder X-ray diffraction(XRD),X-ray photoelectron spectroscopy (XPS),energy-dispersive X-ray spectroscopy(EDX),transmission electron microscopy(TEM),and scanning electron microscopy(SEM).SEM images of the films show that the resulting surface exhibits flower-shaped micro- and nano-structure.The surfaces of the prepared films were composed of ZnO nanorods which were wurtzite structure.The special flower-like micro- and nano-structure along with the low surface energy leads to the surface superhydrophobicity.

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

    Science.gov (United States)

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

    2017-08-08

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

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

    Science.gov (United States)

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

    2002-03-01

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

  7. Surelease or organic solution of ethylcellulose in preparation of sustained release theophylline micromatrices or matrices using spray drying technique.

    Science.gov (United States)

    Afrasiabi Garekani, Hadi; Sedighi, Samira; Sadeghi, Fatemeh

    2015-03-01

    This study evaluated ethylcellulose (EC) in two forms in preparation of sustained release theophylline microparticles using spray drying. Spray dried (SD) samples at different drug:polymer ratios were prepared using Surelease (SDaq) or organic solutions of ethylcellulose (SDor). Properties of particles (yield, particle morphology, size distribution and release profiles) were examined. Differential scanning calorimetry (DSC) and infrared spectroscopy (IR) studies were performed to track polymorphic changes and/or drug polymer interactions. SD samples were compressed and crushing strengths and release profiles were determined. The yields were in the range of 55-70%. The SD samples were nearly spherical with numerous fine particles attached to their surfaces. The SDor samples showed the smallest particle size. No polymorphism or drug-polymer interaction was observed. Uncompressed SDaq samples showed inadequate sustained release of drug compared to SDor samples. Surelease content did not affect drug release from SDaq samples. Tablets prepared from SDaq were softer and showed some plasticity, while those prepared from SDor exhibited higher crushing strengths. Tablets prepared from SDaq showed sustained release properties while the release of drug from compressed SDor samples were too slow. Overall Surelease was unable to sustain release of theophylline from SDaq microparticles, however, in compacted form showed more appropriate drug release than compacted SDor.

  8. Morphology, thermal and mechanical properties of PVC/MMT nanocomposites prepared by solution blending and solution blending + melt compounding

    DEFF Research Database (Denmark)

    Madaleno, Liliana Andreia Oliveira; Schjødt-Thomsen, Jan; Pinto, José Cruz

    2010-01-01

    and solution blending + melt compounding The effects on morphology, thermal and mechanical properties of the PVC/MMT nanocomposites were studied by varying the amount of Na-MMT and OMMT in both methods SEM and XRD analysis revealed that possible intercalated and exfoliated structures were obtained in all...... of the PVC/MMT nanocomposites Thermogravimetric analysis revealed that PVC/Na-MMT nanocomposites have better thermal stability than PVC/OMMT nanocomposites and PVC. In general, PVC/MMT nanocomposites prepared by solution blending + melt compounding revealed improved thermal properties compared to PVC....../MMT nanocomposites prepared by solution blending Vicar tests revealed a significant decrease in Vicar softening temperature of PVC/MMT nanocomposites prepared by solution blending + melt compounding compared to unfilled PVC The mechanical properties of the PVC/MMT nanocomposites were, in general, greatly improved...

  9. A 96-well screen filter plate for high-throughput biological sample preparation and LC-MS/MS analysis.

    Science.gov (United States)

    Peng, Sean X; Cousineau, Martin; Juzwin, Stephen J; Ritchie, David M

    2006-01-01

    A novel 96-well screen filter plate (patent pending) has been invented to eliminate a time-consuming and labor-intensive step in preparation of in vivo study samples--to remove blood or plasma clots. These clots plug the pipet tips during a manual or automated sample-transfer step causing inaccurate pipetting or total pipetting failure. Traditionally, these blood and plasma clots are removed by picking them out manually one by one from each sample tube before any sample transfer can be made. This has significantly slowed the sample preparation process and has become a bottleneck for automated high-throughput sample preparation using robotic liquid handlers. Our novel screen filter plate was developed to solve this problem. The 96-well screen filter plate consists of 96 stainless steel wire-mesh screen tubes connected to the 96 openings of a top plate so that the screen filter plate can be readily inserted into a 96-well sample storage plate. Upon insertion, the blood and plasma clots are excluded from entering the screen tube while clear sample solutions flow freely into it. In this way, sample transfer can be easily completed by either manual or automated pipetting methods. In this report, three structurally diverse compounds were selected to evaluate and validate the use of the screen filter plate. The plasma samples of these compounds were transferred and processed in the presence and absence of the screen filter plate and then analyzed by LC-MS/MS methods. Our results showed a good agreement between the samples prepared with and without the screen filter plate, demonstrating the utility and efficiency of this novel device for preparation of blood and plasma samples. The device is simple, easy to use, and reusable. It can be employed for sample preparation of other biological fluids that contain floating particulates or aggregates.

  10. Preparation of zein fibers using solution blow spinning method

    Science.gov (United States)

    Zein fibers were successfully fabricated via solution blow spinning (SBS) using acetic acid as solvent. Surface tension, viscosity and modulus of zein solutions were respectively determined by force tensiometer and rheometer. Increases of these properties were observed with an increase of concentrat...

  11. Quantitative Analysis of Heavy Metals in Water Based on LIBS with an Automatic Device for Sample Preparation

    Science.gov (United States)

    Hu, Li; Zhao, Nanjing; Liu, Wenqing; Meng, Deshuo; Fang, Li; Wang, Yin; Yu, Yang; Ma, Mingjun

    2015-08-01

    Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection. supported by National Natural Science Foundation of China (No. 60908018), National High Technology Research and Development Program of China (No. 2013AA065502) and Anhui Province Outstanding Youth Science Fund of China (No. 1108085J19)

  12. Chitosan-based hydrogel for dye removal from aqueous solutions: Optimization of the preparation procedure

    Science.gov (United States)

    Gioiella, Lucia; Altobelli, Rosaria; de Luna, Martina Salzano; Filippone, Giovanni

    2016-05-01

    The efficacy of chitosan-based hydrogels in the removal of dyes from aqueous solutions has been investigated as a function of different parameters. Hydrogels were obtained by gelation of chitosan with a non-toxic gelling agent based on an aqueous basic solution. The preparation procedure has been optimized in terms of chitosan concentration in the starting solution, gelling agent concentration and chitosan-to-gelling agent ratio. The goal is to properly select the material- and process-related parameters in order to optimize the performances of the chitosan-based dye adsorbent. First, the influence of such factors on the gelling process has been studied from a kinetic point of view. Then, the effects on the adsorption capacity and kinetics of the chitosan hydrogels obtained in different conditions have been investigated. A common food dye (Indigo Carmine) has been used for this purpose. Noticeably, although the disk-shaped hydrogels are in the bulk form, their adsorption capacity is comparable to that reported in the literature for films and beads. In addition, the bulk samples can be easily separated from the liquid phase after the adsorption process, which is highly attractive from a practical point of view. Compression tests reveal that the samples do not breakup even after relatively large compressive strains. The obtained results suggest that the fine tuning of the process parameters allows the production of mechanical resistant and highly adsorbing chitosan-based hydrogels.

  13. Amphiphilic mediated sample preparation for micro-flow cytometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-03-17

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

  14. Preparation and Evaluation of Veterinary 0.1% Injectable Solution of Atropine Sulphate

    Directory of Open Access Journals (Sweden)

    F K Mohammad

    2012-06-01

    Full Text Available This study introduces the know-how of preparing a multiple injection form atropine sulphate solution. An injectable aqueous solution of atropine sulphate at a concentration of 0.1%. was prepared under aseptic conditions in dark glass bottles each containing 50 ml. The preparation was intended for animal use only. It contained 1g atropine sulphate, 9 g sodium chloride as a normal saline, benzyl alcohol 15 ml as a preservative and water for injection up to 1000 ml. The pH of the solution was adjusted to 4.2 (range 3.0-6.5. The preparation of 0.1% atropine sulphate solution was clear colorless solution free from undesired particles. It complied with the requirements for injectable solutions. Further, the preparation was safe when used under laboratory conditions in chicks, rats and donkeys. It was also effective in preventing dichlorvos (an organophosphate insecticide-induced poisoning in chicks in a manner comparable to a commercial preparation of 0.1% atropine sulphate. In conclusion, the know-how of a preparation of 0.1% atropine sulphate solution is presented for veterinary use. [Vet. World 2012; 5(3.000: 145-149

  15. Human genomic DNA analysis using a semi-automated sample preparation, amplification, and electrophoresis separation platform.

    Science.gov (United States)

    Raisi, Fariba; Blizard, Benjamin A; Raissi Shabari, Akbar; Ching, Jesus; Kintz, Gregory J; Mitchell, Jim; Lemoff, Asuncion; Taylor, Mike T; Weir, Fred; Western, Linda; Wong, Wendy; Joshi, Rekha; Howland, Pamela; Chauhan, Avinash; Nguyen, Peter; Petersen, Kurt E

    2004-03-01

    The growing importance of analyzing the human genome to detect hereditary and infectious diseases associated with specific DNA sequences has motivated us to develop automated devices to integrate sample preparation, real-time PCR, and microchannel electrophoresis (MCE). In this report, we present results from an optimized compact system capable of processing a raw sample of blood, extracting the DNA, and performing a multiplexed PCR reaction. Finally, an innovative electrophoretic separation was performed on the post-PCR products using a unique MCE system. The sample preparation system extracted and lysed white blood cells (WBC) from whole blood, producing DNA of sufficient quantity and quality for a polymerase chain reaction (PCR). Separation of multiple amplicons was achieved in a microfabricated channel 30 microm x 100 microm in cross section and 85 mm in length filled with a replaceable methyl cellulose matrix operated under denaturing conditions at 50 degrees C. By incorporating fluorescent-labeled primers in the PCR, the amplicons were identified by a two-color (multiplexed) fluorescence detection system. Two base-pair resolution of single-stranded DNA (PCR products) was achieved. We believe that this integrated system provides a unique solution for DNA analysis.

  16. Sample preparation for laser-microdissection of soybean shoot apical meristem

    Directory of Open Access Journals (Sweden)

    Chui E. Wong

    2012-10-01

    Full Text Available The shoot apical meristem houses stem cells responsible for the continuous formation of aerial plant organs including leaves and stems throughout the life of plants. Laser-microdissection in combination with high-throughput technology such as next generation sequencing permits an in-depth analysis of molecular events associated with specific cell type of interest. Sample preparation is the most critical step in ensuring good quality RNA to be extracted from samples following laser-microdissection. Here, we optimized the sample preparation for a major legume crop, soybean. We used Farmer’s solution as a fixative and paraffin as the embedding medium for soybean shoot apical meristem tissue without the use of any specialized equipment. Shorter time for tissue fixation (two days was found to be critical for the preservation of RNA in soybean shoot apical meristem. We further demonstrated the utility of this method for different tissues derived from soybean and rice. The method outlined here shall facilitate studies on crop plants involving laser-microdissection.

  17. Application of a Dual-Arm Robot in Complex Sample Preparation and Measurement Processes.

    Science.gov (United States)

    Fleischer, Heidi; Drews, Robert Ralf; Janson, Jessica; Chinna Patlolla, Bharath Reddy; Chu, Xianghua; Klos, Michael; Thurow, Kerstin

    2016-10-01

    Automation systems with applied robotics have already been established in industrial applications for many years. In the field of life sciences, a comparable high level of automation can be found in the areas of bioscreening and high-throughput screening. Strong deficits still exist in the development of flexible and universal fully automated systems in the field of analytical measurement. Reasons are the heterogeneous processes with complex structures, which include sample preparation and transport, analytical measurements using complex sensor systems, and suitable data analysis and evaluation. Furthermore, the use of nonstandard sample vessels with various shapes and volumes results in an increased complexity. The direct use of existing automation solutions from bioscreening applications is not possible. A flexible automation system for sample preparation, analysis, and data evaluation is presented in this article. It is applied for the determination of cholesterol in biliary endoprosthesis using gas chromatography-mass spectrometry (GC-MS). A dual-arm robot performs both transport and active manipulation tasks to ensure human-like operation. This general robotic concept also enables the use of manual laboratory devices and equipment and is thus suitable in areas with a high standardization grade.

  18. 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.

  19. Preparing Culturally Diverse Special Education Faculty: Challenges and Solutions

    Science.gov (United States)

    Peterson, Patricia; Showalter, Stephen

    2010-01-01

    This paper describes why more bilingual culturally responsive special education faculty are needed to meet the needs of the increasing number of culturally and linguistically diverse students with disabilities in the United States. In addition, the paper presents the successes and challenges in the journey to prepare university faculty leaders in…

  20. Sampling in Developmental Science: Situations, Shortcomings, Solutions, and Standards.

    Science.gov (United States)

    Bornstein, Marc H; Jager, Justin; Putnick, Diane L

    2013-12-01

    Sampling is a key feature of every study in developmental science. Although sampling has far-reaching implications, too little attention is paid to sampling. Here, we describe, discuss, and evaluate four prominent sampling strategies in developmental science: population-based probability sampling, convenience sampling, quota sampling, and homogeneous sampling. We then judge these sampling strategies by five criteria: whether they yield representative and generalizable estimates of a study's target population, whether they yield representative and generalizable estimates of subsamples within a study's target population, the recruitment efforts and costs they entail, whether they yield sufficient power to detect subsample differences, and whether they introduce "noise" related to variation in subsamples and whether that "noise" can be accounted for statistically. We use sample composition of gender, ethnicity, and socioeconomic status to illustrate and assess the four sampling strategies. Finally, we tally the use of the four sampling strategies in five prominent developmental science journals and make recommendations about best practices for sample selection and reporting.

  1. Simple, Expendable, 3D-Printed Microfluidic Systems for Sample Preparation of Petroleum.

    Science.gov (United States)

    Kataoka, Érica M; Murer, Rui C; Santos, Jandyson M; Carvalho, Rogério M; Eberlin, Marcos N; Augusto, Fabio; Poppi, Ronei J; Gobbi, Angelo L; Hantao, Leandro W

    2017-03-21

    In this study, we introduce a simple protocol to manufacture disposable, 3D-printed microfluidic systems for sample preparation of petroleum. This platform is produced with a consumer-grade 3D-printer, using fused deposition modeling. Successful incorporation of solid-phase extraction (SPE) to microchip was ensured by facile 3D element integration using proposed approach. This 3D-printed μSPE device was applied to challenging matrices in oil and gas industry, such as crude oil and oil-brine emulsions. Case studies investigated important limitations of nonsilicon and nonglass microchips, namely, resistance to nonpolar solvents and conservation of sample integrity. Microfluidic features remained fully functional even after prolonged exposure to nonpolar solvents (20 min). Also, 3D-printed μSPE devices enabled fast emulsion breaking and solvent deasphalting of petroleum, yielding high recovery values (98%) without compromising maltene integrity. Such finding was ascertained by high-resolution molecular analyses using comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry by monitoring important biomarker classes, such as C10 demethylated terpanes, ααα-steranes, and monoaromatic steroids. 3D-Printed chips enabled faster and reliable preparation of maltenes by exhibiting a 10-fold reduction in sample processing time, compared to the reference method. Furthermore, polar (oxygen-, nitrogen-, and sulfur-containing) analytes found in low-concentrations were analyzed by Fourier transform ion cyclotron resonance mass spectrometry. Analysis results demonstrated that accurate characterization may be accomplished for most classes of polar compounds, except for asphaltenes, which exhibited lower recoveries (82%) due to irreversible adsorption to sorbent phase. Therefore, 3D-printing is a compelling alternative to existing microfabrication solutions, as robust devices were easy to prepare and operate.

  2. Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology.

    Science.gov (United States)

    Causon, Tim J; Hann, Stephan

    2016-09-28

    Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid

  3. Comparison of physicomechanical properties of films prepared from organic solutions and aqueous dispersion of Eudragit RL

    Directory of Open Access Journals (Sweden)

    H Afrasiabi Garekani

    2011-05-01

    Full Text Available Background and the purpose of the study: Mechanical properties of films prepared from aqueous dispersion and organic solutions of Eudragit RL were assessed and the effects of plasticizer type, concentration and curing were examined. Methods: Films were prepared from aqueous dispersion and solutions of Eudragit RL (isopropyl alcohol-water 9:1 containing 0, 10 or 20% (based on polymer weight of PEG 400 or Triethyl Citrate (TEC as plasticizer using casting method. Samples of films were stored in oven at 60ºC for 24 hrs (Cured. The stress-strain curve was obtained for each film using material testing machine and tensile strength, elastic modulus, %elongation and work of failure were calculated. Results and major conclusion: The films with no plasticizer showed different mechanical properties depending on the vehicle used. Addition of 10% or 20% of plasticizer decreased the tensile strength and elastic modulus and increased %elongation and work of failure for all films. The effect of PEG400 on mechanical properties of Eudragit RL films was more pronounced. The differences in mechanical properties of the films due to vehicle decreased by addition of plasticizer and increase in its concentration. Curing process weakened the mechanical properties of the films with no plasticizer and for films with 10% plasticizer no considerable difference in mechanical properties was observed before and after curing. For those with 20% plasticizer only films prepared from aqueous dispersion showed remarkable difference in mechanical properties before and after curing. Results of this study suggest that the mechanical properties of the Eudragit RL films were affected by the vehicle, type of plasticizer and its concentration in the coating liquid.

  4. Epidural top-up solutions for emergency caesarean section: a comparison of preparation times.

    Science.gov (United States)

    Lucas, D N; Borra, P J; Yentis, S M

    2000-04-01

    We compared the preparation times of three solutions commonly used for epidural top-up for emergency Caesarean section. Twenty-two anaesthetists were asked to prepare fresh solutions in random order as quickly as possible: 0.5% bupivacaine 20 ml (B); 2% lidocaine 20 ml with 1:200,000 epinephrine (LE); and 0.5% bupivacaine 10 ml and 2% lidocaine 10 ml with 1:200,000 epinephrine and 8.4% sodium bicarbonate 2 ml (BLEB). Preparation times for B were approximately half of those for LE, which in turn were approximately half of those for BLEB (P = 0.0001). If local anaesthetic solutions with additives such as epinephrine or bicarbonate are prepared just before emergency Caesarean section, any possible reduction in onset time that they might afford may be offset by the additional preparation time required.

  5. Preparation of {0 1 0}-faceted anatase TiO2 nanocuboids from peroxotitanium complex solution

    Science.gov (United States)

    Miao, Yigao; Gao, Jiacheng

    2012-12-01

    {0 1 0}-faceted anatase TiO2 nanocuboids have been fabricated by hydrothermal route using peroxotitanium complex solution as precursor. The effects of reaction time, the amount of urea and temperature on the formation of {0 1 0}-faceted anatase TiO2 were characterized by XRD, FESEM and TEM. The growth mechanism of nanocuboids was proposed that the nanocuboids were formed by the transition from H2Ti2O5·H2O phase to anatase TiO2 in the basic condition. The photocatalytic performance of the prepared samples was tested in the degradation of Rhodamine B and the anatase nanocuboids exhibited enhanced photocatalytic activity compared with the standard P25 powders.

  6. Semiautomated Sample Preparation for Protein Stability and Formulation Screening via Buffer Exchange.

    Science.gov (United States)

    Ying, William; Levons, Jaquan K; Carney, Andrea; Gandhi, Rajesh; Vydra, Vicky; Rubin, A Erik

    2016-06-01

    A novel semiautomated buffer exchange process workflow was developed to enable efficient early protein formulation screening. An antibody fragment protein, BMSdab, was used to demonstrate the workflow. The process afforded 60% to 80% cycle time and scientist time savings and significant material efficiencies. These efficiencies ultimately facilitated execution of this stability work earlier in the drug development process, allowing this tool to inform the developability of potential candidates for development from a formulation perspective. To overcome the key technical challenges, the protein solution was buffer-exchanged by centrifuge filtration into formulations for stability screening in a 96-well plate with an ultrafiltration membrane, leveraging automated liquid handling and acoustic volume measurements to allow several cycles of exchanges. The formulations were transferred into a vacuum manifold and sterile filtered into a rack holding 96 glass vials. The vials were sealed with a capmat of individual caps and placed in stability stations. Stability of the samples prepared by this process and by the standard process was demonstrated to be comparable. This process enabled screening a number of formulations of a protein at an early pharmaceutical development stage with a short sample preparation time.

  7. Preview of the NASA NNWG NDE Sample Preparation Handbook

    Science.gov (United States)

    2010-01-01

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

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

    Lifescience Database Archive (English)

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

  9. Preparation of Chemical Samples On Relevant Surfaces Using Inkjet Technology

    Science.gov (United States)

    2013-04-01

    moisture is absorbed by the chemical from the air. The weight eventually stabilizes as the chemical moisture content approaches that of the air. This...when similar chemical solutions are paint -sprayed onto a hot (70 °C) substrate, the crystals are smaller, more numerous, and more closely spaced. To...gravity, surface tension, particle size, and chemical composition. Substrate material may be wood, metal, glass, plastic, concrete, road blacktop, dirt

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

    Lifescience Database Archive (English)

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

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

    Institute of Scientific and Technical Information of China (English)

    Zhang Xiaohui; Peng Xigao

    2010-01-01

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

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

    Lifescience Database Archive (English)

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

  13. Preparation of Zeolite A from alkali solutions containing potassium

    Energy Technology Data Exchange (ETDEWEB)

    Goryachev, A.A.; Kuks, V.F.

    1983-03-20

    The most inexpensive general-purpose zeolite is Zeolite A. It is widely used as an adsorbent for drying hydrocarbon gases, for separation of normal paraffins, and recently as a component of synthetic detergents. The goal of this work was to study the effect of potassium, in crystallizing mixtures analogous to those used in industry, on the production of powdered Zeolite A and Zeolite A without binder on the basis of kaolin. It has been found that Zeolite A may be obtained upon crystallization of aluminosilica gel on the basis of aluminate and silicate solutions with a relative potassium content in the mixture to be crystallized that is not more than 0.8-0.14 mole fraction of the sum of the cations. In the case of crystallization of Zeolite A without binder on the basis of product, the amount of potassium should not be more than 5 rel. %. This is explained by the difference in the crystallization mechanism and the properties of the aluminate solutions containing potassium and silicon.

  14. Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

    Science.gov (United States)

    Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

    2016-04-01

    We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents.

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

    OpenAIRE

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

    2006-01-01

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

  16. 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.

  17. Advanced titania buffer layer architectures prepared by chemical solution deposition

    Science.gov (United States)

    Kunert, J.; Bäcker, M.; Brunkahl, O.; Wesolowski, D.; Edney, C.; Clem, P.; Thomas, N.; Liersch, A.

    2011-08-01

    Chemical solution deposition (CSD) was used to grow high-quality (100) oriented films of SrTiO3 (STO) on CSD CaTiO3 (CTO), Ba0.1Ca0.9TiO3 (BCT) and STO seed and template layers. These template films bridge the lattice misfit between STO and the nickel-tungsten (NiW) substrate, assisting in dense growth of textured STO. Additional niobium (Nb) doping of the STO buffer layer reduces oxygen diffusion which is necessary to avoid undesired oxidation of the NiW. The investigated templates offer suitable alternatives to established standard buffer systems like La2Zr2O7 (LZO) and CeO2 for coated conductors.

  18. Structure of a passivated Ge surface prepared from aqueous solution.

    Energy Technology Data Exchange (ETDEWEB)

    Lyman, P. F.; Sakata, O.; Marasco, D, L.; Lee, T.-L.; Breneman, K. D.; Keane, D. T.; Bedzyk, M. J.; Materials Science Division; Northwestern Univ.; Univ. of Wisconsin at Milwaukee

    2000-08-10

    The structure of a passivating sulfide layer on Ge(001) was studied using X-ray standing waves and X-ray fluorescence. The sulfide layer was formed by reacting clean Ge substrates in (NH{sub 4}){sub 2}S solutions of various concentrations at 80{sup o}C. For each treatment, a sulfide layer containing approximately two to three monolayers (ML) of S was formed on the surface, and an ordered structure was found at the interface that contained approximately 0.4 ML of S. Our results suggest the rapid formation of a glassy GeS{sub x} layer containing 1.5-2.5 ML S residing atop a partially ordered interfacial layer of bridge-bonded S. The passivating reaction appears to be self-limited to 2-3 ML at this reaction temperature.

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

    NARCIS (Netherlands)

    Roelofs, Susan Helena

    2015-01-01

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

  20. Microsystem strategies for sample preparation in biological detection.

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-03-01

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

  1. Effect of Preparation Method on Surface Area and Crystalline Form of CeO2-ZrO2 Solid Solution

    Institute of Scientific and Technical Information of China (English)

    王晓红; 郭耘; 卢冠忠; 郭杨龙; 王筠松; 张志刚; 刘晓晖

    2004-01-01

    The CeO2-ZrO2 solid solutions were prepared by a reverse microemulsion method. The effect of preparation parameters on the surface area and crystalline form of the solid solutions were studied by the BET surface area and XRD analysis. The studies indicate that the separation of the microemulsion phase during the preparation procedure can decrease the specific surface area of sample, adding hydrogen peroxide in the matrix solution can increase the specific surface area and stability of sample. The surface area of sample calcined at 550 ℃ for 5 h is 149 m2·g-1, and that calcined at 900 ℃ for 6 h is 88 m2·g-1.The sample with tetragonal symmetry Ce0.5Zr0.5O2 phase has a higher stability.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-22

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

  3. Comparison of detergent-based sample preparation workflows for LTQ-Orbitrap analysis of the Escherichia coli proteome.

    Science.gov (United States)

    Tanca, Alessandro; Biosa, Grazia; Pagnozzi, Daniela; Addis, Maria Filippa; Uzzau, Sergio

    2013-09-01

    This work presents a comparative evaluation of several detergent-based sample preparation workflows for the MS-based analysis of bacterial proteomes, performed using the model organism Escherichia coli. Initially, RapiGest- and SDS-based buffers were compared for their protein extraction efficiency and quality of the MS data generated. As a result, SDS performed best in terms of total protein yields and overall number of MS identifications, mainly due to a higher efficiency in extracting high molecular weight (MW) and membrane proteins, while RapiGest led to an enrichment in periplasmic and fimbrial proteins. Then, SDS extracts underwent five different MS sample preparation workflows, including: detergent removal by spin columns followed by in-solution digestion (SC), protein precipitation followed by in-solution digestion in ammonium bicarbonate or urea buffer, filter-aided sample preparation (FASP), and 1DE separation followed by in-gel digestion. On the whole, about 1000 proteins were identified upon LC-MS/MS analysis of all preparations (>1100 with the SC workflow), with FASP producing more identified peptides and a higher mean sequence coverage. Each protocol exhibited specific behaviors in terms of MW, hydrophobicity, and subcellular localization distribution of the identified proteins; a comparative assessment of the different outputs is presented.

  4. Preparation of 3-D porous fibroin scaffolds by freeze drying with treatment of methanol solutions

    Institute of Scientific and Technical Information of China (English)

    ZHAN JingLin; SUN XiaoDan; CUI FuZhai; KONG XiangDong

    2007-01-01

    In this study,silk scaffolds with appropriate porous structures were prepared by adjusting solution concentrations and providing treatment with methanol solutions in the way of freeze drying. The effects of the preparation conditions on the microstructures and properties of the scaffolds were discussed. Fibroin solutions with different concentrations of 4,6,8,10 wt% were used respectively to prepare the scaffolds. The effects of the addition of 20 vol% methanol before or after freeze drying to the 4 wt% fibroin solution were investigated. As demonstrated by Scanning Electron Microscope (SEM),the fibroin scaffolds prepared without methanol had porous microstructures composed of thin sheets,and the sizes of the pores decreased with the increase of the fibroin solution concentrations,while the scaffolds prepared in the presence of methanol showed porous microstructures formed by fine-particle aggregates. The porosities and mechanical properties of the prepared fibroin scaffolds under different conditions were tested. The crystalline structures and conformations of the fibroin scaffolds were detected by Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD).

  5. Sample preparation and assay refinements for pathogen detection platforms

    Science.gov (United States)

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

    2009-02-01

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

  6. Morphology control of brushite prepared by aqueous solution synthesis

    Directory of Open Access Journals (Sweden)

    T. Toshima

    2014-03-01

    Full Text Available Dicalcium phosphate dihydrate (DCPD, CaHPO4·2H2O, also known as brushite, is one of the important bioceramics due to not only diseases factors such as kidney stone and plaque formation but also purpose as fluoride insolubilization material. It is used medicinally to supply calcium, and is of interest for its unique properties in biological and pathological mineralization. It is important to control the crystal morphology of brushite since its chemical reactivity depends strongly on its surface properties; thus, its morphology is a key issue for its applications as a functional material or precursor for other bioceramics. Here, we report the effects of the initial pH and the Ca and phosphate ion concentrations on the morphology of DCPD particles during aqueous solution synthesis. Crystal morphologies were analyzed by scanning electron microscopy and X-ray diffraction. The morphology phase diagram of DCPD crystallization revealed that increasing the initial pH and/or ion concentration transformed DCPD morphology from petal-like into plate-like structures.

  7. GAMSOR: Gamma Source Preparation and DIF3D Flux Solution

    Energy Technology Data Exchange (ETDEWEB)

    Smith, M. A. [TerraPower, Bellevue, WA (United States); Lee, C. H. [TerraPower, Bellevue, WA (United States); Hill, R. N. [TerraPower, Bellevue, WA (United States)

    2017-06-28

    Nuclear reactors that rely upon the fission reaction have two modes of thermal energy deposition in the reactor system: neutron absorption and gamma absorption. The gamma rays are typically generated by neutron capture reactions or during the fission process which means the primary driver of energy production is of course the neutron interaction. In conventional reactor physics methods, the gamma heating component is ignored such that the gamma absorption is forced to occur at the gamma emission site. For experimental reactor systems like EBR-II and FFTF, the placement of structural pins and assemblies internal to the core leads to problems with power heating predictions because there is no fission power source internal to the assembly to dictate a spatial distribution of the power. As part of the EBR-II support work in the 1980s, the GAMSOR code was developed to assist analysts in calculating the gamma heating. The GAMSOR code is a modified version of DIF3D and actually functions within a sequence of DIF3D calculations. The gamma flux in a conventional fission reactor system does not perturb the neutron flux and thus the gamma flux calculation can be cast as a fixed source problem given a solution to the steady state neutron flux equation. This leads to a sequence of DIF3D calculations, called the GAMSOR sequence, which involves solving the neutron flux, then the gamma flux, and then combining the results to do a summary edit. In this manuscript, we go over the GAMSOR code and detail how it is put together and functions. We also discuss how to setup the GAMSOR sequence and input for each DIF3D calculation in the GAMSOR sequence.

  8. Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

    Science.gov (United States)

    Stark, Peter C.; Zurek, Eduardo; Wheat, Jeffrey V.; Dunbar, John M.; Olivares, Jose A.; Garcia-Rubio, Luis H.; Ward, Michael D.

    2011-07-26

    There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

  9. Adsorption of Pb(2+) from aqueous solution using spinel ferrite prepared from steel pickling sludge.

    Science.gov (United States)

    Fang, Binbin; Yan, Yubo; Yang, Yang; Wang, Fenglian; Chu, Zhen; Sun, Xiuyun; Li, Jiansheng; Wang, Lianjun

    2016-01-01

    In this paper, spinel ferrite with high crystallinity and high saturation magnetization was successfully prepared from steel pickling sludge by adding iron source and precipitator in the hydrothermal condition. The obtained spinel ferrite was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), vibrating sample magnetometer (VSM), and Zeta potential methods and investigated as an adsorbent for removal of Pb(2+) from aqueous solution. Batch experiments were performed by varying the pH values, contact time, temperature and initial metal concentration. The result of pH impact showed that the adsorption of Pb(2+) was a pH dependent process, and the pH 5.8 ± 0.2 was found to be the optimum condition. The achieved experimental data were analyzed with various kinetic and isotherm models. The kinetic studies revealed that Pb(2+) adsorption onto spinel ferrite followed a pseudo-second order model, and the Langmuir isotherm model provided the perfect fit to the equilibrium experimental data. At different temperatures, the maximum Pb(2+) adsorption capacities calculated from the Langmuir equation were in the range of 126.5-175.4 mg/g, which can be in competition with other adsorbents. The thermodynamic results showed that the spinel ferrite could spontaneously and endothermically adsorb Pb(2+) from aqueous solution. The regeneration studies showed that spinel ferrite could be used five times (removal efficiency (%) >90%) by desorption with HNO3 reagent.

  10. Levels of carnitine and acylcarnitines in reconstituted red blood cell samples washed with different concentrations of saline solutions

    Directory of Open Access Journals (Sweden)

    José Henry Osorio

    2011-01-01

    Full Text Available Objective: To evaluate the percentage of carnitine and acylcarnitines remaining in red blood cells after washing them with different concentrations of saline solution. Materials and methods: Human blood samples were centrifuged and the blood cells were washed with different saline solutions. The final pellet was resuspended in PBS for card preparation and tandem mass spectrometry analysis. Results: It was found that carnitine, as well as short-chain, medium-chain, and long-chain acylcarnitines remain in red blood cells at average percentages of 19.3; 34; 34; and 32%, respectively. Significant differences were found for carnitine and acylcarnitine levels in blood washed with an isotonic solution compared to their levels using several hypotonic solutions (p<0.05. Conclusion: Because carnitine and acylcarnitines remained associated with the blood cells, we recommend using whole blood to measure these metabolites.

  11. Levels of carnitine and acylcarnitines in reconstituted red blood cell samples washed with different concentrations of saline solutions

    Directory of Open Access Journals (Sweden)

    José Henry Osorio

    2010-12-01

    Full Text Available Objective: To evaluate the percentage of carnitine and acylcarnitines remaining in red blood cells after washing them with different concentrations of saline solution.Materials and methods: Human blood samples were centrifuged and the blood cells were washed with different saline solutions. The final pellet was resuspended in PBS for card preparation and tandem mass spectrometry analysis.Results: It was found that carnitine, as well as short-chain, medium-chain, and long-chain acylcarnitines remain in red blood cells at average percentages of 19.3; 34; 34; and 32%, respectively. Significant differences were found for carnitine and acylcarnitine levels in blood washed with an isotonic solution compared to their levels using several hypotonic solutions (p<0.05.Conclusion: Because carnitine and acylcarnitines remained associated with the blood cells, we recommend using whole blood to measure these metabolites.

  12. 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.

  13. GAMSOR: Gamma Source Preparation and DIF3D Flux Solution

    Energy Technology Data Exchange (ETDEWEB)

    Smith, M. A. [Argonne National Lab. (ANL), Argonne, IL (United States); Lee, C. H. [Argonne National Lab. (ANL), Argonne, IL (United States); Hill, R. N. [Argonne National Lab. (ANL), Argonne, IL (United States)

    2016-12-15

    Nuclear reactors that rely upon the fission reaction have two modes of thermal energy deposition in the reactor system: neutron absorption and gamma absorption. The gamma rays are typically generated by neutron absorption reactions or during the fission process which means the primary driver of energy production is of course the neutron interaction. In conventional reactor physics methods, the gamma heating component is ignored such that the gamma absorption is forced to occur at the gamma emission site. For experimental reactor systems like EBR-II and FFTF, the placement of structural pins and assemblies internal to the core leads to problems with power heating predictions because there is no fission power source internal to the assembly to dictate a spatial distribution of the power. As part of the EBR-II support work in the 1980s, the GAMSOR code was developed to assist analysts in calculating the gamma heating. The GAMSOR code is a modified version of DIF3D and actually functions within a sequence of DIF3D calculations. The gamma flux in a conventional fission reactor system does not perturb the neutron flux and thus the gamma flux calculation can be cast as a fixed source problem given a solution to the steady state neutron flux equation. This leads to a sequence of DIF3D calculations, called the GAMSOR sequence, which involves solving the neutron flux, then the gamma flux, then combining the results to do a summary edit. In this manuscript, we go over the GAMSOR code and detail how it is put together and functions. We also discuss how to setup the GAMSOR sequence and input for each DIF3D calculation in the GAMSOR sequence. With the GAMSOR capability, users can take any valid steady state DIF3D calculation and compute the power distribution due to neutron and gamma heating. The MC2-3 code is the preferable companion code to use for generating neutron and gamma cross section data, but the GAMSOR code can accept cross section data from other sources. To further

  14. 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.

  15. Improved mass spectrometric analysis of membrane proteins based on rapid and versatile sample preparation on nanodiamond particles.

    Science.gov (United States)

    Pham, Minh D; Yu, Steve S-F; Han, Chau-Chung; Chan, Sunney I

    2013-07-16

    We have developed a novel streamlined sample preparation procedure for mass spectrometric (MS) analysis of membrane proteins using surface-oxidized nanodiamond particles. The platform consists of solid-phase extraction and elution of the membrane proteins on nanodiamonds, concentrating the membrane proteins on the nanodiamonds and separating out detergents, chaotropic agents, and salts, and other impurities that are often present at high concentrations in solubilized membrane preparations. In this manner, membrane-protein extracts are transformed into MS-ready samples in minutes. The protocol is not only fast, but also widely adaptable and highly effective for preparing generic membrane protein samples for both MALDI-MS studies of membrane-protein complexes and shotgun membrane proteomics studies. As proof of concept, we have demonstrated substantial improvements in the MALDI-MS analysis of the particulate methane monooxygenase (pMMO) complex, a three-subunit transmembrane protein solubilized in various detergent buffers. Enzymatic digestions of membrane proteins are also greatly facilitated since the proteins extracted on to the nanodiamonds are exposed on the surface of the nanoparticles rather than in SDS gels or in detergent solutions. We illustrate the effectiveness of nanodiamonds for SDS removal in the preparation of membrane proteins for MS analysis on the proteome level by examining the quality of the tryptic peptides prepared by on-surface nanodiamond digestion of an E. coli membrane fraction for shotgun proteomics.

  16. Interstitial positions of tin ions in alpha-(FerichSn)(2)O-3 solid solutions prepared by mechanical alloying

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Lin, Rong; Nielsen, Kurt

    1997-01-01

    The microstructure of samples of 91, 85, and 71 mol % alpha-Fe-2-O-3-SnO2. prepared by mechanical alloying, has been studied by x-ray diffraction with Rietveld structure refinements, On the basis of the structure refinements to the whole x-ray diffraction patterns for the four as-milled samples......, it is found that tin ions do not substitute iron ions in the solid solution, although this model is generally assumed in the literature. The Sn4+ ions occupy the empty octahedral holes in the lattice of the alpha-Fe2O3 phase....

  17. Preparation and Characterization of CeO2-ZrO2 Solid Solution Ultrafine Particles Using Reversed Microemulsion

    Institute of Scientific and Technical Information of China (English)

    An Yuan; Li Li; Wang Jun; Shen Meiqing

    2005-01-01

    Ce0.6Zr0.4O2 solid solution ultrafine particle was prepared in the cyclohexane/water/OP-10/n-hexanol reversed microemulsion. The quasi-ternary phase diagram investigations showed that the system has narrow W/O type microemulison region, so it is the proper system to prepare Ce0.6Zr0.4O2 solid solution ultrafine particle. Some physical-chemical techniques such as TG/DTA, XRD, BET, and HRTEM are used to characterize the resultant powders. The results show that the fluorite cubic Ce0.6Zr0.4O2 solid solution is obtained at 400 ℃. The surface area is (146.7 m2·g-1), which is higher than the surface area for sol-gel prepared sample (59.5 m2·g-1). HRTEM images indicated that the Ce0.6Zr0.4O2 solid solution ultrafine particle is well-crystallized, narrow size distribution, less agglomeration, within mean size of 5~7 nm.

  18. Adsorption of cadmium from aqueous solutions on sulfurized activated carbon prepared from nut shells.

    Science.gov (United States)

    Fouladi Tajar, Amir; Kaghazchi, Tahereh; Soleimani, Mansooreh

    2009-06-15

    Low-cost activated carbon, derived from nut shells, and its modified sample have been used as replacements for the current expensive methods of removing cadmium from aqueous solutions and waste waters. Adsorption of cadmium onto four kinds of activated carbons has been studied; prepared activated carbon (PAC), commercial activated carbon (CAC), and the sulfurized ones (SPAC & SCAC). The activated carbon has been derived, characterized, treated with sulfur and then utilized for the removal of Cd(2+). Sulfurizing agent (SO(2) gas) was successfully used in adsorbents' modification process at the ambient temperature. Samples were then characterized and tested as adsorbents of cadmium. Effect of some parameters such as contact time, initial concentration and pH were examined. With increasing pH, the adsorption of cadmium ions was increased and maximum removal, 92.4% for SPAC, was observed in pH>8.0 (C(0)=100mg/L). The H-type adsorption isotherms, obtained for the adsorbents, indicated a favorable process. Adsorption data on both prepared and commercial activated carbon, before and after sulfurization, followed both the Frendlich and Langmuir models. They were better fitted by Frendlich isotherm as compared to Langmuir. The maximum adsorption capacities were 90.09, 104.17, 126.58 and 142.86 mg/g for CAC, PAC, SCAC and SPAC, respectively. Accordingly, surface modification of activated carbons using SO(2) greatly enhanced cadmium removal. The reversibility of the process has been studied in a qualitative manner and it shows that the spent SPAC can be effectively regenerated for further use easily.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-03-15

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

  20. METHODOLOGICAL ASPECTS OF MOLASSES SAMPLE PREPARATION IN SULFUR DIOXIDE CONTENT DETERMINING

    Directory of Open Access Journals (Sweden)

    M. I. Egorova

    2015-01-01

    Full Text Available Summary. Molasses is characterized as sugar production by-product from primary or secondary sacchariferous raw materials. The features of the appearance, the chemical composition, molasses and exit directions of its use, depending on the type of production, in which it is formed. The value of molasses is demonstrated according to its total composition as well as its use directions. Statistics on beet molasses amounts in Russia is presented. Described consumer market molasses in Russia and abroad with its exports. Shown regulations contain requirements for the quality and safety of molasses, including sulfur dioxide. The data on sulfur allergenic properties are presented. Showing source of the sulfur dioxide in the residual molasses number of processing aids and the impact of its level in the value of raw molasses for use in biotechnological processes and fodder production. The necessity to develop methodology for determining the sulfur dioxide content in the molasses to control its security. The iodometric method, which is used in practice for determination of sulphur dioxide in foods are characterized. Differences molasses and sugar as objects of iodometric determination of sulfur dioxide, which leads to the inability to ascertain the equivalence point. The variants eliminate interfering background of dark-colored foods common in analytical chemistry. Advantages and disadvantages of the background masking and stripping the determination of sulfur dioxide in the darkcolored products. It was characterized by clarifying sugar solutions in optical control methods. The hypothesis about preferability of its use in sample molasses preparation for equivalence point fixation in iodometric titration is suggested. The tasks of experimental research for the development of sample preparation algorithm molasses in determining the content of sulphurous acid.

  1. Can mothers safely prepare labon-gur salt-sugar solution after demonstration in a diarrhoeal hospital?

    DEFF Research Database (Denmark)

    Islam, M A; Kofoed, Poul-Erik; Begum, S

    1992-01-01

    Home-based salt-sugar solution (SSS) prepared with labon (locally produced sea salt) and gur (unrefined brown sugar) has been recommended as a cheap, locally available and a simple tool to prevent and treat diarrhoeal dehydration. Preparation of labon-gur SSS is demonstrated to the patients...... and the attendants at ICDDR, Bangladesh. To evaluate performances, 150 mothers were asked to measure labon and gur by finger pinch and first method and 100 mothers measured half a seer of water to prepare labon-gur SSS, shortly after the demonstration sessions. 4.0% of the samples exceeded the upper safety limit...... this knowledge. Our study suggests that demonstration of home-based SSS in a diarrhoeal hospital may positively affect health education and that health personnel should actively participate in increasing health awareness....

  2. Suspension trapping (STrap) sample preparation method for bottom-up proteomics analysis.

    Science.gov (United States)

    Zougman, Alexandre; Selby, Peter J; Banks, Rosamonde E

    2014-05-01

    Despite recent developments in bottom-up proteomics, the need still exists in a fast, uncomplicated, and robust method for comprehensive sample processing especially when applied to low protein amounts. The suspension trapping method combines the advantage of efficient SDS-based protein extraction with rapid detergent removal, reactor-type protein digestion, and peptide cleanup. Proteins are solubilized in SDS. The sample is acidified and introduced into the suspension trapping tip incorporating the depth filter and hydrophobic compartments, filled with the neutral pH methanolic solution. The instantly formed fine protein suspension is trapped in the depth filter stack-this crucial step is aimed at separating the particulate matter in space. SDS and other contaminants are removed in the flow-through, and a protease is introduced. Following the digestion, the peptides are cleaned up using the tip's hydrophobic part. The methodology allows processing of protein loads down to the low microgram/submicrogram levels. The detergent removal takes about 5 min, whereas the tryptic proteolysis of a cellular lysate is complete in as little as 30 min. We have successfully utilized the method for analysis of cellular lysates, enriched membrane preparations, and immunoprecipitates. We expect that due to its robustness and simplicity, the method will become an essential proteomics tool.

  3. 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

  4. 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.

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

    Directory of Open Access Journals (Sweden)

    A Poorbafrani

    2008-07-01

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

  6. Preparation of optimized uranium and thorium bearing brabantite or monazite/brabantite solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Terra, O.; Dacheux, N.; Clavier, N. [Univ Paris 11, IPNO, Grp Radiochim, F-91406 Orsay, (France); Terra, O.; Audubert, F. [CEA Cadarache, DEN/DEC, F-13108 St Paul Les Durance, (France); Dacheux, N.; Clavier, N.; Podor, R. [ICMS UMR 5257, CNRS/CEA/UM2/ENSCM, F-30207 Bagnols Sur Ceze, (France); Podor, R. [Univ Nancy 1, LCSM, F-54506 Vandoeuvre Les Nancy, (France)

    2008-07-01

    The simultaneous incorporation of thorium and uranium(IV) in the rare-earth ortho-phosphates from a mixture of powdered AnO{sub 2}, (NH{sub 4})(H{sub 2}PO{sub 4}), and Ca(HPO{sub 4}).2H{sub 2}O was successfully performed, leading to the formation of single-phase Th-brabantite (Ca{sub 0.5}Th{sub 0.5}PO{sub 4}), U-brabantite (Ca{sub 0.5}U{sub 0.5}PO{sub 4}), and (Th,U)-brabantites (Ca{sub 0.5}Th{sub 0.5-y}U{sub y}PO{sub 4}). The repetition of several cycles composed of a grinding step (30 Hz, 15 min) and of a heat treatment (T=1200 degrees C, 10 h, Ar atmosphere) allowed preparation of single-phase and homogeneous compounds. The complete characterization of the samples by the means of X-Ray powder diffraction, electron probe micro-analyses, and {mu}-Raman spectrometry did not reveal either the presence of minor phases or the partial oxidation of uranium(IV) into uranyl. This study also evidenced the formation of a complete Ca{sub 0.5}Th{sub 0.5-y}U{sub y}PO{sub 4} solid solution with the associated linear decrease of a, b, and c unit cell parameters and beta increase versus the uranium mole loading. Even if the samples were found to be single phase, the significant improvement of the cation distribution in the materials was reached by the mean of the repetition of grinding/heating cycles. The same solid-state process was applied with success to the preparation of homogeneous and single-phase (Th,U)-monazite/brabantite solid solutions with general formula Ln{sub 1-2x}Ca{sub x}Th{sub x-y}U{sub y}PO{sub 4} (with 0.1 {<=} x {<=} 0.4 and y=x/5). (authors)

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

    Science.gov (United States)

    2015-11-13

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

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

    Science.gov (United States)

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

    2017-02-01

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

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

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

    Data.gov (United States)

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

  11. Benchmarking sample preparation/digestion protocols reveals tube-gel being a fast and repeatable method for quantitative proteomics.

    Science.gov (United States)

    Muller, Leslie; Fornecker, Luc; Van Dorsselaer, Alain; Cianférani, Sarah; Carapito, Christine

    2016-12-01

    Sample preparation, typically by in-solution or in-gel approaches, has a strong influence on the accuracy and robustness of quantitative proteomics workflows. The major benefit of in-gel procedures is their compatibility with detergents (such as SDS) for protein solubilization. However, SDS-PAGE is a time-consuming approach. Tube-gel (TG) preparation circumvents this drawback as it involves directly trapping the sample in a polyacrylamide gel matrix without electrophoresis. We report here the first global label-free quantitative comparison between TG, stacking gel (SG), and basic liquid digestion (LD). A series of UPS1 standard mixtures (at 0.5, 1, 2.5, 5, 10, and 25 fmol) were spiked in a complex yeast lysate background. TG preparation allowed more yeast proteins to be identified than did the SG and LD approaches, with mean numbers of 1979, 1788, and 1323 proteins identified, respectively. Furthermore, the TG method proved equivalent to SG and superior to LD in terms of the repeatability of the subsequent experiments, with mean CV for yeast protein label-free quantifications of 7, 9, and 10%. Finally, known variant UPS1 proteins were successfully detected in the TG-prepared sample within a complex background with high sensitivity. All the data from this study are accessible on ProteomeXchange (PXD003841).

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

    Directory of Open Access Journals (Sweden)

    Eve Avel

    2013-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Nomura, Cassiana S. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil); Silva, Cintia S. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil); Nogueira, Ana R.A. [Embrapa Pecuaria Sudeste, CP 339, Sao Carlos, SP 13560-970 (Brazil); Oliveira, Pedro V. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil)]. E-mail: pvolivei@iq.usp.br

    2005-06-30

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 {mu}g of W + 200 {mu}g of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 {mu}g for Cu and 30 {mu}g for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg{sup -} {sup 1} and 128 mg kg{sup -} {sup 1}, respectively. The relative standard deviations were lower

  14. Electrophoretic painting on AZ31 Mg alloy pretreated in cerium conversion coating solutions prepared in ethanol-water mixtures

    Science.gov (United States)

    Van Phuong, Nguyen; Fazal, Basit Raza; Moon, Sungmo

    2017-01-01

    Electrophoretic painting (E-paint) was prepared on AZ31 Mg alloy samples pretreated in cerium conversion coating (CeCC) solutions with various ratios of ethanol and water mixture and its characteristics, adhesion and corrosion resistance were investigated. It was found that CeCC formed on AZ31 Mg alloy in a CeCC solution without ethanol was partly cracked structure and mainly consisted of Mg(OH)2/MgO, which exhibited weak adhesion with E-painting layer after water immersion test, and low corrosion resistance, as indicated by rapid formation of blisters and paint delamination during salt spray test. The addition of ethanol promoted the growth of a fine nano-crystalline CeO2 layer over the entire substrate surface. The E-paint on AZ31 pretreated in the CeCC solutions with addition of ethanol showed also improved corrosion resistance, as represented by the delayed time for paint delamination and blister formation. The E-paint layers on the CeCC layers formed in solutions containing 50-80 vol% ethanol showed stronger adhesion and better corrosion resistance than those formed on the samples treated in a non-ethanol containing CeCC solution.

  15. Preparation of CdTe nanocrystal-polymer composite microspheres in aqueous solution by dispersing method

    Institute of Scientific and Technical Information of China (English)

    LI Minjie; WANG Chunlei; HAN Kun; YANG Bai

    2005-01-01

    Highly fluorescent CdTe nanocrystals were synthesized in aqueous solution, and then processible CdTe nanocrystal-polymer composites were fabricated by coating the aqueous nanocrystals with copolymers of styrene and octadecyl-p-vinyl-benzyldimethylammonium chloride (SOV- DAC) directly. A dichloromethane solution of CdTe nano- crystal-polymer composites was dispersed in the aqueous solution of poly (vinyl alcohol) (PVA) generating highly fluorescent microspheres. Experimental parameters such as the concentration of nanocrystal-polymer composites, the concentration of PVA, and stirring speed which had important effect on the preparation of the microspheres were investigated in detail with fluorescent microscope characterization.

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

    Science.gov (United States)

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

    2015-03-01

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

  17. Preparation of Ultrafine Cobalt Powder by Chemical Reduction in Aqueous Solution

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Nanocrystalline cobalt powders have been prepared from aqueous solution by reducing their corresponding metal salts under suitable conditions. The experimental conditions have been studied in detail. X-ray powder diffraction patterns show that the cobalt powder is hexagonal crystallite. The average particle size of the ultrafine cobalt powder is 55 nm.

  18. Preparation and utilization of wheat straw anionic sorbent for the removal of nitrate from aqueous solution.

    Science.gov (United States)

    Wang, Yu; Gao, Bao-yu; Yue, Wen-wen; Yue, Qin-yan

    2007-01-01

    In order to reduce the impact of eutrophication caused by agricultural residues (i.e., excess nitrate) in aqueous solution, economic and effective anionic sorbents are required. In this article, we prepared anionic sorbent using wheat straw. Its structural characteristics and adsorption properties for nitrate removal from aqueous solution were investigated. The results indicate that the yield of the prepared anionic sorbent, the total exchange capacity, and the maximum adsorption capacity were 350%, 2.57 mEq/g, and 2.08 mmol/g, respectively. The Freundlich isotherm mode is more suitable than the Langmuir mode and the adsorption process accords with the first order reaction kinetic rate equation. When multiple anions (SO4(2-), H2PO4(-), NO3(-), and NO2(-)) were present, the isotherm mode of prepared anionic sorbent for nitrate was consistent with Freundlich mode; however, the capacity of nitrate adsorption was reduced by 50%. In alkaline solutions, about 90% of adsorbed nitrate ions could be desorbed from prepared anionic sorbent. The results of this study confirmed that the wheat straw anionic sorbent can be used as an excellent nitrate sorbent that removes nitrate from aqueous solutions.

  19. Epitaxial ternary nitride thin films prepared by a chemical solution method

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Hongmei [Los Alamos National Laboratory; Feldmann, David M [Los Alamos National Laboratory; Wang, Haiyan [TEXAS A& M; Bi, Zhenxing [TEXAS A& M

    2008-01-01

    It is indispensable to use thin films for many technological applications. This is the first report of epitaxial growth of ternary nitride AMN2 films. Epitaxial tetragonal SrTiN2 films have been successfully prepared by a chemical solution approach, polymer-assisted deposition. The structural, electrical, and optical properties of the films are also investigated.

  20. LiFePO4 doped with magnesium prepared by hydrothermal reaction in glucose solution

    Institute of Scientific and Technical Information of China (English)

    Xiu Qin Ou; Guang Chuan Liang; Jin Sheng Liang; Sheng Zhao Xu; Xia Zhao

    2008-01-01

    Lithium iron phosphate (LiFePO4) doped with magnesium was hydrothermally synthesized from commercial LiOH, FeSO4, H3PO4 and MgSO4 with glucose as carbon precursor in aqueous solution. The samples were characterized by X-ray powder diffraction, scanning electron microscopy and constant charge-discharge cycling. The results show that the synthesized powders have been in situ coated with carbon precursor produced from caramel reaction of glucose. At ambient temperature (28±2℃, the electrochemical performances of LiFePO4 prepared exhibit the high discharge capacity of 135 mAh g(-1) at 5C and good capacity retention of 98% over 90 cycles. The excellent electrochemical performances should be correlated with the intimate contact between carbon and LiFePO4 primary and secondary particles, resulting from the in situ formation of carbon precursor/carbon, leading to the increase in conductivity of LiFePO4.

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

    Science.gov (United States)

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

    2016-02-01

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

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

    Science.gov (United States)

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

    2011-06-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

  4. Investigation of the sample preparation and curing treatment effects on mechanical properties and bioactivity of silica rich metakaolin geopolymer.

    Science.gov (United States)

    Catauro, M; Bollino, F; Papale, F; Lamanna, G

    2014-03-01

    In many biomedical applications both the biological and mechanical behaviours of implants are of relevant interest; in the orthopaedic field, for example, favourable bioactivity and biocompatibility capabilities are necessary, but at the same time the mechanical characteristics of the implants must be such as to allow one to support the body weight. In the present work, the authors have examined the application of geopolymers with composition H24AlK7Si31O79 and ratio Si/Al=31 to be used in biomedical field, considering two different preparation methods: one of the activators (KOH) has been added as pellets in the potassium silicate solution, in the other as a water solution with 8M concentration. Moreover, a different water content was used and only some of the synthesized samples were heat treated. The chemical and microstructural characterizations of those materials have been carried out by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Subsequently, the effects of the adopted preparation on the mechanical and biological properties have been studied: compressive strength tests have demonstrated that more fragile specimens were obtained when KOH was added as a solution. The bioactivity was successfully evaluated with the soaking of the samples in a simulated body fluid (SBF) for 3 weeks. The formation of a layer of hydroxyapatite on the surface of the materials has been shown both by SEM micrographs and EDS analyses.

  5. Preparation of stable aqueous solution of keratins, and physiochemical and biodegradational properties of films.

    Science.gov (United States)

    Yamauchi, K; Yamauchi, A; Kusunoki, T; Kohda, A; Konishi, Y

    1996-08-01

    A stable aqueous solution of reduced keratins was prepared by extracting the proteins from wool (Corriedale) with a mixture of urea, mercaptanol, surfactant, and water at 40-60 degrees C. Sodium dodecyl sulfate was especially effective as a surfactant, not only in promoting extraction but also in stabilizing the aqueous protein solution. The proteins had the following constants: MW, 52,000-69,000 daltons; cysteine content, 8-9 mol%; pl about 6.7. A clear film was readily prepared from a keratin solution containing glycerol. The film was insoluble in water and organic solvents including dimethyl sulfoxide. The keratin film was permeable to glucose, urea, and sodium chloride. The keratin film was degraded in vitro (by trypsin) and in vivo (by subcutaneous embedding in mice).

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

    Science.gov (United States)

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

    2016-08-01

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

  7. Sample contamination with NMP-oxidation products and byproduct-free NMP removal from sample solutions

    Energy Technology Data Exchange (ETDEWEB)

    Cesar Berrueco; Patricia Alvarez; Silvia Venditti; Trevor J. Morgan; Alan A. Herod; Marcos Millan; Rafael Kandiyoti [Imperial College London, London (United Kingdom). Department of Chemical Engineering

    2009-05-15

    1-Methyl-2-pyrrolidinone (NMP) is widely used as a solvent for coal-derived products and as eluent in size exclusion chromatography. It was observed that sample contamination may take place, through reactions of NMP, during extraction under refluxing conditions and during the process of NMP evaporation to concentrate or isolate samples. In this work, product distributions from experiments carried out in contact with air and under a blanket of oxygen-free nitrogen have been compared. Gas chromatography/mass spectrometry (GC-MS) clearly shows that oxidation products form when NMP is heated in the presence of air. Upon further heating, these oxidation products appear to polymerize, forming material with large molecular masses. Potentially severe levels of interference have been encountered in the size exclusion chromatography (SEC) of actual samples. Laser desorption mass spectrometry and SEC agree in showing an upper mass limit of nearly 7000 u for a residue left after distilling 'pure' NMP in contact with air. Furthermore, experiments have shown that these effects could be completely avoided by a strict exclusion of air during the refluxing and evaporation of NMP to dryness. 45 refs., 13 figs.

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

    Science.gov (United States)

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

    2007-10-01

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

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

    Science.gov (United States)

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

    2012-11-01

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

  10. Predictive Sampling of Rare Conformational Events in Aqueous Solution: Designing a Generalized Orthogonal Space Tempering Method.

    Science.gov (United States)

    Lu, Chao; Li, Xubin; Wu, Dongsheng; Zheng, Lianqing; Yang, Wei

    2016-01-12

    In aqueous solution, solute conformational transitions are governed by intimate interplays of the fluctuations of solute-solute, solute-water, and water-water interactions. To promote molecular fluctuations to enhance sampling of essential conformational changes, a common strategy is to construct an expanded Hamiltonian through a series of Hamiltonian perturbations and thereby broaden the distribution of certain interactions of focus. Due to a lack of active sampling of configuration response to Hamiltonian transitions, it is challenging for common expanded Hamiltonian methods to robustly explore solvent mediated rare conformational events. The orthogonal space sampling (OSS) scheme, as exemplified by the orthogonal space random walk and orthogonal space tempering methods, provides a general framework for synchronous acceleration of slow configuration responses. To more effectively sample conformational transitions in aqueous solution, in this work, we devised a generalized orthogonal space tempering (gOST) algorithm. Specifically, in the Hamiltonian perturbation part, a solvent-accessible-surface-area-dependent term is introduced to implicitly perturb near-solute water-water fluctuations; more importantly in the orthogonal space response part, the generalized force order parameter is generalized as a two-dimension order parameter set, in which essential solute-solvent and solute-solute components are separately treated. The gOST algorithm is evaluated through a molecular dynamics simulation study on the explicitly solvated deca-alanine (Ala10) peptide. On the basis of a fully automated sampling protocol, the gOST simulation enabled repetitive folding and unfolding of the solvated peptide within a single continuous trajectory and allowed for detailed constructions of Ala10 folding/unfolding free energy surfaces. The gOST result reveals that solvent cooperative fluctuations play a pivotal role in Ala10 folding/unfolding transitions. In addition, our assessment

  11. SAMPL5: 3D-RISM partition coefficient calculations with partial molar volume corrections and solute conformational sampling

    Science.gov (United States)

    Luchko, Tyler; Blinov, Nikolay; Limon, Garrett C.; Joyce, Kevin P.; Kovalenko, Andriy

    2016-11-01

    Implicit solvent methods for classical molecular modeling are frequently used to provide fast, physics-based hydration free energies of macromolecules. Less commonly considered is the transferability of these methods to other solvents. The Statistical Assessment of Modeling of Proteins and Ligands 5 (SAMPL5) distribution coefficient dataset and the accompanying explicit solvent partition coefficient reference calculations provide a direct test of solvent model transferability. Here we use the 3D reference interaction site model (3D-RISM) statistical-mechanical solvation theory, with a well tested water model and a new united atom cyclohexane model, to calculate partition coefficients for the SAMPL5 dataset. The cyclohexane model performed well in training and testing (R=0.98 for amino acid neutral side chain analogues) but only if a parameterized solvation free energy correction was used. In contrast, the same protocol, using single solute conformations, performed poorly on the SAMPL5 dataset, obtaining R=0.73 compared to the reference partition coefficients, likely due to the much larger solute sizes. Including solute conformational sampling through molecular dynamics coupled with 3D-RISM (MD/3D-RISM) improved agreement with the reference calculation to R=0.93. Since our initial calculations only considered partition coefficients and not distribution coefficients, solute sampling provided little benefit comparing against experiment, where ionized and tautomer states are more important. Applying a simple pK_{ {a}} correction improved agreement with experiment from R=0.54 to R=0.66, despite a small number of outliers. Better agreement is possible by accounting for tautomers and improving the ionization correction.

  12. Copper zinc tin sulfide layers prepared from solution processable metal dithiocarbamate precursors

    Energy Technology Data Exchange (ETDEWEB)

    Edler, Michael [Institute for Chemistry and Technology of Materials, Graz University of Technology, Stremayrgasse 9, 8010 Graz (Austria); Christian Doppler Laboratory for Nanocomposite Solar Cells, Graz University of Technology and NanoTecCenter Weiz, Forschungsgesellschaft mbH (Austria); Rath, Thomas, E-mail: thomas.rath@tugraz.at [Institute for Chemistry and Technology of Materials, Graz University of Technology, Stremayrgasse 9, 8010 Graz (Austria); Christian Doppler Laboratory for Nanocomposite Solar Cells, Graz University of Technology and NanoTecCenter Weiz, Forschungsgesellschaft mbH (Austria); Schenk, Alexander [Institute for Chemistry and Technology of Materials, Graz University of Technology, Stremayrgasse 9, 8010 Graz (Austria); Fischereder, Achim [Institute for Chemistry and Technology of Materials, Graz University of Technology, Stremayrgasse 9, 8010 Graz (Austria); Christian Doppler Laboratory for Nanocomposite Solar Cells, Graz University of Technology and NanoTecCenter Weiz, Forschungsgesellschaft mbH (Austria); Haas, Wernfried [Christian Doppler Laboratory for Nanocomposite Solar Cells, Graz University of Technology and NanoTecCenter Weiz, Forschungsgesellschaft mbH (Austria); Institute for Electron Microscopy and Fine Structure Research, Graz University of Technology, Steyrergasse 17, 8010 Graz (Austria); Edler, Matthias [Chair of Chemistry of Polymeric Materials, University of Leoben, Otto Gloeckel-Strasse 2, 8700 Leoben (Austria); Chernev, Boril [Institute for Electron Microscopy and Fine Structure Research, Graz University of Technology, Steyrergasse 17, 8010 Graz (Austria); Kunert, Birgit [Institute of Solid State Physics, Graz University of Technology, Petersgasse 16, 8010 Graz (Austria); Hofer, Ferdinand [Institute for Electron Microscopy and Fine Structure Research, Graz University of Technology, Steyrergasse 17, 8010 Graz (Austria); and others

    2012-10-15

    In this contribution we present a solution based route toward copper zinc tin sulfide - CZTS - layers using metal dithiocarbamate precursors. We focus on the synthesis of the precursor materials as well as on the fabrication of thin CZTS layers at low temperatures of 350 Degree-Sign C and their characterization. Powder X-ray diffraction measurements show that a precursor solution containing an excess of the zinc precursor, compared to the Cu and Sn precursors, has to be used to obtain CZTS films without secondary phases. Thus, the prepared films are Zn-rich, which is beneficial for solar cell applications. Raman as well as X-ray photoelectron spectroscopy studies confirm the formation of CTZS. No clear evidence for free ZnS has been found. Electron microscopy shows agglomerates of 10 nm-sized crystallites forming spherical particles with a diameter between 50 nm and 400 nm. The prepared films possess high optical absorption (>1.10{sup 4} cm{sup -1}) and an optical band gap of approximately 1.6 eV. Highlights: Black-Right-Pointing-Pointer CZTS layers are prepared from metal dithiocarbamate precursor solu-tions. Black-Right-Pointing-Pointer No additional sulfur sources or capping agents are necessary. Black-Right-Pointing-Pointer Prepared CZTS layers are zinc rich. Black-Right-Pointing-Pointer CZTS layers show a high absorption coefficient and a band gap of 1.6 eV.

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

    DEFF Research Database (Denmark)

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

    2015-01-01

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

  14. 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.

  15. Stoichiometry-controlled high-performance LiCoO 2 electrode materials prepared by a spray solution technique

    Science.gov (United States)

    Konstantinov, K.; Wang, G. X.; Yao, J.; Liu, H. K.; Dou, S. X.

    LiCoO 2 cathode materials have been prepared by a spray-drying technique. The stoichiometry of the materials, their morphology, and the phase composition and electrochemical performance have been studied. The effects of thermal annealing and decomposition processes on the structure are discussed in detail. The changes of Li content in materials were monitored by ICP spectrometry. It was established that the decomposition of the acetates at around 450 °C is a slurry-making process that compacts the powder. It was found that well lithiated samples with good life cycle and high capacity can be prepared using acetate precursors and a spray solution technique. The morphology, grain size and texturing can be controlled by the sintering time and temperature in combination with intermediate grinding.

  16. Optimizing Frozen Sample Preparation for Laser Microdissection: Assessment of CryoJane Tape-Transfer System®.

    Directory of Open Access Journals (Sweden)

    Yelena G Golubeva

    Full Text Available Laser microdissection is an invaluable tool in medical research that facilitates collecting specific cell populations for molecular analysis. Diversity of research targets (e.g., cancerous and precancerous lesions in clinical and animal research, cell pellets, rodent embryos, etc. and varied scientific objectives, however, present challenges toward establishing standard laser microdissection protocols. Sample preparation is crucial for quality RNA, DNA and protein retrieval, where it often determines the feasibility of a laser microdissection project. The majority of microdissection studies in clinical and animal model research are conducted on frozen tissues containing native nucleic acids, unmodified by fixation. However, the variable morphological quality of frozen sections from tissues containing fat, collagen or delicate cell structures can limit or prevent successful harvest of the desired cell population via laser dissection. The CryoJane Tape-Transfer System®, a commercial device that improves cryosectioning outcomes on glass slides has been reported superior for slide preparation and isolation of high quality osteocyte RNA (frozen bone during laser dissection. Considering the reported advantages of CryoJane for laser dissection on glass slides, we asked whether the system could also work with the plastic membrane slides used by UV laser based microdissection instruments, as these are better suited for collection of larger target areas. In an attempt to optimize laser microdissection slide preparation for tissues of different RNA stability and cryosectioning difficulty, we evaluated the CryoJane system for use with both glass (laser capture microdissection and membrane (laser cutting microdissection slides. We have established a sample preparation protocol for glass and membrane slides including manual coating of membrane slides with CryoJane solutions, cryosectioning, slide staining and dissection procedure, lysis and RNA extraction

  17. Development of the Dried Spot Sample Preparation Methodology and Applications to XRMF Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Colletti, Lisa P.; Havrilla, George J.

    1997-12-31

    The dried spot method has significant potential for trace elemental analysis using x-ray fluorescence. Small sample size coupled with spatially resolved excitation offers increased sensitivity for aqueous solutions. The primary limitation in applying this method to routine analyses is that much of the method development and fundamental aspects have not been investigated. We have studied the effects of a number of parameters on the quantitative capabilities of the dried spot method. These include thin-film substrates, drying methods, and solution composition. The small sample size offers opportunities for the analysis of a wide array of sample types including highly radioactive specimens.

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

    Science.gov (United States)

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

    2017-01-01

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

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

    DEFF Research Database (Denmark)

    Skov, Kasper; Hadrup, Niels; Smedsgaard, Jørn

    2015-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    王兴无

    2015-01-01

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

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

    Science.gov (United States)

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

    2016-03-01

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

  2. [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.

  3. Low temperature preparation of nanocrystalline solid solution of strontium barium niobate by chemical process

    Indian Academy of Sciences (India)

    Asit B Panda; Amita Pathak; Panchanan Pramanik

    2002-11-01

    SrBa1–Nb2O6 (with = 0.4, 0.5 and 0.6) powders have been prepared by thermolysis of aqueous precursor solutions consisting of triethanolamine (TEA), niobium tartarate and, EDTA complexes of strontium and barium ions. Complete evaporation of the precursor solution by heating at ∼ 200°C, yields in a fluffy, mesoporous carbon rich precursor material, which on calcination at 750°C/2 h has resulted in the pure SBN powders. The crystallite and average particle sizes are found to be around 15 nm and 20 nm, respectively.

  4. Aqueous Solution Preparation of Ruthenium Nanoparticles Using Ammonium Formate as the Reducing Agent

    Institute of Scientific and Technical Information of China (English)

    LIU Shaohong; CHEN Jialin; GUAN Weiming; BI Jun; CHEN Nanguang; CHEN Dengquan; LIU Manmen; SUN Xudong

    2012-01-01

    Ruthenium,one of the platinum group metals,has drawn much attention due to its catalytic behavior,hardness,electrical conductivity and density.Ruthenium particles are usually prepared on a small scale by the polyol process,however,the size of the obtained ruthenium nanoparticles is most below 10 nm.In this work,ruthenium particles about 200 nm in diameter were obtained in aqueous solution by using ammonium formate as the reducing agent.Tohave a better control of particle's size and shape,the effects of PVP,mixing mode,reaction temperature,solution pH and calcination temperature were investigated.

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

    DEFF Research Database (Denmark)

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

    2017-01-01

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

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

    DEFF Research Database (Denmark)

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

    2015-01-01

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

  7. Characteristics of zinc oxide nanorod array/titanium oxide film heterojunction prepared by aqueous solution deposition

    Science.gov (United States)

    Lee, Ming-Kwei; Hong, Min-Hsuan; Li, Bo-Wei

    2016-07-01

    The characteristics of a ZnO nanorod array/TiO2 film heterojunction were investigated. A TiO2 film was prepared on glass by aqueous solution deposition with precursors of ammonium hexafluorotitanate and boric acid at 40 °C. Then, a ZnO seed layer was prepared on a TiO2 film/glass substrate by RF sputtering. A vertically oriented ZnO nanorod array was grown on a ZnO seed layer/TiO2 film/glass substrate by aqueous solution deposition with precursors of zinc nitrate and hexamethylenetetramine (HMT) at 70 °C. After thermal annealing in N2O ambient at 300 °C, this heterojunction used as an oxygen gas sensor shows much better rise time, decay time, and on/off current ratio than as-grown and annealed ZnO nanorods.

  8. Preparation of activated carbons from Iris tectorum employing ferric nitrate as dopant for removal of tetracycline from aqueous solutions.

    Science.gov (United States)

    Li, Gang; Zhang, Dongsheng; Wang, Man; Huang, Ji; Huang, Lihui

    2013-12-01

    Ferric nitrate was employed to modify activated carbon prepared from Iris tectorum during H₃PO₄ activation and ability of prepared activated carbon for removal of tetracycline (TC) was investigated. The properties of the activated carbon samples with or without ferric nitrate, ITAC-Fe and ITAC, were measured by scanning electron microscopy (SEM), N₂ adsorption/desorption isotherms, Fourier transform infrared spectroscopy (FTIR) and Boehm's titration. The results showed that mixing with iron increased the BET surface area, total pore volume and the adsorption capacity as compared to the original carbon. FTIR and Boehm's titration suggested that ITAC-Fe was characteristic of more acidic functional groups than ITAC. Adsorption of TC on both samples exhibited a strong pH-dependent behavior and adsorption capacity reduced rapidly with the increasing solution pH. The adsorption kinetics agreed well with the pseudo-second-order model and the adsorption isotherms data were well described by Langmuir model with the maximum adsorption capacity of 625.022 mg/g for ITAC and 769.231 mg/g for ITAC-Fe. The present work suggested that ITAC-Fe could be used to remove tetracycline effectively from aqueous solutions.

  9. 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.

  10. Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

    Science.gov (United States)

    Kaltenbach, Angela; Noordmann, Janine; Görlitz, Volker; Pape, Carola; Richter, Silke; Kipphardt, Heinrich; Kopp, Gernot; Jährling, Reinhard; Rienitz, Olaf; Güttler, Bernd

    2015-04-01

    Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

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

    Science.gov (United States)

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

    2012-01-01

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

  12. The beauty of being (label)-free: sample preparation methods for SWATH-MS and next-generation targeted proteomics

    Science.gov (United States)

    Campbell, Kate; Deery, Michael J.; Lilley, Kathryn S.; Ralser, Markus

    2014-01-01

    The combination of qualitative analysis with label-free quantification has greatly facilitated the throughput and flexibility of novel proteomic techniques. However, such methods rely heavily on robust and reproducible sample preparation procedures. Here, we benchmark a selection of in gel, on filter, and in solution digestion workflows for their application in label-free proteomics. Each procedure was associated with differing advantages and disadvantages. The in gel methods interrogated were cost effective, but were limited in throughput and digest efficiency. Filter-aided sample preparations facilitated reasonable processing times and yielded a balanced representation of membrane proteins, but led to a high signal variation in quantification experiments. Two in solution digest protocols, however, gave optimal performance for label-free proteomics. A protocol based on the detergent RapiGest led to the highest number of detected proteins at second-best signal stability, while a protocol based on acetonitrile-digestion, RapidACN, scored best in throughput and signal stability but came second in protein identification. In addition, we compared label-free data dependent (DDA) and data independent (SWATH) acquisition on a TripleTOF 5600 instrument. While largely similar in protein detection, SWATH outperformed DDA in quantification, reducing signal variation and markedly increasing the number of precisely quantified peptides. PMID:24741437

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

    Science.gov (United States)

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

    2010-01-01

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

  14. Surface and Texture Properties of Tb-Doped Ceria-Zirconia Solid Solution Prepared by Sol-Gel Method

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The three-way catalysts (TWCs) promoters Ce0.6Zr0.4-xTbxO2-y were prepared by sol-gel method. BET surface areas analysis indicated that an increase of the dopant Tb content from x=0.05 to x=0.15 favors an increase of surface area from 66.8 to 80.4 m2·g-1 compared with the undoped sample Ce0.60Zr0.40O2 65.1 m2·g-1 after calcination at 650 ℃. Transmission electron microscopy (TEM) observation indicated that the doped samples have a higher thermal stability. The XRD and Raman spectra confirmed that the Ce0.6Zr0.4-xTbxO2-y cubic solid solution is formed. XPS analysis revealed that Ce and Tb mainly existed in the form of Ce4+ and Tb3+, and Zr existed in the form of Zr4+ on the surface of the samples. The doped samples were homogenous in composition;the introduction of Tb into the CeO2-ZrO2 promoters resulted in the formation of a solid solution, and the concentration of surface lattice oxygen was increased.

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

    DEFF Research Database (Denmark)

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

    2012-01-01

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

  16. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-25

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

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

    Science.gov (United States)

    McCubbin, Francis M.

    2017-01-01

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

  19. Controlling sources of preanalytical variability in doping samples: challenges and solutions.

    Science.gov (United States)

    Lippi, Giuseppe; Mattiuzzi, Camilla; Banfi, Giuseppe

    2013-06-01

    The use of illicit substances and methods contravenes the ethics of sports and may be associated with side effects. Antidoping testing is an essential tool for preventing or limiting the consequences of cheating in sports. As for conventional laboratory testing, major emphasis has been placed on analytical quality, overlooking the inherent risks that may arise from analysis of unsuitable doping samples. The adherence to scrupulous criteria for collection, handling, transportation and storage of samples, especially blood and urine samples, is essential. The leading preanalytical variables that influence doping sample quality include biological variability, sample collection, venous stasis, spurious hemolysis and presence of other interfering substances, sample manipulation and degradation, and inappropriate conditions for transportation and storage. This article provides a personal overview about the current challenges in preanalytical management of doping samples, as well as potential solutions for preventing the negative impact of preanalytical variables on sample quality and test results.

  20. Preparation of Laminin-apatite-polymer Composites Using Metastable Calcium Phosphate Solutions

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    A synthetic polymer with a laminin-apatite composite layer on its surface would be useful as a percutaneous device. The preparation of such a composite was attempted in the present study using poly ( ethylene terephthalate ) (PET) and polyethylene ( PE ) as the synthetic polymer. PET and PE plates and those pretreated with an oxygen plasma were alternately dipped in calcium and phosphate ion solutions, and then immersed in a metastable ealcium phosphate solution supplemented with laminin ( LCP solution ). The PET and PE plates pretreated with an oxygen plasma formed a uniform and continuous layer of a laminin- apatite composite on their surfaces. In contrast, the PET and PE plates that had not been pretreated with an oxygen plasma did not form a continuous layer of a laminin-apatite composite on their surfaces. The hydrophilic functional groups on the PET and PE surfaces introduced by the plasma treatment were responsible for the successful laminin-apatite composite coating.

  1. Factors influencing HPAM solution viscosity prepared by produced water using orthogonal method

    Institute of Scientific and Technical Information of China (English)

    康万利; 王志伟; 周阳; 孟令伟; 刘述忍; 白宝君

    2008-01-01

    The effect of temperature and metal ion components on the viscosity of HPAM solution was studied by means of orthogonal method.Five factors and 4 levels were considered for the orthogonal design.The five factors included temperature,contents of Na+,Mg2+,Ca2+ and S2-,and the four levels mainly considered the level of produced water components in main oilfields in China.The experiment results show that temperature is the most important factor to control HPAM solution viscosity prepared by produced water.The effect of ions was in order of Na+>S2->Mg2+>Ca2+.The mechanism of each factor influencing viscosity was also discussed.Based on the actual condition of Nanyang oilfield,the desulfurization was used to improve the solution viscosity,and satisfactory result was obtained.

  2. Media-fill simulation tests in manual and robotic aseptic preparation of injection solutions in syringes.

    Science.gov (United States)

    Krämer, Irene; Federici, Matteo; Kaiser, Vanessa; Thiesen, Judith

    2016-04-01

    The purpose of this study was to evaluate the contamination rate of media-fill products either prepared automated with a robotic system (APOTECAchemo™) or prepared manually at cytotoxic workbenches in the same cleanroom environment and by experienced operators. Media fills were completed by microbiological environmental control in the critical zones and used to validate the cleaning and disinfection procedures of the robotic system. The aseptic preparation of patient individual ready-to-use injection solutions was simulated by using double concentrated tryptic soy broth as growth medium, water for injection and plastic syringes as primary packaging materials. Media fills were either prepared automated (500 units) in the robot or manually (500 units) in cytotoxic workbenches in the same cleanroom over a period of 18 working days. The test solutions were incubated at room temperature (22℃) over 4 weeks. Products were visually inspected for turbidity after a 2-week and 4-week period. Following incubation, growth promotion tests were performed with Staphylococcus epidermidis. During the media-fill procedures, passive air monitoring was performed with settle plates and surface monitoring with contact plates on predefined locations as well as fingerprints. The plates got incubated for 5-7 days at room temperature, followed by 2-3 days at 30-35℃ and the colony forming units (cfu) counted after both periods. The robot was cleaned and disinfected according to the established standard operating procedure on two working days prior to the media-fill session, while on six other working days only six critical components were sanitized at the end of the media-fill sessions. Every day UV irradiation was operated for 4 h after finishing work. None of the 1000 media-fill products prepared in the two different settings showed turbidity after the incubation period thereby indicating no contamination with microorganisms. All products remained uniform, clear, and light

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

    Science.gov (United States)

    Yamazaki, Taichi; Nakamura, Satoe; Saito, Takeshi

    2017-04-01

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

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

    Science.gov (United States)

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

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

    NARCIS (Netherlands)

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

    2013-01-01

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

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

    NARCIS (Netherlands)

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

    2013-01-01

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

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

    DEFF Research Database (Denmark)

    Alimadadi, Hossein; Pantleon, Karen

    2009-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Paul M. Pellegrino

    2013-05-01

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

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

    Science.gov (United States)

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

    2017-08-16

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

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

    Science.gov (United States)

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

    2012-01-01

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

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

    NARCIS (Netherlands)

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

    2013-01-01

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

  12. Sample preparation followed by HPLC under harmless 100% aqueous conditions for determination of oxytetracycline in milk and eggs.

    Science.gov (United States)

    Furusawa, Naoto

    2004-05-01

    A simple and hazardous chemical-free method for the high-performance liquid chromatographic determination of oxytetracycline (OTC) residues in milk and eggs has been developed. Sample preparation consists in homogenization with an aqueous solution by means of a handheld ultrasonic homogenizer followed by centrifugal ultrafiltration. HPLC is performed with an isocratic aqueous mobile phase and a photodiode array detector. Average recoveries of OTC (0.05, 0.1, and 0.2 microg mL(-1) for milk; 0.1, 0.2, and 0.4 microg mL(-1) for eggs) were > or =84% with relative standard deviations of < or =2.3%. The total time required for the analysis of one sample and LOQs were <30 min and <0.1 microg mL(-1), respectively. In all the processes, no organic solvents or hazardous reagents were used.

  13. Quantitative study on exact reconstruction sampling condition by verifying solution uniqueness in limited-view CT.

    Science.gov (United States)

    Yan, Bin; Zhang, Wenkun; Li, Lei; Zhang, Hanming; Wang, Linyuan

    2016-10-01

    In limited-view computed tomography reconstruction, iterative image reconstruction with sparsity-exploiting methods, such as total variation (TV) minimization, inspired by compressive sensing, potentially claims large reductions in sampling requirements. However, a quantitative notion of this claim is non-trivial because of the ill-defined reduction in sampling achieved by the sparsity-exploiting method. In this paper, exact reconstruction sampling condition for limited-view problem is studied by verifying the uniqueness of solution in TV minimization model. Uniqueness is tested by solving a convex optimization problem derived from the sufficient and necessary condition of solution uniqueness. Through this method, the sufficient sampling number of exact reconstruction is quantified for any fixed phantom and settled geometrical parameter in the limited-view problem. This paper provides a reference to quantify the sampling condition. Three phantoms are tested to study the sampling condition of limited view exact reconstruction in this paper. The experiment results show the quantified sampling number and indicate that an object would be accurately reconstructed as the scanning range becomes narrower by increasing sampling number. The increased samplings compensate for the deficiency of the projection angle. However, the lower bound of the scanning range corresponding to three different phantoms are presented, in which an exact reconstruction cannot be obtained once the projection angular is narrowed to this extent no matter how to increase sampling.

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

    Science.gov (United States)

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

    2011-01-01

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

  15. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

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

    Science.gov (United States)

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

    2013-02-01

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

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

    Science.gov (United States)

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

    2016-03-01

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

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

    Science.gov (United States)

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

    2012-09-10

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

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

    KAUST Repository

    Xue, Zheng

    2014-07-15

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

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

    Science.gov (United States)

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

    2014-01-01

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

  2. Investigation of the sample preparation and curing treatment effects on mechanical properties and bioactivity of silica rich metakaolin geopolymer

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, M., E-mail: michelina.catauro@unina2.it; Bollino, F.; Papale, F.; Lamanna, G.

    2014-03-01

    In many biomedical applications both the biological and mechanical behaviours of implants are of relevant interest; in the orthopaedic field, for example, favourable bioactivity and biocompatibility capabilities are necessary, but at the same time the mechanical characteristics of the implants must be such as to allow one to support the body weight. In the present work, the authors have examined the application of geopolymers with composition H{sub 24}AlK{sub 7}Si{sub 31}O{sub 79} and ratio Si/Al = 31 to be used in biomedical field, considering two different preparation methods: one of the activators (KOH) has been added as pellets in the potassium silicate solution, in the other as a water solution with 8 M concentration. Moreover, a different water content was used and only some of the synthesized samples were heat treated. The chemical and microstructural characterizations of those materials have been carried out by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Subsequently, the effects of the adopted preparation on the mechanical and biological properties have been studied: compressive strength tests have demonstrated that more fragile specimens were obtained when KOH was added as a solution. The bioactivity was successfully evaluated with the soaking of the samples in a simulated body fluid (SBF) for 3 weeks. The formation of a layer of hydroxyapatite on the surface of the materials has been shown both by SEM micrographs and EDS analyses. - Highlights: • Rich metakaolin geopolymer activated with KOH/K{sub 2}SiO{sub 3} and thermal treatment • Mechanical and bioactivity test to evaluate consolidation and bone bonding ability • Order of addition of reactants and thermal treatment influence mechanical properties.

  3. Anisotropic surface hole-transport property of triphenylamine-derivative single crystal prepared by solution method

    Science.gov (United States)

    Umeda, Minoru; Katagiri, Mitsuhiko; Shironita, Sayoko; Nagayama, Norio

    2016-12-01

    This paper reports the anisotropic hole transport at the triphenylamine-derivative single crystal surface prepared by a solution method. Triphenylamine derivatives are commonly used in a hole-transport material for organic photoconductors of laser-beam printers, in which the materials are used as an amorphous form. For developing organic photovoltaics using the photoconductor's technology, preparation of a single crystal seems to be a specific way by realizing the high mobility of an organic semiconductor. In this study, a single crystal of 4-(2,2-diphenylethenyl)-N,N-bis(4-methylphenyl)-benzenamine (TPA) was prepared and its anisotropic hole-transport property measured. First, the hole-transport property of the TPA was investigated based on its chemical structure and electrochemical redox characteristics. Next, a large-scale single crystal formation at a high rate was developed by employing a solution method based on its solubility and supersolubility curves. The grown TPA was found to be a single crystal based on the polarization micrograph observation and crystallographic analysis. For the TPA single crystal, an anisotropic surface conduction was found, which was well explained by its molecular stack structure. The measured current in the long-axis direction is one order of magnitude greater than that of amorphous TPA.

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

    Science.gov (United States)

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

    2008-01-15

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

  5. Studies on adsorption of mercury from aqueous solution on activated carbons prepared from walnut shell.

    Science.gov (United States)

    Zabihi, M; Haghighi Asl, A; Ahmadpour, A

    2010-02-15

    The adsorption ability of a powdered activated carbons (PAC) derived from walnut shell was investigated in an attempt to produce more economic and effective sorbents for the control of Hg(II) ion from industrial liquid streams. Carbonaceous sorbents derived from local walnut shell, were prepared by chemical activation methods using ZnCl(2) as activating reagents. Adsorption of Hg(II) from aqueous solutions was carried out under different experimental conditions by varying treatment time, metal ion concentration, pH and solution temperature. It was shown that Hg(II) uptake decreases with increasing pH of the solution. The proper choice of preparation conditions were resulted in microporous activated carbons with different BET surface areas of 780 (Carbon A, 1:0.5 ZnCl(2)) and 803 (Carbon B, 1:1 ZnCl(2))m(2)/g BET surface area. The monolayer adsorption capacity of these particular adsorbents were obtained as 151.5 and 100.9 mg/g for carbons A and B, respectively. It was determined that Hg(II) adsorption follows both Langmuir and Freundlich isotherms as well as pseudo-second-order kinetics.

  6. Preparation and characterization of regenerated fiber from the aqueous solution of Bombyx mori cocoon silk fibroin

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Zhenghua [Department of Biotechnology, Tokyo University of Agriculture and Technology, Koganei, Tokyo 184-8588 (Japan); Department of Application Engineering, ZheJiang Vocational College of Economic and Trade, HangZhou, ZheJiang 310018 (China); Imada, Takuzo [Department of Biotechnology, Tokyo University of Agriculture and Technology, Koganei, Tokyo 184-8588 (Japan); Asakura, Tetsuo, E-mail: asakura@cc.tuat.ac.jp [Department of Biotechnology, Tokyo University of Agriculture and Technology, Koganei, Tokyo 184-8588 (Japan)

    2009-10-15

    The regenerated silk fibers with high strength and high biodegradability were prepared from the aqueous solution of Bombyx mori silk fibroin from cocoons with wet spinning method. Although the tensile strength of the regenerated silk fibroin fiber, 210 MPa is still half of the strength of native silk fiber, the diameter of the fiber is about 100 {mu}m which is suitable for monofilament of suture together with high biodegradability. The high concentration (30%, w/v) of the aqueous solution of the silk fibroin which corresponds to the high concentration in the middle silkgland of silkworm was obtained. This was performed by adjusting the pH of the aqueous solution to 10.4 which corresponds to pK{sub a} value of the OH group of Tyr residues in the silk fibroin. The mixed solvent, methanol/acetic acid (7:3 in volume ratio) was used as coagulant solvent for preparing the regenerated fiber. The structural change of silk fibroin fiber by stretching was monitored with both {sup 13}C solid state NMR and X-ray diffraction methods, indicating that the high strength of the fiber is related with the long-range orientation of the silk fibroin chain with {beta}-sheet structure.

  7. Synthesis and characterization of quaternized bacterial cellulose prepared in homogeneous aqueous solution.

    Science.gov (United States)

    Zhang, Hairong; Guo, Haijun; Wang, Bo; Shi, Silan; Xiong, Lian; Chen, Xinde

    2016-01-20

    In this work, bacterial cellulose (BC) was activated by ethylenediamine (EDA) and then dissolved in lithium chloride/N,N-dimethylacetamide (LiCl/DMAc) aqueous solutions. The resulting transparent solution was cast on a glass plate to prepare regenerated BC. Then cationic BC was prepared homogeneously by the reaction between regenerated BC and 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTAC) in a NaOH/urea aqueous solution. Structure and properties of the BC and its products were characterized by different techniques such as X-ray diffraction (XRD), Fourier transform spectroscopy (FT-IR), scanning electron microscopy (SEM) and thermo-gravimetric analysis (TGA). The results showed that there was no significant difference between the structures of BC, activated BC and regenerated BC. The effects of different temperature and molar ratio of CHPTAC to anhydroglucose unit (AGU) on the degree of substitution (DS) value were examined. The DS values of cationic BC ranged between 0.21 and 0.51.

  8. In situ sampling of small volumes of soil solution using modified micro-suction cups

    NARCIS (Netherlands)

    Shen, Jianbo; Hoffland, E.

    2007-01-01

    Two modified designs of micro-pore-water samplers were tested for their capacity to collect unbiased soil solution samples containing zinc and citrate. The samplers had either ceramic or polyethersulfone (PES) suction cups. Laboratory tests of the micro-samplers were conducted using (a) standard sol

  9. 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.

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

    Science.gov (United States)

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

    2017-05-15

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

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

    Science.gov (United States)

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

    2012-07-01

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

  12. PREPARATION OF POLY(METHYL METHACRYLATE)/LAYERED DOUBLE HYDROXIDES NANOCOMPOSITES via in situ SOLUTION POLYMERIZATION

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    An exfoliated layered double hydroxides/poly(methyl methacrylate) (LDHs/PMMA) nanocomposite was prepared by in situ solution polymerization of methyl methacrylate (MMA) in the presence of 4-vinylbenzenesulfonate intercalated LDHs(MgAl-VBS LDHs). MgAl-VBS LDHs was prepared by the ion exchange method, and the structure and composition of the MgAl-VBS LDHs were determined by X-ray diffraction (XRD), infrared spectroscopy and elemental analysis. XRD and transmission electron microscopy (TEM) were employed to examine the structure of LDHs/PMMA nanocomposite. It was indicated that the LDHs layers were well exfoliated and dispersed in the PMMA matrix. The grafting of PMMA onto LDHs was confirmed by the extraction result and the weight fraction of grafted PMMA increased as the weight fraction of LDHs in the nanocomposites increased.

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

    Science.gov (United States)

    Wahba, Adel Maher; Mohamed, Mohamed Bakr

    2017-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-01-15

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

  15. Effect of Soft-annealing on the Properties of CIGSe Thin Films Prepared from Solution Precursors

    Energy Technology Data Exchange (ETDEWEB)

    Sung, Shijoon; Park, Misun; Kim, Daehwan; Kang, Jinkyu [Daegu Gyeongbuk Institute of Science and Technology, Daegu (Korea, Republic of)

    2013-05-15

    Solution-based deposition of CuIn{sub x}Ga{sub 1-x}Se{sub 2} (CIGSe) thin films is well known non-vacuum process for the fabrication of CIGSe solar cells. However, due to the usage of organic chemicals in the preparation of CIG precursor solutions, the crystallization of the polycrystalline CIGSe and the performance of CIGSe thin film solar cells were significantly affected by the carbon residues from the organic chemicals. In this work, we have tried to eliminate the carbon residues in the CIG precursor thin films efficiently by using soft-annealing process. By adjusting soft-annealing temperature, it is possible to control the amount of carbon residues in CIG precursor thin films. The reduction of the carbon residues in CIG precursors by high temperature soft-annealing improves the grain size and morphology of polycrystalline CIGSe thin films, which are also closely related with the electrical properties of CIGSe thin film solar cells.

  16. Preparation, Characterization and Catalytic Performance of Nanometer Ceria-Zirconia Solid Solution

    Institute of Scientific and Technical Information of China (English)

    Hu Yucai; Wang Yinghui; Pan Junyan

    2004-01-01

    Ce0.6Zr0.4O2 solid solution was prepared by co-precipitation technique using hydrazine hydrate as precipitator.Various physico-chemical techniques such as XRD, FT-Raman, SEM, TEM, etc.were used to characterize the resultant powder.Meanwhile, its catalytic activity was evaluated in the synthesis of n-butyl acetate by the reaction of acetic acid and n-butyl alcohol.The results show that ceria-zirconia solid solution forms single cubic structure and its particle diameter is less than 100 nm.As a sort of solid acid, it possesses high catalytic activity and can be easily separated from reaction liquid.After it is used for ten times, its activity basically kees unchanging.

  17. High Throughput Sample Preparation and Analysis for DNA Sequencing, PCR and Combinatorial Screening of Catalysis Based on Capillary Array Technique

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yonghua [Iowa State Univ., Ames, IA (United States)

    2000-01-01

    Sample preparation has been one of the major bottlenecks for many high throughput analyses. The purpose of this research was to develop new sample preparation and integration approach for DNA sequencing, PCR based DNA analysis and combinatorial screening of homogeneous catalysis based on multiplexed capillary electrophoresis with laser induced fluorescence or imaging UV absorption detection. The author first introduced a method to integrate the front-end tasks to DNA capillary-array sequencers. protocols for directly sequencing the plasmids from a single bacterial colony in fused-silica capillaries were developed. After the colony was picked, lysis was accomplished in situ in the plastic sample tube using either a thermocycler or heating block. Upon heating, the plasmids were released while chromsomal DNA and membrane proteins were denatured and precipitated to the bottom of the tube. After adding enzyme and Sanger reagents, the resulting solution was aspirated into the reaction capillaries by a syringe pump, and cycle sequencing was initiated. No deleterious effect upon the reaction efficiency, the on-line purification system, or the capillary electrophoresis separation was observed, even though the crude lysate was used as the template. Multiplexed on-line DNA sequencing data from 8 parallel channels allowed base calling up to 620 bp with an accuracy of 98%. The entire system can be automatically regenerated for repeated operation. For PCR based DNA analysis, they demonstrated that capillary electrophoresis with UV detection can be used for DNA analysis starting from clinical sample without purification. After PCR reaction using cheek cell, blood or HIV-1 gag DNA, the reaction mixtures was injected into the capillary either on-line or off-line by base stacking. The protocol was also applied to capillary array electrophoresis. The use of cheaper detection, and the elimination of purification of DNA sample before or after PCR reaction, will make this approach an

  18. High Throughput Sample Preparation and Analysis for DNA Sequencing, PCR and Combinatorial Screening of Catalysis Based on Capillary Array Technique

    Energy Technology Data Exchange (ETDEWEB)

    Yonghua Zhang

    2002-05-27

    Sample preparation has been one of the major bottlenecks for many high throughput analyses. The purpose of this research was to develop new sample preparation and integration approach for DNA sequencing, PCR based DNA analysis and combinatorial screening of homogeneous catalysis based on multiplexed capillary electrophoresis with laser induced fluorescence or imaging UV absorption detection. The author first introduced a method to integrate the front-end tasks to DNA capillary-array sequencers. protocols for directly sequencing the plasmids from a single bacterial colony in fused-silica capillaries were developed. After the colony was picked, lysis was accomplished in situ in the plastic sample tube using either a thermocycler or heating block. Upon heating, the plasmids were released while chromsomal DNA and membrane proteins were denatured and precipitated to the bottom of the tube. After adding enzyme and Sanger reagents, the resulting solution was aspirated into the reaction capillaries by a syringe pump, and cycle sequencing was initiated. No deleterious effect upon the reaction efficiency, the on-line purification system, or the capillary electrophoresis separation was observed, even though the crude lysate was used as the template. Multiplexed on-line DNA sequencing data from 8 parallel channels allowed base calling up to 620 bp with an accuracy of 98%. The entire system can be automatically regenerated for repeated operation. For PCR based DNA analysis, they demonstrated that capillary electrophoresis with UV detection can be used for DNA analysis starting from clinical sample without purification. After PCR reaction using cheek cell, blood or HIV-1 gag DNA, the reaction mixtures was injected into the capillary either on-line or off-line by base stacking. The protocol was also applied to capillary array electrophoresis. The use of cheaper detection, and the elimination of purification of DNA sample before or after PCR reaction, will make this approach an

  19. SANS studies of solutions and molecular composites prepared from cellulose tricarbanilate

    CERN Document Server

    Alava, C; Cameron, J D; Cowie, J M G; Vaqueiro, P; Möller, A; Triolo, A

    2002-01-01

    We report on SANS measurements carried out on the instrument SANS1 (V4) at the BENSC facility on solutions and composites of cellulose tricarbanilate (CTC). This cellulose derivative exhibits lyotropic behaviour in methylacrylate (MA). The SANS data indicate that in the isotropic liquid state (up to 25% wt CTC in MA) the CTC chains behave like rods of mass per unit length (M/L). In the liquid crystalline (LC) phase (at and above 35% wt CTC in MA), the Q dependence varies from Q sup - sup 1 to Q sup - sup 4 , probably as a result of self-assembling of the CTC chains. The general aim of our work is to prepare molecular composites, i.e. miscible blends of rigid-rod and flexible-coil polymers, from CTC solutions in polymerizable media. To establish the degree of homogeneity of the composites, we performed SANS measurements on UV-cured CTC/MA solutions. Here, we compare the SANS data of CTC/monomer solutions with those of the corresponding composites. (orig.)

  20. SANS studies of solutions and molecular composites prepared from cellulose tricarbanilate

    Energy Technology Data Exchange (ETDEWEB)

    Alava, C.; Arrighi, V.; Cameron, J.D.; Cowie, J.M.G.; Vaqueiro, P. [Department of Chemistry, Heriot-Watt University, Edinburgh EH14 4AS (United Kingdom); Moeller, A.; Triolo, A. [Hahn-Meitner-Institut-BENSC, Glienicker Strasse 100, 14109 Berlin (Germany)

    2002-07-01

    We report on SANS measurements carried out on the instrument SANS1 (V4) at the BENSC facility on solutions and composites of cellulose tricarbanilate (CTC). This cellulose derivative exhibits lyotropic behaviour in methylacrylate (MA). The SANS data indicate that in the isotropic liquid state (up to 25% wt CTC in MA) the CTC chains behave like rods of mass per unit length (M/L). In the liquid crystalline (LC) phase (at and above 35% wt CTC in MA), the Q dependence varies from Q{sup -1} to Q{sup -4}, probably as a result of self-assembling of the CTC chains. The general aim of our work is to prepare molecular composites, i.e. miscible blends of rigid-rod and flexible-coil polymers, from CTC solutions in polymerizable media. To establish the degree of homogeneity of the composites, we performed SANS measurements on UV-cured CTC/MA solutions. Here, we compare the SANS data of CTC/monomer solutions with those of the corresponding composites. (orig.)

  1. Frontally eluted components procedure with thin layer chromatography as a mode of sample preparation for high performance liquid chromatography quantitation of acetaminophen in biological matrix.

    Science.gov (United States)

    Klimek-Turek, A; Sikora, M; Rybicki, M; Dzido, T H

    2016-03-04

    A new concept of using thin-layer chromatography to sample preparation for the quantitative determination of solute/s followed by instrumental techniques is presented Thin-layer chromatography (TLC) is used to completely separate acetaminophen and its internal standard from other components (matrix) and to form a single spot/zone containing them at the solvent front position (after the final stage of the thin-layer chromatogram development). The location of the analytes and internal standard in the solvent front zone allows their easy extraction followed by quantitation by HPLC. The exctraction procedure of the solute/s and internal standard can proceed from whole solute frontal zone or its part without lowering in accuracy of quantitative analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2013-08-01

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

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

    Science.gov (United States)

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

    2017-02-22

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

  4. Preparation and characterization of irradiated carboxymethyl sago starch-acid hydrogel and its application as metal scavenger in aqueous solution.

    Science.gov (United States)

    Basri, Sri Norleha; Zainuddin, Norhazlin; Hashim, Kamaruddin; Yusof, Nor Azah

    2016-03-15

    Carboxymethyl sago starch-acid hydrogel was prepared via irradiation technique to remove divalent metal ions (Pb, Cu and Cd) from their aqueous solution. The hydrogel was characterized by using Fourier Transform Infrared (FT-IR), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The removal of these metal ions was analyzed by using inductively coupled plasma-optic emission spectra (ICP-OES) to study the amount of metal uptake by the hydrogel. Parameters of study include effect of pH, amount of sample, contact time, initial concentration of metal solution and reaction temperature. FTIR spectroscopy shows the CMSS hydrogel absorption peaks at 1741cm(-1), 1605cm(-1) and 1430cm(-1) which indicates the substitution of carboxymethyl group of modified sago starch. The degradation temperature of CMSS hydrogel is higher compared to CMSS due to the crosslinking by electron beam radiation and formed a porous hydrogel. From the data obtained, about 93.5%, 88.4% and 85.5% of Pb, Cu and Cd ions has been respectively removed from their solution under optimum condition. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

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

    2000-06-01

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

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

    Directory of Open Access Journals (Sweden)

    Schmid Michael

    2004-06-01

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

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

    Science.gov (United States)

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

    2004-07-01

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

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

    Science.gov (United States)

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

    2008-01-01

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

  9. Sampling Molecular Conformers in Solution with Quantum Mechanical Accuracy at a Nearly Molecular-Mechanics Cost.

    Science.gov (United States)

    Rosa, Marta; Micciarelli, Marco; Laio, Alessandro; Baroni, Stefano

    2016-09-13

    We introduce a method to evaluate the relative populations of different conformers of molecular species in solution, aiming at quantum mechanical accuracy, while keeping the computational cost at a nearly molecular-mechanics level. This goal is achieved by combining long classical molecular-dynamics simulations to sample the free-energy landscape of the system, advanced clustering techniques to identify the most relevant conformers, and thermodynamic perturbation theory to correct the resulting populations, using quantum-mechanical energies from density functional theory. A quantitative criterion for assessing the accuracy thus achieved is proposed. The resulting methodology is demonstrated in the specific case of cyanin (cyanidin-3-glucoside) in water solution.

  10. Study of Penetration Kinetics of Sodium Hydroxide Aqueous Solution into Wood Samples

    Directory of Open Access Journals (Sweden)

    Lubomír Lapčík

    2013-12-01

    Full Text Available The kinetics of unidirectional penetration of NaOH aqueous solution into rectangular samples of wood oriented parallel to a stern axis were studied. Scots pine (Pinus sylvestris, European larch (Larix decidua, blackthorn (Prunus spinosa, white willow (Salix alba, and horse-chestnut wood (Aesculus hippocastanum were studied in this work. The time dependence of liquid incorporation was measured by the volumetric method as a change of total volume of coexisting liquid (NaOH/H2O phase. The total thickness of the swollen surface layer d and mean value of the apparent diffusion coefficient of aqueous NaOH solution at 22 °C were determined.

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

    Directory of Open Access Journals (Sweden)

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

    2016-11-01

    Full Text Available Calcium plays an important role in the metabolism of plants and animals. In this paper, the preparation method of plant 41Ca for accelerator mass spectrometry (AMS measurement was developed for the first time in China. AMS, with its advantages of high sensitivity, small dose of radioactivity, high accuracy, large measuring range, and long tracer cycle, can be used to measure cosmogenic nuclide 41Ca , which has long half-life. The intensity of the beam in ion source is an important parameter for the sensitivity of AMS measurement. The high beam current can improve the sensitivity of AMS. The preparation methods of plant samples of 41Ca tracer were systematically studied to obtain high beam current using wet, dry and a combining method with wet and dry re-fluoride. A reliable preparation procedure of plant samples for 41Ca tracer and its optimization parameters were determined by testing beam currents of various samples and lay a foundation for the 41Ca-AMS technology at plant tracer applications.

  12. 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.

  13. DNA isolation and sample preparation for quantification of adduct levels by accelerator mass spectrometry.

    Science.gov (United States)

    Dingley, Karen H; Ubick, Esther A; Vogel, John S; Ognibene, Ted J; Malfatti, Michael A; Kulp, Kristen; Haack, Kurt W

    2014-01-01

    Accelerator mass spectrometry (AMS) is a highly sensitive technique used for the quantification of adducts following exposure to carbon-14- or tritium-labeled chemicals, with detection limits in the range of one adduct per 10(11)-10(12) nucleotides. The protocol described in this chapter provides an optimal method for isolating and preparing DNA samples to measure isotope-labeled DNA adducts by AMS. When preparing samples, special precautions must be taken to avoid cross-contamination of isotope among samples and produce a sample that is compatible with AMS. The DNA isolation method described is based upon digestion of tissue with proteinase K, followed by extraction of DNA using Qiagen isolation columns. The extracted DNA is precipitated with isopropanol, washed repeatedly with 70 % ethanol to remove salt, and then dissolved in water. DNA samples are then converted to graphite or titanium hydride and the isotope content measured by AMS to quantify adduct levels. This method has been used to reliably generate good yields of uncontaminated, pure DNA from animal and human tissues for analysis of adduct levels.

  14. Improved sample preparation and counting techniques for enhanced tritium measurement sensitivity

    Science.gov (United States)

    Moran, J.; Aalseth, C.; Bailey, V. L.; Mace, E. K.; Overman, C.; Seifert, A.; Wilcox Freeburg, E. D.

    2015-12-01

    Tritium (T) measurements offer insight to a wealth of environmental applications including hydrologic tracking, discerning ocean circulation patterns, and aging ice formations. However, the relatively short half-life of T (12.3 years) limits its effective age dating range. Compounding this limitation is the decrease in atmospheric T content by over two orders of magnitude (from 1000-2000 TU in 1962 to low background proportional counters which, when combined, offer improved T measurement sensitivity (~4.5 mmoles of H2 equivalent) and will help expand the application of T age dating to smaller sample sizes linked to persistent environmental questions despite the limitations above. For instance, this approach can be used to T date ~ 2.2 mmoles of CH4 collected from sample-limited systems including microbial communities, soils, or subsurface aquifers and can be combined with radiocarbon dating to distinguish the methane's formation age from C age in a system. This approach can also expand investigations into soil organic C where the improved sensitivity will permit resolution of soil C into more descriptive fractions and provide direct assessments of the stability of specific classes of organic matter in soils environments. We are employing a multiple step sample preparation system whereby organic samples are first combusted with resulting CO2 and H2O being used as a feedstock to synthesize CH4. This CH4 is mixed with Ar and loaded directly into an ultra-low background proportional counter for measurement of T β decay in a shallow underground laboratory. Analysis of water samples requires only the addition of geologic CO2 feedstock with the sample for methane synthesis. The chemical nature of the preparation techniques enable high sample throughput with only the final measurement requiring T decay with total sample analysis time ranging from 2 -5 weeks depending on T content.

  15. A single lysis solution for the analysis of tissue samples by different proteomic technologies

    DEFF Research Database (Denmark)

    Gromov, P.; Celis, J.E.; Gromova, I.

    2008-01-01

    Cancer, being a major healthcare concern worldwide, is one of the main targets for the application of emerging proteomic technologies and these tools promise to revolutionize the way cancer will be diagnosed and treated in the near future. Today, as a result of the unprecedented advances that have...... dissease, is driving scientists to increasingly use clinically relevant samples for biomarker and target discovery. Tissues are heterogeneous and as a result optimization of sample preparation is critical for generating accurate, representative, and highly reproducible quantitative data. Although a large...

  16. Preparation of chitosan films using different neutralizing solutions to improve endothelial cell compatibility.

    Science.gov (United States)

    He, Qing; Ao, Qiang; Gong, Yandao; Zhang, Xiufang

    2011-12-01

    The development of chitosan-based constructs for application in large-size defects or highly vascularized tissues is still a challenging issue. The poor endothelial cell compatibility of chitosan hinders the colonization of vascular endothelial cells in the chitosan-based constructs, and retards the establishment of a functional microvascular network following implantation. The aim of the present study is to prepare chitosan films with different neutralization methods to improve their endothelial cell compatibility. Chitosan salt films were neutralized with either sodium hydroxide (NaOH) aqueous solution, NaOH ethanol solution, or ethanol solution without NaOH. The physicochemical properties and endothelial cell compatibility of the chitosan films were investigated. Results indicated that neutralization with different solutions affected the surface chemistry, swelling ratio, crystalline conformation, nanotopography, and mechanical properties of the chitosan films. The NaOH ethanol solution-neutralized chitosan film (Chi-NaOH/EtOH film) displayed a nanofiber-dominant surface, while the NaOH aqueous solution-neutralized film (Chi-NaOH/H(2)O film) and the ethanol solution-neutralized film (Chi-EtOH film) displayed nanoparticle-dominant surfaces. Moreover, the Chi-NaOH/EtOH films exhibited a higher stiffness as compared to the Chi-NaOH/H(2)O and Chi-EtOH films. Endothelial cell compatibility of the chitosan films was evaluated with a human microvascular endothelial cell line, HMEC-1. Compared with the Chi-NaOH/H(2)O and Chi-EtOH films, HMECs cultured on the Chi-NaOH/EtOH films fully spread and exhibited significantly higher levels of adhesion and proliferation, with retention of the endothelial phenotype and function. Our findings suggest that the surface nanotopography and mechanical properties contribute to determining the endothelial cell compatibility of chitosan films. The nature of the neutralizing solutions can affect the physicochemical properties and

  17. Reducing time and increasing sensitivity in sample preparation for adherent mammalian cell metabolomics.

    Science.gov (United States)

    Lorenz, Matthew A; Burant, Charles F; Kennedy, Robert T

    2011-05-01

    A simple, fast, and reproducible sample preparation procedure was developed for relative quantification of metabolites in adherent mammalian cells using the clonal β-cell line INS-1 as a model sample. The method was developed by evaluating the effect of different sample preparation procedures on high performance liquid chromatography- mass spectrometry quantification of 27 metabolites involved in glycolysis and the tricarboxylic acid cycle on a directed basis as well as for all detectable chromatographic features on an undirected basis. We demonstrate that a rapid water rinse step prior to quenching of metabolism reduces components that suppress electrospray ionization thereby increasing signal for 26 of 27 targeted metabolites and increasing total number of detected features from 237 to 452 with no detectable change of metabolite content. A novel quenching technique is employed which involves addition of liquid nitrogen directly to the culture dish and allows for samples to be stored at -80 °C for at least 7 d before extraction. Separation of quenching and extraction steps provides the benefit of increased experimental convenience and sample stability while maintaining metabolite content similar to techniques that employ simultaneous quenching and extraction with cold organic solvent. The extraction solvent 9:1 methanol: chloroform was found to provide superior performance over acetonitrile, ethanol, and methanol with respect to metabolite recovery and extract stability. Maximal recovery was achieved using a single rapid (∼1 min) extraction step. The utility of this rapid preparation method (∼5 min) was demonstrated through precise metabolite measurements (11% average relative standard deviation without internal standards) associated with step changes in glucose concentration that evoke insulin secretion in the clonal β-cell line INS-1.

  18. Preparation of conductive PDDA/(PEDOT:PSS) multilayer thin film: influence of polyelectrolyte solution composition.

    Science.gov (United States)

    Jurin, F E; Buron, C C; Martin, N; Filiâtre, C

    2014-10-01

    Self-assembled multilayer films made of PEDOT:PSS poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) and PDDA poly(diallyldimethylammonium chloride) were prepared using layer-by-layer method. In order to modify the growth regime of the multilayer, to fabricate an electrical conductive film and to control its thickness, the effects of pH, type of electrolyte, ionic strength and polyelectrolyte concentration were investigated. Optical reflectometry measurements show that the pH of the solutions has no effect on the film growth while the adsorbed amount increases more rapidly when BaCl2 is used instead of NaCl as electrolyte. An increase in the ionic strength (with NaCl) induces a change in the growth regime from a linear to an exponential one at low polyelectrolyte concentration. As UV-vis measurements indicate, no decomplexation of PEDOT was recorded after film preparation. With polyelectrolyte concentration below 1 g L(-1), no conductive films were obtained even if 50 bilayers were deposited. A conductive film was prepared with a polyelectrolyte concentration of 1 g L(-1) and the measured conductivity was 0.3 S m(-1). A slight increase in conductivity was recorded when BaCl2 was used probably due to a modification of the film structure. Copyright © 2014 Elsevier Inc. All rights reserved.

  19. Optimization of coating solution for preparation of antibacterial copper-polyethylene nanocomposite

    Science.gov (United States)

    Ghorbani, Hamid Reza; Molaei, Mazaher

    2017-06-01

    Polyethylene film was coated with copper nanoparticles and its antibacterial properties were investigated. To make nanocomposite film, the solutions containing the copper nanoparticles were prepared using polyamide resin in six different concentrations of copper nanoparticles (1%, 2%, 3%, 5%, 7% and 10 wt%). Corona discharge was used to improve the nonpolar surface of polyethylene and prepare it for coating. Corona discharge was carried out in 5 min with power of 10 000 W. Characterisation of nanoparticles and the coated surface were performed using dynamic light scattering (DLS), x-ray diffraction (XRD) and scanning electron microscope (SEM). The antibacterial activity of polyethylene-copper nanocomposite against two type of bacteria including gram-negative Escherichia coli and gram-positive Staphylococcus aureus was measured by disc-diffusion method. In addition, the optimum concentration of copper nanoparticles was determined about 5 wt%. The current technique of coated film preparation reduces the amount of required nanoparticles which finally offers lower production cost.

  20. Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition.

    Science.gov (United States)

    Carretero-Genevrier, Adrián; Gich, Martí

    2015-12-21

    This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr(2+) act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

  1. Preparation of porous carbon sphere from waste sugar solution for electric double-layer capacitor

    Science.gov (United States)

    Hao, Zhi-Qiang; Cao, Jing-Pei; Wu, Yan; Zhao, Xiao-Yan; Zhuang, Qi-Qi; Wang, Xing-Yong; Wei, Xian-Yong

    2017-09-01

    Waste sugar solution (WSS), which contains abundant 2-keto-L-gulonic acid, is harmful to the environment if discharged directly. For value-added utilization of the waste resource, a novel process is developed for preparation of porous carbon spheres by hydrothermal carbonization (HTC) of WSS followed by KOH activation. Additionally, the possible preparation mechanism of carbon spheres is proposed. The effects of hydrothermal and activation parameters on the properties of the carbon sphere are also investigated. The carbon sphere is applied to electric double-layer capacitor and its electrochemical performance is studied. These results show that the carbon sphere obtained by HTC at 180 °C for 12 h with the WSS/deionized water volume ratio of 2/3 possess the highest specific capacitance under identical activation conditions. The specific capacitance of the carbon spheres can reach 296.1 F g-1 at a current density of 40 mA g-1. Besides, excellent cycle life and good capacitance retention (89.6%) are observed at 1.5 A g-1 after 5000 cycles. This study not only provides a facile and potential method for the WSS treatment, but also achieves the high value-added recycling of WSS for the preparation of porous carbon spheres with superior electrochemical properties.

  2. 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.

  3. Sample preparation and direct electrospray ionization on a tip column for rapid mass spectrometry analysis of complex samples.

    Science.gov (United States)

    Huang, Yun-Qing; You, Jin-Qing; Yuan, Bi-Feng; Feng, Yu-Qi

    2012-10-07

    A handheld pipette tip column electrospray ionization source (PTC-ESI source) was developed for rapid mass spectrometry analysis at ambient pressure. The PTC-ESI source was made up of three main component parts including a micro DC high voltage (HV) power supply, a micropipette and a disposable micropipette tip filled with a plug of adsorbent. A DC high voltage was applied to the sharp point of the micropipette tip column to induce electrospray ionization. The PTC-ESI source was successfully used for direct analysis of basic organic compounds, organic acids and peptides in a simple matrix. In the case of complex samples, micro-extraction based on the adsorbent phase filled in the pipette tip was used to remove impurities and concentrate target analytes prior to ionization. The eluting solution was not pipetted out, but directly dispersed in the form of electrospray from the pipette tip for ionization. The effectiveness of the PTC-ESI source has been further demonstrated by fast analysis of therapeutic compounds and endogenous bioactive chemicals in complex biological samples.

  4. Rapid Measurement of Food Adulteration with Minimal Sample Preparation and No Chromatography Using Ambient Ionization Mass Spectrometry.

    Science.gov (United States)

    Dalmia, Avinash

    2017-03-01

    A rapid method, with minimal sample preparation and no chromatography, was developed for analyzing food samples such as olive oil and pomegranate juice to measure adulteration with cheaper ingredients using the novel Direct Sample Analysis™ (DSA) ion source in conjunction with a time-of-flight (TOF)-MS. In less than 30 s, with minimal sample preparation and method development, adulteration of olive oil and pomegranate juice with cheaper seed oils and fruit juices, respectively, was measured with DSA/TOF-MS.

  5. Membrane-based sample preparation for ion chromatography-Techniques, instrumental configurations and applications.

    Science.gov (United States)

    Frenzel, Wolfgang; Markeviciute, Inga

    2017-01-06

    Sample preparation is the bottleneck of many analytical methods, including ion chromatography (IC). Procedures based on the application of membranes are important, yet not well appreciated means for clean-up and analyte preconcentration of liquid samples. Filtration, ultrafiltration, the variety of dialysis techniques, i.e. passive dialysis, Donnan dialysis and electrodialysis, as well as gas-diffusion are being reviewed here with respect to their application in combination with IC. Instrumental aspects including hardware requirements, configuration of membrane separation units and membrane characteristics are presented. Operation in batch and flow-through mode is described with emphasis on the latter to in-line coupling with IC, permitting fully automated operation. Attention is also drawn to dialysis probes and microdialysis both providing options for in-situ measurements with inherent selective sampling of analytes and sample preparation. The respective features of the various techniques are outlined with respect to the possibilities of matrix removal and selectivity enhancement. In this article, we provide examples of application of the diverse membrane separation techniques and discuss the benefits and limitations thereof.

  6. 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.

  7. Removal of interfering substances in samples prepared for two-dimensional (2-D) electrophoresis.

    Science.gov (United States)

    Berkelman, Tom

    2008-01-01

    Biological samples may contain contaminants that interfere with analysis by two-dimensional (2-D) electrophoresis. Lysates or biological fluids are complex mixtures that contain a wide variety of nonprotein substances in addition to the proteins to be analyzed. These substances often interfere with the resolution of the electrophoretic separation or the visualization of the result. Macromolecules (e.g., polysaccharides and DNA) can interfere with electrophoretic separation by clogging gel pores. Small ionic molecules can impair isoelectric focusing (IEF) separation by rendering the sample too conductive. Other substances (e.g., phenolics and lipids) can bind to proteins, influencing their electrophoretic properties or solubility. In many cases, measures to remove interfering substances can result in significantly clearer 2-D patterns with more visible spots and better resolution. It should be borne in mind, however, that analysis of samples by 2-D electrophoresis is usually most successful and informative when performed with minimally processed samples, so it is important that any steps taken to remove interfering substance be appropriate to the sample and only performed when necessary. Procedures for the removal of interfering substances therefore represent a compromise between removing nonprotein contaminants, and minimizing interference with the integrity and relative abundances of the sample proteins. This chapter presents a number of illustrative examples of optimized sample preparation methods in which specific interfering substances are removed by a variety of different strategies.

  8. Well-conditioning effects on bubblepoint pressure of fluid samples from solution-gas-drive reservoirs

    Energy Technology Data Exchange (ETDEWEB)

    Reynolds, A.C. (Univ. of Tulsa, Tulsa, OK (US)); Peres, A.M.M.; Serra, K.V. (Petrobas (BR)); Macias-Chapa, L. (National Autonomous Univ. of Mexico (MX))

    1990-12-01

    This paper considers the determination of the initial or average reservoir bubblepoint pressure from a fluid sample obtained from a well producing a solution-gas-drive reservoir. It is shown that standard API recommended well-conditioning procedures (rate reductions) for obtaining a single-phase (liquid) bottomhole fluid sample do not always redissolve all free gas. Thus, it is not always possible to obtain a single-phase liquid (oil) bottomhole fluid sample that has a bubblepoint pressure equal to the initial or average reservoir bubblepoint pressure. Moreover, monitoring the producing GOR and bottomhole pressure does not always reliably indicate whether two-phase (oil and gas) or single-phase (oil) flow is prevalent in the near-wellbore region. Contrary to current opinion, it is shown that recombination of surface samples of oil and gas form the producing GOR usually yields reliable estimates of average reservoir bubblepoint pressure.

  9. Preparation of C₁₈-functionalized magnetic polydopamine microspheres for the enrichment and analysis of alkylphenols in water samples.

    Science.gov (United States)

    Wang, Xianying; Deng, Chunhui

    2016-02-01

    In this work, C18-functionalized magnetic polydopamine microspheres (Fe3O4@PDA@C18) were successfully synthesized and applied to the analysis of alkylphenols in water samples. The magnetic Fe3O4 particles coated with hydrophilic surface were synthesized via a solvothermal reaction and the self-polymerization of dopamine. And then the C18 groups were fabricated by a silylanization method. Benefit from the merits of Fe3O4 particles, polydopamine coating and C18 groups, the Fe3O4@PDA@C18 material possessed several properties of super magnetic responsiviness, good water dispersibility, π-electron system and hydrophobic C18 groups. Thus, the materials had great potential to be developed as the adsorbent for the magnetic solid-phase extraction (MSPE) technique. Here, we selected three kinds of alkylphenols (4-tert-octylphenol, 4-n-nonylphenol, 4-n-octylphenol) to be the target analyst for evaluating the performance of the prepared material. In this study, various extraction parameters were investigated and optimized, such as pH values of water sample solution, amount of adsorbents, adsorption and desorption time, the species of desorption solution. Meanwhile, the method validations were studied, including linearity, limit of detection and method precision. From the results, Fe3O4@PDA@C18 composites were successfully applied as the adsorbents for the extraction of alkylphenols in water samples. The proposed material provided an approach for a simple, rapid magnetic solid-phase extraction for hydrophobic compounds in environmental samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. A modified coaxial electrospinning for preparing fibers from a high concentration polymer solution

    Directory of Open Access Journals (Sweden)

    2011-08-01

    Full Text Available A new process technology modified from conventional coaxial electrospinning process has been developed to prepare polymer fibers from a high concentration solution. This process involves a pure solvent concentrically surrounding polymer fluid in the spinneret. The concentric spinneret was constructed simply by inserting a metal needle through a high elastic silica gel tube. Two syringe pumps were used to drive the core polymer solution and the sheath solvent. Using polyvinylpyrrolidone (PVP as the polymer model, which normally has an electrospinnable concentration of 10% w/v in ethanol, it was possible to electrospin 35% w/v of PVP in the same solvent, when pure N, N-dimethylacetamide (DMAc was used as sheath fluid. The resultant fibers have a smooth surface morphology and good structural uniformity. The diameter of the fibers was 2.0±0.25 µm when the DMAc-to-polymer-solution flow rate ratio was set as 0.1. The process technology reported here opens a new window to tune the polymer fibers obtained by the electrospinning, and is useful for improving productivity of the electrospinning process.

  11. 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.

  12. Evaluation of neon focused ion beam milling for TEM sample preparation.

    Science.gov (United States)

    Pekin, T C; Allen, F I; Minor, A M

    2016-10-01

    Gallium-based focused ion beams generated from liquid-metal sources are widely used in micromachining and sample preparation for transmission electron microscopy, with well-known drawbacks such as sample damage and contamination. In this work, an alternative (neon) focused ion beam generated by a gas field-ionization source is evaluated for the preparation of electron-transparent specimens. To do so, electron-transparent sections of Si and an Al alloy are prepared with both Ga and Ne ion beams for direct comparison. Diffraction-contrast imaging and energy dispersive x-ray spectroscopy are used to evaluate the relative damage induced by the two beams, and cross-sections of milled trenches are examined to compare the implantation depth with theoretical predictions from Monte Carlo simulations. Our results show that for the beam voltages and materials systems investigated, Ne ion beam milling does not significantly reduce the focused ion beam induced artefacts. However, the Ne ion beam does enable more precise milling and may be of interest in cases where Ga contamination cannot be tolerated.

  13. A Novel Sample Preparation for Shotgun Proteomics Characterization of HCPs in Antibodies.

    Science.gov (United States)

    Huang, Lihua; Wang, Ning; Mitchell, Charles E; Brownlee, Tammy; Maple, Steven R; De Felippis, Michael R

    2017-05-16

    Residual host cell proteins (HCPs) in biopharmaceuticals derived from recombinant DNA technology can present potential safety risks to patients or compromise product stability. Thus, the downstream purification process is designed to demonstrate robust removal of these impurities. ELISA using polyclonal anti-HCP antibodies as reagents for capture, detection, and quantitation purposes is most commonly used to monitor HCP removal during process development, but this technique has limitations. More recently, LC-MS for residual HCP characterization has emerged as a powerful tool to support purification process development. However, mass spectrometry needs to overcome the enormous dynamic range to detect low ppm levels of residual HCPs in biopharmaceutical samples. We describe a simple and powerful methodology to characterize residual HCPs in (monoclonal) antibodies by combining a novel sample preparation procedure using trypsin digestion and a shotgun proteomics approach. Differing from the traditional methodology, the sample preparation approach maintains nearly intact antibody while HCPs are digested. Thus, the dynamic range for HCP detection by MS is 1 to 2 orders of magnitude less than the traditional trypsin digestion sample preparation procedure. HCP spiking experiments demonstrated that our method could detect 0.5 ppm of HCP with molecular weight >60 kDa, such as rPLBL2. Application of our method to analyze a high-purity NIST monoclonal antibody standard RM 8670 derived from a murine cell line expression system resulted in detection of 60 mouse HCPs; twice as many as previously reported with 2D-UPLC/IM/MS(E) method. A control monoclonal antibody used for 70 analyses over 450 days demonstrated that our method is robust.

  14. Sample preparation methods for beeswax characterization by gas chromatography with flame ionization detection.

    Science.gov (United States)

    Jiménez, J J; Bernal, J L; del Nozal, M A J; Martín, M A T; Bernal, J

    2006-10-06

    New and simpler methods of sample preparation to determine several families of compounds in beeswax by conventional and high temperature gas chromatography are proposed. To analyze hydrocarbons and palmitates, a dilution of sample is enough whereas for the total acid content, a hydrolysis and simultaneous methylation with BF3-methanol results more effective than the usual methods; for the total content of alcohols, a further acetylation with acetic anhydride is necessary. Free alcohols are directly acetylated in a sample dissolution but for free acids and monoesterified 1,2,3-propanetriols analysis, a previous extraction with acetonitrile is required. The concentrations of all the compounds studied are expressed in weight percentage referred only to one standard: octadecyl octadecanoate. The precision of the analytical methods has been evaluated showing its importance in the analysis of beeswaxes used in apiculture.

  15. Practical Guide to Using Cryoprotectants in Biological Sample Preparation at Cryogenic temperature for Electron Microscopic Studies

    Directory of Open Access Journals (Sweden)

    A-Reum Je

    2011-10-01

    Full Text Available Cryo-fixation enables the preservation of the fine structures of intracellular organelles in a condition that is as close to their native state as possible compared with chemical fixation and room temperature processing. Fixation is the initial step for biological sample preparation in electron microscopy. This step is critically important because the goals of electron microscopic observation are fundamentally dependent on well-preserved specimens resulting from this fixation. In the present work, key components of cryo-fixation, cryoprotectants, are tested with various cell types of interest. The results show that dextran can be easily adapted for use with animal cells and cyanobacteria, whereas 1-hexadecene is applicable to plant and yeast cells. The current report provides useful information on the preparation of cryo-fixed biological specimens using high pressure freezing and freeze-substitution aimed at electron microscopic observation.

  16. Laboratory Investigation of Rivers State Clay Samples for Drilling Mud Preparation

    Directory of Open Access Journals (Sweden)

    Nmegbu, Chukwuma Godwin Jacob

    2014-06-01

    Full Text Available Drilling fluids are an integral part of any oil and gas industry, providing the ease to which wells are drilled to access subsurface reservoir fluids. Certain rheology and mineralogical properties of the clay material used for drilling mud preparation must be critically investigated since clay deposits in different location exhibits different characteristics. Clay samples were collected from three different geographical locations namely; Egbamini (Emolga, Afam Street (Port Harcourt and Oboboru (onelga local government areas in Rivers state. Their rheological and wall building properties were measured in the laboratory to determine their suitability for drilling mud formulation. Results showed that in their respective native states, they proved unsuitable for drilling mud preparation when compared to standard Bentonite because they were observed to show responses far below the required API standards for mud formulation.

  17. Preparation of carbon-nitride bulk samples in the presence of seed carbon-nitride films

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J. I. [Korea University of Technology and Education, Chonan (Korea, Republic of); Zorov, N. B. [Moscow State University, Moscow (Russian Federation)

    2004-05-15

    A procedure was developed for preparing bulk carbon-nitride crystals from polymeric alpha-C{sub 3}N{sub 4.2} at high pressure and high temperature in the presence of seeds of crystalline carbon-nitride films prepared by using a high-voltage discharge plasma combined with pulsed laser ablation of a graphite target. The samples were evaluated by using X-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, Auger electron spectroscopy (AES), secondary-ion mass spectrometry (SIMS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Notably, XPS studies of the film composition before and after thermobaric treatments demonstrated that the nitrogen composition in the alpha-C{sub 3}N{sub 4.2} material, which initially contained more than 58 % nitrogen, decreased during the annealing process and reached a common, stable composition of approx 45 %. The thermobaric experiments were performed at 10 - 77 kbar and 350 - 1200 .deg. C.

  18. Improved sample preparation for CE-LIF analysis of plant N-glycans.

    Science.gov (United States)

    Nagels, Bieke; Santens, Francis; Weterings, Koen; Van Damme, Els J M; Callewaert, Nico

    2011-12-01

    In view of glycomics studies in plants, it is important to have sensitive tools that allow one to analyze and characterize the N-glycans present on plant proteins in different species. Earlier methods combined plant-based sample preparations with CE-LIF N-glycan analysis but suffered from background contaminations, often resulting in non-reproducible results. This publication describes a reproducible and sensitive protocol for the preparation and analysis of plant N-glycans, based on a combination of the 'in-gel release method' and N-glycan analysis on a multicapillary DNA sequencer. Our protocol makes it possible to analyze plant N-glycans starting from low amounts of plant material with highly reproducible results. The developed protocol was validated for different plant species and plant cells.

  19. Continuous absorption of CO2 in packed column using MDEA solution for biomethane preparation

    Science.gov (United States)

    Mindaryani, A.; Budhijanto, W.; Ningrum, S. S.

    2016-11-01

    Nowadays, the energy consumption in Indonesia is increasing. Raising of energy consumption force Indonesia to find other energy resources. Biogas is one of the renewable energy, which was developed in anticipation to the fossil energy reduction. Reducing the content of impurities in biogas may reduce the corrosion impact and increase the combustion efficiency. The biomethane can be utilised as fuel for generator in small and medium scale industries (IKM). Continuous CO2 absorption in packed column using MDEA solution as absorbent is studied for biomethane preparation. CO2 absorption experiments was performed continuously in the packed absorption column with a diameter of 6 cm and 75 cm length. Gas is sparged from the bottom of the column while the liquid is pumped through the top of the column. The concentration of CO2 at exit gas is analysed by GC and recorded as a function of time. The flowrate of the inlet gas was varied at 1 LPM; 1.5 LPM; and 1.8 LPM. Variation of MDEA solution concentration used was 20% and 35.31%. Mathematical model for unsteady state CO2 absorption in packed column was developed. The reaction rate constant (k) and mass transfer coefficient KGa were determined by fitting the outlet CO2 concentration data as a function of time to the model solution with smallest Sum of Square of Errors (SSE). The experimental data shows that absorption of 1 LPM gas flow rate with 0,15 LPM MDEA solution flow rate may reduce 40 % CO2 to be 17 % CO2 in outlet gas. The steady state process reaches at 10 minutes. Increasing gas flow rates shows the higher overall mass transfer coefficient. The reaction rate constant is not affected by gas flow rate variation.

  20. Assessment of preparation methods for organic phosphorus analysis in phosphorus-polluted Fe/Al-rich Haihe river sediments using solution 31P-NMR.

    Directory of Open Access Journals (Sweden)

    Wenqiang Zhang

    Full Text Available Fe/Al-rich river sediments that were highly polluted with phosphorus (P were used in tests to determine the optimum preparation techniques for measuring organic P (Po using solution (31P nuclear magnetic resonance spectroscopy ((31P-NMR. The optimum pre-treatment, extraction time, sediment to solution ratio and sodium hydroxide-ethylenediaminetetraacetic acid (NaOH-EDTA extractant solution composition were determined. The total P and Po recovery rates were higher from freeze- and air-dried samples than from fresh samples. An extraction time of 16 h was adequate for extracting Po, and a shorter or longer extraction time led to lower recoveries of total P and Po, or led to the degradation of Po. An ideal P recovery rate and good-quality NMR spectra were obtained at a sediment:solution ratio of 1:10, showing that this ratio is ideal for extracting Po. An extractant solution of 0.25 M NaOH and 50 mM EDTA was found to be more appropriate than either NaOH on its own, or a more concentrated NaOH-EDTA mixture for (31P-NMR analysis, as this combination minimized interference from paramagnetic ions and was appropriate for the detected range of Po concentrations. The most appropriate preparation method for Po analysis, therefore, was to extract the freeze-dried and ground sediment sample with a 0.25 M NaOH and 50 mM EDTA solution at a sediment:solution ratio of 1:10, for 16 h, by shaking. As lyophilization of the NaOH-EDTA extracts proved to be an optimal pre-concentration method for Po analysis in the river sediment, the extract was lyophilized as soon as possible, and analyzed by (31P-NMR.

  1. Preparation of Modified Magnetic Nanocomposites Dithiooxamide/Fe3O4 for Preconcentration and Determination of Trace Amounts of Cobalt Ions in Food and Natural Water Samples

    Directory of Open Access Journals (Sweden)

    Ali Mirabi

    2016-09-01

    Full Text Available The first study on the high efficiency of nanometer-sized magnetic nanoparticles (Fe3O4 coated with sodium dodecyl sulfate (SDS and dithiooxamide as a new sorbent solid phase extraction has been reported. Modified magnetic nanicomposites was used to preconcentrate and separate Co (II ions in food and environmental water samples. Magnetic nanoparticles were prepared by chemical precipitation of Fe (II and Fe (III salts from aqueous solution by ammonia solution. These magnetic nanoparticles and nanocomposites were characterized by scanning electron microscopy (SEM, transmission electron microscopy (TEM, thermo gravimetric analysis (TGA and elemental analysis CHNS. A micro sample introduction system was employed for the nebulization micro-volume of diluted solution into flame atomic absorption spectrometry (FAAS. The extraction conditions were optimized by selecting the appropriate extraction parameters including the amount of nanosorbent, pH value, volume of dithiooxamide and condition of eluting solution. The detection limit of this method for Co (II ions was 1.21 ng ml-1 and the R.S.D. was 0.9% (n=6. The advantages of this new method include rapidity, easy preparation of nanosorbents and a high preconcentration factor. The proposed method has been applied to the determination of Co (II ions at trace levels in real samples such as, kiwi, orange, cucumber, apple, green pepper, honey, potato, tap water, river water and sea water with satisfactory results.

  2. Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications.

    Science.gov (United States)

    Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

    2015-01-01

    Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed.

  3. Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications

    Science.gov (United States)

    Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

    2015-01-01

    Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed. PMID:26491320

  4. [Nasal submicron emulsion of Scutellariae Radix extract preparation technology research based on phase transfer of solute technology].

    Science.gov (United States)

    Shi, Ya-jun; Shi, Jun-hui; Chen, Shi-bin; Yang, Ming

    2015-07-01

    Based on the demand of nasal drug delivery high drug loadings, using the unique phase transfer of solute, integrating the phospholipid complex preparation and submicron emulsion molding process of Scutellariae Radix extract, the study obtained the preparation of the high drug loadings submicron emulsion of Scutellariae Radix extract. In the study of drug solution dispersion method, the uniformity of drug dispersed as the evaluation index, the traditional mixing method, grinding, homogenate and solute phase transfer technology were investigated, and the solute phase transfer technology was adopted in the last. With the adoption of new technology, the drug loading capacity reached 1.33% (phospholipid complex was 4%). The drug loading capacity was improved significantly. The transfer of solute method and timing were studied as follows,join the oil phase when the volume of phospholipid complex anhydrous ethanol solution remaining 30%, the solute phase transfer was completed with the continued recycling of anhydrous ethanol. After drug dissolved away to oil phase, the preparation technology of colostrum was determined with the evaluation index of emulsion droplet form. The particle size of submicron emulsion, PDI and stability parameters were used as evaluation index, orthogonal methodology were adopted to optimize the submicron emulsion ingredient and main influential factors of high pressure homogenization technology. The optimized preparation technology of Scutellariae Radix extract nasal submicron emulsion is practical and stable.

  5. 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.

  6. Error baseline rates of five sample preparation methods used to characterize RNA virus populations

    Science.gov (United States)

    Kugelman, Jeffrey R.; Wiley, Michael R.; Nagle, Elyse R.; Reyes, Daniel; Pfeffer, Brad P.; Kuhn, Jens H.; Sanchez-Lockhart, Mariano; Palacios, Gustavo F.

    2017-01-01

    Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic “no amplification” method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a “targeted” amplification method, sequence-independent single-primer amplification (SISPA) as a “random” amplification method, rolling circle reverse transcription sequencing (CirSeq) as an advanced “no amplification” method, and Illumina TruSeq RNA Access as a “targeted” enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4−5) of all compared methods. PMID:28182717

  7. MWCNTs/Cellulose Hydrogels Prepared from NaOH/Urea Aqueous Solution with Improved Mechanical Properties

    Directory of Open Access Journals (Sweden)

    Yingpu Zhang

    2015-01-01

    Full Text Available Novel high strength composite hydrogels were designed and synthesized by introducing multiwalled carbon nanotubes (MWCNTs into cellulose/NaOH/urea aqueous solution and then cross-linked by epichlorohydrin. MWCNTs were used to modify the matrix of cellulose. The structure and morphology of the hydrogels were characterized by Fourier transform infrared (FT-IR spectroscopy, high resolution transmission electron microscopy (HR-TEM, and scanning electron microscopy (SEM. The results from swelling testing revealed that the equilibrium swelling ratio of hydrogels decreased with the increment of MWCNTs content. Thermogravimetric analysis (TGA and dynamic mechanical analysis (DMA results demonstrated that the introduction of MWCNT into cellulose hydrogel networks remarkably improved both thermal and mechanical properties of the composite hydrogels. The preparation of MWCNTs modifiedcellulose-based composites with improved mechanical properties was the first important step towards the development of advanced functional materials.

  8. High quality thin films of thermoelectric misfit cobalt oxides prepared by a chemical solution method

    Science.gov (United States)

    Rivas-Murias, Beatriz; Manuel Vila-Fungueiriño, José; Rivadulla, Francisco

    2015-01-01

    Misfit cobaltates ([Bi/Ba/Sr/Ca/CoO]nRS[CoO2]q) constitute the most promising family of thermoelectric oxides for high temperature energy harvesting. However, their complex structure and chemical composition makes extremely challenging their deposition by high-vacuum physical techniques. Therefore, many of them have not been prepared as thin films until now. Here we report the synthesis of high-quality epitaxial thin films of the most representative members of this family of compounds by a water-based chemical solution deposition method. The films show an exceptional crystalline quality, with an electrical conductivity and thermopower comparable to single crystals. These properties are linked to the epitaxial matching of the rock-salt layers of the structure to the substrate, producing clean interfaces free of amorphous phases. This is an important step forward for the integration of these materials with complementary n-type thermoelectric oxides in multilayer nanostructures. PMID:26153533

  9. High quality thin films of thermoelectric misfit cobalt oxides prepared by a chemical solution method.

    Science.gov (United States)

    Rivas-Murias, Beatriz; Manuel Vila-Fungueiriño, José; Rivadulla, Francisco

    2015-07-08

    Misfit cobaltates ([Bi/Ba/Sr/Ca/CoO]n(RS)[CoO2]q) constitute the most promising family of thermoelectric oxides for high temperature energy harvesting. However, their complex structure and chemical composition makes extremely challenging their deposition by high-vacuum physical techniques. Therefore, many of them have not been prepared as thin films until now. Here we report the synthesis of high-quality epitaxial thin films of the most representative members of this family of compounds by a water-based chemical solution deposition method. The films show an exceptional crystalline quality, with an electrical conductivity and thermopower comparable to single crystals. These properties are linked to the epitaxial matching of the rock-salt layers of the structure to the substrate, producing clean interfaces free of amorphous phases. This is an important step forward for the integration of these materials with complementary n-type thermoelectric oxides in multilayer nanostructures.

  10. The first preparative solution phase synthesis of melanotan II

    Directory of Open Access Journals (Sweden)

    2008-10-01

    Full Text Available Melanotan II is a synthetic cyclic heptapeptide used to prevent a sunlight-induced skin cancer by stimulating the skin tanning process. In this paper we report the first solution phase synthesis of the title compound. The hexapeptide sequence has been assembled by [(2+2+1+1] scheme. After removing the orthogonal protection, a carbodiimide mediated lactamization, involving the ε-amino group of lysine and γ-carboxy group of aspartic acid, led to a cyclic intermediate. Appending N-acetylnorleucine concluded the assembly of melanotan II molecule. Protection of the lateral groups in arginine and tryptophan was omitted for atom and step economy reasons. The total synthesis of melanotan II was accomplished in 12 steps with 2.6% overall yield, affording >90% pure peptide without using preparative chromatography.

  11. Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

    Energy Technology Data Exchange (ETDEWEB)

    Jakeman, David L.; Mitchell, Dan J.; Shuttleworth, Wendy A.; Evans, Jeremy N.S. [Washington State University, Department of Biochemistry and Biophysics (United States)

    1998-10-15

    Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of {sup 13}P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 {+-} 12 Hz and 125 {+-} 7 Hz respectively, by a variety of methods involving additives and freezing techniques.

  12. Comparison of soil solution sampling techniques to assess metal fluxes from contaminated soil to groundwater.

    Science.gov (United States)

    Coutelot, F; Sappin-Didier, V; Keller, C; Atteia, O

    2014-12-01

    The unsaturated zone plays a major role in elemental fluxes in terrestrial ecosystems. A representative chemical analysis of soil pore water is required for the interpretation of soil chemical phenomena and particularly to assess Trace Elements (TEs) mobility. This requires an optimal sampling system to avoid modification of the extracted soil water chemistry and allow for an accurate estimation of solute fluxes. In this paper, the chemical composition of soil solutions sampled by Rhizon® samplers connected to a standard syringe was compared to two other types of suction probes (Rhizon® + vacuum tube and Rhizon® + diverted flow system). We investigated the effects of different vacuum application procedures on concentrations of spiked elements (Cr, As, Zn) mixed as powder into the first 20 cm of 100-cm columns and non-spiked elements (Ca, Na, Mg) concentrations in two types of columns (SiO2 sand and a mixture of kaolinite + SiO2 sand substrates). Rhizon® was installed at different depths. The metals concentrations showed that (i) in sand, peak concentrations cannot be correctly sampled, thus the flux cannot be estimated, and the errors can easily reach a factor 2; (ii) in sand + clay columns, peak concentrations were larger, indicating that they could be sampled but, due to sorption on clay, it was not possible to compare fluxes at different depths. The different samplers tested were not able to reflect the elemental flux to groundwater and, although the Rhizon® + syringe device was more accurate, the best solution remains to be the use of a lysimeter, whose bottom is kept continuously at a suction close to the one existing in the soil.

  13. Bayesian Reliability Modeling and Assessment Solution for NC Machine Tools under Small-sample Data

    Institute of Scientific and Technical Information of China (English)

    YANG Zhaojun; KAN Yingnan; CHEN Fei; XU Binbin; CHEN Chuanhai; YANG Chuangui

    2015-01-01

    Although Markov chain Monte Carlo(MCMC) algorithms are accurate, many factors may cause instability when they are utilized in reliability analysis; such instability makes these algorithms unsuitable for widespread engineering applications. Thus, a reliability modeling and assessment solution aimed at small-sample data of numerical control(NC) machine tools is proposed on the basis of Bayes theories. An expert-judgment process of fusing multi-source prior information is developed to obtain the Weibull parameters’ prior distributions and reduce the subjective bias of usual expert-judgment methods. The grid approximation method is applied to two-parameter Weibull distribution to derive the formulas for the parameters’ posterior distributions and solve the calculation difficulty of high-dimensional integration. The method is then applied to the real data of a type of NC machine tool to implement a reliability assessment and obtain the mean time between failures(MTBF). The relative error of the proposed method is 5.8020×10-4 compared with the MTBF obtained by the MCMC algorithm. This result indicates that the proposed method is as accurate as MCMC. The newly developed solution for reliability modeling and assessment of NC machine tools under small-sample data is easy, practical, and highly suitable for widespread application in the engineering field; in addition, the solution does not reduce accuracy.

  14. Materials of 2nd Poznan analytical meeting: Modern methods of sample preparation and trace elements analysis; Materialy 2. Poznanskiego Kowersatorium Analitycznego: Nowoczesne metody przygotowania probek i oznaczania sladowych zawartosci pierwiastkow

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1993-12-31

    The modern methods for sample preparation and treatment before analysis have been presented. The neutron activation analysis, PIXE, X-ray fluorescence analysis and other methods have been used for trace element analysis in samples of different origin. The new technical solutions and modern equipment for trace amount analysis have been also performed. During the conference 20 lectures have been presented.

  15. Urine sample preparation and fractionation for global proteome profiling by LC-MS.

    Science.gov (United States)

    Court, Magali; Garin, Jérôme; Masselon, Christophe D

    2015-01-01

    Urine has garnered tremendous interest over the past decade as a potential source of protein biomarkers for various pathologies. However, due to its low protein concentration and the presence of interfering compounds, urine constitutes a challenging analyte in proteomics. In the context of a project aimed at the discovery and evaluation of new candidate biomarkers of bladder cancer in urine, our laboratory has implemented and evaluated an array of preparation techniques for urinary proteome analysis. We present here the protocol that, in our hands, yielded the best overall proteome coverage with the lowest analytical effort. It begins with protein precipitation using trichloroacetic acid, in solution digestion and RP-C18 cartridge desalting of the resulting peptides mixture, and is followed by peptide fractionation by gel-free isoelectric focusing, and nano-LC-MS/MS for database compilation.

  16. Clozapine-carboxylic acid plasticized co-amorphous dispersions: Preparation, characterization and solution stability evaluation

    Directory of Open Access Journals (Sweden)

    Ali Ahmed Mahmoud Abdelhaleem

    2015-06-01

    Full Text Available This study addressed the possibility of forming of co-amorphous systems between clozapine (CZ and various carboxylic acid plasticizers (CAPs. The aim was to improve the solubility and oral bioavailability of clozapine. Co-amorphous dispersions were prepared using modified solvent evaporation methodology at drug/plasticizer stoichiometric ratios of 1:1, 1:1.5 and 1:2. Solid state characterization was performed using differential scanning calorimetry, X-ray diffraction and infra red spectroscopy. Highly soluble homogeneous co-amorphous dispersions were formed between clozapine and CAPs via hydrogen bonding. The co-amorphous dispersions formed with tartaric acid (1:2 showed the highest dissolution percentage (> 95 % in 20 minutes compared to pure crystalline CZ (56 %. Highly stable solutions were obtained from co-amorphous CZ-citric and CZ-tartaric acid at 1:1.5 molar ratio. The prepared dispersions suggest the possibility of peroral or sublingual administration of highly soluble clozapine at a reduced dose with the great chance to bypass the first pass metabolism.

  17. Results for the first quarter calendar year 2017 tank 50H salt solution sample

    Energy Technology Data Exchange (ETDEWEB)

    Crawford, C. L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-04-12

    In this memorandum, the chemical and radionuclide contaminant results from the First Quarter Calendar Year 2017 (CY17) sample of Tank 50H salt solution are presented in tabulated form. The First Quarter CY17 Tank 50H samples [a 200 mL sample obtained 6” below the surface (HTF-50-17-7) and a 1 L sample obtained 66” from the tank bottom (HTF-50-17-8)] were obtained on January 15, 2017 and received at Savannah River National Laboratory (SRNL) on January 16, 2017. Prior to obtaining the samples from Tank 50H, a single pump was run at least 4.4 hours and the samples were pulled immediately after pump shut down. All volatile organic analysis (VOA) and semi-volatile organic analysis (SVOA) were performed on the surface sample and all other analyses were performed on the variable depth sample. The information from this characterization will be used by Savannah River Remediation (SRR) for the transfer of aqueous waste from Tank 50H to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets. The chemical and radionuclide contaminant results from the characterization of the First Quarter CY17 sampling of Tank 50H were requested by SRR personnel and details of the testing are presented in the SRNL Task Technical and Quality Assurance Plan (TTQAP). This memorandum is part of Deliverable 2 from SRR request. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the TTQAP for the Tank 50H saltstone task.

  18. Sample preparation and separation techniques for bioanalysis of morphine and related substances.

    Science.gov (United States)

    Hansen, Steen Honoré

    2009-03-01

    In present time the use or misuse of morphine and its derivatives are monitored by assaying the presence of the drug and its metabolites in biofluids. In the present review, focus is placed on the sample preparation and on the separation techniques used in the current best practices of bioanalysis of morphine and its major metabolites. However, as methods for testing the misuse of heroin, a morphine derivative, often involve bioanalytical methods that cover a number of other illicit drug substances, such methods are also included in the review. Furthermore, the review also includes bioanalysis in a broader perspective as analysis of plant materials, cell cultures and environmental samples. The review is not intended to cover all publications that include bioanalysis of morphine but is more to be considered a view into the current best practices of bioanalysis of morphine, its metabolites and other related substances.

  19. Standard Methods of Analysis of Sulfochromate Etch Solution Used in Surface Preparation of Aluminum

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2012-01-01

    1.1 These methods offer a means for controlling the effectiveness of the etchant which is normally used for preparing the surface of aluminum alloys for subsequent adhesive bonding. As the etchant reacts with the aluminum, hexavalent chromium is converted to trivalent chromium; a measure of the two and the difference can be used to determine the amount of dichromate used. 1.2 The sulfochromate solution can be replenished by restoring the sodium dichromate and the sulfuric acid to the original formulation levels. The lower limit of usefulness will vary depending upon solution storage, adhesives used, critical nature of bond capability, variety of metals processed, etc. and should be determined. Replenishment will be limited to the number of times the chemical ingredients can be restored and maintained to the required levels and should be determined by the user. Sludge collecting in the bottom of a tank should be minimized by periodic removal of sludge. For some applications, the hexavalent chromium should not ...

  20. Preparation and Characterization of Biochars from Eichornia crassipes for Cadmium Removal in Aqueous Solutions.

    Directory of Open Access Journals (Sweden)

    Feng Li

    Full Text Available The study investigated the preparation and characterization of biochars from water hyacinth at 300°C to 700°C for cadmium (Cd removal from aqueous solutions. The adsorption process was dominated by oxygen-containing functional groups with irregular surfaces via esterification reactions. Furthermore, the mineral components in the biochars also contributed to Cd absorption through precipitation. Parameters such as the effects of solution pH, contact time, and initial concentration were studied. The optimum pH value was observed at 5.0, in which nearly 90% of Cd was removed. The maximum Cd adsorption capacities based on the Langmuir isotherm were calculated at 49.837, 36.899, and 25.826 mg g(-1. The adsorption processes of the biochars followed the pseudo-second-order kinetics, with the equilibrium achieved around 5 h. The biochar from E. crassipes is a promising adsorbent for the treatment of wastewater, which can in turn convert one environmental problem to a new cleaning Technology.

  1. Phosphite determination in fertilizers after online sequential sample preparation in a flow injection system.

    Science.gov (United States)

    Dametto, Patrícia Roberta; Franzini, Vanessa Pezza; Gomes Neto, José Anchieta

    2007-07-25

    A flow injection spectrophotometric system is proposed for phosphite determination in fertilizers by the molybdenum blue method after the processing of each sample two times on-line without and with an oxidizing step. The flow system was designed to add sulfuric acid or permanganate solutions alternately into the system by simply displacing the injector-commutator from one resting position to another, allowing the determination of phosphate and total phosphate, respectively. The concentration of phosphite is obtained then by difference between the two measurents. The influence of flow rates, sample volume, and dimension of flow line connecting the injector-commutator to the main analytical channel was evaluated. The proposed method was applied to phosphite determination in commercial liquid fertilizers. Results obtained with the proposed FIA system were not statistically different from those obtained by titrimetry at the 95% confidence level. In addition, recoveries within 94 and 100% of spiked fertilizers were found. The relative standard deviation (n = 12) related to the phosphite-converted-phosphate peak alone was solution. Precision due to the differences of total phosphate and phosphate was 1.1% for 10 mg L(-1) P (phosphate) + 3000 mg L(-1) P (phosphite) solution. The sampling rate was calculated as 15 determinations per hour, and the reagent consumption was about 6.3 mg of KMnO4, 200 mg of (NH4)6Mo7O24.4H2O, and 40 mg of ascorbic acid per measurement.

  2. Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

    Science.gov (United States)

    Yokochi, Reika

    2016-09-01

    Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

  3. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices.

    Science.gov (United States)

    Naccarato, Attilio; Pawliszyn, Janusz

    2016-09-01

    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future.

  4. Performance Evaluation of Fast Microfluidic Thermal Lysis of Bacteria for Diagnostic Sample Preparation

    Directory of Open Access Journals (Sweden)

    Evangelyn C. Alocilja

    2013-01-01

    Full Text Available Development of new diagnostic platforms that incorporate lab-on-a-chip technologies for portable assays is driving the need for rapid, simple, low cost methods to prepare samples for downstream processing or detection. An important component of the sample preparation process is cell lysis. In this work, a simple microfluidic thermal lysis device is used to quickly release intracellular nucleic acids and proteins without the need for additional reagents or beads used in traditional chemical or mechanical methods (e.g., chaotropic salts or bead beating. On-chip lysis is demonstrated in a multi-turn serpentine microchannel with external temperature control via an attached resistive heater. Lysis was confirmed for Escherichia coli by fluorescent viability assay, release of ATP measured with bioluminescent assay, release of DNA measured by fluorometry and qPCR, as well as bacterial culture. Results comparable to standard lysis techniques were achievable at temperatures greater than 65 °C and heating durations between 1 and 60 s.

  5. A rapid HPLC column switching method for sample preparation and determination of β-carotene in food supplements.

    Science.gov (United States)

    Brabcová, Ivana; Hlaváčková, Markéta; Satínský, Dalibor; Solich, Petr

    2013-11-15

    A simple and automated HPLC column-switching method with rapid sample pretreatment has been developed for quantitative determination of β-carotene in food supplements. Commercially samples of food supplements were dissolved in chloroform with help of saponification with 1M solution of sodium hydroxide in ultrasound bath. A 20-min sample dissolution/extraction step was necessary before chromatography analysis to transfer β-carotene from solid state of food supplements preparations (capsules,tablets) to chloroform solution. Sample volume - 3μL of chloroform phase was directly injected into the HPLC system. Next on-line sample clean-up was achieved on the pretreatment precolumn Chromolith Guard Cartridge RP-18e (Merck), 10×4.6mm, with a washing mobile phase (methanol:water, 92:8, (v/v)) at a flow rate of 1.5mL/min. Valve switch to analytical column was set at 2.5min in a back-flush mode. After column switching to the analytical column Ascentis Express C-18, 30×4.6mm, particle size 2.7μm (Sigma Aldrich), the separation and determination of β-carotene in food supplements was performed using a mobile phase consisting of 100% methanol, column temperature at 60°C and flow rate 1.5mL/min. The detector was set at 450nm. Under the optimum chromatographic conditions standard calibration curve was measured with good linearity - correlation coefficient for β-carotene (r(2)=0.999014; n=6) between the peak areas and concentration of β-carotene 20-200μg/mL. Accuracy of the method defined as a mean recovery was in the range 96.66-102.40%. The intraday method precision was satisfactory at three concentration levels 20, 125 and 200μg/mL and relative standard deviations were in the range 0.90-1.02%. The chromatography method has shown high sample throughput during column-switching pretreatment process and analysis in one step in short time (6min) of the whole chromatographic analysis.

  6. H2 Production Under Visible Light Irradiation from Aqueous Methanol Solution on CaTiO3:Cu Prepared by Spray Pyrolysis

    Science.gov (United States)

    Lim, Sung Nam; Song, Shin Ae; Jeong, Yong-Cheol; Kang, Hyun Woo; Park, Seung Bin; Kim, Ki Young

    2017-10-01

    Perovskite-type photocatalysts of CaCu x Ti1- x O3 (0 ≤ x ≤ 0.02) powder were prepared by spray pyrolysis of aqueous solution or aqueous solution with polymeric additive. The effects of the amount of copper ions doped in the photocatalyst and the precursor type on the photocatalytic activity under visible-light irradiation were investigated. The crystal structure, oxidation state, and light adsorption properties of the prepared photocatalysts were analyzed using x-ray diffraction, x-ray photoelectron spectroscopy, and diffuse reflectance spectroscopy, respectively. The doping of copper ions in CaTiO3 allowed visible-light absorption owing to a narrowing of the band gap energy of the host material through the formation of a new donor level for copper ions. Among the doped samples prepared from the aqueous precursor, CaTiO3 doped with 1 mol.% copper ions had the highest hydrogen evolution rate (140.7 μmol g-1 h-1). Notably, the hydrogen evolution rate of the photocatalyst doped with 1 mol.% copper ions prepared from the aqueous precursor with polymeric additive (295.0 μmol g-1 h-1) was two times greater than that prepared from the aqueous precursor, due to the morphology effect.

  7. Evaluation of sample preparation methods and optimization of nickel determination in vegetable tissues

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar

    2011-02-01

    Full Text Available Nickel, although essential to plants, may be toxic to plants and animals. It is mainly assimilated by food ingestion. However, information about the average levels of elements (including Ni in edible vegetables from different regions is still scarce in Brazil. The objectives of this study were to: (a evaluate and optimize a method for preparation of vegetable tissue samples for Ni determination; (b optimize the analytical procedures for determination by Flame Atomic Absorption Spectrometry (FAAS and by Electrothermal Atomic Absorption (ETAAS in vegetable samples and (c determine the Ni concentration in vegetables consumed in the cities of Lorena and Taubaté in the Vale do Paraíba, State of São Paulo, Brazil. By means of the analytical technique for determination by ETAAS or FAAS, the results were validated by the test of analyte addition and recovery. The most viable method tested for quantification of this element was HClO4-HNO3 wet digestion. All samples but carrot tissue collected in Lorena contained Ni levels above the permitted by the Brazilian Ministry of Health. The most disturbing results, requiring more detailed studies, were the Ni concentrations measured in carrot samples from Taubaté, where levels were five times higher than permitted by Brazilian regulations.

  8. Preparation of Magnetic Hollow Molecularly Imprinted Polymers for Detection of Triazines in Food Samples.

    Science.gov (United States)

    Wang, Aixiang; Lu, Hongzhi; Xu, Shoufang

    2016-06-22

    Novel magnetic hollow molecularly imprinted polymers (M-H-MIPs) were proposed for highly selective recognition and fast enrichment of triazines in food samples. M-H-MIPs were prepared on the basis of multi-step swelling polymerization, followed by in situ growth of magnetic Fe3O4 nanoparticles on the surface of hollow molecularly imprinted polymers (H-MIPs). Transmission electron microscopy and scanning electron microscopy confirmed the successful immobilization of Fe3O4 nanoparticles on the surface of H-MIPs. M-H-MIPs could be separated simply using an external magnet. The binding adsorption results indicated that M-H-MIPs displayed high binding capacity and fast mass transfer property and class selective property for triazines. Langmuir isotherm and pseudo-second-order kinetic models fitted the best adsorption models for M-H-MIPs. M-H-MIPs were used to analyze atrazine, simazine, propazine, and terbuthylazine in corn, wheat, and soybean samples. Satisfactory recoveries were in the range of 80.62-101.69%, and relative standard deviation was lower than 5.2%. Limits of detection from 0.16 to 0.39 μg L(-1) were obtained. When the method was applied to test positive samples that were contaminated with triazines, the results agree well with those obtained from an accredited method. Thus, the M-H-MIP-based dispersive solid-phase extraction method proved to be a convenient and practical platform for detection of triazines in food samples.

  9. Optimized sample preparation of endoscopic collected pancreatic fluid for SDS-PAGE analysis.

    Science.gov (United States)

    Paulo, Joao A; Lee, Linda S; Wu, Bechien; Repas, Kathryn; Banks, Peter A; Conwell, Darwin L; Steen, Hanno

    2010-07-01

    The standardization of methods for human body fluid protein isolation is a critical initial step for proteomic analyses aimed to discover clinically relevant biomarkers. Several caveats have hindered pancreatic fluid proteomics, including the heterogeneity of samples and protein degradation. We aim to optimize sample handling of pancreatic fluid that has been collected using a safe and effective endoscopic collection method (endoscopic pancreatic function test). Using SDS-PAGE protein profiling, we investigate (i) precipitation techniques to maximize protein extraction, (ii) auto-digestion of pancreatic fluid following prolonged exposure to a range of temperatures, (iii) effects of multiple freeze-thaw cycles on protein stability, and (iv) the utility of protease inhibitors. Our experiments revealed that TCA precipitation resulted in the most efficient extraction of protein from pancreatic fluid of the eight methods we investigated. In addition, our data reveal that although auto-digestion of proteins is prevalent at 23 and 37 degrees C, incubation on ice significantly slows such degradation. Similarly, when the sample is maintained on ice, proteolysis is minimal during multiple freeze-thaw cycles. We have also determined the addition of protease inhibitors to be assay-dependent. Our optimized sample preparation strategy can be applied to future proteomic analyses of pancreatic fluid.

  10. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Corina Mahu Ştefania

    2015-12-01

    Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

  11. Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Taflik, Ticiane; Antes, Fabiane G.; Paniz, Jose N.G.; Flores, Erico M.M.; Dressler, Valderi L., E-mail: valdres@quimica.ufsm.br [Departamento de Quimica, Universidade Federal de Santa Maria, RS (Brazil); Duarte, Fabio A. [Escola de Quimica e Alimentos, Universidade Federal do Rio Grande, Rio Grande, RS (Brazil); Flores, Eder L.M. [Coordenacao de Engenharia de Alimentos, Universidade Tecnologica Federal do Parana, Medianeira, PR (Brazil)

    2012-03-15

    Pyrohydrolysis was employed for mineral supplements decomposition prior to F, Br and I determination. Fluoride determination was carried out by potentiometry using a fluoride-ion selective electrode, whereas Br and I were determined by inductively coupled plasma mass spectrometry. The main parameters that influence on pyrohydrolysis were investigated. After evaluation, the following conditions were established: reactor temperature of 1000 deg C during 10 min; sample plus accelerator mass ratio of 1 + 5 and carrier gas (air) flow rate of 200 mL min{sup -1} . The accuracy of the proposed method was evaluated by analyte recovery tests and analysis of certified reference materials of phosphate rock and soil. Commercial mineral supplement samples were analyzed. The limits of quantification were 16, 0.3 and 0.07 {mu}g g{sup -1} for F, Br and I, respectively. By using a relatively simple and low cost pyrohydrolysis system up to 5 samples can be processed per hour. The developed sample preparation procedure can be routinely employed for F, Br and I determination in mineral supplements. (author)

  12. Preparative divergent flow IEF without carrier ampholytes for separation of complex biological samples.

    Science.gov (United States)

    Stastna, Miroslava; Slais, Karel

    2010-01-01

    Efficient separation method is a crucial part of the process in which components of highly complex biological sample are identified and characterized. Based on the principles of recently newly established electrophoretic method called divergent flow IEF (DF IEF), we have tested the DF IEF instrument which is able to operate without the use of background carrier ampholytes. We have verified that during separation and focusing of sample consisting of high numbers of proteins (yeast lysate and wheat flour extract), the pH gradient of preparative DF IEF can be created by autofocusing of the sample components themselves without any addition of carrier ampholytes. In DF IEF, the proteins are separated, desalted and concentrated in one step. The fractions of yeast lysate sample, collected at the DF IEF output and subjected to gel IEF, contained the zones of proteins gradually covering the pI values from 3.7 to 8.5. In our experimental arrangement, the highest number of proteins has been found in fractions with pI values around 5.3 as detected by polyacrylamide gel IEF with CBB staining. During DF IEF, the selected protein bands have been concentrated up to 16.8-fold.

  13. Sample preparation for scanning electron microscopy of plant surfaces--horses for courses.

    Science.gov (United States)

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

    2008-12-01

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

  14. RNA SAMPLE PREPARATION APPLIED TO GENE EXPRESSION PROFILING FOR THE HORSE BIOLOGICAL PASSPORT.

    Science.gov (United States)

    Bailly-Chouriberry, Ludovic; Baudoin, Florent; Cormant, Florence; Glavieux, Yohan; Loup, Benoit; Garcia, Patrice; Popot, Marie-Agnès; Bonnaire, Yves

    2017-04-05

    The improvement of doping control is an on-going race. Techniques to fight against doping are usually based on the direct detection of drugs or their metabolites by analytical methods such as chromatography hyphenated to mass spectrometry after ad hoc sample preparation. Nowadays, omic methods constitute an attractive development and advances have been achieved particularly by application of molecular biology tools for detection of anabolic androgenic steroids (AAS), erythropoiesis-stimulating agent (ESA) or to control human growth hormone misuses. These interesting results across different animal species have suggested that modification of gene expression offers promising new methods of improving the window of detection of banned substances by targeting their effects on blood cell gene expression. In this context, the present study describes the possibility of using a modified version of the dedicated Human IVD (in vitro Diagnostics) PAXgene® Blood RNA Kit for horse gene expression analysis in blood collected on PAXgene® tubes applied to the Horse Biological Passport. The commercial kit was only approved for human blood samples and has required an optimization of specific technical requirements for equine blood samples. Improvements and recommendations were achieved for sample collection, storage and RNA extraction procedure. Following these developments, RNA yield and quality were demonstrated to be suitable for downstream gene expression analysis by qPCR techniques.

  15. Buffer-free therapeutic antibody preparations provide a viable alternative to conventionally buffered solutions: from protein buffer capacity prediction to bioprocess applications.

    Science.gov (United States)

    Bahrenburg, Sven; Karow, Anne R; Garidel, Patrick

    2015-04-01

    Protein therapeutics, including monoclonal antibodies (mAbs), have significant buffering capacity, particularly at concentrations>50 mg/mL. This report addresses pH-related issues critical to adoption of self-buffered monoclonal antibody formulations. We evaluated solution conditions with protein concentrations ranging from 50 to 250 mg/mL. Samples were both buffer-free and conventionally buffered with citrate. Samples were non-isotonic or adjusted for isotonicity with NaCl or trehalose. Studies included accelerated temperature stability tests, shaking stability studies, and pH changes in infusion media as protein concentrate is added. We present averaged buffering slopes of capacity that can be applied to any mAb and present a general method for calculating buffering capacity of buffer-free, highly concentrated antibody liquid formulations. In temperature stability tests, neither buffer-free nor conventionally buffered solution conditions showed significant pH changes. Conventionally buffered solutions showed significantly higher opalescence than buffer-free ones. In general, buffer-free solution conditions showed less aggregation than conventionally buffered solutions. Shaking stability tests showed no differences between buffer-free and conventionally buffered solutions. "In-use" preparation experiments showed that pH in infusion bag medium can rapidly approximate that of self-buffered protein concentrate as concentrate is added. In summary, the buffer capacity of proteins can be predicted and buffer-free therapeutic antibody preparations provide a viable alternative to conventionally buffered solutions. Copyright © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Preparation and analysis of dust samples for medical examinations; Praeparation und Analytik der Staubproben fuer medizinische Untersuchungen

    Energy Technology Data Exchange (ETDEWEB)

    Armbruster, L. [Deutsche Montan Technologie GmbH, Essen (Germany). Gas and Fire Div.

    2004-07-01

    For medical research within this project three respirable dust samples have been prepared and analysed. The original bulk material came from three different stratigraphic horizons, for the preparation a multiplex classifier was used. The respirable samples showed the same size distribution as the samples used in former projects. The quartz content was rather low, but within the normal variability. Pure quartz particles without surface contamination are not present in the three samples. Nickel, lead, cobalt, and arsenic are the most significant trace elements in the samples. (orig.)

  17. Preparing and measuring ultra-small radiocarbon samples with the ARTEMIS AMS facility in Saclay, France

    Energy Technology Data Exchange (ETDEWEB)

    Delque-Kolic, E., E-mail: emmanuelle.delque-kolic@cea.fr [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France); Comby-Zerbino, C.; Ferkane, S.; Moreau, C.; Dumoulin, J.P.; Caffy, I.; Souprayen, C.; Quiles, A.; Bavay, D.; Hain, S.; Setti, V. [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France)

    2013-01-15

    The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18 ml for the first line and 12 ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10 {mu}g of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5 mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring {sup 14}C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1 {+-} 0.8 and 0.2 {+-} 0.1 {mu}g, respectively. The results presented here were obtained for IAEA-C1, {sup 14}C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

  18. Automation of sample preparation for mass cytometry barcoding in support of clinical research: protocol optimization.

    Science.gov (United States)

    Nassar, Ala F; Wisnewski, Adam V; Raddassi, Khadir

    2017-03-01

    Analysis of multiplexed assays is highly important for clinical diagnostics and other analytical applications. Mass cytometry enables multi-dimensional, single-cell analysis of cell type and state. In mass cytometry, the rare earth metals used as reporters on antibodies allow determination of marker expression in individual cells. Barcode-based bioassays for CyTOF are able to encode and decode for different experimental conditions or samples within the same experiment, facilitating progress in producing straightforward and consistent results. Herein, an integrated protocol for automated sample preparation for barcoding used in conjunction with mass cytometry for clinical bioanalysis samples is described; we offer results of our work with barcoding protocol optimization. In addition, we present some points to be considered in order to minimize the variability of quantitative mass cytometry measurements. For example, we discuss the importance of having multiple populations during titration of the antibodies and effect of storage and shipping of labelled samples on the stability of staining for purposes of CyTOF analysis. Data quality is not affected when labelled samples are stored either frozen or at 4 °C and used within 10 days; we observed that cell loss is greater if cells are washed with deionized water prior to shipment or are shipped in lower concentration. Once the labelled samples for CyTOF are suspended in deionized water, the analysis should be performed expeditiously, preferably within the first hour. Damage can be minimized if the cells are resuspended in phosphate-buffered saline (PBS) rather than deionized water while waiting for data acquisition.

  19. The influence of swabbing solutions on DNA recovery from touch samples.

    Science.gov (United States)

    Thomasma, Sarah M; Foran, David R

    2013-03-01

    There has been minimal research into how to best obtain DNA from touch samples. Many forensic laboratories simply moisten a swab with water and use it for collecting cells/DNA from evidentiary samples. However, this and other methods have not been objectively studied in order to maximize DNA yields. In this study, fingerprints were collected using swabs moistened with water or laboratory or commercially available detergents, including sodium dodecyl sulfate (SDS), Triton X-100, Tween 20, Formula 409(®) , and Simple Green(®) . Prints were swabbed, DNA isolated using an organic extraction, yields quantified, and relative yields compared. In all cases, the detergent-based swabbing solutions outperformed water, with SDS and Triton X-100 producing significant increases in yield. Short tandem repeat profiles were consistent with the individuals that placed them. Subsequent analysis of SDS concentrations for collecting touch DNA demonstrated an increase in DNA yield with increasing SDS concentration, with an optimal concentration of approximately 2%.

  20. Results For The Third Quarter Calendar Year 2016 Tank 50H Salt Solution Sample

    Energy Technology Data Exchange (ETDEWEB)

    Crawford, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-10-13

    In this memorandum, the chemical and radionuclide contaminant results from the Third Quarter Calendar Year 2016 (CY16) sample of Tank 50H salt solution are presented in tabulated form. The Third Quarter CY16 Tank 50H samples (a 200 mL sample obtained 6” below the surface (HTF-5-16-63) and a 1 L sample obtained 66” from the tank bottom (HTF-50-16-64)) were obtained on July 14, 2016 and received at Savannah River National Laboratory (SRNL) on the same day. Prior to obtaining the samples from Tank 50H, a single pump was run at least 4.4 hours and the samples were pulled immediately after pump shut down. The information from this characterization will be used by Defense Waste Processing Facility (DWPF) & Saltstone Facility Engineering for the transfer of aqueous waste from Tank 50H to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets.2 Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the Task Technical and Quality Assurance Plan (TTQAP) for the Tank 50H saltstone task. The chemical and radionuclide contaminant results from the characterization of the Third Quarter CY16 sampling of Tank 50H were requested by Savannah River Remediation (SRR) personnel and details of the testing are presented in the SRNL TTQAP.

  1. Results For The Third Quarter Calendar Year 2016 Tank 50H Salt Solution Sample

    Energy Technology Data Exchange (ETDEWEB)

    Crawford, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-10-13

    In this memorandum, the chemical and radionuclide contaminant results from the Third Quarter Calendar Year 2016 (CY16) sample of Tank 50H salt solution are presented in tabulated form. The Third Quarter CY16 Tank 50H samples (a 200 mL sample obtained 6” below the surface (HTF-5-16-63) and a 1 L sample obtained 66” from the tank bottom (HTF-50-16-64)) were obtained on July 14, 2016 and received at Savannah River National Laboratory (SRNL) on the same day. Prior to obtaining the samples from Tank 50H, a single pump was run at least 4.4 hours, and the samples were pulled immediately after pump shut down. The information from this characterization will be used by Defense Waste Processing Facility (DWPF) & Saltstone Facility Engineering for the transfer of aqueous waste from Tank 50H to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the Task Technical and Quality Assurance Plan (TTQAP) for the Tank 50H saltstone task. The chemical and radionuclide contaminant results from the characterization of the Third Quarter CY16 sampling of Tank 50H were requested by Savannah River Remediation (SRR) personnel and details of the testing are presented in the SRNL TTQAP.

  2. Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

    Energy Technology Data Exchange (ETDEWEB)

    Pietrzyńska, Monika, E-mail: monikapietrzynska@gmail.com; Voelkel, Adam; Bielicka-Daszkiewicz, Katarzyna

    2013-05-07

    Graphical abstract: -- Highlights: •MINE device for isolation of analytes from water samples. •Nine polymer poly(styrene-divinylbenzene) monoliths prepared in stainless steel needles. •High efficiency of in-needle extraction systems based on monolithic materials. •New possibilities in sample preparation area. -- Abstract: Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg.

  3. Preparation and characterization of superparamagnetic molecularly imprinted polymers for selective adsorption and separation of vanillin in food samples.

    Science.gov (United States)

    Ning, Fangjian; Peng, Hailong; Dong, Liling; Zhang, Zhong; Li, Jinhua; Chen, Lingxin; Xiong, Hua

    2014-11-19

    Novel water-compatible superparamagnetic molecularly imprinted polymers (M-MIPs) were prepared by coating superparamagnetic Fe3O4 nanoparticles with MIPs in a methanol-water reaction system. The M-MIPs were used for the selective adsorption and separation of vanillin from aqueous solution. The M-MIPs were characterized by X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), vibrating sample magnetometry (VSM), and scanning electron microscopy (SEM). Results indicated that a core-shell structure of M-MIPs was obtained by coating a layer of silica and MIPs on the surface of the Fe3O4 nanoparticles. The obtained M-MIPs possess a loose and porous structure and can be rapidly separated from the solution using a magnet. The adsorption experiments showed that the binding capacity of the M-MIPs was significantly higher than that of the superparamagnetic non-molecularly imprinted polymers (M-NIPs). Meanwhile, the adsorption of M-MIPs reached equilibrium within 100 min, and the apparent maximum adsorption quantity (Qmax) and dissociation constant (Kd) were 64.12 μmol g(-1) and 58.82 μmol L(-1), respectively. The Scatchard analysis showed that homogeneous binding sites were formed on the M-MIP surface. The recoveries of 83.39-95.58% were achieved when M-MIPs were used for the pre-concentration and selective separation of vanillin in spiked food samples. These results provided the possibility for the separation and enrichment of vanillin from complicated food matrices by M-MIPs.

  4. Ce1-xLaxOy solid solution prepared from mixed rare earth chloride for soot oxidation

    Institute of Scientific and Technical Information of China (English)

    韩雪; 王亚飞; 郝红蕊; 郭荣贵; 胡运生; 蒋文全

    2016-01-01

    Ce1–xLaxOy solid solution was simply prepared using mixed rare earth chloride (RECl3·xH2O, RE=Ce, La>99%, containing unseparated Ce and La from rare earth metallurgical industry) as precursor by ultrasonic-assisted co-precipitation method with differ-ent ultrasonic frequencies (CLf,f=200, 400, 600, 800, 1000 Hz). A compared Ce1–xLaxOy solid solution (CL*) was also prepared by the same mothod with 10% less precipitant. X-ray diffraction results confirmed the formation of Ce1–xLaxOy solid solution, and the crystal structures of these catalysts were not very sensitive to ultrasonic frequency and precipitant amount. However, both of the fac-tors had obvious effect on morphology and surface area of CL, and precipitant amount seem to play a more crucial role than ultra-sonic frequency for Ce1–xLaxOy solid solution preparation. When soot and catalyst were tight contacted, the peak temperature (Tpeak) of soot oxidation and oxygen reducing temperature for CLf catalysts decreased linearly with increasing surface area. Under loose contact condition, theTpeak had obvious negative correlation with H2 consumption. It was inferred that good reducibility of the Ce1–xLaxOy solid solution favored the soot oxidation reaction. The Ce1–xLaxOy solid solution prepared from unseparated rare earth chloride showed a good soot oxidaiton activity. Controlling the preparation conditions to prepare a CL catalyst would high surface area will enhance its reducibility and activity.

  5. Automated nanoliter solution deposition for total reflection X-ray fluorescence analysis of semiconductor samples

    Energy Technology Data Exchange (ETDEWEB)

    Sparks, Chris M. [Process Characterization Laboratory, ATDF, Austin, TX 78741 (United States)]. E-mail: chris.sparks@atdf.com; Gondran, Carolyn H. [Process Characterization Laboratory, ATDF, Austin, TX 78741 (United States); Havrilla, George J. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Hastings, Elizabeth P. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2006-11-15

    In this study, a BioDot BioJet dispensing system was investigated as a nanoliter sample deposition method for total reflection X-ray fluorescence (TXRF) analysis. The BioDot system was programmed to dispense arrays of 20 nL droplets of sample solution on Si wafers. Each 20 nL droplet was approximately 100 {mu}m in diameter. A 10 x 10 array (100 droplets) was deposited and dried in less than 2 min at room temperature and pressure, demonstrating the efficiency of the automated deposition method. Solutions of various concentrations of Ni and Ni in different matrices were made from stock trace element standards to investigate of the effect of the matrix on the TXRF signal. The concentrations were such that the levels of TXRF signal saturation could be examined. Arrays were deposited to demonstrate the capability of drying 100 {mu}L of vapor phase decomposition-like residue in the area of a typical TXRF detector.

  6. A general solution and approximation for the diffusion of gas in a spherical coal sample

    Institute of Scientific and Technical Information of China (English)

    Wang Yucang; Xue Sheng; Xie Jun

    2014-01-01

    The square root relationship of gas release in the early stage of desorption is widely used to provide a simple and fast estimation of the lost gas in coal mines. However, questions arise as to how the relation-ship was theoretically derived, what are the assumptions and applicable conditions and how large the error will be. In this paper, the analytical solutions of gas concentration and fractional gas loss for the dif-fusion of gas in a spherical coal sample were given with detailed mathematical derivations based on the diffusion equation. The analytical solutions were approximated in case of small values of time and the error analyses associated with the approximation were also undertaken. The results indicate that the square root relationship of gas release is the first term of the approximation, and care must be taken in using the square root relationship as a significant error might be introduced with increase in the lost time and decrease in effective diameter of a spherical coal sample.

  7. Inverse problems with non-trivial priors: efficient solution through sequential Gibbs sampling

    DEFF Research Database (Denmark)

    Hansen, Thomas Mejer; Cordua, Knud Skou; Mosegaard, Klaus

    2012-01-01

    Markov chain Monte Carlo methods such as the Gibbs sampler and the Metropolis algorithm can be used to sample solutions to non-linear inverse problems. In principle, these methods allow incorporation of prior information of arbitrary complexity. If an analytical closed form description of the pri...... also reduce the computation time for the inversion dramatically. The method works for any statistical model for which sequential simulation can be used to generate realizations. This applies to most algorithms developed in the geostatistical community.......Markov chain Monte Carlo methods such as the Gibbs sampler and the Metropolis algorithm can be used to sample solutions to non-linear inverse problems. In principle, these methods allow incorporation of prior information of arbitrary complexity. If an analytical closed form description of the prior...... for applying the sequential Gibbs sampler and illustrate how it works. Through two case studies, we demonstrate the application of the method to a linear image restoration problem and to a non-linear cross-borehole inversion problem. We demonstrate how prior information can reduce the complexity of an inverse...

  8. Formation of a 25 mol% Fe2O3-Al2O3 solid solution prepared by ball milling

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Mørup, Steen; Linderoth, Søren

    1996-01-01

    The phase transformation process of a 25 mol% Fe2O3-Al2O3 powder mixture during high-energy ball milling has been studied by x-ray diffraction and Mossbauer spectroscopy. A metastable solid solution of 25 mol % Fe2O3 in Al2O3 with corundum structure has successfully been prepared after a milling...... time of 122 h. This demonstrates that the high-energy ball milling technique is able to prepare metastable solid solutions with an extended range of compositions in ceramic/ceramic systems with a positive hear of mixing....

  9. Preparation of Al(OH)3 by ion membrane electrolysis and precipitation of sodium aluminate solution with seeds

    Institute of Scientific and Technical Information of China (English)

    LI Yuan-gao; CHEN Qi-yuan; WANG Song-sen; YIN Zhou-lan; ZHANG Ping-min

    2008-01-01

    The preparation of Al(OH)3 by the ion exchange membrane electrolysis followed by the precipitation of sodium aluminate solution with seeds was made. During the process of ion membrane electrolysis, the sodium aluminate solution is rapidly acidified and the caustic ratio (aK) is decreased due to oxygen evolution in the anodic region. And the causticity of solution is increased due to hydrogen evolution in the cathode region, producing the high concentration of caustic soda solution. Regulating the acidity of the anodic solution by controlling the electric quantity in the electrolysis and subsequent decomposing the solution, Al(OH)3 could yield with very large rate and high efficiency. The experiments also indicate that the quality of aluminum hydroxide product is greatly affected by the impurity silicon.

  10. Microwave processing for sample preparation to evaluate mitochondrial ultrastructural damage in hemorrhagic shock.

    Science.gov (United States)

    Josephsen, Gary D; Josephsen, Kelly A; Beilman, Greg J; Taylor, Jodie H; Muiler, Kristine E

    2005-12-01

    This is a report of the adaptation of microwave processing in the preparation of liver biopsies for transmission electron microscopy (TEM) to examine ultrastructural damage of mitochondria in the setting of metabolic stress. Hemorrhagic shock was induced in pigs via 35% total blood volume bleed and a 90-min period of shock followed by resuscitation. Hepatic biopsies were collected before shock and after resuscitation. Following collection, biopsies were processed for TEM by a rapid method involving microwave irradiation (Giberson, 2001). Samples pre- and postshock of each of two animals were viewed and scored using the mitochondrial ultrastructure scoring system (Crouser et al., 2002), a system used to quantify the severity of ultrastructural damage during shock. Results showed evidence of increased ultrastructural damage in the postshock samples, which scored 4.00 and 3.42, versus their preshock controls, which scored 1.18 and 1.27. The results of this analysis were similar to those obtained in another model of shock (Crouser et al., 2002). However, the amount of time used to process the samples was significantly shortened with methods involving microwave irradiation.

  11. Using Exclusion-Based Sample Preparation (ESP to Reduce Viral Load Assay Cost.

    Directory of Open Access Journals (Sweden)

    Scott M Berry

    Full Text Available Viral load (VL measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD, accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1 and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP.71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL and high accuracy (average difference between methods of 0.08 log, R2 = 0.97. Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  12. Using Exclusion-Based Sample Preparation (ESP) to Reduce Viral Load Assay Cost.

    Science.gov (United States)

    Berry, Scott M; Pezzi, Hannah M; Williams, Eram D; Loeb, Jennifer M; Guckenberger, David J; Lavanway, Alex J; Puchalski, Alice A; Kityo, Cissy M; Mugyenyi, Peter N; Graziano, Franklin M; Beebe, David J

    2015-01-01

    Viral load (VL) measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD), accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1) and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP).71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL) and high accuracy (average difference between methods of 0.08 log, R2 = 0.97). Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  13. Modular approach to customise sample preparation procedures for viral metagenomics: a reproducible protocol for virome analysis.

    Science.gov (United States)

    Conceição-Neto, Nádia; Zeller, Mark; Lefrère, Hanne; De Bruyn, Pieter; Beller, Leen; Deboutte, Ward; Yinda, Claude Kwe; Lavigne, Rob; Maes, Piet; Van Ranst, Marc; Heylen, Elisabeth; Matthijnssens, Jelle

    2015-11-12

    A major limitation for better understanding the role of the human gut virome in health and disease is the lack of validated methods that allow high throughput virome analysis. To overcome this, we evaluated the quantitative effect of homogenisation, centrifugation, filtration, chloroform treatment and random amplification on a mock-virome (containing nine highly diverse viruses) and a bacterial mock-community (containing four faecal bacterial species) using quantitative PCR and next-generation sequencing. This resulted in an optimised protocol that was able to recover all viruses present in the mock-virome and strongly alters the ratio of viral versus bacterial and 16S rRNA genetic material in favour of viruses (from 43.2% to 96.7% viral reads and from 47.6% to 0.19% bacterial reads). Furthermore, our study indicated that most of the currently used virome protocols, using small filter pores and/or stringent centrifugation conditions may have largely overlooked large viruses present in viromes. We propose NetoVIR (Novel enrichment technique of VIRomes), which allows for a fast, reproducible and high throughput sample preparation for viral metagenomics studies, introducing minimal bias. This procedure is optimised mainly for faecal samples, but with appropriate concentration steps can also be used for other sample types with lower initial viral loads.

  14. ROTOR AND SCREW TECHNOLOGICAL SYSTEMS FOR PREPARATION OF SOLUTIONS AND CONCRETE

    Directory of Open Access Journals (Sweden)

    Belokur K. A.

    2016-04-01

    Full Text Available We have provided technical solutions to improve performance of technological systems for the preparation of solutions and concrete based on the use of screw rotors in the form of drums with helix lines formed on the perimeter as interconnect lines of his spiral surfaces. We discuss the six varieties of devices and installations for mixing, including concrete mixers, reels which are of a complicated geometric body formed by helical surfaces with variable or constant pitch and which creates screw lines in the places of their connection. In the form of screw drums, they may be conical, concave, convex, cylindrical. The experimental test was conducted on the concrete mixer drums, which are arranged one in the other. The implementation of the mixer in the form of coaxially edited two barrels provides not only a reduction in size in length, but a significant reduction in energy consumption due to the use of heat, released during the activation process of inert heating of the concrete mix as when re-mixing and concrete mix when mixing it with water and transportation. The drums of such systems is made of flat elements with the formation of the helical lines discretely spaced around the perimeter of different pitch and with different numbers directed towards each other helical surfaces. In the process of transporting the components of concrete in the internal screw drum there is active mixture of sand, gravel and cement. Thus, there is not only the destruction of lumpy, sticky components of the raw materials, but also active uniform distribution of particles of cement, sand and gravel into a homogenous mass. The implementation of the proposed technology and equipment ensures not only reduction of the dimensions of the mixer length, but also improving the quality of finished products, as well as potential cement savings of 3-5%

  15. Preparation of xerogel SiO2 from roasted iron sand under various acidic solution

    Science.gov (United States)

    Ramelan, A. H.; Wahyuningsih, S.; Ismoyo, Y. A.; Pranata, H. P.; Munawaroh, H.

    2016-11-01

    Xerogel SiO2 had been prepared from roasted iron sand through variation of Na2CO3 addition and sol-gel process under various acidic solution. Roasting treatment was carried out on the compositional variation of iron sand:Na2CO3 = 1:2; 1:1 and 2:1 at 1100 °C. While the sol-gel process was conducted at room temperature and neutralized using HCl 0.1 M and 6 M. The color characteristics of roasted iron sand shown light brown, dark brown and dark gray of the compositional variation of iron sand:Na2CO3 = 1:2; 1:1 and 2:1, respectively. In addition, the levels of thoughness increased by increasing the ratio of sand in the composition of the mixture. The best composition of roasted treatment was at a variety of iron sand:Na2SiO3 = 1:2 with 57.72% had been dissolved in hot water. The addition of Na2CO3 will influence the Na2SiO3 formation, because of the increase of Na2CO3 capable produced the iron sand decomposition product. Na2SiO3 gel had been produced after it was neutralized with certain amount of HCl solution. The neutralization was more effective if using high concentration of HCl because of the formation of gel SiO2 will be easier occurred. The results of SiO2 had been identified by the FTIR spectra, which an absorption spectra of Si-O-Si asymmetric stretching at 1098.51 cm-1, symmetric stretching of Si-O-Si at 804.35 cm-1 and the bending O-Si-O at 469.69 cm'1. The result of SiO2 content by XRF analysis is about 85.15%.

  16. Effects of sample preparation on the optical properties of breast tissue

    Science.gov (United States)

    Marks, Fay A.

    1996-04-01

    The optical properties of biological tissue should be determined in vivo whenever possible. However, for those instances when in vivo studies are impractical, too expensive or inappropriate, and when blood flow is not an issue, the ability to perform in vitro studies then becomes invaluable. Optical absorption spectroscopy shows that it may be possible to obtain meaningful information about the optical properties of human breast tissue from in vitro samples if strict preparation and measuring protocols are used. That a strict protocol for storing and handling tissue is critical can be seen from our observations of changes in the optical absorption spectra that occur in response to formalin fixation, the passage of time, application of stains and dyes, and storage in growth medium of the excised tissue. In vivo optical absorption spectroscopy measurements have been made on human breast cancer xenografts and compared with in vitro measurements on breast biopsies prepared according to precise collection and treatment protocols. There is a 'window of opportunity' before time dependent changes in the UV optical absorption spectra of the excised tissue specimens occur. This time window of opportunity widens at longer wavelengths with the least changes occurring in the optical spectra in the NIR.

  17. Lights Will Guide You : Sample Preparation and Applications for Integrated Laser and Electron Microscopy

    Science.gov (United States)

    Karreman, M. A.

    2013-03-01

    Correlative microscopy is the combined use of two different forms of microscopy in the study of a specimen, allowing for the exploitation of the advantages of both imaging tools. The integrated Laser and Electron Microscope (iLEM), developed at Utrecht University, combines a fluorescence microscope (FM) and a transmission electron microscope (TEM) in a single set-up. The region of interest in the specimen is labeled or tagged with a fluorescent probe and can easily be identified within a large field of view with the FM. Next, this same area is retraced in the TEM and can be studied at high resolution. The iLEM demands samples that can be imaged with both FM and TEM. Biological specimen, typically composed of light elements, generate low image contrast in the TEM. Therefore, these samples are often ‘contrasted’ with heavy metal stains. FM, on the other hand, images fluorescent samples. Sample preparation for correlative microscopy, and iLEM in particular, is complicated by the fact that the heavy metals stains employed for TEM quench the fluorescent signal of the probe that is imaged with FM. The first part of this thesis outlines preparation procedures for biological material yielding specimen that can be imaged with the iLEM. Here, approaches for the contrasting of thin sections of cells and tissue are introduced that do not affect the fluorescence signal of the probe that marks the region of interest. Furthermore, two novel procedures, VIS2FIXH and VIS2FIX­FS are described that allow for the chemical fixation of thin sections of cryo-immobilized material. These procedures greatly expedite the sample preparation process, and open up novel possibilities for the immuno-labeling of difficult antigens, eg. proteins and lipids that are challenging to preserve. The second part of this thesis describes applications of iLEM in research in the field of life and material science. The iLEM was employed in the study of UVC induced apoptosis (programmed cell death) of

  18. Sample Preparation for Headspace GC Analysis of Residual Solvents in Hyaluronic Acid Derivative Fiber

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hoon Joo; Kim, Dong Min; Yang, Jeong Soo [LG life Sciences, Ltd./R and D Park, Daejeon (Korea, Republic of); Kim, Chan Wha [Korea University, Seoul (Korea, Republic of)

    2006-02-15

    The aim of this study is to develop efficient sample preparation method for HS-GC analysis of residual solvents in HA derivative fiber. Compared to direct extraction of residual solvents from HA derivative fiber, the extraction through the hydrolysis of HA derivative fiber by HAse gave more complete and higher reproducible quantification of residual solvent. To validate HS-GC analysis method of residual solvents, specificity, limits of detection and quantification, linearity, accuracy and precision are investigated in the study. HA derivative fiber was hydrolyzed using HAse for headspace gas chromatographic analysis of residual solvents of ethanol, acetone and isopropanol in HA derivative fiber. This study showed that the developed method had specificity, linearity, accuracy and precision. In addition, it demonstrated that HS-GC coupled with matrix-breaking method such as hydrolysis was available for the determination of residual solvents in a matrix like HA derivative fiber.

  19. Applied Study on Magnetic Nanometer Beads in Preparation of Genechip Samples

    Institute of Scientific and Technical Information of China (English)

    陈慧; 高华方; 谢欣; 马雪梅; 杨渝珍

    2004-01-01

    Summary: A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid-phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads with karyocyte as template directly and the PCR products were applied on an oligonucleotide array to do gene typing. The HLA-A PCR amplification system and a small HLA-A oligonucleotide microarray were applied as the platform and an experiment protocol of separating karyocyte from whole blood using the magnetic nanometer beads (Fe2O3) were set up.The experimental conditions were also discussed. It showed that pH level of PBS eluent, Taq enzyme quantity and fragment length of products could influent the amplification results, and the magnetic nano-beads could succeed in sample preparation in microarray to provide a promising way in automatic detection and lab-on-a-chip.

  20. NGSI FY15 Final Report. Innovative Sample Preparation for in-Field Uranium Isotopic Determinations

    Energy Technology Data Exchange (ETDEWEB)

    Yoshida, Thomas M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Meyers, Lisa [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-11-10

    Our FY14 Final Report included an introduction to the project, background, literature search of uranium dissolution methods, assessment of commercial off the shelf (COTS) automated sample preparation systems, as well as data and results for dissolution of bulk quantities of uranium oxides, and dissolution of uranium oxides from swipe filter materials using ammonium bifluoride (ABF). Also, discussed were reaction studies of solid ABF with uranium oxide that provided a basis for determining the ABF/uranium oxide dissolution mechanism. This report details the final experiments for optimizing dissolution of U3O8 and UO2 using ABF and steps leading to development of a Standard Operating Procedure (SOP) for dissolution of uranium oxides on swipe filters.

  1. Agarose- and alginate-based biopolymers for sample preparation: Excellent green extraction tools for this century.

    Science.gov (United States)

    Sanagi, Mohd Marsin; Loh, Saw Hong; Wan Ibrahim, Wan Nazihah; Pourmand, Neda; Salisu, Ahmed; Wan Ibrahim, Wan Aini; Ali, Imran

    2016-03-01

    Recently, there has been considerable interest in the use of miniaturized sample preparation techniques before the chromatographic monitoring of the analytes in unknown complex compositions. The use of biopolymer-based sorbents in solid-phase microextraction techniques has achieved a good reputation. A great variety of polysaccharides can be extracted from marine plants or microorganisms. Seaweeds are the major sources of polysaccharides such as alginate, agar, agarose, as well as carrageenans. Agarose and alginate (green biopolymers) have been manipulated for different microextraction approaches. The present review is focused on the classification of biopolymer and their applications in multidisciplinary research. Besides, efforts have been made to discuss the state-of-the-art of the new microextraction techniques that utilize commercial biopolymer interfaces such as agarose in liquid-phase microextraction and solid-phase microextraction.

  2. ALGORITHM OF PREPARATION OF THE TRAINING SAMPLE USING 3D-FACE MODELING

    Directory of Open Access Journals (Sweden)

    D. I. Samal

    2016-01-01

    Full Text Available The algorithm of preparation and sampling for training of the multiclass qualifier of support vector machines (SVM is provided. The described approach based on the modeling of possible changes of the face features of recognized person. Additional features like perspectives of shooting, conditions of lighting, tilt angles were introduced to get improved identification results. These synthetic generated changes have some impact on the classifier learning expanding the range of possible variations of the initial image. The classifier learned with such extended example is ready to recognize unknown objects better. The age, emotional looks, turns of the head, various conditions of lighting, noise, and also some combinations of the listed parameters are chosen as the key considered parameters for modeling. The third-party software ‘FaceGen’ allowing to model up to 150 parameters and available in a demoversion for free downloading is used for 3D-modeling.The SVM classifier was chosen to test the impact of the introduced modifications of training sample. The preparation and preliminary processing of images contains the following constituents like detection and localization of area of the person on the image, assessment of an angle of rotation and an inclination, extension of the range of brightness of pixels and an equalization of the histogram to smooth the brightness and contrast characteristics of the processed images, scaling of the localized and processed area of the person, creation of a vector of features of the scaled and processed image of the person by a Principal component analysis (algorithm NIPALS, training of the multiclass SVM-classifier.The provided algorithm of expansion of the training selection is oriented to be used in practice and allows to expand using 3D-models the processed range of 2D – photographs of persons that positively affects results of identification in system of face recognition. This approach allows to compensate

  3. NANO-STRUCTURED SILVER COATING ON COPPER PREPARED IN AN ETHANOL-BASED SOLUTION

    Institute of Scientific and Technical Information of China (English)

    Zheliang Wei; Dian Tang; Thomas O'Keefe

    2005-01-01

    Recently, silver as an electrochemical deposit on copper substrate has been attracting much attention in the microelectronics field. To deposit nano-scale silver particles on copper, immersion plating using cyanide-based baths is commonly used. In this study, non-toxic ethanol was used as the plating solution. Sputtered copper samples were terized by a field emission scanning electron microscope (FE-SEM), an energy dispersive X-ray spectroscope (EDS),and an atomic force microscope (AFM). It was found that the deposited particles are metallic silver. After 3 s immersion,fine particles whose diameters were around 6 nm had covered about 40% of the surface of the copper substrate. After10 s immersion, the copper surface was completely covered by silver particles, the diameters of which have increased to about 10-15 nm. After the whole surface was covered, a dense and smooth silver coating was obtained.

  4. Preparation of SrZrO3 Thermal Barrier Coating by Solution Precursor Plasma Spray

    Science.gov (United States)

    Li, Xinhui; Ma, Wen; Wen, Jing; Bai, Yu; Sun, Li; Chen, Baodong; Dong, Hongying; Shuang, Yingchai

    2017-02-01

    The solution precursor plasma spray (SPPS) process is capable of depositing highly durable thermal barrier coatings (TBCs). In this study, an aqueous chemical precursor feedstock was injected into the plasma jet to deposit SrZrO3 thermal barrier coating on metal substrate. Taguchi design of experiments was employed to optimize the SPPS process. The thermal characteristics and phase evolution of the SrZrO3 precursor, as well as the influence of various spray parameters on the coating deposition rate, microhardness, microstructure, and phase stability, were investigated. The experimental results showed that, at given spray distance, feedstock flow rate, and atomization pressure, the optimized spray parameters were arc current of 600 A, argon flow rate of 40 L/min, and hydrogen flow rate of 10 L/min. The SrZrO3 coating prepared using the optimized spray parameters had single-pass thickness of 6.0 μm, porosity of 18%, and microhardness of 6.8 ± 0.1 GPa. Phase stability studies indicated that the as-sprayed SrZrO3 coating had good phase stability in the temperature range from room temperature to 1400 °C, gradually exhibiting a phase transition from t'-ZrO2 to m-ZrO2 in the SrZrO3 coating at 1450 °C with increasing time, while the SrZrO3 phase did not change.

  5. Preparation, Structural and Dielectric Properties of Solution Grown Polyvinyl Alcohol(PVA) Film

    Science.gov (United States)

    Nangia, Rakhi; Shukla, Neeraj K.; Sharma, Ambika

    2017-08-01

    Flexible dielectrics with high permittivity have been investigated extensively due to their applications in electronic industry. In this work, structural and electrical characteristics of polymer based film have been analysed. Poly vinyl alcohol (PVA) film was prepared by solution casting method. X-ray diffraction (XRD) characterization technique is used to investigate the structural properties. The semi-crystalline nature has been determined by the analysis of the obtained XRD pattern. Electrical properties of the synthesized film have been analysed from the C-V and I-V curves obtained at various frequencies and temperatures. Low conductivity values confirm the insulating behaviour of the film. However, it is found that conductivity increases with temperature. Also, the dielectric permittivity is found to be higher at lower frequencies and higher temperatures, that proves PVA to be an excellent dielectric material which can be used in interface electronics. Dielectric behaviour of the film has been explained based on dipole orientations to slow and fast varying electric field. However further engineering can be done to modulate the structural, electrical properties of the film.

  6. PHASE STRUCTURE AND COMPATIBILITY OF LADDERLIKE POLYPHENYLSILSESQUIOXANE (PPSQ)/POLYCARBONATE (PC) BLENDS PREPARED BY SOLUTION CASTING

    Institute of Scientific and Technical Information of China (English)

    Gui-zhi Li; Liang-he Shi

    1999-01-01

    Blends of PC and PPSQ (A) with high Mw and good ladderlike regularity or PPSQ(B) with low Mw and more defective Si-atoms in its structure have been prepared by solution casting. The dispersed spheres (PPSQ(A)-rich) are unevenly dispersed in the continuous PC-rich phase and there is no phase-inversion as PPSQ(A) content increases when the percentage of PPSQ(A) is not more than70%. PPSQ(B)-rich spheres are evenly dispersed in the continuous phase (PC-rich) and phaseinversion occurs when PPSQ(B) percentage is up to 70%. Tg of PPSQ(A)/PC or PPSQ(B)/PC at some compositions are lower than that of pure PC due to the enlarged free-volume of PC-rich phase because some spheres of rigid PPSQ chains are included in the PC-rich phase. PC and PPSQ(A) or PPSQ(B)are partially compatible. The compatibility of PC and PPSQ(B) is better than that of PC and PPSQ(A)with high Mw and good ladderlike regularity. Heat history has some influence on the TgS and compatibility of PPSQ(A)/PC and PPSQ(B)/PC blends.

  7. Ciprofloxacin adsorption from aqueous solution onto chemically prepared carbon from date palm leaflets.

    Science.gov (United States)

    El-Shafey, El-Said Ibrahim; Al-Lawati, Haider; Al-Sumri, Asmaa Soliman

    2012-01-01

    A chemically prepared carbon was synthesized from date palm leaflets via sulphuric acid carbonization at 160 degrees C. Adsorption of ciprofloxacin (CIP) from aqueous solution was investigated in terms of time, pH, concentration, temperature and adsorbent status (wet and dry). The equilibrium time was found to be 48 hr. The adsorption rate was enhanced by raising the temperature for both adsorbents, with adsorption data fitting a pseudo second-order model well. The activation energy, Ea, was found to be 17 kJ/mol, indicating a diffusion-controlled, physical adsorption process. The maximum adsorption was found at initial pH 6. The wet adsorbent showed faster removal with higher uptake than the dry adsorbent, with increased performance as temperature increased (25-45 degrees C). The equilibrium data were found to fit the Langmuir model better than the Freundlich model. The thermodynamic parameters showed that the adsorption process is spontaneous and endothermic. The adsorption mechanism is mainly related to cation exchange and hydrogen bonding.

  8. Optimization of the design and preparation of nanoscale phospholipid bilayers for its application to solution NMR.

    Science.gov (United States)

    Puthenveetil, Robbins; Vinogradova, Olga

    2013-07-01

    Despite arduous efforts and recent technological developments structural investigation of integral membrane proteins remains a challenge. The primary deterrents include difficulties with their expression, low inherent solubility, and problems associated with existing membrane mimicking systems. A relatively new class of membrane mimetics, nanodiscs, is emerging as a promising alternative. Although nanodiscs have been proven successful for several biophysical applications, they yet remain to become the system of preferred choice for structure determination. We have hereby made nanodiscs more suitable for solution NMR applications by reducing the diameter of the self-assembly complex to its potential limit. We achieved a noticeable improvement in the quality of NMR spectra obtained for the transmembrane and cytoplasmic domains of integrin αIIb incorporated into these smaller discs rendering them susceptible for a thorough structural investigation. In addition, we also present an on-column method for a rapid, efficient, single-step preparation of protein incorporated nanodiscs at high concentrations. These discs have been fully characterized by transmission electron microscopy, dynamic light scattering, and differential scanning calorimetry.

  9. Advanced sample preparation for the molecular quantification of Staphylococcus aureus in artificially and naturally contaminated milk.

    Science.gov (United States)

    Aprodu, Iuliana; Walcher, Georg; Schelin, Jenny; Hein, Ingeborg; Norling, Börje; Rådström, Peter; Nicolau, Anca; Wagner, Martin

    2011-03-01

    Sample treatment is an essential element when using real-time PCR for quantification of pathogens directly on food samples. This study comparatively evaluated three different principles of sample treatment, i.e. immunomagnetic separation based on phage-derived cell wall binding molecules, matrix solubilization and flotation, in order to establish their suitability for quantifying low numbers of Staphylococcus aureus in milk. All three procedures succeeded to remove S. aureus from the milk matrix, either raw or pasteurized, and, as a result of the concentration of the target cells, minimized the effect of milk associated PCR inhibitors. Sample preparation based on immunomagnetic separation albeit of being user friendly, specific and rapid, failed to allow quantification of low and medium numbers (<10(4)CFU) of S. aureus. In a mastitic milk model cell wall binding domain (CBD)-based target cell extraction revealed results most closely matching those derived from culture-based quantification. Both matrix lysis and flotation allowed quantification of S. aureus at a level of 1-10 cells per ml. Both methods resulted in higher numbers of bacterial cell equivalents (bce) than plating could reveal. Since both methods harvest cells that have been subjected to either mechanical and chemical stresses before quantification, we concluded that the higher bce numbers resulted from a disaggregation of S. aureus clusters initially present in the inoculum. Conclusively, since likely each S. aureus cell of a toxigenic strain contributes to enterotoxin production, molecular quantification could provide an even more realistic impact assessment in outbreak investigations than plating does.

  10. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

    Science.gov (United States)

    Yang, Bin; Smith, A. M.; Long, S.

    2015-10-01

    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0-3 bar) and so has the capacity to graphitise CO2 samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a 'budget' fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  11. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Bin; Smith, A.M.; Long, S.

    2015-10-15

    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0–3 bar) and so has the capacity to graphitise CO{sub 2} samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a ‘budget’ fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  12. Analytical Results from Salt Solution Feed Tank (SSFT) Samples HTF-16-6 and HTF-16-40

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-09-23

    Two samples from the Salt Solution Feed Tank (SSFT) were analyzed by SRNL, HTF-16-6 and HTF-16-40. Multiple analyses of these samples indicate a general composition almost identical to that of the Salt Batch 8-B feed and the Tank 21H sample results.

  13. Results for the Fourth Quarter Calendar Year 2015 Tank 50H Salt Solution Sample

    Energy Technology Data Exchange (ETDEWEB)

    Crawford, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-01-11

    In this memorandum, the chemical and radionuclide contaminant results from the Fourth Quarter Calendar Year 2015 (CY15) sample of Tank 50H salt solution are presented in tabulated form. The Fourth Quarter CY15 Tank 50H samples were obtained on October 29, 2015 and received at Savannah River National Laboratory (SRNL) on October 30, 2015. The information from this characterization will be used by Defense Waste Processing Facility (DWPF) & Saltstone Facility Engineering for the transfer of aqueous waste from Tank 50H to the Salt Feed Tank in the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the Task Technical and Quality Assurance Plan (TTQAP) for the Tank 50H saltstone task. The chemical and radionuclide contaminant results from the characterization of the Fourth Quarter Calendar Year 2015 (CY15) sampling of Tank 50H were requested by SRR personnel and details of the testing are presented in the SRNL Task Technical and Quality Assurance Plan.

  14. Electrochemical studies on stress corrosion cracking of incoloy-800 in caustic solution. Part II: Precracking samples

    Directory of Open Access Journals (Sweden)

    Dinu Alice

    2006-01-01

    Full Text Available Stress corrosion cracking (SCC in a caustic medium may affect the secondary circuit tubing of a CANDU NPP cooled with river water, due to an accidental formation of a concentrated alkaline environment in the areas with restricted circulation, as a result of a leakage of cooling water from the condenser. To evaluate the susceptibility of Incoloy-800 (used to manufacture steam generator tubes for CANDU NPP to SCC, some accelerated corrosion tests were conducted in an alkaline solution (10% NaOH, pH = 13. These experiments were performed at ambient temperature and 85 °C. We used the potentiodynamic method and the potentiostatic method, simultaneously monitoring the variation of the open circuit potential during a time period (E corr/time curve. The C-ring method was used to stress the samples. In order to create stress concentrations, mechanical precracks with a depth of 100 or 250 μm were made on the outer side of the C-rings. Experimental results showed that the stressed samples were more susceptible to SCC than the unstressed samples whereas the increase in temperature and crack depth lead to an increase in SCC susceptibility. Incipient micro cracks of a depth of 30 μm were detected in the area of the highest peak of the mechanical precrack.

  15. Optical biosensor system with integrated microfluidic sample preparation and TIRF based detection

    Science.gov (United States)

    Gilli, Eduard; Scheicher, Sylvia R.; Suppan, Michael; Pichler, Heinz; Rumpler, Markus; Satzinger, Valentin; Palfinger, Christian; Reil, Frank; Hajnsek, Martin; Köstler, Stefan

    2013-05-01

    There is a steadily growing demand for miniaturized bioanalytical devices allowing for on-site or point-of-care detection of biomolecules or pathogens in applications like diagnostics, food testing, or environmental monitoring. These, so called labs-on-a-chip or micro-total analysis systems (μ-TAS) should ideally enable convenient sample-in - result-out type operation. Therefore, the entire process from sample preparation, metering, reagent incubation, etc. to detection should be performed on a single disposable device (on-chip). In the early days such devices were mainly fabricated using glass or silicon substrates and adapting established fabrication technologies from the electronics and semiconductor industry. More recently, the development focuses on the use of thermoplastic polymers as they allow for low-cost high volume fabrication of disposables. One of the most promising materials for the development of plastic based lab-on-achip systems are cyclic olefin polymers and copolymers (COP/COC) due to their excellent optical properties (high transparency and low autofluorescence) and ease of processing. We present a bioanalytical system for whole blood samples comprising a disposable plastic chip based on TIRF (total internal reflection fluorescence) optical detection. The chips were fabricated by compression moulding of COP and microfluidic channels were structured by hot embossing. These microfluidic structures integrate several sample pretreatment steps. These are the separation of erythrocytes, metering of sample volume using passive valves, and reagent incubation for competitive bioassays. The surface of the following optical detection zone is functionalized with specific capture probes in an array format. The plastic chips comprise dedicated structures for simple and effective coupling of excitation light from low-cost laser diodes. This enables TIRF excitation of fluorescently labeled probes selectively bound to detection spots at the microchannel surface

  16. Thermoluminescence study of Cu and Ag doped lithium tetraborate samples synthesized by water/solution assisted method

    Energy Technology Data Exchange (ETDEWEB)

    Thiyagarajan, S.; Kumar, S.; Vallejo, M.; Sosa, M. [Universidad de Guanajuato, Departamento de Ingenieria Fisica, 37150 Leon, Guanajuato (Mexico); Velusamy, J., E-mail: thiya93@gmail.com [Centro de Investigaciones en Optica, Apdo. Postal 1-948, Leon, Guanajuato (Mexico)

    2016-10-15

    In this paper lithium tetraborate (Li{sub 2}B{sub 4}O{sub 7}) was produced by water/solution assisted synthesis method. Transition metals, such as Cu and Ag were used to dope Li{sub 2}B{sub 4}O{sub 7} in order to enhance its thermoluminescent properties. The heating temperature parameters for synthesis were 750 degrees Celsius for 2 hours and 150 degrees Celsius for another 2 hours. The samples produced by water assisted method were doped at different doping percentage (0.08, 0.12, 0.5, 0.1 and 1%) of Cu and Ag. Pellets of samples were prepared and there were irradiated with different doses (58, 100, 500 and 945 mGy) by using and X-ray source. The characteristics of undoped and doped Li{sub 2}B-4O{sub 7} were determined by X-ray diffraction (XRD), scanning electron microscopy (Sem), photoluminescence and ultraviolet-visible spectroscopy. The chemical composition and their morphologies of the obtained Li{sub 2}B{sub 4}O{sub 7} and Li{sub 2}B{sub 4}O{sub 7}:Cu, Ag was confirmed by XRD and Sem results. The most intense peak of the XRD pattern of the lithium tetraborate sample was determined by comparing to the reference data and was found to have a tetragonal structure. The thermoluminescent glow curves of the pellets exposed to different doses exhibited a clear response to X-ray irradiation. Especially Li{sub 2}B{sub 4}O{sub 7}:Cu presented a good glow curve in all kind of doses. The experimental results showed that this could have good potential applications in radiation dosimetry. The order of kinetics (b), frequency factor (s) and activation energy (E) or the trapping parameters were calculated using peak shape method. (Author)

  17. Preparation1 and utilization of wheat straw anionic sorbent for the removal of nitrate from aqueous solution

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    In order to reduce the impact of eutrophication caused by agricultural residues (i.e. excess nitrate) in aqueous solution, economic and effective anionic sorbents are required. In this article, we prepared anionic sorbent using wheat straw. Its structural characteristics and adsorption properties for nitrate removal from aqueous solution were investigated. The results indicate that the yield of the prepared anionic sorbent, the total exchange capacity, and the maximum adsorption capacity were 350%, 2.57 mEq/g, and 2.08 mmol/g, respectively. The Freundlich isotherm mode is more suitable than the Langmuir mode and the adsorption process accords with the first order reaction kinetic rate equation. When multiple anions (SO42-, H2PO4-, NO3-, and NO2-) were present, the isotherm mode of prepared anionic sorbent for nitrate was consistent with Freundlich mode; however, the capacity of nitrate adsorption was reduced by 50%. In alkaline solutions, about 90% of adsorbed nitrate ions could be desorbed from prepared anionic sorbent. The results of this study confirmed that the wheat straw anionic sorbent can be used as an excellent nitrate sorbent that removes nitrate from aqueous solutions.

  18. Procedure for obtaining an extract rich in triterpenic acids from solutions from the process of preparation of table olives

    OpenAIRE

    2008-01-01

    [EN] Procedure for obtaining an extract having a high proportion of triterpenic acids, preferably of oleanolic and maslinic acids, from the solutions obtained in the process of preparation of table olives. Furthermore the invention refers to the extract obtained through said procedure and to application thereof in the food, cosmetic or pharmaceutical industries.

  19. Strain effects in Nb3Al multifilamentary conductors prepared by phase transformation from bcc supersaturated-solid solution

    NARCIS (Netherlands)

    Takeuchi, T.; Iijima, Y.; Inoue, K.; Wada, H.; Haken, ten B.; Kate, ten H.H.J.; Fukuda, K.; Iwaki, G.; Sakai, S.; Moriai, H.

    1997-01-01

    Strain effects on critical current densities have been examined for conductors containing nearly stoichiometric Nb3Al filaments with fine grains. The Nb3Al phase in these multifilamentary conductors are prepared by phase transformation from supersaturated Nb(Al) bcc solid solution and show high-fiel

  20. Sample preparation for metalloprotein analysis: A case study using horse chestnuts.

    Science.gov (United States)

    de Magalhães, Cristiana Schmidt; Arruda, Marco Aurélio Zezzi

    2007-03-30

    In the present work, 11 different procedures for protein and metalloprotein extraction from horse chestnuts (Aescullus hippocastanum L.) in natura were tested. After each extraction, total protein was determined and, after protein separation through sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), those metals belonging to the protein structure were mapped by synchrotron radiation X-ray fluorescence (SRXRF). After mapping the elements (Cr, Fe and Mn) in the protein bands (ca. 33 and 23.7kDa), their concentrations were determined using atomic absorption spectrometry (ET AAS). Good results were obtained for protein extraction using a combination of grinding and sonication. However, this strategy was not suitable to preserve metal ions in the protein structure. In fact, there was 42% decrease on Mn concentration using this procedure, compared to that performed with sample agitation in water (taken as reference). On the other hand, when grinding and agitation with an extracting buffer was used, there was a 530% increase of Mn concentration, when compared to the reference procedure. These results indicate agreement between metal identification and determination in proteins as well as the great influence of the extraction procedure (i.e., the sample preparation step) for preserving metals in the protein structures.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-06-01

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

  2. Investigation into Alternative Sample Preparation Techniques for the Determination of Heavy Metals in Stationary Source Emission Samples Collected on Quartz Filters

    Directory of Open Access Journals (Sweden)

    Sharon L. Goddard

    2014-11-01

    Full Text Available Monitoring stationary source emissions for heavy metals generally requires the use of quartz filters to collect samples because of the high temperature and high moisture sampling environment. The documentary standard method sample preparation technique in Europe, EN 14385, uses digestion in hydrofluoric acid and nitric acid (HF/HNO3 followed by complexing with boric acid (H3BO3 prior to analysis. However, the use of this method presents a number of problems, including significant instrumental drift during analysis caused by the matrix components, often leading to instrument breakdown and downtime for repairs, as well as posing significant health and safety risks. The aim of this work was to develop an alternative sample preparation technique for emissions samples on quartz filters. The alternative techniques considered were: (i acid digestion in a fluoroboric acid (HBF4 and HNO3 mixture and (ii acid extraction in an aqua regia (AR mixture (HCl and HNO3. Assessment of the effectiveness of these options included determination of interferences and signal drift, as well as validating the different methods by measurement of matrix certified reference materials (CRMs, and comparing the results obtained from real test samples and sample blanks to determine limits of detection. The results showed that the HBF4/HNO3 mixture provides the most viable alternative to the documentary standard preparation technique.

  3. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

    Science.gov (United States)

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

    2016-01-28

    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed.

  4. Magnetocaloric effect in Ni-Zn ferrite nanoparticles prepared by using solution combustion

    Energy Technology Data Exchange (ETDEWEB)

    Lee, K. D.; Kambale, R. C.; Hur, N. [Inha University, Incheon (Korea, Republic of)

    2014-12-15

    Ni{sub x}Zn{sub 1-x}Fe{sub 2}O{sub 4} (x = 0.2 and 0.3) ferrite nanoparticles with sizes ranging from 65 to 70 nm were synthesized employing the solution combustion route. The magnetocaloric behavior was investigated within the 50 K ≤ T ≤ 400 K range of temperatures (T). The entropy change (ΔS) and the adiabatic temperature change (ΔT) were derived from magnetization (M) and specific heat (C{sub P} ) measurements. Both compositions exhibited broad peaks for the isothermal entropy change. The magnetic field (H)-dependent ΔT was analyzed within the mean-field approximation scheme, and the observed magnetocaloric properties of the nanoparticle samples were compared with those of a bulk sample. Our study suggests that the magnetocaloric properties of magnetic oxides strongly depend on the particle size; thus, particle size should be considered as a key tuning parameter in the optimization of magnetic refrigeration.

  5. Preparation of porous n-type silicon sample plates for desorption/ionization on silicon mass spectrometry (DIOS-MS).

    Science.gov (United States)

    Tuomikoski, S; Huikko, K; Grigoras, K; Ostman, P; Kostiainen, R; Baumann, M; Abian, J; Kotiaho, T; Franssila, S

    2002-11-01

    This study focuses on porous silicon (pSi) fabrication methods and properties for desorption ionization on silicon mass spectrometry (DIOS-MS). PSi was prepared using electrochemical etching of n-type silicon in HF-ethanol solution. Porous areas were defined by a double-sided illumination arrangement: front-side porous areas were masked by a stencil mask, eliminating the need for standard photolithography, and backside illumination was used for the backside ohmic contact. Backside illumination improved the uniformity of the porosified areas. Porosification conditions, surface derivatizations and storage conditions were explored to optimize pSi area, pore size and pore depth. Chemical derivatization of the pSi surfaces improved the DIOS-MS performance providing better ionization efficiency and signal stability with lower laser energy. Droplet spreading and drying patterns on pSi were also examined. Pore sizes of 50-200 nm were found to be optimal for droplet evaporation and pore filling with the sample liquid, as measured by DIOS efficiency. With DIOS, significantly better detection sensitivity was obtained (e.g. 150 fmol for midazolam) than with desorption ionization from a standard MALDI steel plate without matrix addition (30 pmol for midazolam). Also the noise that disturbs the detection of low-molecular weight compounds at m/z < 500 with MALDI could be clearly reduced with DIOS. Low background MS spectra and good detection sensitivity at the 100-150 fmol level for pharmaceutical compounds were achieved with DIOS-MS.

  6. Effects of Temperature and Method of Solution Preparation on the Performance of a Typical Red Mud Flocculent

    Science.gov (United States)

    Ferland, Pierre; Malito, John T.; Phillips, Everett C.

    Alcan International Ltd. in collaboration with Ondeo Nalco Company have carried out a fundamental study on the dissolution and performance of a 100% anionic polymer. The effects of method of preparation, solvent composition, temperature and exposure time on flocculent activity under conditions relevant to both atmospheric and pressure decantation were investigated. Flocculent activity was determined using static and dynamic settling tests, and the results were correlated with the reduced specific viscosity (RSV). For any given method of preparation of the flocculent solutions (makeup/dilution) the RSV tended to decrease with increasing solution ionic strength, independent of ionic speciation. While a significant loss in flocculent activity occurred with long exposure of the solution to high temperature, only a minor loss occurred in the short time required to flocculate and settle the mud in a decanter operating at 150 °C. Recent results in an actual plant pressure decanter appear to validate this conclusion.

  7. Toward a Fieldable Atomic Mass Spectrometer for Safeguards Applications: Sample Preparation and Ionization

    Energy Technology Data Exchange (ETDEWEB)

    Barinaga, Charles J.; Hager, George J.; Hart, Garret L.; Koppenaal, David W.; Marcus, R. Kenneth; Jones, Sarah MH; Manard, Benjamin T.

    2014-10-31

    The International Atomic Energy Agency’s (IAEA’s) long-term research and development plan calls for the development of new methods to detect misuse at nuclear fuel cycle facilities such as reprocessing and enrichment plants. At enrichment plants, for example, the IAEA’s contemporary safeguards approaches are based on a combination of routine and random inspections that include collection of UF6 samples from in-process material and selected cylinders for subsequent analyses. These analyses include destructive analysis (DA) in a laboratory (typically by mass spectrometry [MS]) for isotopic characterization, and environmental sampling (ES) for subsequent laboratory elemental and isotopic analysis (also both typically by MS). One area of new method development includes moving this kind of isotope ratio analytical capability for DA and ES activities into the field. Some of the reasons for these developments include timeliness of results, avoidance of hazardous material shipments, and guidance for additional sample collecting. However, this capability does not already exist for several reasons, such as that most lab-based chemical and instrumental methods rely on laboratory infrastructure (highly trained staff, power, space, hazardous material handling, etc.) and require significant amounts of consumables (power, compressed gases, etc.). In addition, there are no currently available, fieldable instruments for atomic or isotope ratio analysis. To address these issues, Pacific Northwest National Laboratory (PNNL) and collaborator, Clemson University, are studying key areas that limit the fieldability of isotope ratio mass spectrometry for atomic ions: sample preparation and ionization, and reducing the physical size of a fieldable mass spectrometer. PNNL is seeking simple and robust techniques that could be effectively used by inspectors who may have no expertise in analytical MS. In this report, we present and describe the preliminary findings for three candidate

  8. A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS.

    Science.gov (United States)

    Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas

    2017-03-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

  9. High-throughput analysis for preparation, processing and analysis of TiO{sub 2} coatings on steel by chemical solution deposition

    Energy Technology Data Exchange (ETDEWEB)

    Cuadrado Gil, Marcos, E-mail: Marcos.cuadradogil@ugent.be [SCRIPTS - Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281 (S3) (Belgium); Van Driessche, Isabel, E-mail: Isabel.VanDriessche@ugent.be [SCRIPTS - Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281 (S3) (Belgium); Van Gils, Sake, E-mail: Sake.Vangils@arcelormittal.com [OCAS - ArcelorMittal Gent R and D Centre, Pres. J.F. Kennedylaan 3, Zelzate B-9060 (Belgium); Lommens, Petra, E-mail: Petra.Lommens@ugent.be [SCRIPTS - Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281 (S3) (Belgium); Castelein, Pieter, E-mail: Pieter.Castelein@flamac.be [Flamac - A Division of SIM, Technologiepark 903, Zwijnaarde 9052 (Belgium); De Buysser, Klaartje, E-mail: Klaartje.DeBuysser@ugent.be [SCRIPTS - Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281 (S3) (Belgium)

    2012-11-05

    Highlights: Black-Right-Pointing-Pointer High-throughput preparation of TiO{sub 2} aqueous precursors. Black-Right-Pointing-Pointer Analysis of stability and surface tension. Black-Right-Pointing-Pointer Deposition of TiO{sub 2} coatings. - Abstract: A high-throughput preparation, processing and analysis of titania coatings prepared by chemical solution deposition from water-based precursors at low temperature ( Almost-Equal-To 250 Degree-Sign C) on two different types of steel substrates (Aluzinc Registered-Sign and bright annealed) is presented. The use of the high-throughput equipment allows fast preparation of multiple samples saving time, energy and material; and helps to test the scalability of the process. The process itself includes the use of IR curing for aqueous ceramic precursors and possibilities of using UV irradiation before the final sintering step. The IR curing method permits a much faster curing step compared to normal high temperature treatments in traditional convection devices (i.e., tube furnaces). The formulations, also prepared by high-throughput equipment, are found to be stable in the operational pH range of the substrates (6.5-8.5). Titanium alkoxides itself lack stability in pure water-based environments, but the presence of the different organic complexing agents prevents it from hydrolysis and precipitation reactions. The wetting interaction between the substrates and the various formulations is studied by the determination of the surface free energy of the substrates and the polar and dispersive components of the surface tension of the solutions. The mild temperature program used for preparation of the coatings however does not lead to the formation of pure crystalline material, necessary for the desired photocatalytic and super-hydrophilic behavior of these coatings. Nevertheless, some activity can be reported for these amorphous coatings by monitoring the discoloration of methylene blue in water under UV irradiation.

  10. Preparation of edible wild fruit and plant samples for analysis and some difficulties encountered in such analyses

    CSIR Research Space (South Africa)

    Strydom, ESP

    1969-12-01

    Full Text Available Freeze-dried samples are used for analysis and the methods of preparation of samples for freeze-drying are discussed. Freeze-drying has obvious advantages but has also a few minor disadvantages. Difficulties encountered in the determination of some...

  11. Selectivity in the sample preparation for the analysis of drug residues in products of animal origin using LC-MS

    NARCIS (Netherlands)

    Berendsen, B.J.A.; Stolker, A.A.M.; Nielen, M.W.F.

    2013-01-01

    Sample preparation is critical in relation to analysis time, sample throughput and therefore analysis costs. Due to recent advances in liquid chromatography-mass spectrometry (LC-MS) instrumentation, the detection of many compounds within one run became possible, and methods for the simultaneous ana

  12. New Sample Preparation Method for Quantification of Phenolic Compounds of Tea (Camellia sinensis L. Kuntze: A Polyphenol Rich Plant

    Directory of Open Access Journals (Sweden)

    P. A. Nimal Punyasiri

    2015-01-01

    Full Text Available Chemical analysis of the Sri Lankan tea (Camellia sinensis, L. germplasm would immensely contribute to the success of the tea breeding programme. However, the polyphenols, particularly catechins (flavan-3-ols, are readily prone to oxidation in the conventional method of sample preparation. Therefore, optimization of the present sample preparation methodology for the profiling of metabolites is much important. Two sample preparation methodologies were compared, fresh leaves (as in the conventional procedures and freeze-dried leaves (a new procedure, for quantification of major metabolites by employing two cultivars, one is known to be high quality black tea and the other low quality black tea. The amounts of major metabolites such as catechins, caffeine, gallic acid, and theobromine, recorded in the new sampling procedure via freeze-dried leaves, were significantly higher than those recorded in the conventional sample preparation procedure. Additionally new method required less amount of leaf sample for analysis of major metabolites and facilitates storage of samples until analysis. The freeze-dried method would be useful for high throughput analysis of large number of samples in shorter period without chemical deterioration starting from the point of harvest until usage. Hence, this method is more suitable for metabolite profiling of tea as well as other phenol rich plants.

  13. Polyvinyl pyrrolidone capped fluorescent anthracene nanoparticles for sensing fluorescein sodium in aqueous solution and analytical application for ophthalmic samples.

    Science.gov (United States)

    Bhopate, Dhanaji P; Mahajan, Prasad G; Garadkar, Kalyanrao M; Kolekar, Govind B; Patil, Shivajirao R

    2015-11-01

    Based on the known complexation ability between polyvinyl pyrrolidone (PVP) and fluorescein sodium (FL Na(+)), fluorescent PVP capped anthracene nanoparticles (PVP-ANPs) were prepared using a reprecipitation method for detection of fluorescein in aqueous solution using the fluorescence resonance energy transfer (FRET) approach. A dynamic light scattering histogram of PVP-ANPs showed narrower particle size distribution and the average particle size was 15 nm. The aggregation-induced enhanced emission (AIEE) of PVP-ANPs was red shifted from its monomer by 1087.22 cm(-1). The maximum emission was seen to occur at 420 nm. The presence of FL Na(+) in the vicinity of PVP-ANPs quenched the fluorescence of PVP-ANPs because of its adsorption on the surface of PVP-ANPs in aqueous suspension. The FL Na(+) and PVP-ANPs were brought close enough, typically to 7.89 nm, which was less than the distance of 10 nm that is required between the energy donor-acceptor molecule for efficient FRET. The quenching results fit into the Stern-Volmer relationship even at temperatures greater than ambient temperatures. The thermodynamic parameters determined from FRET results helped to propose binding mechanisms involving hydrophobic and electrostatic molecular interaction. The fluorescence quenching results were used further to develop an analytical method for estimation of fluorescein sodium from ophthalmic samples available commercially in the market.

  14. CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.13)

    Science.gov (United States)

    The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

  15. CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.13)

    Science.gov (United States)

    The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

  16. Dynamical traps in Wang-Landau sampling of continuous systems: Mechanism and solution.

    Science.gov (United States)

    Koh, Yang Wei; Sim, Adelene Y L; Lee, Hwee Kuan

    2015-08-01

    We study the mechanism behind dynamical trappings experienced during Wang-Landau sampling of continuous systems reported by several authors. Trapping is caused by the random walker coming close to a local energy extremum, although the mechanism is different from that of the critical slowing-down encountered in conventional molecular dynamics or Monte Carlo simulations. When trapped, the random walker misses the entire or even several stages of Wang-Landau modification factor reduction, leading to inadequate sampling of the configuration space and a rough density of states, even though the modification factor has been reduced to very small values. Trapping is dependent on specific systems, the choice of energy bins, and the Monte Carlo step size, making it highly unpredictable. A general, simple, and effective solution is proposed where the configurations of multiple parallel Wang-Landau trajectories are interswapped to prevent trapping. We also explain why swapping frees the random walker from such traps. The efficacy of the proposed algorithm is demonstrated.

  17. Preparation and Characterization of Micronized Artemisinin via a Rapid Expansion of Supercritical Solutions (RESS Method

    Directory of Open Access Journals (Sweden)

    Xiaonan Zhang

    2012-04-01

    Full Text Available The particle sizes of pharmaceutical substances are important for their bioavailability. Bioavailability can be improved by reducing the particle size of the drug. In this study, artemisinin was micronized by the rapid expansion of supercritical solutions (RESS. The particle size of the unprocessed white needle-like artemisinin particles was 30 to 1200 µm. The optimum micronization conditions are determined as follows: extraction temperature of 62 °C, extraction pressure of 25 MPa, precipitation temperature 45 °C and nozzle diameter of 1000 μm. Under the optimum conditions, micronized artemisinin with a (mean particle size MPS of 550 nm is obtained. By analysis of variance (ANOVA, extraction temperature and pressure have significant effects on the MPS of the micronized artemisinin. The particle size of micronized artemisinin decreased with increasing extraction temperature and pressure. Moreover, the SEM, LC-MS, FTIR, DSC and XRD allowed the comparison between the crystalline initial state and the micronization particles obtained after the RESS process. The results showed that RESS process has not induced degradation of artemisinin and that processed artemisinin particles have lower crystallinity and melting point. The bulk density of artemisinin was determined before and after RESS process and the obtained results showed that it passes from an initial density of 0.554 to 0.128 g·cm−3 after the processing. The decrease in bulk density of the micronized powder can increase the liquidity of drug particles when they are applied for medicinal preparations. These results suggest micronized powder of artemisinin can be of great potential in drug delivery systems.

  18. Preparation and characterization of novel P(HEA/IA) hydrogels for Cd{sup 2+} ion removal from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Antić, Katarina M.; Babić, Marija M.; Vuković, Jovana J. Jovašević [Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, Belgrade (Serbia); Vasiljević-Radović, Dana G. [Institute for Chemistry, Technology and Metallurgy, University of Belgrade, Njegoseva 12, Belgrade (Serbia); Onjia, Antonije E. [Vinca Institute of Nuclear Sciences, University of Belgrade, P.O. Box 522, Belgrade (Serbia); Filipović, Jovanka M. [Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, Belgrade (Serbia); Tomić, Simonida Lj., E-mail: simonida@tmf.bg.ac.rs [Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, Belgrade (Serbia)

    2015-05-30

    Highlights: • Hydrogels based on 2-hydroxyethyl acrylate and itaconic acid (P(HEA/IA)) were synthesized. • Cd{sup 2+} ion removal was investigated. • The surface and cross-section of hydrogels were observed by SEM and AFM. • The adsorption kinetics and isotherms of cadmium ions on the hydrogel were studied. • Approximately 95% of the adsorbed cadmium could be recovered by 0.1 M HNO{sub 3} treatment. - Abstract: Series of novel hydrogels based on 2-hydroxyethyl acrylate (HEA) and itaconic acid (IA), P(HEA/IA) copolymers, were prepared by free radical cross-linking copolymerization and investigated as potential adsorbents for Cd{sup 2+} removal from aqueous solution. The hydrogels before and after Cd{sup 2+} adsorption were characterized using FTIR, DSC, SEM/EDX, AFM and DMA analysis. The swelling results showed that these hydrogels are pH and temperature sensitive. In order to evaluate adsorption behavior of samples various factors affecting the Cd{sup 2+} uptake behavior, such as: contact time, temperature, pH, ionic strength, adsorbent weight, competitive ions and initial concentration of the metal ions were investigated. Five adsorption isotherms and two kinetic models were studied. The adsorption behavior can be very well described by the pseudo-second order kinetic model and Langmuir isotherm. Multicomponent adsorption studies revealed that adsorption of cadmium depends on the type of metal ions present in the system. Desorption studies showed that hydrogel can be reused three times with only 15% loss of adsorption capacity. All results indicate that the sample with the highest IA content is the most promising adsorbent for Cd{sup 2+} removal.

  19. A lab-on-a-chip system with integrated sample preparation and loop-mediated isothermal amplification for rapid and quantitative detection of Salmonella spp. in food samples

    DEFF Research Database (Denmark)

    Sun, Yi; Than Linh, Quyen; Hung, Tran Quang

    2015-01-01

    and usually take a few hours to days to complete. In response to the demand for rapid on line or at site detection of pathogens, in this study, we describe for the first time an eight-chamber lab-on-a-chip (LOC) system with integrated magnetic beads-based sample preparation and loop-mediated isothermal...

  20. Demonstration of a frozen sample aliquotter to prepare plasma and serum aliquots without thawing frozen parent samples.

    Science.gov (United States)

    Ellis, Helena Judge; Venturini, Deborah S

    2013-06-01

    Human biospecimens represent invaluable resources to advance molecular medicine, epidemiology, and biomarker discovery/validation, among other biomedical research. Biobanks typically cryopreserve biospecimens to safeguard their biochemical composition. However, exposing specimens repeatedly to freeze/thaw cycles can degrade their integrity in unforeseen ways. Those biobanks storing liquid samples, thus, regularly make a fundamental compromise at collection time between freezing samples in many small volumes (e.g., 0.5 mL or smaller) or in fewer, larger volumes (e.g., 1.8 mL). The former eliminates the need to expose samples to repeated freeze/thaw cycling, although increasing up-front labor costs, consumables used, and cold storage space requirements. The latter decreases up-front labor costs, consumables, and cold storage requirements, yet exposes samples repeatedly to damaging freeze/thaw cycles when smaller aliquots are needed for analysis. The Rhode Island BioBank at Brown University (RIBB) thoroughly evaluated the performance of an original technology that minimizes a sample's exposure to freeze/thaw cycling by enabling the automated extraction of frozen aliquots from one single frozen parent sample without thawing it. A technology that eliminates unnecessary sample exposures to freeze/thaw cycles could help protect sample integrity, extend its useful life, and effectively rectify and eliminate the aforementioned need to compromise. This report presents the results of the evaluation, and conclusively demonstrates the technology's ability to extract multiple uniform frozen aliquots from a single cryotube of never-thawed frozen human plasma, which faithfully represent the parent sample when analyzed for typical biochemical analytes, showing a coefficient of variability lower than 5.5%.

  1. Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Takayama, Yuki; Nakasako, Masayoshi [Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Mikaduki, Sayo, Hyogo 679-5148 (Japan)

    2012-05-15

    Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

  2. Rapid Preparation Methods of Biological Samples for Ionic Compounds Using Ion Exchange Type Monolithic Silica Spin Column

    OpenAIRE

    宮崎, 将太; 山田, 智子; 太田, 茂徳; 斉藤, 剛; 奈女良, 昭; 大平, 真義

    2010-01-01

    We developed a device comprising a spin column packed with ion exchange type (SCX and SAX) monolithic silica for extracting ionic compounds from biological samples. The methods involving the use of these spin column are not useful for the extraction of ionic analytes, but are highly reproducible for the analysis in serum and urine. This spin column enabled sample preparation in less than 10 min. Handling such as sample loading, washing, and elution of analytes, was exhibited by the centrifuga...

  3. Quality analysis of salmon calcitonin in a polymeric bioadhesive pharmaceutical formulation: sample preparation optimization by DOE.

    Science.gov (United States)

    D'Hondt, Matthias; Van Dorpe, Sylvia; Mehuys, Els; Deforce, Dieter; DeSpiegeleer, Bart

    2010-12-01

    A sensitive and selective HPLC method for the assay and degradation of salmon calcitonin, a 32-amino acid peptide drug, formulated at low concentrations (400 ppm m/m) in a bioadhesive nasal powder containing polymers, was developed and validated. The sample preparation step was optimized using Plackett-Burman and Onion experimental designs. The response functions evaluated were calcitonin recovery and analytical stability. The best results were obtained by treating the sample with 0.45% (v/v) trifluoroacetic acid at 60 degrees C for 40 min. These extraction conditions did not yield any observable degradation, while a maximum recovery for salmon calcitonin of 99.6% was obtained. The HPLC-UV/MS methods used a reversed-phase C(18) Vydac Everest column, with a gradient system based on aqueous acid and acetonitrile. UV detection, using trifluoroacetic acid in the mobile phase, was used for the assay of calcitonin and related degradants. Electrospray ionization (ESI) ion trap mass spectrometry, using formic acid in the mobile phase, was implemented for the confirmatory identification of degradation products. Validation results showed that the methodology was fit for the intended use, with accuracy of 97.4+/-4.3% for the assay and detection limits for degradants ranging between 0.5 and 2.4%. Pilot stability tests of the bioadhesive powder under different storage conditions showed a temperature-dependent decrease in salmon calcitonin assay value, with no equivalent increase in degradation products, explained by the chemical interaction between salmon calcitonin and the carbomer polymer.

  4. Preparation of Ultrafine Fe-Pt Alloy and Au Nanoparticle Colloids by KrF Excimer Laser Solution Photolysis.

    Science.gov (United States)

    Watanabe, Masato; Takamura, Hitoshi; Sugai, Hiroshi

    2009-03-10

    We prepared ultrafine Fe-Pt alloy nanoparticle colloids by UV laser solution photolysis (KrF excimer laser of 248 nm wavelength) using precursors of methanol solutions into which iron and platinum complexes were dissolved together with PVP dispersant to prevent aggregations. From TEM observations, the Fe-Pt nanoparticles were found to be composed of disordered FCC A1 phase with average diameters of 0.5-3 nm regardless of the preparation conditions. Higher iron compositions of nanoparticles require irradiations of higher laser pulse energies typically more than 350 mJ, which is considered to be due to the difficulty in dissociation of Fe(III) acetylacetonate compared with Pt(II) acetylacetonate. Au colloid preparation by the same method was also attempted, resulting in Au nanoparticle colloids with over 10 times larger diameters than the Fe-Pt nanoparticles and UV-visible absorption peaks around 530 nm that originate from the surface plasmon resonance. Differences between the Fe-Pt and Au nanoparticles prepared by the KrF excimer laser solution photolysis are also discussed.

  5. Preparation of Ultrafine Fe–Pt Alloy and Au Nanoparticle Colloids by KrF Excimer Laser Solution Photolysis

    Directory of Open Access Journals (Sweden)

    Sugai Hiroshi

    2009-01-01

    Full Text Available Abstract We prepared ultrafine Fe–Pt alloy nanoparticle colloids by UV laser solution photolysis (KrF excimer laser of 248 nm wavelength using precursors of methanol solutions into which iron and platinum complexes were dissolved together with PVP dispersant to prevent aggregations. From TEM observations, the Fe–Pt nanoparticles were found to be composed of disordered FCC A1 phase with average diameters of 0.5–3 nm regardless of the preparation conditions. Higher iron compositions of nanoparticles require irradiations of higher laser pulse energies typically more than 350 mJ, which is considered to be due to the difficulty in dissociation of Fe(III acetylacetonate compared with Pt(II acetylacetonate. Au colloid preparation by the same method was also attempted, resulting in Au nanoparticle colloids with over 10 times larger diameters than the Fe–Pt nanoparticles and UV–visible absorption peaks around 530 nm that originate from the surface plasmon resonance. Differences between the Fe–Pt and Au nanoparticles prepared by the KrF excimer laser solution photolysis are also discussed.

  6. Method of solution preparation of polyolefin class polymers for electrospinning processing included

    Science.gov (United States)

    Rabolt, John F. (Inventor); Lee, Keun-Hyung (Inventor); Givens, Steven R. (Inventor)

    2011-01-01

    A process to make a polyolefin fiber which has the following steps: mixing at least one polyolefin into a solution at room temperature or a slightly elevated temperature to form a polymer solution and electrospinning at room temperature said polymer solution to form a fiber.

  7. Adjustable virtual pore-size filter for automated sample preparation using acoustic radiation force

    Energy Technology Data Exchange (ETDEWEB)

    Jung, B; Fisher, K; Ness, K; Rose, K; Mariella, R

    2008-05-22

    We present a rapid and robust size-based separation method for high throughput microfluidic devices using acoustic radiation force. We developed a finite element modeling tool to predict the two-dimensional acoustic radiation force field perpendicular to the flow direction in microfluidic devices. Here we compare the results from this model with experimental parametric studies including variations of the PZT driving frequencies and voltages as well as various particle sizes and compressidensities. These experimental parametric studies also provide insight into the development of an adjustable 'virtual' pore-size filter as well as optimal operating conditions for various microparticle sizes. We demonstrated the separation of Saccharomyces cerevisiae and MS2 bacteriophage using acoustic focusing. The acoustic radiation force did not affect the MS2 viruses, and their concentration profile remained unchanged. With optimized design of our microfluidic flow system we were able to achieve yields of > 90% for the MS2 with > 80% of the S. cerevisiae being removed in this continuous-flow sample preparation device.

  8. Dynamic simulation tools for the analysis and optimization of novel collection, filtration and sample preparation systems

    Energy Technology Data Exchange (ETDEWEB)

    Clague, D; Weisgraber, T; Rockway, J; McBride, K

    2006-02-12

    The focus of research effort described here is to develop novel simulation tools to address design and optimization needs in the general class of problems that involve species and fluid (liquid and gas phases) transport through sieving media. This was primarily motivated by the heightened attention on Chem/Bio early detection systems, which among other needs, have a need for high efficiency filtration, collection and sample preparation systems. Hence, the said goal was to develop the computational analysis tools necessary to optimize these critical operations. This new capability is designed to characterize system efficiencies based on the details of the microstructure and environmental effects. To accomplish this, new lattice Boltzmann simulation capabilities where developed to include detailed microstructure descriptions, the relevant surface forces that mediate species capture and release, and temperature effects for both liquid and gas phase systems. While developing the capability, actual demonstration and model systems (and subsystems) of national and programmatic interest were targeted to demonstrate the capability. As a result, where possible, experimental verification of the computational capability was performed either directly using Digital Particle Image Velocimetry or published results.

  9. Methodologies and perspectives of proteomics applied to filamentous fungi: from sample preparation to secretome analysis.

    Science.gov (United States)

    Bianco, Linda; Perrotta, Gaetano

    2015-03-12

    Filamentous fungi possess the extraordinary ability to digest complex biomasses and mineralize numerous xenobiotics, as consequence of their aptitude to sensing the environment and regulating their intra and extra cellular proteins, producing drastic changes in proteome and secretome composition. Recent advancement in proteomic technologies offers an exciting opportunity to reveal the fluctuations of fungal proteins and enzymes, responsible for their metabolic adaptation to a large variety of environmental conditions. Here, an overview of the most commonly used proteomic strategies will be provided; this paper will range from sample preparation to gel-free and gel-based proteomics, discussing pros and cons of each mentioned state-of-the-art technique. The main focus will be kept on filamentous fungi. Due to the biotechnological relevance of lignocellulose degrading fungi, special attention will be finally given to their extracellular proteome, or secretome. Secreted proteins and enzymes will be discussed in relation to their involvement in bio-based processes, such as biomass deconstruction and mycoremediation.

  10. Atmospheric pressure microwave sample preparation procedure for the combined analysis of total phosphorus and kjeldahl nitrogen.

    Science.gov (United States)

    Collins, L W; Chalk, S J; Kingston, H M

    1996-08-01

    An atmospheric pressure microwave digestion method has been developed for the combined analysis of total phosphorus and Kjeldahl nitrogen in complex matrices. In comparison to the digestion steps in EPA Methods 365.4 (total phosphorus) and 351.x (Kjeldahl nitrogen), this method requires less time, eliminates the need for a catalyst, and reduces the toxicity of the waste significantly. It employs a microwave-assisted digestion step, using refluxing borosilicate glass vessels at atmospheric pressure. Traditionally, this method has a time-consuming sample preparation step and generates toxic waste through the use of heavy metal catalysts. These advantages are gained by the combination of a high boiling point acid (sulfuric acid) and the application of focused microwave irradiation, which enhances the digestion process by direct energy coupling. NIST standard reference materials 1572 (citrus leaves), 1577a (bovine liver), and 1566 (oyster tissue) and tryptophan were analyzed to validate the method. Phosphorus concentrations were determined by the colorimetric ascorbic acid method outlined in EPA Method 365.3. Kjeldahl nitrogen concentrations were determined using EPA Method 351.1. The results of the analyses showed good precision and are in excellent agreement with the NIST published values for both elements.

  11. Development of a sample preparation procedure for the simultaneous determination of Np and Pu in clay samples

    Energy Technology Data Exchange (ETDEWEB)

    Renz, Tobias; Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Bauer, Andreas; Geckeis, Horst [INE, KIT, Eggenstein-Leopoldshafen (Germany); Taubald, Heinrich [Eberhard Karls Universitaet, Tuebingen (Germany)

    2015-07-01

    Neptunium (Np) and plutonium (Pu) are two key radionuclides for the long-term disposal of nuclear waste. Within this context Opalinus Clay formations are considered as a potential location for disposal of high-level radioactive waste. In the framework of experiments studying the diffusion behavior and retention of actinides under repository conditions, the present work focuses on the development of an analytical-chemical procedure for the determination of Np and Pu in clay (or clay-rich soil) samples. The procedure aims at the simultaneous determination of Np and Pu at femto- to attogram levels with AMS. Fields of application are the investigation of global fallout actinides in environmental clay-rich samples or the diffusion behavior of actinides in compacted clay liners used as technical barriers in nuclear waste repositories. Clay samples are spiked with certified standards of Pu-242 and Np-237. The analytical method, including a) leaching of the spiked clay samples, b) redox adjustments of Np and Pu, c) chromatographic separation of Np and Pu from the sample matrix and d) measurement of the actinides with Sector Field (SF)-ICP-MS will be presented. The suitability of a Pu isotope as non-isotopic tracer for determination of Np-237 is evaluated by determining the chemical yield using SF-ICP-MS.

  12. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Directory of Open Access Journals (Sweden)

    Christina Schreier

    2013-01-01

    Full Text Available Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after 1H NMR spectroscopy. Results. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at −20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Conclusion. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  13. Reproducibility of NMR analysis of urine samples: impact of sample preparation, storage conditions, and animal health status.

    Science.gov (United States)

    Schreier, Christina; Kremer, Werner; Huber, Fritz; Neumann, Sindy; Pagel, Philipp; Lienemann, Kai; Pestel, Sabine

    2013-01-01

    Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining (1)H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after (1)H NMR spectroscopy. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at -20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  14. Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

    Science.gov (United States)

    Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

    2014-05-01

    MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

  15. Stable dispersion of graphene solution prepared by hydrothermai reduction%高压釜热还原制备稳定分散的石墨烯溶液

    Institute of Scientific and Technical Information of China (English)

    冉启燕; 张海燕; 陈易明; 叶剑; 李春辉

    2012-01-01

    A improved Hummers method was employed to prepare graphite oxide using natural flake graphite as raw materials. The graphene oxide solution was prepared by ultrasonic dispersion, and the pH value of solution was changed through adding different volume fraction of hydrazine hydrate. After hydrothermal reduction in au- toclave, stable dispersion graphene solutions were obtained. The as prepared samples were characterized by X- ray diffraction, scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, atomic force microscope, zeta potential and optical microscope. The influence of temperature and pH value of the sta- bility of graphene solutions was investigated.%以天然鳞片石墨为原料,用改进的Hummers法制备氧化石墨。超声分散制备氧化石墨烯溶液,通过加入不同量的水合肼调节溶液的pH值,再通过水热法热还原,制备了在水中稳定分散的石墨烯溶液。利用扫描电子显微镜(SEM)、高分辨透射电镜(HR-TEM)、拉曼光谱(Raman)、原子力显微镜(AFM)、X射线衍射分析(XRD)、zeta电位及光学显微镜对制备的样品进行了表征,研究了不同温度、pH值对石墨烯溶液稳定性的影响。

  16. Automated Gel Size Selection to Improve the Quality of Next-generation Sequencing Libraries Prepared from Environmental Water Samples.

    Science.gov (United States)

    Uyaguari-Diaz, Miguel I; Slobodan, Jared R; Nesbitt, Matthew J; Croxen, Matthew A; Isaac-Renton, Judith; Prystajecky, Natalie A; Tang, Patrick

    2015-04-17

    Next-generation sequencing of environmental samples can be challenging because of the variable DNA quantity and quality in these samples. High quality DNA libraries are needed for optimal results from next-generation sequencing. Environmental samples such as water may have low quality and quantities of DNA as well as contaminants that co-precipitate with DNA. The mechanical and enzymatic processes involved in extraction and library preparation may further damage the DNA. Gel size selection enables purification and recovery of DNA fragments of a defined size for sequencing applications. Nevertheless, this task is one of the most time-consuming steps in the DNA library preparation workflow. The protocol described here enables complete automation of agarose gel loading, electrophoretic analysis, and recovery of targeted DNA fragments. In this study, we describe a high-throughput approach to prepare high quality DNA libraries from freshwater samples that can be applied also to other environmental samples. We used an indirect approach to concentrate bacterial cells from environmental freshwater samples; DNA was extracted using a commercially available DNA extraction kit, and DNA libraries were prepared using a commercial transposon-based protocol. DNA fragments of 500 to 800 bp were gel size selected using Ranger Technology, an automated electrophoresis workstation. Sequencing of the size-selected DNA libraries demonstrated significant improvements to read length and quality of the sequencing reads.

  17. Iron-based adsorbent prepared from Litchi peel biomass via pyrolysis process for the removal of pharmaceutical pollutant from synthetic aqueous solution.

    Science.gov (United States)

    Foletto, Vitória Segabinazzi; Ferreira, Ananda Bulegon; da Cruz Severo, Eric; Collazzo, Gabriela Carvalho; Foletto, Edson Luiz; Dotto, Guilherme Luiz

    2017-03-10

    A porous iron-based adsorbent obtained from litchi peel via pyrolysis process was prepared in this work, in order to evaluate its adsorptive potential for the removal of a pharmaceutical dye (amaranth) from aqueous solution. The material was characterized by X-ray diffraction, nitrogen adsorption-desorption isotherms, and scanning electron microscopy. Several isotherm and kinetic models were tested aiming to represent the amaranth dye adsorption. The prepared sample presented magnetic property, and a mesoporous texture constituted of graphite and three iron-based phases. The adsorption kinetics of amaranth on the adsorbent followed the pseudo-second-order model, whereas the equilibrium data were in good agreement with the BET isotherm, being represented by a sigmoid-shaped adsorption isotherm. The maximum adsorption capacity for the amaranth dye was found to be 44.87 mg g(-1), demonstrating that the material prepared in this work showed to be a promising adsorbent for the removal of amaranth from aqueous solution.

  18. Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

    Science.gov (United States)

    Wang, Xuan; Ye, Nengsheng

    2017-09-04

    In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  19. An On-Target Desalting and Concentration Sample Preparation Protocol for MALDI-MS and MS/MS Analysis

    DEFF Research Database (Denmark)

    Zhang, Xumin; Wang, Quanhui; Lou, Xiaomin;

    2012-01-01

    2DE coupled with MALDI-MS is one of the most widely used and powerful analytic technologies in proteomics study. The MALDI sample preparation method has been developed and optimized towards the combination of simplicity, sample-cleaning, and sample concentration since its introduction. Here we...... present a protocol of the so-called Sample loading, Matrix loading, and on-target Wash (SMW) method which fulfills the three criteria by taking advantage of the AnchorChip™ targets. Our method is extremely simple and no pre-desalting or concentration is needed when dealing with samples prepared from 2DE....... The protocol is amendable for automation and would pave the road for high-throughput MALDI-MS or MS/MS-based proteomics studies with guaranteed sensitivity and high identification rate. The method has been successfully applied to mouse liver proteome study and so far has been employed in other proteome studies...

  20. Preparation and Characterization of Coating Solution Based on Waterborne Polyurethane Dispersion containing Fluorine for Primer on Electro Galvanized Steel Sheet

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Chung Keun; Lim, Sung Hyung [Buhmwoo Institute of Technology Research, Hwaseong (Korea, Republic of)

    2015-10-15

    The purpose of this research was to synthesize fluorine modified waterborne polyurethane dispersion (F-WPU) by soap-free (internal emulsifier) emulsion polymerization techniques, to prepare coating solution based on fluorine modified waterborne polyurethane dispersion (F-WPU) and to compare the chemical and thermo-mechanical properties on the electrogalvanized steel sheet. Environmentally friendly F-WPU was prepared with a fluorinated polyol containing 60 wt% of fluorine. There are various ways of combining a wide variety of fluorinated polyols and diisocyanate to exhibit novel properties of waterborne polyurethane dispersion. Components of coating solution were largely divided into 4 kinds i.e., F-WPU, acrylic emulsion, silane coupling agent, and colloidal silicate. F-WPU coating solution on the electro-galvanized steel sheet showed excellent properties of corrosion resistance, alkali resistance and heat resistance, as compared to other coating solutions using a general waterborne resin. The F-WPU coating solution's reliable effects are possibly due to the fluorine atoms incorporated even in a small amount of F-WPU.

  1. Preparation

    Directory of Open Access Journals (Sweden)

    M.M. Dardir

    2014-03-01

    Full Text Available Some hexanamide-mono and di-linoleniate esters were prepared by the reaction of linolenic acid and hexanamide (derived from the reaction of hexanoic acid and diethanolamine. The chemical structure for the newly prepared hexanamide-mono and di-linoleniate esters were elucidated using elemental analysis, (FTIR, H 1NMR and chemical ionization mass spectra (CI/Ms spectroscopic techniques. The results of the spectroscopic analysis indicated that they were prepared through the right method and they have high purity. The new prepared esters have high biodegradability and lower toxicity (environmentally friendly so they were evaluated as a synthetic-based mud (ester-based mud for oil-well drilling fluids. The evaluation included study of the rheological properties, filtration and thermal properties of the ester based-muds formulated with the newly prepared esters compared to the reference commercial synthetic-based mud.

  2. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments

    Science.gov (United States)

    Round, Adam; Felisaz, Franck; Fodinger, Lukas; Gobbo, Alexandre; Huet, Julien; Villard, Cyril; Blanchet, Clement E.; Pernot, Petra; McSweeney, Sean; Roessle, Manfred; Svergun, Dmitri I.; Cipriani, Florent

    2015-01-01

    Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC. PMID:25615861

  3. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments.

    Science.gov (United States)

    Round, Adam; Felisaz, Franck; Fodinger, Lukas; Gobbo, Alexandre; Huet, Julien; Villard, Cyril; Blanchet, Clement E; Pernot, Petra; McSweeney, Sean; Roessle, Manfred; Svergun, Dmitri I; Cipriani, Florent

    2015-01-01

    Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC.

  4. Determination of Nd3+ Ions in Solution Samples by a Coated Wire Ion-Selective Sensor

    Directory of Open Access Journals (Sweden)

    Hassan Ali Zamani

    2012-01-01

    Full Text Available A new coated wire electrode (CWE using 5-(methylsulfanyl-3-phenyl-1H-1,2,4-triazole (MPT as an ionophore has been developed as a neodymium ion-selective sensor. The sensor exhibits Nernstian response for the Nd3+ ions in the concentration range of 1.0×10−6-1.0×10−2 M with detection limit of 3.7×10−7 M. It displays a Nernstian slope of 20.2±0.2 mV/decade in the pH range of 2.7–8.1. The proposed sensor also exhibits a fast response time of ∼5 s. The sensor revealed high selectivity with respect to all common alkali, alkaline earth, transition and heavy metal ions, including members of the lanthanide family other than Nd3+. The electrode was used as an indicator electrode in the potentiometric titration of Nd(III ions with EDTA. The electrode was also employed for the determination of the Nd3+ ions concentration in water solution samples.

  5. Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

    Science.gov (United States)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

    2012-01-01

    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  6. CTEPP STANDARD OPERATING PROCEDURE FOR PREPARATION OF SURROGATE RECOVERY STANDARD AND INTERNAL STANDARD SOLUTIONS FOR POLAR TARGET ANALYTES (SOP-5.26)

    Science.gov (United States)

    This SOP describes the method used for preparing surrogate recovery standard and internal standard solutions for the analysis of polar target analytes. It also describes the method for preparing calibration standard solutions for polar analytes used for gas chromatography/mass sp...

  7. Evaluation of Electrospray as a Sample Preparation Tool for Electron Microscopic Investigations: Toward Quantitative Evaluation of Nanoparticles.

    Science.gov (United States)

    Mielke, Johannes; Dohányosová, Pavla; Müller, Philipp; López-Vidal, Silvia; Hodoroaba, Vasile-Dan

    2017-02-01

    The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension.

  8. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments

    Energy Technology Data Exchange (ETDEWEB)

    Round, Adam, E-mail: around@embl.fr; Felisaz, Franck [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Fodinger, Lukas; Gobbo, Alexandre [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Huet, Julien [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Villard, Cyril [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Blanchet, Clement E., E-mail: around@embl.fr [EMBL c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Pernot, Petra; McSweeney, Sean [ESRF, 6 Rue Jules Horowitz, 38000 Grenoble (France); Roessle, Manfred; Svergun, Dmitri I. [EMBL c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Cipriani, Florent, E-mail: around@embl.fr [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France)

    2015-01-01

    A robotic sample changer for solution X-ray scattering experiments optimized for speed and to use the minimum amount of material has been developed. This system is now in routine use at three high-brilliance European synchrotron sites, each capable of several hundred measurements per day. Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC.

  9. Characterization and Electrochemical Properties of LiMn2O4 Thin Films Prepared by Solution Deposition

    Institute of Scientific and Technical Information of China (English)

    WU Xianming; HE Zeqiang; XU Mingfei; LI Xinhai; XIAO Zhuobing

    2006-01-01

    LiMn2O4 thin films were prepared by solution deposition using lithium acetate and manganese acetate as raw materials. The phase constitution and surface morphology were observed by X-ray diffraction and scanning electron microscopy. The electrochemical properties of the thin films were studied by cyclic voltammetry, charge-discharge experiments and impedance spectroscopy in 1 mol·L-1 LiPF6/EC-DMC solution using lithium metal as both the counter and reference electrodes. The films prepared by this method are of spinel phase. The lattice parameter increases with the annealing temperature and annealing time. The film annealed at 750 ℃ for 30 minutes has the highest capacity of 34.5 μAh·cm-2·μm-1, and its capacity loss per cycle is 0.05% after being cycled 100 times.

  10. Monitoring of praseodymium(III) ions in aqueous solutions, soil and sediment samples by a PVC membrane sensor based on a furan-triazole derivative

    Energy Technology Data Exchange (ETDEWEB)

    Pourjavid, Mohammad Reza [Islamic Azad University, Tehran (Iran, Islamic Republic of). Dept. of Medicinal Chemistry. Nuclear Science and Technology Research Institute; Rezaee, Mohammad; Hosseini, Majid Haji [Nuclear Science and Technology Research Institute, Tehran (Iran, Islamic Republic of); Razavi, Taherehsadat, E-mail: pourjavid@gmail.com [Research Institute of Petroleum Industry, Tehran (Iran, Islamic Republic of). Instrumental Analysis Dept.

    2012-07-01

    A furan-triazole derivative has been explored as an ionophore for preparation of a highly selective Pr(III) membrane sensor. The proposed sensor exhibits a Nernstian response for Pr(III) activity over a wide concentration range with a detection limit of 5.2 x 10{sup -8}M. Its response is independent of pH of the solution in the range 3.0-8.8 and offers the advantages of fast response time. To investigate the analytical applicability of the sensor, it was applied successfully as an indicator electrode in potentiometric titration of Pr(III) solution and also in the direct and indirect determination of trace Pr(III) ions in some samples. (author)

  11. Microstructural features of the La{sub 1−x}Ca{sub x}FeO{sub 3−δ} solid solutions prepared via Pechini route

    Energy Technology Data Exchange (ETDEWEB)

    Gerasimov, E.Yu., E-mail: gerasimov@catalysis.ru [Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Pr. Acad. Lavrentieva 5, Novosibirsk 630090 (Russian Federation); Novosibirsk State University, Pirogova Str. 2, Novosibirsk 630090 (Russian Federation); Isupova, L.A. [Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Pr. Acad. Lavrentieva 5, Novosibirsk 630090 (Russian Federation); Tsybulya, S.V. [Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Pr. Acad. Lavrentieva 5, Novosibirsk 630090 (Russian Federation); Novosibirsk State University, Pirogova Str. 2, Novosibirsk 630090 (Russian Federation)

    2015-10-15

    Highlights: • La{sub 1−x}Ca{sub x}FeO {sub (3−δ)} (0 ≤ x ≤ 0.7) perovskite were prepared by Pechini method. • Planar defects in direction (1 0 1) were observed in the perovskite surface. • α-Fe{sub 2}O{sub 3} particles (1–10 nm) on the surface of perovskite were revealed. • Amount of α-Fe{sub 2}O{sub 3} particles on the perovskite surface grew with rising x values. - Abstract: Solid solutions with La{sub 1−x}Ca{sub x}FeO{sub 3−δ} (0 ≤ x ≤ 0.7) perovskite-like structure prepared via Pechini route have been investigated by using high resolution transmission electron microscopy and X-ray diffraction. Extended planar defects lying in (1 0 1) crystallographic planes and α-Fe{sub 2}O{sub 3} nanoparticles on the surface of perovskite microcrystals are characteristic of the samples under investigation. It was found that testing of the samples in catalytic deep CH{sub 4} oxidation process results in partial destruction of solid solutions with formation of planar defects in the bulk and α-Fe{sub 2}O{sub 3} particles on the surface.

  12. Recovery of Salmonella from internally and externally contaminated whole tomatoes using several different sample preparation procedures.

    Science.gov (United States)

    Wang, Hua; Gill, Vikas S; Irvin, Kari A; Byrd, Mindi; Bolger, Cathryn M; Zheng, Jie; Dickey, Erin E; Duvall, Robert E; Jacobson, Andrew P; Hammack, Thomas S

    2012-01-01

    Studies were conducted to determine the relative effectiveness of whole soak [current Bacteriological Analytical Manual-(BAM) Salmonella method], quarter, stomach, and blend methods for the recovery of Salmonella organisms from internally and externally contaminated tomatoes. Tomatoes were subjected to three inoculation methods: surface inoculation, internal inoculation by injection, and immersion with single Salmonella serovars. The inoculation levels ranged from 1 to 100 CFU/tomato for surface and injection inoculation or 1 to 100 CFU/mL for immersion inoculation. Tomatoes were held for 3 days after inoculation at 2-6 degrees C prior to initiation of analysis. Contaminated tomatoes were soaked, quartered, stomached, and blended in appropriate portions of Universal Pre-enrichment broth, and incubated for 24 h at 35 +/- 2 degrees C. The BAM Salmonella culture method was followed thereafter, and tomatoes were treated as a low-microbial-load food. The stomaching procedure was significantly (P < 0.05) more effective than the whole soak procedure for recovery of internalized Salmonella from tomatoes (by injection). The blending procedure was arithmetically superior to the stomaching procedure for detection of internalized Salmonella from tomatoes (by immersion). The blending procedure showed the same effectiveness as the whole soak procedure for the detection of Salmonella on tomato surfaces. Comparisons between test portion-to-broth ratios (weight to volume) showed that a 1:3 test portion-to-broth ratio had a better buffering capacity for blended tomatoes than a 1:1 test portion-to-broth ratio. It is recommended that the current whole soak BAM tomato sample preparation procedure be replaced with a blending procedure and a 1:3 test portion-to-broth ratio.

  13. Preparative chromatography for specific δ13C isotopic analysis of individual carbohydrates in environmental samples

    Science.gov (United States)

    Nouara, Amel; Panagiotopoulos, Christos; Balesdent, Jérôme; Sempéré, Richard

    2017-04-01

    Carbohydrates are among the most abundant organic molecules on the Earth and are present in all geochemical systems. Despite their high abundance in the environment, very few studies assessed their origin using molecular carbohydrate isotopic analyses. In contrast with bulk stable isotope analysis (BSIA), which gives the isotopic signature of the entire sample without any specification about its chemical composition, compound specific 13C isotopic analysis of individual sugars (CSIA) offers valuable information about the origin of single molecules. Previous investigations used gas or liquid chromatography coupled with isotope ratio mass spectroscopy (GC-IRMS; HPLC-IRMS) for CSIA of sugars however the former requires δ13C corrections due to the carbon added to the sugar (derivatization) while the later does not provide always adequate separations among monosaccharides. Here we used cation preparative chromatography (Ca2+, Pb2+ and Na+) with refractive index detection in order to produce pure monosaccharide targets for subsequent EA-IRMS analyses. Milli-Q water was used as eluant at a flow rate 0.6 ml min-1. In general, three successive purifications (Ca2+, Pb2+, Ca2+) were sufficient to produce pure compounds. Pure monosaccharides were compared with authentic monosaccharide standards using 1H NMR and/or mass spectroscopy. The detection limit of our technique was about 1µM/sugar with a precision of 10% (n=6). Blanks run with Milli-Q water after three successive purifications resulted in carbon content of 0.13 to 2.77 µgC per collected sugar. These values are much lower than the minimum required amount (5 µgC) of the EA-IRSMS system with a precision of ± 0.35 ‰. Application of our method to environmental samples resulted in δ13C values of glucose, fructose, and levoglucosan in the range of -24 to -26 ‰ (PM10 atmospheric particles), and -15‰ to -22 ‰ for arabinose, glucose, and xylose (marine high molecular dissolved organic matter). These results fall in

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

    Science.gov (United States)

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

    2014-01-01

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

  15. Quantitative in-situ TEM nanotensile testing of single crystal Ni facilitated by a new sample preparation approach.

    Science.gov (United States)

    Samaeeaghmiyoni, Vahid; Idrissi, Hosni; Groten, Jonas; Schwaiger, Ruth; Schryvers, Dominique

    2017-03-01

    Twin-jet electro-polishing and Focused Ion Beam (FIB) were combined to produce small size Nickel single crystal specimens for quantitative in-situ nanotensile experiments in the transmission electron microscope. The combination of these techniques allows producing samples with nearly defect-free zones in the centre in contrast to conventional FIB-prepared samples. Since TEM investigations can be performed on the electro-polished samples prior to in-situ TEM straining, specimens with desired crystallographic orientation and initial microstructure can be prepared. The present results reveal a dislocation nucleation-controlled plasticity, in which small loops induced by FIB near the edges of the samples play a central role. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Preparation and Photocatalytic Properties of Ti1-xZrxO2 Solid Solution

    Institute of Scientific and Technical Information of China (English)

    GAO,Bi-Fen; MA,Ying; CAO,Ya-An; GU,Zhan-Jun; ZHANG,Guang-Jin; YAO,Jian-Nian

    2007-01-01

    A series of Ti1-xZrxO2 materials were synthesized through a multistep sol-gel process.The structural characteristics were investigated using X-ray diffraction(XRD),X-ray photoelectron spectroscopy(XPS)and Raman measurements.The experimental results showed that a solid solution could be obtained at low Zr/(Ti+Zr)molar ratios(x≤0.319).Raman measurements exhibited that the presence of zirconium in the solid solutions greatly retarded the amoorphous-anatase and anatase-rutile transitions.The diffuse reflectance UV-Vis spectra revealed that the bandgap of the solid solution was enlarged gradually with the increment of incorporated zirconium content.The Til-xZrxO2solid solutions exhibited higher photocatalytic activity than pure TiO2 for the degradation of 4-chlorophenol aqueous solution.

  17. Development of a surface plasmon resonance biosensing approach for the rapid detection of porcine circovirus type2 in sample solutions.

    Directory of Open Access Journals (Sweden)

    Jiandong Hu

    Full Text Available A sensitive and label-free analytical approach for the detection of porcine circovirus type 2 (PCV2 instead of PCV2 antibody in serum sample was systematically investigated in this research based on surface plasmon resonance (SPR with an establishment of special molecular identification membrane. The experimental device for constructing the biosensing analyzer is composed of an integrated biosensor, a home-made microfluidic module, and an electrical control circuit incorporated with a photoelectric converter. In order to detect the PCV2 using the surface plasmon resonance immunoassay, the mercaptopropionic acid has been used to bind the Au film in advance through the known form of the strong S-Au covalent bonds formed by the chemical radical of the mercaptopropionic acid and the Au film. PCV2 antibodies were bonded with the mercaptopropionic acid by covalent -CO-NH- amide bonding. For the purpose of evaluating the performance of this approach, the known concentrations of PCV2 Cap protein of 10 µg/mL, 7.5 µg/mL, 5 µg/mL, 2.5 µg/mL, 1 µg/mL, and 0.5 µg/mL were prepared by diluting with PBS successively and then the delta response units (ΔRUs were measured individually. Using the data collected from the linear CCD array, the ΔRUs gave a linear response over a wide concentration range of standard known concentrations of PCV2 Cap protein with the R-Squared value of 0.99625. The theoretical limit of detection was calculated to be 0.04 µg/mL for the surface plasmon resonance biosensing approach. Correspondingly, the recovery rate ranged from 81.0% to 89.3% was obtained. In contrast to the PCV2 detection kits, this surface plasmon resonance biosensing system was validated through linearity, precision and recovery, which demonstrated that the surface plasmon resonance immunoassay is reliable and robust. It was concluded that the detection method which is associated with biomembrane properties is expected to contribute much to determine the PCV2

  18. Development of a surface plasmon resonance biosensing approach for the rapid detection of porcine circovirus type2 in sample solutions.

    Science.gov (United States)

    Hu, Jiandong; Wang, Tingting; Wang, Shun; Chen, Mingwen; Wang, Manping; Mu, Linying; Chen, Hongyin; Hu, Xinran; Liang, Hao; Zhu, Juanhua; Jiang, Min

    2014-01-01

    A sensitive and label-free analytical approach for the detection of porcine circovirus type 2 (PCV2) instead of PCV2 antibody in serum sample was systematically investigated in this research based on surface plasmon resonance (SPR) with an establishment of special molecular identification membrane. The experimental device for constructing the biosensing analyzer is composed of an integrated biosensor, a home-made microfluidic module, and an electrical control circuit incorporated with a photoelectric converter. In order to detect the PCV2 using the surface plasmon resonance immunoassay, the mercaptopropionic acid has been used to bind the Au film in advance through the known form of the strong S-Au covalent bonds formed by the chemical radical of the mercaptopropionic acid and the Au film. PCV2 antibodies were bonded with the mercaptopropionic acid by covalent -CO-NH- amide bonding. For the purpose of evaluating the performance of this approach, the known concentrations of PCV2 Cap protein of 10 µg/mL, 7.5 µg/mL, 5 µg/mL, 2.5 µg/mL, 1 µg/mL, and 0.5 µg/mL were prepared by diluting with PBS successively and then the delta response units (ΔRUs) were measured individually. Using the data collected from the linear CCD array, the ΔRUs gave a linear response over a wide concentration range of standard known concentrations of PCV2 Cap protein with the R-Squared value of 0.99625. The theoretical limit of detection was calculated to be 0.04 µg/mL for the surface plasmon resonance biosensing approach. Correspondingly, the recovery rate ranged from 81.0% to 89.3% was obtained. In contrast to the PCV2 detection kits, this surface plasmon resonance biosensing system was validated through linearity, precision and recovery, which demonstrated that the surface plasmon resonance immunoassay is reliable and robust. It was concluded that the detection method which is associated with biomembrane properties is expected to contribute much to determine the PCV2 in sample

  19. GC/MS method for determining carbon isotope enrichment and concentration of underivatized short-chain fatty acids by direct aqueous solution injection of biogas digester samples.

    Science.gov (United States)

    Mulat, Daniel Girma; Feilberg, Anders

    2015-10-01

    In anaerobic digestion of organic matter, several metabolic pathways are involved during the simultaneous production and consumption of short-chain fatty acids (SCFA) in general and acetate in particular. Understanding the role of each pathway requires both the determination of the concentration and isotope enrichment of intermediates in conjunction with isotope labeled substrates. The objective of this study was to establish a rapid and simple GC/MS method for determining the isotope enrichment of acetate and concentration of underivatized short-chain fatty acids (SCFA) in biogas digester samples by direct liquid injection of acidified aqueous samples. Sample preparation involves only acidification, centrifugation and filtration of the aqueous solution followed by direct injection of the aqueous supernatant solution onto a polar column. With the sample preparation and GC/MS conditions employed, well-resolved and sharp peaks of underivatized SCFA were obtained in a reasonably short time. Good recovery (96.6-102.3%) as well as low detection (4-7 µmol/L) and quantification limits (14-22 µmol/L) were obtained for all the 6 SCFA studied. Good linearity was achieved for both concentration and isotope enrichment measurement with regression coefficients higher than 0.9978 and 0.9996, respectively. The method has a good intra- and inter-day precision with a relative standard deviation (RSD) below 6% for determining the tracer-to-tracee ratio (TTR) of both [2-(13)C]acetate and [U-(13)C]acetate. It has also a good intra- and inter-day precision with a RSD below 6% and 5% for determining the concentration of standard solution and biogas digester samples, respectively. Acidification of biogas digester samples with oxalic acid provided the low pH required for the protonation of SCFA and thus, allows the extraction of SCFA from the complex sample matrix. Moreover, oxalic acid was the source of formic acid which was produced in the injector set at high temperature. The produced

  20. Preparation and Characterization of Palmitoyl Grafted Cellulose Nano Absorbent for the Efficient Adsorption of Pyrene from Aqueous Solution.

    Science.gov (United States)

    Jadhav, Arvind H; Mai, Xuan Thang; Appiah-Ntiamoah, Richard; Lee, Hanyeong; Momade, Francis W Y; Seo, Jeong Gil; Kim, Hern

    2015-10-01

    Palmitoyl grafted modified cellulose were prepared by simple chemical grafting method and applied as nano adsorbent for removal of pyrene from aqueous solution. The chemical properties and morphology of prepared nano-adsorbent were characterized by FT-IR, XRD, SEM, EDX, TGA, and contact angle. Results showed that palmitoyl successfully grafted on the surface of cellulose and possess effective organic functional groups for the adsorption of pyrene from aqueous solution. The adsorption performance of modified cellulose was significantly improved toward pyrene in aqueous solution. It is worthy to note that 0.25 g of palmitoyl grafted cellulose (PMC) removed 92% pyrene compared to unmodified cellulose which adsorbed 36% pyrene from 1.65 ppm aqueous solution of pyrene in very short contact time at room temperature. Results showed that, presence of various organic functional groups from palmitoyl chains grafted on cellulose backbone affected to pyrene removal. After completion of adsorption phenomenon nano-adsorbent can be removed by simply filtration process and reused several times. The adsorption capacity was studied under different experimental conditions and their effects on adsorption such as temperature, pH, and contact time were also studied. The kinetics and isotherms of material were also determined.

  1. Effective removal of tetracycline from aqueous solution using activated carbon prepared from tomato (Lycopersicon esculentum Mill.) industrial processing waste.

    Science.gov (United States)

    Sayğılı, Hasan; Güzel, Fuat

    2016-09-01

    Activated carbon (TAC) prepared under optimized conditions with ZnCl2 activation from a new precursor; tomato industrial processing waste (TW), was applied as an adsorbent to remove tetracycline (TC) from aqueous solution. The factors (TAC dosage, initial TC concentration, contact time, ionic strength and solution temperature) affecting the adsorption process were examined at natural pH (5.7) of TAC-TC system in aqueous solution. Kinetic data was found to be best complied by the pseudo-second order model. The isotherm analysis indicated that the equilibrium data could be represented by the Langmuir model. The maximum adsorption capacity was identified as 500.0mgg(-1) at 308K.

  2. Comparative study of the various methods of preparation of silicate solution and its effect on the geopolymerization reaction

    Science.gov (United States)

    Essaidi, N.; Laou, L.; Yotte, S.; Ulmet, L.; Rossignol, S.

    This paper is based on the characterization of synthesized geopolymer binders based on either powder or solution silicate, and the amount of water contained in synthesized binders is determined to evaluate their possibility to coat a brick. The structural evolution of the formed geopolymers was investigated using FTIR spectroscopy. The mechanical properties were evaluated using compression tests. The structural evolution ensured that the solutions prepared from silicate powder or liquid had different degrees of polymerization, which modified the polycondensation reaction of the mixture. Nevertheless, the use of aluminosilicate solutions based on powder or liquid display similar behavior in a polycondensation reaction. The obtained materials show good mechanical properties, and it is possible to deposit this binder on the brick depending on the water content.

  3. Development of a Novel Self-Enclosed Sample Preparation Device for DNA/RNA Isolation in Space

    Science.gov (United States)

    Zhang, Ye; Mehta, Satish K.; Pensinger, Stuart J.; Pickering, Karen D.

    2011-01-01

    Modern biology techniques present potentials for a wide range of molecular, cellular, and biochemistry applications in space, including detection of infectious pathogens and environmental contaminations, monitoring of drug-resistant microbial and dangerous mutations, identification of new phenotypes of microbial and new life species. However, one of the major technological blockades in enabling these technologies in space is a lack of devices for sample preparation in the space environment. To overcome such an obstacle, we constructed a prototype of a DNA/RNA isolation device based on our novel designs documented in the NASA New Technology Reporting System (MSC-24811-1/3-1). This device is self-enclosed and pipette free, purposely designed for use in the absence of gravity. Our design can also be modified easily for preparing samples in space for other applications, such as flowcytometry, immunostaining, cell separation, sample purification and separation according to its size and charges, sample chemical labeling, and sample purification. The prototype of our DNA/RNA isolation device was tested for efficiencies of DNA and RNA isolation from various cell types for PCR analysis. The purity and integrity of purified DNA and RNA were determined as well. Results showed that our developed DNA/RNA isolation device offers similar efficiency and quality in comparison to the samples prepared using the standard protocol in the laboratory.

  4. An automated on-line multidimensional HPLC system for protein and peptide mapping with integrated sample preparation

    NARCIS (Netherlands)

    Wagner, K.; Miliotis, T.; Marko-Varga, G; Bischoff, Rainer; Unger, K.K.

    2002-01-01

    A comprehensive on-line two-dimensional 2D-HPLC system with integrated sample preparation was developed for the analysis of proteins and peptides with a molecular weight below 20 kDa. The system setup provided fast separations and high resolving power and is considered to be a complementary techniqu

  5. A novel sample preparation method of matrix-assisted laser desorption/ionization time of flight mass spectrometry for polystyrene

    Institute of Scientific and Technical Information of China (English)

    Shu Zhang; Zhen Wen Zhao; Lei Xiong; Bin Xin; Wei Hua Hu; Shao Xiang Xiong

    2007-01-01

    A novel sample preparation method of matrix-assisted laser desorption/ionization mass spectrometry for polystyrene was reported.Compared to the conventional dried-droplet method, the efficiency of ionization and signal intensity of mass spectra were improved.The mechanism was also analyzed.

  6. Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

    Energy Technology Data Exchange (ETDEWEB)

    Bannochie, C. J. [Savannah River Site (SRS), Aiken, SC (United States); Diprete, D. P. [Savannah River Site (SRS), Aiken, SC (United States); Pareizs, J. M. [Savannah River Site (SRS), Aiken, SC (United States)

    2016-02-10

    Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

  7. Sludge batch 9 (SB9) accepance evaluation: Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

    Energy Technology Data Exchange (ETDEWEB)

    Bannochie, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Diprete, D. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Pareizs, J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-03-01

    Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

  8. [Preparation and immunological evaluation of oral solution of egg yolk-derived hepatitis B virus-specific transfer factor].

    Science.gov (United States)

    Xu, Yanping; Zhang, Qing; Zhan, Xuejun; Xie, Daze; Dai, Ge; Yang, Hui

    2013-12-01

    To prepare the oral solution of egg yolk hepatitis B virus (HBV)-specific transfer factor (EYHBV-TF) and evaluate its immunological activity as an immune regulator against hepatitis B. From hens immunized with the Hepatitis B vaccine the egg yolk was isolated to extract the specific transfer factor EYHBV-TF, and its physicochemical properties were examined. Leukocyte adhesion inhibition test (LAI) was performed to detect the immunogenic activity of EYHBV-TF. The solution of EYHBV-TF was then administered orally in normal mice, and the specific cellular immune activity induced was assayed with delayed type skin hypersensitivity test (DTH), with the non-specific immune activity assessed with immune organ index. The immune responses induced by oral EYHBV-STF solution were compared with those by EYHBV-STF injection and by different dosages (injection and oral) of porcine spleen HBV-specific transfer factor (PSHBV-STF), porcine spleen nonspecific transfer factor, and egg yolk extracts from non-immunized hens. The prepared EYHBV-STF oral solution, which met the standards for biological products, could inhibit leukocyte adhesion in vitro and significantly enhance mouse foot pad swelling, demonstrating its capability of transferring antigen-specific delayed type hypersensitivity reactions to naive recipient. EYHBV-STF oral solution also significantly improved the immune organ index in mice (P<0 01) with similar effects to those caused by EYHBV-STF injections and by PSHBV-STF injection and oral solution. Orally administered EYHBV-STF and EYHBV-STF injection both possess hepatitis B antigen-specific cellular immune activity and can significantly enhance specific cellular immune responses.

  9. Synthesis, sintering and dissolution of thorium and uranium (IV) mixed oxide solid solutions: influence of the method of precursor preparation; Synthese, frittage et caracterisation de solutions solides d'oxydes mixtes de thorium et d'uranium (IV): influence de la methode de preparation du precurseur

    Energy Technology Data Exchange (ETDEWEB)

    Hingant, N

    2008-12-15

    Mixed actinide dioxides are currently considered as potential fuels for the third and fourth generations of nuclear reactors. In this context, thorium-uranium (IV) dioxide solid solutions were studied as model compounds to underline the influence of the method of preparation on their physico-chemical properties. Two methods of synthesis, both based on the initial precipitation of oxalate precursors have been developed. The first consisted in the direct precipitation ('open' system) while the second involved hydrothermal conditions ('closed' system). The second method led to a significant improvement in the crystallization of the samples especially in the field of the increase of the grain size. In these conditions, the formation of a complete solid solution Th{sub 1-x}U{sub x}(C{sub 2}O{sub 4}){sub 2}.2H{sub 2}O was prepared between both end-members. Its crystal structure was also resolved. Whatever the initial method considered, these compounds led to the final dioxides after heating above 400 C. The various steps associated to this transformation, involving the dehydration of precursors then the decomposition of oxalate groups have been clarified. Moreover, the use of wet chemistry methods allowed to reduce the sintering temperature of the final thorium-uranium (IV) dioxide solid solutions. Whatever the method of preparation considered, dense samples (95% to 97% of the calculated value) were obtained after only 3 hours of heating at 1500 C. Additionally, the use of hydrothermal conditions significantly increased the grain size, leading to the reduction of the occurrence of the grain boundaries and of the global residual porosity. The significant improvement in the homogeneity of cations distribution in the samples was also highlighted. Finally, the chemical durability of thorium-uranium (IV) dioxide solid solutions was evaluated through the development of leaching tests in nitric acid. The optimized homogeneity especially in terms of the

  10. Phase analysis of aluminium modified GeSbTe bulk prepared from XRD of samples

    Science.gov (United States)

    Sandhu, Sharanjit; Singh, D.; Kumar, S.; Thangaraj, R.

    2016-05-01

    Various compositions of Aluminium modified GST as Alx(Ge2Sb2Te5)1-x x= 0, 0.15, 0.20, 0.25, 0.30 are prepared to study as a phase change material. Bulk prepared is studied with XRD scans for various phases formed. Phases other than Ge2Sb2Te5 do come in but dominated one is Ge2Sb2Te5 hexagonal phase.

  11. Determination of total iodine in serum and urine samples by ion chromatography with pulsed amperometric detection - studies on analyte loss, optimization of sample preparation procedures, and validation of analytical method.

    Science.gov (United States)

    Błażewicz, Anna; Klatka, Maria; Dolliver, Wojciech; Kocjan, Ryszard

    2014-07-01

    A fast, accurate and precise ion chromatography method with pulsed amperometric detection was applied to evaluate a variety of parameters affecting the determination of total iodine in serum and urine of 81 subjects, including 56 obese and 25 healthy Polish children. The sample pretreatment methods were carried out in a closed system and with the assistance of microwaves. Both alkaline and acidic digestion procedures were developed and optimized to find the simplest combination of reagents and the appropriate parameters for digestion that would allow for the fastest, least time consuming and most cost-effective way of analysis. A good correlation between the certified and the measured concentrations was achieved. The best recoveries (96.8% for urine and 98.8% for serum samples) were achieved using 1ml of 25% tetramethylammonium hydroxide solution within 6min for 0.1ml of serum/urine samples. Using 0.5ml of 65% nitric acid solution the best recovery (95.3%) was obtained when 7min of effective digestion time was used. Freeze-thaw stability and long-term stability were checked. After 24 weeks 14.7% loss of iodine in urine, and 10.9% in serum samples occurred. For urine samples, better correlation (R(2)=0.9891) of various sample preparation procedures (alkaline digestion and application of OnGuard RP cartidges) was obtained. Significantly lower iodide content was found in samples taken from obese children. Serum iodine content in obese children was markedly variable in comparison with the healthy group, whereas the difference was less evident when urine samples were analyzed. The mean content in serum was 59.12±8.86μg/L, and in urine 98.26±25.93 for obese children when samples were prepared by the use of optimized alkaline digestion reinforced by microwaves. In healthy children the mean content in serum was 82.58±6.01μg/L, and in urine 145.76±31.44μg/L.

  12. Preparation and characterization of chitosan-clay nanocomposites for the removal of Cu(II) from aqueous solution.

    Science.gov (United States)

    Azzam, Eid M S; Eshaq, Gh; Rabie, A M; Bakr, A A; Abd-Elaal, Ali A; El Metwally, A E; Tawfik, Salah M

    2016-08-01

    In the present study, chitosan assembled on gold and silver nanoparticles were prepared and characterized by UV-vis, TEM, EDX and DLS techniques. The nanocomposites chitosan (Ch)/clay, chitosan (Ch)/AgNPs/clay and chitosan (Ch)/AuNPs/clay were prepared by solution mixing method and characterized by FTIR, XRD, and SEM techniques. The adsorption of copper(II) ions onto the prepared hybrid composites from an aqueous solution using batch adsorption was examined. The results showed that benefiting from the surface property of clay, the abundant amino and hydroxyl functional groups of chitosan, the adsorbent provides adequate and versatile adsorption for the Cu(II) ions under investigation. The batch adsorption experiments showed that the adsorption of the Cu(II) is considerably dependent on pH of milieu, the amount of adsorbent, and contact time. Batch adsorption studies revealed that the adsorption capacity of Cu(II) increased with increase in initial concentration and contact time with optimum pH in the range around neutral. The maximum uptake of Cu(II) ions by (Ch)/AgNPs/clay composite was found to be 181.5mg/g. The adsorption efficiency of Cu(II) ions by prepared (Ch)/AgNPs/clay and (Ch)/AuNPs/clay is bigger than that the individual chitosan (Ch)/clay composite which clarifies the role of metal nanoparticles in enhancement the adsorption characters. The study suggests that the (Ch)/AgNPs/clay hybrid composite is a promising nano-adsorbent for the removal of Cu(II) ions from aqueous solution.

  13. Safety and quality assurance of chemotherapeutic preparations in a hospital production unit: acceptance sampling plan and economic impact.

    Science.gov (United States)

    Paci, A; Borget, I; Mercier, L; Azar, Y; Desmaris, R P; Bourget, P

    2012-06-01

    The opportunity to apply a sampling plan was evaluated. Costs were computed by a microcosting study. In 2003, a sampling plan was defined to reduce the number of chemotherapy quality controls while preserving the same level of quality. Recent qualitative and quantitative changes led us to define a second sampling plan supplemented by an economic evaluation to determine the cost and cost-savings of quality control. The study considers preparation produced during four semesters classified into three groups. The first one includes drugs produced below 200 batches a semester. Group 2, those for which the lot of preparation lots would have been rejected twice among these four semesters. Group 3, those would have been accepted (≥3 'acceptable lot'). A single sampling plan by attributes was applied to this group with an acceptance quality level of 1.65% and a lot tolerance percent defective below 5%. A micro-costing study was conducted on quality control, from the sampling to the validation of the results. Among 39 cytotoxic drugs, 11 were sampled which enabled to avoid a mean of 17,512 control assays per year. Each batch of the 28 non-sampled drugs was however analyzed. Costs were estimated at 2.98€ and 5.25€ for control assays depending of the analytical method. The savings from the application of the sampling plans was 153,207€ in 6 years. The sampling plan allowed maintaining constancy in number of controls and the level of quality with significant costsavings, despite a substantial increase in drugs to assay and in the number of preparations produced.

  14. Combining Endometrium Sampling Device and SurePath Preparation to Screen for Endometrial Carcinoma: A Validation Study

    Directory of Open Access Journals (Sweden)

    Jia Wen

    2015-01-01

    Full Text Available Background: The aim of this study was to compare specimen adequacy of SAP-1 provided for cytology with that of dilation and curettage (D & C or hysteroscopy for histology, and evaluate the accuracy of combining endometrium sampling by SAP-1 and liquid-based cytology using SurePath preparation for screening endometrial carcinoma and its precursor. Methods: Endometrial specimens from women (n = 1514 with risk factors were obtained using an SAP-1 device for cytological analysis; histological samples were obtained from 375 of these women who underwent D & C or hysteroscopy. Cytological specimens were prepared to liquid-based smear using SurePath technology and stained by Papanicolaou. Histological samples were processed in routine pathology and stained by hematoxylin and eosin. Results: Adequate specimens for cytology were obtained from 1458/1541 patients (96.3%, while adequate samples for pathology were obtained from 285/375 patients (76%. However, for postmenopausal women, 1006 of 1045 cytology (86.3% were adequate, 153 of 238 histology (64.3% were adequate, it was easier to collect cytological specimens than histological specimens (P < 0.05. The accuracy of endometrial cytology for detecting endometrial carcinoma and its precursor was 92.4% (sensitivity, 73%; specificity, 95.8%; positive predictive value, 75%; and negative predictive value, 95.3%. Conclusions: Endometrial cytology using SAP-1 sampling and SurePath preparation may be a reliable approach for screening patients with endometrial carcinoma and its precursor.

  15. Continuous-flow PCR using segmented flow and integrating sample preparation

    Science.gov (United States)

    Becker, Holger; Hlawatsch, Nadine; Carstens, Cornelia; Klemm, Richard; Gärtner, Claudia

    2009-02-01

    Continuous-flow PCR has proven to be a powerful method for the amplification of genetic material due to its high speed and the possibility to perform amplicon detection and separation on-chip. A unique possibility of this method is the simultaneous amplification of several samples within a single chip by sample stacking, either having identical samples in several sample plugs separated by e.g. a mineral oil or using different samples in each sample plug. We have demonstrated the viability of sample stacking with a commercially available continuous-flow PCR system with a variety of protocols and samples. Further integration steps like thermal lysis and on-chip lyophilisate storage have been performed, with subsequent successful PCR. Chip modules for DNA extraction either with magnetic beads or membrane filters have been developed.

  16. Powder Handling Device for X-ray Diffraction Analysis with Minimal Sample Preparation Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This project consists of developing a Vibrating Sample Holder (VSH) for planetary X-Ray Diffraction (XRD) instruments. The principle of this novel sample handling...

  17. Preparation and adsorption properties of nano magnetite chitosan films for heavy metal ions from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Lasheen, M.R., E-mail: ragaei24@link.net [Water Pollution Research Department, Environmental Research Division, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); El-Sherif, Iman Y., E-mail: iman57us@yahoo.com [Water Pollution Research Department, Environmental Research Division, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); Tawfik, Magda E., E-mail: magdaemileta@yahoo.com [Polymers and Pigments Department, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); El-Wakeel, S.T., E-mail: shaimaa_tw@yahoo.com [Water Pollution Research Department, Environmental Research Division, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); El-Shahat, M.F., E-mail: elshahatmf@hotmail.com [Faculty of Science, Ain Shams University, Khalifa El-Maamon St., Abbasiya Sq., 11566, Cairo (Egypt)

    2016-08-15

    Highlights: • Nano magnetite–chitosan films were prepared by casting method. • The efficiency of the prepared films for removing heavy metals was investigated. • The adsorption mechanism was studied using different isotherm and kinetic models. • Films reuse and metals recovery were studied. - Abstract: Nano magnetite chitosan (NMag–CS) film was prepared and characterized with different analytical methods. X-ray diffraction (XRD) patterns confirmed the formation of a pure magnetite structure and NMag–CS nanocomposite. TEM image of the film, revealed the uniform dispersion of magnetite nanoparticles inside chitosan matrix. The adsorption properties of the prepared film for copper, lead, cadmium, chromium and nickel metal ions were evaluated. Different factors affecting the uptake behavior by the composite films such as time, initial pH and film dose were investigated. The adsorption equilibrium attained using 2 g/L of the film after 120 min of reaction. The equilibrium data were analyzed using Langmuir and Freundlich models. The adsorption kinetics followed the mechanism of the pseudo-second-order equation for all metals. The metals regenerated from films with an efficiency greater than 95% using 0.1 M ethylene diamine tetra acetic acid (EDTA) and films were successfully reused for adsorption.

  18. Preparation and characterization of magnetic carboxylated nanodiamonds for vortex-assisted magnetic solid-phase extraction of ziram in food and water samples.

    Science.gov (United States)

    Yılmaz, Erkan; Soylak, Mustafa

    2016-09-01

    A simple and rapid vortex-assisted magnetic solid phase extraction (VA-MSPE) method for the separation and preconcentration of ziram (zinc dimethyldithiocarbamate), subsequent detection of the zinc in complex structure of ziram by flame atomic absorption spectrometry (AAS) has been developed. The ziram content was calculated by using stoichiometric relationship between the zinc and ziram. Magnetic carboxylated nanodiamonds (MCNDs) as solid-phase extraction adsorbent was prepared and characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry and scanning electron microscopy (SEM). These magnetic carboxylated nanodiamonds carrying the ziram could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Some important factors influencing the extraction efficiency of ziram such as pH of sample solution, amount of adsorbent, type and volume of eluent, extraction and desorption time and sample volume were studied and optimized. The total extraction and detection time was lower than 10min The preconcentration factor (PF), the precision (RSD, n=7), the limit of detection (LOD) and limit of quantification (LOQ) were 160, 7.0%, 5.3µgL(-1) and 17.5µgL(-1), respectively. The interference of various ions has been examined and the method has been applied for the determination of ziram in various waters, foodstuffs samples and synthetic mixtures.

  19. Diagnostic PCR: validation and sample preparation are two sides of the same coin

    DEFF Research Database (Denmark)

    Hoorfar, Jeffrey; Wolffs, Petra; Radstrøm, Peter

    2004-01-01

    Increased use of powerful PCR technology for the routine detection of pathogens has focused attention on the need for international validation and preparation of official non-commercial guidelines. Bacteria of epidemiological importance should be the prime focus, although a "validation infrastruc......Increased use of powerful PCR technology for the routine detection of pathogens has focused attention on the need for international validation and preparation of official non-commercial guidelines. Bacteria of epidemiological importance should be the prime focus, although a "validation...

  20. A Note on Sample Size and Solution Propriety for Confirmatory Factor Analytic Models

    Science.gov (United States)

    Jackson, Dennis L.; Voth, Jennifer; Frey, Marc P.

    2013-01-01

    Determining an appropriate sample size for use in latent variable modeling techniques has presented ongoing challenges to researchers. In particular, small sample sizes are known to present concerns over sampling error for the variances and covariances on which model estimation is based, as well as for fit indexes and convergence failures. The…

  1. U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Prabhakaran, Ramprashad [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Joshi, Vineet V. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Rhodes, Mark A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Schemer-Kohrn, Alan L. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Guzman, Anthony D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lavender, Curt A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-10-01

    The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

  2. U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Prabhakaran, Ramprashad [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Joshi, Vineet V. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Rhodes, Mark A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Schemer-Kohrn, Alan L. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Guzman, Anthony D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lavender, Curt A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-03-30

    The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

  3. Determination of protein carbonyls in plasma, cell extracts, tissue homogenates, isolated proteins: Focus on sample preparation and derivatization conditions.

    Science.gov (United States)

    Weber, Daniela; Davies, Michael J; Grune, Tilman

    2015-08-01

    Protein oxidation is involved in regulatory physiological events as well as in damage to tissues and is thought to play a key role in the pathophysiology of diseases and in the aging process. Protein-bound carbonyls represent a marker of global protein oxidation, as they are generated by multiple different reactive oxygen species in blood, tissues and cells. Sample preparation and stabilization are key steps in the accurate quantification of oxidation-related products and examination of physiological/pathological processes. This review therefore focuses on the sample preparation processes used in the most relevant methods to detect protein carbonyls after derivatization with 2,4-dinitrophenylhydrazine with an emphasis on measurement in plasma, cells, organ homogenates, isolated proteins and organelles. Sample preparation, derivatization conditions and protein handling are presented for the spectrophotometric and HPLC method as well as for immunoblotting and ELISA. An extensive overview covering these methods in previously published articles is given for researchers who plan to measure protein carbonyls in different samples.

  4. Optimization of crude enzyme preparation methods for analysis of glutamine synthetase activity in phytoplankton and field samples

    Institute of Scientific and Technical Information of China (English)

    WANG Yujue; WANG Dazhi; HONG Huasheng

    2009-01-01

    Glutamine synthetase (GS) is an important enzyme involved in nitrogen assimilation and metabolism in marine phytoplankton. However, little work has been done in situ due to the limitation of crude enzyme preparation methods. In this study, three enzyme preparation methods, high-speed centrifugation (HC, <10 000 g), ultracentrifugation (UC, 70 000 g), and ultrafiltration (UF) with 100 kμ, molecular weight cutoff, were compared using two diatom species (Asterionellopsis glacialis and Thalassiosira weissflogii), and two dinoflagellate species (Alexandrium catenella and Prorocentrum donghaiense) as experimental materials together with field samples collected from Xiamen Harbor, China. The results showed that HC is the best method to prepare crude enzymes for glutamine synthetase activity (GSA) in diatom species and diatom-dominant samples, while UF is the best method to extract GS from dinoflagellate species and dinoflagellate-dominant samples. For the HC method, the optimal centrifugal speed and time were 10 000 g and 35 min, respectively, and under these conditions, the highest GSA was obtained in all samples. This study indicates that both methods (HC and UF) overcome the limitation of centrifugal speed and could be applied to in situ GSA analysis, especially at sea.

  5. Study of sample preparation for quantitative analysis of amino acids in human sweat by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Delgado-Povedano, M M; Calderón-Santiago, M; Priego-Capote, F; Luque de Castro, M D

    2016-01-01

    The determination of physiological levels of amino acids is important to aid in the diagnosis and treatment of several diseases and nutritional status of individuals. Amino acids are frequently determined in biofluids such as blood (serum or plasma) and urine; however, there are less common biofluids with different concentration profiles of amino acids that could be of interest. One of these biofluids is sweat that can be obtained in a non-invasive manner and is characterized by low complex composition. The analysis of amino acids in human sweat requires the development of sample preparation strategies according to the sample matrix and small collected volume. The influence of sample preparation on the quantitative analysis of amino acids in sweat by LC-MS/MS has been assessed through a comparison between two strategies: dilution of sweat and centrifugal microsolid-phase extraction (c-μSPE). In both cases, several dilution factors were assayed for in-depth knowledge of the matrix effects, and the use of c-μSPE provided the best results in terms of accuracy. The behavior of the target analytes was a function of the dilution factor, thus providing a pattern for sample preparation that depended on the amino acid to be determined. The concentration of amino acids in sweat ranges between 6.20 ng mL(-1) (for homocysteine) and 259.77 µg mL(-1) (for serine) with precision, expressed as relative standard deviation, within 1.1-21.4%.

  6. Liquid crystalline solutions of cellulose in phosphoric acid for preparing cellulose yarns

    NARCIS (Netherlands)

    Boerstoel, H.

    2006-01-01

    The presen thesis describes a new process for manufacturing high tenacity and high modulus cellulose yarns. A new direct solvent for cellulose has been discovered, leading to liquid crystalline solutions. This new solvent, superphosphoric acid, rapidly dissolves cellulose. These liquid crystalline s

  7. PREPARATION AND CORROSION RESISTANCE OF NiP/TiO2 COMPOSITE FILM ON CARBON STEEL IN SULFURIC ACID SOLUTION

    Institute of Scientific and Technical Information of China (English)

    L.Z. Song; S.Z. Song; J. Zhao

    2006-01-01

    A NiP/TiO2 composite film on carbon steel was prepared by electroless plating and sol-gel composite process. An artificial neural network was applied to optimize the prepared condition of the composite film. Corrosion behavior of the NiP/TiO2 composite film was investigated by polarization resistance measurement, anode polarization, ESEM (environmental scanning electron microscopy)and EIS (electrochemical impedance spectroscopy) measurements. Results showed that the NiP/TiO2 composite film has a good corrosion resistance in 0.5mol/L H2SO4 solution. The element valence of the composite film was characterized by XPS (X-ray photoelectron spectroscopy) spectrum, and an anticorrosion mechanism of the composite film was discussed.

  8. PREPARATION OF Co50Ni50 ULTRAFINES BY CO-REDUCTION OF SOLUTION IN PRESENCE OF POLYMER

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    The reduction reaction of aqueous Co2+ -hydrazine, which cannot be conducted under the common condition, is carried out by using both of low-temperature heating and stirring. Metallic ultrafines are prepared by this method. In the presence of polyvinyl alcohol (PVA), it is absorbed on the surface of particles of the product and forms a structure of complex particle, which is favorable to the stability of the powder size distribution. Co50Ni50 magnetic alloy ultrafines with fcc-cubic system can also be prepared from Co2+ -Ni2 +hybrid solution by the same method in the presence of PVA. The effect of PVA amount on the particle size and the stability of Co50Ni50 alloy ultrafines are emphatically discussed.

  9. Impact of heating rate and solvent on Ni-based catalysts prepared by solution combustion method for syngas methanation

    Directory of Open Access Journals (Sweden)

    Zeng Yan

    2014-12-01

    Full Text Available Ni-Al2O3 catalysts prepared by solution combustion method for syngas methanation were enhanced by employing various heating rate and different solvent. The catalytic properties were tested in syngas methanation. The result indicates that both of heating rate and solvent remarkably affect Ni particle size, which is a key factor to the catalytic activity of Ni-Al2O3 catalysts for syngas methanation. Moreover, the relationship between Ni particle size and the production rate of methane per unit mass was correlated. The optimal Ni-Al2O3 catalyst prepared in ethanol at 2°C/min, achieves a maximum production rate of methane at the mean size of 20.8 nm.

  10. Stability of Melphalan in 0.9% Sodium Chloride Solutions Prepared in Polyvinyl Chloride Bags for Intravenous Injection.

    Science.gov (United States)

    Desmaris, Romain-Pacôme; Mercier, Lionel; Paci, Angelo

    2015-09-01

    Melphalan is an alkylating agent frequently used in an intravenous formulation to treat hematologic malignancies and solid tumors in both adults and children. According to the manufacturer, melphalan is stable in sterile 0.9% sodium chloride for 90 min at room temperature (RT). Several authors have studied the stability of different concentrations of melphalan; however, most were not adapted to the current manufacturing process applied in pharmaceutical centralized units. This study was conducted to determine the stability of melphalan in 0.9% sodium chloride solutions at concentrations used for intravenous injection in practice. Melphalan is commonly prepared in diluted solutions ranging from 2 to 4 mg/ml for the treatment of adult patients and at lower concentrations (down to 0.5 mg/ml) for pediatric use. Accordingly, these were the three concentrations chosen for this study. Melphalan concentrations were measured with high-performance thin-layer chromatography (HPTLC). At RT, admixtures prepared at 4 mg/ml were stable for up to 8 h without protection from light; however, at lower concentrations, such as 0.5 and 2 mg/ml, stability did not exceed 2 h. When refrigerated, melphalan was stable for 24 h at 2 mg/ml; however, at 0.5 and 4 mg/ml, the drug was not stable. Melphalan solutions present with limited stability at 0.5, 2, and 4 mg/ml and are not adapted for delayed administration in pharmaceutical centralized units. However, at 4 mg/ml and at RT, a stability of 8 h is very interesting in practice and allows sufficient time for preparation, pharmaceutical control, transport, and administration.

  11. Photoactive composite films prepared from mixtures of polystyrene microgel dispersions and poly(3-hexylthiophene) solutions.

    Science.gov (United States)

    Chen, Mu; Cui, Zhengxing; Edmondson, Steve; Hodson, Nigel; Zhou, Mi; Yan, Junfeng; O'Brien, Paul; Saunders, Brian R

    2015-11-14

    Whilst polystyrene microgels belong to the oldest family of microgel particles, their behaviours when deposited onto substrates or prepared as composites have received little attention. Because polystyrene microgels are solvent-swellable, and inherently colloidally stable, they are well suited to form composites with conjugated polymers. Here, we investigate the morphology and light absorption properties of spin coated composite films prepared from mixed dispersions of polystyrene microgels and poly(3-hexylthiophene) (P3HT) for the first time. We compare the morphologies of the composite films to spin coated microgel films. The films were studied using optical microscopy, SEM, AFM, wide-angle X-ray diffraction and UV-visible spectroscopy. The films contained flattened microgel particles with an aspect ratio of ∼10. Microgel islands containing hexagonally close packed particles were evident for both the pure microgel and microgel/P3HT composite films. The latter were electrically conducting. The composite film morphology was dependent on the microgel and P3HT concentration used for film preparation and a morphology phase diagram was constructed. The P3HT phase acted as an electrically conducting cement and increased the robustness of the films to solvent washing. The composite films were photoactive due to the P3HT component. The absorbance for the films was tuneable and increased linearly with both microgel and P3HT concentration. The results of the study should apply to other organic swellable microgel/conjugated polymer combinations and may lead to new colloidal composites for future optoelectronic applications.

  12. Preparation and Characterization of Activated Carbon from Coconut Shell – Doped Tio2 in Water Solution

    Directory of Open Access Journals (Sweden)

    Maulidiyah

    2015-12-01

    Full Text Available The objective of the study was to prepare the activated carbon material doped TiO2-P25 (P25in order to determine the interaction occured in the water medium. The method was to prepare the activated carbon from coconut shell which had been cleaned, pyrolyzed, sievedthen followed by physical activation using a thermal process. Preparation of P25 was to form structures of anatase crystals in the furnace at temperature of 500°C for 3 hours. Both materials were mixed using distilled water until sol-gel was formed. Results of characterization using SEM showed that there is interaction between the activated carbon and P25inserted in the pores of the carbon, while SEM-EDX showed the composition of carbon, titanium and oxide are 46.9%; 27.5% and 25.6%, respectively. Data from XRD showed the formation of peaks from P25 anatase crystals and the carbon. It was supported by data of Flourier Transform Infra Red (FTIR which showed the bonds of –OH; C-H; C=C; COand the O-Ti-O.

  13. Adsorption of Reactive Blue 171 from Aqueous Solution using Low Cost Activated Carbon Prepared from Agricultural Solid Waste: Albizia amara

    Directory of Open Access Journals (Sweden)

    K. Anitha

    2015-07-01

    Full Text Available The adsorption of Reactive Blue 171 (Reactive Dye from aqueous solution using activated carbon prepared from Albizia amara pod shell waste as an adsorbent have been carried out. The experimental adsorption data fitted reasonably well to Langmuir and Freundlich adsorption isotherms. Kinetic parameters as a function of Initial dye concentration have been calculated and the kinetic data were substituted in Pseudo First Order, Elovich and Pseudo Second order equations. A probable explanation is offered to account for the results of kinetic study. The thermodynamic parameter enthalpy change (∆H suggests the exothermic nature of absorption of Reactive Blue 171 onto activated Albizia amara pod shell waste carbon.

  14. Advances in preparation of modified activated carbon and its applications in the rem