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Sample records for detecting residual palladium

  1. A Colorimetric Chemodosimeter for Pd(II): A Method for Detecting Residual Palladium in Cross-Coupling Reactions

    Science.gov (United States)

    Houk, Ronald J. T.; Wallace, Karl J.; Hewage, Himali S.; Anslyn, Eric V.

    2008-01-01

    A colorimetric chemodosimeter (SQ1) for the detection of trace palladium salts in cross-coupling reactions mediated by palladium is described. Decolorization of SQ1 is affected by nucleophilic attack of ethanethiol in basic DMSO solutions. Thiol addition is determined to have an equilibrium constant (Keq) of 2.9 × 106 M-1, with a large entropic and modest enthalpic driving force. This unusual result is attributed to solvent effects arising from a strong coordinative interaction between DMSO and the parent squaraine. Palladium detection is achieved through thiol scavenging from the SQ1-ethanethiol complex leading to a color “turn-on” of the parent squaraine. It was found that untreated samples obtained directly from Suzuki couplings showed no response to the assay. However, treatment of the samples with aqueous nitric acid generates a uniform Pd(NO3)2 species, which gives an appropriate response. “Naked-eye” detection of Pd(NO3)2 was estimated to be as low as 0.5 ppm in solution, and instrument-based detection was tested as low as 100 ppb. The average error over the working range of the assay was determined to be 7%. PMID:19122841

  2. Palladium configuration dependence of hydrogen detection sensitivity based on graphene FET for breath analysis

    Science.gov (United States)

    Sakamoto, Yuri; Uemura, Kohei; Ikuta, Takashi; Maehashi, Kenzo

    2018-04-01

    We have succeeded in fabricating a hydrogen gas sensor based on palladium-modified graphene field-effect transistors (FETs). The negative-voltage shift in the transfer characteristics was observed with exposure to hydrogen gas, which was explained by the change in work function. The hydrogen concentration dependence of the voltage shift was investigated using graphene FETs with palladium deposited by three different evaporation processes. The results indicate that the hydrogen detection sensitivity of the palladium-modified graphene FETs is strongly dependent on the palladium configuration. Therefore, the palladium-modified graphene FET is a candidate for breath analysis.

  3. Detecting Airborne Mercury by Use of Palladium Chloride

    Science.gov (United States)

    Ryan, Margaret; Shevade, Abhijit; Kisor, Adam; Homer, Margie; Jewell, April; Manatt, Kenneth; Torres, Julia; Soler, Jessica; Taylor, Charles

    2009-01-01

    Palladium chloride films have been found to be useful as alternatives to the gold films heretofore used to detect airborne elemental mercury at concentrations of the order of parts per billion (ppb). Somewhat more specifically, when suitably prepared palladium chloride films are exposed to parts-per-billion or larger concentrations of airborne mercury, their electrical resistances change by amounts large enough to be easily measurable. Because airborne mercury adversely affects health, it is desirable to be able to detect it with high sensitivity, especially in enclosed environments in which there is a risk of leakage of mercury from lamps or other equipment. The detection of mercury by use of gold films involves the formation of gold/mercury amalgam. Gold films offer adequate sensitivity for detection of airborne mercury and could easily be integrated into an electronic-nose system designed to operate in the temperature range of 23 to 28 C. Unfortunately, in order to regenerate a gold-film mercury sensor, one must heat it to a temperature of 200 C for several minutes in clean flowing air. In preparation for an experiment to demonstrate the present sensor concept, palladium chloride was deposited from an aqueous solution onto sets of gold electrodes and sintered in air to form a film. Then while using the gold electrodes to measure the electrical resistance of the films, the films were exposed, at a temperature of 25 C, to humidified air containing mercury at various concentrations from 0 to 35 ppb (see figure). The results of this and other experiments have been interpreted as signifying that sensors of this type can detect mercury in room-temperature air at concentrations of at least 2.5 ppb and can readily be regenerated at temperatures <40 C.

  4. Palladium nanoparticles on InP for hydrogen detection

    Czech Academy of Sciences Publication Activity Database

    Černohorský, Ondřej; Žďánský, Karel; Zavadil, Jiří; Kacerovský, Pavel; Piksová, K.

    2011-01-01

    Roč. 6, č. 410 (2011), s. 4101-4104 ISSN 1931-7573 R&D Projects: GA AV ČR(CZ) KAN401220801; GA ČR GA102/09/1037 Institutional research plan: CEZ:AV0Z20670512 Keywords : palladium * indium phosphide Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 2.726, year: 2011

  5. Palladium nanoparticles on InP for hydrogen detection

    Directory of Open Access Journals (Sweden)

    Zdansky Karel

    2011-01-01

    Full Text Available Abstract Layers of palladium (Pd nanoparticles on indium phosphide (InP were prepared by electrophoretic deposition from the colloid solution of Pd nanoparticles. Layers prepared by an opposite polarity of deposition showed different physical and morphological properties. Particles in solution are separated and, after deposition onto the InP surface, they form small aggregates. The size of the aggregates is dependent on the time of deposition. If the aggregates are small, the layer has no lateral conductance. Forward and reverse I-V characteristics showed a high rectification ratio with a high Schottky barrier height. The response of the structure on the presence of hydrogen was monitored.

  6. Flexible palladium-based H2 sensor with fast response and low leakage detection by nanoimprint lithography.

    Science.gov (United States)

    Lim, Su Hui; Radha, Boya; Chan, Jie Yong; Saifullah, Mohammad S M; Kulkarni, Giridhar U; Ho, Ghim Wei

    2013-08-14

    Flexible palladium-based H2 sensors have a great potential in advanced sensing applications, as they offer advantages such as light weight, space conservation, and mechanical durability. Despite these advantages, the paucity of such sensors is due to the fact that they are difficult to fabricate while maintaining excellent sensing performance. Here, we demonstrate, using direct nanoimprint lithography of palladium, the fabrication of a flexible, durable, and fast responsive H2 sensor that is capable of detecting H2 gas concentration as low as 50 ppm. High resolution and high throughput patterning of palladium gratings over a 2 cm × 1 cm area on a rigid substrate was achieved by heat-treating nanoimprinted palladium benzyl mercaptide at 250 °C for 1 h. The flexible and robust H2 sensing device was fabricated by subsequent transfer nanoimprinting of these gratings into a polycarbonate film at its glass transition temperature. This technique produces flexible H2 sensors with improved durability, sensitivity, and response time in comparison to palladium thin films. At ambient pressure and temperature, the device showed a fast response time of 18 s at a H2 concentration of 3500 ppm. At 50 ppm concentration, the response time was found to be 57 s. The flexibility of the sensor does not appear to compromise its performance.

  7. Influence of residual catalyst on the properties of conjugated polyphenylenevinylene materials: Palladium nanoparticles and poor electrical performance

    DEFF Research Database (Denmark)

    Krebs, Frederik C; Nyberg, R.B.; Jørgensen, M.

    2004-01-01

    polymer material prepared by two different routes: the palladium route and the condensation route. The performance in a device application of the two polymer materials was, however, very different, and the palladium route was demonstrated to give poor films with low breakdown voltages and short circuits....

  8. Palladium modified porous silicon as multi-functional MALDI chip for serum peptide detection.

    Science.gov (United States)

    Li, Xiao; Chen, Xiaoming; Tan, Jie; Liang, Xiao; Wu, Jianmin

    2017-02-14

    Interest in using mesoporous materials for peptidomic research has increased recently. The present study reports a new type of matrix assisted laser desorption/ionization (MALDI) plate derived from electrochemically etched porous silicon (PSi) whose surface was modified with palladium nanoparticles (PdNPs). Owing to the well-tailored pore size and the molecular filtration effect of the PSi, peptides in serum samples can be selectively captured and enriched in the pore channel, thereby eliminating the interference from large proteins in subsequent MALDI-MS detection. On the other hand, the PdNPs with localized surface plasmon resonance (LSPR) effect can help to enhance the efficiency of energy absorption in the UV region. Meanwhile, the charge separation effect between the PSi semiconductor and PdNPs also can be applied to promote the accumulation of positive charges on PdNPs, resulting in an improvement in laser desorption/ionization (LDI) efficiency under positive linear detection mode. The interplay among these unique properties of PSi and PdNPs can synergistically increase the overall sensitivity in serum peptide detection. Using this technology, serum sample can be directly detected on the PSi-PdNPs chip without complicated pretreatment process. Therefore, a high fidelity serum peptide fingerprint can be acquired in a high throughput way. With the assistance of statistical analysis, colorectal cancer patients and healthy people can be accurately distinguished based on the serum peptide fingerprints.

  9. Detecting organic gunpowder residues from handgun use

    Science.gov (United States)

    MacCrehan, William A.; Ricketts, K. Michelle; Baltzersen, Richard A.; Rowe, Walter F.

    1999-02-01

    The gunpowder residues that remain after the use of handguns or improvised explosive devices pose a challenge for the forensic investigator. Can these residues be reliably linked to a specific gunpowder or ammunition? We investigated the possibility by recovering and measuring the composition of organic additives in smokeless powder and its post-firing residues. By determining gunpowder additives such as nitroglycerin, dinitrotoluene, ethyl- and methylcentralite, and diphenylamine, we hope to identify the type of gunpowder in the residues and perhaps to provide evidence of a match to a sample of unfired powder. The gunpowder additives were extracted using an automated technique, pressurized fluid extraction (PFE). The conditions for the quantitative extraction of the additives using neat and solvent-modified supercritical carbon dioxide were investigated. All of the major gunpowder additives can be determined with baseline resolution using capillary electrophoresis (CE) with a micellar agent and UV absorbance detection. A study of candidate internal standards for use in the CE method is also presented. The PFE/CE technique is used to evaluate a new residue sampling protocol--asking shooters to blow their noses. In addition, an initial investigation of the compositional differences among unfired and post-fired .22 handgun residues is presented.

  10. Residual generator for cardiovascular anomalies detection

    KAUST Repository

    Belkhatir, Zehor

    2014-06-01

    This paper discusses the possibility of using observer-based approaches for cardiovascular anomalies detection and isolation. We consider a lumped parameter model of the cardiovascular system that can be written in a form of nonlinear state-space representation. We show that residuals that are sensitive to variations in some cardiovascular parameters and to abnormal opening and closure of the valves, can be generated. Since the whole state is not easily available for measurement, we propose to associate the residual generator to a robust extended kalman filter. Numerical results performed on synthetic data are provided.

  11. Development of a SERS aptasensor for detection of medical residues

    DEFF Research Database (Denmark)

    Frøhling, Kasper Bayer

    Low levels of medical residues in environmental, industrial and domestic water systems is a growing concern. The biosensor industry is trying to accomodate the need of sensitive and specific sensor systems capable of ultra-low level detection of medical residues. In this PhD project a surface...... for sensitive and selective capture of medical residues....

  12. A micromachined calorimetric gas sensor: an application of electrodeposited nanostructured palladium for the detection of combustible gases.

    Science.gov (United States)

    Bartlett, Philip N; Guerin, Samuel

    2003-01-01

    Palladium films with regular nanoarchitectures were electrochemically deposited from the hexagonal (H1) lyotropic liquid crystalline phase of the nonionic surfactant octaethyleneglycol monohexadecyl ether (C16EO8) onto micromachined silicon hotplate structures. The H1-e Pd films were shown to have high surface areas (approximately 28 m2 g(-1)) and to act as effective and stable catalysts for the detection of methane in air on heating to 500 degrees C. The response of the H1-e Pd-coated planar pellistors was found to be linearly proportional to the concentration of methane between 0 and 2.5% in air with a detection limit below 0.125%. Our results show that the electrochemical deposition of nanostructured metal films offers a promising approach to the fabrication of micromachined calorimetric gas sensors for combustible gases.

  13. Palladium Nanoparticle Hydrogen Sensor

    Directory of Open Access Journals (Sweden)

    I. Pavlovsky

    2006-12-01

    Full Text Available An innovative hydrogen sensor based on palladium (Pd nanoparticle networks is described in the article. Made by Applied Nanotech Inc. sensor has a fast response time, in the range of seconds, which is increased at 80 °C due to higher hydrogen diffusion rates into the palladium lattice. The low detection limit of the sensor is 10 ppm of H2, and the high limit is 40,000 ppm. This is 100% of a lowest flammability level of hydrogen. This range of sensitivities complies with the requirements that one would expect for a reliable hydrogen sensor.

  14. Palladium Nanoparticles-Based Fluorescence Resonance Energy Transfer Aptasensor for Highly Sensitive Detection of Aflatoxin M₁ in Milk.

    Science.gov (United States)

    Li, Hui; Yang, Daibin; Li, Peiwu; Zhang, Qi; Zhang, Wen; Ding, Xiaoxia; Mao, Jin; Wu, Jing

    2017-10-13

    A highly sensitive aptasensor for aflatoxin M₁ (AFM₁) detection was constructed based on fluorescence resonance energy transfer (FRET) between 5-carboxyfluorescein (FAM) and palladium nanoparticles (PdNPs). PdNPs (33 nm) were synthesized through a seed-mediated growth method and exhibited broad and strong absorption in the whole ultraviolet-visible (UV-Vis) range. The strong coordination interaction between nitrogen functional groups of the AFM₁ aptamer and PdNPs brought FAM and PdNPs in close proximity, which resulted in the fluorescence quenching of FAM to a maximum extent of 95%. The non-specific fluorescence quenching caused by PdNPs towards fluorescein was negligible. After the introduction of AFM₁ into the FAM-AFM₁ aptamer-PdNPs FRET system, the AFM₁ aptamer preferentially combined with AFM₁ accompanied by conformational change, which greatly weakened the coordination interaction between the AFM₁ aptamer and PdNPs. Thus, fluorescence recovery of FAM was observed and a linear relationship between the fluorescence recovery and the concentration of AFM₁ was obtained in the range of 5-150 pg/mL in aqueous buffer with the detection limit of 1.5 pg/mL. AFM₁ detection was also realized in milk samples with a linear detection range from 6 pg/mL to 150 pg/mL. The highly sensitive FRET aptasensor with simple configuration shows promising prospect in detecting a variety of food contaminants.

  15. Synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel for electrochemical detection of dopamine

    Energy Technology Data Exchange (ETDEWEB)

    Li, Ruiyi; Yang, Tingting [School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China); Li, Zaijun, E-mail: zaijunli@jiangnan.edu.cn [School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China); Key Laboratory of Food Colloids and Biotechnology, Ministry of Education, Wuxi 214122 (China); Gu, Zhiguo; Wang, Guangli; Liu, Junkang [School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China)

    2017-02-15

    Integration of noble metal nanomaterials on graphene nanosheets potentially paves one way to improve their electronic, chemical and electrochemical properties. The study reported synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel composite (Pd@Au/N,S-MGA). The as-prepared composite offers a well-defined three-dimensional architecture with rich of mesopores. The Pd@Au nanoalloys were dispersed on the graphene framework networks and their active sites were fully exposed. The unique structure achieves to ultra high electron/ion conductivity, electrocatalytic activity and structural stability. The sensor based on the Pd@Au/N,S-MGA creates ultrasensitive electrochemical response towards dopamine due to significantly electrochemical synergy between Pd, Au and N,S-MGA. Its differential pulse voltammetric signal linearly increases with the increase of dopamine concentration in the range from 1.0 × 10{sup −9} M to 4.0 × 10{sup −5} M with the detection limit of 3.6 × 10{sup −10} M (S/N = 3). The analytical method provides the advantage of sensitivity, reproducibility, rapidity and long-term stability. It has been successfully applied in the detection of trace dopamine in biological samples. The study also opens a window on the electronic properties of graphene aerogel and metal nanomaterials as well their nanohybrids to meet needs of further applications as nanoelectronics in diagnosis, bioanalysis and catalysis. - Graphical abstract: We reported a new palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel. The sensor based on the nanohybrid exhibits ultrahigh sensitivity, reproducibility and stability to electrochemical detection of dopamine. - Highlights: • We reported Pd@A/nitrogen and sulphur-functionalized multiple graphene aerogel. • The nanohybrid offers unique three-dimensional architecture with rich of mesopores. • The architecture achieve to ultrahigh

  16. Synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel for electrochemical detection of dopamine

    International Nuclear Information System (INIS)

    Li, Ruiyi; Yang, Tingting; Li, Zaijun; Gu, Zhiguo; Wang, Guangli; Liu, Junkang

    2017-01-01

    Integration of noble metal nanomaterials on graphene nanosheets potentially paves one way to improve their electronic, chemical and electrochemical properties. The study reported synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel composite (Pd@Au/N,S-MGA). The as-prepared composite offers a well-defined three-dimensional architecture with rich of mesopores. The Pd@Au nanoalloys were dispersed on the graphene framework networks and their active sites were fully exposed. The unique structure achieves to ultra high electron/ion conductivity, electrocatalytic activity and structural stability. The sensor based on the Pd@Au/N,S-MGA creates ultrasensitive electrochemical response towards dopamine due to significantly electrochemical synergy between Pd, Au and N,S-MGA. Its differential pulse voltammetric signal linearly increases with the increase of dopamine concentration in the range from 1.0 × 10"−"9 M to 4.0 × 10"−"5 M with the detection limit of 3.6 × 10"−"1"0 M (S/N = 3). The analytical method provides the advantage of sensitivity, reproducibility, rapidity and long-term stability. It has been successfully applied in the detection of trace dopamine in biological samples. The study also opens a window on the electronic properties of graphene aerogel and metal nanomaterials as well their nanohybrids to meet needs of further applications as nanoelectronics in diagnosis, bioanalysis and catalysis. - Graphical abstract: We reported a new palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel. The sensor based on the nanohybrid exhibits ultrahigh sensitivity, reproducibility and stability to electrochemical detection of dopamine. - Highlights: • We reported Pd@A/nitrogen and sulphur-functionalized multiple graphene aerogel. • The nanohybrid offers unique three-dimensional architecture with rich of mesopores. • The architecture achieve to ultrahigh electron

  17. Residual generator for cardiovascular anomalies detection

    KAUST Repository

    Belkhatir, Zehor; Laleg-Kirati, Taous-Meriem; Tadjine, Mohamed

    2014-01-01

    This paper discusses the possibility of using observer-based approaches for cardiovascular anomalies detection and isolation. We consider a lumped parameter model of the cardiovascular system that can be written in a form of nonlinear state

  18. Detecting chlorinated hydrocarbon residues: Rachel Carson's villains.

    Science.gov (United States)

    Travis, Anthony S

    2012-07-01

    In 1962, Rachel Carson's Silent Spring drew the public's attention to the deleterious effects of chlorinated hydrocarbons employed as economic poisons in agriculture. However, she did not discuss how their residues could be routinely identified and quantified. In part, this was because the introduction of instruments for use in environmental analysis had only just begun, and she was probably unaware of their existence. The development of the instrumental methods began in industry, particularly at Dow and Shell, in the mid-1950s. Dow scientists, by combining mass spectrometry with gas chromatography, developed the most powerful technique, then and now, for the separation, quantitation and identification of chlorinated hydrocarbons. Shell scientists were no less innovative, particularly with the application of highly sensitive gas chromatography detectors to trace analysis. The first of these detectors, the electron capture detector, was invented by James Lovelock at the National Institute of Medical Research, North London, at the end of the 1950s. Around the same time, Dale Coulson in the USA developed his microcoulometric detector.

  19. Nanomolar electrochemical detection of caffeic acid in fortified wine samples based on gold/palladium nanoparticles decorated graphene flakes.

    Science.gov (United States)

    Thangavelu, Kokulnathan; Raja, Nehru; Chen, Shen-Ming; Liao, Wei-Cheng

    2017-09-01

    Amalgamation of noble metal nanomaterials on graphene flakes potentially paves one way to improve their physicochemical properties. This paper deals with the simultaneous electrochemical deposition of gold and palladium nanoparticles on graphene flakes (Au/PdNPs-GRF) for the sensitive determination of caffeic acid (CA). The physiochemical properties of the prepared Au/PdNPs-GRF was characterized by using numerous analytical techniques such as scanning electron microscopy, electron dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction, Raman spectroscopy and electrochemical impedance spectroscopy. The enhanced electrochemical determination of CA at Au/PdNPs deposition on GRF were studied by using cyclic voltammetry and differential pulse voltammetry. In results, Au/PdNPs-GRF electrode exhibited an excellent electrocatalytic activity towards CA with wide linear range and low limit of detection of 0.03-938.97µM and 6nM, respectively. Eventually, the Au/PdNPs-GRF was found as a selective and stable active material for the sensing of CA. In addition, the proposed sensor showed the adequate results in real sample analysis. Copyright © 2017 Elsevier Inc. All rights reserved.

  20. Detection of residues antibiotics in food using a microbiological method

    International Nuclear Information System (INIS)

    Ben Ali, Ahmed

    2007-01-01

    Antibiotics are effective therapeutic agents because of their property of selective bacterial toxicity which helps controlling infections. Animals, just like humans, can be treated with antibiotics. This use of antibiotics can lead to the development of resistance. Resistant strains may cause severe infections in humans and animals. In addition, antibiotic residues might represent a problem for human health. Our objective is to develop a microbiological method for the detection of antibiotic residues in poultry(muscle, liver,...). For this purpose, antibiotic sensitive bacteria and selective agar media were used. An inhibition growth zone surrounds each of the food samples containing antibiotic residues after a prescribed incubation time. (Author). 23 refs

  1. The importance of antibiotic residues presence detection in milk

    Directory of Open Access Journals (Sweden)

    Dubravka Samaržija

    2002-01-01

    Full Text Available Antibiotic residues are the most present inhibitory substances in milkhaving undesirable effect on human health, technological characteristics and the quality of milk and dairy products. In order to protect consumer's health and to ensure high quality milk production, European Union (EU regulation 2377/90 sets a maximum permitted levels for antibiotic residues in milk. Although the presence of antibiotic residues in milk can be due to animal diseases treatment, and in the case of milking animals, they are mostly present after mastitis treatment. The aim of this work is to stress the importance of the continuous control on antibiotic residues presence in milk, due to the role that milk and dairy products have in human nutrition. In this paper, different groups of antibiotics, mechanisms of theirs action, mistakes occurring in dairy products manufacture as well as the methods for theirs detection are described.

  2. Detection of antibiotic residues in food by Charm II test

    International Nuclear Information System (INIS)

    Addali, Mohamed

    2014-01-01

    Antibiotics are used in food to: -therapy and prophylaxis, -increase the productivity of the food producing animals. The presence of antimicrobial residues: -constitutes a potential human health hazard. has significant impact on international food trade. has implications on technological process in dairy industry. Detection of antibiotic residues is of great interest. It helps protect humans against the effects of such residues, the more it can support the participation of our country in international trade. Charm II test is one of the methods of detection of antimicrobial residues. The tests utilize microbial or antibody receptor assay technology. The sample is incubated with a binding agent (microbial cells with specific receptor sites or with specific antibodies attached) and a tracer (the radio-labeled version of the antibiotic to be detected). The amount of tracer on the binding agent is measured using a scintillation counter and is compared to a pre-determined cut-off or control point. If contaminating antibiotic is present, it will prevent the binding of the tracer by occupying the receptors on the binding agent. The less labeled tracer detected, the more contaminating antibiotic there is present in the sample. This work, carried out at the Radiochemical Laboratory of the National Centre of Nuclear Science and Technology, has two parts: 1/ The first is reserved to a literature review provides an overview on antibiotics and the charm II method. 2/ The second is devoted to the experimental study and presentation of results.

  3. Field Test Kit for Gun Residue Detection; TOPICAL

    International Nuclear Information System (INIS)

    WALKER, PAMELA K.; RODACY, PHILIP J.

    2002-01-01

    One of the major needs of the law enforcement field is a product that quickly, accurately, and inexpensively identifies whether a person has recently fired a gun--even if the suspect has attempted to wash the traces of gunpowder off. The Field Test Kit for Gunshot Residue Identification based on Sandia National Laboratories technology works with a wide variety of handguns and other weaponry using gunpowder. There are several organic chemicals in small arms propellants such as nitrocellulose, nitroglycerine, dinitrotoluene, and nitrites left behind after the firing of a gun that result from the incomplete combustion of the gunpowder. Sandia has developed a colorimetric shooter identification kit for in situ detection of gunshot residue (GSR) from a suspect. The test kit is the first of its kind and is small, inexpensive, and easily transported by individual law enforcement personnel requiring minimal training for effective use. It will provide immediate information identifying gunshot residue

  4. A new approach for the detection of ethylene using silica-supported palladium complexes.

    Science.gov (United States)

    Cabanillas-Galán, Patricia; Farmer, Linda; Hagan, Terence; Nieuwenhuyzen, Mark; James, Stuart L; Lagunas, M Cristina

    2008-10-06

    The coordination of olefins to square-planar Pd(II) and Pt(II) complexes containing 2,9-dimethylphenanthroline ( L1) often involves a change of color associated with a change of geometry at the metal center. In order to obtain suitable colorimetric detectors for ethylene gas, a series of new Pd(II) and Pt(II) compounds with a range of 2,9-disubstituted phenanthroline ligands [2,9-di- n-butyl-1,10-phenanthroline ( L2), 2,9-di- s-butyl-1,10-phenanthroline ( L3), 2,9-diphenyl-1,10-phenanthroline ( L4), and 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (bathocuproine, L5)] have been prepared and their reactivity toward ethylene investigated both in solution and after depositing the detector compounds on a variety of solid supports. The Pd(II) complex [PdCl 2( L2)] supported on silica undergoes a clear color change upon exposure to ethylene, while remaining stable toward air and water, and forms the basis for new simple colorimetric detectors with potential applications in ethylene pipe-leak detection and the monitoring of fruit ripening. Encouragingly, the detector is able to discriminate between fruit at different stages of ripening. The response of the detector to other volatiles was also examined, and specific color changes were also observed upon exposure to aromatic acetylenes. The crystal structures of four new derivatives, including the ethylene-Pt(II) complex [PtCl 2(C 2H 4)( L2)], are also described.

  5. Application of Stable Isotope in Detection of Veterinary Drug Residues

    International Nuclear Information System (INIS)

    Wang Wei; Liu Zhanfeng; Du Xiaoning

    2010-01-01

    In recent years, there has happened a series of significant food safety events worldwide, which lower down consumers' confidence in food safety, and they are taking increasing care about the sources of their foods. The safety problem of animal-origin foods has become a global topic for discussion. Therefore, it is a pressing task to establish a precise, sensitive and reliable method for analyzing veterinary drug residue. An introduction of the present status regarding veterinary drug residue analysis was made in the paper, and it briefly summarized the limit of detection (LOD) and quantification (LOQ) which could be reached in veterinary drug residue analysis by isotopic internal standard method domestically and abroad. The paper also made a review of the progress in applied research of stable isotope labeled compound in veterinary drug residue analysis of, such as, antibiotic medicines, furans and sulfonamides. The paper elucidated the great importance of the application of stable isotopes in the sane development of China's food safety system. (authors)

  6. Residual signal feature extraction for gearbox planetary stage fault detection

    DEFF Research Database (Denmark)

    Skrimpas, Georgios Alexandros; Ursin, Thomas; Sweeney, Christian Walsted

    2017-01-01

    Faults in planetary gears and related bearings, e.g. planet bearings and planet carrier bearings, pose inherent difficulties on their accurate and consistent detection associated mainly to the low energy in slow rotating stages and the operating complexity of planetary gearboxes. In this work......, identification of the expected spectral signature for proper residual signal calculation and filtering of any frequency component not related to the planetary stage. Two field cases of planet carrier bearing defect and planet wheel spalling are presented and discussed, showing the efficiency of the followed...

  7. Rapid surface enhanced Raman scattering detection method for chloramphenicol residues

    Science.gov (United States)

    Ji, Wei; Yao, Weirong

    2015-06-01

    Chloramphenicol (CAP) is a widely used amide alcohol antibiotics, which has been banned from using in food producing animals in many countries. In this study, surface enhanced Raman scattering (SERS) coupled with gold colloidal nanoparticles was used for the rapid analysis of CAP. Density functional theory (DFT) calculations were conducted with Gaussian 03 at the B3LYP level using the 3-21G(d) and 6-31G(d) basis sets to analyze the assignment of vibrations. Affirmatively, the theoretical Raman spectrum of CAP was in complete agreement with the experimental spectrum. They both exhibited three strong peaks characteristic of CAP at 1104 cm-1, 1344 cm-1, 1596 cm-1, which were used for rapid qualitative analysis of CAP residues in food samples. The use of SERS as a method for the measurements of CAP was explored by comparing use of different solvents, gold colloidal nanoparticles concentration and absorption time. The method of the detection limit was determined as 0.1 μg/mL using optimum conditions. The Raman peak at 1344 cm-1 was used as the index for quantitative analysis of CAP in food samples, with a linear correlation of R2 = 0.9802. Quantitative analysis of CAP residues in foods revealed that the SERS technique with gold colloidal nanoparticles was sensitive and of a good stability and linear correlation, and suited for rapid analysis of CAP residue in a variety of food samples.

  8. Laccases as palladium oxidases.

    Science.gov (United States)

    Mekmouche, Yasmina; Schneider, Ludovic; Rousselot-Pailley, Pierre; Faure, Bruno; Simaan, A Jalila; Bochot, Constance; Réglier, Marius; Tron, Thierry

    2015-02-01

    The first example of a coupled catalytic system involving an enzyme and a palladium(ii) catalyst competent for the aerobic oxidation of alcohol in mild conditions is described. In the absence of dioxygen, the fungal laccase LAC3 is reduced by a palladium(0) species as evidenced by the UV/VIS and ESR spectra of the enzyme. During the oxidation of veratryl alcohol performed in water, at room temperature and atmospheric pressure, LAC3 regenerates the palladium catalyst, is reduced and catalyzes the four-electron reduction of dioxygen into water with no loss of enzyme activity. The association of a laccase with a water-soluble palladium complex results in a 7-fold increase in the catalytic efficiency of the complex. This is the first step in the design of a family of renewable palladium catalysts for aerobic oxidation.

  9. On the fractional systems fault detection: a comparison between fractional and rational residual sensitivity

    International Nuclear Information System (INIS)

    Aoun, M.; Aribi, A.; Najar, S.; Abdelkrim, M.N.

    2011-01-01

    This paper shows the interest of extending the dynamic parity space fault detection method for fractional systems. Accordingly, a comparison between fractional and rational residual generators using the later method is presented. An analysis of fractional and rational residuals sensitivity shows the merits of the fractional residual generators. A numerical example illustrating the advantage of using fractional residual generators for fractional systems diagnosis is given.

  10. A Design of Finite Memory Residual Generation Filter for Sensor Fault Detection

    Directory of Open Access Journals (Sweden)

    Kim Pyung Soo

    2017-04-01

    Full Text Available In the current paper, a residual generation filter with finite memory structure is proposed for sensor fault detection. The proposed finite memory residual generation filter provides the residual by real-time filtering of fault vector using only the most recent finite measurements and inputs on the window. It is shown that the residual given by the proposed residual generation filter provides the exact fault for noisefree systems. The proposed residual generation filter is specified to the digital filter structure for the amenability to hardware implementation. Finally, to illustrate the capability of the proposed residual generation filter, extensive simulations are performed for the discretized DC motor system with two types of sensor faults, incipient soft bias-type fault and abrupt bias-type fault. In particular, according to diverse noise levels and windows lengths, meaningful simulation results are given for the abrupt bias-type fault.

  11. Microbial screening methods for detection of antibiotic residues in slaughter animals

    NARCIS (Netherlands)

    Pikkemaat, M.G.

    2009-01-01

    Monitoring of food products from animal origin for the presence of antimicrobial residues is preferably done using microbial screening methods because of their high cost-effectiveness. Traditionally applied methods fail to detect the maximum residue limits which were established when EU Council

  12. Functionalized Palladium Nanoparticles for Hydrogen Peroxide Biosensor

    Directory of Open Access Journals (Sweden)

    H. Baccar

    2011-01-01

    Full Text Available We present a comparison between two biosensors for hydrogen peroxide (H2O2 detection. The first biosensor was developed by the immobilization of Horseradish Peroxidase (HRP enzyme on thiol-modified gold electrode. The second biosensor was developed by the immobilization of cysteamine functionalizing palladium nanoparticles on modified gold surface. The amino groups can be activated with glutaraldehyde for horseradish peroxidase immobilization. The detection of hydrogen peroxide was successfully observed in PBS for both biosensors using the cyclic voltammetry and the chronoamperometry techniques. The results show that the limit detection depends on the large surface-to-volume ratio attained with palladium nanoparticles. The second biosensor presents a better detection limit of 7.5 μM in comparison with the first one which is equal to 75 μM.

  13. Matrix-Matching as an Improvement Strategy for the Detection of Pesticide Residues.

    Science.gov (United States)

    Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

    2016-05-01

    More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent-matched and matrix-matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix-matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel. © 2016 Institute of Food Technologists®

  14. A Design of Portable Pesticide Residue Detection System Based on the Enzyme Electrode

    Directory of Open Access Journals (Sweden)

    Xia SUN

    2013-03-01

    Full Text Available In this paper, a portable detection system was designed based on amperometric acetylcholinesterase biosensor for rapidly detecting pesticide residues in fruits and vegetables. There were potentiostat, three electrode system, differential amplification circuit and double integral analog to digital (A/D circuit modules in this system. The measurement principle of this system was depended on the weak current from enzyme catalyzing substrate in acetylcholinesterase biosensor for detecting pesticide residues. The weak current generated by the enzyme biosensor was changed into 0-5 V standard voltage signal by this system as an output signal. The proposed system was investigated with eight kinds of standard pesticide of different concentrations, the results showed that the detection limits were all lower than 10 ng/kg. Thus, a new effective home-made system of detecting pesticide residues with portable, easy-to-use, fast response was developed. The pesticide residues rapid detection system can collect the weak current signal generated by electrochemical reaction and on-site detect the concentration of pesticide residues in real fruits and vegetables samples.

  15. Optimization of immunochemistry for sensing techniques to detect pesticide residues in water

    DEFF Research Database (Denmark)

    Uthuppu, Basil; Kostesha, Natalie; Jakobsen, Mogens Havsteen

    2011-01-01

    We are working on the development of a real-time electrochemical sensor based on an immunoassay detection system to detect and quantify the presence of pesticide residues in ground water. Highly selective and sensitive immuno-reactions are being investigated to be optimized in order to bring them...

  16. Receptor-based screening assays for the detection of antibiotics residues - A review.

    Science.gov (United States)

    Ahmed, Saeed; Ning, Jianan; Cheng, Guyue; Ahmad, Ijaz; Li, Jun; Mingyue, Liu; Qu, Wei; Iqbal, Mujahid; Shabbir, M A B; Yuan, Zonghui

    2017-05-01

    Consumer and regulatory agencies have a high concern to antibiotic residues in food producing animals, so appropriate screening assays of fast, sensitive, low cost, and easy sample preparation for the identification of these residues are essential for the food-safety insurance. Great efforts in the development of a high-throughput antibiotic screening assay have been made in recent years. Concerning the screening of antibiotic residue, this review elaborate an overview on the availability, advancement and applicability of antibiotic receptor based screening assays for the safety assessment of antibiotics usage (i.e. radio receptor assay, enzyme labeling assays, colloidal gold receptor assay, enzyme colorimetry assay and biosensor assay). This manuscript also tries to shed a light on the selection, preparation and future perspective of receptor protein for antibiotic residue detection. These assays have been introduced for the screening of numerous food samples. Receptor based screening technology for antibiotic detection has high accuracy. It has been concluded that at the same time, it can detect a class of drugs for certain receptor, and realize the multi-residue detection. These assays offer fast, easy and precise detection of antibiotics. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Development of immunoassays for detecting clothianidin residue in agricultural products.

    Science.gov (United States)

    Li, Ming; Sheng, Enze; Cong, Lujing; Wang, Minghua

    2013-04-17

    Two enzyme-linked immunosorbent assays (ELISAs) based on polyclonal antibodies (PcAbs) for clothianidin are described: colorimetric detection format (ELISA) and pattern of chemiluminescent assay (CLEIA). Clothianidin hapten was synthesized and conjugated to bovine serum albumin (BSA) and ovalbumin (OVA) to produce immunogen and coating antigen. Anticlothianidin PcAbs were obtained from immunized New Zealand white rabbits. Under optimal conditions, the half-maximal inhibition concentration (IC₅₀) and the limit of detection (LOD, IC₂₀) of clothianidin were 0.046 and 0.0028 mg/L for the ELISA and 0.015 and 0.0014 mg/L for the CLEIA, respectively. There were no obvious cross-reactivities of the antibodies with its analogues except for dinotefuran. Recoveries of 76.4-116.4% for the immunoassays were achieved from spiked samples. The results of immunoassays for the spiked and authentic samples were largely consistent with gas chromatography. Therefore, the proposed immunoassays would be convenient and satisfactory analytical methods for the monitoring of clothianidin in agricultural products.

  18. Pesticide residues in grain from Kazakhstan and potential health risks associated with exposure to detected pesticides.

    Science.gov (United States)

    Lozowicka, B; Kaczynski, P; Paritova, Capital A Cyrillic Е; Kuzembekova, G B; Abzhalieva, A B; Sarsembayeva, N B; Alihan, K

    2014-02-01

    This paper presents the first study of pesticide residue results in grain from Kazakhstan. A total of 80 samples: barley, oat, rye, and wheat were collected and tested in the accredited laboratory. Among 180 pesticides, 10 active substances were detected. Banned pesticides, such as DDTs, γ-HCH, aldrin and diazinon were found in cereal grain. Chlorpyrifos methyl and pirimiphos methyl were the most frequently detected residues. No residues were found in 77.5% of the samples, 13.75% contained pesticide residues at or below MRLs, and 8.75% above MRLs. The greatest percentage of samples with residues (29%) was noted for wheat, and the lowest for rye (20%). Obtained data were used to estimate potential health risks associated with exposure to these pesticides. The highest estimated daily intakes (EDIs) were as follows: 789% of the ADI for aldrin (wheat) and 49.8% of the ADI for pirimiphos methyl (wheat and rye). The acute risk from aldrin and tebuconazole in wheat was 315.9% and 98.7% ARfD, respectively. The results show that despite the highest EDIs of pesticide residues in cereals, the current situation could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring of pesticide residues in grain is recommended. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Improvement of the Raman detection system for pesticide residues on/in fruits and vegetables

    Science.gov (United States)

    Li, Yan; Peng, Yankun; Zhai, Chen; Chao, Kuanglin; Qin, Jianwei

    2017-05-01

    Pesticide residue is one of the major challenges to fruits safety, while the traditional detection methods of pesticide residue on fruits and vegetables can't afford the demand of rapid detection in actual production because of timeconsuming. Thus rapid identification and detection methods for pesticide residue are urgently needed at present. While most Raman detection systems in the market are spot detection systems, which limits the range of application. In the study, our lab develops a Raman detection system to achieve area-scan thorough the self-developed spot detection Raman system with a control software and two devices. In the system, the scanning area is composed of many scanning spots, which means every spot needs to be detected and more time will be taken than area-scan Raman system. But lower detection limit will be achieved in this method. And some detection device is needed towards fruits and vegetables in different shape. Two detection devices are developed to detect spherical fruits and leaf vegetables. During the detection, the device will make spherical fruit rotate along its axis of symmetry, and leaf vegetables will be pressed in the test surface smoothly. The detection probe will be set to keep a proper distance to the surface of fruits and vegetables. It should make sure the laser shins on the surface of spherical fruit vertically. And two software are used to detect spherical fruits and leaf vegetables will be integrated to one, which make the operator easier to switch. Accordingly two detection devices for spherical fruits and leaf vegetables will also be portable devices to make it easier to change. In the study, a new way is developed to achieve area-scan result by spot-scan Raman detection system.

  20. Quantum Dots Applied to Methodology on Detection of Pesticide and Veterinary Drug Residues.

    Science.gov (United States)

    Zhou, Jia-Wei; Zou, Xue-Mei; Song, Shang-Hong; Chen, Guan-Hua

    2018-02-14

    The pesticide and veterinary drug residues brought by large-scale agricultural production have become one of the issues in the fields of food safety and environmental ecological security. It is necessary to develop the rapid, sensitive, qualitative and quantitative methodology for the detection of pesticide and veterinary drug residues. As one of the achievements of nanoscience, quantum dots (QDs) have been widely used in the detection of pesticide and veterinary drug residues. In these methodology studies, the used QD-signal styles include fluorescence, chemiluminescence, electrochemical luminescence, photoelectrochemistry, etc. QDs can also be assembled into sensors with different materials, such as QD-enzyme, QD-antibody, QD-aptamer, and QD-molecularly imprinted polymer sensors, etc. Plenty of study achievements in the field of detection of pesticide and veterinary drug residues have been obtained from the different combinations among these signals and sensors. They are summarized in this paper to provide a reference for the QD application in the detection of pesticide and veterinary drug residues.

  1. MONTANA PALLADIUM RESEARCH INITIATIVE

    Energy Technology Data Exchange (ETDEWEB)

    Peters, John; McCloskey, Jay; Douglas, Trevor; Young, Mark; Snyder, Stuart; Gurney, Brian

    2012-05-09

    Project Objective: The overarching objective of the Montana Palladium Research Initiative is to perform scientific research on the properties and uses of palladium in the context of the U.S. Department of Energy's Hydrogen, Fuel Cells and Infrastructure Technologies Program. The purpose of the research will be to explore possible palladium as an alternative to platinum in hydrogen-economy applications. To achieve this objective, the Initiatives activities will focus on several cutting-edge research approaches across a range of disciplines, including metallurgy, biomimetics, instrumentation development, and systems analysis. Background: Platinum-group elements (PGEs) play significant roles in processing hydrogen, an element that shows high potential to address this need in the U.S. and the world for inexpensive, reliable, clean energy. Platinum, however, is a very expensive component of current and planned systems, so less-expensive alternatives that have similar physical properties are being sought. To this end, several tasks have been defined under the rubric of the Montana Palladium Research Iniative. This broad swath of activities will allow progress on several fronts. The membrane-related activities of Task 1 employs state-of-the-art and leading-edge technologies to develop new, ceramic-substrate metallic membranes for the production of high-purity hydrogen, and develop techniques for the production of thin, defect-free platinum group element catalytic membranes for energy production and pollution control. The biomimetic work in Task 2 explores the use of substrate-attached hydrogen-producing enzymes and the encapsulation of palladium in virion-based protein coats to determine their utility for distributed hydrogen production. Task 3 work involves developing laser-induced breakdown spectroscopy (LIBS) as a real-time, in situ diagnostic technique to characterize PGEs nanoparticles for process monitoring and control. The systems engineering work in task 4

  2. Migration behavior of palladium in UO2, (3)

    International Nuclear Information System (INIS)

    Yoneyama, Mitsuru; Sato, Seichi; Ohashi, Hiroshi; Ogawa, Toru; Ito, Akinori; Fukuda, Kousaku.

    1992-08-01

    Palladium (Pd) is easily released from UO 2 kernels in HTGR coated fuel particles, and reacts with SiC coating layer. In addition, Pd is one of metallic fission products in irradiation UO 2 , which constitutes in dissoluble residue in reprocessing of LWR fuels. In the present investigation, the migration of palladium in UO 2 was examined by heating diffusion pairs sandwiched Pd foil between UO 2 wafers at 1300 ∼ 1800degC. Experiments were also carried out on affinity of Pd to UP 2 and a formation of U-Pd alloy. Pd was found mainly in the pores of UO 2 . The maximum depth intruded by Pd in fairly large amount was more than 100 μm for UO 2 with 90%TD and 50μm for UO 2 with 95%TD, while the maximum length of open pores was 330 μm for UO 2 with 90%TD, and 50 m for that with 95%TD. Fused Pd wetted UO 2 very much. Pd intruded deeply into UO 2 , especially in the edge of Pd droplet. Furthermore, U was detected either in precipitates or the Pd source with α-Pd phase of U-Pd alloy containing Pd at about 10at%. This fact indicates that Pd highly reacts with UO 2 . From the above results, the transport of Pd in UO 2 was explained by the model of gaseous diffusion through pores in UO 2 , which is retarded by formation of U-Pd alloy. It is also indicated that UPd 3 forms even at the oxygen potential condition of O/U ratio, which is a little higher than 2.00 on the basis of thermodynamic calculation. (author)

  3. Detection of residual packets in cocaine body packers: low accuracy of abdominal radiography - a prospective study

    Energy Technology Data Exchange (ETDEWEB)

    Rousset, Pascal; Vadrot, Dominique; Revel, Marie-Pierre [Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Hotel Dieu, Department of Radiology, Paris (France); Universite Paris-Descartes, Paris (France); Chaillot, Pierre-Fleury [Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Hotel Dieu, Department of Radiology, Paris (France); Audureau, Etienne [Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Hotel Dieu, Department of Biostatistics and Epidemiology, Paris (France); Universite Paris-Descartes, Paris (France); Rey-Salmon, Caroline; Becour, Bertrand [Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Hotel Dieu, Department of Forensic, Paris (France); Fitton, Isabelle [Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Europeen Georges Pompidou, Department of Radiology, Paris (France)

    2013-08-15

    To evaluate the accuracy of abdominal radiography (AXR) for the detection of residual cocaine packets by comparison with computed tomography (CT). Over a 1-year period unenhanced CT was systematically performed in addition to AXR for pre-discharge evaluation of cocaine body packers. AXR and CT were interpreted independently by two radiologists blinded to clinical outcome. Patient and packet characteristics were compared between the groups with residual portage and complete decontamination. Among 138 body packers studied, 14 (10 %) had one residual packet identified on pre-discharge CT. On AXR, at least one reader failed to detect the residual packet in 10 (70 %) of these 14 body packers. The sensitivity and specificity of AXR were 28.6 % (95 % CI: 8.4-58.1) and 100.0 % (95 % CI: 97.0-100.0) for reader 1 and 35.7 % (95 % CI: 12.8-64.9) and 97.6 % (95 % CI: 93.1-99.5) for reader 2. There were no significant patient or packet characteristics predictive of residual portage or AXR false negativity. All positive CT results were confirmed by delayed expulsion or surgical findings, while negative results were confirmed by further surveillance. Given the poor performance of AXR, CT should be systematically performed to ensure safe hospital discharge of cocaine body packers. (orig.)

  4. Detection of residual packets in cocaine body packers: low accuracy of abdominal radiography - a prospective study

    International Nuclear Information System (INIS)

    Rousset, Pascal; Vadrot, Dominique; Revel, Marie-Pierre; Chaillot, Pierre-Fleury; Audureau, Etienne; Rey-Salmon, Caroline; Becour, Bertrand; Fitton, Isabelle

    2013-01-01

    To evaluate the accuracy of abdominal radiography (AXR) for the detection of residual cocaine packets by comparison with computed tomography (CT). Over a 1-year period unenhanced CT was systematically performed in addition to AXR for pre-discharge evaluation of cocaine body packers. AXR and CT were interpreted independently by two radiologists blinded to clinical outcome. Patient and packet characteristics were compared between the groups with residual portage and complete decontamination. Among 138 body packers studied, 14 (10 %) had one residual packet identified on pre-discharge CT. On AXR, at least one reader failed to detect the residual packet in 10 (70 %) of these 14 body packers. The sensitivity and specificity of AXR were 28.6 % (95 % CI: 8.4-58.1) and 100.0 % (95 % CI: 97.0-100.0) for reader 1 and 35.7 % (95 % CI: 12.8-64.9) and 97.6 % (95 % CI: 93.1-99.5) for reader 2. There were no significant patient or packet characteristics predictive of residual portage or AXR false negativity. All positive CT results were confirmed by delayed expulsion or surgical findings, while negative results were confirmed by further surveillance. Given the poor performance of AXR, CT should be systematically performed to ensure safe hospital discharge of cocaine body packers. (orig.)

  5. Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

    Science.gov (United States)

    El-Safty, Sherif A.; Shenashen, Mohamed A.; Sakai, Masaru; Elshehy, Emad; Halada, Kohmei

    2015-01-01

    Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobaltmetals. PMID:26709467

  6. Rapid Detection Technology for Pesticides Residues Based on Microelectrodes Impedance Immunosensor

    Directory of Open Access Journals (Sweden)

    Wen Ping Zhao

    2014-09-01

    Full Text Available Compared with conventional methods, electrochemical immunosensors have many advantages, such as low cost, high sensitivity, and rapid detection, and has certain prospects for realizing real-time-monitoring. In this paper, a design of portable pesticide residues detection instrument was presented based on an electrochemical impedance immunosensor. Firstly, we studied on an impedance immunosensor based on interdigitated array microelectrode (IDAM coupled with magnetic nanobeads-antibody conjugates (MNAC for the pesticide detection. Magnetic nanobeads (diameter 150 nm coated with anti-carbofuran antibodies were used for further amplification of the binding reaction between antibody and hapten (carbofuran. Secondly, in order to develop a portable pesticide residue apparatus, we designed the impedance detection electric circuit. Main work included designing and constructing of the system circuit, designing and debugging of the system software and so on. Thirdly, the apparatus was used for the standard pesticides solutions testing combined with immunosensor to test the reliability and stability. The pesticide added standard recovery was more than 70 % and the impedance test error was less than 5 %. The results showed that the proposed instrument had a good consistence compared with the traditional analytical methods. Thus, it would be a promising rapid detection instrument for pesticide residues in agricultural products.

  7. Highly sensitive and selective colorimetric detection of cartap residue in agricultural products.

    Science.gov (United States)

    Liu, Wei; Zhang, Daohong; Tang, Yafan; Wang, Yashan; Yan, Fei; Li, Zhonghong; Wang, Jianlong; Zhou, H Susan

    2012-11-15

    The residue of pesticide has posed a serious threat to human health. Fast, broad-spectrum detection methods are necessary for on-site screening of various types of pesticides. With citrate-coated Au nanoparticles (Au NPs) as colorimetric probes, a visual and spectrophotometric method for rapid assay of cartap, which is one of the most important pesticides in agriculture, is reported for the first time. Based on the color change of Au colloid solution from wine-red to blue resulting from the aggregation of Au NPs, cartap could be detected in the concentration range of 0.05-0.6 mg/kg with a low detection limit of 0.04 mg/kg, which is much lower than the strictest cartap safety requirement of 0.1 mg/kg. Due to the limited research on the rapid detection of cartap based on Au NPs, the performance of the present method was evaluated through aggregation kinetics, interference influence, and sample pretreatment. To further demonstrate the selectivity and applicability of the method, cartap detection is realized in cabbage and tea with excellent analyte concentration recovery. These results demonstrate that the present method provides an easy and effective way to analyze pesticide residue in common products, which is of benefit for the rapid risk evaluation and on-site screening of pesticide residue. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Detection of Carbendazim Residues with a Colorimetric Sensor Based on Gold Nanoparticles

    Science.gov (United States)

    Ma, Y.; Jiang, H.; Shen, C.; Hou, Ch.; Huo, D.; Wu, H.; Yang, M.

    2017-07-01

    Carbendazim is among the most popular benzimidazole bactericides that are widely used to boost food production, and its residue poses a great threat to human health and the environment. In this paper, we presented a colorimetric sensor based on gold nanoparticles (Au-NPs) for the detection of carbendazim residues. The Au-NPs were stabilized by citric acid synthesized by chloroauric acid and sodium citrate with a diameter of about 13 nm. Upon reaction with carbendazim, the sensor gave a clear color change that could be distinguished with the naked eye. Thus we elaborated a new method for rapid determination of this benzimidazole bactericide. After optimization of the detection conditions, the sensor showed a very good linear relationship with the carbendazim concentrations varying from 10 to 600 ppb with a detection limit down to 3.4 ppb (S/N = 3). These preliminary results demonstrate that the presented sensor is promising for fast carbendazim analysis.

  9. Highly sensitive rapid fluorescence detection of protein residues on surgical instruments

    International Nuclear Information System (INIS)

    Kovalev, Valeri I; Bartona, James S; Richardson, Patricia R; Jones, Anita C

    2006-01-01

    There is a risk of contamination of surgical instruments by infectious protein residues, in particular, prions which are the agents for Creutzfeldt-Jakob Disease in humans. They are exceptionally resistant to conventional sterilization, therefore it is important to detect their presence as contaminants so that alternative cleaning procedures can be applied. We describe the development of an optimized detection system for fluorescently labelled protein, suitable for in-hospital use. We show that under optimum conditions the technique can detect ∼10 attomole/cm 2 with a scan speed of ∼3-10 cm 2 /s of the test instrument's surface. A theoretical analysis and experimental measurements will be discussed

  10. Automatic detection of photoresist residual layer in lithography using a neural classification approach

    KAUST Repository

    Gereige, Issam

    2012-09-01

    Photolithography is a fundamental process in the semiconductor industry and it is considered as the key element towards extreme nanoscale integration. In this technique, a polymer photo sensitive mask with the desired patterns is created on the substrate to be etched. Roughly speaking, the areas to be etched are not covered with polymer. Thus, no residual layer should remain on these areas in order to insure an optimal transfer of the patterns on the substrate. In this paper, we propose a nondestructive method based on a classification approach achieved by artificial neural network for automatic residual layer detection from an ellipsometric signature. Only the case of regular defect, i.e. homogenous residual layer, will be considered. The limitation of the method will be discussed. Then, an experimental result on a 400 nm period grating manufactured with nanoimprint lithography is analyzed with our method. © 2012 Elsevier B.V. All rights reserved.

  11. Detection of chloramphenicol residue in bovine meat using Liquid Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Widiastuti R

    2014-03-01

    Full Text Available Chloramphenicol (CAP is a broad spectrum antibiotic that has been banned in many countries due to its serius side effect to human. Detection of CAP residue in food has been determined to a minimum required performance limit (MRPL of 0.3 ng/g. The purpose of this research was to conduct the analysis of CAP residue in bovine meat by using LCMS and to study the presence of CAP residue in marketed bovine meat samples. LC separation was done on a Shimpack column C18 with ammonium acetate 10 mM/water as mobile phase, and ESI-MS analysis in negative ion mode. The coefficient of determination, R2 = 0.9981 at concentration of 0.125, 0.25, 0.63, 1,00 and 2.00 ng/g. Recovery at three fortification levels (0.25, 0.50 and 1.00 ng/g was in the range 77.5, 97.3 and 83.4%. The decision limit and the detection capability were 0.15 ng/g and 0.17 ng/g respectively. Analysis results of 52 marketed samples showed that CAP residue were detected in 9 samples in the concentration range of 0.14 to 2.70 ng/g and 6 among those positive samples were above the MRPL value. Therefore, it is important to increase the awareness and also to monitor regularly CAP residues in food originated from animal to provide safe food for the consumers.

  12. Automated detection of residual cells after sex-mismatched stem-cell transplantation – evidence for presence of disease-marker negative residual cells

    Directory of Open Access Journals (Sweden)

    Johannes Tilman

    2009-05-01

    Full Text Available Abstract Background A new chimerism analysis based on automated interphase fluorescence in situ hybridization (FISH evaluation was established to detect residual cells after allogene sex-mismatched bone marrow or blood stem-cell transplantation. Cells of 58 patients were characterized as disease-associated due to presence of a bcr/abl-gene-fusion or a trisomy 8 and/or a simultaneous hybridization of gonosome-specific centromeric probes. The automatic slide scanning platform Metafer with its module MetaCyte was used to analyse 3,000 cells per sample. Results Overall 454 assays of 58 patients were analyzed. 13 of 58 patients showed residual recipient cells at one stage of more than 4% and 12 of 58 showed residual recipient cells less than 4%, respectively. As to be expected, patients of the latter group were associated with a higher survival rate (48 vs. 34 month. In only two of seven patients with disease-marker positive residual cells between 0.1–1.3% a relapse was observed. Besides, disease-marker negative residual cells were found in two patients without relapse at a rate of 2.8% and 3.3%, respectively. Conclusion The definite origin and meaning of disease-marker negative residual cells is still unclear. Overall, with the presented automatic chimerism analysis of interphase FISH slides, a sensitive method for detection of disease-marker positive residual cells is on hand.

  13. Palladium nanoparticle anchored polyphosphazene nanotubes ...

    Indian Academy of Sciences (India)

    607–610. c Indian Academy of Sciences. Palladium ... 2Department of Chemistry, APA College of Arts and Culture, Palani, Tamil Nadu 624 601, India. 3Department of .... K Dinakaran acknowledges the financial support from. Department of ...

  14. Detection of metal residues on bone using SEM-EDS. Part I: Blunt force injury.

    Science.gov (United States)

    Pechníková, Markéta; Porta, Davide; Mazzarelli, Debora; Rizzi, Agostino; Drozdová, Eva; Gibelli, Daniele; Cattaneo, Cristina

    2012-11-30

    Previous studies have indicated that metal particles remain on bone after sharp force injury or gunshot and that their detection by scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDS) could greatly help in tool identification. However, the presence of metal particles on bone surfaces in the context of blunt force trauma has never been assessed experimentally. For this reason the present paper represents an experimental study of the behaviour of metal residues on bone following blunt force injury. Ten fresh sub-adult bovine metatarsal bones were manually cleaned of soft tissues. They were then struck by metal bars (copper, iron or aluminium) on the external surface of the mid-diaphysis. All blunt metal instruments used in this study left a sign in the form of single particles, a smear or a powder-like deposit on the bone surface. The residues of all three metal implements were detected on the bone surface, 0.3-10 mm from the fracture border. The presence of metal particles was confirmed in all samples struck with iron and copper and in two of six aluminium samples; no particles were detected on the negative control. Chemical composition of residues highly corresponded with the composition of applied bars. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  15. A C. elegans-based foam for rapid on-site detection of residual live virus.

    Energy Technology Data Exchange (ETDEWEB)

    Negrete, Oscar A.; Branda, Catherine; Hardesty, Jasper O. E. (Sandia National Laboratories, Albuquerque, NM); Tucker, Mark David (Sandia National Laboratories, Albuquerque, NM); Kaiser, Julia N. (Global Product Management, Hilden, Germany); Kozina, Carol L.; Chirica, Gabriela S.

    2012-02-01

    In the response to and recovery from a critical homeland security event involving deliberate or accidental release of biological agents, initial decontamination efforts are necessarily followed by tests for the presence of residual live virus or bacteria. Such 'clearance sampling' should be rapid and accurate, to inform decision makers as they take appropriate action to ensure the safety of the public and of operational personnel. However, the current protocol for clearance sampling is extremely time-intensive and costly, and requires significant amounts of laboratory space and capacity. Detection of residual live virus is particularly problematic and time-consuming, as it requires evaluation of replication potential within a eukaryotic host such as chicken embryos. The intention of this project was to develop a new method for clearance sampling, by leveraging Sandia's expertise in the biological and material sciences in order to create a C. elegans-based foam that could be applied directly to the entire contaminated area for quick and accurate detection of any and all residual live virus by means of a fluorescent signal. Such a novel technology for rapid, on-site detection of live virus would greatly interest the DHS, DoD, and EPA, and hold broad commercial potential, especially with regard to the transportation industry.

  16. Sensitization to palladium in Europe

    DEFF Research Database (Denmark)

    Muris, Joris; Goossens, An; Gonçalo, Margarida

    2015-01-01

    BACKGROUND: Recently, sodium tetrachloropalladate (Na2 PdCl4 ) was found to be a more sensitive palladium patch test allergen than palladium dichloride (PdCl2 ). OBJECTIVES: To determine the optimal test concentration of Na2 PdCl4 , to evaluate the prevalence of palladium sensitization with Na2 P...... patch test concentration. Sensitization to palladium is almost as prevalent as sensitization to nickel. The sex distribution is different between nickel-sensitized and palladium-sensitized patients, suggesting different sources of exposure.......Cl4 and PdCl2 , and to compare the results with nickel sensitization in a European multicentre study. MATERIALS AND METHODS: In addition to the European or national baseline series including NiSO4 ·6H2 0 5% pet., consecutive patients were tested with PdCl2 and Na2 PdCl4 2%, 3% and 4% pet. in eight...... European dermatology clinics. The age and sex distributions were also evaluated in patients sensitized to nickel and palladium. RESULTS: In total, 1651 patients were tested. Relative to 3% Na2 PdCl4 , 4% Na2 PdCl4 did not add any information. Two per cent Na2 PdCl4 resulted in more doubtful reactions...

  17. Porous palladium coated conducting polymer nanoparticles for ultrasensitive hydrogen sensors

    Science.gov (United States)

    Lee, Jun Seop; Kim, Sung Gun; Cho, Sunghun; Jang, Jyongsik

    2015-12-01

    Hydrogen, a clean-burning fuel, is of key importance to various industrial applications, including fuel cells and in the aerospace and automotive industries. However, hydrogen gas is odorless, colorless, and highly flammable; thus appropriate safety protocol implementation and monitoring are essential. Highly sensitive hydrogen leak detection and surveillance sensor systems are needed; additionally, the ability to maintain uniformity through repetitive hydrogen sensing is becoming increasingly important. In this report, we detail the fabrication of porous palladium coated conducting polymer (3-carboxylate polypyrrole) nanoparticles (Pd@CPPys) to detect hydrogen gas. The Pd@CPPys are produced by means of facile alkyl functionalization and chemical reduction of a pristine 3-carboxylate polypyrrole nanoparticle-contained palladium precursor (PdCl2) solution. The resulting Pd@CPPy-based sensor electrode exhibits ultrahigh sensitivity (0.1 ppm) and stability toward hydrogen gas at room temperature due to the palladium sensing layer.Hydrogen, a clean-burning fuel, is of key importance to various industrial applications, including fuel cells and in the aerospace and automotive industries. However, hydrogen gas is odorless, colorless, and highly flammable; thus appropriate safety protocol implementation and monitoring are essential. Highly sensitive hydrogen leak detection and surveillance sensor systems are needed; additionally, the ability to maintain uniformity through repetitive hydrogen sensing is becoming increasingly important. In this report, we detail the fabrication of porous palladium coated conducting polymer (3-carboxylate polypyrrole) nanoparticles (Pd@CPPys) to detect hydrogen gas. The Pd@CPPys are produced by means of facile alkyl functionalization and chemical reduction of a pristine 3-carboxylate polypyrrole nanoparticle-contained palladium precursor (PdCl2) solution. The resulting Pd@CPPy-based sensor electrode exhibits ultrahigh sensitivity (0.1 ppm

  18. Low-cost method for fabricating palladium and palladium-alloy thin films on porous supports

    Science.gov (United States)

    Lee, Tae H; Park, Chan Young; Lu, Yunxiang; Dorris, Stephen E; Balachandran, Uthamalingham

    2013-11-19

    A process for forming a palladium or palladium alloy membrane on a ceramic surface by forming a pre-colloid mixture comprising a powder palladium source, carrier fluid, dispersant and a pore former and a binder. Ultrasonically agitating the precolloid mixture and applying to a substrate with an ultrasonic nozzle and heat curing the coating form a palladium-based membrane.

  19. Zeranol: a review of the metabolism, toxicology, and analytical methods for detection of tissue residues

    International Nuclear Information System (INIS)

    Baldwin, R.S.; Williams, R.D.; Terry, M.K.

    1983-01-01

    Zeranol, an anabolic agent produced commercially for use in cattle and sheep intended for human consumption, is noncarcinogenic, nonteratogenic, and nonmutagenic. Toxicity testing (acute, subacute, and chronic) in several species by various routes of administration reveals an extremely low toxicity, the oral rat LD 50 exceeding 40 g/kg. Postmortem abnormalities of high-dose animals are attributed to the effects of the compound on the endocrine system. Both zeranol itself and zearalanone, the major Phase I metabolite in the seven species studied, are excreted in the feces and in the urine, either free or as sulfates/glucuronides. A minor urinary metabolite has been identified as taleranol, an epimer of zeranol. Both metabolites exhibit a very low order of toxicity (oral rat LD 50 exceeding 10 g/kg in both cases), and both exhibit less biological activity than the parent compound. The four types of analytical methods which have been employed for the specific detection and quantitation of residues of zeranol in edible tissues are: (1) gas chromatography (detection limit . 20 ppb), (2) high-performance liquid chromatography (detection limit . 5 ppb), (3) thin-layer chromatography (detection limit . 1-3 ppb), and (4) radioimmunoassay methods (detection limit to be published). The following residue levels were determined radiometrically in tissue samples taken 45 days after implantation of cattle with 36 mg tritiated zeranol: less than or equal to 2 ppb in liver, less than or equal to 1 ppb in kidney and fat, and less than or equal to 0.2 ppb in muscle and plasma. A no-effect level (NEL) of 0.225 mg/kg was determined as the highest oral dosage of zeranol which produced no estrogenic effects in female monkeys. Based on the NEL, a tolerance level for tissue residues of zeranol was calculated as 315 ppb

  20. Effect of the sequence data deluge on the performance of methods for detecting protein functional residues.

    Science.gov (United States)

    Garrido-Martín, Diego; Pazos, Florencio

    2018-02-27

    The exponential accumulation of new sequences in public databases is expected to improve the performance of all the approaches for predicting protein structural and functional features. Nevertheless, this was never assessed or quantified for some widely used methodologies, such as those aimed at detecting functional sites and functional subfamilies in protein multiple sequence alignments. Using raw protein sequences as only input, these approaches can detect fully conserved positions, as well as those with a family-dependent conservation pattern. Both types of residues are routinely used as predictors of functional sites and, consequently, understanding how the sequence content of the databases affects them is relevant and timely. In this work we evaluate how the growth and change with time in the content of sequence databases affect five sequence-based approaches for detecting functional sites and subfamilies. We do that by recreating historical versions of the multiple sequence alignments that would have been obtained in the past based on the database contents at different time points, covering a period of 20 years. Applying the methods to these historical alignments allows quantifying the temporal variation in their performance. Our results show that the number of families to which these methods can be applied sharply increases with time, while their ability to detect potentially functional residues remains almost constant. These results are informative for the methods' developers and final users, and may have implications in the design of new sequencing initiatives.

  1. Simple detection of residual enrofloxacin in meat products using microparticles and biochips.

    Science.gov (United States)

    Ha, Mi-Sun; Chung, Myung-Sub; Bae, Dong-Ho

    2016-05-01

    A simple and sensitive method for detecting enrofloxacin, a major veterinary fluoroquinolone, was developed. Monoclonal antibody specific for enrofloxacin was immobilised on a chip and fluorescent dye-labelled microparticles were covalently bound to the enrofloxacin molecules. Enrofloxacin in solution competes with the microparticle-immobilised enrofloxacin (enroMPs) to bind to the antibody on the chip. The presence of enrofloxacin was verified by detecting the fluorescence of enrofloxacin-bound microparticles. Under optimum conditions, a high dynamic range was achieved at enrofloxacin concentrations ranging from 1 to 1000 μg kg(-1). The limits of detection and quantification for standard solutions were 5 and 20 μg kg(-1) respectively, which are markedly lower than the maximum residue limit. Using simple extraction methods, recoveries from fortified beef, pork and chicken samples were 43.4-62.3%. This novel method also enabled approximate quantification of enrofloxacin concentration: the enroMP signal intensity decreased with increasing enrofloxacin concentration. Because of its sensitivity, specificity, simplicity and rapidity, the method described herein will facilitate the detection and approximate quantification of enrofloxacin residues in foods in a high-throughput manner.

  2. Quantum-Dot-Based Lateral Flow Immunoassay for Detection of Neonicotinoid Residues in Tea Leaves.

    Science.gov (United States)

    Wang, Shuangjie; Liu, Ying; Jiao, Shasha; Zhao, Ying; Guo, Yirong; Wang, Mengcen; Zhu, Guonian

    2017-11-22

    Neonicotinoid insecticides are commonly used for pest control on tea plantations as a result of their broad-spectrum activity. However, neonicotinoid residues released from tea leaves into tea infusions pose a dietary risk to consumers. Therefore, a rapid, sensitive, and reliable on-site detection method for neonicotinoids is needed. We developed a quantum-dot-based fluorescent lateral flow immunochromatographic strip (LFICS) combined with a broad-specific antibody for detection of typical neonicotinoids (imidacloprid, imidaclothiz, and clothianidin), with sensitivities [50% inhibitory concentration (IC 50 )] of 0.104-0.33 ng/mL and visual detection limits of 0.5-1 ng/mL. The strip assay could be completed in less than 30 min. Using the LFICS to analyze spiked tea samples (green tea, black tea, and oolong tea), the average recovery of the three neonicotinoids ranged between 71 and 111%, with the coefficient of variation below 12%. The results from the LFICS tests for field samples were consistent with results from ultraperformance liquid chromatography-tandem mass spectrometry. The newly developed strip is a useful tool for the on-site detection of neonicotinoid residues in tea.

  3. Detection of Clenbuterol Hydrochloride Residuals in Pork Liver Using a Customized Surface Plasmon Resonance Bioanalyzer

    Science.gov (United States)

    Hu, Jiandong; Chen, Ruipeng; Wang, Shun; Wang, Tingting; Zhao, Yuanyuan; Li, Jianwei; Hu, Xinran; Liang, Hao; Zhu, Juanhua; Sun, Xiaohui; Ma, Liuzheng; Jiang, Min

    2015-01-01

    A surface plasmon resonance (SPR) immunoassay with an immobilization of self-assembled molecular identification membrane for the detection of residual Clenbuterol Hydrochloride (CLB) in pork liver was systematically investigated and experimentally validated for its high performance. SPR immunoassay with a regular competitive inhibition assay cannot be directly verified to detect CLB residuals. In this study, the binding of Au film with mercaptopropionic acid was investigated using the known form of the strong S-Au covalent bonds formed by the chemical radical of the mercaptopropionic acid and the Au film. After that, the immunoglobulin IgG of swine (SwIgG-CLB) was bonded with the mercaptopropionic acid by covalent -CO-NH- amide bonding. The modified comprehensive analysis of how the membrane structure works was introduced together with the customized SPR bioanalyzer. In order to evaluate the performance of this biomembrane structure, the concentrations of CLB-contained solutions of 0 ng•mL-1, 10 ng•mL-1, 20 ng•mL-1, 33.3 ng•mL-1, and 40 ng•mL-1 were prepared by adding CLB reagents into the solutions of CLB antibody (Clenbuterol Hydrochloride Antibody, CLB-Ab), successively and then the response unit (RU) was measured individually. Using the data collected from the linear CCD array, the fitting curve was established with the R-Square value of 0.9929. Correspondingly, the recovery rate ranged from 88.48% to 103.21% was experimented and the limit of detection of CLB in 1.26 ng•mL-1 was obtained efficiently. It was concluded that the detection method associated with biomembrane properties is expected to contribute much to the determination of residual CLB in pork liver quantitatively by using the customized SPR bioanalyzer. PMID:25799327

  4. Detection of clenbuterol hydrochloride residuals in pork liver using a customized surface plasmon resonance bioanalyzer.

    Directory of Open Access Journals (Sweden)

    Jiandong Hu

    Full Text Available A surface plasmon resonance (SPR immunoassay with an immobilization of self-assembled molecular identification membrane for the detection of residual Clenbuterol Hydrochloride (CLB in pork liver was systematically investigated and experimentally validated for its high performance. SPR immunoassay with a regular competitive inhibition assay cannot be directly verified to detect CLB residuals. In this study, the binding of Au film with mercaptopropionic acid was investigated using the known form of the strong S-Au covalent bonds formed by the chemical radical of the mercaptopropionic acid and the Au film. After that, the immunoglobulin IgG of swine (SwIgG-CLB was bonded with the mercaptopropionic acid by covalent -CO-NH- amide bonding. The modified comprehensive analysis of how the membrane structure works was introduced together with the customized SPR bioanalyzer. In order to evaluate the performance of this biomembrane structure, the concentrations of CLB-contained solutions of 0 ng · mL(-1, 10 ng · mL(-1, 20 ng · mL(-1, 33.3 ng · mL(-1, and 40 ng · mL(-1 were prepared by adding CLB reagents into the solutions of CLB antibody (Clenbuterol Hydrochloride Antibody, CLB-Ab, successively and then the response unit (RU was measured individually. Using the data collected from the linear CCD array, the fitting curve was established with the R-Square value of 0.9929. Correspondingly, the recovery rate ranged from 88.48% to 103.21% was experimented and the limit of detection of CLB in 1.26 ng · mL(-1 was obtained efficiently. It was concluded that the detection method associated with biomembrane properties is expected to contribute much to the determination of residual CLB in pork liver quantitatively by using the customized SPR bioanalyzer.

  5. Detection and measurement of gamma-ray self-attenuation in plutonium residues

    International Nuclear Information System (INIS)

    Prettyman, T.H.; Foster, L.A.; Estep, R.J.

    1996-01-01

    A new method to correct for self-attenuation in gamma-ray assays of plutonium is presented. The underlying assumptions of the technique are based on a simple but accurate physical model of plutonium residues, particularly pyrochemical salts, in which it is assumed that the plutonium is divided into two portions, each of which can be treated separately from the standpoint of gamma-ray analysis: a portion that is in the form of plutonium metal shot; and a dilute portion that is mixed with the matrix. The performance of the technique is evaluated using assays of plutonium residues by tomographic gamma scanning at the Los Alamos Plutonium Facility. The ability of the method to detect saturation conditions is examined

  6. Highly sensitive rapid fluorescence detection of protein residues on surgical instruments

    Energy Technology Data Exchange (ETDEWEB)

    Kovalev, Valeri I [School of Engineering and Physical Sciences, Heriot-Watt University, Edinburgh EH14 4AS (United Kingdom); Bartona, James S [School of Engineering and Physical Sciences, Heriot-Watt University, Edinburgh EH14 4AS (United Kingdom); Richardson, Patricia R [School of Chemistry, University of Edinburgh, Edinburgh, EH9 3JJ (United Kingdom); Jones, Anita C [School of Chemistry, University of Edinburgh, Edinburgh, EH9 3JJ (United Kingdom)

    2006-07-15

    There is a risk of contamination of surgical instruments by infectious protein residues, in particular, prions which are the agents for Creutzfeldt-Jakob Disease in humans. They are exceptionally resistant to conventional sterilization, therefore it is important to detect their presence as contaminants so that alternative cleaning procedures can be applied. We describe the development of an optimized detection system for fluorescently labelled protein, suitable for in-hospital use. We show that under optimum conditions the technique can detect {approx}10 attomole/cm{sup 2} with a scan speed of {approx}3-10 cm{sup 2}/s of the test instrument's surface. A theoretical analysis and experimental measurements will be discussed.

  7. Palladium on Carbon-Catalyzed Suzuki-Miyaura Coupling Reaction Using an Efficient and Continuous Flow System

    Directory of Open Access Journals (Sweden)

    Tomohiro Hattori

    2015-01-01

    Full Text Available The continuous flow Suzuki-Miyaura reaction between various haloarenes and arylboronic acids was successfully achieved within only ca. 20 s during the single-pass through a cartridge filled with palladium on carbon (Pd/C. No palladium leaching was observed in the collected reaction solution by atomic absorption spectrometry (detection limit: 1 ppm.

  8. A Hypergraph and Arithmetic Residue-based Probabilistic Neural Network for classification in Intrusion Detection Systems.

    Science.gov (United States)

    Raman, M R Gauthama; Somu, Nivethitha; Kirthivasan, Kannan; Sriram, V S Shankar

    2017-08-01

    Over the past few decades, the design of an intelligent Intrusion Detection System (IDS) remains an open challenge to the research community. Continuous efforts by the researchers have resulted in the development of several learning models based on Artificial Neural Network (ANN) to improve the performance of the IDSs. However, there exists a tradeoff with respect to the stability of ANN architecture and the detection rate for less frequent attacks. This paper presents a novel approach based on Helly property of Hypergraph and Arithmetic Residue-based Probabilistic Neural Network (HG AR-PNN) to address the classification problem in IDS. The Helly property of Hypergraph was exploited for the identification of the optimal feature subset and the arithmetic residue of the optimal feature subset was used to train the PNN. The performance of HG AR-PNN was evaluated using KDD CUP 1999 intrusion dataset. Experimental results prove the dominance of HG AR-PNN classifier over the existing classifiers with respect to the stability and improved detection rate for less frequent attacks. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Gas chromatography with flame photometric detection of 31 organophosphorus pesticide residues in Alpinia oxyphylla dried fruits.

    Science.gov (United States)

    Zhao, Xiangsheng; Kong, Weijun; Wei, Jianhe; Yang, Meihua

    2014-11-01

    A simple, rapid and effective gas chromatography-flame photometric detection method was established for simultaneous multi-component determination of 31 organophosphorus pesticides (OPPs) residues in Alpinia oxyphylla, which is widely consumed as a traditional medicine and food in China. Sample preparation was completed in a single step without any clean-up procedure. All pesticides expressed good linear relationships between 0.004 and 1.0 μg/mL with correlation coefficients higher than 0.9973. The method gave satisfactory recoveries for most pesticides. The limits of detection varied from 1 to 10 ng/mL, and the limits of quantification (LOQs) were between 4 and 30 ng/mL. The proposed method was successfully applied to 55 commercial samples purchased from five different areas. Five pesticide residues were detected in four (7.27%) samples. The positive samples were confirmed by gas chromatography with tandem mass spectrometry (GC-MS/MS). Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. [Research on rapid and quantitative detection method for organophosphorus pesticide residue].

    Science.gov (United States)

    Sun, Yuan-Xin; Chen, Bing-Tai; Yi, Sen; Sun, Ming

    2014-05-01

    The methods of physical-chemical inspection is adopted in the traditional pesticide residue detection, which require a lot of pretreatment processes, are time-consuming and complicated. In the present study, the authors take chlorpyrifos applied widely in the present agricultural field as the research object and propose a rapid and quantitative detection method for organophosphorus pesticide residues. At first, according to the chemical characteristics of chlorpyrifos and comprehensive chromogenic effect of several colorimetric reagents and secondary pollution, the pretreatment of the scheme of chromogenic reaction of chlorpyrifos with resorcin in a weak alkaline environment was determined. Secondly, by analyzing Uv-Vis spectrum data of chlorpyrifos samples whose content were between 0. 5 and 400 mg kg-1, it was confirmed that the characteristic information after the color reaction mainly was concentrated among 360 approximately 400 nm. Thirdly, the full spectrum forecasting model was established based on the partial least squares, whose correlation coefficient of calibration was 0. 999 6, correlation coefficient of prediction reached 0. 995 6, standard deviation of calibration (RMSEC) was 2. 814 7 mg kg-1, and standard deviation of verification (RMSEP) was 8. 012 4 mg kg-1. Fourthly, the wavelengths whose center wavelength is 400 nm was extracted as characteristic region to build a forecasting model, whose correlation coefficient of calibration was 0. 999 6, correlation coefficient of prediction reached 0. 999 3, standard deviation of calibration (RMSEC) was 2. 566 7 mg kg-1 , standard deviation of verification (RMSEP) was 4. 886 6 mg kg-1, respectively. At last, by analyzing the near infrared spectrum data of chlorpyrifos samples with contents between 0. 5 and 16 mg kg-1, the authors found that although the characteristics of the chromogenic functional group are not obvious, the change of absorption peaks of resorcin itself in the neighborhood of 5 200 cm

  11. Computation of a Reference Model for Robust Fault Detection and Isolation Residual Generation

    Directory of Open Access Journals (Sweden)

    Emmanuel Mazars

    2008-01-01

    Full Text Available This paper considers matrix inequality procedures to address the robust fault detection and isolation (FDI problem for linear time-invariant systems subject to disturbances, faults, and polytopic or norm-bounded uncertainties. We propose a design procedure for an FDI filter that aims to minimize a weighted combination of the sensitivity of the residual signal to disturbances and modeling errors, and the deviation of the faults to residual dynamics from a fault to residual reference model, using the ℋ∞-norm as a measure. A key step in our procedure is the design of an optimal fault reference model. We show that the optimal design requires the solution of a quadratic matrix inequality (QMI optimization problem. Since the solution of the optimal problem is intractable, we propose a linearization technique to derive a numerically tractable suboptimal design procedure that requires the solution of a linear matrix inequality (LMI optimization. A jet engine example is employed to demonstrate the effectiveness of the proposed approach.

  12. Gas chromatographic determination with electron capture detection of residual ethylene oxide in intraocular lenses

    Energy Technology Data Exchange (ETDEWEB)

    Kikuchi, H.; Nakamura, A.; Tsuji, K.

    1988-01-01

    A sensitive method is described to determine trace quantities of ethylene oxide (EO) in EO-sterilized intraocular lenses (IOLs). An IOL is dipped in ethanol containing 0.25 ppm propylene oxide (PO) in a 4 mL vial, 2 drops of freshly distilled hydrobromic acid is added through a septum, and the mixture is warmed at 50/sup 0/C for 24 h. It is then neutralized by vigorous shaking with sodium bicarbonate, dehydrated with anhydrous sodium sulfate, and filtered. The filtrate is injected into a gas chromatograph with electron-capture detection, and the peak height ratio of ethylene bromohydrin/propylene bromohydrin is measured. EO residue is calculated from the calibration curve obtained through a similar procedure with the standard EO/PO solutions. The limit of determination is 0.04 ..mu..g/lens (ca 2.0 ppm). When EO residue levels were determined for IOLs sampled at 3 different aeration periods after stabilization, the authors found that 9 days of aeration was necessary to meet the US Food and Drug Administration proposed limit for EO residue in IOLs.

  13. Comparison of different agar diffusion methods for the detection of residues in the kidneys of pigs treated with antimicrobial drugs.

    Science.gov (United States)

    Korkeala, H; Sorvettula, O; Mäki-Petäys, O; Hirn, J

    1983-01-01

    Residue analyses of the kidneys of twenty-six pigs treated with various antimicrobial drugs 20 h before slaughter and of eleven untreated pigs were performed. The effects of storage temperature of the kidneys, and of sampling location, on the residue analysis were also studied. No method alone was sufficient for the detection of residues. Oxytetracycline residues could be detected at pH 6, dihydrostreptomycin residues at pH 8, and sulphonamide residues if trimethoprim was present in the medium. Chloramphenicol, penicillin G procaine, tylosin and lincomycin residues were not detectable with the methods used. The concentration of ampicillin decreased during the storage of samples at +4°C. Most methods also yielded zones of inhibition for the frozen kidneys from untreated pigs. It seems necessary to use agar media of two different pH values: the addition of trimethoprim to the medium is also needed. The use of fresh pig kidneys, and samples containing both kidney medulla and kidney cortex, is recommended in residue analysis. Copyright © 1983. Published by Elsevier Ltd.

  14. Determination of palladium content in palladium-alumina/palladium-silica/palladium-tin oxide catalyst for nuclear reactor applications

    International Nuclear Information System (INIS)

    Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.

    2012-01-01

    Alumina and silica act as support for finely divided palladium metal powder in synthesis of catalyst. These catalyst (Pd-Al 2 O 3 , Pd-SiO 2 and Pd-SnO 2 ) used in nuclear power reactor (moderator cover gas system) for the conversion of hydrogen. In Indian nuclear power programme these catalyst are regularly used in Kaiga 1 and 2 and Rajasthan atomic power plant 3 and 4. The performance of the catalyst, solely depends on the concentration of palladium, which is the active component in this catalyst composition. Therefore it is highly desirable to have rouged analytical methodology for the accurate estimation of palladium. Leaching of Pd from the bulk matrix is tedious due to the less reactive nature of Pd therefore complete solubilization of the matrix is carried out by fusion method

  15. Effects of Palladium Loading on the Response of Thick Film Flame-made ZnO Gas Sensor for Detection of Ethanol Vapor

    Directory of Open Access Journals (Sweden)

    Sukon Phanichphant

    2007-07-01

    Full Text Available ZnO nanoparticles doped with 0-5 mol% Pd were successfully produced in asingle step by flame spray pyrolysis (FSP using zinc naphthenate and palladium (IIacetylacetonate dissolved in toluene-acetonitrile (80:20 vol% as precursors. The effect ofPd loading on the ethanol gas sensing performance of the ZnO nanoparticles and thecrystalline sizes were investigated. The particle properties were analyzed by XRD, BET,AFM, SEM (EDS line scan mode, TEM, STEM, EDS, and CO-pulse chemisorptionmeasurements. A trend of an increase in specific surface area of samples and a decrease inthe dBET with increasing Pd concentrations was noted. ZnO nanoparticles were observed asparticles presenting clear spheroidal, hexagonal and rod-like morphologies. The sizes ofZnO spheroidal and hexagonal particle crystallites were in the 10-20 nm range. ZnOnanorods were in the range of 10-20 nm in width and 20-50 nm in length. The size of Pdnanoparticles increased and Pd-dispersion% decreased with increasing Pd concentrations.The sensing films were produced by mixing the particles into an organic paste composedof terpineol and ethyl cellulose as a vehicle binder. The paste was doctor-bladed ontoAl2O3 substrates interdigitated with Au electrodes. The film morphology was analyzed bySEM and EDS analyses. The gas sensing of ethanol (25-250 ppm was studied in dry air at400°C. The oxidation of ethanol on the sensing surface of the semiconductor wasconfirmed by MS. A well-dispersed of 1 mol%Pd/ZnO films showed the highest sensitivityand the fastest response time (within seconds.

  16. Formation, separation and detection of evaporation residues produced in complete fusion reactions

    CERN Document Server

    Sagaidak, R N

    2015-01-01

    Some aspects of formation, separation and detection of evaporation residues (ERs) produced in complete fusion reactions induced by accelerated heavy ions are considered. These reactions allow to obtain heavy neutron-deficient nuclei and to study their properties. The statistical model analysis of the production cross sections for these nuclei obtained in a wide range of their neutron numbers allows to trace the changes in their macroscopic properties such as fission barriers. The fusion probability of massive projectile and target nuclei is of interest. Empirical estimates of this value allow to verify the predictions of theoretical models for the optimal ways of synthesis of unknown nuclei. Some peculiarities in the separation and detection of ERs in experiments are briefly considered by the example of the Ra ERs produced in the 12 C+Pb reactions. The reliable cross sections for ERs produced in very asymmetric projectile-target combination, such as 12 C+Pb, are important for the em...

  17. Empirical likelihood based detection procedure for change point in mean residual life functions under random censorship.

    Science.gov (United States)

    Chen, Ying-Ju; Ning, Wei; Gupta, Arjun K

    2016-05-01

    The mean residual life (MRL) function is one of the basic parameters of interest in survival analysis that describes the expected remaining time of an individual after a certain age. The study of changes in the MRL function is practical and interesting because it may help us to identify some factors such as age and gender that may influence the remaining lifetimes of patients after receiving a certain surgery. In this paper, we propose a detection procedure based on the empirical likelihood for the changes in MRL functions with right censored data. Two real examples are also given: Veterans' administration lung cancer study and Stanford heart transplant to illustrate the detecting procedure. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  18. A multigene array for measurable residual disease detection in AML patients undergoing SCT

    Science.gov (United States)

    Goswami, M; McGowan, K S; Lu, K; Jain, N; Candia, J; Hensel, N F; Tang, J; Calvo, K R; Battiwalla, M; Barrett, A J; Hourigan, C S

    2015-01-01

    AML is a diagnosis encompassing a diverse group of myeloid malignancies. Heterogeneous genetic etiology, together with the potential for oligoclonality within the individual patient, have made the identification of a single high-sensitivity marker of disease burden challenging. We developed a multiple gene measurable residual disease (MG-MRD) RQ–PCR array for the high-sensitivity detection of AML, retrospectively tested on 74 patients who underwent allo-SCT at the NHLBI in the period 1994–2012. MG-MRD testing on peripheral blood samples prior to transplantation demonstrated excellent concordance with traditional BM-based evaluation and improved risk stratification for post-transplant relapse and OS outcomes. Pre-SCT assessment by MG-MRD predicted all clinical relapses occurring in the first 100 days after allo-SCT compared with 57% sensitivity using WT1 RQ–PCR alone. Nine patients who were negative for WT1 prior to transplantation were correctly reclassified into a high-risk MG-MRD-positive group, associated with 100% post-transplant mortality. This study provides proof of principle that a multiple gene approach may be superior to the use of WT1 expression alone for AML residual disease detection. PMID:25665046

  19. A deep 3D residual CNN for false-positive reduction in pulmonary nodule detection.

    Science.gov (United States)

    Jin, Hongsheng; Li, Zongyao; Tong, Ruofeng; Lin, Lanfen

    2018-05-01

    The automatic detection of pulmonary nodules using CT scans improves the efficiency of lung cancer diagnosis, and false-positive reduction plays a significant role in the detection. In this paper, we focus on the false-positive reduction task and propose an effective method for this task. We construct a deep 3D residual CNN (convolution neural network) to reduce false-positive nodules from candidate nodules. The proposed network is much deeper than the traditional 3D CNNs used in medical image processing. Specifically, in the network, we design a spatial pooling and cropping (SPC) layer to extract multilevel contextual information of CT data. Moreover, we employ an online hard sample selection strategy in the training process to make the network better fit hard samples (e.g., nodules with irregular shapes). Our method is evaluated on 888 CT scans from the dataset of the LUNA16 Challenge. The free-response receiver operating characteristic (FROC) curve shows that the proposed method achieves a high detection performance. Our experiments confirm that our method is robust and that the SPC layer helps increase the prediction accuracy. Additionally, the proposed method can easily be extended to other 3D object detection tasks in medical image processing. © 2018 American Association of Physicists in Medicine.

  20. Rapid detection of chlorpyrifos pesticide residue concentration in agro-product using Raman spectroscopy

    Science.gov (United States)

    Dhakal, Sagar; Peng, Yankun; Li, Yongyu; Chao, Kuanglin; Qin, Jianwei; Zhang, Leilei; Xu, Tianfeng

    2014-05-01

    Different chemicals are sprayed in fruits and vegetables before and after harvest for better yield and longer shelf-life of crops. Cases of pesticide poisoning to human health are regularly reported due to excessive application of such chemicals for greater economic benefit. Different analytical technologies exist to detect trace amount of pesticides in fruits and vegetables, but are expensive, sample destructive, and require longer processing time. This study explores the application of Raman spectroscopy for rapid and non-destructive detection of pesticide residue in agricultural products. Raman spectroscopy with laser module of 785 nm was used to collect Raman spectral information from the surface of Gala apples contaminated with different concentrations of commercially available organophosphorous (48% chlorpyrifos) pesticide. Apples within 15 days of harvest from same orchard were used in this study. The Raman spectral signal was processed by Savitzky-Golay (SG) filter for noise removal, Multiplicative Scatter Correction (MSC) for drift removal and finally polynomial fitting was used to eliminate the fluorescence background. The Raman spectral peak at 677 cm-1 was recognized as Raman fingerprint of chlorpyrifos. Presence of Raman peak at 677 cm-1 after fluorescence background removal was used to develop classification model (presence and absence of pesticide). The peak intensity was correlated with actual pesticide concentration obtained using Gas Chromatography and MLR prediction model was developed with correlation coefficient of calibration and validation of 0.86 and 0.81 respectively. Result shows that Raman spectroscopy is a promising tool for rapid, real-time and non-destructive detection of pesticide residue in agro-products.

  1. Analytical strategy for the detection of antibiotic residues in sheep and goat’s milk

    Energy Technology Data Exchange (ETDEWEB)

    Beltrán, M.C.; Althaus, R.L.; Molina, A.; Berruga, M.I.; Molina, M.P.

    2015-07-01

    The use of antibiotics to treat mastitis and other infectious diseases in dairy sheep and goats is a widespread practice nowadays that can, when not properly applied, result in the contamination of the milk supply. Spanish legislation establishes the control of the presence of antibiotic residues in sheep and goat’s milk using screening methods that detect, at least, beta-lactam drugs. Microbial inhibitor tests using Geobacillus stearothermophilus var. calidolactis and specific receptor-binding assays are most widely employed for this purpose. The detection rates of screening tests routinely used in Spain have been calculated considering the frequency of use of veterinary drugs commonly applied in ovine and caprine livestock to treat and prevent mastitis as well as the test sensitivity toward these substances at safety levels. In general, the use of a single test allows detecting 62.8-82.4% of the antibiotics employed. For sheep milk, the total detection range achieved with microbial tests was significantly higher than that reached with rapid receptor tests. However, no significant differences between the two types of methods were found when goat's milk was analysed. In both types of milk, the simultaneous use of two screening tests with a different analytical basis increases the total detection range significantly, reaching values ≥ 90% in some cases (81.5-90.1% for sheep and 84.7-92.6% for goats). However, the periodical use of screening tests able to detect quinolones, macrolides or aminoglycosides would be recommended to carry out more efficient screening and ensure the safety of milk and dairy products from sheep and goats. (Author)

  2. Analytical strategy for the detection of antibiotic residues in sheep and goat’s milk

    Directory of Open Access Journals (Sweden)

    M. Carmen Beltrán

    2015-03-01

    Full Text Available The use of antibiotics to treat mastitis and other infectious diseases in dairy sheep and goats is a widespread practice nowadays that can, when not properly applied, result in the contamination of the milk supply. Spanish legislation establishes the control of the presence of antibiotic residues in sheep and goat’s milk using screening methods that detect, at least, beta-lactam drugs. Microbial inhibitor tests using Geobacillus stearothermophilus var. calidolactis and specific receptor-binding assays are most widely employed for this purpose. The detection rates of screening tests routinely used in Spain have been calculated considering the frequency of use of veterinary drugs commonly applied in ovine and caprine livestock to treat and prevent mastitis as well as the test sensitivity toward these substances at safety levels. In general, the use of a single test allows detecting 62.8-82.4% of the antibiotics employed. For sheep milk, the total detection range achieved with microbial tests was significantly higher than that reached with rapid receptor tests. However, no significant differences between the two types of methods were found when goat’s milk was analysed. In both types of milk, the simultaneous use of two screening tests with a different analytical basis increases the total detection range significantly, reaching values ≥ 90% in some cases (81.5-90.1% for sheep and 84.7-92.6% for goats. However, the periodical use of screening tests able to detect quinolones, macrolides or aminoglycosides would be recommended to carry out more efficient screening and ensure the safety of milk and dairy products from sheep and goats.

  3. Analytical strategy for the detection of antibiotic residues in sheep and goat’s milk

    International Nuclear Information System (INIS)

    Beltrán, M.C.; Althaus, R.L.; Molina, A.; Berruga, M.I.; Molina, M.P.

    2015-01-01

    The use of antibiotics to treat mastitis and other infectious diseases in dairy sheep and goats is a widespread practice nowadays that can, when not properly applied, result in the contamination of the milk supply. Spanish legislation establishes the control of the presence of antibiotic residues in sheep and goat’s milk using screening methods that detect, at least, beta-lactam drugs. Microbial inhibitor tests using Geobacillus stearothermophilus var. calidolactis and specific receptor-binding assays are most widely employed for this purpose. The detection rates of screening tests routinely used in Spain have been calculated considering the frequency of use of veterinary drugs commonly applied in ovine and caprine livestock to treat and prevent mastitis as well as the test sensitivity toward these substances at safety levels. In general, the use of a single test allows detecting 62.8-82.4% of the antibiotics employed. For sheep milk, the total detection range achieved with microbial tests was significantly higher than that reached with rapid receptor tests. However, no significant differences between the two types of methods were found when goat's milk was analysed. In both types of milk, the simultaneous use of two screening tests with a different analytical basis increases the total detection range significantly, reaching values ≥ 90% in some cases (81.5-90.1% for sheep and 84.7-92.6% for goats). However, the periodical use of screening tests able to detect quinolones, macrolides or aminoglycosides would be recommended to carry out more efficient screening and ensure the safety of milk and dairy products from sheep and goats. (Author)

  4. Detection of residual rifampicin in urine via fluorescence quenching of gold nanoclusters on paper.

    Science.gov (United States)

    Chatterjee, Krishnendu; Kuo, Chiung Wen; Chen, Ann; Chen, Peilin

    2015-06-26

    Rifampicin or rifampin (R) is a common drug used to treat inactive meningitis, cholestatic pruritus and tuberculosis (TB), and it is generally prescribed for long-term administration under regulated dosages. Constant monitoring of rifampicin is important for controlling the side effects and preventing overdose caused by chronic medication. In this study, we present an easy to use, effective and less costly method for detecting residual rifampicin in urine samples using protein (bovine serum albumin, BSA)-stabilized gold nanoclusters (BSA-Au NCs) adsorbed on a paper substrate in which the concentration of rifampicin in urine can be detected via fluorescence quenching. The intensity of the colorimetric assay performed on the paper-based platforms can be easily captured using a digital camera and subsequently analyzed. The decreased fluorescence intensity of BSA-Au NCs in the presence of rifampicin allows for the sensitive detection of rifampicin in a range from 0.5 to 823 µg/mL. The detection limit for rifampicin was measured as 70 ng/mL. The BSA-Au NCs were immobilized on a wax-printed paper-based platform and used to conduct real-time monitoring of rifampicin in urine. We have developed a robust, cost-effective, and portable point-of-care medical diagnostic platform for the detection of rifampicin in urine based on the ability of rifampicin to quench the fluorescence of immobilized BSA-Au NCs on wax-printed papers. The paper-based assay can be further used for the detection of other specific analytes via surface modification of the BSA in BSA-Au NCs and offers a useful tool for monitoring other diseases.

  5. Palladium alloys for hydrogen diffusion

    International Nuclear Information System (INIS)

    1977-01-01

    A palladium-base alloy with tin and/or a silicon addition and its use in the production of hydrogen from water via a cycle of chemical reactions, of which the decomposition of HI into H 2 and I 2 is the most important, is described

  6. Palladium-Catalysed Coupling Reactions

    NARCIS (Netherlands)

    de Vries, Johannes G.; Beller, M; Blaser, HU

    2012-01-01

    Palladium-catalysed coupling reactions have gained importance as a tool for the production of pharmaceutical intermediates and to a lesser extent also for the production of agrochemicals, flavours and fragrances, and monomers for polymers. In this review only these cases are discussed where it seems

  7. Porogen residues detection in optical properties of low-k dielectrics cured by ultraviolet radiation

    Energy Technology Data Exchange (ETDEWEB)

    Marsik, Premysl, E-mail: marsik@physics.muni.c [UFKL, Masaryk University, Kotlarska 2, 61137 Brno (Czech Republic); IMEC, Kapeldreef 75, 3001 Leuven (Belgium); Verdonck, Patrick [IMEC, Kapeldreef 75, 3001 Leuven (Belgium); De Roest, David [ASM Belgium, Kapeldreef 75, 3001 Leuven (Belgium); Baklanov, Mikhail R. [IMEC, Kapeldreef 75, 3001 Leuven (Belgium)

    2010-05-31

    The optical properties of low dielectric constant (low-k) films have been determined by variable angle spectroscopic ellipsometry in the range from 2 eV to 9 eV to characterize the process of porogen removal during the UV-cure. The studied carbon doped oxide (SiCOH) porous dielectric films have been prepared by plasma enhanced chemical vapor deposition. The films have been deposited as a composition of a matrix precursor and an organic porogen. After deposition, the films have been cured by thermal annealing and UV irradiation ({lambda} = 172 nm) to remove the porogen and create a porosity of 33%, reaching a dielectric constant of 2.3. The process of porogen decomposition and removal has been studied on series of low-k samples, UV-cured for various times. Additional samples have been prepared by the deposition and curing of the porogen film, without SiCOH matrix, and the matrix material itself, without porogen. The analysis of the optical response of the porous dielectric as a mixture of matrix material, porogen and voids, together with Fourier transform infrared analysis, allows the sensitive detection of the volume of the porogen and indicates the existence of decomposed porogen residues inside the pores, even for long curing time. The variation of the deposition and curing conditions can control the amount of the porogen residues and the final porosity.

  8. Residual chromosomal damage after radiochemotherapy with and without amifostine detected by 24-color FISH

    International Nuclear Information System (INIS)

    Kuechler, A.; Wendt, T.G.; Dreidax, M.; Liehr, T.; Claussen, U.; Pigorsch, S.U.; Dunst, J.

    2003-01-01

    group either. Conclusion: While there was a significant amifostine-mediated clinical amelioration of normal tissue toxicity, the comparison of residual chromosomal damage 2-3 years after completion of radiochemotherapy was characterized by a high interindividual variation, and no equivalent difference could be detected between the two groups. (orig.)

  9. A novel chemiluminescence assay of organophosphorous pesticide quinalphos residue in vegetable with luminol detection

    Directory of Open Access Journals (Sweden)

    Yao Xin

    2010-06-01

    Full Text Available Abstract Background Organophosphorous pesticides are the most popular pesticides used in agriculture. As acetylcholinesterase inhibitors, organophosphorous pesticides are toxic organic chemicals. The control and detection of organophosphorous pesticide residue in food, water, and environment therefore plays a very important role in maintaining physical health. A sensitive, rapid, simple chemiluminescence(CL method has been developed for the determination of quinalphos based on the reaction of quinalphos with luminol-H2O2 in an alkaline medium. The method has been applied to detection of quinalphos in vegetable samples with satisfactory results. Results The CL method for the determination of organophosphorous pesticide quinalphos is based on the phenomenon that quinalphos can apparently enhance the CL intensity of the luminol-H2O2 system. The optimal conditions were: luminol concentration 5.0 × 10-4 mol/L, H2O2 concentration 0.05 mol/L.pH value 13. In order to restrain the interference from metal ions, 1.0 × 10-3 mol/L of EDTA was added to the luminol solution. The possible mechanism was proposed. Conclusion Under the optimum reaction conditions, CL was linear with the concentration of quinalphos in the range of 0.02 μg/mL -1.0 μg/mL and the detection limit was 0.0055 μg/mL (3σ. This method has been successfully applied to the detection of quinalphos in vegetable samples. According to the experimental data, the average recoveries for quinalphos in cherry tomato and green pepper 97.20% and 90.13%. Meanwhile, the possible mechanism was proposed.

  10. Residu Deltamethrin Terlacak pada Hati Ayam Pedaging yang Dipasarkan di Yogyakarta (DETECTION OF DELTAMETHRIN RESIDUE IN BROILER LIVER TRADED IN YOGYAKARTA

    Directory of Open Access Journals (Sweden)

    Gagak Donny Satria

    2014-05-01

    Full Text Available The consumer assurance to get safe, hygienic, whole, and halal food is an important concern. Analysisof chemical residue is one of some ways  to examine food safety. The objective of this research was to detectdeltamethrin residue in broiler liver sold in Yogyakarta, Indonesia. The isocratic HPLC method was usedin this research, using Shimadzu 6.1, 80% of Acetonitrile in Aquabides as mobile phase, with 1ml/minutesof flow rate. C-18 was used as column and the wavelength of UV-Vis detector was 270 nm. The result of theresearch was get from HPLC’s analyses. Deltamethrin’s peak area would be presented in retention time 8-12minutes with specific profile of curve. The result of the research showed that deltamethrin was positivelydetected in 13 broiler livers. It’s concluded that broiler livers that sold in Yogyakarta are detected to containdeltamethrin-contaminated.

  11. [Determination of emamectin benzoate residue in vegetables by high performance liquid chromatography with fluorescence detection].

    Science.gov (United States)

    Zhang, Yan; Wu, Yinliang; Hu, Jiye; Wang, Hongwei; Pan, Canping; Liu, Fengmao

    2008-01-01

    A method was developed for the determination of emamectin benzoate residue in cabbage and mushroom using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. The sample was extracted with ethyl acetate. Further cleanup was performed on a propylsulfonic acid solid phase extraction cartridge, followed by the derivatization with trifluoroacetic anhydride in the presence of N-methylimidazole. The amount of derivatized emamectin benzoate was determined by fluorescence detector after separation by HPLC. The detection limit was 0.10 microg/kg for cabbage and mushroom samples. The recoveries of emamectin benzoate in cabbage and mushroom samples were 78.6%-84.9%. The inter-day relative standard deviation (RSD) and intra-day RSD were 2.7%-6.0% and 3.1%-8.9%, respectively, at the fortified levels of 1.0-20.0 microg/kg. The calibration curve of emamectin benzoate in vegetables at the concentration range of 0.002 mg/L to 0.10 mg/L was linear (r = 0.9999).

  12. Post-mortem detection of gasoline residues in lung tissue and heart blood of fire victims.

    Science.gov (United States)

    Pahor, Kevin; Olson, Greg; Forbes, Shari L

    2013-09-01

    The purpose of this study was to determine whether gasoline residues could be detected post-mortem in lung tissue and heart blood of fire victims. The lungs and heart blood were investigated to determine whether they were suitable samples for collection and could be collected without contamination during an autopsy. Three sets of test subjects (pig carcasses) were investigated under two different fire scenarios. Test subjects 1 were anaesthetized following animal ethics approval, inhaled gasoline vapours for a short period and then euthanized. The carcasses were clothed and placed in a house where additional gasoline was poured onto the carcass post-mortem in one fire, but not in the other. Test subjects 2 did not inhale gasoline, were clothed and placed in the house and had gasoline poured onto them in both fires. Test subjects 3 were clothed but had no exposure to gasoline either ante- or post-mortem. Following controlled burns and suppression with water, the carcasses were collected, and their lungs and heart blood were excised at a necropsy. The headspace from the samples was analysed using thermal desorption-gas chromatography-mass spectroscopy. Gasoline was identified in the lungs and heart blood from the subjects that were exposed to gasoline vapours prior to death (test subjects 1). All other samples were negative for gasoline residues. These results suggest that it is useful to analyse for volatile ignitable liquids in lung tissue and blood as it may help to determine whether a victim was alive and inhaling gases at the time of a fire.

  13. Determination of palladium in various samples by atomic absorption spectrometry after preconcentration with dimethylglyoxime on silica gel

    International Nuclear Information System (INIS)

    Tokalioglu, Serife; Oymak, Tuelay; Kartal, Senol

    2004-01-01

    A preconcentration method based on the adsorption of palladium-dimethylglyoxime (DMG) complex on silica gel for the determination of palladium at trace levels by atomic absorption spectrometry (AAS) has been developed. The retained palladium as Pd(DMG) 2 complex was eluted with 1 mol l -1 HCl in acetone. The effect of some analytical parameters such as pH, amount of reagent and the sample volume on the recovery of palladium was examined in synthetic solutions containing street dust matrix. The influence of some matrix ions on the recovery of palladium was investigated by using the developed method when the elements were present both individually and together. The results showed that 2500 μg ml -1 Na + , K + , Mg 2+ , Al 3+ and Fe 3+ ; 5000 μg ml -1 Ca 2+ ; 500 μg ml -1 Pb 2+ ; 125 μg ml -1 Zn 2+ ; 50 μg ml -1 Cu 2+ and 25 μg ml -1 Ni 2+ did not interfere with the palladium signal. At the optimum conditions determined experimentally, the recovery for palladium was found to be 95.3±1.2% at the 95% confidence level. The relative standard deviation and limit of detection (3s/b) of the method were found to be 1.7% and 1.2 μg l -1 , respectively. In order to determine the adsorption behaviour of silica gel, the adsorption isotherm of palladium was studied and the binding equilibrium constant and adsorption capacity were calculated to be 0.38 l mg -1 and 4.06 mg g -1 , respectively. The determination of palladium in various samples was performed by using both flame AAS and graphite furnace AAS. The proposed method was successfully applied for the determination of palladium in the street dust, anode slime, rock and catalytic converter samples

  14. Radiochemical neutron activation analysis of high pure palladium and platinum by ion exchange chromatography

    International Nuclear Information System (INIS)

    Sadikov, I.I.; Zinov'ev, V.G.; Sadikova, Z.O.; Salimov, M.I.

    2006-01-01

    volume was obtained by elution curve of the determined elements and distribution profile of the matrix elements. Chemical yields of determined elements were measured by 'entered - found' method. Chemical yields of Sn is 31.2%; Zn is 54.5%; Se is 74.%1, and for other elements it is more than 85 %. Based on the carried out researches the radiochemical neutron activation analysis techniques of a high pure palladium and platinum are developed. These techniques allow determination of more than 30 elements with detection limits 10 -5 -10 -9 % with S r 0.15-0.2. (author)

  15. Label-Free and Multiplex Detection of Antibiotic Residues in Milk Using Imaging Surface Plasmon Resonance-Based Immunosensor

    NARCIS (Netherlands)

    Raz, Sabina Rebe; Bremer, Maria G. E. G.; Haasnoot, Willem; Norde, Willem

    2009-01-01

    Monitoring of antimicrobial drug residues in foods relies greatly on the availability of adequate analytical techniques. Currently, there is a need for a high-throughput screening method with a broad-spectrum detection range. This paper describes the development of a microarray biosensor, based on

  16. Label-Free and Multiplex Detection of Antibiotic Residues in Milk Using Imaging surface Plasmon Resonance-Based immunosensor

    NARCIS (Netherlands)

    Rebe, S.; Bremer, M.G.E.G.; Haasnoot, W.; Norde, W.

    2009-01-01

    Monitoring of antimicrobial drug residues in foods relies greatly on the availability of adequate analytical techniques. Currently, there is a need for a high-throughput screening method with a broad-spectrum detection range. This paper describes the development of a microarray biosensor, based on

  17. Detection and quantification of Roundup Ready soybean residues in sausage samples by conventional and real-time PCR.

    OpenAIRE

    MARCELINO-GUIMARÃES, F. C.; GUIMARÃES, M. F. M.; DE-BARROS, E. G.

    2009-01-01

    The increasing presence of products derived from genetically modified (GM) plants in human and animal diets has led to the development of detection methods to distinguish biotechnology-derived foods from conventional ones. The conventional and real-time PCR have been used, respectively, to detect and quantify GM residues in highly processed foods. DNA extraction is a critical step during the analysis process. Some factors such as DNA degradation, matrix effects, and the presence of PCR inhibi...

  18. Development and validation of a rapid test system for detection of pork meat and collagen residues.

    Science.gov (United States)

    Masiri, J; Benoit, L; Barrios-Lopez, B; Thienes, C; Meshgi, M; Agapov, A; Dobritsa, A; Nadala, C; Samadpour, M

    2016-11-01

    Mislabeling, contamination, and economic adulteration of meat products with undeclared pork tissues are illegal under regulations promulgated by numerous regulatory agencies. Nonetheless, analysis of the European meat industry has revealed pervasive meat adulteration, necessitating more extensive application of meat authentication testing. As existing methods for meat speciation require specialized equipment and/or training, we developed a detection system based on a lateral flow device (LFD) assay format capable of rapidly (~35min) identifying porcine residues derived from raw meat, cooked meat, and gelatin down to 0.01%, 1.0%, and 2.5% contamination, respectively. Specificity analysis revealed no cross-reactivity with meat derived from chicken, turkey, horse, beef, lamb, or goat. Comparison with a commercial ELISA kit and PCR method revealed similar if not improved sensitivity, with the added feature that the LFD-based system required considerably less time to perform. Accordingly, this test system should aid the food industry and food control authorities in monitoring for adulteration with pork. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Prognostic value of deep sequencing method for minimal residual disease detection in multiple myeloma

    Science.gov (United States)

    Lahuerta, Juan J.; Pepin, François; González, Marcos; Barrio, Santiago; Ayala, Rosa; Puig, Noemí; Montalban, María A.; Paiva, Bruno; Weng, Li; Jiménez, Cristina; Sopena, María; Moorhead, Martin; Cedena, Teresa; Rapado, Immaculada; Mateos, María Victoria; Rosiñol, Laura; Oriol, Albert; Blanchard, María J.; Martínez, Rafael; Bladé, Joan; San Miguel, Jesús; Faham, Malek; García-Sanz, Ramón

    2014-01-01

    We assessed the prognostic value of minimal residual disease (MRD) detection in multiple myeloma (MM) patients using a sequencing-based platform in bone marrow samples from 133 MM patients in at least very good partial response (VGPR) after front-line therapy. Deep sequencing was carried out in patients in whom a high-frequency myeloma clone was identified and MRD was assessed using the IGH-VDJH, IGH-DJH, and IGK assays. The results were contrasted with those of multiparametric flow cytometry (MFC) and allele-specific oligonucleotide polymerase chain reaction (ASO-PCR). The applicability of deep sequencing was 91%. Concordance between sequencing and MFC and ASO-PCR was 83% and 85%, respectively. Patients who were MRD– by sequencing had a significantly longer time to tumor progression (TTP) (median 80 vs 31 months; P < .0001) and overall survival (median not reached vs 81 months; P = .02), compared with patients who were MRD+. When stratifying patients by different levels of MRD, the respective TTP medians were: MRD ≥10−3 27 months, MRD 10−3 to 10−5 48 months, and MRD <10−5 80 months (P = .003 to .0001). Ninety-two percent of VGPR patients were MRD+. In complete response patients, the TTP remained significantly longer for MRD– compared with MRD+ patients (131 vs 35 months; P = .0009). PMID:24646471

  20. Development and primary application of ELISA method for detecting residual calf serum protein

    International Nuclear Information System (INIS)

    Li Hua; Yu Jiankun; Hong Chao; Long Ruixiang; Zhai Yougang; Xu Qiongfang; Cui Pingfang; Ding Xuefeng; Xie Zhongping

    2005-01-01

    To develop a new DAS-ELISA (double antibody sandwich ELISA) kit for detecting residual calf serum protein (CSP) in vaccines, calf sera from different district were pooled and used to immunize rabbits and hens respectively. Then, the IgY from yolk and the anti-CSP IgG from rabbit were separated and purified. The purified IgY was used as the coating antibody, and purified rabbit anti-CSP IgG was labeled by HRP. The optimal concentration of IgY was 25-30 μg/mL. The coating buffer was 0.01mol/L PBS(pH7.4) containing 0.4% glutin. The optimal dilutions of HRP-IgG were from 1:2000 to 1:3000. The sensitivity of this ELISA method was higher (up to 2.5μg/mL) than that of current RPHA, the variation coefficient was about 6.3%-9.4%, and the recovery rate was 90.4%-112.8%. Furthermore, there was no cross-reaction with sera of pig, monkey and guinea pig. Twenty lots of vaccines with Al(OH) 3 or without Al(OH) 3 were tested by ELISA and RPHA respectively. The results proved that the adjuvant of Al(OH) 3 had fewer influence on ELISA than on RPHA, the variation of PRHA among different lots of vaccines was more significant than ELISA. The ELISA method is a highly sensitive and useful method to detect CSP in vaccines. (authors)

  1. Palladium allergy in relation to dentistry

    NARCIS (Netherlands)

    Muris, J.

    2015-01-01

    Palladium is a metal that is used as alloying metal for dental crowns and bridges. This thesis focusses on the possible impact of oral exposure to this metal on the immune system, and allergy in particular. An alternative skin test allergen for diagnosing palladium allergy is introduced: (di)sodium

  2. In-situ observation of deuteride formation in palladium electrochemical cathode by X-ray diffraction method

    International Nuclear Information System (INIS)

    Yamamoto, Takao; Oka, Takashi; Taniguchi, Ryoichi

    1990-01-01

    In-situ X-ray diffraction observation of palladium foil cathode (10 μm) was carried out during electrolysis of 0.1N-LiOD heavy water solution in order to estimate the deuterium content in palladium during the detection of charged particles in our previous work. A complete transformation into β-palladium deuteride phase was observed, and its maximum lattice constant 4.06 A was evaluated as corresponding to D/Pd = 0.73. The deuterium concentration in the previous work was estimated as higher than this considering the difference in cell conditions. (author)

  3. with palladium (ii)

    African Journals Online (AJOL)

    Mgina

    Mercury telluride is an important semi conductor with application in infra-red detection (Charlon 1982, Mullin & Irrine. 1985). Photolysis of mixture of the organometallic compounds RHgTeR and. RCdTeR can produce mercury cadmium telluride. Haris and Nissan (1987) prepared. (t-butyl)HgTe(t-butyl) and demonstrated that.

  4. Effects of magnetic core geometry on false detection in residual current sensor

    International Nuclear Information System (INIS)

    Colin, Bruno; Chillet, Christian; Kedous-Lebouc, Afef; Mas, Patrick

    2006-01-01

    Under high-supply current, residual circuit breakers are subject to abnormal tripping, caused by false residual currents. Geometric or magnetic anomalies in the circuit breaker ring core seem to be responsible for these abnormal currents. This paper studies a few anomalies (spiral shape effect, conductor eccentricity, lamination effect) and calculates different contributions using the finite element simulations. The results show that the ring core, made of thin wound magnetic tape, is particularly sensitive to primary conductor eccentricity

  5. DETECTION OF LASALOCID RESIDUES IN THE TISSUES OF BROILER CHICKENS BY A NEW SCREENING TEST TOTAL ANTIBIOTICS

    Directory of Open Access Journals (Sweden)

    Martin Levkut, ml.

    2011-04-01

    Full Text Available The aim of the present study was to evaluate the microbial growth inhibition test Total antibiotics for the screening of lasalocid residues in the tissues of broiler chickens after its oral administration in medicated feed. The residues were investigated throughout the 5-day withdrawal period /WP/ and also on day 6 representing the first day following the WP. All broiler chicken tissues were positive for lasalocid. The breast muscle was positive (the presence of residues at/above the detection limit /LOD/ of method up to day 1 of the WP, the thigh muscle, gizzard, heart, skin and fat up to day 3 of the WP and the liver and kidneys up to day 4 of the WP. When evaluating the dubious results (the presence of residues just below the LOD of method, the breast muscle was suspect positive up to day 3 of the WP and the gizzard, skin and fat up to day 4 of the WP. No positive or dubious results were detected on day 5 of the WP. The LOD of Bacillus stearothermophilus var. calidolactis for maduramycin was 500 µg.l-1.doi:10.5219/140

  6. Detection of pesticides residues in water samples from organic and conventional paddy fields of Ledang, Johor, Malaysia

    Science.gov (United States)

    Abdullah, Md Pauzi; Othman, Mohamed Rozali; Ishak, Anizan; Nabhan, Khitam Jaber

    2016-11-01

    Pesticides have been used extensively by the farmers in Malaysia during the last few decades. Sixteen water samples, collected from paddy fields both organic and conventional, from Ledang, Johor, were analyzed to determine the occurrence and distribution of organochlorine (OCPs) and organophosphorus (OPPs) pesticide residues. GC-ECD instrument was used to identify and determine the concentrations of these pesticide residues. Pesticide residues were detected in conventional fields in the range about 0.036-0.508 µg/L higher than detected in organic fields about 0.015-0.428 µg/L. However the level of concentration of pesticide residues in water sample from both paddy fields are in the exceed limit for human consumption, according to European Economic Commission (EEC) (Directive 98/83/EC) at 0.1 µg/L for any pesticide or 0.5 µg/L for total pesticides. The results that the organic plot is still contaminated with pesticides although pesticides were not use at all in plot possibly from historical used as well as from airborne contamination.

  7. Divergent unprotected peptide macrocyclisation by palladium-mediated cysteine arylation.

    Science.gov (United States)

    Rojas, Anthony J; Zhang, Chi; Vinogradova, Ekaterina V; Buchwald, Nathan H; Reilly, John; Pentelute, Bradley L; Buchwald, Stephen L

    2017-06-01

    Macrocyclic peptides are important therapeutic candidates due to their improved physicochemical properties in comparison to their linear counterparts. Here we detail a method for a divergent macrocyclisation of unprotected peptides by crosslinking two cysteine residues with bis-palladium organometallic reagents. These synthetic intermediates are prepared in a single step from commercially available aryl bis-halides. Two bioactive linear peptides with cysteine residues at i , i + 4 and i , i + 7 positions, respectively, were cyclised to introduce a diverse array of aryl and bi-aryl linkers. These two series of macrocyclic peptides displayed similar linker-dependent lipophilicity, phospholipid affinity, and unique volume of distributions. Additionally, one of the bioactive peptides showed target binding affinity that was predominantly affected by the length of the linker. Collectively, this divergent strategy allowed rapid and convenient access to various aryl linkers, enabling the systematic evaluation of the effect of appending unit on the medicinal properties of macrocyclic peptides.

  8. Intra-operative X-ray diagnostics in the detection and localization of residual concretions in the kidney

    International Nuclear Information System (INIS)

    Soekeland, J.; Degenhardt, W.

    1979-01-01

    Problems of intra-operative X-ray diagnostics in the detection and localization of residual concretions in the kidney are discussed, together with the limitations of image-intensifier techniques, automatic exposure control, and the use of modified dental X-ray equipment. A technique using a film-screen combination and X-ray tube designed for mammography is discussed, together with its applications and possible future development. (Auth.)

  9. Usefulness of Choline-PET for the detection of residual hemangiopericytoma in the skull base: comparison with FDG-PET

    Directory of Open Access Journals (Sweden)

    Ito Shin

    2012-02-01

    Full Text Available Abstract Background Choline is a new PET tracer that is useful for the detection of malignant tumor. Choline is a precursor of the biosynthesis of phosphatidylcholine, a major phospholipid in the cell membrane of eukaryotic cells. Malignant tumors have an elevated level of phosphatidylcholine in cell membrane. Thus, choline is a marker of tumor malignancy. Method The patient was a 51-year-old man with repeated recurrent hemangiopericytoma in the skull base. We performed Choline-PET in this patient after various treatments and compared findings with those of FDG-PET. Results Choline accumulated in this tumor, but FDG did not accumulate. We diagnosed this tumor as residual hemangiopericytoma and performed the resection of the residual tumor. FDG-PET is not appropriate for skull base tumor detection because uptake in the brain is very strong. Conclusion We emphasize the usefulness of Choline-PET for the detection of residual hemangiopericytoma in the skull base after various treatments, compared with FDG-PET.

  10. Manufacturing inspection of electrical steels using Magnetic Barkhausen Noise: residual stress detection

    Energy Technology Data Exchange (ETDEWEB)

    Samimi, A.A., E-mail: 9aa8@queensu.ca [Queen' s Univ., Applied Magnetics Group, Kingston, Ontario (Canada); Krause, T.W. [Royal Military College of Canada, NDE Lab., Kingston, Ontario (Canada); Clapham, L. [Queen' s Univ., Applied Magnetics Group, Kingston, Ontario (Canada); Gallaugher, M.; Ding, Y.; Chromik, R. [McGill Univ., Dept. of Mining and Materials Engineering, Montreal, Quebec (Canada)

    2016-09-15

    Non-oriented Electrical Steel (NOES) is the magnetic core lamination material used for flux transfer in rotary machines. The presence of residual stress associated with material processing may be detrimental to magnetic domain structure refinement and as a result, magnetic performance of NOES. Therefore, manufacturing inspection of NOES that identifies the presence of residual stress could contribute to the production of more energy efficient cores. However, standard materials evaluation is limited to destructive and off-line techniques. The present work employed Magnetic Barkhausen Noise (MBN) for nondestructive identification of local residual stress associated with stages in material processing. Analysis of MBN from single strips of NOES demonstrated clear response to applied tensile stress, mechanical shearing, the presence of an insulating coating and punching. The results establish the potential of MBN as a nondestructive testing technology for quality control of electrical steels at various stages of manufacture. (author)

  11. Qualitative screening method for pesticide residues detection in fruits and vegetables

    Directory of Open Access Journals (Sweden)

    Iván Mauricio Huérfano Barco

    2018-01-01

    Full Text Available Because of the importance of developing methodologies that allow agricultural residues analysis, a rapid screening qualitative method for the determination of pesticides residues in fruits and vegetables was validated. The methodology was based on the European QuEChERS extraction method with an additional cleaning step by gel permeation chromatography (GPC, which helped to reduce the number of matrix components in the final extract. The analysis was carried out by gas chromatography coupled to mass spectrometry with a single quadrupole analyzer. The methodology was appropriate for the qualitative analysis of 31 pesticides at their respective maximum residue limits. Consistent results were obtained with respect to a quantitative routine methodology in the analysis of real samples, hence the methodology was proven to be a good alternative for the fast analysis of these contaminants in fruits and vegetables.

  12. Anionic Palladium(0) and Palladium(II) Ate Complexes.

    Science.gov (United States)

    Kolter, Marlene; Böck, Katharina; Karaghiosoff, Konstantin; Koszinowski, Konrad

    2017-10-16

    Palladium ate complexes are frequently invoked as important intermediates in Heck and cross-coupling reactions, but so far have largely eluded characterization at the molecular level. Here, we use electrospray-ionization mass spectrometry, electrical conductivity measurements, and NMR spectroscopy to show that the electron-poor catalyst [L 3 Pd] (L=tris[3,5-bis(trifluoromethyl)phenyl]phosphine) readily reacts with Br - ions to afford the anionic, zero-valent ate complex [L 3 PdBr] - . In contrast, more-electron-rich Pd catalysts display lower tendencies toward the formation of ate complexes. Combining [L 3 Pd] with LiI and an aryl iodide substrate (ArI) results in the observation of the Pd II ate complex [L 2 Pd(Ar)I 2 ] - . © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Radiofrequency ablation of renal tumours: diagnostic accuracy of contrast-enhanced ultrasound for early detection of residual tumour

    International Nuclear Information System (INIS)

    Hoeffel, Christine; Pousset, Maud; Elie, Caroline; Timsit, Marc-Olivier; Mejean, Arnaud; Merran, Samuel; Tranquart, Francois; Khairoune, Ahmed; Helenon, Olivier; Correas, Jean-Michel; Joly, Dominique; Richard, Stephane

    2010-01-01

    To evaluate the diagnostic accuracy of contrast-enhanced ultrasound (CEUS) in the early detection of residual tumour after radiofrequency ablation (RFA) of renal tumours. Patients referred to our institution for RFA of renal tumours prospectively underwent CEUS and computed tomography (CT) or magnetic resonance imaging (MRI) before, within 1 day and 6 weeks after treatment. Identification of residual tumour was assessed by three blinded radiologists. Reference standard was CT/MRI performed at least 1 year after RFA. A total of 66 renal tumours in 43 patients (median age 62 years; range 44-71.5) were studied. Inter-reader agreement (κ value) was 0.84 for CEUS. Prevalence of residual disease was 19%. Sensitivity, specificity, positive predictive value (PPV) and negative predictive value (NPV), respectively, were as follows: 64% [confidence interval (CI) 39-84], 98% [CI 91-100], 82% [CI 52-95] and 92% [CI 83-97] on 24-h CEUS; 79% [CI 52-92], 100% [CI 94-100], 100% [CI 74-100] and 95% [CI 87-100] on 6-week CEUS; 79% [CI 52-92], 95% [CI 86-98], 79% [CI 52-92] and 95% [CI 86-98] on 24-h CT/MRI; and 100% [CI 72-100], 98% [CI 90-100], 91% [CI 62-98] and 100% [CI 93-100] on 6-week CT/MRI. CEUS has high specificity for the early diagnosis of residual tumour after renal RFA. (orig.)

  14. Measurement of capillary permeability in canine heart determined by the tissue injection, residue detection method

    DEFF Research Database (Denmark)

    Svendsen, Jesper Hastrup; Paaske, W P; Haunsø, S

    1991-01-01

    (apparent) interstitial volume of distribution, tev is the mean transit time of the indicator, and klo is the recorded fractional initial washout rate constant. In experiments on open chest dog hearts we examined capillary permeability for 51Cr-EDTA and 99mTc-DTPA with the tissue injection, residue...

  15. Detection of organic residues on poultry processing equipment surfaces by LED-induced fluorescence imaging

    Science.gov (United States)

    Organic residues on equipment surfaces in poultry processing plants can generate cross- contamination and increase the risk of unsafe food for consumers. This research was aimed to investigate the potential of LED-induced fluorescence imaging technique for rapid inspection of stainless steel proces...

  16. The detection, rate and manifestation of residual sexuality in apomictic populations of Pilosella (Asteraceae, Lactuceae)

    Czech Academy of Sciences Publication Activity Database

    Krahulcová, Anna; Rotreklová, O.; Krahulec, František

    2014-01-01

    Roč. 49, č. 2 (2014), s. 239-258 ISSN 1211-9520 R&D Projects: GA ČR GAP506/10/1363 Institutional support: RVO:67985939 Keywords : facultative apomixis * haploid parthenogenesis * interspecific hybridization * Pilosella * residual sexuality Subject RIV: EF - Botanics Impact factor: 1.778, year: 2014

  17. Determination of palladium by flame photometry

    International Nuclear Information System (INIS)

    Parellada Bellod, R.

    1964-01-01

    A study on the determination of palladium by lame photometry, fixing the most convent experimental conditions and using solvents to increase the emission of this elements is carried out. Among the organic solvents, acetone has been found the most efficient. The interferences produced by anions and cations have also been studied and an analytical method is related, in which lines of calibration of 0 to 100 ppm palladium re used. (Author) 7 refs

  18. [THE COMPARISON OF RESULTS OF DETECTION OF MINIMAL RESIDUAL DISEASE IN PERIPHERAL BLOOD AND MARROW IN CHILDREN OF THE FIRST YEAR OF LIFE WITH ACUTE LYMPHOBLASTIC LEUCOSIS].

    Science.gov (United States)

    Tsaur, G A; Riger, T O; Popov, A M; Nasedkina, T V; Kustanovich, A M; Solodovnikov, A G; Streneva, O V; Shorikov, E V; Tsvirenko, S V; Saveliev, L I; Fechina, L G

    2015-04-01

    The occurrence of minimal residual disease is an important prognostic factor under acute lymphoblastic leucosis in children and adults. In overwhelming majority of research studies bone marrow is used to detect minimal residual disease. The comparative characteristic of detection of minimal residual disease in peripheral blood and bone marrow was carried out. The prognostic role of occurrence of minimal residual disease in peripheral blood and bone marrow under therapy according protocol MLL-Baby was evaluated. The analysis embraced 142 pair samples from 53 patients with acute lymphoblastic leucosis and various displacements of gene MLL younger than 365 days. The minimal residual disease was detected by force of identification of chimeric transcripts using polymerase chain reaction in real-time mode in 7 sequential points of observation established by protocol of therapy. The comparability of results of qualitative detection of minimal residual disease in bone marrow and peripheral blood amounted to 84.5%. At that, in all 22 (15.5%) discordant samples minimal residual disease was detected only in bone marrow. Despite of high level of comparability of results of detection of minimal residual disease in peripheral blood and bone marrow the occurrence of minimal residual disease in peripheral blood at various stages of therapy demonstrated no independent prognostic significance. The established differences had no relationship with sensitivity of method determined by value of absolute expression of gene ABL. Most likely, these differences reflected real distribution of tumor cells. The results of study demonstrated that application of peripheral blood instead of bone marrow for monitoring of minimal residual disease under acute lymphoblastic leucosis in children of first year of life is inappropriate. At the same time, retention of minimal residual disease in TH4 in bone marrow was an independent and prognostic unfavorable factor under therapy of acute lymphoblastic

  19. Shaping surface of palladium nanospheres through the control of reaction parameters

    International Nuclear Information System (INIS)

    Wang Lianmeng; Tan Enzhong; Guo Lin; Wang Lihua; Han Xiaodong

    2011-01-01

    Solid, cracked, and flower-shaped surfaces of palladium nanospheres with high yields and good uniformity were successfully prepared by a wet chemical method. On the basis of the experimental data, the same size of palladium nanosphere with different surface morphologies can be regulated only by changing the amount of ammonium hydroxide and reductant in one experimental system. The as-prepared products were studied by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and x-ray diffraction (XRD). In addition, surface-enhanced Raman scattering (SERS) spectra on the as-prepared different surface of palladium nanospheres exhibit high activity towards p-aminothiophenol (PATP) detection, and the result further reveals that the predominance of the a1 vibration mode in the SERS spectra via an electromagnetic (EM) mechanism is significant.

  20. Evaluation of Total Nitrite Pattern Visualization as an Improved Method for Gunshot Residue Detection and its Application to Casework Samples.

    Science.gov (United States)

    Berger, Jason; Upton, Colin; Springer, Elyah

    2018-04-23

    Visualization of nitrite residues is essential in gunshot distance determination. Current protocols for the detection of nitrites include, among other tests, the Modified Griess Test (MGT). This method is limited as nitrite residues are unstable in the environment and limited to partially burned gunpowder. Previous research demonstrated the ability of alkaline hydrolysis to convert nitrates to nitrites, allowing visualization of unburned gunpowder particles using the MGT. This is referred to as Total Nitrite Pattern Visualization (TNV). TNV techniques were modified and a study conducted to streamline the procedure outlined in the literature to maximize the efficacy of the TNV in casework, while reducing the required time from 1 h to 5 min, and enhancing effectiveness on blood-soiled samples. The TNV method was found to provide significant improvement in the ability to detect significant nitrite residues, without sacrificing efficiency, that would allow for the determination of the muzzle-to-target distance. © 2018 American Academy of Forensic Sciences.

  1. Accuracy of high-field intraoperative MRI in the detectability of residual tumor in glioma grade IV resections

    Energy Technology Data Exchange (ETDEWEB)

    Hesselmann, Volker; Mager, Ann-Kathrin [Asklepios-Klinik Nord, Hamburg (Germany). Radiology/Neurologie; Goetz, Claudia; Kremer, Paul [Asklepios-Klinik Nord, Hamburg (Germany). Dept. of Neurosurgery; Detsch, Oliver [Asklepios-Klinik Nord, Hamburg (Germany). Dept. of Anaesthesiology and Intensive Care Medicine; Theisgen, Hannah-Katharina [Universitaetsklinikum Schleswig-Holstein, Kiel (Germany). Dept. of Neurosurgery; Friese, Michael; Gottschalk, Joachim [Asklepios-Klinik Nord, Hamburg (Germany). Dept. of Pathology and Neuropathology; Schwindt, Wolfram [Univ. Hospital Muenster (Germany). Dept. of Clinical Radiology

    2017-06-15

    To assess the sensitivity/specificity of tumor detection by T1 contrast enhancement in intraoperative MRI (ioMRI) in comparison to histopathological assessment as the gold standard in patients receiving surgical resection of grade IV glioblastoma. 68 patients with a primary or a recurrent glioblastoma scheduled for surgery including fluorescence guidance and neuronavigation were included (mean age: 59 years, 26 female, 42 male patients). The ioMRI after the first resection included transverse FLAIR, DWI, T2-FFE and T1 - 3 d FFE ± GD-DPTA. The second resection was performed whenever residual contrast-enhancing tissue was detected on ioMRI. Resected tissue samples were histopathologically evaluated (gold standard). Additionally, we evaluated the early postoperative MRI scan acquired within 48 h post-OP for remaining enhancing tissue and compared them with the ioMRI scan. In 43 patients ioMRI indicated residual tumorous tissue, which could be confirmed in the histological specimens of the second resection. In 16 (4 with recurrent, 12 with primary glioblastoma) cases, ioMRI revealed truly negative results without residual tumor and follow-up MRI confirmed complete resection. In 7 cases (3 with recurrent, 4 with primary glioblastoma) ioMRI revealed a suspicious result without tumorous tissue in the histopathological workup. In 2 (1 for each group) patients, residual tumorous tissue was detected in spite of negative ioMRI. IoMRI had a sensitivity of 95 % (94 % recurrent and 96 % for primary glioblastoma) and a specificity of 69.5 % (57 % and 75 %, respectively). The positive predictive value was 86 % (84 % for recurrent and 87 % for primary glioblastoma), and the negative predictive value was 88 % (80 % and 92 %, respectively). ioMRI is effective for detecting remaining tumorous tissue after glioma resection. However, scars and leakage of contrast agent can be misleading and limit specificity. Intraoperative MRI (ioMRI) presents with a high sensitivity for residual

  2. Accuracy of high-field intraoperative MRI in the detectability of residual tumor in glioma grade IV resections

    International Nuclear Information System (INIS)

    Hesselmann, Volker; Mager, Ann-Kathrin; Goetz, Claudia; Kremer, Paul; Detsch, Oliver; Theisgen, Hannah-Katharina; Friese, Michael; Gottschalk, Joachim; Schwindt, Wolfram

    2017-01-01

    To assess the sensitivity/specificity of tumor detection by T1 contrast enhancement in intraoperative MRI (ioMRI) in comparison to histopathological assessment as the gold standard in patients receiving surgical resection of grade IV glioblastoma. 68 patients with a primary or a recurrent glioblastoma scheduled for surgery including fluorescence guidance and neuronavigation were included (mean age: 59 years, 26 female, 42 male patients). The ioMRI after the first resection included transverse FLAIR, DWI, T2-FFE and T1 - 3 d FFE ± GD-DPTA. The second resection was performed whenever residual contrast-enhancing tissue was detected on ioMRI. Resected tissue samples were histopathologically evaluated (gold standard). Additionally, we evaluated the early postoperative MRI scan acquired within 48 h post-OP for remaining enhancing tissue and compared them with the ioMRI scan. In 43 patients ioMRI indicated residual tumorous tissue, which could be confirmed in the histological specimens of the second resection. In 16 (4 with recurrent, 12 with primary glioblastoma) cases, ioMRI revealed truly negative results without residual tumor and follow-up MRI confirmed complete resection. In 7 cases (3 with recurrent, 4 with primary glioblastoma) ioMRI revealed a suspicious result without tumorous tissue in the histopathological workup. In 2 (1 for each group) patients, residual tumorous tissue was detected in spite of negative ioMRI. IoMRI had a sensitivity of 95 % (94 % recurrent and 96 % for primary glioblastoma) and a specificity of 69.5 % (57 % and 75 %, respectively). The positive predictive value was 86 % (84 % for recurrent and 87 % for primary glioblastoma), and the negative predictive value was 88 % (80 % and 92 %, respectively). ioMRI is effective for detecting remaining tumorous tissue after glioma resection. However, scars and leakage of contrast agent can be misleading and limit specificity. Intraoperative MRI (ioMRI) presents with a high sensitivity for residual

  3. Detection of Salmonella spp., Candida albicans, Aspergillus spp., and Antimicrobial Residues in Raw and Processed Cow Milk from Selected Smallholder Farms of Zimbabwe

    Directory of Open Access Journals (Sweden)

    Tryness Anastazia Mhone

    2012-01-01

    Full Text Available A cross-sectional study was conducted to detect the presence of Salmonella spp., Candida albicans, Aspergillus spp., and antimicrobial residues in raw milk (n=120 and processed cow milk (n=20 from smallholder dairy farms from three sites in Zimbabwe. Culture and isolation of Salmonella spp., C. albicans, and Aspergillus spp. were performed using selective media, while antimicrobial residues were detected by a dye reduction test. No Salmonella, but C. albicans (17.5%; 21/120, Aspergillus spp. (0.8%; 1/120, and antimicrobial residues (2.5%; 3/120 were detected from raw milk. C. albicans was isolated from all three sites, while Aspergillus spp. and antimicrobial residues were detected from sites 1 and 3, respectively. From processed milk, only C. albicans (5% was isolated while Aspergillus spp. and antimicrobial residues were not detected. These results suggested low prevalence of Salmonella spp. and Aspergillus spp. and a relatively high prevalence of C. albicans in raw milk from the smallholder farms. The potential public health risks of C. albicans and the detected antimicrobial residues need to be considered. Thus, educating farmers on improving milking hygiene and storage of milk and establishing programmes for monitoring antimicrobial residues may help to improve the safety of milk from smallholder farms.

  4. Detection of gunshot primer residue on bone in an experimental setting-an unexpected finding.

    Science.gov (United States)

    Berryman, Hugh E; Kutyla, Alicja K; Russell Davis, J

    2010-03-01

    Pork ribs with intact muscle tissue were used in an experimental attempt to identify bullet wipe on bone at distances from 1 to 6 feet with 0.45 caliber, full metal jacket ammunition. This resulted in the unexpected finding of primer-derived gunshot residue (GSR) deep within the wound tract. Of significance is the fact that the GSR was deposited on the bone, under the periosteum, after the bullet passed through a Ziploc bag and c. 1 inch of muscle tissue. It is also important to note that the GSR persisted on the bone after the periosteum was forcibly removed. The presence of primer-derived GSR on bone provides the potential to differentiate gunshot trauma from blunt trauma when the bone presents an atypical gunshot wound. In this study, the presence of gunshot primer residue at a distance of 6 feet demonstrates the potential for establishing maximum gun-to-target distance for remote shootings.

  5. Preparation of palladium impregnated alumina adsorbents: Thermal and neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Mukherjee, Sumanta; Gupta, N.K.; Roy, S.P.; Dash, S.; Kumar, A.; Bamankar, Y.R.; Rao, T.V. Vittal [Product Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Kumar, N. [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Naik, Y., E-mail: ynaik@barc.gov.in [Product Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)

    2016-02-10

    Highlights: • Pd/Al{sub 2}O{sub 3} composite microspheres particles with high surface area were prepared sol–gel process. • Scanning electron microscopy (SEM) studies on silver coated particle. • Content of the palladium was determined using Neutron Activation Analysis (NAA). • Decomposition study has been done by quadrupole mass analyser. - Abstract: Pd/Al{sub 2}O{sub 3} composite microspheres particles with high surface area were prepared sol–gel process. The decomposition of dried gel-particles was studied by TGA/DTA and FT-IR technique. TGA studies indicated that formation of palladium is marked by a broad exothermic peak with a loss of water and oxidation of trapped HMTA/Urea nitrate mixture. The main decomposition reaction took place in the temperature range of 660–1250 K in helium and relatively lower temperature of 400 K to 1250 K in oxygen. Optical microscopy indicated that the distribution of palladium is uniform. SEM studies on silver coated particle indicated that there was surface erosion of some gel spheres while in few of them micro cracks were seen at high resolution. Content of the palladium was determined using Neutron Activation Analysis (NAA). Decomposition at various temperatures was studied using Residual gas analyser and decomposition species were identified using quadrupole mass analyser.

  6. Role of CD81 and CD58 in minimal residual disease detection in pediatric B lymphoblastic leukemia.

    Science.gov (United States)

    Tsitsikov, E; Harris, M H; Silverman, L B; Sallan, S E; Weinberg, O K

    2018-06-01

    Minimal residual disease (MRD) in B lymphoblastic leukemia has been demonstrated to be a powerful predictor of clinical outcome in numerous studies in both children and adults. In this study, we evaluated 86 pediatric patients with both diagnostic and remission flow cytometry studies and compared expression of CD81, CD58, CD19, CD34, CD20, and CD38 in the detection of MRD. We evaluated 86 patients with B lymphoblastic leukemia who had both diagnostic studies and remission studies for the presence of MRD using multicolor flow cytometry. We established our detection limit for identifying abnormal lymphoblasts using serial dilutions. We also compared flow cytometry findings with molecular MRD detection in a subset of patients. We found that we can resolve differences between hematogones and lymphoblasts in 85 of 86 cases using a combination of CD45, CD19, CD34, CD10, CD20, CD38, CD58, and CD81. Our detection limit using flow cytometry is 0.002% for detecting a population of abnormal B lymphoblasts. Comparison with MRD assessment by molecular methods showed a high concordance rate with flow cytometry findings. Our study highlights importance of using multiple markers to detect MRD in B lymphoblastic leukemia. Our findings indicate that including both CD58 and CD81 markers in addition to CD19, CD34, CD20, CD38, and CD10 are helpful in MRD detection by flow cytometry. © 2018 John Wiley & Sons Ltd.

  7. Detection of clarithromycin-resistant Helicobacter pylori by polymerase chain reaction using residual samples from rapid urease test

    Directory of Open Access Journals (Sweden)

    Jae-Sik Jeon

    2017-01-01

    Full Text Available Background: Approximately 50% of the world population is infected with Helicobacter pylori, which corresponds to a high infection rate. Furthermore, the incidence of antibiotic-resistant H. pylori has increased with the recent rise in use of antibiotics for H. pylori elimination, suggesting growing treatment failures. Aim: The study was aimed to assess the use of residual samples from rapid urease test (RUT for biomolecular testing as an effective and accurate method to detect antibiotic-resistant H. pylori. Settings and Design: This study was a retrospective study performed using data obtained from medical records of previously isolated H. pylori strains. Materials and Methods: RUT was conducted for 5440 biopsy samples from individuals who underwent health examination in South Korea. Subsequently, 469 RUT residual samples were randomly selected and subjected to polymerase chain reaction (PCR to detect antibiotic-resistant H. pylori. Statistical Analysis Used: The Chi-square test was used to analyse categorical data. P < 0.05 was considered statistically significant. Results: The results showed a concordance between the results of PCR and conventional RUT in 450 of 469 samples, suggesting that the H. pylori PCR test is a time- and cost-effective detection method. Conclusions: This study demonstrated that PCR test can aid physicians to prescribe the appropriate antibiotics at the time of diagnosis, thus preventing the reduction in H. pylori eradication due to antibiotic resistance, averting progression to serious diseases and increasing the treatment success rate.

  8. Rapid Colorimetric Detection of Cartap Residues by AgNP Sensor with Magnetic Molecularly Imprinted Microspheres as Recognition Elements

    Directory of Open Access Journals (Sweden)

    Mao Wu

    2018-06-01

    Full Text Available The overuse of cartap in tea tree leads to hazardous residues threatening human health. A colorimetric determination was established to detect cartap residues in tea beverages by silver nanoparticles (AgNP sensor with magnetic molecularly imprinted polymeric microspheres (Fe3O4@mSiO2@MIPs as recognition elements. Using Fe3O4 as supporting core, mesoporous SiO2 as intermediate shell, methylacrylic acid as functional monomer, and cartap as template, Fe3O4@mSiO2@MIPs were prepared to selectively and magnetically separate cartap from tea solution before colorimetric determination by AgNP sensors. The core-shell Fe3O4@mSiO2@MIPs were also characterized by FT-IR, TEM, VSM, and experimental adsorption. The Fe3O4@mSiO2@MIPs could be rapidly separated by an external magnet in 10 s with good reusability (maintained 95.2% through 10 cycles. The adsorption process of cartap on Fe3O4@mSiO2@MIPs conformed to Langmuir adsorption isotherm with maximum adsorption capacity at 0.257 mmol/g and short equilibrium time of 30 min at 298 K. The AgNP colorimetric method semi-quantified cartap ≥5 mg/L by naked eye and quantified cartap 0.1–5 mg/L with LOD 0.01 mg/L by UV-vis spectroscopy. The AgNP colorimetric detection after pretreatment with Fe3O4@mSiO2@MIPs could be successfully utilized to recognize and detect cartap residues in tea beverages.

  9. Palladium coated fibre Bragg grating based hydrogen sensor

    International Nuclear Information System (INIS)

    Kasinathan, M.; Sosamma, S.; Kishore, S.; Elumalai, V.; Krishnan, R.; Babu Rao, C.; Dash, Sitaram; Murali, N.; Jayakumar, T.

    2011-01-01

    Detection of steam generator leaks in fast nuclear reactors is carried out by monitoring hydrogen in argon cover-gas. Hydrogen released during sodium cleaning of fast reactor components is required to be monitored. Hydrogen sensors with good sensitivity, stability and response time are required for all the above applications. We report a new type of hydrogen sensor with a Fibre Bragg Grating (FBG) coated with palladium thin film which is used to detect the leak of hydrogen gas in the Steam Generator (SG) module of the Fast Breeder Reactor (FBR). If water leaks into sodium, it results in sodium-water reaction. In this reaction hydrogen and sodium hydroxide are formed. Due to the explosive risk of hydrogen system, hydrogen sensors are of great interest in this case. It is known that hydrogen forms an explosive mixture with air once its concentration exceeds beyond the explosion limit of four percent. The advantages of FBG based hydrogen sensor over the other hydrogen sensors are its inherent property of safety from sparking, immunity to ambient electromagnetic interference. The sensing mechanism in this device is based on mechanical strain that is induced in the palladium coating when it absorbs hydrogen. This process physically stretches the grating and causes the grating period and grating's refractive index, to change. The Bragg wavelength shift is directly proportional to the strain induced and can be directly related to the percentage of hydrogen exposure. The online monitoring of palladium thin film coating on FBG is carried out and recorded the wavelength change and strain induced on the FBG. A hydrogen sensor set up have been fabricated which consists of SS vessel of capacity 10 litres, provided with pressure gauge, Argon filling line with a valve, Hydrogen injection line with flange, a vent line with valve and Hydrogen sensor fixing point. The Palladium coated FBG based Hydrogen sensor is tested in this experimental facility in the exposure of hydrogen in

  10. Copper-based electrochemical sensor with palladium electrode for cathodic stripping voltammetry of manganese.

    Science.gov (United States)

    Kang, Wenjing; Pei, Xing; Bange, Adam; Haynes, Erin N; Heineman, William R; Papautsky, Ian

    2014-12-16

    In this work, we report on the development of a palladium-based, microfabricated point-of-care electrochemical sensor for the determination of manganese using square wave cathodic stripping voltammetry. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Voltammetry offers an attractive approach to metal detection on the microscale, but traditional carbon, gold, or platinum electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor uses palladium working and auxiliary electrodes and integrates them with a copper-based reference electrode for simple fabrication and compatibility with microfabrication and printed circuit board processing, while maintaining competitive performance in electrochemical detection. Copper electrodes were prepared on glass substrate using a combination of microfabrication procedures followed by electrodeposition of palladium. The disposable sensor system was formed by bonding a poly(dimethylsiloxane) (PDMS) well to the glass substrate. Cathodic stripping voltammetry of manganese using our new disposable palladium-based sensors exhibited 334 nM (18.3 ppb) limit of detection in borate buffer. The sensor was used to demonstrate manganese determination in natural water samples from a pond in Burnet Woods, located in Cincinnati, OH, and the Ohio River.

  11. Residual tissue post splenectomy detected by splenic scintillography with erythrocytes damaged by heat

    International Nuclear Information System (INIS)

    Rivera B, B.; Garcia C, E.S.; Garcia O, J.R.

    2005-01-01

    Feminine of 26 years old with diagnostic of purple thrombocytopenic idiopathic to those 4 years of age, tried with steroids and splenectomy at 11 years old. Pathway practically asymptomatic until 4 months ago she had presented asthenia, adynamia and general uneasiness, with platelet figures of 40,000 plat/microliter. It was carried out scintillographic study with damaged erythrocytes for post surgical remainder search. Its were took two-dimensional images and tomography by single photon emission (SPECT), being knitted splenic residual in area of anatomical projection of the spleen. (Author)

  12. Suitability of the charm HVS and a microbiological multiplate system for detection of residues in raw milk at EU maximum residue levels

    NARCIS (Netherlands)

    Nouws, J.F.M.; Egmond, van H.; Loeffen, G.; Schouten, J.; Keukens, H.; Smulders, I.; Stegeman, H.

    1999-01-01

    In this paper we assessed the suitability of the Charm HVS and a newly developed microbiological multiplate system as post-screening tests to confirm the presence of residues in raw milk at or near the maximum permissible residue level (MRL). The multiplate system is composed of Bacillus

  13. Palladium-cobalt particles as oxygen-reduction electrocatalysts

    Science.gov (United States)

    Adzic, Radoslav [East Setauket, NY; Huang, Tao [Manorville, NY

    2009-12-15

    The present invention relates to palladium-cobalt particles useful as oxygen-reducing electrocatalysts. The invention also relates to oxygen-reducing cathodes and fuel cells containing these palladium-cobalt particles. The invention additionally relates to methods for the production of electrical energy by using the palladium-cobalt particles of the invention.

  14. Unexpectedly high uptake of palladium by bituminous coals

    Energy Technology Data Exchange (ETDEWEB)

    Lakatos, J. [Research Lab. for Mining Chemistry, Hungarian Academy of Sciences, Miskolc-Egyetemvaros (Hungary); Brown, S.D.; Snape, C.E. [Univ. of Strathclyde, Dept. of Pure and Applied Chemistry, Glasgow (United Kingdom)

    1997-12-31

    The uptake of palladium as a conversion catalyst onto coals of different rank was investigated. Palladium fixation occurs by a different mode to that for alkaline earth and first row transition metals. Therefore, the dispersion of relatively high concentration of palladium by an ion sorption process is even possible for bituminous coals. (orig.)

  15. : Recyclable, ligand free palladium(II) catalyst for Heck reaction

    Indian Academy of Sciences (India)

    well as heterogeneous palladium catalysts, generated from either palladium(0) compounds or palladium(II) acetate or chloride salts.6 Several ligands such as phosphines, phoshites, carbenes, thioethers have been successfully employed for this reaction.7 However, homogeneous catalysis results in problems of recovery.

  16. Sensitivity of enhanced MRI for the detection of breast cancer: new, multicentric, residual, and recurrent

    International Nuclear Information System (INIS)

    Davis, P.L.; McCarty, K.S. Jr.

    1997-01-01

    Magnetic resonance imaging (MRI) of the breast brings the advantages of high resolution cross-sectional imaging to breast cancer diagnosis, treatment and research: improved cancer detection, staging, selection of therapy, evaluation of therapeutic response in vivo, detection of recurrence, and even the development of new therapies. Until now breast cancer treatment and research has been impeded by the limited means of evaluating the breast cancer in vivo: primarily clinical palpation and mammography of the breast tumor. A review of the initial studies shows that with the use of paramagnetic contrast agents, MRI has a sensitivity of 96 % for detecting breast cancers. MRI detects multicentric disease with a sensitivity of 98 %, superior to any other modality. The ability of MRI to detect recurrent local breast cancer in the conservatively treated breast is nearly 100 %. MRI is capable of monitoring tumor response to chemotherapy and actually guiding therapeutic interventions such as interstitial laser photocoagulation. (orig.)

  17. Study on the determination of palladium in biological samples by the method of neutron activation analysis

    International Nuclear Information System (INIS)

    Cavalcante, Cassio Queiroz

    2007-01-01

    transferred to polyethylene capsules and analyzed by ENAA. Comparisons of palladium results obtained using different procedures of neutron activations analysis showed good agreement and precision. The relative standard deviations of palladium results varied between 2 and 14 %. The recovery yields obtained in the pre-separation procedure varied from 70.9 to 97.7 %, depending on the matrices analyzed and method of separation. Detection limits of 11.0 and 0.4 μg g-1 were obtained in the Pd determination in bovine muscle samples by INAA and ENAA, respectively. For reference material BCR- 723 road dust detection limits of 24.0 and 1.7 mug g-1 were obtained by INAA and ENAA, respectively. These results indicated that the detection limit depends on the matrix type to be analyzed and the epithermal neutron activation allowed high sensitivity for Pd determination due to the reduction of interferences. In regards to palladium determination using pre-separation procedures, the detection limit values indicated that the extraction procedure provides higher sensitivity, when compared to purely instrumental ENAA. (author)

  18. The detection of metallic residues in skin stab wounds by means of SEM-EDS: A pilot study.

    Science.gov (United States)

    Palazzo, Elisa; Amadasi, Alberto; Boracchi, Michele; Gentile, Guendalina; Maciocco, Francesca; Marchesi, Matteo; Zoja, Riccardo

    2018-05-01

    The morphological analysis of stab wounds may often not be accurate enough to link it with the type of wounding weapon, but a further evaluation may be performed with the search for metallic residues left during the contact between the instrument and the skin. In this study, Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS) was applied to the study of cadaveric stab wounds performed with kitchen knives composed of iron, chromium and nickel, in order to verify the presence of metallic residues on the wound's edge. Two groups of 10 corpses were selected: group A, including victims of stab wounds and a control group B (died of natural causes). Samplings were performed on the lesions and in intact areas of group A, whereas in group B sampling were performed in non-exposed intact skin. Samples were then analysed with optical microscopy and SEM-EDS. In group A, optical microscopic analysis showed the presence of vital haemorrhagic infiltration, while SEM-EDS showed evidence of microscopic metal traces, isolated or clustered, consisting of iron, chromium and nickel. Moreover, in two cases organic residues of calcium and phosphate were detected, as a probable sign of bone lesion. Control samples (group A in intact areas and group B), were negative for the search of exogenous material to optical microscopy and SEM-EDS. The results show the utility and possible application of the SEM-EDS in theidentification of metallic residues from sharp weapons on the skin. Copyright © 2017 The Chartered Society of Forensic Sciences. Published by Elsevier B.V. All rights reserved.

  19. Palladium transport in SiC

    International Nuclear Information System (INIS)

    Olivier, E.J.; Neethling, J.H.

    2012-01-01

    Highlights: ► We investigate the reaction of Pd with SiC at typical HTGR operating temperatures. ► The high temperature mobility of palladium silicides within polycrystalline SiC was studied. ► Corrosion of SiC by Pd was seen in all cases. ► The preferential corrosion and penetration of Pd along grain boundaries in SiC was found. ► The penetration and transport of palladium silicides in SiC along grain boundaries was found. - Abstract: This paper reports on a transmission electron microscopy (TEM) and scanning electron microscopy (SEM) study of Pd corroded SiC. The reaction of Pd with different types of SiC at typical HTGR operating temperatures was examined. In addition the high temperature mobility of palladium silicides within polycrystalline SiC was investigated. The results indicated corrosion of the SiC by Pd in all cases studied. The corrosion leads to the formation of palladium silicides within the SiC, with the predominant phase found being Pd 2 Si. Evidence for the preferential corrosion and penetration of Pd along grain boundaries in polycrystalline SiC was found. The penetration and transport, without significant corrosion, of palladium silicides into polycrystalline SiC along grain boundaries was also observed. Implications of the findings with reference to the use of Tri Isotropic particles in HTGRs will be discussed.

  20. Palladium transport in SiC

    Energy Technology Data Exchange (ETDEWEB)

    Olivier, E.J., E-mail: jolivier@nmmu.ac.za [Centre for High Resolution Transmission Electron Microscopy, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa); Neethling, J.H. [Centre for High Resolution Transmission Electron Microscopy, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa)

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer We investigate the reaction of Pd with SiC at typical HTGR operating temperatures. Black-Right-Pointing-Pointer The high temperature mobility of palladium silicides within polycrystalline SiC was studied. Black-Right-Pointing-Pointer Corrosion of SiC by Pd was seen in all cases. Black-Right-Pointing-Pointer The preferential corrosion and penetration of Pd along grain boundaries in SiC was found. Black-Right-Pointing-Pointer The penetration and transport of palladium silicides in SiC along grain boundaries was found. - Abstract: This paper reports on a transmission electron microscopy (TEM) and scanning electron microscopy (SEM) study of Pd corroded SiC. The reaction of Pd with different types of SiC at typical HTGR operating temperatures was examined. In addition the high temperature mobility of palladium silicides within polycrystalline SiC was investigated. The results indicated corrosion of the SiC by Pd in all cases studied. The corrosion leads to the formation of palladium silicides within the SiC, with the predominant phase found being Pd{sub 2}Si. Evidence for the preferential corrosion and penetration of Pd along grain boundaries in polycrystalline SiC was found. The penetration and transport, without significant corrosion, of palladium silicides into polycrystalline SiC along grain boundaries was also observed. Implications of the findings with reference to the use of Tri Isotropic particles in HTGRs will be discussed.

  1. Contamination Detection and Mitigation Strategies for Unsymmetric Dimethylhydrazine/Nitrogen Tetroxide Non-Combustion Product Residues

    Science.gov (United States)

    Greene, Benjamin; Buchanan, Vanessa D.; Baker, David L.

    2006-01-01

    Dimethylamine and nitrite, which are non-combustion reaction products of unsymmetrical dimethylhydrazine (UDMH) and nitrogen tetroxide (NTO) propellants, can contaminate spacesuits during extra-vehicular activity (EVA) operations. They can react with water in the International Space Station (ISS) airlock to form N-nitrosodimethylamine (NDMA), a carcinogen. Detection methods for assessing nitrite and dimethylamine contamination were investigated. The methods are based on color-forming reactions in which intensity of color is proportional to concentration. A concept color detection kit using a commercially available presumptive field test for methamphetamine coupled with nitrite test strips was developed and used to detect dimethylamine and nitrite. Contamination mitigation strategies were also developed.

  2. Detection of residual disease after neoadjuvant chemoradiotherapy for oesophageal cancer (preSANO): a prospective multicentre, diagnostic cohort study.

    Science.gov (United States)

    Noordman, Bo Jan; Spaander, Manon C W; Valkema, Roelf; Wijnhoven, Bas P L; van Berge Henegouwen, Mark I; Shapiro, Joël; Biermann, Katharina; van der Gaast, Ate; van Hillegersberg, Richard; Hulshof, Maarten C C M; Krishnadath, Kausilia K; Lagarde, Sjoerd M; Nieuwenhuijzen, Grard A P; Oostenbrug, Liekele E; Siersema, Peter D; Schoon, Erik J; Sosef, Meindert N; Steyerberg, Ewout W; van Lanschot, J Jan B

    2018-05-31

    After neoadjuvant chemoradiotherapy for oesophageal cancer, roughly half of the patients with squamous cell carcinoma and a quarter of those with adenocarcinoma have a pathological complete response of the primary tumour before surgery. Thus, the necessity of standard oesophagectomy after neoadjuvant chemoradiotherapy should be reconsidered for patients who respond sufficiently to neoadjuvant treatment. In this study, we aimed to establish the accuracy of detection of residual disease after neoadjuvant chemoradiotherapy with different diagnostic approaches, and the optimal combination of diagnostic techniques for clinical response evaluations. The preSANO trial was a prospective, multicentre, diagnostic cohort study at six centres in the Netherlands. Eligible patients were aged 18 years or older, had histologically proven, resectable, squamous cell carcinoma or adenocarcinoma of the oesophagus or oesophagogastric junction, and were eligible for potential curative therapy with neoadjuvant chemoradiotherapy (five weekly cycles of carboplatin [area under the curve 2 mg/mL per min] plus paclitaxel [50 mg/m 2 of body-surface area] combined with 41·4 Gy radiotherapy in 23 fractions) followed by oesophagectomy. 4-6 weeks after completion of neoadjuvant chemoradiotherapy, patients had oesophagogastroduodenoscopy with biopsies and endoscopic ultrasonography with measurement of maximum tumour thickness. Patients with histologically proven locoregional residual disease or no-pass during endoscopy and without distant metastases underwent immediate surgical resection. In the remaining patients a second clinical response evaluation was done (PET-CT, oesophagogastroduodenoscopy with biopsies, endoscopic ultrasonography with measurement of maximum tumour thickness, and fine-needle aspiration of suspicious lymph nodes), followed by surgery 12-14 weeks after completion of neoadjuvant chemoradiotherapy. The primary endpoint was the correlation between clinical response during

  3. A New On-Line Detecting Apparatus of the Residual Chlorine in Disinfectant for Fresh-Cut Vegetables

    Science.gov (United States)

    Hu, Chao; Su, Shu-Qiang; Li, Bao-Guo; Liu, Meng-Fang

    With the fast development of modern food and beverage industry, fresh-cut vegetables have wider application than before. During the process of sterilization in fresh-cut vegetables, the concentration of chloric disinfectant is usually so high that the common sensor can't be used directly on the product line. In order to solve this problem, we have invented a new detecting apparatus which could detect high concentration of chloric disinfectant directly. In this paper, the working principle, main monitor indicators, application and technical creations of the on-line apparatus have been discussed, and we also carried on the experimental analysis for its performance. The actual demands in factory could be met when the detecting flux is 2L/min, the dilution ratio is 15 and input amount of the disinfectant is 200ml per time, the max of the detecting deviation achieves ±4.8ppm(mg/L). The main detecting range of residual chlorine is 0~300ppm.

  4. Label-free aptamer-based sensor for specific detection of malathion residues by surface-enhanced Raman scattering

    Science.gov (United States)

    Nie, Yonghui; Teng, Yuanjie; Li, Pan; Liu, Wenhan; Shi, Qianwei; Zhang, Yuchao

    2018-02-01

    A novel label-free aptamer surface-enhanced Raman scattering (SERS) sensor for trace malathion residue detection was proposed. In this process, the binding of malathion molecule with aptamer is identified directly. The silver nanoparticles modified with positively charged spermine served as enhancing and capture reagents for the negatively charged aptamer. Then, the silver nanoparticles modified by aptamer were used to specifically capture the malathion. The SERS background spectra of spermine, aptamer, and malathion were recorded and distinguished with the spectrum of malathion-aptamer. To enhance the characteristic peak signal of malathion captured by the aptamer, the aggregate reagents (NaCl, KCl, MgCl2) were compared and selected. The selectivity of this method was verified in the mixed-pesticide standard solution, which included malathion, phosmet, chlorpyrifos-methyl, and fethion. Results show that malathion can be specifically identified when the mixed-pesticide interferences existed. The standard curve was established, presenting a good linear range of 5 × 10- 7 to 1 × 10- 5 mol·L- 1. The spiked experiments for tap water show good recoveries from 87.4% to 110.5% with a relative standard deviation of less than 4.22%. Therefore, the proposed label-free aptamer SERS sensor is convenient, specifically detects trace malathion residues, and can be applied for qualitative and quantitative analysis of other pesticides.

  5. Immunology-Based Techniques for the Detection of Veterinary Drug Residues in Foods

    Science.gov (United States)

    Reig, Milagro; Toldrá, Fidel

    Veterinary drugs are used in farm animals, via the feed or the drinking water, to prevent the outbreak of diseases or even for the treatment of diseases. However, the growth of animals may be promoted through the use of hormones and antibiotics. Depending on the type of residue and the application and washing conditions, these substances or its metabolites may remain in meat and other foods of animal origin and may cause adverse effects on consumers’ health. This is the main reason why its use is strictly regulated or even banned (case of the European Union) in different countries. Antibiotics typically used for growth promotion include chloramphenicol, nitrofurans, and enrofloxacin but others like sulphonamides, macrolides etc. may also be used (Reig & Toldrá, 2007).

  6. Preliminary results for the detection method of perfluoroalkyl substances (PFASs residues in pork

    Directory of Open Access Journals (Sweden)

    Shih-kuo Lin

    2017-05-01

    Full Text Available The perfluoroalkyl substances (PFASs residues, which come from environmental pollution, tend to accumulate in the food chain (EFSA, 2008; Guerranti et al., 2013. 17 chemicals of PFASs family were selected for this study. Fresh pork samples were extracted by Waters® WAX SPE (solid phase extraction cartridges. All extracted samples were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS. The results of calibration curves of each PFAS were good, the R2 values ranging from 0.9901 to 0.9993. The Recoveries were in the range 80%-119%. The protocol of extraction by Waters® WAX SPE cartridge will be applied in future studies.

  7. Hydrogen sensor based on palladium-yttrium alloy nanosheet

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Boyi [Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan, QLD 4111 (Australia); Zhu, Yong, E-mail: y.zhu@griffith.edu.au [Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan, QLD 4111 (Australia); Chen, Youping; Song, Han; Huang, Pengcheng [School of Mechanical Science and Engineering, Huazhong University of Science and Technology, Wuhan, 430074 (China); Dao, Dzung Viet [Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan, QLD 4111 (Australia)

    2017-06-15

    This paper presents a hydrogen sensor based on palladium-yttrium (Pd-Y) alloy nanosheet. Zigzag-shaped Pd-Y nanosheet with a thickness of 19.3 nm was deposited on a quartz substrate by using an ultrahigh-vacuum magnetron sputtering system and shadow mask. The atomic ratio of palladium to yttrium in the nanosheet was 0.92/0.08. The fabrication process was simple and low-cost, and the sensor can be mass-produced. The experimental results show the sensor has a superior sensitivity, reversibility, and reproducibility. The resistive-based hydrogen detection mechanism in this research is much simpler and more compact compared to the optical-based detection method. - Highlights: • Pd-Y sensing element was fabricated using a magnetron sputtering system and shadow mask. • The Pd-Y compound consisted of 92% Pd and 8% Y. • The fabrication process was simple, low-cost, and mass-production compatible. • The sensor showed superior sensitivity, reversibility, and reproducibility to hydrogen gas. • The device is more compact than the optical-based counterpart.

  8. Hydrogen sensor based on palladium-yttrium alloy nanosheet

    International Nuclear Information System (INIS)

    Wang, Boyi; Zhu, Yong; Chen, Youping; Song, Han; Huang, Pengcheng; Dao, Dzung Viet

    2017-01-01

    This paper presents a hydrogen sensor based on palladium-yttrium (Pd-Y) alloy nanosheet. Zigzag-shaped Pd-Y nanosheet with a thickness of 19.3 nm was deposited on a quartz substrate by using an ultrahigh-vacuum magnetron sputtering system and shadow mask. The atomic ratio of palladium to yttrium in the nanosheet was 0.92/0.08. The fabrication process was simple and low-cost, and the sensor can be mass-produced. The experimental results show the sensor has a superior sensitivity, reversibility, and reproducibility. The resistive-based hydrogen detection mechanism in this research is much simpler and more compact compared to the optical-based detection method. - Highlights: • Pd-Y sensing element was fabricated using a magnetron sputtering system and shadow mask. • The Pd-Y compound consisted of 92% Pd and 8% Y. • The fabrication process was simple, low-cost, and mass-production compatible. • The sensor showed superior sensitivity, reversibility, and reproducibility to hydrogen gas. • The device is more compact than the optical-based counterpart.

  9. Californium Recovery from Palladium Wire

    Energy Technology Data Exchange (ETDEWEB)

    Burns, Jon D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2014-08-01

    The recovery of 252Cf from palladium-252Cf cermet wires was investigated to determine the feasibility of implementing it into the cermet wire production operation at Oak Ridge National Laboratory’s Radiochemical Engineering Development Center. The dissolution of Pd wire in 8 M HNO3 and trace amounts of HCl was studied at both ambient and elevated temperatures. These studies showed that it took days to dissolve the wire at ambient temperature and only 2 hours at 60°C. Adjusting the ratio of the volume of solvent to the mass of the wire segment showed little change in the kinetics of dissolution, which ranged from 0.176 mL/mg down to 0.019 mL/mg. A successful chromatographic separation of 153Gd, a surrogate for 252Cf, from Pd was demonstrated using AG 50x8 cation exchange resin with a bed volume of 0.5 mL and an internal diameter of 0.8 cm.

  10. The Effect of Different Methods of Fermentation on the Detection of Milk Protein Residues in Retail Cheese by Enzyme-Linked Immunosorbent Assay (ELISA).

    Science.gov (United States)

    Ivens, Katherine O; Baumert, Joseph L; Hutkins, Robert L; Taylor, Steve L

    2017-11-01

    Milk and milk products are among the most important allergenic food ingredients, both in the United States and throughout the world; cheeses are among the most important of these milk products. Milk contains several major antigenic proteins, each with differing susceptibilities to proteolytic enzymes. The extent of proteolysis in cheese varies as a result of conditions during manufacture and ripening. Proteolysis has the potential to degrade antigenic and allergenic epitopes that are important for residue detection and elicitation of allergic reactions. Commercial enzyme-linked immunosorbent assays (ELISAs) are not currently validated for use in detecting residues in hydrolyzed or fermented food products. Eighteen retail cheeses produced using 5 different styles of fermentation were investigated for detectable milk protein residues with 4 commercial ELISA kits. Mozzarella, Swiss, Blue, Limburger, and Brie cheeses were assessed. The Neogen Veratox® Casein and Neogen Veratox® Total Milk kits were capable of detecting milk residues in most cheeses evaluated, including blue-veined cheeses that exhibit extensive proteolysis. The other 2 ELISA kits evaluated, r-Biopharm® Fast Casein and ELISA Systems™ Casein, can detect milk residues in cheeses other than blue-veined varieties. ELISA results cannot be quantitatively compared among kits. The quantitative reliability of ELISA results in detection of cheese residues is questionable, but some methods are sufficiently robust to use as a semi-quantitative indication of proper allergen control for the validation of cleaning programs in industry settings. Many commercially available enzyme-linked immunosorbent assays (ELISAs) are not validated for detection of allergenic residues in fermented or hydrolyzed products. This research seeks to determine if commercial milk ELISAs can detect milk residues in varieties of cheese that have undergone different styles of fermentation and different degrees of proteolysis. Only certain

  11. Silver-Palladium Surfaces Inhibit Biofilm Formation

    DEFF Research Database (Denmark)

    Chiang, Wen-Chi; Schroll, Casper; Hilbert, Lisbeth Rischel

    2009-01-01

    Undesired biofilm formation is a major concern in many areas. In the present study, we investigated biofilm-inhibiting properties of a silver-palladium surface that kills bacteria by generating microelectric fields and electrochemical redox processes. For evaluation of the biofilm inhibition...... efficacy and study of the biofilm inhibition mechanism, the silver-sensitive Escherichia coli J53 and the silver-resistant E. coli J53[pMG101] strains were used as model organisms, and batch and flow chamber setups were used as model systems. In the case of the silver-sensitive strain, the silver......-palladium surfaces killed the bacteria and prevented biofilm formation under conditions of low or high bacterial load. In the case of the silver-resistant strain, the silver-palladium surfaces killed surface-associated bacteria and prevented biofilm formation under conditions of low bacterial load, whereas under...

  12. P-aminobenzoic acid and tritiated cyanoborohydride for the detection of pyruvoyl residues in proteins

    International Nuclear Information System (INIS)

    van Poelje, P.D.; Snell, E.E.

    1987-01-01

    A procedure for the detection of covalently bound pyruvic acid in purified proteins or in crude extracts is described. The dialyzed sample is first treated with sodium cyanoborohydride to reduce any Schiff bases present and then incubated with p-aminobenzoic acid and sodium [ 3 H]cyanoborohydride. Derivatized proteins are visualized by fluorography following sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Gel slices containing the labeled proteins are hydrolyzed, and, after removal of polyacrylic acid, the hydrolysate is subjected to ion-exchange high-performance liquid chromatography. The presence of pyruvic acid is established by the detection of a tritiated, 280-nm absorbing compound with a retention time corresponding to that of synthetic N-(p-carboxyphenyl)alanine. The procedure is capable of detecting protein-bound pyruvic acid in the picomolar range and is easily modified to screen for other covalently bound keto acids

  13. Comparative analysis of minimal residual disease detection by multiparameter flow cytometry and enhanced ASO RQ-PCR in multiple myeloma

    International Nuclear Information System (INIS)

    Silvennoinen, R; Lundan, T; Kairisto, V; Pelliniemi, T-T; Putkonen, M; Anttila, P; Huotari, V; Mäntymaa, P; Siitonen, S; Uotila, L; Penttilä, T-L; Juvonen, V; Selander, T; Remes, K

    2014-01-01

    Multiparameter flow cytometry (MFC) and allele-specific oligonucleotide real-time quantitative PCR (ASO RQ-PCR) are the two most sensitive methods to detect minimal residual disease (MRD) in multiple myeloma (MM). We compared these methods in 129 paired post-therapy samples from 22 unselected, consecutive MM patients in complete/near complete remission. Appropriate immunophenotypic and ASO RQ-PCR-MRD targets could be detected and MRD analyses constructed for all patients. The high PCR coverage could be achieved by gradual widening of the primer sets used for clonality detection. In addition, for 13 (55%) of the patients, reverse orientation of the ASO primer and individual design of the TaqMan probe improved the sensitivity and specificity of ASO RQ-PCR analysis. A significant nonlinear correlation prevailed between MFC-MRD and PCR-MRD when both were positive. Discordance between the methods was found in 32 (35%) paired samples, which were negative by MFC-MRD, but positive by ASO RQ-PCR. The findings suggest that with the described technique, ASO RQ-PCR can be constructed for all patients with MM. ASO RQ-PCR is slightly more sensitive in MRD detection than 6−10-color flow cytometry. Owing to technical demands ASO RQ-PCR could be reserved for patients in immunophenotypic remission, especially in efficacy comparisons between different drugs and treatment modalities

  14. Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorus detection

    NARCIS (Netherlands)

    Brinkman, J.H.W.; Dijk, A.G. van; Wagenaar, R.; Quirijns, J.K.

    1996-01-01

    A method was developed for the determination of daminozide in apples using gas chromatography (GC) with nitrogen-phosphorus detection (NPD). Daminozide is hydrolysed to 1,1-dimethylhydrazine (UDMH) by alkaline digestion. The UDMH generated is distilled from the apple matrix, derivatized with

  15. Detection of fecal residue on poultry carcasses by laser induced fluorescence imaging techniques

    Science.gov (United States)

    The potential use of laser-induced fluorescence imaging techniques was investigated for the detection of diluted fecal matters from various parts of the digestive tract, including colon, ceca, small intestine, and duodenum, on poultry carcasses. One of the challenges for using fluorescence imaging f...

  16. Continued development of a portable widefield hyperspectral imaging (HSI) sensor for standoff detection of explosive, chemical, and narcotic residues

    Science.gov (United States)

    Nelson, Matthew P.; Gardner, Charles W.; Klueva, Oksana; Tomas, David

    2014-05-01

    Passive, standoff detection of chemical, explosive and narcotic threats employing widefield, shortwave infrared (SWIR) hyperspectral imaging (HSI) continues to gain acceptance in defense and security fields. A robust and user-friendly portable platform with such capabilities increases the effectiveness of locating and identifying threats while reducing risks to personnel. In 2013 ChemImage Sensor Systems (CISS) introduced Aperio, a handheld sensor, using real-time SWIR HSI for wide area surveillance and standoff detection of explosives, chemical threats, and narcotics. That SWIR HSI system employed a liquid-crystal tunable filter for real-time automated detection and display of threats. In these proceedings, we report on a next generation device called VeroVision™, which incorporates an improved optical design that enhances detection performance at greater standoff distances with increased sensitivity and detection speed. A tripod mounted sensor head unit (SHU) with an optional motorized pan-tilt unit (PTU) is available for precision pointing and sensor stabilization. This option supports longer standoff range applications which are often seen at checkpoint vehicle inspection where speed and precision is necessary. Basic software has been extended to include advanced algorithms providing multi-target display functionality, automatic threshold determination, and an automated detection recipe capability for expanding the library as new threats emerge. In these proceedings, we report on the improvements associated with the next generation portable widefield SWIR HSI sensor, VeroVision™. Test data collected during development are presented in this report which supports the targeted applications for use of VeroVision™ for screening residue and bulk levels of explosive and drugs on vehicles and personnel at checkpoints as well as various applications for other secure areas. Additionally, we highlight a forensic application of the technology for assisting forensic

  17. Laser methods for detecting explosive residues on surfaces of distant objects

    Energy Technology Data Exchange (ETDEWEB)

    Skvortsov, L A [Institute of Cryptography, Communications and Informatics, Moscow (Russian Federation)

    2012-01-31

    The basic methods of laser spectroscopy that are used for standoff detection and identification of explosive traces in the form of particles on the surfaces of objects tested under real or close-toreal conditions are briefly considered. The advantages and drawbacks of all methods are discussed and their characteristics are compared. Particular attention has been given to the prospects of development and practical implementation of the technologies discussed and justification of their most preferred applications. (review)

  18. Screening method for detecting cross-contamination residues of tiamulin in swine feeds.

    Science.gov (United States)

    Rodríguez-Comesaña, Mirian; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2003-01-01

    A method was developed for the determination of tiamulin (TML), 14-deoxy-14-[(2-diethylaminoethyl)mercaptoacetoxy]mutilin hydrogen fumarate, a semisynthetic derivative of the naturally occurring antibiotic pleuromutilin produced by the fungus Pleurotus mutilis. This drug, with high activity against Gram-positive bacteria, some Gram-negative bacteria, and several strains of mycoplasms is administered to animals in food, drinking water, or by injection; however, its chemical structure causes problems in analysis of feeds. Although the molecule is charged below pH 8, attempts to analyze TML-containing extracts on ion-exchange columns or other polar stationary phases have failed. Additionally, TML shows no fluorescence activity and only poor UV activity. The present method consists of organic solvent extraction followed by liquid chromatography with UV detection. A low wavelength (208 nm) was used for detection. Limits of detection and quantitation, as well as data for recovery and repeatability obtained during characterization of the method, are described. The applicability of the optimized method was tested by analyzing commercial blank feeds processed after TML-medicated feeds.

  19. System for the chemical professing and evaluation gives the residual thickness the gives detecting for gives appearances LR115 type 2

    International Nuclear Information System (INIS)

    Carrazana Gonzalez, J.A.; Tomas Zerquera, J.; Prendes Alonso, M.

    1998-01-01

    In this work the system is described built in the CPHR for the homogeneous chemical processing gives detecting gives nuclear appearances. A new developed method is exposed, based on the application gives the technique optical densitometry, for the precise estimate gives the residual thickness, gives detecting, gives nuclear appearances LR115 type 2 after the process gives chemical engraving

  20. Minimal Residual Disease Detection and Evolved IGH Clones Analysis in Acute B Lymphoblastic Leukemia Using IGH Deep Sequencing.

    Science.gov (United States)

    Wu, Jinghua; Jia, Shan; Wang, Changxi; Zhang, Wei; Liu, Sixi; Zeng, Xiaojing; Mai, Huirong; Yuan, Xiuli; Du, Yuanping; Wang, Xiaodong; Hong, Xueyu; Li, Xuemei; Wen, Feiqiu; Xu, Xun; Pan, Jianhua; Li, Changgang; Liu, Xiao

    2016-01-01

    Acute B lymphoblastic leukemia (B-ALL) is one of the most common types of childhood cancer worldwide and chemotherapy is the main treatment approach. Despite good response rates to chemotherapy regiments, many patients eventually relapse and minimal residual disease (MRD) is the leading risk factor for relapse. The evolution of leukemic clones during disease development and treatment may have clinical significance. In this study, we performed immunoglobulin heavy chain ( IGH ) repertoire high throughput sequencing (HTS) on the diagnostic and post-treatment samples of 51 pediatric B-ALL patients. We identified leukemic IGH clones in 92.2% of the diagnostic samples and nearly half of the patients were polyclonal. About one-third of the leukemic clones have correct open reading frame in the complementarity determining region 3 (CDR3) of IGH , which demonstrates that the leukemic B cells were in the early developmental stage. We also demonstrated the higher sensitivity of HTS in MRD detection and investigated the clinical value of using peripheral blood in MRD detection and monitoring the clonal IGH evolution. In addition, we found leukemic clones were extensively undergoing continuous clonal IGH evolution by variable gene replacement. Dynamic frequency change and newly emerged evolved IGH clones were identified upon the pressure of chemotherapy. In summary, we confirmed the high sensitivity and universal applicability of HTS in MRD detection. We also reported the ubiquitous evolved IGH clones in B-ALL samples and their response to chemotherapy during treatment.

  1. Determination of benzimidazole residues and their metabolites in raw milk using high performance liquid chromatography-diode array detection

    Directory of Open Access Journals (Sweden)

    Marija Denžić Lugomer

    2017-01-01

    Full Text Available A new analytical method using high performance liquid chromatography-diode array detector (HPLC-DAD was developed for the analysis of 18 benzimidazoles and their metabolites in milk. Samples were extracted with acetonitrile and n-hexane and purified by polymer cation exchange (PCX solid phase extraction cartridges. LC separation was performed on Xbridge C18 with gradient elution using acetonitrile and ammonium acetate buffer. The DAD detection was set at 298, 312, 254 and 290 nm. The method was validated according to the criteria of Commission Decision 2002/657/EC. The following validation parameters were set: accuracy (expressed as recovery 31.7-137.6 %, limit of decision (CCα 6.0-120.6 μg kg-1, detection capability (CCβ 6.1-120.8 μg kg-1, limit of detection (LOD 1-4 μg kg-1, limit of quantification (LOQ 4-18 μg kg-1, precision as CV 7.0-22.5 %, withinlaboratory reproducibility expressed as CV 8.8-30.6 %. Finally, the developed method was applied to the analysis of collected milk samples. A total of 50 milk samples was analysed for benzimidazole residues. All obtained concentrations for all compounds were below the LOQ values.

  2. Production of a monoclonal antibody against oxytetracycline and its application for oxytetracycline residue detection in shrimp*

    Science.gov (United States)

    Wongtangprasert, Tossapon; Natakuathung, Wirongrong; Pimpitak, Umaporn; Buakeaw, Anumart; Palaga, Tanapat; Komolpis, Kittinan; Khongchareonporn, Nanthika

    2014-01-01

    A novel monoclonal antibody (MAb) against oxytetracycline (OTC) was generated and characterized. The MAb was used in the development of an enzyme-linked immunosorbant assay (ELISA)-based detection system. An OTC-bovine serum albumin (BSA) conjugate was prepared and used in the immunization of mice. A conventional somatic cell fusion technique was used to generate MAb-secreting hybridomas denoted 2-4F, 7-3G, and 11-11A. An indirect competitive ELISA (icELISA) was applied to measure the sensitivity and specificity of each MAb in terms of its 50% inhibitory concentration (IC50) and percentage of cross-reactivity, respectively. MAb 2-4F exhibited the highest sensitivity, with an IC50 of 7.01 ng/ml. This MAb showed strong cross-reactivity to rolitetracycline, but no cross-reactivity to other unrelated antibiotics. When MAb 2-4F was used to detect OTC from shrimp samples, the recoveries were in the range of 82%–118% for an intra-assay and 96%–113% for an inter-assay. The coefficients of variation of the assays were 3.9%–13.9% and 5.5%–14.9%, respectively. PMID:24510709

  3. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    International Nuclear Information System (INIS)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Brozek-Mucha, Z.; Biegstraaten, J.; Horvath, R.

    2007-01-01

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification

  4. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Steffen, S. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Otto, M. [TU Bergakademie Freiberg (TU BAF), Institute for Analytical Chemistry, Leipziger Str. 29, D - 09599 Freiberg (Germany)], E-mail: matthias.otto@chemie.tu-freiberg.de; Niewoehner, L.; Barth, M. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Brozek-Mucha, Z. [Instytut Ekspertyz Sadowych (IES), Westerplatte St. 9, PL - 31-033 Krakow (Poland); Biegstraaten, J. [Nederlands Forensisch Instituut (NFI), Fysische Technologie, Laan van Ypenburg 6, NL-2497 GB Den Haag (Netherlands); Horvath, R. [Kriminalisticky a Expertizny Ustav (KEU PZ), Institute of Forensic Science, Sklabinska 1, SK - 812 72 Bratislava (Slovakia)

    2007-09-15

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  5. Palladium-Catalyzed Asymmetric Quaternary Stereocenter Formation

    NARCIS (Netherlands)

    Gottumukkala, Aditya L.; Matcha, Kiran; Lutz, Martin; de Vries, Johannes G.; Minnaard, Adriaan J.

    2012-01-01

    An efficient palladium catalyst is presented for the formation of benzylic quaternary stereocenters by conjugate addition of arylboronic acids to a variety of beta,beta-disubstituted carbocyclic, heterocyclic, and acyclic enones. The catalyst is readily prepared from PdCl2, PhBOX, and AgSbF6, and

  6. Palladium-catalyzed asymmetric quaternary stereocenter formation

    NARCIS (Netherlands)

    Gottumukkala, A.L.; Matcha, K.; Lutz, M.; de Vries, J.G.; Minnaard, A.J.

    2012-01-01

    An efficient palladium catalyst is presented for the formation of benzylic quaternary stereocenters by conjugate addition of arylboronic acids to a variety of β,β-disubstituted carbocyclic, heterocyclic, and acyclic enones. The catalyst is readily prepared from PdCl2, PhBOX, and AgSbF6, and provides

  7. Confocal detection of Rayleigh scattering for residual stress measurement in chemically tempered glass

    Energy Technology Data Exchange (ETDEWEB)

    Hödemann, S., E-mail: siim.hodemann@ut.ee; Möls, P.; Kiisk, V.; Saar, R.; Kikas, J. [Institute of Physics, University of Tartu, Wilhelm Ostwald st., Tartu 50411 (Estonia); Murata, T. [Nippon Electric Glass Co., 7-1 Seiran 2-chome, Otsu-shi, Shiga 520-8639 (Japan)

    2015-12-28

    A new optical method is presented for evaluation of the stress profile in chemically tempered (chemically strengthened) glass based on confocal detection of scattered laser beam. Theoretically, a lateral resolution of 0.2 μm and a depth resolution of 0.6 μm could be achieved by using a confocal microscope with high-NA immersion objective. The stress profile in the 250 μm thick surface layer of chemically tempered lithium aluminosilicate glass was measured with a high spatial resolution to illustrate the capability of the method. The confocal method is validated using transmission photoelastic and Na{sup +} ion concentration profile measurement. Compositional influence on the stress-optic coefficient is calculated and discussed. Our method opens up new possibilities for three-dimensional scattered light tomography of mechanical imaging in birefringent materials.

  8. Digital PCR analysis of circulating tumor DNA: a biomarker for chondrosarcoma diagnosis, prognostication, and residual disease detection.

    Science.gov (United States)

    Gutteridge, Alice; Rathbone, Victoria M; Gibbons, Rebecca; Bi, Mark; Archard, Nicholas; Davies, Kate E J; Brown, Jake; Plagnol, Vincent; Pillay, Nischalan; Amary, Fernanda; O'Donnell, Paul; Gupta, Manu; Tirabosco, Roberto; Flanagan, Adrienne M; Forshew, Tim

    2017-10-01

    Conventional chondrosarcoma is the most common primary bone tumor in adults. Prognosis corresponds with tumor grade but remains variable, especially for individuals with grade (G) II disease. There are currently no biomarkers available for monitoring or prognostication of chondrosarcoma. Circulating tumor DNA (ctDNA) has recently emerged as a promising biomarker for a broad range of tumor types. To date, little has been done to study the presence of ctDNA and its potential utility in the management of sarcomas, including chondrosarcoma. In this study, we have assessed ctDNA levels in a cohort of 71 patients, 32 with sarcoma, including 29 individuals with central chondrosarcoma (CS) and 39 with locally aggressive and benign bone and soft tissue tumors, using digital PCR. In patients with CS, ctDNA was detected in pretreatment samples in 14/29 patients, which showed clear correlation with tumor grade as demonstrated by the detection of ctDNA in all patients with GIII and dedifferentiated disease (n = 6) and in 8/17 patients with GII disease, but never associated with GI CS. Notably detection of ctDNA preoperatively in GII disease was associated with a poor outcome. A total of 14 patients with CS had ctDNA levels assessed at multiple time points and in most patients there was a clear reduction following surgical removal. This research lays the foundation for larger studies to assess the utility of ctDNA for chondrosarcoma diagnosis, prognostication, early detection of residual disease and monitoring disease progression. © 2017 The Authors. Cancer Medicine published by John Wiley & Sons Ltd.

  9. Detection of Residual Levels and Associated Health Risk of Seven Pesticides in Fresh Eggplant and Tomato Samples from Narayanganj District, Bangladesh

    Directory of Open Access Journals (Sweden)

    Md. Nur Alam

    2015-01-01

    Full Text Available Residual levels of seven frequently used pesticides were investigated in 140 samples of two common vegetables, eggplants and tomatoes, from agricultural fields in the Narayanganj district of Bangladesh. The analysis of pesticide residues was performed by high-performance liquid chromatography with photodiode array detection. A large percentage of the eggplants (50% and tomatoes (60% from the Narayanganj district were contaminated with pesticides, and all of the levels were above the maximum residual limit (MRL proposed by the EC regulation. Diazinon was the most common (35% pesticide detected in the vegetable samples at a concentration of 45–450 times higher than the MRL. The health risk index for diazinon was highest for both eggplant and tomato samples, which may be due to its physiochemical properties. Fenitrothion and linuron are the two second most common types of pesticides detected in the vegetable samples. Regular monitoring of the use of common pesticides on vegetables should be conducted.

  10. Construction of genetically engineered bacteria that degrades organophosphorus pesticide residues and can be easily detected by the fluorescence.

    Science.gov (United States)

    Li, Qin; Wang, Pan; Chen, Rui; Li, Wei; Wu, Yi-Jun

    2014-01-01

    Organophosphorus compounds (OPs) are widely used in agriculture and industry and there is increased concern about their toxicological effects in the environment. Bioremediation can offer an efficient and cost-effective option for the removal of OPs. Herein, we describe the construction of a genetically engineered microorganism (GEM) that can degrade OPs and be directly detected and monitored in the environment using an enhanced green fluorescent protein (EGFP) fusion strategy. The coding regions of EGFP, a reporter protein that can fluoresce by itself, and organophosphorus hydrolase (OPH), which has a broad substrate specificity and is able to hydrolyse a number of organophosphorus pesticides, were cloned into the expression vector pET-28b. The fusion protein of EGFP-OPH was expressed in E. coli BL21 (DE3) and the protein expression reached the highest level at 11 h after isopropyl beta-D-thiogalactopyranoside induction. The fluorescence of the GEM was detected by fluorescence spectrophotometry and microscopy, and its ability to degrade OPs was determined by OPH activity assay. Those GEM that express the fusion protein (EGFP and OPH) exhibited strong fluorescence intensity and also potent hydrolase activity, which could be used to degrade organophosphorus pesticide residues in the environment and can also be directly monitored by fluorescence.

  11. Early detection of tumor relapse/regrowth by consecutive minimal residual disease monitoring in high-risk neuroblastoma patients

    Science.gov (United States)

    Hirase, Satoshi; Saitoh, Atsuro; Hartomo, Tri Budi; Kozaki, Aiko; Yanai, Tomoko; Hasegawa, Daiichiro; Kawasaki, Keiichiro; Kosaka, Yoshiyuki; Matsuo, Masafumi; Yamamoto, Nobuyuki; Mori, Takeshi; Hayakawa, Akira; Iijima, Kazumoto; Nishio, Hisahide; Nishimura, Noriyuki

    2016-01-01

    Neuroblastoma is an aggressive pediatric tumor accounting for ~15% of cancer-associated mortalities in children. Despite the current intensive therapy, >50% of high-risk patients experience tumor relapse or regrowth caused by the activation of minimal residual disease (MRD). Although several MRD detection protocols using various reverse transcription-quantitative polymerase chain reaction (RT-qPCR) markers have been reported to evaluate the therapeutic response and disease status of neuroblastoma patients, their clinical significance remains elusive. The present study reports two high-risk neuroblastoma patients, whose MRD was consecutively monitored using 11 RT-qPCR markers (CHRNA3, CRMP1, DBH, DCX, DDC, GABRB3, GAP43, ISL1, KIF1A, PHOX2B and TH) during their course of treatment. The two patients initially responded to the induction therapy and reached MRD-negative status. The patients' MRD subsequently became positive with no elevation of their urinary homovanillic acid, urinary vanillylmandelic acid and serum neuron-specific enolase levels at 13 or 19 weeks prior to the clinical diagnosis of tumor relapse or regrowth. The present cases highlight the possibility of consecutive MRD monitoring using 11 markers to enable an early detection of tumor relapse or regrowth in high-risk neuroblastoma patients. PMID:27446404

  12. Detection of pyridaben residue levels in hot pepper fruit and leaves by liquid chromatography-tandem mass spectrometry: effect of household processes.

    Science.gov (United States)

    Kim, Sung-Woo; Abd El-Aty, A M; Rahman, Md Musfiqur; Choi, Jeong-Heui; Choi, Ok-Ja; Rhee, Gyu-Seek; Chang, Moon-Ik; Kim, Heejung; Abid, Morad D N; Shin, Sung Chul; Shim, Jae-Han

    2015-07-01

    Following quick, easy, cheap, effective, rugged and safe (QuEChERS) and LC/MS/MS analysis, pyridaben residual levels were determined in unprocessed and processed hot pepper fruit and leaves. The linearities were satisfactory with determination coefficients (R(2)) in excess of 0.995 in processed and unprocessed pepper fruit and leaves. Recoveries at various concentrations were 79.9-105.1% with relative standard deviations ≤15%. The limits of quantitation of 0.003-0.012 mg/kg were very low compared with the maximum residue limits (2-5 mg/kg) set by the Ministry of Food and Drug Safety, Republic of Korea. The effects of various household processes, including washing, blanching, frying and drying under different conditions (water volume, blanching time and temperature) on residual concentrations were evaluated. Both washing and blanching (in combination with high water volume and time factor) significantly reduced residue levels in hot pepper fruit and leaves compared with other processes. In sum, the developed method was satisfactory and could be used to accurately detect residues in unprocessed and processed pepper fruit and leaves. It is recommended that pepper fruit/leaves be blanched after washing before being consumed to protect consumers from the negative health effects of detected pesticide residues. Copyright © 2014 John Wiley & Sons, Ltd.

  13. Palladium(II)-catalyzed desulfitative synthesis of aryl ketones from sodium arylsulfinates and nitriles: scope, limitations, and mechanistic studies.

    Science.gov (United States)

    Skillinghaug, Bobo; Sköld, Christian; Rydfjord, Jonas; Svensson, Fredrik; Behrends, Malte; Sävmarker, Jonas; Sjöberg, Per J R; Larhed, Mats

    2014-12-19

    A fast and efficient protocol for the palladium(II)-catalyzed production of aryl ketones from sodium arylsulfinates and various organic nitriles under controlled microwave irradiation has been developed. The wide scope of the reaction has been demonstrated by combining 14 sodium arylsulfinates and 21 nitriles to give 55 examples of aryl ketones. One additional example illustrated that, through the choice of the nitrile reactant, benzofurans are also accessible. The reaction mechanism was investigated by electrospray ionization mass spectrometry and DFT calculations. The desulfitative synthesis of aryl ketones from nitriles was also compared to the corresponding transformation starting from benzoic acids. Comparison of the energy profiles indicates that the free energy requirement for decarboxylation of 2,6-dimethoxybenzoic acid and especially benzoic acid is higher than the corresponding desulfitative process for generating the key aryl palladium intermediate. The palladium(II) intermediates detected by ESI-MS and the DFT calculations provide a detailed understanding of the catalytic cycle.

  14. Dendritic surface morphology of palladium hydride produced by electrolytic deposition

    International Nuclear Information System (INIS)

    Julin, Peng; Bursill, L.A.

    1990-01-01

    Conventional and high-resolution electron microscopic studies of electrolytically-deposited palladium hydride reveal a fascinating variety of surface profile morphologies. The observations provide direct information concerning the surface structure of palladium electrodes and the mechanism of electrolytic deposition of palladium black. Both classical electrochemical mechanisms and recent 'modified diffusion-limited-aggregation' computer simulations are discussed in comparison with the experimental results. 13 refs., 9 figs

  15. Trace analysis of multi-class pesticide residues in Chinese medicinal health wines using gas chromatography with electron capture detection

    Science.gov (United States)

    Kong, Wei-Jun; Liu, Qiu-Tao; Kong, Dan-Dan; Liu, Qian-Zhen; Ma, Xin-Ping; Yang, Mei-Hua

    2016-02-01

    A method is described for multi-residue, high-throughput determination of trace levels of 22 organochlorine pesticides (OCPs) and 5 pyrethroid pesticides (PYPs) in Chinese medicinal (CM) health wines using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) based extraction method and gas chromatography-electron capture detection (GC-ECD). Several parameters were optimized to improve preparation and separation time while still maintaining high sensitivity. Validation tests of spiked samples showed good linearities for 27 pesticides (R = 0.9909-0.9996) over wide concentration ranges. Limits of detection (LODs) and quantification (LOQs) were measured at ng/L levels, 0.06-2 ng/L and 0.2-6 ng/L for OCPs and 0.02-3 ng/L and 0.06-7 ng/L for PYPs, respectively. Inter- and intra-day precision tests showed variations of 0.65-9.89% for OCPs and 0.98-13.99% for PYPs, respectively. Average recoveries were in the range of 47.74-120.31%, with relative standard deviations below 20%. The developed method was then applied to analyze 80 CM wine samples. Beta-BHC (Benzene hexachloride) was the most frequently detected pesticide at concentration levels of 5.67-31.55 mg/L, followed by delta-BHC, trans-chlordane, gamma-BHC, and alpha-BHC. The validated method is simple and economical, with adequate sensitivity for trace levels of multi-class pesticides. It could be adopted by laboratories for this and other types of complex matrices analysis.

  16. Adding Endoscopist-Directed Flexible Endoscopic Evaluation of Swallowing to the Videofluoroscopic Swallowing Study Increased the Detection Rates of Penetration, Aspiration, and Pharyngeal Residue.

    Science.gov (United States)

    Park, Won Young; Lee, Tae Hee; Ham, Nam Seok; Park, Ji Woong; Lee, Yang Gyun; Cho, Sang Jin; Lee, Joon Seong; Hong, Su Jin; Jeon, Seong Ran; Kim, Hyun Gun; Cho, Joo Young; Kim, Jin Oh; Cho, Jun Hyung; Lee, Ji Sung

    2015-09-23

    Currently, the videofluoroscopic swallowing study (VFSS) is the standard tool for evaluating dysphagia. We evaluated whether the addition of endoscopist-directed flexible endoscopic evaluation of swallowing (FEES) to VFSS could improve the detection rates of penetration, aspiration, and pharyngeal residue, compared the diagnostic efficacy between VFSS and endoscopist-directed FEES and assessed the adverse events of the FEES. In single tertiary referral center, a retrospective analysis of prospectively collected data was conducted. Fifty consecutive patients suspected of oropharyngeal dysphagia were enrolled in this study between January 2012 and July 2012. The agreement in the detection of penetration and aspiration between VFSS and FEES of viscous food (κ=0.34; 95% confidence interval [CI], 0.15 to 0.53) and liquid food (κ=0.22; 95% CI, 0.02 to 0.42) was "fair." The agreement in the detection of pharyngeal residue between the two tests was "substantial" with viscous food (κ=0.63; 95% CI, 0.41 to 0.94) and "fair" with liquid food (κ=0.37; 95% CI, 0.10 to 0.63). Adding FEES to VFSS significantly increased the detection rates of penetration, aspiration, and pharyngeal residue. No severe adverse events were noted during FEES, except for two cases of epistaxis, which stopped spontaneously without requiring any packing. This study demonstrated that the addition of endoscopist-directed FEES to VFSS increased the detection rates of penetration, aspiration, and pharyngeal residue.

  17. Culture-Independent Techniques for Rapid Detection of Bacteria Associated with Loss of Chloramine Residual in a Drinking Water System

    Science.gov (United States)

    Hoefel, Daniel; Monis, Paul T.; Grooby, Warwick L.; Andrews, Stuart; Saint, Christopher P.

    2005-01-01

    Chloramination is often the disinfection regimen of choice for extended drinking water systems. However, this process is prone to instability due to the growth of nitrifying bacteria. This is the first study to use alternative approaches for rapid investigation of chloraminated drinking water system instability in which flow cytometric cell sorting of bacteria with intact membranes (membrane-intact fraction) (BacLight kit) or with active esterases (esterase-active fraction) (carboxyfluorescein diacetate) was combined with 16S rRNA gene-directed PCR and denaturing gradient gel electrophoresis (DGGE). No active bacteria were detected when water left the water treatment plant (WTP), but 12 km downstream the chloramine residual had diminished and the level of active bacteria in the bulk water had increased to more than 1 × 105 bacteria ml−1. The bacterial diversity in the system was represented by six major DGGE bands for the membrane-intact fraction and 10 major DGGE bands for the esterase-active fraction. PCR targeting of the 16S rRNA gene of chemolithotrophic ammonia-oxidizing bacteria (AOB) and subsequent DGGE and DNA sequence analysis revealed the presence of an active Nitrosospira-related species and Nitrosomonas cryotolerans in the system, but no AOB were detected in the associated WTP. The abundance of active AOB was then determined by quantitative real-time PCR (qPCR) targeting the amoA gene; 3.43 × 103 active AOB ml−1 were detected in the membrane-intact fraction, and 1.40 × 104 active AOB ml−1 were detected in the esterase-active fraction. These values were several orders of magnitude greater than the 2.5 AOB ml−1 detected using a routine liquid most-probable-number assay. Culture-independent techniques described here, in combination with existing chemical indicators, should allow the water industry to obtain more comprehensive data with which to make informed decisions regarding remedial action that may be required either prior to or during an

  18. Adsorption of palladium ions by modified carbons from rice husks

    International Nuclear Information System (INIS)

    Mostafa, M.R.

    1994-01-01

    Steam activated carbon of high surface area does not show palladium ions adsorption. Treatment of this carbon with HF acid increases to a great extent the gas adsorption capacity expressed as nitrogen surface area as well as the adsorption capacity of palladium ions from aqueous solution. HHB was loaded in different amounts on to these carbons. The acid sites represent the active fraction of the surface on which the adsorption palladium ions proceed. The uptake of palladium ions by HHB treated carbons is related to the total number of HHB molecules loaded on the carbon surface. (author)

  19. Development of Separation Materials Containing Palladium for Hydrogen Isotopes Separation

    International Nuclear Information System (INIS)

    Deng Xiaojun; Luo Deli; Qian Xiaojing

    2010-01-01

    Displacement chromatography (DC) is a ascendant technique for hydrogen isotopes separation. The performance of separation materials is a key factor to determine the separation effect of DC. At present,kinds of materials are researched, including palladium materials and non-palladium materials. It is hardly replaceable because of its excellent separation performance, although palladium is expensive. The theory of hydrogen isotopes separation using DC was introduced at a brief manner, while several palladium separation materials were expatiated in detail(Pd/K, Pd-Al 2 O 3 , Pd-Pt alloy). Development direction of separation materials for DC was forecasted elementarily. (authors)

  20. Determination of emamectin residues in the tissues of Atlantic salmon (Salmo salar L.) using HPLC with fluorescence detection.

    Science.gov (United States)

    Kim-Kang, H; Crouch, L S; Bova, A; Robinson, R A; Wu, J

    2001-11-01

    An accurate, reliable, and reproducible assay for the determination of residual concentrations of emamectin B(1a) in muscle, skin, and intact muscle/skin in natural proportions from Atlantic salmon treated with SCH 58854 (emamectin benzoate) is described. The determinative method was developed and validated using fortified control tissues at five levels over a range of 50-800 ng/g as well as tissues containing incurred levels in the same range. Incurred tissues were obtained from a metabolism study of [(3)H]emamectin benzoate in Atlantic salmon. The assay employs processing of a tissue ethyl acetate extract on a propylsulfonic acid solid phase extraction cartridge, followed by derivatization with trifluoroacetic anhydride in the presence of N-methylimidazole. Following separation using reversed phase HPLC, the amount of derivatized emamectin B(1a) is determined by fluorescence detection. The theoretical limits of detection were determined from the analysis of control tissue matrices to be 2.6, 3.3, and 3.8 ng/g as emamectin B(1a) for muscle, skin, and intact muscle/skin, respectively. Likewise, the theoretical limits of quantitation (LOQ) were determined to be 6.9, 8.1, and 9.5 ng/g as emamectin B(1a) for muscle, skin, and intact muscle/skin, respectively. The lowest fortification level used for method validation was 50 ng/g, which served as the effective LOQ for the method. The overall percent recoveries (+/-% CV) were 94.4 +/- 6.89% (n = 25) for muscle, 88.4 +/- 5.35% (n = 25) for skin, and 88.0 +/- 3.73% for intact muscle/skin (n = 25). Accuracy, precision, linearity, selectivity, and ruggedness were demonstrated. The structure of the final fluorescent derivative of emamectin B(1a) free base was identified by ESI(+)/LC-MS. The frozen storage stability of [(3)H]emamectin B(1a) in tissues with incurred residues was demonstrated for approximately 15 months by radiometric analysis and for an additional approximately 13 months by fluorometric analysis for a total of

  1. Residual tissue post splenectomy detected by splenic scintillography with erythrocytes damaged by heat; Tejido residual postesplenectomia detectado por centellografia esplenica con eritrocitos danados por calor

    Energy Technology Data Exchange (ETDEWEB)

    Rivera B, B; Garcia C, E S; Garcia O, J R [Centro Medico ABC, Departamento de Medicina Nuclear, Mexico, D.F. (Mexico)

    2005-07-01

    Feminine of 26 years old with diagnostic of purple thrombocytopenic idiopathic to those 4 years of age, tried with steroids and splenectomy at 11 years old. Pathway practically asymptomatic until 4 months ago she had presented asthenia, adynamia and general uneasiness, with platelet figures of 40,000 plat/microliter. It was carried out scintillographic study with damaged erythrocytes for post surgical remainder search. Its were took two-dimensional images and tomography by single photon emission (SPECT), being knitted splenic residual in area of anatomical projection of the spleen. (Author)

  2. Neutron measurements in deuterated palladium cathodes subjected to pulsed electrolytic currents

    International Nuclear Information System (INIS)

    Granada, J.R.; Mayer, R.E.; Guido, G.; Florido, P.C.; Patino, N.E.; Gillette, V.H.; Sobehart, L.; Gomez, S.; Larreteguy, A.; Universidad Nacional de Cuyo, San Carlos de Bariloche

    1989-01-01

    We report on neutron measurements performed on electrolytic cells using a high efficiency (22%) detection system in combination with a procedure involving a non-stationary current through the cell's circuit. Under these conditions, neutron production was observed in cells containing LiH dissolved in heavy water with a Palladium cathode. Characteristic patterns showing one or two bumps were obtained in a repeatable fashion, depending on the previous charging history of the cathode. (orig.)

  3. Spectroscopic study of low-temperature hydrogen absorption in palladium

    Energy Technology Data Exchange (ETDEWEB)

    Ienaga, K., E-mail: ienaga@issp.u-tokyo.ac.jp; Takata, H.; Onishi, Y.; Inagaki, Y.; Kawae, T. [Department of Applied Quantum Physics, Faculty of Engineering, Kyushu University, Motooka, Nishi-Ku, Fukuoka 819-0395 (Japan); Tsujii, H. [Department of Physics, Faculty of Education, Kanazawa University, Kakuma-machi, Kanazawa 920-1192 (Japan); Kimura, T. [Department of Physics, Kyushu University, Hakozaki, Higashi-Ku, Fukuoka 812-8581 (Japan)

    2015-01-12

    We report real-time detection of hydrogen (H) absorption in metallic palladium (Pd) nano-contacts immersed in liquid H{sub 2} using inelastic electron spectroscopy (IES). After introduction of liquid H{sub 2}, the spectra exhibit the time evolution from the pure Pd to the Pd hydride, indicating that H atoms are absorbed in Pd nano-contacts even at the temperature where the thermal process is not expected. The IES time and bias voltage dependences show that H absorption develops by applying bias voltage 30 ∼ 50 mV, which can be explained by quantum tunneling. The results represent that IES is a powerful method to study the kinetics of high density H on solid surface.

  4. Oxygen isotope exchange on palladium catalysts

    International Nuclear Information System (INIS)

    Kravchuk, L.S.; Beschetvertnaya, T.I.; Novorodskij, V.G.; Novikova, M.G.; Zaretskij, M.V.; Valieva, S.V.

    1983-01-01

    Oxygen heteromolecular isotope exchange on unreduced palladium catalysts, distingushing by metal content is studied. Content of 18 O in gaseous phase is eoual to 46%. Calculations of heteroexchange rates are conducted with decrease of the 18 O in the gaseous phase over solid sample. Method of oxygen thermodesorption has been used to establish that palladium, deposited on γ-Al 2 O 3 during exchange process is in oxidized state; in this case strength of Pd-O bond is determined by content dispersity) of the metal. It is shown that significant increase of exchange rate on the samples with Pd >> 0.5 mass.% content can be induced as by side decomposition reaction of its oxide and corresponding dilution of gaseous mixture by ''light'' oxygen so by possibility of exchange with oxygen of PdO phase

  5. Immunoglobulin kappa deleting element rearrangements in precursor-B acute lymphoblastic leukemia are stable targets for detection of minimal residual disease by real-time quantitative PCR

    NARCIS (Netherlands)

    van der Velden, V. H. J.; Willemse, M. J.; van der Schoot, C. E.; Hählen, K.; van Wering, E. R.; van Dongen, J. J. M.

    2002-01-01

    Immunoglobulin gene rearrangements are used as PCR targets for detection of minimal residual disease (MRD) in acute lymphoblastic leukemia (ALL). We Investigated the occurrence of monoclonal immunoglobulin kappa-deleting element (IGK-Kde) rearrangements by Southern blotting and PCR/heteroduplex

  6. Rapid Detection of Pesticide Residues in Chinese Herbal Medicines by Fourier Transform Infrared Spectroscopy Coupled with Partial Least Squares Regression

    Directory of Open Access Journals (Sweden)

    Tianming Yang

    2016-01-01

    Full Text Available This paper reports a simple, rapid, and effective method for simultaneous detection of cartap (Ca, thiocyclam (Th, and tebufenozide (Te in Chinese herbal medicines including Radix Angelicae Dahuricae and Liquorices using Fourier transform infrared spectroscopy (FT-IR coupled with partial least squares regression (PLSR. The proposed method can handle the intrinsic interferences of herbal samples; satisfactory average recoveries attained from near-infrared (NIR and mid-infrared (MIR PLSR models were 99.0±10.8 and 100.2±1.0% for Ca, 100.2±6.9 and 99.7±2.5% for Th, and 99.1±6.3 and 99.6±1.0% for Te, respectively. Furthermore, some statistical parameters and figures of merit are fully investigated to evaluate the performance of the two models. It was found that both models could give accurate results and only the performance of MIR-PLSR was slightly better than that of NIR-PLSR in the cases suffering from herbal matrix interferences. In conclusion, FT-IR spectroscopy in combination with PLSR has been demonstrated for its application in rapid screening and quantitative analysis of multipesticide residues in Chinese herbal medicines without physical or chemical separation pretreatment step and any spectral processing, which also implies other potential applications such as food and drug safety, herbal plants quality, and environmental evaluation, due to its advantages of nontoxic and nondestructive analysis.

  7. Detection of residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region of San Luis Potosi, Mexico.

    Science.gov (United States)

    Velasco, Antonio; Hernández, Sergio; Ramírez, Martha; Ortíz, Irmene

    2014-01-01

    Organochlorine pesticides were intensively used in Mexico from 1950 until their ban and restriction in 1991. However, the presence of these compounds is commonly reported in many regions of the country. The aim of the present study was to identify and quantify residual organochlorine and organophosphorus pesticides in agricultural soil in Rio Verde region, San Luis Potosi state, which has been identified as possibly polluted by pesticides. Composed samples from 24 zones covering an area of approximately 5,440 ha were analyzed. The most frequently found pesticides were p,p'-DDT followed by ,p,p'-DDE, heptachlor, endosulfan and γ-HCH whose frequency rates were 100, 91, 83 and 54%, respectively. The concentration of p,p'-DDT in the crops grown in these soils was in the following order: chili > maize > tomato > alfalfa. The results obtained in this study show that p,p'-DDT values are lower or similar to those found in other agricultural regions of Mexico. Methyl and ethyl parathion were the most frequent organophosphate pesticide detected in 100% and 62.5% of the samples with average concentrations of 25.20 and 47.48 μg kg(-1), respectively. More research is needed to establish the background levels of pesticides in agricultural soils and their potential ecological and human health effects in this region.

  8. Optical properties of palladium nanoparticles under exposure of hydrogen and inert gas prepared by dewetting synthesis of thin-sputtered layers

    Energy Technology Data Exchange (ETDEWEB)

    Kracker, Michael, E-mail: Michael.Kracker@uni-jena.de; Worsch, Christian; Ruessel, Christian [Otto-Schott-Institut, Jena University (Germany)

    2013-04-15

    Thin layers of palladium with a thickness of 5 nm were sputtered on fused silica substrates. Subsequently, the coated glasses were annealed at a temperature of 900 Degree-Sign C for 1 h. This resulted in the formation of small and well-separated palladium nanoparticles with diameters in the range from 20 to 200 nm on the glass surface. The existence of a palladium oxide layer can be detected using optical absorption spectroscopy. Purging with hydrogen leads to an irreversible change in the optical spectra due to the reduction of PdO to metallic palladium. Changing the gas atmosphere from hydrogen to argon leads to significant reversible changes in the optical properties of the particle layer. Based on Mie theory and the respective dielectric functions, the spectra were calculated using the real particle size distribution, weighted dispersions relation to adapt the geometrical conditions and complex dielectric functions of palladium and palladium hydride. A good agreement with measured spectra was found and the dependency of the surrounding media can be explained.Graphical Abstract.

  9. Extracellular Palladium Nanoparticle Production using Geobacter sulfurreducens

    KAUST Repository

    Yates, Matthew D.

    2013-09-03

    Sustainable methods are needed to recycle precious metals and synthesize catalytic nanoparticles. Palladium nanoparticles can be produced via microbial reduction of soluble Pd(II) to Pd(0), but in previous tests using dissimilatory metal reducing bacteria (DMRB), the nanoparticles were closely associated with the cells, occupying potential reductive sites and eliminating the potential for cell reuse. The DMRB Geobacter sulfurreducens was shown here to reduce soluble Pd(II) to Pd(0) nanoparticles primarily outside the cell, reducing the toxicity of metal ions, and allowing nanoparticle recovery without cell destruction that has previously been observed using other microorganisms. Cultures reduced 50 ± 3 mg/L Pd(II) with 1% hydrogen gas (v/v headspace) in 6 h incubation tests [100 mg/L Pd(II) initially], compared to 8 ± 3 mg/L (10 mM acetate) without H2. Acetate was ineffective as an electron donor for palladium removal in the presence or absence of fumarate as an electron acceptor. TEM imaging verified that Pd(0) nanoparticles were predominantly in the EPS surrounding cells in H2-fed cultures, with only a small number of particles visible inside the cell. Separation of the cells and EPS by centrifugation allowed reuse of the cell suspensions and effective nanoparticle recovery. These results demonstrate effective palladium recovery and nanoparticle production using G. sulfurreducens cell suspensions and renewable substrates such as H2 gas. © 2013 American Chemical Society.

  10. Immobilized Palladium Nanoparticles on Zirconium Carboxy-Aminophosphonates Nanosheets as an Efficient Recoverable Heterogeneous Catalyst for Suzuki–Miyaura and Heck Coupling

    Directory of Open Access Journals (Sweden)

    Vadym Kozell

    2017-06-01

    Full Text Available Zirconium phosphate glycine diphosphonate nanosheets (ZPGly have been used as support for the preparation of solid palladium nanoparticles, namely Pd@ZPGly. Thanks to the presence of carboxy-aminophosponate groups on the layer surface, ZPGly-based materials were able to stabilize a high amount of palladium (up to 22 wt % also minimizing the amount of metal leached in the final products of representative important cross-coupling processes selected for proving the catalysts’ efficiency. The catalytic systems have been fully characterized and used in low amounts (0.1 mol % in the Suzuki–Miyaura and Heck cross-couplings. Moreover, the protocols were optimized for the use of recoverable azeotropic mixtures (aq. EtOH 96% or aq. CH3CN 84%, respectively and in the flow procedure allowing one to isolate the final pure products, without any purification step, with very low residual palladium content and with a very low waste production.

  11. Detecting and confirming residual hotspots of lymphatic filariasis transmission in American Samoa 8 years after stopping mass drug administration.

    Science.gov (United States)

    Lau, Colleen L; Sheridan, Sarah; Ryan, Stephanie; Roineau, Maureen; Andreosso, Athena; Fuimaono, Saipale; Tufa, Joseph; Graves, Patricia M

    2017-09-01

    The Global Programme to Eliminate Lymphatic Filariasis (LF) aims to eliminate the disease as a public health problem by 2020 by conducting mass drug administration (MDA) and controlling morbidity. Once elimination targets have been reached, surveillance is critical for ensuring that programmatic gains are sustained, and challenges include timely identification of residual areas of transmission. WHO guidelines encourage cost-efficient surveillance, such as integration with other population-based surveys. In American Samoa, where LF is caused by Wuchereria bancrofti, and Aedes polynesiensis is the main vector, the LF elimination program has made significant progress. Seven rounds of MDA (albendazole and diethycarbamazine) were completed from 2000 to 2006, and Transmission Assessment Surveys were passed in 2010/2011 and 2015. However, a seroprevalence study using an adult serum bank collected in 2010 detected two potential residual foci of transmission, with Og4C3 antigen (Ag) prevalence of 30.8% and 15.6%. We conducted a follow up study in 2014 to verify if transmission was truly occurring by comparing seroprevalence between residents of suspected hotspots and residents of other villages. In adults from non-hotspot villages (N = 602), seroprevalence of Ag (ICT or Og4C3), Bm14 antibody (Ab) and Wb123 Ab were 1.2% (95% CI 0.6-2.6%), 9.6% (95% CI 7.5%-12.3%), and 10.5% (95% CI 7.6-14.3%), respectively. Comparatively, adult residents of Fagali'i (N = 38) had significantly higher seroprevalence of Ag (26.9%, 95% CI 17.3-39.4%), Bm14 Ab (43.4%, 95% CI 32.4-55.0%), and Wb123 Ab 55.2% (95% CI 39.6-69.8%). Adult residents of Ili'ili/Vaitogi/Futiga (N = 113) also had higher prevalence of Ag and Ab, but differences were not statistically significant. The presence of transmission was demonstrated by 1.1% Ag prevalence (95% CI 0.2% to 3.1%) in 283 children aged 7-13 years who lived in one of the suspected hotspots; and microfilaraemia in four individuals, all of whom lived in the

  12. Thermosonic wire bonding of IC devices using palladium wire

    International Nuclear Information System (INIS)

    Shze, J.H.; Poh, M.T.; Tan, R.M.

    1996-01-01

    The feasibility of replacing gold wire by palladium wire in thermosonic wire bonding of CMOS and bipolar devices are studied in terms of the manufacturability, physical, electrical and assembly performance. The results that palladium wire is a viable option for bonding the bipolar devices but not the CMOS devices

  13. Thermodynamics of the hybrid interaction of hydrogen with palladium nanoparticles

    NARCIS (Netherlands)

    Griessen, R.P.; Strohfeldt, N.; Giessen, H.

    2015-01-01

    Palladium-hydrogen is a prototypical metal-hydrogen system. It is therefore not at all surprising that a lot of attention has been devoted to the absorption and desorption of hydrogen in nanosized palladium particles. Several seminal articles on the interaction of H with Pd nanocubes and

  14. Disappearance of Ph1 chromosome with intensive chemotherapy and detection of minimal residual disease by polymerase chain reaction in a patient with blast crisis of chronic myelogenous leukemia.

    Science.gov (United States)

    Honda, H; Miyagawa, K; Endo, M; Takaku, F; Yazaki, Y; Hirai, H

    1993-06-01

    We diagnosed a patient with chronic myelogenous leukemia (CML) in chronic phase (CP) on the basis of clinical findings, Ph1 chromosome detected by cytogenetic analysis, and bcr-abl fusion mRNA detected by reverse transcriptase-dependent polymerase chain reaction (RT-PCR). One month after diagnosis, the patient developed extramedullary blast crisis in the lymph nodes, and then medullary blast crisis in the bone marrow, in which different surface markers were shown. Combination chemotherapy with BH-AC, VP16, and mitoxantrone was administered; this resulted in rapid disappearance of the lymphadenopathy, restoration of normal hematopoiesis, and no Ph1 chromosome being detected by cytogenetic analysis. RT-PCR performed to detect the residual Ph1 clone revealed that although the Ph1 clone was preferentially suppressed, it was still residual. The intensive chemotherapy regimen preferentially suppressed the Ph1-positive clone and led to both clinical and cytogenetic remission in this patient with BC of CML; we suggest that RT-PCR is a sensitive and useful method for detecting minimal residual disease during the clinical course of this disease.

  15. Nonenzymatic glucose sensing based on deposited palladium nanoparticles on epoxy-silver electrodes

    International Nuclear Information System (INIS)

    Gutes, Albert; Carraro, Carlo; Maboudian, Roya

    2011-01-01

    Highlights: → New nonenzymatic glucose sensor material. → Modified epoxy-silver electrodes with palladium nanoparticles. → Simple electroless surface modification. → Wide linear response range. → Easy implementation. - Abstract: A new approach for nonenzymatic glucose sensing, based on a simple modification of epoxy-silver surfaces deposited on the tip of commercial copper electric wires, is presented. Palladium was galvanically displaced on the surface of the epoxy-silver surface in order to obtain metal nanoparticles that act as catalyst for the direct oxidation of glucose. Scanning electron microscopy revealed the formation of the metal nanoparticles. X-ray photoelectron spectroscopy confirmed the metallic nature of the formed nanostructures on the surface. Electrochemical characterization and calibration of the palladium-modified epoxy-silver electrode is reported, obtaining a linear range of 1-20 mM for the detection of glucose with low interference of ascorbic acid and uric acid. A simple 3-step coulometry was used as the detection technique. The developed sensing material is believed to be a great candidate for integration in small devices for clinical essays, due to the simplicity and cost effectiveness of the presented approach, compared to the state-of-the-art devices reported recently in the literature. Simplicity in the coulometry determinations makes these Pd-modified epoxy-silver sensors a good candidate for easy glucose determinations.

  16. Detection of colorectal masses in CT colonography: application of deep residual networks for differentiating masses from normal colon anatomy

    Science.gov (United States)

    Näppi, Janne J.; Hironaka, Toru; Yoshida, Hiroyuki

    2018-02-01

    Even though the clinical consequences of a missed colorectal cancer far outweigh those of a missed polyp, there has been little work on computer-aided detection (CADe) for colorectal masses in CT colonography (CTC). One of the problems is that it is not clear how to manually design mathematical image-based features that could be used to differentiate effectively between masses and certain types of normal colon anatomy such as ileocecal valves (ICVs). Deep learning has demonstrated ability to automatically determine effective discriminating features in many image-based problems. Recently, residual networks (ResNets) were developed to address the practical problems of constructing deep network architectures for optimizing the performance of deep learning. In this pilot study, we compared the classification performance of a conventional 2D-convolutional ResNet (2D-ResNet) with that of a volumetric 3D-convolutional ResNet (3D-ResNet) in differentiating masses from normal colon anatomy in CTC. For the development and evaluation of the ResNets, 695 volumetric images of biopsy-proven colorectal masses, ICVs, haustral folds, and rectal tubes were sampled from 196 clinical CTC cases and divided randomly into independent training, validation, and test datasets. The training set was expanded by use of volumetric data augmentation. Our preliminary results on the 140 test samples indicate that it is feasible to train a deep volumetric 3D-ResNet for performing effective image-based discriminations in CTC. The 3D-ResNet slightly outperformed the 2D-ResNet in the discrimination of masses and normal colon anatomy, but the statistical difference between their very high classification accuracies was not significant. The highest classification accuracy was obtained by combining the mass-likelihood estimates of the 2D- and 3D-ResNets, which enabled correct classification of all of the masses.

  17. Determination of diacylhydrazines-type insect growth regulator JS-118 residues in cabbage and soil by high performance liquid chromatography with DAD detection.

    Science.gov (United States)

    Hu, J-Y; Deng, Z-B; Qin, D-M

    2009-12-01

    JS-118 is a diacylhydrazines-type insect growth regulator used extensively in China now. An analytical method for residues determination of JS-118 in cabbage and soil samples by high performance liquid chromatography with DAD detection was established and optimized. Primary secondary amine solid phase extraction cartridge was used for sample preparation. Mean recoveries for the analyte ranged from 96.6% to 107.0% with CV value less than 4.7%. The limit of quantification is 0.01 mg/kg. Direct confirmation of JS-118 residues in samples was realized by high performance liquid chromatography-mass spectrometry. The proposed method is simple, rapid and reliable to perform and could be utilized for monitoring of pesticides residues.

  18. Chemical recovery of a palladium-103 from irradiated silver target

    International Nuclear Information System (INIS)

    Lapshina, E.V.; Kokhanyuk, V.M.; Zhuikov, B.L.; Myasoedova, G.V.; Zakhartchenko, E.A.; Phillips, D.R.; Jamriska, D.J.

    2003-01-01

    The goal of this work is to develop an extraction method of no-carrier-added palladium-103 from silver. Metallic silver targets were irradiated by protons with the energy of 60-140 MeV to generate palladium-103. Other radioactive isotopes of rhodium, ruthenium, technetium, palladium and silver are also formed at the same time. Two methods of Pd-103 recovering from irradiated silver target are considered. The first one includes the dissolving of the irradiated silver target in nitric acid followed by adding of hydrochloric acid to the solution. Palladium with rhodium, ruthenium and technetium completely remained in solution while silver was precipitated in the form of silver chloride. Extraction of palladium from the obtained solution was provided by the formation of palladium complex with a chelate sorbent which is specific to palladium in acidic solutions. The sorbent makes it possible to separate palladium from admixtures of rhodium, ruthenium and technetium isotopes. The polymeric complex-forming sorbent of fibrous structure with the groups of 3 (5) - methylpyrazole (POLYORGS-15n) is used. An other possible method has been also studied. It includes again dissolving of metallic silver in nitric acid, but does not need silver chloride precipitation. Silver may be sorbed by the complex-forming sorbents, but its sorption is very sensitive to acid concentration. Chelate sorbents of fibrous structure with the groups of amidoxime and hydrazidine (POLYORGS-33n) have been successfully used in our experiments. A high efficiency of palladium extraction by POLYORGS-33n from 2-4 M nitric acid solutions was achieved. Concentrated hydrochloric acid (without heating) was used for palladium desorption with higher yield than in the first method. (authors)

  19. Comparison of thallium-201 SPET and CT/MRI in the detection of residual/recurrent squamous cell carcinoma of the oral cavity

    International Nuclear Information System (INIS)

    Lee, Jong-Kang; Tyan, Yeu-Sheng; Huang, Wen-Sheng

    2004-01-01

    This study was designed to compare the effectiveness of thallium-201 single-photon emission tomography (SPET) and conventional imaging, comprising computed tomography (CT) and magnetic resonance imaging (MRI), in the detection of residual/recurrent squamous cell carcinoma (SCC) of the oral cavity. Thirty-two patients with clinically suspected recurrent SCC of the oral cavity were recruited. All patients underwent 201 Tl SPET and CT or MRI within 2 weeks. The final diagnoses were based on the histology of the biopsy specimen. 201 Tl SPET and CT/MRI both accurately detected 17 of 18 residual/recurrent tumours. CT/MRI yielded eight false-positive studies, whereas 201 Tl SPET successfully excluded all tumours. The sensitivity, specificity, positive and negative predictive values and accuracy of 201 Tl SPET for the detection of recurrent oral SCC were 94%, 100%, 100%, 93% and 97%, respectively. The sensitivity, specificity, positive and negative predictive values and accuracy of CT/MRI for the detection of recurrent oral SCC were 94%, 43%, 68%, 86% and 72%, respectively. Thallium-201 SPET is more accurate than conventional imaging (CT or MRI) in differentiating residual/recurrent oral SCC from post-therapy changes. (orig.)

  20. Validation of a high-performance liquid chromatographic method with UV detection for the determination of ethopabate residues in poultry liver.

    Science.gov (United States)

    Granja, Rodrigo H M M; Niño, Alfredo M Montes; Zucchetti, Roberto A M; Niño, Rosario E Montes; Salerno, Alessandro G

    2008-01-01

    Ethopabate is frequently used in the prophylaxis and treatment of coccidiosis in poultry. Residues of this drug in food present a potential risk to consumers. A simple, rapid, and sensitive column high-performance liquid chromatographic (HPLC) method with UV detection for determination of ethopabate in poultry liver is presented. The drug is extracted with acetonitrile. After evaporation, the residue is dissolved with an acetone-hexane mixture and cleaned up by solid-phase extraction using Florisil columns. The analyte is then eluted with methanol. LC analysis is carried out on a C18 5 microm Gemini column, 15 cm x 4.6 mm. Ethopabate is quantified by means of UV detection at 270 nm. Parameters such as decision limit, detection capability, precision, recovery, ruggedness, and measurement uncertainty were calculated according to method validation guidelines provided in 2002/657/EC and ISO/IEC 17025:2005. Decision limit and detection capability were determined to be 2 and 3 microg/kg, respectively. Average recoveries from poultry samples fortified with 10, 15, and 20 microg/kg levels of ethopabate were 100-105%. A complete statistical analysis was performed on the results obtained, including an estimation of the method uncertainty. The method is to be implemented into Brazil's residue monitoring and control program for ethopabate.

  1. Organophosphorus and Carbamate Pesticide Residues Detected in Water Samples Collected from Paddy and Vegetable Fields of the Savar and Dhamrai Upazilas in Bangladesh

    Directory of Open Access Journals (Sweden)

    Nurul Karim

    2012-09-01

    Full Text Available Several types of organophosphorous and carbamate pesticides have been used extensively by the farmers in Bangladesh during the last few decades. Twenty seven water samples collected from both paddy and vegetable fields in the Savar and Dhamrai Upazilas in Bangladesh were analyzed to determine the occurrence and distribution of organo-phosphorus (chlorpyrifos, malathion and diazinon and carbamate (carbaryl and carbofuran pesticide residues. A high performance liquid chromatograph instrument equipped with a photodiode array detector was used to determine the concentrations of these pesticide residues. Diazinon and carbofuran were detected in water samples collected from Savar Upazila at 0.9 μg/L and 198.7 μg/L, respectively. Malathion was also detected in a single water sample at 105.2 μg/L from Dhamrai Upazila. Carbaryl was the most common pesticide detected in Dhamrai Upazila at 14.1 and 18.1 μg/L, while another water sample from Dhamrai Upazila was contaminated with carbofuran at 105.2 μg/L. Chlorpyrifos was not detected in any sample. Overall, the pesticide residues detected were well above the maximum acceptable levels of total and individual pesticide contamination, at 0.5 and 0.1 μg/L, respectively, in water samples recommended by the European Economic Community (Directive 98/83/EC. The presence of these pesticide residues may be attributed by their intense use by the farmers living in these areas. Proper handling of these pesticides should be ensured to avoid direct or indirect exposure to these pesticides.

  2. AFNOR validation of Premi Test, a microbiological-based screening tube-test for the detection of antimicrobial residues in animal muscle tissue.

    Science.gov (United States)

    Gaudin, Valerie; Juhel-Gaugain, Murielle; Morétain, Jean-Pierre; Sanders, Pascal

    2008-12-01

    Premi Test contains viable spores of a strain of Bacillus stearothermophilus which is sensitive to antimicrobial residues, such as beta-lactams, tetracyclines, macrolides and sulphonamides. The growth of the strain is inhibited by the presence of antimicrobial residues in muscle tissue samples. Premi Test was validated according to AFNOR rules (French Association for Normalisation). The AFNOR validation was based on the comparison of reference methods (French Official method, i.e. four plate test (FPT) and the STAR protocol (five plate test)) with the alternative method (Premi Test). A preliminary study was conducted in an expert laboratory (Community Reference Laboratory, CRL) on both spiked and incurred samples (field samples). Several method performance criteria (sensitivity, specificity, relative accuracy) were estimated and are discussed, in addition to detection capabilities. Adequate agreement was found between the alternative method and the reference methods. However, Premi Test was more sensitive to beta-lactams and sulphonamides than the FPT. Subsequently, a collaborative study with 11 laboratories was organised by the CRL. Blank and spiked meat juice samples were sent to participants. The expert laboratory (CRL) statistically analysed the results. It was concluded that Premi Test could be used for the routine determination of antimicrobial residues in muscle of different animal origin with acceptable analytical performance. The detection capabilities of Premi Test for beta-lactams (amoxicillin, ceftiofur), one macrolide (tylosin) and tetracycline were at the level of the respective maximum residue limits (MRL) in muscle samples or even lower.

  3. Robust fault detection of turbofan engines subject to adaptive controllers via a Total Measurable Fault Information Residual (ToMFIR) technique.

    Science.gov (United States)

    Chen, Wen; Chowdhury, Fahmida N; Djuric, Ana; Yeh, Chih-Ping

    2014-09-01

    This paper provides a new design of robust fault detection for turbofan engines with adaptive controllers. The critical issue is that the adaptive controllers can depress the faulty effects such that the actual system outputs remain the pre-specified values, making it difficult to detect faults/failures. To solve this problem, a Total Measurable Fault Information Residual (ToMFIR) technique with the aid of system transformation is adopted to detect faults in turbofan engines with adaptive controllers. This design is a ToMFIR-redundancy-based robust fault detection. The ToMFIR is first introduced and existing results are also summarized. The Detailed design process of the ToMFIRs is presented and a turbofan engine model is simulated to verify the effectiveness of the proposed ToMFIR-based fault-detection strategy. Copyright © 2013 ISA. Published by Elsevier Ltd. All rights reserved.

  4. Investigation into periodic process of hydrogen isotope separation by counterflow method in the hydrogen-palladium system

    International Nuclear Information System (INIS)

    Andreev, B.M.; Selivanenko, I.L.; Vedeneev, A.I.; Golubkov, A.N.; Tenyaev, B.N.

    1999-01-01

    The key diagram and results of the investigation into working conditions of the pilot plant for hydrogen isotope separation embodying the concept of continuous counterflow separation in the hydrogen-palladium system are shown. The counterflow of phases in the plant is attained under the motion of palladium solid hydride phase relative to stationary blocks of flow rotation. The column separator is defined as section type one. The plant performs in periodic regime with accumulating vessels for light and heavy components of the separated mixture. Maximum concentration of the separated tritium ranged up to ∼ 96 % in the experiments of the deuterium-tritium separation. Minimum concentration of the residual tritium in the mixture ranged up to ∼ 0.1 %. The plant provides to reprocessing 4.5 moles of the gas a day [ru

  5. [High throuput analysis of organophosphorus pesticide residues and their metabolites in animal original foods by dual gas chromatography-dual pulse flame photometric detection].

    Science.gov (United States)

    Yang, Lixin; Li, Heli; Miao, Hong; Zeng, Fangang; Li, Ruifeng; Chen, Huijing; Zhao, Yunfeng; Wu, Yongning

    2011-10-01

    A method was established for the quantitative determination of 54 organophosphorus pesticide residues and their metabolites in foods of animal origin by dual gas chromatography-dual pulse flame photometric detection. Homogenized samples were extracted with acetone and methylene chloride, and cleaned-up by gel permeation chromatography (GPC). The response of each analyte showed a good linearity with a correlation coefficient not less than 0. 99. The recovery experiments were performed by a blank sample spiked at low, medium and high fortification levels. The recoveries for beef, mutton, pork, chicken were in the range of 50. 5% -128. 1% with the relative standard deviations (n = 6) of 1. 1% -25. 5%, which demonstrated the good precision and accuracy of the present method. The limits of detection for the analytes were in the range of 0. 001 -0. 170 mg/kg, and the limits of quantification were in the range of 0. 002 -0. 455 mg/kg. Animal food samples collected from markets such as meat, liver and kidney were analyzed, and the residues of dichlorovos and disulfoton-sulfoxide were found in the some samples. The established method is sensitive and selective enough to detect organophosphorus pesticide residues in animal foods.

  6. An automated approach to improve efficacy in detecting residual malignant cancer cell for facilitating prognostic assessment of leukemia: an initial study

    Science.gov (United States)

    Qiu, Yuchen; Lu, Xianglan; Tan, Maxine; Li, Shibo; Liu, Hong; Zheng, Bin

    2015-03-01

    The purpose of this study is to investigate the feasibility of applying automatic interphase FISH cells analysis method for detecting the residual malignancy of post chemotherapy leukemia patients. In the experiment, two clinical specimens with translocation between chromosome No. 9 and 22 or No. 11 and 14 were selected from the patients underwent leukemia diagnosis and treatment. The entire slide of each specimen was first digitalized by a commercial fluorescent microscope using a 40× objective lens. Then, the scanned images were processed by a computer-aided detecting (CAD) scheme to identify the analyzable FISH cells, which is accomplished by applying a series of features including the region size, Brenner gradient and maximum intensity. For each identified cell, the scheme detected and counted the number of the FISH signal dots inside the nucleus, using the adaptive threshold of the region size and distance of the labeled FISH dots. The results showed that the new CAD scheme detected 8093 and 6675 suspicious regions of interest (ROI) in two specimens, among which 4546 and 3807 ROI contain analyzable interphase FISH cell. In these analyzable ROIs, CAD selected 334 and 405 residual malignant cancer cells, which is substantially more than those visually detected in a cytogenetic laboratory of our medical center (334 vs. 122, 405 vs. 160). This investigation indicates that an automatic interphase FISH cell scanning and CAD method has the potential to improve the accuracy and efficiency of the prognostic assessment for leukemia and other genetic related cancer patients in the future.

  7. Tritium evolution from various morphologies of palladium

    International Nuclear Information System (INIS)

    Tuggle, D.G.; Claytor, T.N.; Taylor, S.F.

    1994-01-01

    The authors have been able to extend the tritium production techniques to various novel morphologies of palladium. These include small solid wires of various diameters and a type of pressed powder wire and a plasma cell. In most successful experiments, the amount of palladium required, for an equivalent tritium output, has been reduced by a factor of 100 over the older powder methods. In addition, they have observed rates of tritium production (>5 nCi/h) that far exceed most of the previous results. Unfortunately, the methods that they currently use to obtain the tritium are poorly understood and consequently there are numerous variables that need to be investigated before the new methods are as reliable and repeatable as the previous techniques. For instance, it seems that surface and/or bulk impurities play a major role in the successful generation of any tritium. In those samples with total impurity concentrations of >400 ppM essentially no tritium has been generated by the gas loading and electrical simulation methods

  8. Effects of thermal processing on the enzyme-linked immunosorbent assay (ELISA) detection of milk residues in a model food matrix.

    Science.gov (United States)

    Downs, Melanie L; Taylor, Steve L

    2010-09-22

    Food products and ingredients are frequently tested for the presence of undeclared allergenic food residues (including milk) using commercial enzyme-linked immunosorbent assays (ELISAs). However, little is understood about the efficacy of these kits with thermally processed foods. This study evaluated the performance of three milk ELISA kits with a model food processed by several methods. A model food (pastry dough squares) was spiked with nonfat dry milk at several concentrations. The pastry squares were processed by boiling (100 °C for 2 min), baking (190 °C for 30 min), frying (190 °C for 2 min), and retorting (121 °C for 20 min with 17 psi overpressure). Samples were analyzed with three commercial ELISA kits: Neogen Veratox Total Milk, ELISA Systems β-lactoglobulin, and ELISA Systems casein. The detection of milk residues depended upon the type of processing applied to the food and the specific milk analyte targeted by the ELISA kit. Poor recoveries were obtained in all processed samples (2-10% of expected values) using the β-lactoglobulin kit. Better recoveries were obtained in boiled samples (44 and 59%, respectively) using the total milk and casein kits. However, these kits performed poorly with baked (9 and 21%) and fried (7 and 18%) samples. Moderate recoveries were observed in retorted samples (23 and 28%). The decreased detection in processed samples is likely due to protein modifications, including aggregation and Maillard reactions, which affect the solubility and immunoreactivity of the antigens detected by the ELISA methods. The observed decreases in ELISA detection of milk are dramatic enough to affect risk-assessment decisions. However, a lower detection of milk residues does not necessarily indicate decreased allergenicity. These ELISA kits are not acceptable for all applications, and users should understand the strengths and limitations of each method.

  9. The effect of the polymerization initiator and light source on the elution of residual Bis-GMA and TEGDMA monomers: A study using liquid chromatography with UV detection.

    Science.gov (United States)

    Denis, Aline B; Diagone, Cristina A; Plepis, Ana M G; Viana, Rommel B

    2015-12-05

    A method for the extraction and quantification of two residual monomers, bisphenol glycidyl dimethacrylate (Bis-GMA) and triethylene glycol dimethacrylate (TEGDMA), that were evaluated using high efficiency liquid chromatography with UV detection was developed and validated in this study. Three types of solvents were applied in the extraction of the monomers (methanol, ethanol and acetonitrile), where the highest extraction efficiency was obtained using acetonitrile. The different resins were prepared by photoactivation of Bis-GMA and TEGDMA monomers. Additionally, the effects of the addition of two photoinitiators (camphorquinone (CQ) and phenyl propanodione (PPD) and that of a co-initiator (N,N-dimethyl-p-toluidine) were also analyzed. When only the CQ photoinitiator was used, a smaller amount of residual monomers was obtained, whereas a larger amount was obtained with PPD. When the two photoinitiators were used in the same matrix, however, no significant changes were observed in relation to the amount of residual TEGDMA monomers. For the addition of the co-initiator, there were no large changes in the extraction of residual monomers. The effect of the two photoactivation sources (halogen lamp and LED) led to small differences in the elution of the two monomers, although all of the resins differed significantly when photoactivated with a LED. Quantum chemical calculations using Density Functional Theory were carried out to characterize several molecular properties of each monomer. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Characterising palladium-silver and palladium-nickel alloy membranes using SEM, XRD and PIXE

    International Nuclear Information System (INIS)

    Keuler, J.N.; Lorenzen, L.; Sanderson, R.D.; Prozesky, V.; Przybylowicz, W.J.

    1999-01-01

    Palladium alloy membranes were prepared by successive electroless plating steps on an alumina-zirconia support membrane. Palladium, silver and nickel were deposited in layers and then the metal films were heat treated for 5 h in a hydrogen atmosphere at 650 deg. C. The topography of the metal coatings and cross-sections of the films (before and after heating) were characterised using scanning electron microscopy (SEM). XRD was used to determine the crystal phase of the alloy coatings. Both SEM and XRD provide only surface information and therefore micro-PIXE was used to extract depth information of the alloy coating. Concentration profiles across the thickness of the films were constructed to determine penetration of the coating into the support membrane pores during electroless plating and to investigate diffusion of coated layers during the heating step

  11. Analysis of residual products in benzyl chloride used for the industrial synthesis of quaternary compounds by liquid chromatography with diode-array detection.

    Science.gov (United States)

    Prieto-Blanco, M C; López-Mahía, P; Prada-Rodríguez, D

    2009-02-01

    In industrial and pharmaceutical processes, the study of residual products becomes essential to guarantee the quality of compounds and to eliminate or minimize toxic residual products. Knowledge about the origin of impurities (raw materials, processes, the contamination of industrial plants, etc.) is necessary in preventive treatment and in the control of a product's lifecycle. Benzyl chloride is used as raw material to synthesize several quaternary ammonium compounds, such as benzalkonium chloride, which may have pharmaceutical applications. Benzaldehyde, benzyl alcohol, toluene, chloro derivatives of toluene, and dibenzyl ether are compounds that may be found as impurities in technical benzyl chloride. We proposed a high-performance liquid chromatography method for the separation of these compounds, testing two stationary phases with different dimensions and particle sizes, with the application of photodiode array-detection. The linearity for four possible impurities (benzaldehyde, toluene, alpha,alpha-dichlorotoluene, and 2-chlorotoluene) ranged from 0.1 to 10 microg/mL, limits of detection from 11 to 34 ng/mL, and repeatability from 1% to 2.9% for a 0.3-1.2 microg/mL concentration range. The method was applied to samples of technical benzyl chloride, and alpha,alpha-dichlorotoluene and benzaldehyde were identified by spectral analysis and quantitated. The selection of benzyl chloride with lower levels of impurities is important to guarantee the reduction of residual products in further syntheses.

  12. Non-Destructive Detection of Wire Rope Discontinuities from Residual Magnetic Field Images Using the Hilbert-Huang Transform and Compressed Sensing

    Directory of Open Access Journals (Sweden)

    Juwei Zhang

    2017-03-01

    Full Text Available Electromagnetic methods are commonly employed to detect wire rope discontinuities. However, determining the residual strength of wire rope based on the quantitative recognition of discontinuities remains problematic. We have designed a prototype device based on the residual magnetic field (RMF of ferromagnetic materials, which overcomes the disadvantages associated with in-service inspections, such as large volume, inconvenient operation, low precision, and poor portability by providing a relatively small and lightweight device with improved detection precision. A novel filtering system consisting of the Hilbert-Huang transform and compressed sensing wavelet filtering is presented. Digital image processing was applied to achieve the localization and segmentation of defect RMF images. The statistical texture and invariant moment characteristics of the defect images were extracted as the input of a radial basis function neural network. Experimental results show that the RMF device can detect defects in various types of wire rope and prolong the service life of test equipment by reducing the friction between the detection device and the wire rope by accommodating a high lift-off distance.

  13. Fabrication of palladium-based microelectronic devices by microcontact printing

    International Nuclear Information System (INIS)

    Wolfe, Daniel B.; Love, J. Christopher; Paul, Kateri E.; Chabinyc, Michael L.; Whitesides, George M.

    2002-01-01

    This letter demonstrates the patterning of thin films of metallic palladium by microcontact printing (μCP) of octadecanethiol, and the use of the patterned films in the fabrication of a functional sensor. This technique was also used to prepare templates of palladium for the electroless deposition of copper. The resistivity of the palladium and copper microstructures was 13.8 and 2.8 μΩ cm, respectively; these values are approximately 40% larger than the values for the pure bulk metals. Palladium patterned into serpentine wires using μCP functioned as a hydrogen sensor with sensitivity of 0.03 vol % H 2 in N 2 , and a response time of ∼10 s (at room temperature)

  14. Antibacterial properties of palladium nanostructures sputtered on polyethylene naphthalate

    Czech Academy of Sciences Publication Activity Database

    Polívková, M.; Válová, M.; Siegel, J.; Rimpelová, S.; Hubáček, Tomáš; Lyutakov, O.; Švorčík, V.

    2015-01-01

    Roč. 5, č. 90 (2015), s. 73767-73774 ISSN 2046-2069 Institutional support: RVO:60077344 Keywords : polymer * palladium sputtering * annealing * nanostructure * antibacterial effect Subject RIV: JJ - Other Materials Impact factor: 3.289, year: 2015

  15. Palladium-catalysed arylation of sulfonamide stabilised enolates

    CSIR Research Space (South Africa)

    Zeevaart, JG

    2005-03-07

    Full Text Available Alpha-Arylation of inethanesulfonamides using palladium catalysis is described. For example, treatment of N-benzyl-Nmethylmethanesulfonamide with catalytic Pd (OAc) (2) in the presence of sodium tert-butoxide, triphenylphosphine and toluene afforded...

  16. Tapered Optical Fiber Functionalized with Palladium Nanoparticles by Drop Casting and Laser Radiation for H₂ and Volatile Organic Compounds Sensing Purposes.

    Science.gov (United States)

    González-Sierra, Nancy Elizabeth; Gómez-Pavón, Luz Del Carmen; Pérez-Sánchez, Gerardo Francisco; Luis-Ramos, Arnulfo; Zaca-Morán, Plácido; Muñoz-Pacheco, Jesús Manuel; Chávez-Ramírez, Francisco

    2017-09-06

    A comparative study on the sensing properties of a tapered optical fiber pristine and functionalized with the palladium nanoparticles to hydrogen and volatile organic compounds (VOCs), is presented. The sensor response and, response/recovery times were extracted from the measurements of the transient response of the device. The tapered optical fiber sensor was fabricated using a single-mode optical fiber by the flame-brushing technique. Functionalization of the optical fiber was performed using an aqueous solution of palladium chloride by drop-casting technique assisted for laser radiation. The detection principle of the sensor is based on the changes in the optical properties of palladium nanoparticles when exposed to reducing gases, which causes a variation in the absorption of evanescent waves. A continuous wave laser diode operating at 1550 nm is used for the sensor characterization. The sensor functionalized with palladium nanoparticles by this technique is viable for the sensing of hydrogen and VOCs, since it shows an enhancement in sensor response and response time compared to the sensor based on the pristine optical microfiber. The results show that the fabricated sensor is competitive with other fiber optic sensors functionalized with palladium nanoparticles to the hydrogen.

  17. Palladium silicide - a new contact for semiconductor radiation detectors

    International Nuclear Information System (INIS)

    Totterdell, D.H.J.

    1981-11-01

    Silicide layers can be used as low resistance contacts in semiconductor devices. The formation of a metal rich palladium silicide Pd 2 Si is discussed. A palladium film 100A thick is deposited at 300 0 C and the resulting silicide layer used as an ohmic contact in an n + p silicon detector. This rugged contact has electrical characteristics comparable with existing evaporated gold contacts and enables the use of more reproducible bonding techniques. (author)

  18. Toward Efficient Palladium-Catalyzed Allylic C-H Alkylation

    DEFF Research Database (Denmark)

    Jensen, Thomas; Fristrup, Peter

    2009-01-01

    Recent breakthroughs have proved that direct palladium (II)-catalyzed allylic C-H alkylation can be achieved. This new procedure shows that the inherent requirement for a leaving group in the Tsuji-Trost palladium-catalyzed allylic alkylation can be lifted. These initial reports hold great promise...... for the development of allylic C-H alkylation into a widely applicable methodology, thus providing a means to enhance synthetic efficiency in these reactions....

  19. Separation of gold, palladium and platinum in chromite by anion exchange chromatography for inductively coupled plasma atomic emission spectrometric analysis

    International Nuclear Information System (INIS)

    Choi, Kwang Soon; Lee, Chang Heon; Park, Yeong Jae; Joe, Kih Soo; Kim, Won Ho

    2001-01-01

    A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behavior of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(VI) to Cr(III) by H 2 O 2 . AuCl - 4 retained on the resin column was selectively eluted with acetone- HNO 3 -H 2 O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO 3 . The recovery yield of gold with acetone-HNO 3 -H 2 O was 100.7 ± 2.0 % , and the yields of palladium and platinum with concentrated HCl and HNO 3 were 96.1 ± 1.8% and 96.6 ± 1.3%, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 ± 2.2 μg/g and 1.6 ± 0.14 μg/g, respectively. Palladium was not detected

  20. Morphological and immunological criteria of minimal residual disease detection in children with B-cell precursors acute lymphoblastic leukemia

    Science.gov (United States)

    Beznos, O. A.; Grivtsova, L. Yu; Popa, A. V.; Shervashidze, M. A.; Serebtyakova, I. N.; Tupitsyn, N. N.; Selchuk, V. U.; Grebennikova, O. P.; Titova, G. V.

    2018-01-01

    One of the key factors of prognosis and risk stratification in patients with B-cell precursor acute lymphoblastic leukemia (BCP-ALL) is minimal residual disease (MRD). Identification of MRD on the day 15th is one of the most significant in prognosis of the disease. We compared data of a morphological and flow cytometry results of assessment of a bone marrow (BM) at the day 15th of induction chemotherapy in children with BCP-ALL.

  1. Detecting single-abasic residues within a DNA strand immobilized in a biological nanopore using an integrated CMOS sensor.

    Science.gov (United States)

    Kim, Jungsuk; Maitra, Raj D; Pedrotti, Ken; Dunbar, William B

    2013-02-01

    In this paper, we demonstrate the application of a novel current-measuring sensor (CMS) customized for nanopore applications. The low-noise CMS is fabricated in a 0.35μm CMOS process and is implemented in experiments involving DNA captured in an α-hemolysin (α-HL) nanopore. Specifically, the CMS is used to build a current amplitude map as a function of varying positions of a single-abasic residue within a homopolymer cytosine single-stranded DNA (ssDNA) that is captured and held in the pore. Each ssDNA is immobilized using a biotin-streptavidin linkage. Five different DNA templates are measured and compared: one all-cytosine ssDNA, and four with a single-abasic residue substitution that resides in or near the ~1.5nm aperture of the α-HL channel when the strand is immobilized. The CMOS CMS is shown to resolves the ~5Å displacements of the abasic residue within the varying templates. The demonstration represents an advance in application-specific circuitry that is optimized for small-footprint nanopore applications, including genomic sequencing.

  2. Carbon in palladium catalysts: A metastable carbide

    International Nuclear Information System (INIS)

    Seriani, Nicola; Mittendorfer, Florian; Kresse, Georg

    2010-01-01

    The catalytic activity of palladium towards selective hydrogenation of hydrocarbons depends on the partial pressure of hydrogen. It has been suggested that the reaction proceeds selectively towards partial hydrogenation only when a carbon-rich film is present at the metal surface. On the basis of first-principles simulations, we show that carbon can dissolve into the metal because graphite formation is delayed by the large critical nucleus necessary for graphite nucleation. A bulk carbide Pd 6 C with a hexagonal 6-layer fcc-like supercell forms. The structure is characterized by core level shifts of 0.66-0.70 eV in the core states of Pd, in agreement with experimental x-ray photoemission spectra. Moreover, this phase traps bulk-dissolved hydrogen, suppressing the total hydrogenation reaction channel and fostering partial hydrogenation. (author)

  3. Comparative study of three screening tests, two microbiological tube tests, and a multi-sulphonamide ELISA kit for the detection of antimicrobial and sulphonamide residues in eggs.

    Science.gov (United States)

    Gaudin, V; Hedou, C; Rault, A; Sanders, P; Verdon, E

    2009-04-01

    The screening of antimicrobial residues in eggs is an especially important subject. Three different commercial kits for the screening of sulphonamides and other antimicrobials in eggs were validated in accordance with Decision 2002/657/EC: one enzyme-linked immunoabsorbant assay (ELISA) kit multi-sulphonamides (from RAISIO Diagnostics) and two microbiological tests (a Premi test from DSM and an Explorer kit from Zeu-Inmunotec). The false-positive rates were lower than 2% for all kits. The detection capabilities (CCbeta) have to be as low as possible for banned substances and lower than the maximum residue limit (MRL) when MRLs have been set. The sensitivity of the Premi test was better than that of the Explorer test, probably because of the dilution of the eggs before the Explorer test was used. The CCbeta values towards most of the tested sulphonamides were satisfactory with the Premi test (amoxicillin, neomycin, tylosin and erythromycin were lower than their respective MRLs. Detection capabilities for sulphonamides were much lower for the ELISA kit than for microbiological tests. The ELISA kit could be recommended for the targeted screening of sulphonamides in eggs. On the other hand, the Explorer and Premi tests could be used as wide screening tests allowing the detection of most of the antimicrobial families.

  4. Thermal neutron measurements on electrolytic cells with deuterated palladium cathodes subjected to a pulsed current

    International Nuclear Information System (INIS)

    Granada, J.R.; Mayer, R.E.; Guido, G.; Florido, P.C.; Larreteguy, A.; Gillette, V.H.; Patino, N.E.; Converti, J.; Gomez, S.E.

    1990-01-01

    The present work describes the design of a high efficiency thermal neutron detection system and the measurements performed with it on electrolytic cells containing LiH dissolved in D 2 O with palladium cathodes. A procedure involving the use of a non-stationary (pulsed) current through the cell caused a correlated neutron production to be observed in a repeatable manner. These patterns are strongly dependent on the previous charging history of the cathodes. The technique employed seems to be very useful as a research tool for a systematic study of the different variables governing the phenomenon. (author)

  5. Green Chemistry Approach for Synthesis of Effective Anticancer Palladium Nanoparticles.

    Science.gov (United States)

    Gurunathan, Sangiliyandi; Kim, EunSu; Han, Jae Woong; Park, Jung Hyun; Kim, Jin-Hoi

    2015-12-15

    The purpose of this study was to design and synthesize Palladium nanoparticles (PdNPs) using an environmentally friendly approach and evaluate the in vitro efficacy of PdNPs in human ovarian cancer A2780 cells. Ultraviolet-Visible (UV-Vis) spectroscopy was used to monitor the conversion of Pd(II) ions to Pd(0)NPs. X-ray diffraction (XRD) revealed the crystallinity of the as-synthesized PdNPs and Fourier transform infrared spectroscopy (FTIR) further confirmed the role of the leaf extract of Evolvulus alsinoides as a reducing and stabilizing agent for the synthesis of PdNPs. Dynamic light scattering (DLS) and transmission electron microscopy (TEM) showed that the average size of the NPs was 5 nm. After a 24-h exposure to PdNPs, cell viability and light microscopy assays revealed the dose-dependent toxicity of the PdNPs. Furthermore, the dose-dependent cytotoxicity of the PdNPs was confirmed by lactate dehydrogenase (LDH), increased reactive oxygen species (ROS) generation, activation of PdNPs-induced autophagy, impairment of mitochondrial membrane potential (MMP), enhanced caspase-3 activity, and detection of TUNEL-positive cells. Our study demonstrates a single, simple, dependable and green approach for the synthesis of PdNPs using leaf extracts of Evolvulus alsinoides. Furthermore, the in vitro efficacy of PdNPs in human ovarian cancer cells suggests that it could be an effective therapeutic agent for cancer therapy.

  6. Green Chemistry Approach for Synthesis of Effective Anticancer Palladium Nanoparticles

    Directory of Open Access Journals (Sweden)

    Sangiliyandi Gurunathan

    2015-12-01

    Full Text Available The purpose of this study was to design and synthesize Palladium nanoparticles (PdNPs using an environmentally friendly approach and evaluate the in vitro efficacy of PdNPs in human ovarian cancer A2780 cells. Ultraviolet-Visible (UV-Vis spectroscopy was used to monitor the conversion of Pd(II ions to Pd(0NPs. X-ray diffraction (XRD revealed the crystallinity of the as-synthesized PdNPs and Fourier transform infrared spectroscopy (FTIR further confirmed the role of the leaf extract of Evolvulus alsinoides as a reducing and stabilizing agent for the synthesis of PdNPs. Dynamic light scattering (DLS and transmission electron microscopy (TEM showed that the average size of the NPs was 5 nm. After a 24-h exposure to PdNPs, cell viability and light microscopy assays revealed the dose-dependent toxicity of the PdNPs. Furthermore, the dose-dependent cytotoxicity of the PdNPs was confirmed by lactate dehydrogenase (LDH, increased reactive oxygen species (ROS generation, activation of PdNPs-induced autophagy, impairment of mitochondrial membrane potential (MMP, enhanced caspase-3 activity, and detection of TUNEL-positive cells. Our study demonstrates a single, simple, dependable and green approach for the synthesis of PdNPs using leaf extracts of Evolvulus alsinoides. Furthermore, the in vitro efficacy of PdNPs in human ovarian cancer cells suggests that it could be an effective therapeutic agent for cancer therapy.

  7. Detection and analysis of thermal energy loss in the Atucha I nuclear power plant residual heat removal system

    International Nuclear Information System (INIS)

    Berra, Sandra; Guala, Mariana I.; Khon, Hector; Lorenzo, Andrea T.; Raffo Calderon, Maria C.; Urrutia, Guillermo

    1999-01-01

    It is presented the methodology used to detect and to measure energy losses which are existent in the Atucha I nuclear power plant. They were not directly detected, since the magnitude of those was below of the instrumentation precision which is used to measure the electric and thermal power in the plant. To achieve this work temperature special measurements were made. In this way it was possible to quantify the energy losses after operational long periods. (author)

  8. A complementary role of multiparameter flow cytometry and high-throughput sequencing for minimal residual disease detection in chronic lymphocytic leukemia: an European Research Initiative on CLL study.

    LENUS (Irish Health Repository)

    Rawstron, A C

    2016-04-01

    In chronic lymphocytic leukemia (CLL) the level of minimal residual disease (MRD) after therapy is an independent predictor of outcome. Given the increasing number of new agents being explored for CLL therapy, using MRD as a surrogate could greatly reduce the time necessary to assess their efficacy. In this European Research Initiative on CLL (ERIC) project we have identified and validated a flow-cytometric approach to reliably quantitate CLL cells to the level of 0.0010% (10(-5)). The assay comprises a core panel of six markers (i.e. CD19, CD20, CD5, CD43, CD79b and CD81) with a component specification independent of instrument and reagents, which can be locally re-validated using normal peripheral blood. This method is directly comparable to previous ERIC-designed assays and also provides a backbone for investigation of new markers. A parallel analysis of high-throughput sequencing using the ClonoSEQ assay showed good concordance with flow cytometry results at the 0.010% (10(-4)) level, the MRD threshold defined in the 2008 International Workshop on CLL guidelines, but it also provides good linearity to a detection limit of 1 in a million (10(-6)). The combination of both technologies would permit a highly sensitive approach to MRD detection while providing a reproducible and broadly accessible method to quantify residual disease and optimize treatment in CLL.

  9. Highly sensitive in vitro methods for detection of residual undifferentiated cells in retinal pigment epithelial cells derived from human iPS cells.

    Directory of Open Access Journals (Sweden)

    Takuya Kuroda

    Full Text Available Human induced pluripotent stem cells (hiPSCs possess the capabilities of self-renewal and differentiation into multiple cell types, and they are free of the ethical problems associated with human embryonic stem cells (hESCs. These characteristics make hiPSCs a promising choice for future regenerative medicine research. There are significant obstacles, however, preventing the clinical use of hiPSCs. One of the most obvious safety issues is the presence of residual undifferentiated cells that have tumorigenic potential. To locate residual undifferentiated cells, in vivo teratoma formation assays have been performed with immunodeficient animals, which is both costly and time-consuming. Here, we examined three in vitro assay methods to detect undifferentiated cells (designated an in vitro tumorigenicity assay: soft agar colony formation assay, flow cytometry assay and quantitative real-time polymerase chain reaction assay (qRT-PCR. Although the soft agar colony formation assay was unable to detect hiPSCs even in the presence of a ROCK inhibitor that permits survival of dissociated hiPSCs/hESCs, the flow cytometry assay using anti-TRA-1-60 antibody detected 0.1% undifferentiated hiPSCs that were spiked in primary retinal pigment epithelial (RPE cells. Moreover, qRT-PCR with a specific probe and primers was found to detect a trace amount of Lin28 mRNA, which is equivalent to that present in a mixture of a single hiPSC and 5.0×10⁴ RPE cells. Our findings provide highly sensitive and quantitative in vitro assays essential for facilitating safety profiling of hiPSC-derived products for future regenerative medicine research.

  10. Probabilistic reliability analyses to detect weak points in secondary-side residual heat removal systems of KWU PWR plants

    International Nuclear Information System (INIS)

    Schilling, R.

    1984-01-01

    Requirements made by Federal German licensing authorities called for the analysis of the second-side residual heat removal systems of new PWR plants with regard to availability, possible weak points and the balanced nature of the overall system for different incident sequences. Following a description of the generic concept and the process and safety-related systems for steam generator feed and main steam discharge, the reliability of the latter is analyzed for the small break LOCA and emergency power mode incidents, weak points in the process systems are identified, remedial measures of a system-specific and test-strategic nature are presented and their contribution to improving system availability is quantified. A comparison with the results of the German Risk Study on Nuclear Power Plants (GRS) shows a distinct reduction in core meltdown frequency. (orig.)

  11. Reliability analyses to detect weak points in secondary-side residual heat removal systems of KWU PWR plants

    International Nuclear Information System (INIS)

    Schilling, R.

    1983-01-01

    Requirements made by Federal German licensing authorities called for the analysis of the secondary-side residual heat removal systems of new PWR plants with regard to availability, possible weak points and the balanced nature of the overall system for different incident sequences. Following a description of the generic concept and the process and safety-related systems for steam generator feed and main steam discharge, the reliability of the latter is analyzed for the small break LOCA and emergency power mode incidents, weak points in the process systems identified, remedial measures of a system-specific and test-strategic nature presented and their contribution to improving system availability quantified. A comparison with the results of the German Risk Study on Nuclear Power Plants (GRS) shows a distinct reduction in core meltdown frequency. (orig.)

  12. Recovery of Elemental Palladium by Shewanella putrefaciens

    Science.gov (United States)

    Akasaka, S.; Xia, X.; Sawada, K.; Enokida, Y.; Yamamoto, I.; Ohnuki, T.

    2006-12-01

    Microbial reduction of metals plays an important role in environmental behavior and provides a technique for the recovery of metals from industrial wastewater. Recently, demand for platinum group metals (PGMs) increases by their catalytic properties. The extreme rarity of PGMs have led to a growing interest in their recovery. Palladium, one of PGMs, has different oxidation states of Pd(II) and Pd(0). The oxidized form of Pd(II) is soluble, while the reduced form of Pd(0) is insoluble. In this study, microbial reduction of palladium by Fe(III)- reducing bacterium, Shewanella putrefaceins was conducted. This bacterium is known to be capable of reducing metals, such as Mn(IV), U(VI), or Tc(VII) with organic C or H2 as an electron donor. In order to investigate the potential of S. putrefaciens to reduce Pd(II) in solution, resting cells or heat-killed cells were suspended under anaerobic conditions with lactate or H2 as an electron donor. The cells of S. putrefaciens (NBRC3908) were grown in aerobic medium, harvested by centrifugation, and then washed with 25 mmol/dm3 HEPES and 100 mmol/dm3 NaCl (HEPES-NaCl) solution (pH 7.0). The heat-killed cells were autoclaved for 20 min at 121 degrees C. The cell suspension (21.5 mg in dry weight) was resuspended in the HEPES-NaCl solution which contained 1.0 mmol/dm3 Na2PdCl4 (Wako Pure chemical Industries, Ltd). The suspensions were bubbled with N2 for 15 min before 10 mmol/dm3 lactate or 4.8 v/v% H2 was added. The suspensions were then incubated at 30 degrees C. Redox potential (Eh) and pH of the solutions were measured in an inert glove box with Ar gas. Concentration of Pd(II) was measured by Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). Deposited Pd and cells were analyzed by X-ray powder diffraction (XRD) and Scanning Electron Microscope (SEM) with Energy-Dispersive Spectroscopy (EDS). Approximately 86% of Pd(II) of the initial concentration was removed from solution by the resting cells within 24 h when

  13. Expression of the C- KIT Molecule in Acute Myeloid Leukemias: Implications of the Immuno phenotypes CD117 and CD15 in the Detection of Minimal Residual Disease

    International Nuclear Information System (INIS)

    Omar, S.

    2001-01-01

    Study of the c-kit proto-oncogene (CD117) may be of help for the identification of phenotypic profiles that are absent or present at very low frequencies on normal human blast cells and therefore might be of great value for the detection of leukemic cells displaying such immuno phenotypes in patients in complete remission. Design and methods: Ninety patients with acute myeloid leukemias, diagnosed according to FAB criteria and immunological marker studies, were studied for the dual expression on blast cells of the CD117/CD15 immuno phenotype co expression by direct immunofluorescence assay using dual staining combination flow cytometry. Results: In 69/90 acute myeloid leukemia patients analyzed (77%), blast cells expressed the CD117 antigen. Moreover, in 38 of them (42% of acute myeloid leukemia cases), leukemic blasts co expressed the CD117 and CD15 antigens. There was no significant correlation between the FAB classification and the CD117 and CD15 expression in acute myeloid leukemia cases. Conclusions: These results suggest that immunological methods for the detection of MRD based on the existence of aberrant phenotypes could be used in the majority of AML patients. This phenotype CD117/CD15, present in acute myeloid leukemia cases at a relatively high frequency (42%), represents an aberrant phenotype, because it was not detected on normal human blast cells, suggesting that the use of these combinations of monoclonal antibodies could be of help in detecting residual leukemic blasts among normal blast cells. The use of the CD117 antigen in different monoclonal antibodies combinations may be of great help for the detection of minimal residual disease in a high proportion of acute myeloid leukemia cases, especially in those patients displaying the CD117+/CD15+ immuno phenotype, because cells co expressing both antigens in normal blasts, if present, are at very low frequencies. The simultaneous assessment of two or more markers in single cells has facilitated the

  14. Sputtering induced surface composition changes in copper-palladium alloys

    International Nuclear Information System (INIS)

    Sundararaman, M.; Sharma, S.K.; Kumar, L.; Krishnan, R.

    1981-01-01

    It has been observed that, in general, surface composition is different from bulk composition in multicomponent materials as a result of ion beam sputtering. This compositional difference arises from factors like preferential sputtering, radiation induced concentration gradients and the knock-in effect. In the present work, changes in the surface composition of copper-palladium alloys, brought about by argon ion sputtering, have been studied using Auger electron spectroscopy. Argon ion energy has been varied from 500 eV to 5 keV. Enrichment of palladium has been observed in the sputter-altered layer. The palladium enrichment at the surface has been found to be higher for 500 eV argon ion sputtering compared with argon ion sputtering at higher energies. Above 500 eV, the surface composition has been observed to remain the same irrespective of the sputter ion energy for each alloy composition. The bulk composition ratio of palladium to copper has been found to be linearly related to the sputter altered surface composition ratio of palladium to copper. These results are discussed on the basis of recent theories of alloy sputtering. (orig.)

  15. Ageing of palladium tritide: mechanical characterization, helium state and modelling

    International Nuclear Information System (INIS)

    Segard, M.

    2010-01-01

    Palladium is commonly used for the storage of tritium (the hydrogen radioactive isotope), since it forms a low-equilibrium-pressure and reversible tritide. Tritium decay into helium-3 is responsible for the ageing of the tritide, leading to the apparition of helium-3 bubbles for instance. Both experimental and theoretical aspects of this phenomenon are studied here.Previous works on ageing modelling led to two main models, dealing with:- Helium-3 bubbles nucleation (using a cellular automaton), - Bubbles growth (using continuum mechanics).These models were quite efficient, but their use was limited by the lack of input data and fitting experimental parameters.To get through these limitations, this work has consisted in studying the most relevant experimental data to improve the modelling of the palladium tritide ageing.The first part of this work was focused on the assessment of the mechanical properties of the palladium tritide (yield strength, ultimate strength, mechanical behaviour). They were deduced from the in situ tensile tests performed on palladium hydride and deuteride. In the second part, ageing characterization was undertaken, mainly focusing on: - Bubbles observations in palladium tritide using transmission electron microscopy, - Internal bubble pressure measurements using nuclear magnetic resonance, - Macroscopic swelling measurements using pycno-metry.The present work has led to significant progress in ageing understanding and has brought very valuable improvements to the modelling of such a phenomenon. (author) [fr

  16. Atomistic simulation of helium bubble nucleation in palladium

    Energy Technology Data Exchange (ETDEWEB)

    Wang Liang [Department of Applied Physics, Hunan University, Changsha 410082 (China); Hu, Wangyu [Department of Applied Physics, Hunan University, Changsha 410082 (China)], E-mail: wangyuhu2001cn@yahoo.com.cn; Xiao Shifang [Department of Applied Physics, Hunan University, Changsha 410082 (China)], E-mail: sfxiao@yahoo.com.cn; Yang Jianyu [Department of Maths and Physics, Hunan Institute of Engineering, Xiangtan 411104 (China); Deng Huiqiu [Department of Applied Physics, Hunan University, Changsha 410082 (China)

    2009-09-15

    A palladium crystal has been constructed with 11808 atoms. 55 helium atoms occupied the octahedral position of palladium crystal are introduced and retained in a spherical region. Molecular dynamic simulations are performed in a constant temperature and constant volume ensemble (NVT) with temperature controlled by Nose-Hoover thermostat. The interactions between palladium atoms are described with modified analytic embedded atom method (MAEAM), the interactions between palladium atom and helium atom are in the form of Morse potential, and the interactions between helium atoms are in the form of L-J potential function. With the analysis of the radial distribution function (RDF) and microstructure, it reveals that some of helium atoms form a series of clusters with different size, and the nucleation core is random at low temperature, and which is the embryo of helium bubble. Increasing temperature can accelerate the process of bubble nucleation, and the clusters will aggregate and coalesce into a bigger one in which there are no palladium atoms, and it is considered as a helium bubble.

  17. Identification of inorganic improvised explosive devices by analysis of postblast residues using portable capillary electrophoresis instrumentation and indirect photometric detection with a light-emitting diode.

    Science.gov (United States)

    Hutchinson, Joseph P; Evenhuis, Christopher J; Johns, Cameron; Kazarian, Artaches A; Breadmore, Michael C; Macka, Miroslav; Hilder, Emily F; Guijt, Rosanne M; Dicinoski, Greg W; Haddad, Paul R

    2007-09-15

    A commercial portable capillary electrophoresis (CE) instrument has been used to separate inorganic anions and cations found in postblast residues from improvised explosive devices (IEDs) of the type used frequently in terrorism attacks. The purpose of this analysis was to identify the type of explosive used. The CE instrument was modified for use with an in-house miniaturized light-emitting diode (LED) detector to enable sensitive indirect photometric detection to be employed for the detection of 15 anions (acetate, benzoate, carbonate, chlorate, chloride, chlorite, cyanate, fluoride, nitrate, nitrite, perchlorate, phosphate, sulfate, thiocyanate, thiosulfate) and 12 cations (ammonium, monomethylammonium, ethylammonium, potassium, sodium, barium, strontium, magnesium, manganese, calcium, zinc, lead) as the target analytes. These ions are known to be present in postblast residues from inorganic IEDs constructed from ammonium nitrate/fuel oil mixtures, black powder, and chlorate/perchlorate/sugar mixtures. For the analysis of cations, a blue LED (470 nm) was used in conjunction with the highly absorbing cationic dye, chrysoidine (absorption maximum at 453 nm). A nonaqueous background electrolyte comprising 10 mM chrysoidine in methanol was found to give greatly improved baseline stability in comparison to aqueous electrolytes due to the increased solubility of chrysoidine and its decreased adsorption onto the capillary wall. Glacial acetic acid (0.7% v/v) was added to ensure chrysoidine was protonated and to enhance separation selectivity by means of complexation with transition metal ions. The 12 target cations were separated in less than 9.5 min with detection limits of 0.11-2.30 mg/L (calculated at a signal-to-noise ratio of 3). The anions separation system utilized a UV LED (370 nm) in conjunction with an aqueous chromate electrolyte (absorption maximum at 371 nm) consisting of 10 mM chromium(VI) oxide and 10 mM sodium chromate, buffered with 40 mM tris

  18. Metal allergen of the 21st century--a review on exposure, epidemiology and clinical manifestations of palladium allergy

    DEFF Research Database (Denmark)

    Faurschou, Annesofie; Menné, Torkil; Johansen, Jeanne D

    2011-01-01

    Consumers are mainly exposed to palladium from jewellery and dental restorations. Palladium contact allergy is nearly always seen together with nickel allergy, as palladium and nickel tend to cross-react. We aimed to analyse the available palladium patch test data and case reports to determine...

  19. Early recovery of circulating immature B cells in B-lymphoblastic leukemia patients after CD19 targeted CAR T cell therapy: A pitfall for minimal residual disease detection.

    Science.gov (United States)

    Xiao, Wenbin; Salem, Dalia; McCoy, Catharine S; Lee, Daniel; Shah, Nirali N; Stetler-Stevenson, Maryalice; Yuan, Constance M

    2017-09-09

    CD19-targeted chimeric-antigen receptor-modified T-cells (CAR-T) are promising in the treatment of refractory B-lymphoblastic leukemia (B-ALL). Minimal residual disease (MRD) detection by multicolor flow cytometry (FCM) is critical to distinguish B-ALL MRD from regenerating, non-neoplastic B-cell populations. FCM was performed on samples from 9 patients with B-ALL treated with CAR-T. All 9 patients showed response to CAR-T. Additionally, FCM revealed circulating CD10 + B cells, potentially mimicking MRD. Circulating CD10+ B-cells were detected in blood from 3 days to 3 months after CAR-T, comprising 73% (median) of B-cells (52-83%, 95%CI). They expressed CD19, CD10, CD20, bright CD9, CD22, CD24, moderate CD38 and dim CD58, but were CD34 (-), with bright CD45 and polyclonal surface light chain immunoglobulin (sIg) expression. A similar CD10 + B-cell subpopulation was detected by marrow FCM, amidst abundant B-cell precursors. These circulating CD10 + B-cells are compatible with immature B-cells, and are a reflection of B-cell recovery within the marrow. They are immunophenotypically distinguishable from residual B-ALL. Expression of light chain sIg and key surface antigens characterizing regenerating B-cell precursors can distinguish immature B-cells from B-ALL MRD and prevent misdiagnosis. © 2017 International Clinical Cytometry Society. © 2017 International Clinical Cytometry Society.

  20. Superconductivity and the structural phase transitions in palladium hydride and palladium deuteride

    International Nuclear Information System (INIS)

    Standley, R.W.

    1980-01-01

    The results of two experimental studies of the superconducting transition temperature, T/sub c/, of palladium hydride, PdH/sub x/, and palladium deuteride, PdD/sub x/, are presented. In the first study, the superconducting transition temperature of PdH/sub x/(D/sub x/) is studied as a function of H(D) concentration, x, in the temperature range from 0.2 K to 4K. The data join smoothly with those reported previously by Miller and Satterthwaite at higher temperatures, and the composite data are described by the empirical relation T/sub c/ = 150.8 (x-x/sub o/) 2 244 , where x/sub o/ = 0.715 for hydride samples and 0.668 for deuteride samples. The results, when compared with the theoretical predictions of Klein and Papaconstantopoulos, et al., raise questions about the validity of their explanation of the reverse isotope effect, which is based solely on a difference in force constants. In the second study, the effect of the order-disorder structural transition associated with the 50 K anomaly on the superconductivity of PdH/sub x/(D/sub x/) is investigated. Samples were quenched to low temperatures in the disordered state, and their transition temperatures measured. The samples were then annealed just below the anomaly temperature, and the ordering process followed by monitoring the change in sample resistance. The transition temperatures in the ordered state were then measured

  1. Behavior of palladium and its impact on intermetallic growth in palladium-coated Cu wire bonding

    International Nuclear Information System (INIS)

    Xu Hui; Qin, Ivy; Clauberg, Horst; Chylak, Bob; Acoff, Viola L.

    2013-01-01

    This paper describes the behavior of palladium in palladium-coated Cu (PdCu) wire bonding and its impact on bond reliability by utilizing transmission electron microscopy (TEM). A Pd layer approximately 80 nm thick, which is coated on the surface of Cu wire, dissolves into the Cu matrix during ball formation (under N 2 gas protection) when the wire tip is melted to form a ball. As a result of dissolving the very thin Pd layer into the ball, Pd is almost undetectable along the entire bond interface between the ball and the Al pad. The behavior of Pd during thermal aging in air, however, is different for central and peripheral interfaces. At the central interface, less than 5 at.% Pd is present after 168 h aging at 175 °C. At the periphery, however, Pd diffuses back and congregates, reaching a level of ∼12 at.% after 24 h, and a Pd-rich (Cu,Pd) 9 Al 4 layer (>40 at.% Pd) forms after 168 h. Pd acts substitutionally in Cu 9 Al 4 but cannot penetrate into the CuAl 2 or CuAl. By comparison of intermetallic thickness and interfacial morphology between PdCu and bare Cu wire bonds, it is concluded that the presence of Pd reduces intermetallic growth rate, and is associated with numerous nanovoids in PdCu bonds.

  2. Palladium nanoparticles in electrochemical sensing of trace terazosin in human serum and pharmaceutical preparations

    Energy Technology Data Exchange (ETDEWEB)

    Sefid-sefidehkhan, Yasaman [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of); Nekoueian, Khadijeh [Laboratory of Green Chemistry, Faculty of Technology, Lappeenranta University of Technology, Sammonkatu 12, FI-50130 Mikkeli (Finland); Amiri, Mandana, E-mail: mandanaamiri@uma.ac.ir [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of); Sillanpaa, Mika [Laboratory of Green Chemistry, Faculty of Technology, Lappeenranta University of Technology, Sammonkatu 12, FI-50130 Mikkeli (Finland); Eskandari, Habibollah [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of)

    2017-06-01

    In this approach, palladium nanoparticle film was simply fabricated on the surface of carbon paste electrode by electrochemical deposition method. The film was characterized using scanning electron microscopy, electrochemical impedance spectroscopy and cyclic voltammetry. The prepared electrode exhibited an excellent electrocatalytic activity toward detection of trace amounts of terazosin, which is an antihypertensive drug. Under the optimum experimental conditions, a linear range of 1.0 × 10{sup −8}–1.0 × 10{sup −3} mol L{sup −1} with a detection limit of 1.9 × 10{sup −9} mol L{sup −1} was obtained for determination of terazosin using differential pulse voltammetry as a sensitive method. The efficiency of palladium nanoparticle film on the surface of carbon paste electrode successfully proved for determination of terazosin in pharmaceutical sample and human serum sample with promising recovery results. The effect of some foreign species has been studied. - Highlights: • PdNPs were simply fabricated by electrochemical deposition. • PdNPs exhibited an excellent electrocatalytic activity toward oxidation of terazosin. • Terazosin has been determined in pharmaceutical sample and human serum sample.

  3. Superlattices of platinum and palladium nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    MARTIN,JAMES E.; WILCOXON,JESS P.; ODINEK,JUDY G.; PROVENCIO,PAULA P.

    2000-04-06

    The authors have used a nonionic inverse micelle synthesis technique to form nanoclusters of platinum and palladium. These nanoclusters can be rendered hydrophobic or hydrophilic by the appropriate choice of capping ligand. Unlike Au nanoclusters, Pt nanoclusters show great stability with thiol ligands in aqueous media. Alkane thiols, with alkane chains ranging from C{sub 6} to C{sub 18} were used as hydrophobic ligands, and with some of these they were able to form 2-D and/or 3-D superlattices of Pt nanoclusters as small as 2.7 nm in diameter. Image processing techniques were developed to reliably extract from transmission electron micrographs (TEMs) the particle size distribution, and information about the superlattice domains and their boundaries. The latter permits one to compute the intradomain vector pair correlation function of the particle centers, from which they can accurately determine the lattice spacing and the coherent domain size. From these data the gap between the particles in the coherent domains can be determined as a function of the thiol chain length. It is found that as the thiol chain length increases, the gaps between particles within superlattice domains increases, but more slowly than one might expect, possibly indicating thiol chain interdigitation.

  4. Activation and deactivation of neutral palladium(II) phosphinesulfonato polymerization catalysts

    KAUST Repository

    Rünzi, Thomas

    2012-12-10

    polymerization filtrates indicate the presence of (odd- and even-numbered alkyl)(anisyl)phosphine sulfonates (14) and their respective phosphine oxides (15). Furthermore, 2-(vinyl)anisole was detected in NMR tube and reactor polymerizations, which results from ethylene insertion into a palladium-anisyl bond and concomitant β-hydride elimination. In addition to these scrambling reactions, formation of alkanes or fully saturated polymer chains, bis(chelate)palladium complexes [κ2-P,O]2Pd, and palladium black was identified as an irreversible catalyst deactivation pathway. This deactivation proceeds by reaction of palladium alkyl complexes with palladium hydride complexes [κ2-P,O]Pd(H)(L) or by reaction with the free ligand H[P,O] generated by reductive elimination from [κ2-P,O]Pd(H)(L). The model hydride complex 1-H-P tBu3 has been synthesized in order to establish whether 1-H-PtBu3 or H[P,O] is responsible for the irreversible catalyst deactivation. However, upon reaction with 1-(13)CH 3-L or 1-CH2CH3-PPh3, both 1-H-PtBu3 and H[P,O] result in formation of methane or ethane, even though H[P,O] reacts faster than 1-H-PtBu3. DFT calculations show that reductive elimination to form H[P,O] and (alkyl)[P,O] from 1-H/(alkyl)-PtBu3 is kinetically accessible, as is the oxidative readdition of the P-H bond of H[P,O] and the P-anisyl bond of (alkyl)[P,O] to [Pd(PtBu3)2]. These calculations also indicate that for a reaction sequence comprising reductive elimination of H[P,O] from 1-H-PtBu3 and reaction of H[P,O] with 1-CH3-PtBu3, 1-CH3-dmso, or 1-CH2CH3-PPh3 to form methane or ethane, the rate-limiting step is reductive elimination of H[P,O] with a barrier of 124 kJ mol-1. However, a second reaction coordinate was found for the reaction of 1-H-PtBu3 with 1-CH3-P tBu3 or 1-CH3-dmso, which evolves into bimetallic transition-state geometries with a nearly linear H-(CH 3)-Pd alignment and which exhibits a barrier of 131 or 95 kJ mol -1 for the formation of methane. © 2012 American Chemical

  5. Microwave-assisted synthesis of palladium nanocubes and nanobars

    International Nuclear Information System (INIS)

    Yu, Yanchun; Zhao, Yanxi; Huang, Tao; Liu, Hanfan

    2010-01-01

    Microwave was employed in the shape-controlled synthesis of palladium nanoparticles. Palladium nanocubes and nanobars with a mean size of about 23.8 nm were readily synthesized with H 2 PdCl 4 as a precursor, tetraethylene glycol (TEG) as both a solvent and a reducing agent in the presence of PVP and CTAB in 80 s under microwave irradiation. The structures of the as-prepared palladium nanoparticles were characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and ultraviolet-visible (UV-vis) absorption spectroscopy. The formation of PdBr 4 2- due to the coordination replacement of the ligand Cl - ions in PdCl 4 2- ions by Br - ions in the presence of bromide was responsible for the synthesis of Pd nanocubes and nanobars. In addition, a milder reducing power, a higher viscosity and a stronger affinity of TEG were beneficial to the larger sizes of Pd nanocubes and nanobars.

  6. The solubility of palladium(II) bis-dimethylglyoximate

    International Nuclear Information System (INIS)

    Maghzian, R.

    1978-01-01

    The solubility of palladium(II) bis-dimethylglyoximate in different solutions has been determined. Values obtained for the solubility of the palladium complex are tabulated. The solubility is the lowest in water, ammonium acetate and a 25% acetone-water mixture. It is highest in dilute HCl and acetone but precipitation from aqueous acetone should be satisfactory for most purposes if the acetone content of the solvent is roughly less than 50% by volume. The solubility in dilute HCl reflects the concern by previous workers for losses in precipitation from mineral acid. In general, however, the losses are unlikely to be significant unless the quantity of palladium to be precipitated and weighed is small. (T.G.)

  7. Optimization of biological and instrumental detection of explosives and ignitable liquid residues including canines, SPME/ITMS and GC/MSn

    Science.gov (United States)

    Furton, Kenneth G.; Harper, Ross J.; Perr, Jeannette M.; Almirall, Jose R.

    2003-09-01

    A comprehensive study and comparison is underway using biological detectors and instrumental methods for the rapid detection of ignitable liquid residues (ILR) and high explosives. Headspace solid phase microextraction (SPME) has been demonstrated to be an effective sampling method helping to identify active odor signature chemicals used by detector dogs to locate forensic specimens as well as a rapid pre-concentration technique prior to instrumental detection. Common ignitable liquids and common military and industrial explosives have been studied including trinitrotoluene, tetryl, RDX, HMX, EGDN, PETN and nitroglycerine. This study focuses on identifying volatile odor signature chemicals present, which can be used to enhance the level and reliability of detection of ILR and explosives by canines and instrumental methods. While most instrumental methods currently in use focus on particles and on parent organic compounds, which are often involatile, characteristic volatile organics are generally also present and can be exploited to enhance detection particularly for well-concealed devices. Specific examples include the volatile odor chemicals 2-ethyl-1-hexanol and cyclohexanone, which are readily available in the headspace of the high explosive composition C-4; whereas, the active chemical cyclo-1,3,5-trimethylene-2,4,6-trinitramine (RDX) is not. The analysis and identification of these headspace 'fingerprint' organics is followed by double-blind dog trials of the individual components using certified teams in an attempt to isolate and understand the target compounds to which dogs are sensitive. Studies to compare commonly used training aids with the actual target explosive have also been undertaken to determine their suitability and effectiveness. The optimization of solid phase microextraction (SPME) combined with ion trap mobility spectrometry (ITMS) and gas chromatography/mass spectrometry/mass spectrometry (GC/MSn) is detailed including interface development

  8. The Value of PIC Cystography in Detecting De Novo and Residual Vesicoureteral Reflux after Dextranomer/Hyaluronic Acid Copolymer Injection

    Directory of Open Access Journals (Sweden)

    B. W. Palmer

    2011-01-01

    Full Text Available The endoscopic injection of Dx/HA in the management of vesicoureteral reflux (VUR has become an accepted alternative to open surgery. In the current study we evaluated the value of cystography to detect de novo contralateral VUR in unilateral cases of VUR at the time of Dx/HA injection and correlated the findings of immediate post-Dx/HA injection cystography during the same anesthesia to 2-month postoperative VCUG to evaluate its ability to predict successful surgical outcomes. The current study aimed to evaluate whether an intraoperatively performed cystogram could replace postoperative studies. But a negative intraoperative cystogram correlates with the postoperative study in only 80%. Considering the 75–80% success rate of Dx/HA implantation, the addition of intraoperative cystograms cannot replace postoperative studies. In patients treated with unilateral VUR, PIC cystography can detect occult VUR and prevent postoperative contralateral new onset of VUR.

  9. Investigation of radiation-chemical behaviour of divalent palladium in perchloric acid solutions

    International Nuclear Information System (INIS)

    Vladimirova, M.V.; Kalinina, S.V.

    1988-01-01

    Gamma-radiolysis of divalent palladium in perchloric acid solutions is studied. Absorption spectra of intermediate palladium compounds formed in the irradiated solution are taken. The analysis of literature data as well as comparative analysis of the absorption spectra obtained under irradiation of palladium (2) perchloric acid solutions with absorption spectra of palladium chlorocomplexes allows to suppose that the mentioned compounds are chlorocomplexes of palladium (2) of different composition depending on HClO 4 concentration in the initial solution and absorbed radiation dose. Radiation-chemical reduction of palladium (2) up to metal is stated to take place in the whole studied range of initial concentrations of components of the system and dose rates. Kinetic dependences of metallic palladium formation are obtained. Values of radiation-chemical yields of metallic palladium formation depending on the initial concentrations of palladium (2) and perchloric acid are given. A mechanism of radiolytic reduction of palladium (2) in the investigated system is suggested based on the experimental data, and a theoretical value of the radiation-chemical yield of palladium (2) reduction being in a good agreement with experimentally found values is calculated

  10. Detection and assignment of phosphoserine and phosphothreonine residues by {sup 13}C-{sup 31}P spin-echo difference NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    McIntosh, Lawrence P., E-mail: mcintosh@chem.ubc.ca; Kang, Hyun-Seo; Okon, Mark [University of British Columbia, Department of Biochemistry (Canada); Nelson, Mary L.; Graves, Barbara J. [University of Utah, Department of Oncological Sciences, Huntsman Cancer Institute (United States); Brutscher, Bernhard [CNRS, CEA, UJF, Institut de Biologie Structurale Jean-Pierre Ebel (France)], E-mail: bernhard.brutscher@ibs.fr

    2009-01-15

    A simple NMR method is presented for the identification and assignment of phosphorylated serine and threonine residues in {sup 13}C- or {sup 13}C/{sup 15}N-labeled proteins. By exploiting modest ({approx}5 Hz) 2- and 3-bond {sup 13}C-{sup 31}P scalar couplings, the aliphatic {sup 1}H-{sup 13}C signals from phosphoserines and phosphothreonines can be detected selectively in a {sup 31}P spin-echo difference constant time {sup 1}H-{sup 13}C HSQC spectrum. Inclusion of the same {sup 31}P spin-echo element within the {sup 13}C frequency editing period of an intraHNCA or HN(CO)CA experiment allows identification of the amide {sup 1}H{sup N} and {sup 15}N signals of residues (i) for which {sup 13}C{sup {alpha}}(i) or {sup 13}C{sup {alpha}}(i - 1), respectively, are coupled to a phosphate. Furthermore, {sup 31}P resonance assignments can be obtained by applying selective low power cw {sup 31}P decoupling during the spin-echo period. The approach is demonstrated using a PNT domain containing fragment of the transcription factor Ets-1, phosphorylated in vitro at Thr38 and Ser41 with the MAP kinase ERK2.

  11. Hydrogen Production via Steam Reforming of Ethyl Alcohol over Palladium/Indium Oxide Catalyst

    Directory of Open Access Journals (Sweden)

    Tetsuo Umegaki

    2009-01-01

    Full Text Available We report the synergetic effect between palladium and indium oxide on hydrogen production in the steam reforming reaction of ethyl alcohol. The palladium/indium oxide catalyst shows higher hydrogen production rate than indium oxide and palladium. Palladium/indium oxide affords ketonization of ethyl alcohol with negligible by-product carbon monoxide, while indium oxide mainly affords dehydration of ethyl alcohol, and palladium affords decomposition of ethyl alcohol with large amount of by-product carbon monoxide. The catalytic feature of palladium/indium oxide can be ascribed to the formation of palladium-indium intermetallic component during the reaction as confirmed by X-ray diffraction and X-ray photoelectron spectroscopic measurements.

  12. Morphological Study Of Palladium Thin Films Deposited By Sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Salcedo, K L; Rodriguez, C A [Grupo Plasma Laser y Aplicaciones, Ingenieria Fisica, Universidad Tecnologica de Pereira (Colombia); Perez, F A [WNANO, West Virginia University (United States); Riascos, H [Grupo Plasma Laser y Aplicaciones, Departamento de Fisica, Universidad Tecnologica de Pereira (Colombia)

    2011-01-01

    This paper presents a morphological analysis of thin films of palladium (Pd) deposited on a substrate of sapphire (Al{sub 2}O{sub 3}) at a constant pressure of 3.5 mbar at different substrate temperatures (473 K, 523 K and 573 K). The films were morphologically characterized by means of an Atomic Force Microscopy (AFM); finding a relation between the roughness and the temperature. A morphological analysis of the samples through AFM was carried out and the roughness was measured by simulating the X-ray reflectivity curve using GenX software. A direct relation between the experimental and simulation data of the Palladium thin films was found.

  13. Morphological Study Of Palladium Thin Films Deposited By Sputtering

    International Nuclear Information System (INIS)

    Salcedo, K L; Rodriguez, C A; Perez, F A; Riascos, H

    2011-01-01

    This paper presents a morphological analysis of thin films of palladium (Pd) deposited on a substrate of sapphire (Al 2 O 3 ) at a constant pressure of 3.5 mbar at different substrate temperatures (473 K, 523 K and 573 K). The films were morphologically characterized by means of an Atomic Force Microscopy (AFM); finding a relation between the roughness and the temperature. A morphological analysis of the samples through AFM was carried out and the roughness was measured by simulating the X-ray reflectivity curve using GenX software. A direct relation between the experimental and simulation data of the Palladium thin films was found.

  14. Chemical recovery of palladium-103 from irradiated silver target

    International Nuclear Information System (INIS)

    Lapshina, E.V.; Kokhanyuk, V.M.; Zhuikov, B.L.; Myasoedova, G.V.; Zakhartchenko, E.A.; Phillips, D.R.; Jamriska, D.J.

    2003-01-01

    The goal of this work is to develop an extraction method of no-carrier-added palladium-103 from silver. Metallic silver targets may be irradiated by protons with energy of 60-200 MeV or more to generate palladium-103 simultaneously with other radioactive isotopes of rhodium, ruthenium, technetium, palladium and silver. According to the dependence experimental production yield of Pd-103 and isotopes of other elements in thick silver target vs. Proton energy the most suitable energy for maximum yield of Pd-103 and minimum yield of other elements is from about 100 to about 140 MeV. Activity of radionuclides produced in silver target depends from many factors (target thickness, irradiation time, etc.). Two methods of Pd-103 recovering from irradiated silver target are considered in this work: (1) Silver target is dissolved in nitric acid followed by silver precipitation in the form of silver chloride by addition of HCl. The solution containing Pd, Rh and other radionuclides is passed through the layer of fibrous sorbent POLYORGS-15n. Then the sorbent is washed and Pd is desorbed by hot 12 M hydrochloric acid; (2) Silver target is dissolved in nitric acid followed by passing of the obtained solution (2 M HNO 3 ) through a disk set of complex forming sorbent POLYORGS-33n. Under these conditions palladium is sorbed by the sorbent while silver, rhodium, ruthenium and technetium are passed through the sorbent. Then the sorbent is washed with 2M nitric acid, and Pd is desorbed by 12 M hydrochloric acid. Extraction of palladium is occurred during the formation of palladium complex with a chelate sorbent specific to palladium in acidic solutions. Such a sorbent makes possible separation of palladium from accompanying radionuclides such as rhodium, ruthenium and technetium. The polymeric complex-forming sorbent of fibrous structure with the groups of 3(5)-methylpyrazole (POLYORGS-15) is used. The distinctive feature of the sorbents in the form of fibrous 'filled' material is

  15. Establishment of a novel immunoassay system for rapid detection of 2,4-dichlorophenoxyacetic acid residues based on magnetic-fluorescent probes

    Directory of Open Access Journals (Sweden)

    WANG Yuanfeng

    2014-12-01

    Full Text Available A novel immunoassay system based on magnetic-fluorescent probes was established to detect 2.4-dichlorophenoxyacetic acid (2,4-D residue in liquid system in food and agricultural products.The composites of anti-2,4-D antibody bound to Fe3O4@SiO2-NH2 was employed as the solid phase as well as magnetic probe.The composites composed of 2,4-D-OVA labeled with CdTe@SiO2-NH2 as the fluorescent probe was used to produce fluorescent signal.2,4-D and its fluorescent probe competed binding the antibody on the surface of the magnetic probe.The optimization of 2,4-D-OVA dosage,coupling PH and reaction time in preparing the fluorescent probe were investigated.It showed that in the synthesis of fluorescent probe 8.2 was the optimal pH,70 min was the optimal coupling time,500 μL amount of 2,4-D-OVA.The standard curve was obtained with the concentration of 2,4-D and the maximum fluorescence intensity.The detection limit of the assay was gotten and it was 3.55×10-8.One reaction step and one washing step were needed.The assay significantly shortened the testing time and amplified the detection signal compared with classic ELISA.

  16. Development of a new method for the determination of residues of the neonictinoid insecticide imidacloprid in juvenile Chinook (Oncorhynchus tyshawytscha) using ELISA detection

    Science.gov (United States)

    Frew, John A.; Grue, Christian E.

    2012-01-01

    The neonicotinoid insecticide imidacloprid (IMI) has been proposed as an alternative to carbaryl for controlling indigenous burrowing shrimp on commercial oyster beds in Willapa Bay and Grays Harbor, Washington. A focus of concern over the use of this insecticide in an aquatic environment is the potential for adverse effects from exposure to non-target species residing in the Bay, such as juvenile Chinook (Oncorhynchus tshawytscha) and cutthroat trout (O. clarki). Federal registration and State permiting approval for the use of IMI will require confirmation that the compound does not adversely impact these salmonids following field applications. This will necessitate an environmental monitoring program for evaluating exposure in salmonids following the treatment of beds. Quantification of IMI residues in tissue can be used for determining salmonid exposure to the insecticide. Refinement of an existing protocol using liquid-chromatography mass spectrometry (LC-MS) detection would provide the low limits of quantification, given the relatively small tissue sample sizes, necessary for determining exposure in individual fish. Such an approach would not be viable for the environmental monitoring effort in Willapa Bay and Grays Harbor due to the high costs associated with running multiple analyses, however. A new sample preparation protocol was developed for use with a commercially available enzyme-linked immunosorbent assay (ELISA) for the quantification of IMI, thereby providing a low-cost alternative to LC-MS for environmental monitoring in Willapa Bay and Grays Harbor. Extraction of the analyte from the salmonid brain tissue was achieved by Dounce homogenization in 4.0 mL of 20.0 mM Triton X-100, followed by a 6 h incubation at 50–55 °C. Centrifugal ultrafiltration and reversed phase solid phase extraction were used for sample cleanup. The limit of quantification for an average 77.0 mg whole brain sample was calculated at 18.2 μg kg-1 (ppb) with an average

  17. A simple and fast detection method for bovine milk residues in foods: a 2-site monoclonal antibody immunochromatography assay.

    Science.gov (United States)

    Xuli, Wu; Weiyi, He; Ji, Kunmei; Wenpu, Wan; Dongsheng, Hu; Hui, Wu; Xinpin, Luo; Zhigang, Liu

    2013-03-01

    The ingredient declaration on food labels assumes paramount importance in the protection of food-allergic consumers. China has not implemented Food allergen labeling. A gold immunochromatography assay (GICA) was developed using 2 monoclonal antibodies (mAb) against the milk allergen β-lactoglobulin in this study. The GICA was specific for pure milk samples with a sensitivity of 0.2 ng/mL. Milk protein traces extracted from 110 food products were detected by this method. The labels of 106 were confirmed by our GICA method: 57 food samples originally labeled as containing milk were positive for β-lactoglobulin and 49 food samples labeled as not containing milk were negative for β-lactoglobulin. However, 3 food samples falsely labeled as containing milk were found to contain no β-lactoglobulin whereas 1 food sample labeled as not containing milk actually contained β-lactoglobulin. First, these negatives could be because of the addition of a casein fraction. Second, some countries demand that food manufacturers label all ingredients derived from milk as "containing milk" even though the ingredients contain no detectable milk protein by any method. Our GICA method could thus provide a fast and simple method for semiquantitatation of β-lactoglobulin in foods. The present method provides a fast, simple, semiquantitative method for the determination of milk allergens in foods. © 2013 Institute of Food Technologists®

  18. Accelerating Palladium Nanowire H2 Sensors Using Engineered Nanofiltration.

    Science.gov (United States)

    Koo, Won-Tae; Qiao, Shaopeng; Ogata, Alana F; Jha, Gaurav; Jang, Ji-Soo; Chen, Vivian T; Kim, Il-Doo; Penner, Reginald M

    2017-09-26

    The oxygen, O 2 , in air interferes with the detection of H 2 by palladium (Pd)-based H 2 sensors, including Pd nanowires (NWs), depressing the sensitivity and retarding the response/recovery speed in air-relative to N 2 or Ar. Here, we describe the preparation of H 2 sensors in which a nanofiltration layer consisting of a Zn metal-organic framework (MOF) is assembled onto Pd NWs. Polyhedron particles of Zn-based zeolite imidazole framework (ZIF-8) were synthesized on lithographically patterned Pd NWs, leading to the creation of ZIF-8/Pd NW bilayered H 2 sensors. The ZIF-8 filter has many micropores (0.34 nm for gas diffusion) which allows for the predominant penetration of hydrogen molecules with a kinetic diameter of 0.289 nm, whereas relatively larger gas molecules including oxygen (0.345 nm) and nitrogen (0.364 nm) in air are effectively screened, resulting in superior hydrogen sensing properties. Very importantly, the Pd NWs filtered by ZIF-8 membrane (Pd NWs@ZIF-8) reduced the H 2 response amplitude slightly (ΔR/R 0 = 3.5% to 1% of H 2 versus 5.9% for Pd NWs) and showed 20-fold faster recovery (7 s to 1% of H 2 ) and response (10 s to 1% of H 2 ) speed compared to that of pristine Pd NWs (164 s for response and 229 s for recovery to 1% of H 2 ). These outstanding results, which are mainly attributed to the molecular sieving and acceleration effect of ZIF-8 covered on Pd NWs, rank highest in H 2 sensing speed among room-temperature Pd-based H 2 sensors.

  19. A simple method to deposit palladium doped SnO2 thin films using plasma enhanced chemical vapor deposition technique

    International Nuclear Information System (INIS)

    Kim, Young Soon; Wahab, Rizwan; Shin, Hyung-Shik; Ansari, S. G.; Ansari, Z. A.

    2010-01-01

    This work presents a simple method to deposit palladium doped tin oxide (SnO 2 ) thin films using modified plasma enhanced chemical vapor deposition as a function of deposition temperature at a radio frequency plasma power of 150 W. Stannic chloride (SnCl 4 ) was used as precursor and oxygen (O 2 , 100 SCCM) (SCCM denotes cubic centimeter per minute at STP) as reactant gas. Palladium hexafluroacetyleacetonate (Pd(C 5 HF 6 O 2 ) 2 ) was used as a precursor for palladium. Fine granular morphology was observed with tetragonal rutile structure. A peak related to Pd 2 Sn is observed, whose intensity increases slightly with deposition temperature. Electrical resistivity value decreased from 8.6 to 0.9 mΩ cm as a function of deposition temperature from 400 to 600 deg. C. Photoelectron peaks related to Sn 3d, Sn 3p3, Sn 4d, O 1s, and C 1s were detected with varying intensities as a function of deposition temperature.

  20. Residual stresses

    International Nuclear Information System (INIS)

    Sahotra, I.M.

    2006-01-01

    The principal effect of unloading a material strained into the plastic range is to create a permanent set (plastic deformation), which if restricted somehow, gives rise to a system of self-balancing within the same member or reaction balanced by other members of the structure., known as residual stresses. These stresses stay there as locked-in stresses, in the body or a part of it in the absence of any external loading. Residual stresses are induced during hot-rolling and welding differential cooling, cold-forming and extruding: cold straightening and spot heating, fabrication and forced fitting of components constraining the structure to a particular geometry. The areas which cool more quickly develop residual compressive stresses, while the slower cooling areas develop residual tensile stresses, and a self-balancing or reaction balanced system of residual stresses is formed. The phenomenon of residual stresses is the most challenging in its application in surface modification techniques determining endurance mechanism against fracture and fatigue failures. This paper discusses the mechanism of residual stresses, that how the residual stresses are fanned and what their behavior is under the action of external forces. Such as in the case of a circular bar under limit torque, rectangular beam under limt moment, reclaiming of shafts welds and peening etc. (author)

  1. Dynamic contrast-enhanced MRI for automatic detection of foci @]@of residual or recurrent disease after prostatectomy

    Energy Technology Data Exchange (ETDEWEB)

    Parra, N.A.; Orman, Amber; Abramowitz, Matthew; Pollack, Alan; Stoyanova, Radka [University of Miami Miller School of Medicine, Department of Radiation Oncology, Miami, FL (United States); Padgett, Kyle [University of Miami Miller School of Medicine, Department of Radiation Oncology, Miami, FL (United States); University of Miami Miller School of Medicine, Department of Radiology, Miami, FL (United States); Casillas, Victor [University of Miami Miller School of Medicine, Department of Radiology, Miami, FL (United States); Punnen, Sanoj [University of Miami Miller School of Medicine, Department of Urology, Miami, FL (United States)

    2017-01-15

    This study aimed to develop an automated procedure for identifying suspicious foci of residual/recurrent disease in the prostate bed using dynamic contrast-enhanced-MRI (DCE-MRI) in prostate cancer patients after prostatectomy. Data of 22 patients presenting for salvage radiotherapy (RT) with an identified gross tumor volume (GTV) in the prostate bed were analyzed retrospectively. An unsupervised pattern recognition method was used to analyze DCE-MRI curves from the prostate bed. Data were represented as a product of a number of signal-vs.-time patterns and their weights. The temporal pattern, characterized by fast wash-in and gradual wash-out, was considered the ''tumor'' pattern. The corresponding weights were thresholded based on the number (1, 1.5, 2, 2.5) of standard deviations away from the mean, denoted as DCE1.0,.., DCE2.5, and displayed on the T2-weighted MRI. The resultant four volumes were compared with the GTV and maximum pre-RT prostate-specific antigen (PSA) level. Pharmacokinetic modeling was also carried out. Principal component analysis determined 2-4 significant patterns in patients' DCE-MRI. Analysis and display of the identified suspicious foci was performed in commercial software (MIM Corporation, Cleveland, OH, USA). In general, DCE1.0/DCE1.5 highlighted larger areas than GTV. DCE2.0 and GTV were significantly correlated (r = 0.60, p < 0.05). DCE2.0/DCA2.5 were also significantly correlated with PSA (r = 0.52, 0.67, p < 0.05). K{sup trans} for DCE2.5 was statistically higher than the GTV's K{sup trans} (p < 0.05), indicating that the automatic volume better captures areas of malignancy. A software tool was developed for identification and visualization of the suspicious foci in DCE-MRI from post-prostatectomy patients and was integrated into the treatment planning system. (orig.) [German] Entwicklung eines automatischen Analyseverfahrens, um nach Prostatektomie mittels dynamischer kontrastmittelverstaerkter

  2. Ibuprofen analysis in blood samples by palladium particles-impregnated sodium montmorillonite electrodes: Validation using high performance liquid chromatography.

    Science.gov (United States)

    Loudiki, A; Boumya, W; Hammani, H; Nasrellah, H; El Bouabi, Y; Zeroual, M; Farahi, A; Lahrich, S; Hnini, K; Achak, M; Bakasse, M; El Mhammedi, M A

    2016-12-01

    The electrochemical detection of ibuprofen has been studied on Palladium-Montmorillonite (Mt) modified carbon paste electrode using differential pulse voltammetry. The optimization of the modifier preparation and the instrumental parameters was investigated. The results indicate that ibuprofen oxidation was favored in the presence of Pd-PdO particles. The quantitative determination of ibuprofen was statistically analyzed and validated using HPLC method. The detection and quantification limits, specificity and precision were found to be acceptable. Finally, the developed method was successfully applied for ibuprofen determination in human blood samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. A supersensitive silver nanoprobe based aptasensor for low cost detection of malathion residues in water and food samples

    Science.gov (United States)

    Bala, Rajni; Mittal, Sherry; Sharma, Rohit K.; Wangoo, Nishima

    2018-05-01

    In the present study, we report a highly sensitive, rapid and low cost colorimetric monitoring of malathion (an organophosphate insecticide) employing a basic hexapeptide, malathion specific aptamer (oligonucleotide) and silver nanoparticles (AgNPs) as a nanoprobe. AgNPs are made to interact with the aptamer and peptide to give different optical responses depending upon the presence or absence of malathion. The nanoparticles remain yellow in color in the absence of malathion owing to the binding of aptamer with peptide which otherwise tends to aggregate the particles because of charge based interactions. In the presence of malathion, the agglomeration of the particles occurs which turns the solution orange. Furthermore, the developed aptasensor was successfully applied to detect malathion in various water samples and apple. The detection offered high recoveries in the range of 89-120% with the relative standard deviation within 2.98-4.78%. The proposed methodology exhibited excellent selectivity and a very low limit of detection i.e. 0.5 pM was achieved. The developed facile, rapid and low cost silver nanoprobe based on aptamer and peptide proved to be potentially applicable for highly selective and sensitive colorimetric sensing of trace levels of malathion in complex environmental samples. Figure S2. HPLC Chromatogram of KKKRRR. Figure S3. UV- Visible spectra of AgNPs in the presence of increasing peptide concentrations. Inset shows respective color changes of AgNPs with peptide concentrations ranging from 0.1 mM to 100 mM (a to e). Figure S4. UV- Visible spectra of AgNPs in the presence 10 mM peptide and varying aptamer concentrations. Inset shows the corresponding color changes. a to e shows aptamer concentrations ranging from 10 nM to 1000 nM. Figure S5. Interference Studies. Ratio of A520 nm/390 nm of AgNPs in the presence of 10 mM peptide, 500 nM aptamer, 0.5 nM malathion and 0.5 mM interfering components i.e. sodium, potassium, calcium, alanine, arginine

  4. RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Mohammad Rezaee

    2015-05-01

    Full Text Available A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA followed by graphite furnace atomic absorption spectrometry (GFAAS. Ammonium pyrrolidine dithiocarbamate (APDC was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

  5. Cloud point extraction of palladium in water samples and alloy mixtures using new synthesized reagent with flame atomic absorption spectrometry (FAAS)

    International Nuclear Information System (INIS)

    Priya, B. Krishna; Subrahmanayam, P.; Suvardhan, K.; Kumar, K. Suresh; Rekha, D.; Rao, A. Venkata; Rao, G.C.; Chiranjeevi, P.

    2007-01-01

    The present paper outlines novel, simple and sensitive method for the determination of palladium by flame atomic absorption spectrometry (FAAS) after separation and preconcentration by cloud point extraction (CPE). The cloud point methodology was successfully applied for palladium determination by using new reagent 4-(2-naphthalenyl)thiozol-2yl azo chromotropic acid (NTACA) and hydrophobic ligand Triton X-114 as chelating agent and nonionic surfactant respectively in the water samples and alloys. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. The preconcentration factor was found to be (50-fold) for 250 ml of water sample. Under optimum condition the detection limit was found as 0.067 ng ml -1 for palladium in various environmental matrices. The present method was applied for the determination of palladium in various water samples, alloys and the result shows good agreement with reported method and the recoveries are in the range of 96.7-99.4%

  6. Simultaneous determination of palladium, platinum and rhodium by on-line column enrichment and HPLC with 2,4-dihydroxybenzylidenethiorhodanine as pre-column derivatization reagent

    Directory of Open Access Journals (Sweden)

    Dong Xuechang

    2006-01-01

    Full Text Available A new method for the simultaneous determination of palladium, platinum and rhodium ions as metal-DHBTR chelates was developed. The palladium, platinum and rhodium ions were pre-column derivatized with 2,4-dihydroxybenzylidenethiorhodanine (DHBTR to form colored chelates. The Pd-DHBTR, Pt-DHBTR and Rh-DHBTR chelates can be absorbed onto the front of the enrichment column when they were injected into the injector and sent to the enrichment column with a 0.05 mol L-1 sodium acetate-acetic acid buffer solution (pH 3.5 as mobile phase. After the enrichment had finished, by switching the six ports switching valve, the retained chelates were back-flushed by mobile phase and traveling towards the analytical column. These chelates separation on the analytical column was satisfactory with 62% (v/v acetonitrile (containing 0.05 mol L-1 of pH 3.5 sodium acetate-acetic acid buffer salt and 0.1% (m/v of tritonX-100 as mobile phase. The Limits of detection of palladium, platinum and rhodium are 3.6 ng L-1, 3.2 ng L-1 and 4.5 ng L-1, respectively. This method was applied to the determination of palladium, platinum and rhodium in water, urine and soil samples with good results.

  7. {sup 18}F-FDG PET/CT for detection and localization of residual or recurrent disease in patients with multiple myeloma after stem cell transplantation

    Energy Technology Data Exchange (ETDEWEB)

    Derlin, Thorsten; Wisotzki, Christian; Klutmann, Susanne [University Medical Center Hamburg-Eppendorf, Department of Nuclear Medicine, Hamburg (Germany); Weber, Christoph; Habermann, Christian R.; Herrmann, Jochen [University Medical Center Hamburg-Eppendorf, Department of Diagnostic and Interventional Radiology, Hamburg (Germany); Ayuk, Francis; Wolschke, Christine; Kroeger, Nicolaus [University Medical Center Hamburg-Eppendorf, Clinic for Stem Cell Transplantation, Hamburg (Germany)

    2012-03-15

    The aim of the study was to determine the diagnostic performance of {sup 18}F-fluorodeoxyglucose (FDG) positron emission tomography (PET)/CT for the detection and localization of residual or recurrent disease in patients with multiple myeloma (MM) after stem cell transplantation. A total of 197 whole-body {sup 18}F-FDG PET/CT scans were performed in 99 patients with MM at different time points in the course of disease after autologous or allogeneic stem cell transplantation. Post-transplant PET/CT scans and clinical remission status as determined by the clinical gold standard (Uniform Response Criteria) were analysed and compared. A total of 576 focal osseous and extramedullary lesions were detected in 79 scans. Additional diffuse bone marrow involvement was detected in 17 patients. {sup 18}F-FDG PET/CT had a sensitivity of 54.6%, a specificity of 82.1%, a positive predictive value of 82.3%, a negative predictive value of 54.2% and an overall accuracy of 65.5%. The sensitivity of {sup 18}F-FDG PET/CT was shown to depend on the disease category according to the Uniform Response Criteria for myeloma. In patients with MM in the post-transplant setting, {sup 18}F-FDG PET/CT may (1) contribute to the detection and localization of disease, (2) provide information about the extent of distinct myeloma manifestations and the total disease burden and (3) add information about the metabolic activity of disease, but (4) has substantially lower sensitivity for this purpose compared to the pretreatment setting. (orig.)

  8. Hydrogen uptake causes molecular "avalanches" in palladium | Argonne

    Science.gov (United States)

    air cylinders for storing the gas. Palladium, a precious metal closely related to platinum, is that storage or purification, and this research gets us closer to making that a reality. In this study take up hydrogen from the environment. "The ultimate goal is hydrogen storage or purification, and

  9. XPS study of palladium sensitized nano porous silicon thin film

    Indian Academy of Sciences (India)

    Keywords. Porous silicon; passivation; palladium; oxidation; XPS. Abstract. Nano porous silicon (PS) was formed on -type monocrystalline silicon of 2–5 cm resistivity and (100) orientation by electrochemical anodization method using HF and ethanol as the electrolytes. High density of surface states, arising due to its ...

  10. Absorption of hydrogen by vanadium-palladium alloys

    International Nuclear Information System (INIS)

    Artman, D.; Lynch, J.F.; Flanagan, T.B.

    1976-01-01

    Pressure composition isotherms (273-373 K) have been determined for the absorption of hydrogen by a series of six palladium alloys (f.c.c) in the composition range from 1 to 8 at.% vanadium. At a given hydrogen content, the equilibrium hydrogen pressure progressively increases with vanadium content. Thermodynamic parameters for the absorption of hydrogen are reported at infinite dilution of hydrogen and for the formation of the nonstoichiometric hydride from the hydrogen-saturated alloy. The relative, partial molar enthalpy of solution of hydrogen at infinite dilution increases slightly with vanadium content. The presence of vanadium, which absorbs hydrogen itself in its normal b.c.c. structure, greatly inhibits the ability of palladium to absorb hydrogen. For example, the isobaric solubility of hydrogen (1 atm, 298K) decreases from H/Pd=0.7 (palladium) to 0.024 (V(6%)-Pd). The lattice expansion due to the presence of interstitial hydrogen has been determined by X-ray diffraction. From these data it can be concluded that the formation of two non-stoichiometric hydride phases does not occur at vanadium contents greater that 5 at.% (298 K). Electrical resistance has been measured as a function of the hydrogen content of the alloys. The electrical resistance increases more markedly with hydrogen content for these alloys than for any of the palladium alloys previously examined. (Auth.)

  11. Microscopic observations of palladium used for cold fusion

    International Nuclear Information System (INIS)

    Matsumoto, T.

    1991-01-01

    This paper examines the microscopic structures of palladium metals used for cold fusion experiments. Tiny spot defects suggesting cold fusion have been observed in grain boundaries as the Nattoh model predicts. The relationship between these defects and a series of neutron busts and an indirect loop of hydrogen chain reactions are discussed

  12. Palladium-based nanocatalysts for alcohol electrooxidation in alkaline media

    CSIR Research Space (South Africa)

    Modibedi, RM

    2013-01-01

    Full Text Available in the electrocatalytic oxidation of alcohols in alkaline media compared to platinum catalysts. Recent efforts have focused on the discovery of palladium-based electrocatalysts with little or no platinum for oxygen reduction reaction (ORR). This chapter is an overview...

  13. ERRATUM Study of microstructure in vanadium–palladium alloys by ...

    Indian Academy of Sciences (India)

    WINTEC

    ERRATUM. Study of microstructure in vanadium–palladium alloys by X-ray diffraction technique. J Ghosh, S K Chattopadhyay, A K Meikap, S K Chatterjee and P Chatterjee 2007 Bull. Mater. Sci. 30 447–454. In page 448, under §2.1 Warren–Averbach method, after equation (1), the sentence starting with “Then the domain ...

  14. Fractal analysis of electrolytically-deposited palladium hydride dendrites

    International Nuclear Information System (INIS)

    Bursill, L.A.; Julin, Peng; Xudong, Fan.

    1990-01-01

    The fractal scaling characteristics of the surface profile of electrolytically-deposited palladium hydride dendritic structures have been obtained using conventional and high resolution transmission electron microscopy. The results are in remarkable agreement with the modified diffusion-limited aggregation model. 19 refs., 3 tabs., 13 figs

  15. Palladium-catalyzed allylation of tautomerizable heterocycles with alkynes.

    Science.gov (United States)

    Lu, Chuan-Jun; Chen, Dong-Kai; Chen, Hong; Wang, Hong; Jin, Hongwei; Huang, Xifu; Gao, Jianrong

    2017-07-21

    A method for the allylic amidation of tautomerizable heterocycles was developed by a palladium catalyzed allylation reaction with 100% atom economy. A series of structurally diverse N-allylic substituted heterocycles can be synthesized in good yields with high chemo-, regio-, and stereoselectivities under mild conditions.

  16. Supporting Information Palladium Complexes of a New Type of N ...

    Indian Academy of Sciences (India)

    Prasenjit Ghosh

    Palladium Complexes of a New Type of N-heterocyclic Carbene. Ligand Derived From a Tricyclic Triazolooxazine Framework. Manoj Kumar Gangwar, Alok Ch. Kalita and Prasenjit Ghosh*. Department of Chemistry,. Indian Institute of Technology Bombay, ... 2. Figure S1. 1. H NMR spectrum of the compound 1a in CDCl3.

  17. Electronic structure of palladium and its relation to uv spectroscopy

    DEFF Research Database (Denmark)

    Christensen, N.E.

    1976-01-01

    The electronic-energy-band structure of palladium has been calculated by means of the relativistic augmented-plane-wave method covering energies up to 30 eV above the Fermi level. The optical interband transitions producing structure in the dielectric function up to photon energies of 25 eV have ...

  18. Exposure to nickel and palladium from dental appliances

    NARCIS (Netherlands)

    Ventura Da Cruz Rodrigues Milheiro, A.M.

    2015-01-01

    The application of a dental material into the oral cavity is not free of biological implications, as deterioration of the material will undoubtedly occur. The adverse health effects of palladium and nickel are well known and their immunologic cross-reactivity is well established. The aim of this

  19. Study of electroplated silver-palladium biofouling inhibiting coating

    DEFF Research Database (Denmark)

    Chiang, Wen-Chi; Hilbert, Lisbeth Rischel; Schroll, Casper

    2008-01-01

    Biofouling can cause many undesirable effects in industrial and medical settings. In this study, a new biofouling inhibiting Ag-Pd surface was designed to form an inhibiting effect by itself. This design was based on silver combined with nobler palladium, both with catalytic properties. Owing to ...

  20. Confined palladium colloids in mesoporous frameworks for carbon nanotube growth

    NARCIS (Netherlands)

    Berenguer-Murcia, A.; Rebrov, E.V.; Cabaj, M.; Wheatley, A.E.H.; Johnson, B.F.G.; Robertson, J.; Schouten, J.C.

    2009-01-01

    Palladium colloidal nanoparticles with an average size of approximately 2.4 nm have been incorporated into mesoporous inorganic thin films following a multistep approach. This involves the deposition of mesoporous titania thin films with a thickness of 200 nm by spin-coating on titanium plates with

  1. Residual stresses

    International Nuclear Information System (INIS)

    Macherauch, E.

    1978-01-01

    Residual stresses are stresses which exist in a material without the influence of external powers and moments. They come into existence when the volume of a material constantly changes its form as a consequence of mechanical, thermal, and/or chemical processes and is hindered by neighbouring volumes. Bodies with residual stress are in mechanical balance. These residual stresses can be manifested by means of all mechanical interventions disturbing this balance. Acoustical, optical, radiological, and magnetical methods involving material changes caused by residual stress can also serve for determining residual stress. Residual stresses have an ambivalent character. In technical practice, they are feared and liked at the same time. They cause trouble because they can be the cause for unexpected behaviour of construction elements. They are feared since they can cause failure, in the worst case with catastrophical consequences. They are appreciated, on the other hand, because, in many cases, they can contribute to improvements of the material behaviour under certain circumstances. But they are especially liked for their giving convenient and (this is most important) mostly uncontrollable explanations. For only in very few cases we have enough knowledge and possibilities for the objective evaluation of residual stresses. (orig.) [de

  2. Growth and sedimentation of fine particles produced in aqueous solutions of palladium sulfate and palladium sulfate-silver sulfate induced by gamma-ray irradiation

    International Nuclear Information System (INIS)

    Hatada, Motoyoshi; Jonah, C.D.

    1994-10-01

    It is known that palladium and palladium-silver fine particles were formed from deaerated aqueous solutions of palladium sulfate and palladium sulfate-silver sulfate induced by gamma-ray irradiation. Changes in particle size and with amount of particles in the solution with time during and after irradiation were studied using dynamic light scattering technique and UV spectrophotometer. The particles formed from palladium sulfate solution are found to be water-filled bulky particles of diameter of 200 nm, which grow by mutual coagulation even after irradiation was terminated. Average density depends on concentration of palladium ion in the solution and dose, and the lowest density was about 2 g/cm 3 for particles of 200 nm obtained from 0.06 mM solution by 2.4 kGy irradiation. The average density of the particles obtained from palladium sulfate-silver sulfate solutions was smaller than those obtained for the corresponding palladium sulfate solutions. Supersonic agitation destroyed coagulated precipitates to form fine particles, but did not form clusters of a few atoms. (author)

  3. Palladium-Catalyzed Atom-Transfer Radical Cyclization at Remote Unactivated C(sp3 )-H Sites: Hydrogen-Atom Transfer of Hybrid Vinyl Palladium Radical Intermediates.

    Science.gov (United States)

    Ratushnyy, Maxim; Parasram, Marvin; Wang, Yang; Gevorgyan, Vladimir

    2018-03-01

    A novel mild, visible-light-induced palladium-catalyzed hydrogen atom translocation/atom-transfer radical cyclization (HAT/ATRC) cascade has been developed. This protocol involves a 1,5-HAT process of previously unknown hybrid vinyl palladium radical intermediates, thus leading to iodomethyl carbo- and heterocyclic structures. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Fast detection and characterization of organic and inorganic gunshot residues on the hands of suspects by CMV-GC-MS and LIBS.

    Science.gov (United States)

    Tarifa, Anamary; Almirall, José R

    2015-05-01

    A rapid method for the characterization of both organic and inorganic components of gunshot residues (GSR) is proposed as an alternative tool to facilitate the identification of a suspected shooter. In this study, two fast screening methods were developed and optimized for the detection of organic compounds and inorganic components indicative of GSR presence on the hands of shooters and non-shooters. The proposed methods consist of headspace extraction of volatile organic compounds using a capillary microextraction of volatiles (CMV) device previously reported as a high-efficiency sampler followed by detection by GC-MS. This novel sampling technique has the potential to yield fast results (LIBS) screening method for the detection of the inorganic components indicative of the presence of GSR (Sb, Pb and Ba) is described. The sampling method for the inorganics consists of liquid extraction of the target elements from the same cotton swabs (previously analyzed for VOCs) and an additional 30 swab samples followed by spiking 1μL of the extract solution onto a Teflon disk and then analyzed by LIBS. Advantages of LIBS include fast analysis (~12s per sample) and high selectivity and sensitivity, with expected LODs 0.1-18ng for each of the target elements after sampling. The analytical performance of the LIBS method is also compared to previously reported methods (inductively coupled plasma-optical emission spectroscopy). The combination of fast CMV sampling, unambiguous organic compound identification with GC-MS and fast LIBS analysis provides the basis for a new comprehensive screening method for GSR. Copyright © 2015 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

  5. Validated high-performance anion-exchange chromatography with pulsed amperometric detection method for the determination of residual keratan sulfate and other glucosamine impurities in sodium chondroitin sulfate.

    Science.gov (United States)

    Bottelli, Susanna; Grillo, Gianluca; Barindelli, Edoardo; Nencioni, Alessandro; Di Maria, Alessandro; Fossati, Tiziano

    2017-07-07

    An efficient and sensitive analytical method based on high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) was devised for the determination of glucosamine (GlcN) in sodium chondroitin sulfate (CS). Glucosamine (GlcN) is intended as marker of residual keratan sulfate (KS) and other impurities generating glucosamine by acidic hydrolyzation. The latter brings CS and KS to their respective monomers. Since GlcN is present only in KS we developed a method that separates GlcN from GalN, the principal hydrolytic product of CS, and then we validated it in order to quantify GlcN. Method validation was performed by spiking CS raw material with known amounts of KS. Detection limit was 0.5% of KS in CS (corresponding to 0.1μg/ml), and the linear range was 0.5-5% of KS in CS (corresponding to 0.1-1μg/ml). The optimized analysis was carried out on an ICS-5000 system (Dionex, Sunnyvale, CA, USA) equipped with a Dionex Amino Trap guard column (3mm×30mm), Dionex CarboPac-PA20 (3mm×30mm) and a Dionex CarboPac-PA20 analytical column (3mm×150mm) using gradient elution at a 0.5ml/min flow rate. Regression equations revealed good linear relationship (R 2 =0.99, n=5) within the test ranges. Quality parameters, including precision and accuracy, were fully validated and found to be satisfactory. The fully validated HPAEC-PAD method was readily applied for the quantification of residual KS in CS in several raw materials and USP/EP reference substance. Results confirmed that the HPAEC-PAD method is more specific than the electrophoretic method for related substance reported in EP and provides sensitive determination of KS in acid-hydrolyzed CS samples, enabling the quantitation of KS and other impurities (generating glucosamine) in CS. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Evaluation of the Charm maximum residue limit β-lactam and tetracycline test for the detection of antibiotics in ewe and goat milk.

    Science.gov (United States)

    Beltrán, M C; Romero, T; Althaus, R L; Molina, M P

    2013-05-01

    The Charm maximum residue limit β-lactam and tetracycline test (Charm MRL BLTET; Charm Sciences Inc., Lawrence, MA) is an immunoreceptor assay utilizing Rapid One-Step Assay lateral flow technology that detects β-lactam or tetracycline drugs in raw commingled cow milk at or below European Union maximum residue levels (EU-MRL). The Charm MRL BLTET test procedure was recently modified (dilution in buffer and longer incubation) by the manufacturers to be used with raw ewe and goat milk. To assess the Charm MRL BLTET test for the detection of β-lactams and tetracyclines in milk of small ruminants, an evaluation study was performed at Instituto de Ciencia y Tecnologia Animal of Universitat Politècnica de València (Spain). The test specificity and detection capability (CCβ) were studied following Commission Decision 2002/657/EC. Specificity results obtained in this study were optimal for individual milk free of antimicrobials from ewes (99.2% for β-lactams and 100% for tetracyclines) and goats (97.9% for β-lactams and 100% for tetracyclines) along the entire lactation period regardless of whether the results were visually or instrumentally interpreted. Moreover, no positive results were obtained when a relatively high concentration of different substances belonging to antimicrobial families other than β-lactams and tetracyclines were present in ewe and goat milk. For both types of milk, the CCβ calculated was lower or equal to EU-MRL for amoxicillin (4 µg/kg), ampicillin (4 µg/kg), benzylpenicillin (≤ 2 µg/kg), dicloxacillin (30 µg/kg), oxacillin (30 µg/kg), cefacetrile (≤ 63 µg/kg), cefalonium (≤ 10 µg/kg), cefapirin (≤ 30 µg/kg), desacetylcefapirin (≤ 30 µg/kg), cefazolin (≤ 25 µg/kg), cefoperazone (≤ 25 µg/kg), cefquinome (20 µg/kg), ceftiofur (≤ 50 µg/kg), desfuroylceftiofur (≤ 50µg/kg), and cephalexin (≤ 50 µg/kg). However, this test could neither detect cloxacillin nor nafcillin at or below EU-MRL (CCβ >30 µg/kg). The

  7. Fexofenadine Suppresses Delayed-Type Hypersensitivity in the Murine Model of Palladium Allergy

    Directory of Open Access Journals (Sweden)

    Ryota Matsubara

    2017-06-01

    Full Text Available Palladium is frequently used in dental materials, and sometimes causes metal allergy. It has been suggested that the immune response by palladium-specific T cells may be responsible for the pathogenesis of delayed-type hypersensitivity in study of palladium allergic model mice. In the clinical setting, glucocorticoids and antihistamine drugs are commonly used for treatment of contact dermatitis. However, the precise mechanism of immune suppression in palladium allergy remains unknown. We investigated inhibition of the immune response in palladium allergic mice by administration of prednisolone as a glucocorticoid and fexofenadine hydrochloride as an antihistamine. Compared with glucocorticoids, fexofenadine hydrochloride significantly suppressed the number of T cells by interfering with the development of antigen-presenting cells from the sensitization phase. Our results suggest that antihistamine has a beneficial effect on the treatment of palladium allergy compared to glucocorticoids.

  8. Method for recovering palladium and technetium values from nuclear fuel reprocessing waste solutions

    Science.gov (United States)

    Horwitz, E. Philip; Delphin, Walter H.

    1979-07-24

    A method for recovering palladium and technetium values from nuclear fuel reprocessing waste solutions containing these and other values by contacting the waste solution with an extractant of tricaprylmethylammonium nitrate in an inert hydrocarbon diluent which extracts the palladium and technetium values from the waste solution. The palladium and technetium values are recovered from the extractant and from any other coextracted values with a strong nitric acid strip solution.

  9. Preparation of Palladium/Silver-Coated Polyimide Nanotubes: Flexible, Electrically Conductive Fibers

    OpenAIRE

    Lushi Kong; Guanchun Rui; Guangyu Wang; Rundong Huang; Ran Li; Jiajie Yu; Shengli Qi; Dezhen Wu

    2017-01-01

    A simple and practical method for coating palladium/silver nanoparticles on polyimide (PI) nanotubes is developed. The key steps involved in the process are silver ion exchange/reduction and displacement reactions between silver and palladium ions. With the addition of silver, the conductivity of the PI nanotubes is greatly enhanced. Further, the polyimide nanotubes with a dense, homogeneous coating of palladium nanoparticles remain flexible after heat treatment and show the possibility for u...

  10. Surface topography of a palladium cathode after electrolysis in heavy water

    International Nuclear Information System (INIS)

    Silver, D.S.; Dash, J.; Keefe, P.S.

    1993-01-01

    Electrolysis was performed with a palladium cathode and an electrolyte containing both hydrogen and deuterium ions. The cathode bends toward the anode during this process. Examination of both the concave and the convex surfaces with the scanning electron microscope, scanning tunneling microscope, and atomic force microscope shows unusual surface characteristics. Rimmed craters with faceted crystals inside and multitextural surfaces were observed on an electrolyzed palladium cathode but not on palladium that has not been electrolyzed. 9 refs., 9 figs

  11. Determination of the Debye-Waller Factor of hydrogen in Palladium and Palladium Silver alloy

    International Nuclear Information System (INIS)

    Khodabakhsh, R.

    1986-01-01

    The mean square amplitude of the vibrating hydrogen in metals can be determined by using coherent elastic neutron scattering experiments, inelastic one-phonon scattering measurements. To determine the D.W.F. Debye-Waller Factor from the coherent elastic scattering measurements, information about the positions of atoms within the unit is required, and vice versa. The main difficulty concerning the determination of the D.W.F. from the inelastic experiment is in elimination of multi-phonon contribution from the measured spectrum. However, the D.W.F. of hydrogen in palladium has been usually determined by the intensity of the quasi-elastic line. An integration of the measured scattering law S(Q,W) at constant Q, over a certain energy window ΔE, results in the quasi-elastic intensity. To obtain an accurate result, this window has to be chosen large enough to comprise most of the quasi-elastic line, but sufficiently small so that the phonon contributions are small. The MARX spectrometer is ideally constructed for this type of measurement where the window is about +-1 Mev for incident neutron wavelength, =4.115 A. Thus, the quasi-elastic scattering method was considered the best method of determining the D.W.F. of hydrogen in palladium using the MARX spectrometer. However, if the acoustic part overlaps with the quasi-elastic part, one has to obtain the D.W.F. by fitting the data to a quasi-elastic model. The work to be reported here is the investigation of variations of the D.W.F. of hydrogen in Pd and PdAgsub(0.085) with temperature and extension of the available data to as high a temperature as possible. Therefore the integrated intensity of incoherent quasi-elastic neutron scattering by proton in polycrystallin Pd/H and PdAgsub(0.085)/H was investigated as a function of the scattering vector Q. A quasi-harmonic D.W.F. behaviour was observed at elevated temperatures. The observed Debye-Waller Factor depends strongly on the form of the amplitude weighted frequency

  12. Synthesis of an oxytetracyline-tolidin-BSA immunogen and antibodies production of anti-oxytetracyline developed for oxytetracyline residue detection with enzyme-linked immunosorbent assays technique

    Directory of Open Access Journals (Sweden)

    Widiastuti R

    2013-06-01

    Full Text Available An oxytetracycline-tolidin-bovine serum albumin (OTC-tolidin-BSA-conjugate was synthezed as immunogen for producing specific antibodies in immunized rabbits that would be used as reagent for development of OTC residue detection with enzym-linked immunoassays technique. The immunogen was prepared through diazotization tolidin and subsequently reacted with OTC. The red purple immunogen of OTC-tolidin-BSA absorbed at wave lengths of 277 nm and 488 nm under UV screening absorbances and confirmation with the high performance liquid chromatography (HPLC showed the absence of peak at retention time of 3.46 minutes. Characaterized result with SDS-PAGE showed the molecular weight of the OTC-tolidin-BSA at 69.79 kDA. Subsequently, the immunogen was immunized into New Zealand rabbits in order to produce the polyclonal antibodies. The antibodies were purified using a protein A sepharose column. The OD optimum responses of 0.92 to 1.20 were obtained from the second fractionation at dilution of 1/1000 by titrating the antibodies and OTC-tolidin-BSA coating antigen at concentration of 10 µg/mL on several bleeding times.

  13. Coumarins as turn on/off fluorescent probes for detection of residual acetone in cosmetics following headspace single-drop microextraction.

    Science.gov (United States)

    Cabaleiro, N; de la Calle, I; Bendicho, C; Lavilla, I

    2014-11-01

    In this work, a new method based on headspace-single drop microextraction for the determination of residual acetone in cosmetics by microfluorospectrometry is proposed. Acetone causes fluorescence changes in a 2.5 µL-ethanolic drop (40% v/v) containing 3.10(-4) mol L(-1) 7-hydroxy-4-methylcoumarin ('turn off') or 6.10(-6) mol L(-1) 7-diethylamino-4-methylcoumarin ('turn on'). Polarity and ability to form hydrogen bonds of short chain alcohols (polar protic solvents) were crucial in order to observe these changes in the presence of acetone (polar aprotic solvent). Parameters related with the HS-SDME procedure were studied, namely headspace volume, composition, volume and temperature of drop, microextraction time, stirring rate, mass and temperature of sample, as well as the effect of potential interferents (alcohols and fragrances). The high volatility of acetone allows its extraction from an untreated cosmetic sample within 3 min. A detection limit of 0.26 µg g(-1) and repeatability, expressed as relative standard deviation, around 5% were reached. Accuracy of the proposed methodology was evaluated by means of recovery studies. The method was successfully used to analyze different cosmetics. Simplicity and high sample throughput can be highlighted. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. A simple method for detection of gunshot residue particles from hands, hair, face, and clothing using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX).

    Science.gov (United States)

    Kage, S; Kudo, K; Kaizoji, A; Ryumoto, J; Ikeda, H; Ikeda, N

    2001-07-01

    We devised a simple and rapid method for detection of gunshot residue (GSR) particles, using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX) analysis. Experiments were done on samples containing GSR particles obtained from hands, hair, face, and clothing, using double-sided adhesive coated aluminum stubs (tape-lift method). SEM/WDX analyses for GSR were carried out in three steps: the first step was map analysis for barium (Ba) to search for GSR particles from lead styphnate primed ammunition, or tin (Sn) to search for GSR particles from mercury fulminate primed ammunition. The second step was determination of the location of GSR particles by X-ray imaging of Ba or Sn at a magnification of x 1000-2000 in the SEM, using data of map analysis, and the third step was identification of GSR particles, using WDX spectrometers. Analysis of samples from each primer of a stub took about 3 h. Practical applications were shown for utility of this method.

  15. Orthogonal identification of gunshot residue with complementary detection principles of voltammetry, scanning electron microscopy, and energy-dispersive X-ray spectroscopy: sample, screen, and confirm.

    Science.gov (United States)

    O'Mahony, Aoife M; Samek, Izabela A; Sattayasamitsathit, Sirilak; Wang, Joseph

    2014-08-19

    Field-deployable voltammetric screening coupled with complementary laboratory-based analysis to confirm the presence of gunshot residue (GSR) from the hands of a subject who has handled, loaded, or discharged a firearm is described. This protocol implements the orthogonal identification of the presence of GSR utilizing square-wave stripping voltammetry (SWSV) as a rapid screening tool along with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) to confirm the presence of the characteristic morphology and metal composition of GSR particles. This is achieved through the judicious modification of the working electrode of a carbon screen-printed electrode (CSPE) with carbon tape (used in SEM analysis) to fix and retain a sample. A comparison between a subject who has handled and loaded a firearm and a subject who has had no contact with GSR shows the significant variations in voltammetric signals and the presence or absence of GSR-consistent particles and constituent metals. This initial electrochemical screening has no effect on the integrity of the metallic particles, and SEM/EDX analysis conducted prior to and postvoltammetry show no differences in analytical output. The carbon tape is instrumental in retaining the GSR sample after electrochemical analysis, supported by comparison with orthogonal detection at a bare CSPE. This protocol shows great promise as a two-tier detection system for the presence of GSR from the hands of a subject, whereby initial screening can be conducted rapidly onsite by minimally trained operators; confirmation can follow at the same substrate to substantiate the voltammetric results.

  16. Noise temperature measurements for the determination of the thermodynamic temperature of the melting point of palladium

    Energy Technology Data Exchange (ETDEWEB)

    Edler, F.; Kuhne, M.; Tegeler, E. [Bundesanstalt Physikalisch-Technische, Berlin (Germany)

    2004-02-01

    The thermodynamic temperature of the melting point of palladium in air was measured by noise thermometric methods. The temperature measurement was based on noise comparison using a two-channel arrangement to eliminate parasitic noises of electronic components by cross correlation. Three miniature fixed points filled with pure palladium (purity: {approx}99.99%, mass: {approx}90 g) were used to realize the melts of the fixed point metal. The measured melting temperature of palladium in air amounted to 1552.95 deg C {+-} 0.21 K (k = 2). This temperature is 0.45 K lower than the temperature of the melting point of palladium measured by radiation thermometry. (authors)

  17. Solid residues

    International Nuclear Information System (INIS)

    Mulder, E.; Duin, P.J. van; Grootenboer, G.J.

    1995-01-01

    A summary is presented of the many investigations that have been done on solid residues of atmospheric fluid bed combustion (AFBC). These residues are bed ash, cyclone ash and bag filter ash. Physical and chemical properties are discussed and then the various uses of residues (in fillers, bricks, gravel, and for recovery of aluminium) are summarised. Toxicological properties of fly ash and stack ash are discussed as are risks of pneumoconiosis for workers handling fly ash, and contamination of water by ashes. On the basis of present information it is concluded that risks to public health from exposure to emissions of coal fly ash from AFBC appear small or negligible as are health risk to workers in the coal fly ash processing industry. 35 refs., 5 figs., 12 tabs

  18. Impurities determination in precious metals like rhodium, palladium and platinum by neutron activation without separation

    International Nuclear Information System (INIS)

    May, S.; Piccot, D.; Pinte, G.

    1978-01-01

    The possibilities of the method explored using an installation of gamma or X ray spectrometry of good performance. The irradiations were realized in the reactors EL.3 (flux approximately 6.10 12 n.cm -2 .s -1 ) and Osiris (flux > 10 14 n.cm -2 .s -1 ) of the CEN Saclay. In rhodium the presence of iridium limits the analysis possibilities. However gold, silver and platinum are easily determined, just as the other elements (As, Br, Cl, Co, Mn, Na, Sb). In platinum it is possible to determine the elements of long period, especially antimony, silver, cobalt, iridium, tantalum and zinc. As for palladium the principal impurities are gold, silver and ruthenium for what is of precious metals and particularly zinc among the other metals. For the three matrices considered the detection limits of a certain number of elements are indicated [fr

  19. Silica supported palladium nanoparticles for the decarboxylation of high-acid feedstocks: Design, deactivation and regeneration

    Science.gov (United States)

    Ping, Eric Wayne

    2011-12-01

    The major goals of this thesis were to (1) design and synthesize a supported catalyst with well-defined monodisperse palladium nanoparticles evenly distributed throughout an inorganic oxide substrate with tunable porosity characteristics, (2) demonstrate the catalytic activity of this material in the decarboxylation of long chain fatty acids and their derivatives to make diesel-length hydrocarbons, (3) elucidate the deactivation mechanism of supported palladium catalysts under decarboxylation conditions via post mortem catalyst characterization and develop a regeneration methodology thereupon, and (4) apply this catalytic system to a real low-value biofeedstock. Initial catalyst designs were based on the SBA-15 silica support, but in an effort to maximize loading and minimize mass transfer limitations, silica MCF was synthesized as catalyst support. Functionalization with various silane ligands yielded a surface that facilitated even distribution of palladium precursor salts throughout the catalyst particle, and, after reduction, monodisperse palladium nanoparticles approximately 2 nm in diameter. Complete characterization was performed on this Pd-MCF catalyst. The Pd-MCF catalyst showed high one-time activity in the decarboxylation of fatty acids to hydrocarbons in dodecane at 300°C. Hydrogen was found to be an unnecessary reactant in the absence of unsaturations, but was required in their presence---full hydrogenation of the double bonds occurs before any decarboxylation can take place. The Pd-MCF also exhibited good activity for alkyl esters and glycerol, providing a nice hypothetical description of a stepwise reaction pathway for catalytic decarboxylation of acids and their derivatives. As expected, the Pd-MCF catalyst experienced severe deactivation after only one use. Substantial effort was put into elucidating the nature of this deactivation via post mortem catalyst characterization. H2 chemisorption confirmed a loss of active surface area, but TEM and

  20. Kinetic Characteristics of Hydrogen Transfer Through Palladium-Modified Membrane

    Science.gov (United States)

    Petriev, I. S.; Frolov, V. Yu.; Bolotin, S. N.; Baryshev, M. G.; Kopytov, G. F.

    2018-01-01

    The paper deals with hydrogen transfer through Pd-23%Ag alloy membrane, the surface of which is modified by the electrolytic deposition of highly dispersed palladium. The dependence between the density of hydrogen flow and its excess pressure on the input surface of membrane is well approximated by the first-order curve. This fact indicates that the process of hydrogen permeability is defined by its dissociation on the input surface. Activation energy of this process is 47.9 kJ/mol which considerably exceeds that of the process of hydrogen transfer through palladium (22-30 kJ/mol). This confirms the fact that the chemisorption is a rate-controlling step of the hydrogen transfer through membrane.

  1. Analysis of the anomalous hydrogen solubilities in deformed palladiums

    Energy Technology Data Exchange (ETDEWEB)

    Park, Choong Nyeon; Lee, Ho Jong

    1987-02-01

    The anomalous hydrogen solubilities in the deformed palladiums were analyzed by empolying modified Kirchheim's model with considering the partially coherent strain energy which would induced during hydride precipitation around edge dislocations. The dislocation densities, obtained by this model, of the various cold worked and/or reversible US transformed palladium samples were the order of 10/sup 11/cm/sup -2/. The partially coherent strain energies were about 3 kJ/molH and nearly same in the various samples. This value could be compared with the incoherent strain energy, 0.4kJ/molH, which was obtained from the hysteresis on P-C isotherm, and the coherent strain energy calulated, 9.6kJ/molH.

  2. Hydrogenation of carbon monoxide over supported palladium catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Fujimoto, K.; Hashimoto, H.; Kunugi, T.

    1978-03-01

    An alumina-supported 2% palladium catalyst had higher activity for carbon monoxide hydrogenation than a silica-supported 2% palladium catalyst, at 250/sup 0/-400/sup 0/C and 1 atm. The addition of lanthanum oxide or thorium oxide, but not of potassium oxide, to the silica-supported catalyst increased the conversion at 350/sup 0/C from 1.1% to 81.0% with a selectivity of 56.1% for methane, 1.4% for C/sub 2/ compounds, 0.1% for C/sub 3/ compounds, and 42.5% for carbon dioxide. Temperature-programed desorption of carbon monoxide in a hydrogen stream showed that of two desorption peaks observed for carbon monoxide, the one at higher temperature corresponded to the carbon monoxide species which hydrogenates to methane and that the area of this peak increased with increasing thorium content of the catalyst. Graphs, tables, and 12 references.

  3. Adlayers of palladium particles and their aggregates on porous polypropylene hollow fiber membranes as hydrogenization contractors/reactors

    NARCIS (Netherlands)

    Volkov, V.V.; Lebedeva, V.I.; Petrova, I.V.; Bobyl, A.V.; Konnikov, S.G.; Roldughin, V.I.; Erkel, J. van; Tereshchenko, G.F.

    2011-01-01

    Principal approaches for the preparation of catalytic membrane reactors based on polymer membranes containing palladium nanoparticles and for the description of their characteristics are presented. The method for the development of adlayers composed of palladium nanoparticles and their aggregates on

  4. Co-deposition of palladium with hydrogen isotopes

    International Nuclear Information System (INIS)

    Dash, J.; Ambadkar, A.

    2006-01-01

    Palladium was co-deposited with hydrogen isotopes on a Pd cathode. This resulted in enhanced production of excess thermal power. After electrolysis the Pd Lβ/ Lα ratio was found to be increased in characteristic X-ray spectra from localized, microscopic areas on the surface of the Pd cathode. This suggests the possibility that appreciable amounts of silver are present in these areas. (authors)

  5. Unsupported palladium alloy membranes and methods of making same

    Science.gov (United States)

    Way, J. Douglas; Thoen, Paul; Gade, Sabina K.

    2015-06-02

    The invention provides support-free palladium membranes and methods of making these membranes. Single-gas testing of the unsupported foils produced hydrogen permeabilities equivalent to thicker membranes produced by cold-rolling. Defect-free films as thin as 7.2 microns can be fabricated, with ideal H.sub.2/N.sub.2 selectivities as high as 40,000. Homogeneous membrane compositions may also be produced using these methods.

  6. Interaction of CO with Palladium Supported on Oxidized Tungsten

    Czech Academy of Sciences Publication Activity Database

    Jirka, Ivan; Plšek, Jan; Šutara, F.; Matolín, V.; Cháb, Vladimír; Prince, K. C.

    2006-01-01

    Roč. 110, č. 47 (2006), s. 23837-23844 ISSN 1520-6106 R&D Projects: GA ČR GA202/05/0244; GA AV ČR IAA1010413 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z10100521 Keywords : palladium * WOx surfaces * TPD Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.115, year: 2006

  7. Application of Colloidal Palladium Nanoparticles for Labeling in Electron Microscopy

    Czech Academy of Sciences Publication Activity Database

    Vancová, Marie; Šlouf, Miroslav; Langhans, Jan; Pavlová, Eva; Nebesářová, Jana

    2011-01-01

    Roč. 17, č. 5 (2011), s. 810-816 ISSN 1431-9276 R&D Projects: GA AV ČR KAN200520704; GA AV ČR KJB600960906; GA ČR GAP205/10/0348 Institutional research plan: CEZ:AV0Z60220518; CEZ:AV0Z40500505 Keywords : electron microscopy * colloidal palladium * nanoparticles * labeling * salivary glands * Ixodes ricinus Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.007, year: 2011

  8. HE3 outgassing from four working palladium and uranium beds

    International Nuclear Information System (INIS)

    Souers, P. C.; Coronado, P. R.; Fearon, F. M.; Garza, R. G.; Shaw , J. F.; Stump, R. K.; Tsugawa, R. T.

    1988-01-01

    The He 3 output from two palladium and two uranium beds storing T 2 and D-T was studied as a function of time. Three of the beds were started new and watched for a year; the fourth bed was twelve years old. All four were beds used in routine tritium handling. Initial stoichiometries were PdT/sub 0.3/ and UT/sub 0.7/ so that both operated at similar 1 to 130 kPa pressures. The He 3 from palladium ranged from the 0.002 mo1% lower level of sensitivity to 0.01% for PdT 2 at one year of age. The UT system showed 0.1% He 3 at 4 to 62 days and 0.1 to 10% at longer times, with the first cuts being high in He 3 . The palladium bed with 95 to 97% pure T 2 enriches the output to as high as 97 to 99%. 9 refs., 1 fig., 2 tabs

  9. Substoichiometric extraction of traces of gold and palladium

    International Nuclear Information System (INIS)

    Colonat, J.-F.

    1975-01-01

    Several systems for extracting palladium at concentrations ranging from 10 -4 to 10 -6 M/l were studied. Extraction by dithizone is limited by the transformation of the primary complex into a secondary complex which takes place at concentrations around 10 -6 M. This transformation has been demonstrated kinetically. Dimethylglyoxime is an interesting reagent in substoichiometry, in spite of its comparatively low extraction constant. Various complexes which are formed in a highly chlorinated medium have been proposed. Use of copper diethyldithiocarbamate is limited principally by its stability in presence of chlorine ions. The kinetic formation of palladium diethyldithiocarbamate has been studied with greater precision. A direct determination of 100μg of palladium in a copper matrix without preliminary separation has given results comparable in every way with those of other methods. In the case of gold (III) the constants of formation with the diethyldithiocarbamate ion have been determined by an iterative method of calculation, using the influence curves of interfering metals. Finally conditions for an automatization of the substoichiometric extraction, as well as its possibilities for gold determination in the range 200-20ppm, were proposed [fr

  10. Arsenic (III Adsorption Using Palladium Nanoparticles from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Farzaneh Arsiya

    2017-07-01

    Full Text Available The presence of Arsenic in drinking water is the greatest threat to health effects especially in water. The purpose of this study is application of green palladium nanoparticles for removal of trivalent Arsenic from aqueous solutions and also the impact of some factors such as retention time, pH, concentration of palladium nanoparticles and Arsenic concentrations was studied. The values for Arsenic removal from aqueous solutions were measured by furnace atomic adsorption spectrometry (Conter AA700. In the study, Langmuir and Freundlich isotherm models and pseudo-second order kinetic model were studied. The results of  optimization is shown that 0.5 g of nanoparticles can removed %99.8 of Arsenic with initial concentration of  0.5 g/l, in 5 minutes at pH=4. Langmuir model, Freundlich model (R2=0.94 and pseudo-second order kinetic model (R2=0.99 shown high correlation for removing of Arsenic from aqueous solutions. It was found, palladium nanoparticles can be used as an efficient method to remove Arsenic from aqueous solutions in a short time.

  11. Recovery of hydrogen from impurities using a palladium membrane reactor

    International Nuclear Information System (INIS)

    Willms, R.S.; Okuno, K.

    1993-01-01

    One of the important steps in processing the exhaust from a fusion reactor is recovering tritium which is incorporated into molecules such as water and methane. One device which may prove to be very effective for this purpose is a palladium membrane reactor. This is a reactor which incorporates a Pd/Ag membrane in the reactor geometry. Reactions such as water gas shift, steam reforming and methane cracking can be carried out over the reactor catalyst, and the product hydrogen can be simultaneously removed from the reacting mixture. Because product is removed, greater than usual conversions can be obtained. In addition ultrapure hydrogen is produced, eliminating the need for an additional processing step. A palladium membrane reactor has been built and tested with three different catalysts. Initial results with a Ni-based catalyst show that it is very effective at promoting all three reactions listed above. Under the proper conditions, hydrogen recoveries approaching 100% have been observed. This study serves to experimentally validate the palladium membrane reactor as potentially important tool for fusion fuel processing

  12. Advantages and pitfalls of 18F-fluoro-2-deoxy-D-glucose positron emission tomography in detecting locally residual or recurrent nasopharyngeal carcinoma: comparison with magnetic resonance imaging

    International Nuclear Information System (INIS)

    Chan, Sheng-Chieh; Chang, Yu-Chen; Yen, Tzu-Chen; Ng, Shu-Hang; Chang, Joseph Tung-Chieh; Lin, Chien-Yu; Chen, Yen-Chao; Hsu, Cheng-Lung; Wang, Hung-Ming; Liao, Chun-Ta

    2006-01-01

    This prospective study was designed to elucidate the advantages and pitfalls of 18 F-FDG PET in detecting locally residual/recurrent nasopharyngeal carcinoma (NPC) in comparison with MRI. We recruited NPC patients from two ongoing prospective trials. One is being performed to evaluate suspected local recurrence (group A) and the other to assess local treatment response 3 months after therapy (group B). Both groups received 18 F-FDG PET and head and neck MRI. The gold standard was histopathology or clinical/imaging follow-up. An optimal cut-off standardised uptake value (SUV) was retrospectively determined. From January 2002 to August 2004, 146 patients were eligible. Thirty-four were from group A and 112 from group B. In all, 26 had locally recurrent/residual tumours. Differences in detection rate between 18 F-FDG PET and MRI were not statistically significant in either group. However, 18 F-FDG PET showed significantly higher specificity than MRI in detecting residual tumours among patients with initial T4 disease (p=0.04). In contrast, the specificity of 18 F-FDG PET for patients with an initial T1-2 tumour treated with intracavitary brachytherapy (ICBT) was significantly lower than that for patients not treated by ICBT (72.2% vs 98.1%, p=0.003). At an SUV cut-off of 4.2, PET showed an equal and a higher accuracy compared with MRI in groups A and B, respectively. 18 F-FDG PET is superior to MRI in identifying locally residual NPC among patients with initial T4 disease but demonstrates limitations in assessing treatment response in patients with initial T1-2 disease after ICBT. A cut-off SUV is a useful index for aiding in the visual detection of locally residual/recurrent NPC. (orig.)

  13. Palladium alloy membrane process for the treatment of hydrogen isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Hongsuk; Paek, Seungwoo; Lee, Minsoo; Kim, Kwangrag; Yim, Sungpaal; Ahn, Dohee [KAERI, Daejeon (Korea, Republic of); Shim, Myunghwa [Univ. of Science and Technology, Daejeon (Korea, Republic of)

    2005-11-15

    Tritium is a radioactive isotope of hydrogen and it has a half-life of 12.3 years; it decays to He-3 by emitting a low energy beta radiation with an average energy of 5.7 keV and a maximum energy of 18.6 keV. Transfer of environmentally tritiated water to humans takes place via an inhalation, diffusion through the skin and ingestion. Radioactive waste containing tritium is continuously generated by the nuclear industry in, for example, nuclear reactor operations and a radioisotope production, as well as in medical research. Methods for removing tritium from liquid waste provide an alternative to the control of tritium emissions and a personnel exposure. A combined electrolysis and catalytic exchange process is a very effective method to remove small quantities of tritium from light or heavy waste water streams. The process consists of three main steps: (a) A front end step that exchanges the tritium to a less toxic hydrogen phase. This can be performed either through a chemical exchange in the presence of a platinum supported catalyst or through the decomposition of water. (b) A back end process that purifies the tritiated hydrogen gas which evolved from the electrolysis. This can be performed through a palladium alloy membrane separator. (c) A means of storing the concentrated gas safely. Uranium is used if the storage is temporary; titanium is usually employed for long term storage. To gain a better understanding of the tritiated hydrogen gas purification process, a mathematical model of the palladium alloy membrane has been used. This model is described herein, and the representative results of the model calculations are presented. The authors selected the palladium alloy membrane for the hydrogen purification process by considering the membrane properties, such as a chemical resistance, mechanical stability, thermal stability, high permeability, and a stable operation. The solution-diffusion model can be a useful tool for designing a membrane permeator. The

  14. Palladium alloy membrane process for the treatment of hydrogen isotopes

    International Nuclear Information System (INIS)

    Chung, Hongsuk; Paek, Seungwoo; Lee, Minsoo; Kim, Kwangrag; Yim, Sungpaal; Ahn, Dohee; Shim, Myunghwa

    2005-01-01

    Tritium is a radioactive isotope of hydrogen and it has a half-life of 12.3 years; it decays to He-3 by emitting a low energy beta radiation with an average energy of 5.7 keV and a maximum energy of 18.6 keV. Transfer of environmentally tritiated water to humans takes place via an inhalation, diffusion through the skin and ingestion. Radioactive waste containing tritium is continuously generated by the nuclear industry in, for example, nuclear reactor operations and a radioisotope production, as well as in medical research. Methods for removing tritium from liquid waste provide an alternative to the control of tritium emissions and a personnel exposure. A combined electrolysis and catalytic exchange process is a very effective method to remove small quantities of tritium from light or heavy waste water streams. The process consists of three main steps: (a) A front end step that exchanges the tritium to a less toxic hydrogen phase. This can be performed either through a chemical exchange in the presence of a platinum supported catalyst or through the decomposition of water. (b) A back end process that purifies the tritiated hydrogen gas which evolved from the electrolysis. This can be performed through a palladium alloy membrane separator. (c) A means of storing the concentrated gas safely. Uranium is used if the storage is temporary; titanium is usually employed for long term storage. To gain a better understanding of the tritiated hydrogen gas purification process, a mathematical model of the palladium alloy membrane has been used. This model is described herein, and the representative results of the model calculations are presented. The authors selected the palladium alloy membrane for the hydrogen purification process by considering the membrane properties, such as a chemical resistance, mechanical stability, thermal stability, high permeability, and a stable operation. The solution-diffusion model can be a useful tool for designing a membrane permeator. The

  15. New Palladium-Catalyzed Approaches to Heterocycles and Carbocycles

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Qinhua [Iowa State Univ., Ames, IA (United States)

    2004-12-19

    The tert-butylimines of o-(1-alkynyl)benzaldehydes and analogous pyridinecarbaldehydes have been cyclized under very mild reaction conditions in the presence of I2, ICl, PhSeCl, PhSCl and p-O2NC6H4SCl to give the corresponding halogen-, selenium- and sulfur-containing disubstituted isoquinolines and naphthyridines, respectively. Monosubstituted isoquinolines and naphthyridines have been synthesized by the metal-catalyzed ring closure of these same iminoalkynes. This methodology accommodates a variety of iminoalkynes and affords the anticipated heterocycles in moderate to excellent yields. The Pd(II)-catalyzed cyclization of 2-(1-alkynyl)arylaldimines in the presence of various alkenes provides an efficient way to synthesize a variety of 4-(1-alkenyl)-3-arylisoquinolines in moderate to excellent yields. The introduction of an ortho-methoxy group on the arylaldimine promotes the Pd-catalyzed cyclization and stabilizes the resulting Pd(II) intermediate, improving the yields of the isoquinoline products. Highly substituted naphthalenes have been synthesized by the palladium-catalyzed annulation of a variety of internal alkynes, in which two new carbon-carbon bonds are formed in a single step under relatively mild reaction conditions. This method has also been used to synthesize carbazoles, although a higher reaction temperature is necessary. The process involves arylpalladation of the alkyne, followed by intramolecular Heck olefination and double bond isomerization. This method accommodates a variety of functional groups and affords the anticipated highly substituted naphthalenes and carbazoles in good to excellent yields. Novel palladium migratiodarylation methodology for the synthesis of complex fused polycycles has been developed, in which one or more sequential Pd-catalyzed intramolecular migration processes involving C-H activation are employed. The chemistry works best with electron-rich aromatics, which is in agreement

  16. Residual basins

    International Nuclear Information System (INIS)

    D'Elboux, C.V.; Paiva, I.B.

    1980-01-01

    Exploration for uranium carried out over a major portion of the Rio Grande do Sul Shield has revealed a number of small residual basins developed along glacially eroded channels of pre-Permian age. Mineralization of uranium occurs in two distinct sedimentary units. The lower unit consists of rhythmites overlain by a sequence of black shales, siltstones and coal seams, while the upper one is dominated by sandstones of probable fluvial origin. (Author) [pt

  17. Palladium emissions in the environment: analytical methods, environmental assessment and health effects

    National Research Council Canada - National Science Library

    Alt, Friedrich; Zereini, Fathi

    2006-01-01

    ... (Eds)). But there is a clear lack of information concerning palladium. It is very important to condense the present state of research findings from emission to potential health risks for the environment and humans. Very important is the chapter about analytical determination of palladium, which shows clearly the problems of several analytic...

  18. Carbon nanotubes decorated with palladium nanoparticles : Synthesis, characterization, and catalytic activity

    NARCIS (Netherlands)

    Karousis, Nikolaos; Tsotsou, Georgia-Eleni; Evangelista, Fabrizio; Rudolf, Petra; Ragoussis, Nikitas; Tagmatarchis, Nikos

    2008-01-01

    In this article, the in situ preparation of palladium nanoparticles, as mediated by the self-regulated reduction of palladium acetate with the aid of sodium dodecyl sulfate (SDS), followed by subsequent deposition onto single-walled carbon nanotubes and multimalled carbon nanotubes (MWCNTs), is

  19. Oxygen Activated, Palladium Nanoparticle Catalyzed, Ultrafast Cross-Coupling of Organolithium Reagents

    NARCIS (Netherlands)

    Heijnen, Dorus; Tosi, Filippo; Vila, Carlos; Stuart, Marc C. A.; Elsinga, Philip H.; Szymanski, Wiktor; Feringa, Ben L.

    2017-01-01

    The discovery of an ultrafast cross-coupling of alkyland aryllithium reagents with a range of aryl bromides is presented. The essential role of molecular oxygen to form the active palladium catalyst was established; palladium nanoparticles that are highly active in cross-coupling reactions with

  20. Palladium(II)-Stabilized Pyridine-2-Diazotates: Synthesis, Structural Characterization, and Cytotoxicity Studies.

    Science.gov (United States)

    Tskhovrebov, Alexander G; Vasileva, Anna A; Goddard, Richard; Riedel, Tina; Dyson, Paul J; Mikhaylov, Vladimir N; Serebryanskaya, Tatiyana V; Sorokoumov, Viktor N; Haukka, Matti

    2018-02-05

    Well-defined diazotates are scarce. Here we report the synthesis of unprecedented homoleptic palladium(II) diazotate complexes. The palladium(II)-mediated nitrosylation of 2-aminopyridines with NaNO 2 results in the formation of metal-stabilized diazotates, which were found to be cytotoxic to human ovarian cancer cells.

  1. A DFT study of arsine adsorption on palladium doped graphene: Effects of palladium cluster size

    International Nuclear Information System (INIS)

    Kunaseth, Manaschai; Mudchimo, Tanabat; Namuangruk, Supawadee; Kungwan, Nawee; Promarak, Vinich; Jungsuttiwong, Siriporn

    2016-01-01

    Graphical abstract: The relationship between charge difference and adsorption strength demonstrates that charge migration from Pd_n-SDG to AsH_x significantly enhanced adsorption strength, the Pd_6 clusters doped SDG with a steep slope is recommended as a superior adsorbent material for AsH_3 removal from gas stream. - Highlights: • Pd atom and Pd clusters bind strongly onto the defective graphene surface. • Larger size of Pd cluster adsorbs arsine and its hydrogenated products stronger. • Order of adsorption strength on Pd_n doped graphene: As > AsH > AsH_2 > > AsH_3. • Charge migration characterizes the strong adsorption of AsH_2, AsH, and As. • Pd cluster doped graphene is thermodynamically preferable for arsine removal. - Abstract: In this study, we have investigated the size effects of palladium (Pd) doped single-vacancy defective graphene (SDG) surface to the adsorption of AsH_3 and its dehydrogenated products on Pd using density functional theory calculations. Here, Pd cluster binding study revealed that Pd_6 nanocluster bound strongest to the SDG surface, while adsorption of AsH_x (x = 0–3) on the most stable Pd_n doped SDG showed that dehydrogenated arsine compounds adsorbed onto the surface stronger than the pristine AsH_3 molecule. Charge analysis revealed that considerable amount of charge migration from Pd to dehydrogenated arsine molecules after adsorption may constitute strong adsorption for dehydrogenated arsine. In addition, study of thermodynamic pathways of AsH_3 dehydrogenation on Pd_n doped SDG adsorbents indicated that Pd cluster doping on SDG adsorbent tends to be thermodynamically favorable for AsH_3 decomposition than the single-Pd atom doped SDG. Hence, our study has indicated that Pd_6 clusters doped SDG is more advantageous as adsorbent material for AsH_3 removal.

  2. Cobalt nanoparticles as sacrificial templates for the electrodeposition of palladium nanomaterials in an ionic liquid, and its application to electrochemical sensing of hydrazine

    International Nuclear Information System (INIS)

    He, Y.; Zheng, J.; Sheng, Q.

    2012-01-01

    We report on the electrodeposition of palladium nanomaterials in choline chloride-based ionic liquid ethaline. A glassy carbon electrode (GCE) was modified with cobalt nanoparticles (acting as sacrificial templates) and a GCE modified with palladium nanoparticles (PdNPs) were fabricated and used to study the electrocatalytic oxidation of hydrazine (N 2 H 4 ). Scanning electron microscopy revealed that the PdNP modified GCE has a uniform morphology. Zero current potentiometry was used for in-situ probing the changes in interfacial potential of the oxidation of hydrazine. An amperometric study showed that the PdNP modified GCE possesses excellent electrocatalytic activity towards N 2 H 4 . The modified electrode displays a fast response ( -1 ) -1 cm -2 ) and broad linearity in the range from 0.1 to 800 μmol L -1 with a detection limit of 0.03 μmol L -1 (S/N = 3). (author)

  3. Deposition and analytical characterization of fluoropolymer thin films modified by palladium nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Cioffi, Nicola; Torsi, Luisa; Farella, Isabella; Altamura, Davide; Valentini, Antonio; Ditaranto, Nicoletta; Sabbatini, Luigia; Zambonin, Pier Giorgio; Bleve-Zacheo, Teresa

    2004-02-02

    Palladium-fluoropolymer nanostructured composites (Pd-CF{sub x}) are deposited by a separate and simultaneous sputtering of bulk Teflon and palladium targets in a vacuum chamber. Such nano-material can find application as active layer in sensing devices, as it swells when exposed to the vapors of organic solvents such as acetone, chloroform, 2-propanol. Ellipsometry shows that the swelling extent linearly depends on the solvent partial pressure in the measuring chamber. Moreover, Pd-CF{sub x} sensitivity and selectivity features are different to those of a parent gold-fluoropolymer (Au-CF{sub x}) nanocomposite, investigated in previous studies. In particular, Pd-CF{sub x} layers are generally more sensitive than Au-CF{sub x} ones, particularly in the case of chlorinated solvents, which are scarcely detectable by Au-CF{sub x} nanocomposites. The material morphological and chemical structure has been investigated by means of atomic force and transmission electron microscopies along with X-ray photoelectron (XPS) and Fourier transform infra-red spectroscopies. The analytical characterization demonstrates that morphological similarities exist between Pd-CF{sub x} films and Au-CF{sub x} ones having the same metal volume fraction {phi}. XPS also reveals an almost identical surface structure for the dispersing polymer matrix of homologous Pd-CF{sub x} and Au-CF{sub x} films. Metal fluorides and oxides are identified as well and differences in the materials sensing performances are then ascribed to the presence of different amounts of these species that also have a different chemical reactivity and selectivity.

  4. Development of anodic stripping voltametry for the determination of palladium in high level nuclear waste

    Energy Technology Data Exchange (ETDEWEB)

    Bhardwaj, T. K. [North Carolina State University, Raleigh (United States); Sharma, H. S.; Affarwal, S. K. [Bhabha Atomic Research Centre, Mumbai (India); Jain, P. C. [Meerut College, Meerut (India)

    2012-12-15

    Deposition potential, deposition time, square wave frequency, rotation speed of the rotating disc electrode, and palladium concentration were studied on a Glassy Carbon Electrode (GCE) in 0.01M HCl for the determination of palladium in High Level Nuclear Waste (HLNW) by anodic stripping voltammetry. Experimental conditions were optimized for the determination of palladium at two different, 10-8 and 10-7 M, levels. Error and standard deviation of this method were under 1% for all palladium standard solutions. The developed technique was successfully applied as a subsidiary method for the determination of palladium in simulated high level nuclear waste with very good precision and high accuracy (under 1 % error and standard deviation).

  5. Synthetic strategies for controlling inter- and intramolecular interactions: Applications in single-molecule fluorescence imaging, bioluminescence imaging, and palladium catalysis

    Science.gov (United States)

    Conley, Nicholas R.

    The field of synthetic organic chemistry has reached such maturity that, with sufficient effort and resources, the synthesis of virtually any small molecule which exhibits reasonable stability at room temperature can be realized. While representing a monumental achievement for the field, the ability to exert precise control over molecular structure is just a means to an end, and it is frequently the responsibility of the synthetic chemist to determine which molecules should actually be synthesized. For better or worse, there exists no competitive free market in academia for new molecules, and as a result, the decision of which compounds should be synthesized is seldom driven by the forces of supply and demand; rather, it is guided by the synthetic chemist's interest in an anticipated structure-function relationship or in the properties of a previously unstudied class of molecules. As a consequence, there exists a pervasive need for chemists with synthetic expertise in fields (e.g., molecular imaging) and subdisciplines of chemistry (e.g., physical chemistry) in which the identification of promising synthetic targets dramatically outpaces the synthetic output in that field or subdiscipline, and ample opportunities are available for synthetic chemists who choose to pursue such cross-disciplinary research. This thesis describes synthetic efforts that leverage these opportunities to realize applications in biological imaging and in palladium catalysis. In Part I, the synthesis and characterization of three novel luminophores and their imaging applications are discussed. The first is a molecular beacon that utilizes a fluorophorefluorophore pair which exhibits H-dimer quenching in the closed conformation. This probe offers several advantages over conventional fluorophore-quencher molecular beacons in the detection of oligonucleotides, both in bulk and at the single-molecule level. Secondly, a fluorescent, Cy3-Cy5 covalent heterodimer is reported, which on account of the

  6. A DFT study of arsine adsorption on palladium doped graphene: Effects of palladium cluster size

    Energy Technology Data Exchange (ETDEWEB)

    Kunaseth, Manaschai, E-mail: manaschai@nanotec.or.th [National Nanotechnology Center (NANOTEC), National Science and Technology Development Agency (NSTDA) , Pathum Thani 12120 (Thailand); Mudchimo, Tanabat [Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani 34190 (Thailand); Namuangruk, Supawadee [National Nanotechnology Center (NANOTEC), National Science and Technology Development Agency (NSTDA) , Pathum Thani 12120 (Thailand); Kungwan, Nawee [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Promarak, Vinich [Department of Material Science and Engineering, School of Molecular Science and Engineering, Vidyasirimedhi Institute of Science and Technology, Rayong 21201 (Thailand); Jungsuttiwong, Siriporn, E-mail: siriporn.j@ubu.ac.th [Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani 34190 (Thailand)

    2016-03-30

    Graphical abstract: The relationship between charge difference and adsorption strength demonstrates that charge migration from Pd{sub n}-SDG to AsH{sub x} significantly enhanced adsorption strength, the Pd{sub 6} clusters doped SDG with a steep slope is recommended as a superior adsorbent material for AsH{sub 3} removal from gas stream. - Highlights: • Pd atom and Pd clusters bind strongly onto the defective graphene surface. • Larger size of Pd cluster adsorbs arsine and its hydrogenated products stronger. • Order of adsorption strength on Pd{sub n} doped graphene: As > AsH > AsH{sub 2} > > AsH{sub 3}. • Charge migration characterizes the strong adsorption of AsH{sub 2}, AsH, and As. • Pd cluster doped graphene is thermodynamically preferable for arsine removal. - Abstract: In this study, we have investigated the size effects of palladium (Pd) doped single-vacancy defective graphene (SDG) surface to the adsorption of AsH{sub 3} and its dehydrogenated products on Pd using density functional theory calculations. Here, Pd cluster binding study revealed that Pd{sub 6} nanocluster bound strongest to the SDG surface, while adsorption of AsH{sub x} (x = 0–3) on the most stable Pd{sub n} doped SDG showed that dehydrogenated arsine compounds adsorbed onto the surface stronger than the pristine AsH{sub 3} molecule. Charge analysis revealed that considerable amount of charge migration from Pd to dehydrogenated arsine molecules after adsorption may constitute strong adsorption for dehydrogenated arsine. In addition, study of thermodynamic pathways of AsH{sub 3} dehydrogenation on Pd{sub n} doped SDG adsorbents indicated that Pd cluster doping on SDG adsorbent tends to be thermodynamically favorable for AsH{sub 3} decomposition than the single-Pd atom doped SDG. Hence, our study has indicated that Pd{sub 6} clusters doped SDG is more advantageous as adsorbent material for AsH{sub 3} removal.

  7. Palladium-Catalyzed alpha-Arylation of Tetramic Acids

    DEFF Research Database (Denmark)

    Storgaard, Morten; Dorwald, F. Z.; Peschke, B.

    2009-01-01

    A mild, racemization-free, palladium-Catalyzed alpha-arylation of tetramic acids (2,4-pyrrolidinediones) has been developed. Various amino acid-derived tetramic acids were cleanly arylated by treatment with 2 mol % of Pd(OAc)(2), 4 mol % of a sterically demanding biaryl phosphine, 2.3 equiv of K2CO...... no effect on their reactivity: both electron-rich and electron-poor aryl chlorides and bromides or triflates led to good yields. Ortho-substituted aryl halides and heteroaryl halides, however, did not undergo the title reaction....

  8. Growth of nanoparticles in hydrogen-implanted palladium subsurfaces

    International Nuclear Information System (INIS)

    Okuyama, F.

    2010-01-01

    Solid particles with nanometric dimensions are shown to grow in the opened subsurface of a polycrystalline palladium (Pd) hydrogen-implanted at around 500 C. The particles are Pd in main composition and densely grown on sloping walls of fissured grain boundaries or cracks. The average grain size increases from deeper to shallow regions, suggesting that a negative temperature gradient toward the surface existed along the crack walls. The nanoparticles are certain to arise from the condensation of Pd vapors on the walls, forcing us to assume that hydrogen atoms implanted in an overpopulation heated their implantation zone so strongly as to vaporize Pd. (orig.)

  9. Growth of nanoparticles in hydrogen-implanted palladium subsurfaces

    Energy Technology Data Exchange (ETDEWEB)

    Okuyama, F. [Nagoya Institute of Technology, Graduate School of Engineering, Nagoya (Japan)

    2010-07-15

    Solid particles with nanometric dimensions are shown to grow in the opened subsurface of a polycrystalline palladium (Pd) hydrogen-implanted at around 500 C. The particles are Pd in main composition and densely grown on sloping walls of fissured grain boundaries or cracks. The average grain size increases from deeper to shallow regions, suggesting that a negative temperature gradient toward the surface existed along the crack walls. The nanoparticles are certain to arise from the condensation of Pd vapors on the walls, forcing us to assume that hydrogen atoms implanted in an overpopulation heated their implantation zone so strongly as to vaporize Pd. (orig.)

  10. Determination of palladium in biological samples applying nuclear analytical techniques

    International Nuclear Information System (INIS)

    Cavalcante, Cassio Q.; Sato, Ivone M.; Salvador, Vera L. R.; Saiki, Mitiko

    2008-01-01

    This study presents Pd determinations in bovine tissue samples containing palladium prepared in the laboratory, and CCQM-P63 automotive catalyst materials of the Proficiency Test, using instrumental thermal and epithermal neutron activation analysis and energy dispersive X-ray fluorescence techniques. Solvent extraction and solid phase extraction procedures were also applied to separate Pd from interfering elements before the irradiation in the nuclear reactor. The results obtained by different techniques were compared against each other to examine sensitivity, precision and accuracy. (author)

  11. Acoustic emission during hydrogen absorption and desorption in palladium

    International Nuclear Information System (INIS)

    Ramesh, R.; Mukhopadhyay, C.K.; Jayakumar, T.; Baldev Raj

    1996-01-01

    Acoustic emission technique has been used to study charging and discharging of hydrogen in palladium. During charging, breaking of oxide film due to surface activation and saturation of hydrogen absorption have been identified by acoustic emission. In the discharging cycle, the desorption of hydrogen from the specimen leads to high AE activity immediately after initiation of discharging, followed by gradual decrease in the acoustic activity, which reaches a minimum upon completion of the desorption. The potential of the acoustic emission technique for studying the kinetics of hydrogen absorption and desorption in metals has been shown. (author)

  12. Synthesis of Dihydrobenzofurans via Palladium-Catalyzed Heteroannulations

    Energy Technology Data Exchange (ETDEWEB)

    Rozhkov, Roman Vladimirovich [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    Palladium-catalyzed heteroannulation of 1,3-dienes with 3-iodo-2-alkenols, and 2-iodo-2-alkenols, as well as their amino analogs, affords the corresponding cyclic ethers and amines respectively. The presence of a β-hydrogen in the vinylic halide results in β-hydride elimination giving the corresponding alkyne. The presence of a bulky group in the α-position of the vinylic halide results in failure or reduced amounts of annulation products. A chloride source, pyridine base and electron-rich phosphine are essential for this reaction.

  13. Influence of the temperature, volume and type of solution in the mercury vaporization of dental amalgam residue

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Raquel dalla [Department of Chemical Engineering, State University of Maringa, Maringa - PR (Brazil)], E-mail: raqueldc_eng@yahoo.com.br; Cossich, Eneida Sala; Tavares, Celia Regina Granhen [Department of Chemical Engineering, State University of Maringa, Maringa - PR (Brazil)

    2008-12-15

    One of the qualitative methods for the identification of mercury vapor is what it occurs as a way of chemical reaction between palladium chloride and metallic mercury. Palladium chloride ribbons with yellowish coloration put in contact with the vaporized mercury of dental amalgam residue, liberates palladium and forms mercury chloride in your surface, and starts to have black coloration; this form identify the presence of the mercury vapor in the system. This work studies the influence of temperature, volume and type of barrier-solution in the vaporization of mercury during the period of storage of dental amalgam residues, aiming to establish the best conditions for storage of these residues. It was found that for all tested solutions, the longest storage times without any occurrence of mercury vaporization were obtained in the lowest temperatures tested and the largest solution volumes of barrier-solution. The radiographic effluent presented bigger efficacy in the reduction of the volatilization, increasing the period when the residue was stored, however the analysis of this solution after the vaporization test showed the presence of organic mercury. These results show that water is the most efficient barrier against the vaporization of mercury, since it did not result in organic mercury formation in the effluent solution from the storage process.

  14. Influence of the temperature, volume and type of solution in the mercury vaporization of dental amalgam residue

    International Nuclear Information System (INIS)

    Costa, Raquel dalla; Cossich, Eneida Sala; Tavares, Celia Regina Granhen

    2008-01-01

    One of the qualitative methods for the identification of mercury vapor is what it occurs as a way of chemical reaction between palladium chloride and metallic mercury. Palladium chloride ribbons with yellowish coloration put in contact with the vaporized mercury of dental amalgam residue, liberates palladium and forms mercury chloride in your surface, and starts to have black coloration; this form identify the presence of the mercury vapor in the system. This work studies the influence of temperature, volume and type of barrier-solution in the vaporization of mercury during the period of storage of dental amalgam residues, aiming to establish the best conditions for storage of these residues. It was found that for all tested solutions, the longest storage times without any occurrence of mercury vaporization were obtained in the lowest temperatures tested and the largest solution volumes of barrier-solution. The radiographic effluent presented bigger efficacy in the reduction of the volatilization, increasing the period when the residue was stored, however the analysis of this solution after the vaporization test showed the presence of organic mercury. These results show that water is the most efficient barrier against the vaporization of mercury, since it did not result in organic mercury formation in the effluent solution from the storage process

  15. Prolonged persistence of PCR-detectable minimal residual disease after diagnosis or first relapse predicts poor outcome in childhood B-precursor acute lymphoblastic leukemia

    NARCIS (Netherlands)

    Steenbergen, E. J.; Verhagen, O. J.; van Leeuwen, E. F.; van den Berg, H.; Behrendt, H.; Slater, R. M.; von dem Borne, A. E.; van der Schoot, C. E.

    1995-01-01

    The follow up of minimal residual disease (MRD) in childhood B-precursor ALL by polymerase chain reaction (PCR) may be of help for further stratification of treatment protocols, to improve outcome. However, the clinical relevance of this approach has yet to be defined. We report the retrospective

  16. Light microscopic detection of sugar residues in glycoconjugates of salivary glands and the pancreas with lectin-horseradish peroxidase conjugates. I. Mouse.

    Science.gov (United States)

    Schulte, B A; Spicer, S S

    1983-12-01

    Mouse salivary glands and pancreases were stained with a battery of ten horseradish peroxidase-conjugated lectins. Lectin staining revealed striking differences in the structure of oligosaccharides of stored intracellular secretory glycoproteins and glycoconjugates associated with the surface of epithelial cells lining excretory ducts. The percentage of acinar cells containing terminal alpha-N-acetylgalactosamine residues varied greatly in submandibular glands of 30 male mice, but all submandibular acinar cells contained oligosaccharides with terminal sialic acid and penultimate beta-galactose residues. The last named dimer was abundant in secretory glycoprotein of all mucous acinar cells in murine sublingual glands and an additional 20-50% of these cells in all glands contained terminal N-acetylglucosamine residues. In contrast, terminal alpha-N-acetylgalactosamine was abundant in sublingual serous demilune secretions. Serous acinar cells in the exorbital lacrimal gland, posterior lingual gland, parotid gland and pancreas exhibited a staining pattern unique to each organ. In contrast, the apical cytoplasm and surface of striated duct epithelial cells in the submandibular, sublingual, parotid and exorbital lacrimal gland stained similarly. A comparison of staining with conjugated lectins reported biochemically to have very similar carbohydrate binding specificity has revealed some remarkable differences in their reactivity, suggesting different binding specificity for the same terminal sugars having different glycosidic linkages or with different penultimate sugar residues.

  17. Rapid trace level determination of sulfonamide residues in honey with online extraction using short C-18 column by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Sajid, Muhammad; Na, Na; Safdar, Muhammad; Lu, Xin; Ma, Lin; He, Lan; Ouyang, Jin

    2013-11-01

    A sensitive and inexpensive quantification method with online extraction using a short C-18 column for sulfonamide residues in honey by high performance liquid chromatography with fluorescence detector was developed and validated. In sample preparation, acid hydrolysis was used to break the N-glycoside bond between the honey sugar and sulfonamide drugs and derivatization of sulfonamide residues with fluorescamine was conducted at pH 3.5 using a citrate buffer (0.5M) in the honey matrix. The chromatography was carried out on Zorbax Extended C-18 (250mm×4.6mm; 5μm) column, using a mixture of acetonitrile and an acetate buffer (pH 4.50, 20mM) as a mobile phase. A Zorbax Extended C-18 (12mm×4.6mm; 5μm) column was used for online extraction of fifteen sulfonamide residues from honey sample with the help of a two position valve. The limit of quantification of sulfonamide residues in honey was less than 3ngg(-1), and the percentage recovery of study compounds in spiked honey sample was from 80% for sulfacetamide to 100% of sulfachloropyridazine. The developed method has excellent linearity for all studied sulfonamides with a correlation coefficient 0.993. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. The Chemical Deposition Method for the Decoration of Palladium Particles on Carbon Nanofibers with Rapid Conductivity Changes

    Directory of Open Access Journals (Sweden)

    Hoik Lee

    2016-11-01

    Full Text Available Palladium (Pd metal is well-known for hydrogen sensing material due to its high sensitivity and selectivity toward hydrogen, and is able to detect hydrogen at near room temperature. In this work, palladium-doped carbon nanofibers (Pd/CNFs were successfully produced in a facile manner via electrospinning. Well-organized and uniformly distributed Pd was observed in microscopic images of the resultant nanofibers. Hydrogen causes an increment in the volume of Pd due to the ability of hydrogen atoms to occupy the octahedral interstitial positions within its face centered cubic lattice structure, resulting in the resistance transition of Pd/CNFs. The resistance variation was around 400%, and it responded rapidly within 1 min, even in 5% hydrogen atmosphere conditions at room temperature. This fibrous hybrid material platform will open a new and practical route and stimulate further researches on the development of hydrogen sensing materials with rapid response, even to low concentrations of hydrogen in an atmosphere.

  19. A new electrochemical sensor for the simultaneous determination of acetaminophen and codeine based on porous silicon/palladium nanostructure.

    Science.gov (United States)

    Ensafi, Ali A; Ahmadi, Najmeh; Rezaei, Behzad; Abarghoui, Mehdi Mokhtari

    2015-03-01

    A porous silicon/palladium nanostructure was prepared and used as a new electrode material for the simultaneous determination of acetaminophen (ACT) and codeine (COD). Palladium nanoparticles were assembled on porous silicon (PSi) microparticles by a simple redox reaction between the Pd precursor and PSi in an aqueous solution of hydrofluoric acid. This novel nanostructure was characterized by different spectroscopic and electrochemical techniques including scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, fourier transform infrared spectroscopy and cyclic voltammetry. The high electrochemical activity, fast electron transfer rate, high surface area and good antifouling properties of this nanostructure enhanced the oxidation peak currents and reduced the peak potentials of ACT and COD at the surface of the proposed sensor. Simultaneous determination of ACT and COD was explored using differential pulse voltammetry. A linear range of 1.0-700.0 µmol L(-1) was achieved for ACT and COD with detection limits of 0.4 and 0.3 µmol L(-1), respectively. Finally, the proposed method was used for the determination of ACT and COD in blood serum, urine and pharmaceutical compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Residual nilpotence and residual solubility of groups

    International Nuclear Information System (INIS)

    Mikhailov, R V

    2005-01-01

    The properties of the residual nilpotence and the residual solubility of groups are studied. The main objects under investigation are the class of residually nilpotent groups such that each central extension of these groups is also residually nilpotent and the class of residually soluble groups such that each Abelian extension of these groups is residually soluble. Various examples of groups not belonging to these classes are constructed by homological methods and methods of the theory of modules over group rings. Several applications of the theory under consideration are presented and problems concerning the residual nilpotence of one-relator groups are considered.

  1. Palladium sulphide (PdS) films as a new thermoelectric sulphide compound

    Energy Technology Data Exchange (ETDEWEB)

    Ares, J.R.; Diaz-Chao, P.; Clamagirand, J.; Macia, M.D.; Ferrer, I.J.; Sanchez, C. [Universidad Autonoma de Madrid (Spain). Lab. de Materiales de Interes en Energias Renovables

    2010-07-01

    Palladium sulphide (PdS) films have been prepared by direct sulphuration of 20 nm thick palladium films at different temperatures (200 C < T < 450 C). Sulphurated films exhibit an unique crystalline phase: PdS. Seebeck coefficient and electrical resistivity of these films are between -110 and -150 {mu}V/K and {proportional_to} 0.08 to 0.8 {omega}cm depending on the sulphuration temperature. Negative sign of Seebeck coefficient indicates an n type conduction in all films. Discussion is focused on the influence of atomic ratio between sulphur and palladium as well as impurities arising from the substrate on transport properties. (orig.)

  2. Interaction between Palladium Nanoparticles and Surface-Modified Carbon Nanotubes: Role of Surface Functionalities

    DEFF Research Database (Denmark)

    Zhang, Bingsen; Shao, Lidong; Zhang, Wei

    2014-01-01

    degrees C. We focus on probing the effects of oxygen and nitrogen-containing functional groups on supported palladium nanoparticles (NPs) in the model catalytic system. The stability of palladium NPs supported on CNTs depends strongly on the surface properties of CNTs. Moreover, the oxygen...... feature, instability, and subtle response of the components upon application of an external field. Herein, we use insitu TEM, electron energy loss spectroscopy, and X-ray photoelectron spectroscopy techniques to record the interaction in palladium on carbon nanotubes (CNTs) from room temperature to 600...

  3. Supported palladium nanoparticles synthesized by living plants as a catalyst for Suzuki-Miyaura reactions.

    Directory of Open Access Journals (Sweden)

    Helen L Parker

    Full Text Available The metal accumulating ability of plants has previously been used to capture metal contaminants from the environment; however, the full potential of this process is yet to be realized. Herein, the first use of living plants to recover palladium and produce catalytically active palladium nanoparticles is reported. This process eliminates the necessity for nanoparticle extraction from the plant and reduces the number of production steps compared to traditional catalyst palladium on carbon. These heterogeneous plant catalysts have demonstrated high catalytic activity in Suzuki coupling reactions between phenylboronic acid and a range of aryl halides containing iodo-, bromo- and chloro- moieties.

  4. Investigation of mechanical and structural characteristics of platinum and palladium at high temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Trumie, B. T.; Gomidzelovie, L.; Marjanovic, S. R.; Krstic, V. R.

    2015-03-30

    In order to broaden future application of products based on platinum and palladium a comparative analysis of their high-temperature mechanical properties was performed. Platinum and palladium are of great importance and are widely used in chemical industry, electronics, for making laboratory dishes, to name a few. Mechanical properties of pure metals, such as: tensile strength, creep rate and rupture time were investigated using universal testing machine for tensile testing of materials. Microstructure of samples was investigated by optical microscopy. Based on obtained results it can be concluded that the platinum, compared to palladium, is superior for high-temperature applications. (Author)

  5. Investigation of mechanical and structural characteristics of platinum and palladium at high temperatures

    International Nuclear Information System (INIS)

    Trumie, B. T.; Gomidzelovie, L.; Marjanovic, S. R.; Krstic, V. R.

    2015-01-01

    In order to broaden future application of products based on platinum and palladium a comparative analysis of their high-temperature mechanical properties was performed. Platinum and palladium are of great importance and are widely used in chemical industry, electronics, for making laboratory dishes, to name a few. Mechanical properties of pure metals, such as: tensile strength, creep rate and rupture time were investigated using universal testing machine for tensile testing of materials. Microstructure of samples was investigated by optical microscopy. Based on obtained results it can be concluded that the platinum, compared to palladium, is superior for high-temperature applications. (Author)

  6. Carbonylation of 1-hexene in the presence of palladium-anion-exchange resin catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Lapidus, A.L.; Pirozhkov, S.D.; Buiya, M.A.; Lunin, A.F.; Karapetyan, L.P.; Saldadze, K.M.

    1986-06-20

    Activated charcoal, silica gel, and zeolites containing palladium are active in the carbonylation of lower olefins by carbon monoxide. In the present work, they studied the carbonylation of 1-hexene in the presence of a series of palladium catalysts containing An-221, An-251, and AN-511 anion-exchange catalysts produced in the USSR as the supports. A catalyst obtained by the deposition of palladium(II) on weakly basic anion-exchange resins displays high efficiency in the carbonylation of 1-hexene with the formation of a nixture of enanthoic and 2-methylcaproic acids.

  7. Preliminary design of fusion reactor fuel cleanup system by palladium alloy membrane method

    International Nuclear Information System (INIS)

    Yoshida, Hiroshi; Konishi, Satoshi; Naruse, Yuji

    1981-10-01

    A design of palladium diffuser and Fuel Cleanup System (FCU) for D-T fusion reactor is proposed. Feasibility of palladium alloy membrane method is discussed based on the early studies by the authors. Operating conditions of the palladium diffuser are determined experimentally. Dimensions of the diffuser are estimated from computer simulation. FCU system is designed under the feed conditions of Tritium Systems Test Assembly (TSTA) at Los Alamos Scientific Laboratory. The system is composed of Pd-diffusers, catalytic oxidizer, freezer and zink beds, and has some advantages in system layout and operation. This design can readily be extended to other conditions of plasma exhaust gases. (author)

  8. Chlorodifluoromethane-triggered formation of difluoromethylated arenes catalysed by palladium

    Science.gov (United States)

    Feng, Zhang; Min, Qiao-Qiao; Fu, Xia-Ping; An, Lun; Zhang, Xingang

    2017-09-01

    Difluoromethylated aromatic compounds are of increasing importance in pharmaceuticals, agrochemicals and materials. Chlorodifluoromethane (ClCF2H), an inexpensive, abundant and widely used industrial raw material, represents the ideal and most straightforward difluoromethylating reagent, but introduction of the difluoromethyl group (CF2H) from ClCF2H into aromatics has not been reported. Here, we describe a direct palladium-catalysed difluoromethylation method for coupling ClCF2H with arylboronic acids and esters to generate difluoromethylated arenes with high efficiency. The reaction exhibits a remarkably broad substrate scope, including heteroarylboronic acids, and was used for difluoromethylation of a range of pharmaceuticals and biologically active compounds. Preliminary mechanistic studies revealed that a palladium difluorocarbene intermediate is involved in the reaction. Although numerous metal-difluorocarbene complexes have been prepared, the catalytic synthesis of difluoromethylated or difluoromethylenated compounds involving metal-difluorocarbene complexes has not received much attention. This new reaction therefore also opens the door to understand metal-difluorocarbene complex catalysed reactions.

  9. Development and validation of a multi-residue method for the detection of a wide range of hormonal anabolic compounds in hair using gas chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    Rambaud, Lauriane; Monteau, Fabrice; Deceuninck, Yoann; Bichon, Emmanuelle; Andre, Francois; Le Bizec, Bruno

    2007-01-01

    The monitoring of anabolic steroid residues in hair is undoubtedly one of the most efficient strategies to demonstrate the long-term administration of these molecules in meat production animals. A multi-residue sample preparation procedure was developed and validated for 28 steroids. A 100 mg hair sample was grinded into powder and extracted at 50 deg. C with methanol. After acidic hydrolysis and extraction with ethyl acetate, phenolsteroids, such as estrogens, resorcyclic acid lactones and stilbens in one hand, are separated from androgens and progestagens in the other hand. Solid phase extractions were performed before applying a specific derivatisation for each compound sub-group. Detection and identification were achieved using gas chromatography-tandem mass spectrometry with acquisition in the selected reaction monitoring mode after electron ionisation. The method was validated according to the 2002/657/EC guideline. Decision limits (CCα) for main steroids were in the 0.1-10 μg kg -1 range

  10. The critical main-chain length for helix formation in water: determined in a peptide series with alternating Aib and Ala residues exclusively and detected with ECD spectroscopy.

    Science.gov (United States)

    Longo, Edoardo; Moretto, Alessandro; Formaggio, Fernando; Toniolo, Claudio

    2011-10-01

    Critical main-chain length for peptide helix formation in the crystal (solid) state and in organic solvents has been already reported. In this short communication, we describe our results aiming at assessing the aforementioned parameter in water solution. To this goal, we synthesized step-by-step by solution procedures a complete series of N-terminally acetylated, C-terminally methoxylated oligopeptides, characterized only by alternating Aib and Ala residues, from the dimer to the nonamer level. All these compounds were investigated by electronic circular dichroism in the far-UV region in water solution as a function of chemical structure, namely presence/absence of an ester moiety or a negative charge at the C-terminus, and temperature. We find that the critical main-chain lengths for 3(10)- and α-helices, although still formed to a limited extent, in aqueous solution are six and eight residues, respectively. © 2011 Wiley-Liss, Inc.

  11. Eficiência dos testes COPAN (Microplate e Single na detecção de resíduos de antimicrobianos no leite Efficacy of COPAN (Microplate and Single kits in detection of antimicrobials residues in milk

    Directory of Open Access Journals (Sweden)

    C.G.M.S.C. Tenório

    2009-04-01

    Full Text Available Avaliou-se a eficiência dos testes microbiológicos COPAN (Microplate e Single para detecção de resíduos de 13 antimicrobianos inoculados em leite isento de resíduos. Foram utilizadas quatro concentrações, sendo a primeira equivalente à metade do limite de detecção declarado pelo fabricante (C1; a segunda equivalente ao limite máximo de resíduos (LMR estabelecido pela legislação brasileira (C2; a terceira equivalente ao limite de detecção declarado pelo fabricante (C3; e a quarta equivalente ao dobro do limite de detecção declarado pelo fabricante (C4. Os testes apresentaram 100% de sensibilidade na detecção de amoxicilina, ampicilina, cloxacilina, penicilina, tilosina, sulfadiazina, sulfametoxazol, e 96,7% na detecção de oxacilina para as concentrações informadas pelo fabricante como limite de detecção. Em relação às concentrações estabelecidas pela legislação brasileira, verificou-se que os testes foram capazes de detectá-las para a maioria dos antimicrobianos avaliados. Os testes não se mostraram eficientes na detecção das concentrações estabelecidas pela legislação para eritromicina, oxitetraciclina, tetraciclina, trimetoprim e gentamicina (Microplate.The efficacy of the microbiological kits COPAN (Microplate and Single for detection of antimicrobials residues was tested. Thirteen drugs were inoculated into milk without residues at four concentration levels: C1 - half of the detection threshold declared by the manufacturer, C2 - the maximum residues threshold established by the Brazilian legislation, C3 - the detection threshold declared by the manufacturer, and C4 - two fold the detection threshold declared by the manufacturer. The tests showed 100% efficient in detection of amoxicillin, cloxacillin, penicillin, tilosin, sulfadiazine, and sulfa methoxazol; and 96.7% for oxacillin considering the concentration stated by the manufacturer as threshold level. Regarding the concentrations established by

  12. Insertion of molecular oxygen into a palladium(II) methyl bond: a radical chain mechanism involving palladium(III) intermediates.

    Science.gov (United States)

    Boisvert, Luc; Denney, Melanie C; Hanson, Susan Kloek; Goldberg, Karen I

    2009-11-04

    The reaction of (bipy)PdMe(2) (1) (bipy = 2,2'-bipyridine) with molecular oxygen results in the formation of the palladium(II) methylperoxide complex (bipy)PdMe(OOMe) (2). The identity of the product 2 has been confirmed by independent synthesis. Results of kinetic studies of this unprecedented oxygen insertion reaction into a palladium alkyl bond support the involvement of a radical chain mechanism. Reproducible rates, attained in the presence of the radical initiator 2,2'-azobis(2-methylpropionitrile) (AIBN), reveal that the reaction is overall first-order (one-half-order in both [1] and [AIBN], and zero-order in [O(2)]). The unusual rate law (half-order in [1]) implies that the reaction proceeds by a mechanism that differs significantly from those for organic autoxidations and for the recently reported examples of insertion of O(2) into Pd(II) hydride bonds. The mechanism for the autoxidation of 1 is more closely related to that found for the autoxidation of main group and early transition metal alkyl complexes. Notably, the chain propagation is proposed to proceed via a stepwise associative homolytic substitution at the Pd center of 1 with formation of a pentacoordinate Pd(III) intermediate.

  13. PALLADIUM DOPED TIN OXIDE BASED HYDROGEN GAS SENSORS FOR SAFETY APPLICATIONS

    International Nuclear Information System (INIS)

    Kasthurirengan, S.; Behera, Upendra; Nadig, D. S.

    2010-01-01

    Hydrogen is considered to be a hazardous gas since it forms a flammable mixture between 4 to 75% by volume in air. Hence, the safety aspects of handling hydrogen are quite important. For this, ideally, highly selective, fast response, small size, hydrogen sensors are needed. Although sensors based on different technologies may be used, thin-film sensors based on palladium (Pd) are preferred due to their compactness and fast response. They detect hydrogen by monitoring the changes to the electrical, mechanical or optical properties of the films. We report the development of Pd-doped tin-oxide based gas sensors prepared on thin ceramic substrates with screen printed platinum (Pt) contacts and integrated nicrome wire heaters. The sensors are tested for their performances using hydrogen-nitrogen gas mixtures to a maximum of 4%H 2 in N 2 . The sensors detect hydrogen and their response times are less than a few seconds. Also, the sensor performance is not altered by the presence of helium in the test gas mixtures. By the above desired performance characteristics, field trials of these sensors have been undertaken. The paper presents the details of the sensor fabrication, electronic circuits, experimental setup for evaluation and the test results.

  14. Development of polymeric palladium-nanoparticle membrane-installed microflow devices and their application in hydrodehalogenation.

    Science.gov (United States)

    Yamada, Yoichi M A; Watanabe, Toshihiro; Ohno, Aya; Uozumi, Yasuhiro

    2012-02-13

    We have developed a variety of polymeric palladium-nanoparticle membrane-installed microflow devices. Three types of polymers were convoluted with palladium salts under laminar flow conditions in a microflow reactor to form polymeric palladium membranes at the laminar flow interface. These membranes were reduced with aqueous sodium formate or heat to create microflow devices that contain polymeric palladium-nanoparticle membranes. These microflow devices achieved instantaneous hydrodehalogenation of aryl chlorides, bromides, iodides, and triflates by 10-1000 ppm within a residence time of 2-8 s at 50-90 °C by using safe, nonexplosive, aqueous sodium formate to quantitatively afford the corresponding hydrodehalogenated products. Polychlorinated biphenyl (10-1000 ppm) and polybrominated biphenyl (1000 ppm) were completely decomposed under similar conditions, yielding biphenyl as a fungicidal compound. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Nano-palladium is a cellular catalyst for in vivo chemistry

    Science.gov (United States)

    Miller, Miles A.; Askevold, Bjorn; Mikula, Hannes; Kohler, Rainer H.; Pirovich, David; Weissleder, Ralph

    2017-07-01

    Palladium catalysts have been widely adopted for organic synthesis and diverse industrial applications given their efficacy and safety, yet their biological in vivo use has been limited to date. Here we show that nanoencapsulated palladium is an effective means to target and treat disease through in vivo catalysis. Palladium nanoparticles (Pd-NPs) were created by screening different Pd compounds and then encapsulating bis[tri(2-furyl)phosphine]palladium(II) dichloride in a biocompatible poly(lactic-co-glycolic acid)-b-polyethyleneglycol platform. Using mouse models of cancer, the NPs efficiently accumulated in tumours, where the Pd-NP activated different model prodrugs. Longitudinal studies confirmed that prodrug activation by Pd-NP inhibits tumour growth, extends survival in tumour-bearing mice and mitigates toxicity compared to standard doxorubicin formulations. Thus, here we demonstrate safe and efficacious in vivo catalytic activity of a Pd compound in mammals.

  16. Dinuclear Tetrapyrazolyl Palladium Complexes Exhibiting Facile Tandem Transfer Hydrogenation/Suzuki Coupling Reaction of Fluoroarylketone

    KAUST Repository

    Dehury, Niranjan; Maity, Niladri; Tripathy, Suman Kumar; Basset, Jean-Marie; Patra, Srikanta

    2016-01-01

    Herein, we report an unprecedented example of dinuclear pyrazolyl-based Pd complexes exhibiting facile tandem catalysis for fluoroarylketone: Tetrapyrazolyl di-palladium complexes with varying Pd-Pd distances efficiently catalyze the tandem reaction

  17. Synthesis of pyrrolo(2,3-b)quinolines by palladium-catalyzed heteroannulation

    International Nuclear Information System (INIS)

    Gee, Moon Bae; Lee, Won Jung; Yum, Eul Kgun

    2003-01-01

    Palladium-catalyzed heteroannulation of 2-amino-3-iodoquinoline derivatives and 1-trimethylsilyl internal alkynes provided highly regioselective pyrrolo(2,3-b)quinolines with trimethylsilyl group next to the nitrogen atom in the pyrrole ring

  18. Novel O N N Pyrazolyl-imine and Imidazolyl-imine Pincer Palladium ...

    African Journals Online (AJOL)

    NICO

    pincer palladium complexes in Heck coupling reactions. The general form of .... while single crystals suitable for X-ray analyses of complexes 1–4 were grown by ...... non-hydrogen atoms were refined with anisotropic displacement coefficients.

  19. Development of chiral terminal-alkene-phosphine hybrid ligands for palladium-catalyzed asymmetric allylic substitutions.

    Science.gov (United States)

    Liu, Zhaoqun; Du, Haifeng

    2010-07-02

    A variety of novel chiral terminal-alkene-phosphine hybrid ligands were successfully developed from diethyl L-tartrate for palladium-catalyzed asymmetric allylic alkylations, etherifications, and amination to give the desired products in excellent yields and ee's.

  20. Preparation of fluorinated biaryls through direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates

    KAUST Repository

    Fang, Xin; Huang, Yuanyuan; Chen, Xiaoqing; Lin, Xiaoxi; Bai, Zhengshuai; Huang, Kuo-Wei; Yuan, Yaofeng; Weng, Zhiqiang

    2013-01-01

    The direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates gave the desired products of fluorinated biaryls in good to excellent yields. A diverse set of important functional groups including methoxy, aldehyde, ester

  1. Nanocomposite catalyst with palladium nanoparticles encapsulated in a polymeric acid: A model for tandem environmental catalysis

    KAUST Repository

    Isimjan, Tayirjan T.; He, Quan; Liu, Yong; Zhu, Jesse; Puddephatt, Richard J.; Anderson, Darren Jason

    2013-01-01

    The synthesis and characterization of a novel hybrid nanocomposite catalyst comprised of palladium nanoparticles embedded in polystyrene sulfonic acid (PSSH) and supported on metal oxides is reported. The catalysts are intended for application

  2. Determination of palladium by flame photometry; Determinacion de paladio por fotometria de llama

    Energy Technology Data Exchange (ETDEWEB)

    Parallada Bellod, R

    1964-07-01

    A study on the determination of palladium by lame photometry, fixing the most convent experimental conditions and using solvents to increase the emission of this elements is carried out. Among the organic solvents, acetone has been found the most efficient. The interferences produced by anions and cations have also been studied and an analytical method is related, in which lines of calibration of 0 to 100 ppm palladium re used. (Author) 7 refs.

  3. Facile synthesis of bacitracin-templated palladium nanoparticles with superior electrocatalytic activity

    Science.gov (United States)

    Li, Yanji; Wang, Zi; Li, Xiaoling; Yin, Tian; Bian, Kexin; Gao, Faming; Gao, Dawei

    2017-02-01

    Palladium nanomaterials have attracted great attention on the development of electrocatalysts for fuel cells. Herein, we depicted a novel strategy in the synthesis of palladium nanoparticles with superior electrocatalytic activity. The new approach, based on the self-assembly of bacitracin biotemplate and palladium salt for the preparation of bacitracin-palladium nanoparticles (Bac-PdNPs), was simple, low-cost, and green. The complex, composed by a series of spherical Bac-PdNPs with a diameter of 70 nm, exhibited a chain-liked morphology in TEM and a face-centered cubic crystal structure in X-Ray diffraction and selected area electron diffraction. The palladium nanoparticles were mono-dispersed and stable in aqueous solution as shown in TEM and zeta potential. Most importantly, compared to the commercial palladium on carbon (Pd/C) catalyst (8.02 m2 g-1), the Bac-PdNPs showed a larger electrochemically active surface area (47.57 m2 g-1), which endowed the products an excellent electrocatalytic activity for ethanol oxidation in alkaline medium. The strategy in synthesis of Bac-PdNPs via biotemplate approach might light up new ideas in anode catalysts for direct ethanol fuel cells.

  4. Crystal size effect on the electrochemical oxidation of formate on carbon-supported palladium nanoparticles

    International Nuclear Information System (INIS)

    Santos, Rayana Marcela Izidoro da Silva; Nakazato, Roberto Zenhei; Ciapina, Eduardo Goncalves

    2016-01-01

    Full text: The electrochemical oxidation of formate in alkaline electrolytes has emerged an a promising anodic reaction in the Direct Formate Fuel Cells[1]. Although palladium is considered to be one of the best electro catalyst for the oxidation of formate, important structure-activity relationships are still not understood. In the present work, we investigated the effect of the size of the palladium crystals in the electrochemical oxidation of formate in 0.1 mol L -1 KOH. Carbon-supported palladium nanoparticles (Pd/C) were prepared by chemical reduction of palladium (II) chloride in aqueous media by sodium borohydride in the presence of varying quantities of sodium citrate in the reaction media to obtain metallic crystals with distinct sizes. Analysis of the X-ray diffraction profile revealed the presence of palladium crystals in the range of 6 to 19 nm. Potentiostatic oxidation of formate on the distinct Pd/C samples revealed a volcano-like dependence of the specific activity with the size of the palladium crystals, presenting the highest activity for crystals around 7.5 nm. Reference: [1] A.M. Bartrom, J.L. Haan, The direct formate fuel cell with an alkaline anion exchange membrane, J. Power Sources. 214 (2012) 68-74. (author)

  5. Mechanism of the palladium-catalyzed hydrothiolation of alkynes to thioethers: a DFT study.

    Science.gov (United States)

    Zhang, Xing-hui; Geng, Zhi-yuan; Wang, Ke-tai; Li, Shan-shan

    2014-09-01

    The mechanisms of the palladium-catalyzed hydrothiolation of alkynes with thiols were investigated using density functional theory at the B3LYP/6-31G(d, p) (SDD for Pd) level. Solvent effects on these reactions were explored using the polarizable continuum model (PCM) for the solvent tetrahydrofuran (THF). Markovnikov-type vinyl sulfides or cis-configured anti-Markovnikov-type products were formed by three possible pathways. Our calculation results suggested the following: (1) the first step of the cycle is a proton-transfer process from thiols onto the palladium atom to form a palladium-thiolate intermediate. The palladium-thiolate species is attacked on alkynes to obtain an elimination product, liberating the catalyst. (2) The higher activation energies for the alkyne into the palladium-thiolate bond indicate that this step is the rate-determining step. The Markovnikov-type vinyl sulfide product is favored. However, for the aromatic alkyne, the cis-configured anti-Markovnikov-type product is favored. (3) The activation energy would reduce when thiols are substituted with an aromatic group. Our calculated results are consistent with the experimental observations of Frech and colleagues for the palladium-catalyzed hydrothiolation of alkynes to thiols.

  6. Preparation of Palladium-Impregnated Ceria by Metal Complex Decomposition for Methane Steam Reforming Catalysis

    Directory of Open Access Journals (Sweden)

    Worawat Wattanathana

    2017-01-01

    Full Text Available Palladium-impregnated ceria materials were successfully prepared via an integrated procedure between a metal complex decomposition method and a microwave-assisted wetness impregnation. Firstly, ceria (CeO2 powders were synthesized by thermal decomposition of cerium(III complexes prepared by using cerium(III nitrate or cerium(III chloride as a metal source to form a metal complex precursor with triethanolamine or benzoxazine dimer as an organic ligand. Palladium(II nitrate was consequently introduced to the preformed ceria materials using wetness impregnation while applying microwave irradiation to assist dispersion of the dopant. The palladium-impregnated ceria materials were obtained by calcination under reduced atmosphere of 10% H2 in He stream at 700°C for 2 h. Characterization of the palladium-impregnated ceria materials reveals the influences of the metal complex precursors on the properties of the obtained materials. Interestingly, the palladium-impregnated ceria prepared from the cerium(III-benzoxazine dimer complex revealed significantly higher BET specific surface area and higher content of the more active Pdδ+ (δ > 2 species than the materials prepared from cerium(III-triethanolamine complexes. Consequently, it exhibited the most efficient catalytic activity in the methane steam reforming reaction. By optimization of the metal complex precursors, characteristics of the obtained palladium-impregnated ceria catalysts can be modified and hence influence the catalytic activity.

  7. Development of a second generation palladium-catalyzed cycloalkenylation and its application to bioactive natural product synthesis.

    Science.gov (United States)

    Toyota, Masahiro

    2013-07-01

    A novel palladium-catalyzed intramolecular oxidative alkylation of unactivated olefins is described. This protocol was devised to solve one of the drawbacks of the original palladium-catalyzed cycloalkenylation that we developed. We call this new procedure the 'second generation palladium-catalyzed cycloalkenylation'. This protocol has been applied to the total syntheses of cis-195A, trans-195A, boonein, scholareins A, C, D, and alpha-skytanthine.

  8. Controlled immobilization of palladium nanoparticles in two different fluorinated polymeric aggregate cores and their application in catalysis

    DEFF Research Database (Denmark)

    Kijima, Tetsushi; Javakhishvili, Irakli; Jankova Atanasova, Katja

    2012-01-01

    Fluoroalkyl end-capped betaine-type cooligomeric nanocomposites-immobilized palladium nanoparticles were prepared by the reactions of palladium chloride with sodium acetate in the presence of sodium chloride and the corresponding fluorinated cooligomers. Outer blocks of poly(2,3,4,5,6-pentafluoro....... These fluorinated nanocomposites-immobilized palladium nanoparticles were also applied to the catalysts for Suzuki-Miyaura cross-coupling reaction, and the different reactivity between these nanocomposites was observed....

  9. Potential application of palladium nanoparticles as selective recyclable hydrogenation catalysts

    International Nuclear Information System (INIS)

    Mukherjee, DebKumar

    2008-01-01

    The search for more efficient catalytic systems that might combine the advantages of both homogeneous (catalyst modulation) and heterogeneous (catalyst recycling) catalysis is one of the most exciting challenges of modern chemistry. More recently with the advances of nanochemistry, it has been possible to prepare soluble analogues of heterogeneous catalysts. These nanoparticles are generally stabilized against aggregation into larger particles by electrostatic or steric protection. Herein we demonstrate the use of room temperature ionic liquid for the stabilization of palladium nanoparticles that are recyclable catalysts for the hydrogenation of carbon-carbon double bonds and application of these catalysts to the selective hydrogenation of internal or terminal C=C bonds in unsaturated primary alcohols. The particles suspended in room temperature ionic liquid show no metal aggregation or loss of catalytic activity even on prolonged use

  10. Superparamagnetic bimetallic iron-palladium nanoalloy: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Nazir, Rabia; Mazhar, Muhammad [Department of Chemistry, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Akhtar, M Javed; Nadeem, M; Siddique, Muhammad [Physics Division, PINSTECH, PO Nilore, Islamabad 44000 (Pakistan); Shah, M Raza [HEJ Research Institute of Chemistry, University of Karachi, Karachi 75270 (Pakistan); Khan, Nawazish A [Material Science Laboratory, Department of Physics, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Mehmood, Mazhar [National Centre for Nanotechnology, PIEAS, Islamabad 45650 (Pakistan); Butt, N M [Pakistan Science Foundation, Islamabad 44000 (Pakistan)], E-mail: mazhar42pk@yahoo.com

    2008-05-07

    Iron-palladium nanoalloy in the particle size range of 15-30 nm is synthesized by the relatively low temperature thermal decomposition of coprecipitated [Fe(Bipy){sub 3}]Cl{sub 2} and [Pd(Bipy){sub 3}]Cl{sub 2} in an inert ambient of dry argon gas. The silvery black Fe-Pd alloy nanoparticles are air-stable and have been characterized by EDX-RF, XRD, AFM, TEM, magnetometry, {sup 57}Fe Moessbauer and impedance spectroscopy. This Fe-Pd nanoalloy is in single phase and contains iron sites having up to 11 nearest-neighboring atoms. It is superparamagnetic in nature with high magnetic susceptibility, low coercivity and hyperfine field.

  11. Palladium-based electrocatalysts for ethanol oxidation reaction in DEFC

    International Nuclear Information System (INIS)

    Moraes, L.P.R. de; Elsheikh, A.; Silva, E. L. da; Radtke, C.; Amico, S.C.; Malfatti, C.F.

    2014-01-01

    Direct ethanol fuel cells require the use of electrocatalysts to promote bond cleavage of the ethanol molecule in an efficient way. Currently, most electrocatalysts contain platinum, which enables improved catalytic activity and stability in acidic media. However platinum presents high cost and low availability. Based on that, novel catalysts have been developed, such as those based on palladium and its alloys, which have attained excellent results in the oxidation of ethanol in alkaline media. In this work, Pd, PdSn and PdNiSn catalysts supported on Vulcan XC72R carbon were synthesized via impregnation/reduction. The electrocatalysts were characterized by RBS, XRD and cyclic voltammetry. The X-ray diffraction results showed the formation of an alloy and not the deposition of isolated elements. The synthesized catalysts displayed good catalytic activity, as observed by cyclic voltammetry, being the best electrochemical performance achieved by the ternary alloy. (author)

  12. Reactivity indexes for different geometries of palladium leads

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Carrillo, S C; Bolcatto, P G [Departamento de Fisica, Facultad de Ingenieria Quimica, Universidad Nacional de Litoral, Santiago del Estero 2829 S3000AOM Santa Fe Argentina (Argentina); Ortega, J, E-mail: scgomez@fiq.unl.edu.a [Departamento de Fisica Teorica de la Materia Condensada, Universidad Autonoma de Madrid (Spain)

    2009-05-01

    Electronic transport through metallic break junctions or molecules is clearly dependent not only on the electronic structure of the central nanodevice connecting the leads, but also the shape and crystalline orientation of the contacts which can define the possible conduction channels. In this work we examine different geometries of contacts of palladium characterizing them through global and local reactivity indexes as electrophilicity, chemical hardness and Fukui functions. In molecules, these indicators are essentially defined by the energies of the frontier molecular orbitals and in solids they are related with the local and partial density of states. We use for this purpose an ab-initio based code (FIREBALL), applied to plane contacts with (001) fcc faces and also pyramidal tips grown following a (001) and (111) packaging. The results allow us to have an insight about the chemical features of this type of nanojunctions.

  13. Palladium complexes with simple iminopyridines as catalysts for polyketone synthesis.

    Science.gov (United States)

    Rosar, V; Dedeic, D; Nobile, T; Fini, F; Balducci, G; Alessio, E; Carfagna, C; Milani, B

    2016-10-07

    Four iminopyridines (N-N') differing in the nature of the substituents on the iminic carbon and on the ortho positions of the aryl ring (H or CH3) on the iminic nitrogen were used for the synthesis of neutral and monocationic palladium(ii) complexes of general formulae [Pd(CH3)Cl(N-N')] and [Pd(CH3)(NCCH3)(N-N')][PF6]. The detailed NMR characterization in solution highlighted that: (i) for both series of complexes, the Pd-CH3 signal is progressively shifted to a lower frequency on increasing the number of methyl groups on the ligand skeleton; (ii) for the neutral derivatives, the chemical shift of the (15)N NMR signals, determined through {(1)H,(15)N}-HMBC spectra, is significantly affected by the coordination to palladium; (iii) the coordination induced shift (CIS) of the nitrogen atom trans to the CH3 ligand is smaller than the other. The structure in the solid state for the neutral derivatives with all the four ligands was solved, pointing out that: (iv) the Pd-C bond distance increases with the basicity of the nitrogen-donor ligand; (v) the Pd-N bond distance correlates well with the CIS value. The combining of the solution and solid state structural features allows stating that: (vi) the Pd-CH3 singlet is a good probe for the electron donor capability of the ligand; (vii) the CIS value might be used as a probe for the strength of the Pd-N bond. All monocationic complexes generated active catalysts for the CO/vinyl arene copolymerization, leading to prevailingly syndiotactic polyketones. The catalyst performances, both in terms of catalyst productivity and polymer molecular weight, correlate well with the precatalyst structural features.

  14. Electrophysical properties of silicon doped by palladium-103 isotope

    International Nuclear Information System (INIS)

    Makhkamov, Sh.; Tursunov, N.A.; Sattiev, A.R.; Normurodov, A.B.

    2007-01-01

    The work is devoted to study of radiation physical processes taking place in Si under nuclear transmutation, Identification and determination of defects microstructure and homogeneities and their distribution, study of interactions of nuclear-transformed phosphorus isotopes with palladium atoms, and its effect on crystal properties. For examination monocrystalline silicon of n- and p-type conductivity with specific resistance from 1 to 40 Ω·cm, dislocation density ∼10 4 cm -2 and oxygen content ∼10 17 cm -3 has been applied. Doping of silicon plates by examined admixture has been carried out by thermal diffusion method within temperature range 1000-1250 deg. C for 0.5- 5 h. Irradiation of doped silicon was conducted by reactor neutron fluences 5·10 18 - 5·10 19 cm -2 with subsequent annealing at 1000 deg. C for 30 min. Efficiency of mixture centers formation in silicon, effect of concentration of formed mixture-defect centers on electro-physical, photoelectric and recombination parameters of doped silicon and revealing of type and state of generated defects have been controlled by electric, volume and X-ray fluorescent methods. On the base of spectroscopic researches it is shown, that in silicon forbidden zone after Pd diffusion in DLTS spectra peaks related with acceptor (E c -0.18 and E v +0.34 eV) levels, and peak responsible for level E v +0.32 eV of donor character caused by palladium impurity. It is shown, that irradiation of doped silicon samples by neutrons lead to nuclear transmutation of 102 Pd, 104 Pd in 103 Pd isotopes in the crystal volume with following electron capture in stable isotope 103m Rh

  15. Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

    Science.gov (United States)

    Samanidou, Victoria; Michaelidou, Katia; Kabir, Abuzar; Furton, Kenneth G

    2017-06-01

    Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Pore surface fractal analysis of palladium-alumina ceramic membrane using Frenkel-Halsey-Hill (FHH) model.

    Science.gov (United States)

    Ahmad, A L; Mustafa, N N N

    2006-09-15

    The alumina ceramic membrane has been modified by the addition of palladium in order to improve the H(2) permeability and selectivity. Palladium-alumina ceramic membrane was prepared via a sol-gel method and subjected to thermal treatment in the temperature range 500-1100 degrees C. Fractal analysis from nitrogen adsorption isotherm is used to study the pore surface roughness of palladium-alumina ceramic membrane with different chemical composition (nitric acid, PVA and palladium) and calcinations process in terms of surface fractal dimension, D. Frenkel-Halsey-Hill (FHH) model was used to determine the D value of palladium-alumina membrane. Following FHH model, the D value of palladium-alumina membrane increased as the calcinations temperature increased from 500 to 700 degrees C but decreased after calcined at 900 and 1100 degrees C. With increasing palladium concentration from 0.5 g Pd/100 ml H(2)O to 2 g Pd/100 ml H(2)O, D value of membrane decreased, indicating to the smoother surface. Addition of higher amount of PVA and palladium reduced the surface fractal of the membrane due to the heterogeneous distribution of pores. However, the D value increased when nitric acid concentration was increased from 1 to 15 M. The effect of calcinations temperature, PVA ratio, palladium and acid concentration on membrane surface area, pore size and pore distribution also studied.

  17. Rapid Determination of Trace Palladium in Active Pharmaceutical Ingredients by Magnetic Solid-Phase Extraction and Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Yin, Q. H.; Zhu, D. M.; Yang, D. Z.; Hu, Q. F.; Yang, Y. L.

    2018-01-01

    Clutaraldehyde cross-linked magnetic chitosan nanoparticles were synthesized and used as an adsorbent for the dispersive solid-phase extraction of palladium in active pharmaceutical ingredients (APIs) prior to analysis by a flame atomic absorption spectrophotometer. FT-IR, X-ray diffraction, and TEM were used to characterize the adsorbent. Various parameters of experimental performance, such as adsorbent amount, pH, adsorption time, desorption solutions, coexisting ions, and adsorbent reusability, were investigated and optimized. Under the optimized conditions, good linearity was achieved in the 5.0-500 μg/L concentration range, with correlation coefficients of 0.9989. The limit of detection is 2.8 μg/L and the recoveries of spiked samples ranged from 91.7 to 97.6%. It was confirmed that the GMCNs nanocomposite was a promising adsorbing material for extraction and preconcentration of Pd in APIs.

  18. Remediation of trichloroethylene by bio-precipitated and encapsulated palladium nanoparticles in a fixed bed reactor.

    Science.gov (United States)

    Hennebel, Tom; Verhagen, Pieter; Simoen, Henri; De Gusseme, Bart; Vlaeminck, Siegfried E; Boon, Nico; Verstraete, Willy

    2009-08-01

    Trichloroethylene is a toxic and recalcitrant groundwater pollutant. Palladium nanoparticles bio-precipitated on Shewanella oneidensis were encapsulated in polyurethane, polyacrylamide, alginate, silica or coated on zeolites. The reactivity of these bio-Pd beads and zeolites was tested in batch experiments and trichloroethylene dechlorination followed first order reaction kinetics. The calculated k-values of the encapsulated catalysts were a factor of six lower compared to non-encapsulated bio-Pd. Bio-Pd, used as a catalyst, was able to dechlorinate 100 mgL(-1) trichloroethylene within a time period of 1h. The main reaction product was ethane; yet small levels of chlorinated intermediates were detected. Subsequently polyurethane cubes empowered with bio-Pd were implemented in a fixed bed reactor for the treatment of water containing trichloroethylene. The influent recycle configuration resulted in a cumulative removal of 98% after 22 h. The same reactor in a flow through configuration achieved removal rates up to 1059 mg trichloroethylene g Pd(-1)d(-1). This work showed that fixed bed reactors with bio-Pd polyurethane cubes can be instrumental for remediation of water contaminated with trichloroethylene.

  19. Comparative analysis of minimal residual disease detection using four-color flow cytometry, consensus IgH-PCR, and quantitative IgH PCR in CLL after allogeneic and autologous stem cell transplantation.

    Science.gov (United States)

    Böttcher, S; Ritgen, M; Pott, C; Brüggemann, M; Raff, T; Stilgenbauer, S; Döhner, H; Dreger, P; Kneba, M

    2004-10-01

    The clinically most suitable method for minimal residual disease (MRD) detection in chronic lymphocytic leukemia is still controversial. We prospectively compared MRD assessment in 158 blood samples of 74 patients with CLL after stem cell transplantation (SCT) using four-color flow cytometry (MRD flow) in parallel with consensus IgH-PCR and ASO IgH real-time PCR (ASO IgH RQ-PCR). In 25 out of 106 samples (23.6%) with a polyclonal consensus IgH-PCR pattern, MRD flow still detected CLL cells, proving higher sensitivity of flow cytometry over PCR-genescanning with consensus IgH-primers. Of 92 samples, 14 (15.2%) analyzed in parallel by MRD flow and by ASO IgH RQ-PCR were negative by our flow cytometric assay but positive by PCR, thus demonstrating superior sensitivity of RQ-PCR with ASO primers. Quantitative MRD levels measured by both methods correlated well (r=0.93). MRD detection by flow and ASO IgH RQ-PCR were equally suitable to monitor MRD kinetics after allogeneic SCT, but the PCR method detected impending relapses after autologous SCT earlier. An analysis of factors that influence sensitivity and specificity of flow cytometry for MRD detection allowed to devise further improvements of this technique.

  20. Novel method for the rapid and specific extraction of multiple β2 -agonist residues in food by tailor-made Monolith-MIPs extraction disks and detection by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Liu, Haibo; Gan, Ning; Chen, Yinji; Ding, Qingqing; Huang, Jie; Lin, Saichai; Cao, Yuting; Li, Tianhua

    2016-09-01

    A quick and specific pretreatment method based on a series of extraction clean-up disks, consisting of molecularly imprinted polymer monoliths and C18 adsorbent, was developed for the specific enrichment of salbutamol and clenbuterol residues in food. The molecularly imprinted monolithic polymer disk was synthesized using salbutamol as a template through a one-step synthesis process. It can simultaneously and specifically recognize salbutamol and clenbuterol. The monolithic polymer disk and series of C18 disks were assembled with a syringe to form a set of tailor-made devices for the extraction of target molecules. In a single run, salbutamol and clenbuterol can be specifically extracted, cleaned, and eluted by methanol/acetic acid/H2 O. The target molecules, after a silylation derivatization reaction were detected by gas chromatography-mass spectrometry. The parameters including solvent desorption, sample pH, and the cycles of reloading were investigated and discussed. Under the optimized extraction and clean-up conditions, the limits of detection and quantitation were determined as 0.018-0.022 and 0.042-0.049 ng/g for salbutamol and clenbuterol, respectively. The assay described was convenient, rapid, and specific; thereby potentially efficient in the high-throughput analysis of β2 -agonists residues in real food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Development and validation of a solid-phase extraction method coupled to liquid chromatography with fluorescence detection for the determination of fluoroquinolone residues in powdered infant formulae. Application to the analysis of samples from the Spanish and Latin American market.

    Science.gov (United States)

    Rodriguez, E; Moreno-Bondi, M C; Marazuela, M D

    2008-10-31

    This paper describes a new method for the effective extraction, clean-up and chromatographic analysis of residues of four fluoroquinolones (ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in powdered infant formulae and follow-on preparations. Samples were reconstituted following the manufacturer's recommendations and treated with trichloroacetic acid in methanol 10% (w/v) for deproteinization. Two solid-phase extraction cartridges have been evaluated for sample clean-up and preconcentration, Strata Screen A and Strata X and the later provided the best recoveries for all the analytes tested. Chromatographic analysis has been carried out using a polar endcapped column (AQUA C(18)) and fluorescence detection, with lomefloxacin (LOME) as internal standard. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(alpha)) and detection capability (CC(beta)). Typical recoveries ranged between 70 and 110% at levels below and above the maximum residue limits of the target analytes in bovine milk, with an excellent intralab reproducibility (RSDsmarket, using LC-MS/MS as confirmatory technique.

  2. Low-temperature solution processing of palladium/palladium oxide films and their pH sensing performance.

    Science.gov (United States)

    Qin, Yiheng; Alam, Arif U; Pan, Si; Howlader, Matiar M R; Ghosh, Raja; Selvaganapathy, P Ravi; Wu, Yiliang; Deen, M Jamal

    2016-01-01

    Highly sensitive, easy-to-fabricate, and low-cost pH sensors with small dimensions are required to monitor human bodily fluids, drinking water quality and chemical/biological processes. In this study, a low-temperature, solution-based process is developed to prepare palladium/palladium oxide (Pd/PdO) thin films for pH sensing. A precursor solution for Pd is spin coated onto pre-cleaned glass substrates and annealed at low temperature to generate Pd and PdO. The percentages of PdO at the surface and in the bulk of the electrodes are correlated to their sensing performance, which was studied by using the X-ray photoelectron spectroscope. Large amounts of PdO introduced by prolonged annealing improve the electrode's sensitivity and long-term stability. Atomic force microscopy study showed that the low-temperature annealing results in a smooth electrode surface, which contributes to a fast response. Nano-voids at the electrode surfaces were observed by scanning electron microscope, indicating a reason for the long-term degradation of the pH sensitivity. Using the optimized annealing parameters of 200°C for 48 h, a linear pH response with sensitivity of 64.71±0.56 mV/pH is obtained for pH between 2 and 12. These electrodes show a response time shorter than 18 s, hysteresis less than 8 mV and stability over 60 days. High reproducibility in the sensing performance is achieved. This low-temperature solution-processed sensing electrode shows the potential for the development of pH sensing systems on flexible substrates over a large area at low cost without using vacuum equipment. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. The determination of pesticide residues and contaminants in vegetables by means of neutron activation analysis. Part of a coordinated programme on nuclear detection and analysis

    International Nuclear Information System (INIS)

    Mongkolphanta, S.

    1977-11-01

    Neutron activation techniques have been applied to study the existence of pesticide residues (As, Br, Hg) and pollutants (Cd, Co, Zn) in local vegetable and fruit samples, polished and unpolished glutinous and non-glutinous milled rice, and fish caught in polluted and unpolluted areas of the Gulf of Thailand. Since the baseline levels of these toxic elements in vegetables, fruits, rice and fish are not known as yet, the results cannot be regarded as conclusive. Furthermore, no significant difference was observed in the concentration of these elements in fish caught in polluted and unpolluted areas. The Gulf of Thailand does not therefore appear to be polluted at present. The substoichiometric isotope dilution technique was successfully applied to mercury determinations, and only to a limited extent to Cd due to shutdown of the TRR-1 reactor

  4. Flow cytometric minimal residual disease assessment of peripheral blood in acute lymphoblastic leukaemia patients has potential for early detection of relapsed extramedullary disease.

    Science.gov (United States)

    Keegan, Alissa; Charest, Karry; Schmidt, Ryan; Briggs, Debra; Deangelo, Daniel J; Li, Betty; Morgan, Elizabeth A; Pozdnyakova, Olga

    2018-03-27

    To evaluate peripheral blood (PB) for minimal residual disease (MRD) assessment in adults with acute lymphoblastic leukaemia (ALL). We analysed 76 matched bone marrow (BM) aspirate and PB specimens independently for the presence of ALL MRD by six-colour flow cytometry (FC). The overall rate of BM MRD-positivity was 24% (18/76) and PB was also MRD-positive in 22% (4/18) of BM-positive cases. We identified two cases with evidence of leukaemic cells in PB at the time of the extramedullary relapse that were interpreted as MRD-negative in BM. The use of PB MRD as a non-invasive method for monitoring of systemic relapse may have added clinical and diagnostic value in patients with high risk of extramedullary disease. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2018. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

  5. Synthesis of palladium nanoparticle modified reduced graphene oxide and multi-walled carbon nanotube hybrid structures for electrochemical applications

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jie, E-mail: hujie@tyut.edu.cn [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); Zhao, Zhenting; Zhang, Jun; Li, Gang; Li, Pengwei; Zhang, Wendong [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); Lian, Kun, E-mail: liankun@tyut.edu.cn [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); School of Nano-Science and Nano-Engineering, Suzhou & Collaborative Innovation Center of Suzhou Nano Science and Technology, Xi' an Jiaotong University, Xi' an, 710049 (China); Center for Advanced Microstructures and Devices, Louisiana State University, LA, 70806 (United States)

    2017-02-28

    Graphical abstract: A sensitive hydrazine electrochemical sensor was fabricated by using palladium (Pd) nanoparticle functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotube (MWCNTs) hybrid structures (Pd/rGO-MWCNTs). - Highlights: • rGO-MWCNTs hybrid structures and Pd nanoparticles are prepared using electrochemical methods. • rGO-MWCNTs hybrid films are used as supports and co-catalysts for Pd nanoparticles. • The Pd/rGO-MWCNTs hybrid structure based sensor shows an ultra-high sensitivity of 7.09 μA μM{sup −1} cm{sup −2} and a low detection limit of 0.15 μM. • The proposed electrochemical sensor exhibits excellent selectivity. - Abstract: In this work, palladium (Pd) nanoparticles functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotubes (MWCNTs) hybrid structures (Pd/rGO-MWCNTs) were successfully prepared by a combination of electrochemical reduction with electrodeposition method. The morphology, structure, and composition of the Pd/rGO-MWCNTs hybrid were characterized by scanning electron microscopy, transmission electron microscopy and energy dispersive spectroscopy. The as-synthesized hybrid structures were modified on the glassy carbon electrode (GCE) and further utilized for hydrazine sensing. Electrochemical impedance spectroscopic, cyclic voltammetry and single-potential amperometry experiments were carried out on Pd/rGO-MWCNTs hybrid structures to investigate the interface properties and sensing performance. The measured results demonstrate that the fabricated Pd/rGO-MWCNTs/GCE sensor show a high sensitivity of 7.09 μA μM{sup −1} cm{sup −2} in a large concentration range of 1.0 to 1100 μM and a low detection limit of 0.15 μM. Moreover, the as-prepared sensor exhibits good selectivity and stability for the determination of hydrazine under interference conditions.

  6. Synthesis of palladium nanoparticle modified reduced graphene oxide and multi-walled carbon nanotube hybrid structures for electrochemical applications

    International Nuclear Information System (INIS)

    Hu, Jie; Zhao, Zhenting; Zhang, Jun; Li, Gang; Li, Pengwei; Zhang, Wendong; Lian, Kun

    2017-01-01

    Graphical abstract: A sensitive hydrazine electrochemical sensor was fabricated by using palladium (Pd) nanoparticle functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotube (MWCNTs) hybrid structures (Pd/rGO-MWCNTs). - Highlights: • rGO-MWCNTs hybrid structures and Pd nanoparticles are prepared using electrochemical methods. • rGO-MWCNTs hybrid films are used as supports and co-catalysts for Pd nanoparticles. • The Pd/rGO-MWCNTs hybrid structure based sensor shows an ultra-high sensitivity of 7.09 μA μM"−"1 cm"−"2 and a low detection limit of 0.15 μM. • The proposed electrochemical sensor exhibits excellent selectivity. - Abstract: In this work, palladium (Pd) nanoparticles functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotubes (MWCNTs) hybrid structures (Pd/rGO-MWCNTs) were successfully prepared by a combination of electrochemical reduction with electrodeposition method. The morphology, structure, and composition of the Pd/rGO-MWCNTs hybrid were characterized by scanning electron microscopy, transmission electron microscopy and energy dispersive spectroscopy. The as-synthesized hybrid structures were modified on the glassy carbon electrode (GCE) and further utilized for hydrazine sensing. Electrochemical impedance spectroscopic, cyclic voltammetry and single-potential amperometry experiments were carried out on Pd/rGO-MWCNTs hybrid structures to investigate the interface properties and sensing performance. The measured results demonstrate that the fabricated Pd/rGO-MWCNTs/GCE sensor show a high sensitivity of 7.09 μA μM"−"1 cm"−"2 in a large concentration range of 1.0 to 1100 μM and a low detection limit of 0.15 μM. Moreover, the as-prepared sensor exhibits good selectivity and stability for the determination of hydrazine under interference conditions.

  7. The study of hydrogen electrosorption in layered nickel foam/palladium/carbon nanofibers composite electrodes

    International Nuclear Information System (INIS)

    Skowronski, J.M.; Czerwinski, A.; Rozmanowski, T.; Rogulski, Z.; Krawczyk, P.

    2007-01-01

    In the present work, the process of hydrogen electrosorption occurring in alkaline KOH solution on the nickel foam/palladium/carbon nanofibers (Ni/Pd/CNF) composite electrodes is examined. The layered Ni/Pd/CNF electrodes were prepared by a two-step method consisting of chemical deposition of a thin layer of palladium on the nickel foam support to form Ni/Pd electrode followed by coating the palladium layer with carbon nanofibers layer by means of the CVD method. The scanning electron microscope was used for studying the morphology of both the palladium and carbon layer. The process of hydrogen sorption/desorption into/from Ni/Pd as well as Ni/Pd/CNF electrode was examined using the cyclic voltammetry method. The amount of hydrogen stored in both types of composite electrodes was shown to increase on lowering the potential of hydrogen sorption. The mechanism of the anodic desorption of hydrogen changes depending on whether or not CNF layer is present on the Pd surface. The anodic peak corresponding to the removal of hydrogen from palladium is lower for Ni/Pd/CNF electrode as compared to that measured for Ni/Pd one due to a partial screening of the Pd surface area by CNF layer. The important feature of Ni/Pd/CNF electrode is anodic peak appearing on voltammetric curves at potential ca. 0.4 V more positive than the peak corresponding to hydrogen desorption from palladium. The obtained results showed that upon storing the hydrogen saturated Ni/Pd/CNF electrode at open circuit potential, diffusion of hydrogen from carbon to palladium phase occurs due to interaction between carbon fibers and Pd sites on the nickel foam support

  8. The electrocatalytical reduction of m-nitrophenol on palladium nanoparticles modified glassy carbon electrodes

    International Nuclear Information System (INIS)

    Shi Qiaofang; Diao Guowang

    2011-01-01

    Highlights: ► The deposition of palladium on a GC electrode was performed by cyclic voltammetry. ► SEM images showed palladium nanoparticles deposited on a glassy carbon (GC) electrode. ► The Pd/GC electrode can effectively catalyze m-nitrophenol in aqueous media. ► The reduction of m-nitrophenol on the Pd/GC electrode depended on potential and pH. ► XPS spectra of the Pd/GC electrodes demonstrated the presence of palladium. - Abstract: Palladium nanoparticles modified glassy carbon electrodes (Pd/GC) were prepared via the electrodeposition of palladium on a glassy carbon (GC) electrode using cyclic voltammetry in different sweeping potential ranges. The scanning electron microscope images of palladium particles on the GC electrodes indicate that palladium particles with diameters of 20–50 nm were homogeneously dispersed on the GC electrode at the optimal deposition conditions, which can effectively catalyze the reduction of m-nitrophenol in aqueous solutions, but their catalytic activities are strongly related to the deposition conditions of Pd. The X-ray photoelectron spectroscopy spectra of the Pd/GC electrode confirmed that 37.1% Pd was contained in the surface composition of the Pd/GC electrode. The cyclic voltammograms of the Pd/GC electrode in the solution of m-nitrophenol show that the reduction peak of m-nitrophenol shifts towards the more positive potentials, accompanied with an increase in the peak current compared to the bare GC electrode. The electrocatalytic activity of the Pd/GC electrode is affected by pH values of the solution. In addition, the electrolysis of m-nitrophenol under a constant potential indicates that the reduction current of m-nitrophenol on the Pd/GC electrode is approximately 20 times larger than that on the bare GC electrode.

  9. Observation of Binuclear Palladium Clusters Upon ESI-MS Monitoring of the Suzuki-Miyaura Cross-Coupling Catalyzed by a Dichloro-bis(aminophosphine) Complex of Palladium

    Czech Academy of Sciences Publication Activity Database

    Agrawal, Divya; Schröder, Detlef; Frech, C. M.

    2011-01-01

    Roč. 30, č. 13 (2011), s. 3579-3587 ISSN 0276-7333 Institutional research plan: CEZ:AV0Z40550506 Keywords : catalysis * C-C coupling * electrospray ionization * palladium * Suzuki-Miyaura coupling Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.963, year: 2011

  10. A RIKILT yeast estrogen bioassay (REA) for estrogen residue detection in urine of calves experimentally treated with 17ß-estradiol

    NARCIS (Netherlands)

    Divari, S.; Maria, De R.; Cannizzo, F.T.; Spada, F.; Mulasso, C.; Bovee, T.F.H.; Capra, P.; Leporati, M.; Biolatti, B.

    2010-01-01

    17ß-Estradiol is one of the most powerful sex steroids illegally used in bovine production. The objective of this study was to evaluate the application and the specificity of the RIKILT yeast estrogen bioassay (REA) for the detection of molecules with estrogenic activities in the urine of calves

  11. ICG-fluorescence imaging for detection of peritoneal metastases and residual tumoral scars in locally advanced ovarian cancer: A pilot study.

    Science.gov (United States)

    Veys, Isabelle; Pop, Florin-Catalin; Vankerckhove, Sophie; Barbieux, Romain; Chintinne, Marie; Moreau, Michel; Nogaret, Jean-Marie; Larsimont, Denis; Donckier, Vincent; Bourgeois, Pierre; Liberale, Gabriel

    2018-02-01

    No intraoperative imaging techniques exist for detecting tumor nodules or tumor scar tissues in patients treated with upfront or interval cytoreductive surgery (CS) after neoadjuvant chemotherapy (NAC). The aims of this study were to evaluate the role of indocyanine green (ICG) fluorescence imaging (FI) for the detection of peritoneal metastases (PM) and evaluate whether it can be used to detect remnant tumor cells in scar tissue. Patients with PM from ovarian cancer admitted for CS were included. ICG, at 0.25 mg per kg of patient weight, was injected intraoperatively after explorative laparotomy before CS. A total of 108 peritoneal lesions, including 25 scars, were imaged in 20 patients. Seventy-three were malignant (67.6%) and 35 benign (32.4%). The mean Tumor to Background Ratio (ex vivo) was 1.8 (SD 1.3) in malignant and 1.0 (SD 0.79) in benign nodules (P = 0.007). Of 25 post-NAC scars, the mean Tumor to Background Ratio (TBR) (in vivo) was 2.06 (SD 1.15) in malignant and 1.21 (SD 0.50) in benign nodules (P = 0.26). The positive predictive value of ICG-FI to detect tumor cells in scars was 57.1%. ICG-FI is accurate to demonstrate PM in ovarian cancer but unable to discriminate between benign and malignant post-NAC. © 2017 Wiley Periodicals, Inc.

  12. Validation of the System One RemStar Auto A-Flex for Obstructive Sleep Apnea Treatment and Detection of Residual Apnea-Hypopnea Index

    DEFF Research Database (Denmark)

    Gagnadoux, Frédéric; Pevernagie, Dirk; Jennum, Poul

    2017-01-01

    the performance of the System One RemStar Auto A-Flex (Philips Respironics, Murrysville, PA, USA) automatically adjusted positive airway pressure (APAP) mode to manually titrated, fixed pressure CPAP and to validate the device's breathing event detection capabilities against attended in-laboratory PSG. METHODS...

  13. Comparison of Lateral Flow Assay, Kidney Inhibition Swab, and Liquid Chromatography-Tandem Mass Spectrometry for the Detection of Penicillin G Residues in Sow Urine.

    Science.gov (United States)

    Shelver, Weilin L; Chakrabarty, Shubhashis; Smith, David J

    2017-03-01

    Sows (n = 126) were administered penicillin G; urine, collected at slaughter, was screened by kidney inhibition swab (KIS; 4 h testing time) and then stored at -80 °C (∼1200 days) until analysis by lateral flow assay (LF, ∼5 min testing time) and tandem quadrupole LC-MS/MS (TQ) analysis. The stability of penicillin in urine during storage was verified using TQ analyses. Quantitative results were well-correlated (R 2 = 0.98) with only a ∼10% decrease in penicillin concentration during the 3-year storage period. KIS retesting of stored samples returned results consistent with the original analyses. Lateral flow assay results were highly correlated with the KIS and TQ results. A KIS positive sample, which was not confirmed by TQ or LF, was assayed by Triple-TOF LC-MS to determine the cause of the apparent false positive. This study suggests LF can be used to quickly and efficiently screen for penicillin G residues before slaughter.

  14. Clean-up of aqueous acetone vegetable extracts by solid-matrix partition for pyrethroid residue determination by gas chromatography-electron-capture detection.

    Science.gov (United States)

    Di Muccio, A; Barbini, D A; Generali, T; Pelosi, P; Ausili, A; Vergori, F; Camoni, I

    1997-03-21

    Disposable, ready-to-use cartridges filled with macroporous diatomaceous material are used to carry out a partition clean-up that, in a single step, is capable of transferring pesticide residues from aqueous acetone extracts into light petroleum-dichloromethane (75:25, v/v). This procedure takes the place of some functions (such as separatory-funnel partition, drying over anhydrous sodium sulphate and partial adsorption clean-up) usually performed by separate steps in classical schemes. Fourteen pyrethroid pesticides, including tefluthrin, tetramethrin, cyphenothrin, cyfluthrin, flucythrinate, tau-fluvalinate, deltamethrin, bioallethrin, fenpropathrin, lambda-cyhalothrin, permethrin, alpha-cypermethrin, esfenvalerate and tralomethrin were determined using the described procedure with satisfactory recoveries for most of them, at spiking levels ranging from 0.08 to 0.82 mg/kg for the different compounds. Crops subjected to the described procedure included strawberry, apple, and orange gave extracts containing a mass of co-extractives that was between 5 and 30 mg. Compared with classical schemes, the described procedure is simple, less labour intensive, allows parallel handling of several extracts and does not require the preparation and maintenance of equipment. Troublesome emulsions such as those frequently observed in separation funnel partitioning do not occur.

  15. Separation of Hydrogen Isotopes by Palladium Alloy Membranes Separator

    International Nuclear Information System (INIS)

    Jiangfeng, S.; Deli, L.; Yifu, X.; Congxian, L.; Zhiyong, H.

    2007-01-01

    Full text of publication follows: Separation of hydrogen isotope with palladium alloy membranes is one of the promising methods for hydrogen isotope separation. It has several advantages, such as high separation efficiency, smaller tritium inventory, simple separation device, ect. Limited by the manufacture of membrane and cost of gas transportation pump, this method is still at the stage of conceptual study. The relationship between separation factors and temperatures, feed gas components, split ratios have not been researched in detail, and the calculated results of cascade separation have not been validated with experimental data. In this thesis, a palladium alloy membrane separator was designed to further study its separation performance between H 2 and D 2 . The separation factor of the single stage was affected by the temperature, the feed gas component, the split ratio and the gas flow rate, etc. The experimental results showed that the H 2 -D 2 separation factor decreased with the increasing of temperature. On the temperature from 573 K to 773 K, when the feed rate was 5 L/min, the separation factor of 66.2%H 2 - 33.8%D 2 decreased from 2.09 to 1.85 when the split ratio was 0.1 and from 1.74 to 1.52 when the split ratio was 0.2.The separation factor also decreased with the increasing of split ratio. At 573 K and the feed rate of 5 L/min, the separation factor of 15.0%H 2 and 85.0%D 2 decreased from 2.43 to 1.35 with the increasing of split ratio from 0.050 to 0.534,and for 66.2%H 2 -33.8%D 2 , the separation factor decreased from 2.87 to 1.30 with the increasing of split ratio from 0.050 to 0.688. When the separation factor was the biggest, the flow rate of feed gas was in a perfect value. To gain a best separation performance, perfect flow rate, lower temperature and reflux ratio should be chosen. (authors)

  16. Chiral separation of substituted phenylalanine analogues using chiral palladium phosphine complexes with enantioselective liquid-liquid extraction

    NARCIS (Netherlands)

    Verkuijl, B.J.V.; Schuur, B.; Minnaard, A.J.; Vries, de J.G.; Feringa, B.L.

    2010-01-01

    Chiral palladium phosphine complexes have been employed in the chiral separation of amino acids and phenylalanine analogues in particular. The use of (S)-xylyl-BINAP as a ligand for the palladium complex in enantioselective liquid–liquid extraction allowed the separation of the phenylalanine

  17. Palladium-Catalyzed Cross-Coupling Reactions of Perfluoro Organic Compounds

    Directory of Open Access Journals (Sweden)

    Masato Ohashi

    2014-09-01

    Full Text Available In this review, we summarize our recent development of palladium(0-catalyzed cross-coupling reactions of perfluoro organic compounds with organometallic reagents. The oxidative addition of a C–F bond of tetrafluoroethylene (TFE to palladium(0 was promoted by the addition of lithium iodide, affording a trifluorovinyl palladium(II iodide. Based on this finding, the first palladium-catalyzed cross-coupling reaction of TFE with diarylzinc was developed in the presence of lithium iodide, affording α,β,β-trifluorostyrene derivatives in excellent yield. This coupling reaction was expanded to the novel Pd(0/PR3-catalyzed cross-coupling reaction of TFE with arylboronates. In this reaction, the trifluorovinyl palladium(II fluoride was a key reaction intermediate that required neither an extraneous base to enhance the reactivity of organoboronates nor a Lewis acid additive to promote the oxidative addition of a C–F bond. In addition, our strategy utilizing the synergetic effect of Pd(0 and lithium iodide could be applied to the C–F bond cleavage of unreactive hexafluorobenzene (C6F6, leading to the first Pd(0-catalyzed cross-coupling reaction of C6F6 with diarylzinc compounds.

  18. Factors affecting the corrosion of SiC layer by fission product palladium

    International Nuclear Information System (INIS)

    Dewita, E.

    2000-01-01

    HTR is one of the advanced nuclear reactors which has inherent safety system, graphite moderated and helium gas cooled. In general, these reactors are designed with the TRISO coated particle consist of four coating layers that are porous pyrolytic carbon (PyC). inner dense PyC (IPyC), silicon carbide (SiC), and outer dense PyC (OPyC). Among the four coating layers, the SiC plays an important role beside in retaining metallic fission products, it also provides mechanical strength to fuel particle. However, results of post irradiation examination indicate that fission product palladium can react with and corrode SiC layer, This assessment is conducted to get the comprehension about resistance of SiC layer on irradiation effects, especially in order to increase the fuel bum-up. The result of this shows that the corrosion of SiC layer by fission product palladium is beside depend on the material characteristics of SiC, and also there are other factors that affect on the SiC layer corrosion. Fuel enrichment, bum-up, and irradiation time effect on the palladium flux in fuel kernel. While, the fuel density, vapour pressure of palladium (the degree depend on the irradiation temperature and kernel composition) effect on palladium migration in fuel particle. (author)

  19. Some remarks on the neutron elastic- and enelastic-scattering cross sections of palladium

    International Nuclear Information System (INIS)

    Chiba, S.; Guenther, P.T.; Smith, A.B.

    1989-05-01

    The cross sections for the elastic-scattering of 5.9, 7.1 and 8.0 MeV neutrons from elemental palladium were measured at forty scattering angles distributed between ∼15/degree/ and 160/degree/. The inelastic-scattering cross sections for the excitation of palladium levels at energies of 260 keV to 560 keV were measured with high resolution at the same energies, and at a scattering angle of 80/degree/. The experimental results were combined with lower-energy values previously obtained by this group to provide a comprehensive data base extending from near the inelastic-scattering threshold to 8 MeV. That data base was interpreted in terms of a coupled-channel model, including the inelastic excitation of one- and two-phonon vibrational levels of the even isotopes of palladium. It was concluded that the palladium inelastic-scattering cross section, at the low energies of interest in assessment of fast-fission-reactor performance, are large (∼50% greater than given in widely used evaluated fission-product data files). They primarily involve compound-nucleus processes, with only a small direct-reaction component attributable to the excitation of the one-phonon, 2 + , vibrational levels of the even isotopes of palladium. 24 refs., 6 figs

  20. Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.

    Science.gov (United States)

    Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

    2001-12-14

    A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes.

  1. Simultaneous determination of residues of emamectin and its metabolites, and milbemectin, ivermectin, and abamectin in crops by liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Yoshii, K; Kaihara, A; Tsumura, Y; Ishimitsu, S; Tonogai, Y

    2001-01-01

    A liquid chromatographic (LC) method was developed for the determination of emamectin and its metabolites (8,9-Z-isomer, N-demethylated, N-formylated, and N-methylformylated emamectin) in various crops. The analytes were extracted with acetone, cleaned up on cartridge columns (C18 and NH2), derivatized with trifluoroacetic anhydride and 1-methylimidazole, and determined by LC with fluorescence detection. Because radish inhibited the formation of the fluorescent derivatives, an additional Bond Elut PRS cartridge was used in the cleanup of Japanese radish samples. During sample preparation, N-formylated emamectin partially degraded to emamectin B1b and emamectin B1a, and the 8,9-Z-isomer partially degraded to N-demethylated emamectin. Therefore, emamectin and its metabolites were determined as total emamectin, i.e., their sum was estimated as emamectin benzoate. Their recoveries from most crops were approximately 80-110% with the developed method. The detection limits for the analytes in vegetables were 0.1-0.3 parts per trillion (ppt). The results for these compounds were confirmed by LC/mass spectrometry (LC/MS; electrospray ionization mode). Because the fluorescent derivative of emamectin was undetectable by LC/MS, the results for the analyte were confirmed by using a sample solution without derivatization. Limits of detection by LC/MS were similar to the fluorescence detection limits, 0.1-0.3 ppt in vegetables. In addition to the emamectins, milbemectin, ivermectin, and abamectin were also determined by the developed method.

  2. Detection of tannins in modern and fossil barks and in plant residues by high-resolution solid-state /sup 13/C nuclear magnetic resonance

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, M A; Hatcher, P G

    1988-01-01

    Bark samples isolated from brown coal deposits in Victoria, Australia, and buried wood from Rhizophora mangle have been studied by high-resolution solid-state nuclear magnetic resonance (NMR) techniques. Dipolar dephasing /sup 13/C NMR appears to be a useful method of detecting the presence of tannins in geochemical samples including barks, buried woods, peats and leaf litter. It is shown that tannins are selectively preserved in bark during coalification to the brown coal stage. 28 refs., 9 figs., 1 tab.

  3. Detection of tannins in modern and fossil barks and in plant residues by high-resolution solid-state 13C nuclear magnetic resonance

    Science.gov (United States)

    Wilson, M.A.; Hatcher, P.G.

    1988-01-01

    Bark samples isolated from brown coal deposits in Victoria, Australia, and buried wood from Rhizophora mangle have been studies by high-resolution solid-state nuclear magnetic resonance (NMR) techniques. Dipolar dephasing 13C NMR appears to be a useful method of detecting the presence of tannins in geochemical samples including barks, buried woods, peats and leaf litter. It is shown that tannins are selectively preserved in bark during coalification to the brown coal stage. ?? 1988.

  4. Wide-scope analysis of pesticide and veterinary drug residues in meat matrices by high resolution MS: detection and identification using Exactive-Orbitrap.

    Science.gov (United States)

    Gómez-Pérez, María Luz; Romero-González, Roberto; Plaza-Bolaños, Patricia; Génin, Eric; Martínez Vidal, José Luis; Garrido Frenich, Antonia

    2014-01-01

    A multiresidue and multiclass method for the simultaneous determination of more than 350 compounds including pesticides, biopesticides and veterinary drugs in different meat matrices (beef, pork and chicken) by ultra-high performance liquid chromatography coupled to Orbitrap MS has been developed. In the present study, the determination of fragments was accomplished as an essential tool for a reliable identification of compounds using high resolution MS. To obtain these fragments, different strategies have been carried out in order to ensure an appropriate fragment assignment and identification. The analytical method is suitable for qualitative analysis, and it was also evaluated for quantitative analysis. Generic extraction conditions were optimized, obtaining adequate recovery and precision values for most of the studied analytes (>290). The limits of detection ranged from 2 to 16 µg kg(-1). Limits of quantification were 10 µg kg(-1) with the exception of few compounds with a higher value (50 or 100 µg kg(-1)). Limits of identification were also established, and they ranged from 2 to 150 µg kg(-1). This method was applied to the analysis of 18 meat samples and some veterinary drugs as enrofloxacin and sulfadiazine were detected and further identified/quantified (with triple quadrupole) in two different samples at 33 µg kg(-1) and trace levels, respectively. No pesticides were detected in the analyzed samples. Copyright © 2014 John Wiley & Sons, Ltd.

  5. Droplet Digital PCR for BCR/ABL(P210) Detecting of CML: A High Sensitive Method of the Minimal Residual Disease& Disease Progression.

    Science.gov (United States)

    Wang, Wen-Jun; Zheng, Chao-Feng; Liu, Zhuang; Tan, Yan-Hong; Chen, Xiu-Hua; Zhao, Bin-Liang; Li, Guo-Xia; Xu, Zhi-Fang; Ren, Fang-Gang; Zhang, Yao-Fang; Chang, Jian-Mei; Wang, Hong-Wei

    2018-04-25

    The present study intended to establish a droplet digital PCR (dd-PCR) for monitoring minimal residual disease (MRD) in patients with BCR/ABL (P210)-positive CML, thereby achieving deep-level monitoring of tumor load and determining the efficacy for guided clinically individualized treatment. Using dd-PCR and RT-qPCR, two cell suspensions were obtained from K562 cells and normal peripheral blood mononuclear cells by gradient dilution and were measured at the cellular level. At peripheral blood(PB) level, 61 cases with CML-chronic phase (CML-CP) were obtained after tyrosine kinase inhibitors (TKIs) treatment and regular follow-ups. By RT-qPCR, BCR/ABL (P210) fusion gene was undetectable in PB after three successive analyses, which were performed once every three months. At the same time, dd-PCR was performed simultaneously with the last equal amount of cDNA. Ten CML patients with MR4.5 were followed up by the two methods. At the cellular level, consistency of results of dd-PCR and RT-qPCR reached R 2 ≥0.99, with conversion equation of Y=33.148X 1.222 (Y: dd-PCR results; X: RT-qPCR results). In the dd-PCR test, 11 of the 61 CML patients (18.03%) tested positive and showed statistically significant difference (PPCR 3 months earlier than by RT-qPCR. In contrast with RT-qPCR, dd-PCR is more sensitive, thus enabling accurate conversion of dd-PCR results into internationally standard RT-qPCR results by conversion equation, to achieve a deeper molecular biology-based stratification of BCR/ABL(P210) MRD. It has some reference value to monitor disease progression in clinic. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  6. Highly sensitive glucose sensor based on monodisperse palladium nickel/activated carbon nanocomposites.

    Science.gov (United States)

    Koskun, Yağmur; Şavk, Aysun; Şen, Betül; Şen, Fatih

    2018-06-20

    Glucose enzyme biosensors have been used for a variety of applications such as medical diagnosis, bioprocess engineering, beverage industry and environmental scanning etc. and there is still a growing interest in glucose sensors. For this purpose, addressed herein, as a novel glucose sensor, highly sensitive activated carbon (AC) decorated monodisperse nickel and palladium alloy nanocomposites modified glassy carbon electrode (Ni-Pd@AC/GCE NCs) have been synthesized by in-situ reduction technique. Raman Spectroscopy (RS), X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), cyclic voltammetry (CV) and chronoamperometry (CA) were used for the characterization of the prepared non-enzymatic glucose sensor. The characteristic sensor properties of the Ni-Pd@AC/GCE electrode were compared with Ni-Pd NCs/GCE, Ni@AC/GCE and Pd@AC/GCE and the results demonstrate that the AC is very effective in the enhancement of the electrocatalytic properties of sensor. In addition, the Ni-Pd@AC/GCE nanocomposites showed a very low detection limit of 0.014 μM, a wide linear range of 0.01 mM-1 mM and a very high sensitivity of 90 mA mM -1  cm -2 . Furthermore, the recommended sensor offer the various advantageous such as facile preparation, fast response time, high selectivity and sensitivity. Lastly, monodisperse Ni-Pd@AC/GCE was utilized to detect glucose in real sample species. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. A Fumonisins Immunosensor Based on Polyanilino-Carbon Nanotubes Doped with Palladium Telluride Quantum Dots

    Science.gov (United States)

    Masikini, Milua; Mailu, Stephen N.; Tsegaye, Abebaw; Njomo, Njagi; Molapo, Kerileng M.; Ikpo, Chinwe O.; Sunday, Christopher Edozie; Rassie, Candice; Wilson, Lindsay; Baker, Priscilla G. L.; Iwuoha, Emmanuel I.

    2015-01-01

    An impedimetric immunosensor for fumonisins was developed based on poly(2,5-dimethoxyaniline)-multi-wall carbon nanotubes doped with palladium telluride quantum dots onto a glassy carbon surface. The composite was assembled by a layer-by-layer method to form a multilayer film of quantum dots (QDs) and poly(2,5-dimethoxyaniline)-multi-wall carbon nanotubes (PDMA-MWCNT). Preparation of the electrochemical immunosensor for fumonisins involved drop-coating of fumonisins antibody onto the composite modified glassy carbon electrode. The electrochemical impedance spectroscopy response of the FB1 immunosensor (GCE/PT-PDMA-MWCNT/anti-Fms-BSA) gave a linear range of 7 to 49 ng L−1 and the corresponding sensitivity and detection limits were 0.0162 kΩ L ng−1 and 0.46 pg L−1, respectively, hence the limit of detection of the GCE/PT-PDMA-MWCNT immunosensor for fumonisins in corn certified material was calculated to be 0.014 and 0.011 ppm for FB1, and FB2 and FB3, respectively. These results are lower than those obtained by ELISA, a provisional maximum tolerable daily intake (PMTDI) for fumonisins (the sum of FB1, FB2, and FB3) established by the Joint FAO/WHO expert committee on food additives and contaminants of 2 μg kg−1 and the maximum level recommended by the U.S. Food and Drug Administration (FDA) for protection of human consumption (2–4 mg L−1). PMID:25558993

  8. Metallothionein (MT) response after chronic palladium exposure in the zebra mussel, Dreissena polymorpha

    International Nuclear Information System (INIS)

    Frank, Sabrina N.; Singer, Christoph; Sures, Bernd

    2008-01-01

    The effects of different exposure concentrations of palladium (Pd) on relative metallothionein (MT) response and bioaccumulation were investigated in zebra mussels (Dreissena polymorpha). The mussels were exposed to 0.05, 5, 50, and 500 μg/L Pd 2+ for 10 weeks under controlled temperature and fasting conditions. Relative MT contents were assessed by a modified Ag-saturation method, which allows to discriminate between MT bound to Pd (Pd-MT) and MT bound to unidentified metals (Ag-MT). Determination of metal contents resulted from atomic absorption spectrometry following a microwave digestion. For unexposed mussels and mussels exposed to 0.05 μg/L Pd no metal accumulation could be detected. All other exposure concentrations resulted in detectable Pd accumulation in mussels with final tissue concentrations of 96 μg/g (500 μg/L), 45 μg/g (50 μg/L), and 9 μg/g (5 μg/L). Compared with initial levels Pd-MT concentrations at the end of the exposure period were 600 (500 μg/L), 160 (50 μg/L), and 27 (5 μg/L) times higher. These results show that an increase in MTs in D. polymorpha already occurs at relatively low aqueous Pd concentrations indicating that there is the need for detoxification of Pd in the mussel. Furthermore, correlations between Ag-MT and Pd accumulation indicate that higher exposure concentrations are associated with adverse effects on the mussels. Thus, harmful effects of chronic Pd exposure of organisms even in lowest concentrations cannot be excluded in the environment

  9. Self-assembly of palladium nanoparticles on functional TiO{sub 2} nanotubes for a nonenzymatic glucose sensor

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xianlan [School of Science, Honghe University, Mengzi, Yunnan 661100 (China); College of Chemistry, Qishan Campus, Fuzhou University, Fuzhou, Fujian 350108 (China); Fujian Key Lab of Medical Instrument & Pharmaceutical Technology, Yishan Campus, Fuzhou University, Fuzhou, Fujian 350002 (China); Li, Gang; Zhang, Guowei [School of Science, Honghe University, Mengzi, Yunnan 661100 (China); Hou, Keyu [College of Chemistry, Qishan Campus, Fuzhou University, Fuzhou, Fujian 350108 (China); Fujian Key Lab of Medical Instrument & Pharmaceutical Technology, Yishan Campus, Fuzhou University, Fuzhou, Fujian 350002 (China); Pan, Haibo, E-mail: hbpan@fzu.edu.cn [College of Chemistry, Qishan Campus, Fuzhou University, Fuzhou, Fujian 350108 (China); Fujian Key Lab of Medical Instrument & Pharmaceutical Technology, Yishan Campus, Fuzhou University, Fuzhou, Fujian 350002 (China); Du, Min [Fujian Key Lab of Medical Instrument & Pharmaceutical Technology, Yishan Campus, Fuzhou University, Fuzhou, Fujian 350002 (China)

    2016-05-01

    Polydiallyldimethylammonium chloride, PDDA, was used as a stabilizer and linker for functionalized TiO{sub 2} nanotubes (TiO{sub 2} NTs). Self-assembled process with palladium nanoparticles (NPs) was successfully synthesized and used for the oxidation of glucose on glassy carbon electrodes. Based on the voltammetric and amperometric results, Pd NPs efficiently catalyzed the oxidation of glucose at − 0.05 V in the presence of 0.1 M NaCl and showed excellent resistance toward interference poisoning from such interfering species as ascorbic acid, uric acid and urea. To further increase sensitivity, the Pd NPs-PDDA-TiO{sub 2} NTs/GCE was electrochemically treated with H{sub 2}SO{sub 4} and NaOH, the glucose oxidation current was magnified 2.5 times than that before pretreatments due to greatly enhancing the electron transport property of the sensor based on the increased defect sites and surface oxide species. In view of the physiological level of glucose, the wide linear concentration range of glucose (4 × 10{sup −7}–8 × 10{sup −4} M) with a detection limit of 8 × 10{sup −8} M (S/N = 3) was obviously good enough for clinical application. - Highlights: • PDDA was used as a stabilizer and linker for functionalized TiO{sub 2} nanotubes. • Self-assembled process with palladium nanoparticles was synthesized. • After treated both H{sub 2}SO{sub 4} and NaOH, the glucose response was magnified to 2.5 times. • The wide linear concentration range of glucose was obtained with a limit of 8 × 10{sup −8} M.

  10. Development and validation of a multi-residue method for the detection of a wide range of hormonal anabolic compounds in hair using gas chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rambaud, Lauriane [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Monteau, Fabrice [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Deceuninck, Yoann [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Bichon, Emmanuelle [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Andre, Francois [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Le Bizec, Bruno [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France)]. E-mail: lebizec@vet-nantes.fr

    2007-03-14

    The monitoring of anabolic steroid residues in hair is undoubtedly one of the most efficient strategies to demonstrate the long-term administration of these molecules in meat production animals. A multi-residue sample preparation procedure was developed and validated for 28 steroids. A 100 mg hair sample was grinded into powder and extracted at 50 deg. C with methanol. After acidic hydrolysis and extraction with ethyl acetate, phenolsteroids, such as estrogens, resorcyclic acid lactones and stilbens in one hand, are separated from androgens and progestagens in the other hand. Solid phase extractions were performed before applying a specific derivatisation for each compound sub-group. Detection and identification were achieved using gas chromatography-tandem mass spectrometry with acquisition in the selected reaction monitoring mode after electron ionisation. The method was validated according to the 2002/657/EC guideline. Decision limits (CC{alpha}) for main steroids were in the 0.1-10 {mu}g kg{sup -1} range.

  11. Evidence for hydrogen-assisted recovery of cold-worked palladium: hydrogen solubility and mechanical properties studies

    Directory of Open Access Journals (Sweden)

    Maria Ferrer

    2017-07-01

    Full Text Available The influence of hydrogen as an agent to accelerate the thermal recovery of cold-worked palladium has been investigated. The techniques used to characterize the effects of hydrogen on the thermal recovery of palladium were hydrogen solubility and mechanical property measurements. Results show that the presence of modest amounts of hydrogen during annealing of cold-worked palladium does enhance the degree of thermal recovery, with a direct correlation between the amount of hydrogen during annealing and the degree of recovery. The results indicate that the damage resulting from cold-working palladium can be more effectively and efficiently reversed by suitable heat treatments in the presence of appropriate amounts of hydrogen, as compared to heat treatment in vacuum. The somewhat novel technique of using changes in the hydrogen solubility of palladium as an indicator of thermal recovery has been validated and complements the more traditional technique of mechanical property measurements.

  12. In situ synthesis of carbon nanotubes decorated with palladium nanoparticles using arc-discharge in solution method

    International Nuclear Information System (INIS)

    Bera, Debasis; Kuiry, Suresh C.; McCutchen, Matthew; Seal, Sudipta; Heinrich, Helge; Slane, Grady C.

    2004-01-01

    A unique, simple, inexpensive, and one-step synthesis route to produce carbon nanotubes (CNTs) decorated with palladium nanoparticles using a simplified dc arc-discharge in solution is reported. Zero-loss energy filtered transmission electron microscopy and scanning transmission electron microscopy confirm the presence of 3 nm palladium nanoparticles. Such palladium nanoparticles form during the reduction of palladium tetra-chloro-square-planar complex. The deconvoluted x-ray photoelectron spectroscopy envelope shows the presence of palladium on the decorated CNTs. The energy dispersive spectroscopy suggests no functionalization of atomic chlorine to the sidewall of the CNTs. The presence of dislodged graphene sheets with wavy morphology supports the formation of CNTs through the 'scroll mechanism'

  13. Evaluation of residue-residue contact prediction in CASP10

    KAUST Repository

    Monastyrskyy, Bohdan

    2013-08-31

    We present the results of the assessment of the intramolecular residue-residue contact predictions from 26 prediction groups participating in the 10th round of the CASP experiment. The most recently developed direct coupling analysis methods did not take part in the experiment likely because they require a very deep sequence alignment not available for any of the 114 CASP10 targets. The performance of contact prediction methods was evaluated with the measures used in previous CASPs (i.e., prediction accuracy and the difference between the distribution of the predicted contacts and that of all pairs of residues in the target protein), as well as new measures, such as the Matthews correlation coefficient, the area under the precision-recall curve and the ranks of the first correctly and incorrectly predicted contact. We also evaluated the ability to detect interdomain contacts and tested whether the difficulty of predicting contacts depends upon the protein length and the depth of the family sequence alignment. The analyses were carried out on the target domains for which structural homologs did not exist or were difficult to identify. The evaluation was performed for all types of contacts (short, medium, and long-range), with emphasis placed on long-range contacts, i.e. those involving residues separated by at least 24 residues along the sequence. The assessment suggests that the best CASP10 contact prediction methods perform at approximately the same level, and comparably to those participating in CASP9.

  14. Dislocation/hydrogen interaction mechanisms in hydrided nanocrystalline palladium films

    International Nuclear Information System (INIS)

    Amin-Ahmadi, Behnam; Connétable, Damien; Fivel, Marc; Tanguy, Döme; Delmelle, Renaud; Turner, Stuart; Malet, Loic; Godet, Stephane; Pardoen, Thomas; Proost, Joris; Schryvers, Dominique

    2016-01-01

    The nanoscale plasticity mechanisms activated during hydriding cycles in sputtered nanocrystalline Pd films have been investigated ex-situ using advanced transmission electron microscopy techniques. The internal stress developing within the films during hydriding has been monitored in-situ. Results showed that in Pd films hydrided to β-phase, local plasticity was mainly controlled by dislocation activity in spite of the small grain size. Changes of the grain size distribution and the crystallographic texture have not been observed. In contrast, significant microstructural changes were not observed in Pd films hydrided to α-phase. Moreover, the effect of hydrogen loading on the nature and density of dislocations has been investigated using aberration-corrected TEM. Surprisingly, a high density of shear type stacking faults has been observed after dehydriding, indicating a significant effect of hydrogen on the nucleation energy barriers of Shockley partial dislocations. Ab-initio calculations of the effect of hydrogen on the intrinsic stable and unstable stacking fault energies of palladium confirm the experimental observations.

  15. Palladium-catalysed electrophilic aromatic C-H fluorination

    Science.gov (United States)

    Yamamoto, Kumiko; Li, Jiakun; Garber, Jeffrey A. O.; Rolfes, Julian D.; Boursalian, Gregory B.; Borghs, Jannik C.; Genicot, Christophe; Jacq, Jérôme; van Gastel, Maurice; Neese, Frank; Ritter, Tobias

    2018-02-01

    Aryl fluorides are widely used in the pharmaceutical and agrochemical industries, and recent advances have enabled their synthesis through the conversion of various functional groups. However, there is a lack of general methods for direct aromatic carbon-hydrogen (C-H) fluorination. Conventional methods require the use of either strong fluorinating reagents, which are often unselective and difficult to handle, such as elemental fluorine, or less reactive reagents that attack only the most activated arenes, which reduces the substrate scope. A method for the direct fluorination of aromatic C-H bonds could facilitate access to fluorinated derivatives of functional molecules that would otherwise be difficult to produce. For example, drug candidates with improved properties, such as increased metabolic stability or better blood-brain-barrier penetration, may become available. Here we describe an approach to catalysis and the resulting development of an undirected, palladium-catalysed method for aromatic C-H fluorination using mild electrophilic fluorinating reagents. The reaction involves a mode of catalysis that is unusual in aromatic C-H functionalization because no organometallic intermediate is formed; instead, a reactive transition-metal-fluoride electrophile is generated catalytically for the fluorination of arenes that do not otherwise react with mild fluorinating reagents. The scope and functional-group tolerance of this reaction could provide access to functional fluorinated molecules in pharmaceutical and agrochemical development that would otherwise not be readily accessible.

  16. Synthesis, crystal structure and applications of palladium thiosalicylate complexes

    Directory of Open Access Journals (Sweden)

    S.B. Moosun

    2017-05-01

    Full Text Available Three palladium thiosalicylate complexes [Pd(tb(bipy]·3H2O (1, [Pd2(tb2(bipy2]·(dtdb2 (2 and [Pd2(tb2(phen2]·dtdb·H2O (3 (bipy = bipyridine; phen = phenanthroline were prepared from the reaction of PdCl2(CH3CN2 with dithiosalicylic acid (dtdb which underwent cleavage to form thiobenzoate anion (tb in DMF/MeOH. Square planar geometries of the complexes with a N2SO coordination type were proposed on the basis of single crystal X-ray structural study. The presence of trapped and uncoordinated dtdb was observed in complexes 2 and 3. Complexes 1–3 were evaluated as catalysts for Heck coupling reactions of methyl acrylate with iodobenzene, and showed moderate activities at a very low catalyst loading. Complex 1 was found to inhibit the growth of bacteria and scavenge free radicals efficiently.

  17. Biotemplated Palladium Catalysts Can Be Stabilized on Different Support Materials

    KAUST Repository

    Yates, Matthew D.; Logan, Bruce E.

    2014-01-01

    © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Sustainably biotemplated palladium catalysts generated on different carbon-based support materials are examined for durability under electrochemical (oxidative) and mechanical-stress conditions. Biotemplated catalysts on carbon paper under both stresses retain 95% (at 0.6V) of the initial catalytic activity as opposed to 70% for carbon cloth and 60% for graphite. Graphite electrodes retain 95% of initial catalytic activity under a single stress. Using electrodeposited polyaniline (PANI) and polydimethylsiloxane binder increases the current density after the stress tests by 22%, as opposed to a 30% decrease for Nafion. PANI-coated electrodes retain more activity than carbon-paper electrodes under elevated mechanical (94 versus 70%) or increased oxidative (175 versus 62%) stress. Biotemplated catalytic electrodes may be useful alternatives to synthetically produce catalysts for some electrochemical applications. Sustainable electrode fabrication: The biotemplated synthesis of catalytic porous electrodes is a sustainable process and, according to the results of durability tests under electrochemical and mechanical stress, these electrodes (e.g. the Pd/carbon paper electrode shown in the picture) are durable enough to replace catalytic electrodes based on synthetic materials in certain applications.

  18. Biotemplated Palladium Catalysts Can Be Stabilized on Different Support Materials

    KAUST Repository

    Yates, Matthew D.

    2014-07-30

    © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Sustainably biotemplated palladium catalysts generated on different carbon-based support materials are examined for durability under electrochemical (oxidative) and mechanical-stress conditions. Biotemplated catalysts on carbon paper under both stresses retain 95% (at 0.6V) of the initial catalytic activity as opposed to 70% for carbon cloth and 60% for graphite. Graphite electrodes retain 95% of initial catalytic activity under a single stress. Using electrodeposited polyaniline (PANI) and polydimethylsiloxane binder increases the current density after the stress tests by 22%, as opposed to a 30% decrease for Nafion. PANI-coated electrodes retain more activity than carbon-paper electrodes under elevated mechanical (94 versus 70%) or increased oxidative (175 versus 62%) stress. Biotemplated catalytic electrodes may be useful alternatives to synthetically produce catalysts for some electrochemical applications. Sustainable electrode fabrication: The biotemplated synthesis of catalytic porous electrodes is a sustainable process and, according to the results of durability tests under electrochemical and mechanical stress, these electrodes (e.g. the Pd/carbon paper electrode shown in the picture) are durable enough to replace catalytic electrodes based on synthetic materials in certain applications.

  19. Catalytic hydrolysis of ammonia borane via cobalt palladium nanoparticles.

    Science.gov (United States)

    Sun, Daohua; Mazumder, Vismadeb; Metin, Önder; Sun, Shouheng

    2011-08-23

    Monodisperse 8 nm CoPd nanoparticles (NPs) with controlled compositions were synthesized by the reduction of cobalt acetylacetonate and palladium bromide in the presence of oleylamine and trioctylphosphine. These NPs were active catalysts for hydrogen generation from the hydrolysis of ammonia borane (AB), and their activities were composition dependent. Among the 8 nm CoPd catalysts tested for the hydrolysis of AB, the Co(35)Pd(65) NPs exhibited the highest catalytic activity and durability. Their hydrolysis completion time and activation energy were 5.5 min and 27.5 kJ mol(-1), respectively, which were comparable to the best Pt-based catalyst reported. The catalytic performance of the CoPd/C could be further enhanced by a preannealing treatment at 300 °C under air for 15 h with the hydrolysis completion time reduced to 3.5 min. This high catalytic performance of Co(35)Pd(65) NP catalyst makes it an exciting alternative in pursuit of practical implementation of AB as a hydrogen storage material for fuel cell applications. © 2011 American Chemical Society

  20. Palladium-catalysed anti-Markovnikov selective oxidative amination

    Science.gov (United States)

    Kohler, Daniel G.; Gockel, Samuel N.; Kennemur, Jennifer L.; Waller, Peter J.; Hull, Kami L.

    2018-03-01

    In recent years, the synthesis of amines and other nitrogen-containing motifs has been a major area of research in organic chemistry because they are widely represented in biologically active molecules. Current strategies rely on a multistep approach and require one reactant to be activated prior to the carbon-nitrogen bond formation. This leads to a reaction inefficiency and functional group intolerance. As such, a general approach to the synthesis of nitrogen-containing compounds from readily available and benign starting materials is highly desirable. Here we present a palladium-catalysed oxidative amination reaction in which the addition of the nitrogen occurs at the less-substituted carbon of a double bond, in what is known as anti-Markovnikov selectivity. Alkenes are shown to react with imides in the presence of a palladate catalyst to generate the terminal imide through trans-aminopalladation. Subsequently, olefin isomerization occurs to afford the thermodynamically favoured products. Both the scope of the transformation and mechanistic investigations are reported.

  1. Investigation of high temperature reactions on solid substrates with Rutherford backscattering spectrometry: interaction of palladium with selenium on heated graphite surfaces

    International Nuclear Information System (INIS)

    Majidi, V.; Robertson, J.D.

    1991-01-01

    Selenium and palladium interactions on heated pyrolytically coated graphite substrates were investigated using Rutherford backscattering spectrometry. The studies were performed using selenium alone, palladium alone, and a combination of selenium and palladium deposited on the graphite substrates. The results indicate that palladium instantaneously stabilizes selenium at ambient temperatures and prevents the diffusion of selenium into the graphite. As the substrate is heated, temperature dependent diffusion of all analytes into the graphite is observed. Furthermore, it appears that the stabilization of selenium is due to the formation of a stoichiometric compound with palladium and oxygen. This compound decomposes at a temperature between 1070 and 1770 K. (author)

  2. Investigation of high temperature reactions on solid substrates with Rutherford backscattering spectrometry: interaction of palladium with selenium on heated graphite surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Majidi, V.; Robertson, J.D. (Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry)

    1991-01-01

    Selenium and palladium interactions on heated pyrolytically coated graphite substrates were investigated using Rutherford backscattering spectrometry. The studies were performed using selenium alone, palladium alone, and a combination of selenium and palladium deposited on the graphite substrates. The results indicate that palladium instantaneously stabilizes selenium at ambient temperatures and prevents the diffusion of selenium into the graphite. As the substrate is heated, temperature dependent diffusion of all analytes into the graphite is observed. Furthermore, it appears that the stabilization of selenium is due to the formation of a stoichiometric compound with palladium and oxygen. This compound decomposes at a temperature between 1070 and 1770 K. (author).

  3. Application of a novel measure of EEG non-stationarity as 'Shannon- entropy of the peak frequency shifting' for detecting residual abnormalities in concussed individuals.

    Science.gov (United States)

    Cao, Cheng; Slobounov, Semyon

    2011-07-01

    The aim of this report was to propose a novel measure of non-stationarity of EEG signals, named Shannon- entropy of the peak frequency shifting (SEPFS). The feasibility of this method was documented comparing this measure with traditional time domain assessment of non-stationarity and its application to EEG data sets obtained from student-athletes before and after suffering a single episode of mild traumatic brain injury (mTBI) with age-matched normal controls. Instead of assessing the power density distribution on the time-frequency plane, like previously proposed measures of signal non-stationarity, this new measure is based on the shift of the dominant frequency of the EEG signal over time. We applied SEPFS measure to assess the properties of EEG non-stationarity in subjects before and shortly after they suffered mTBI. Student-athletes at high risk for mTBI (n=265) were tested prior to concussive episodes as a baseline. From this subject pool, 30 athletes who suffered from mTBI were retested on day 30 post-injury. Additional subjects pool (student-athletes without history of concussion, n=30) were recruited and test-re-tested within the same 30 day interval. Thirty-two channels EEG signals were acquired in sitting eyes closed condition. The results showed that the SEPFS values significantly decreased in subjects suffering from mTBI. Specifically, reduced EEG non-stationarity was observed in occipital, temporal and central brain areas, indicating the possibility of residual brain dysfunctions in concussed individuals. A similar but less statistically significant trend was observed using traditional time domain analysis of EEG non-stationarity. The proposed measure has at least two merits of interest: (1) it is less affected by the limited resolution of time-frequency representation of the EEG signal; (2) it takes into account the neural characteristics of the EEG signal that have not been considered in previously proposed measures of non-stationarity. This new

  4. Determination of glyphosate residuals and of their metabolite Aminomethyl-Phosphonic acid in waters, by means of liquid chromatography of high efficiency with post-column derivation and fluorescence detection

    International Nuclear Information System (INIS)

    Rodriguez, Hugo A; Guerrero, Jairo; Castro, Rene

    2002-01-01

    The glyphosate is a no selective herbicide largely used in the world in order to control annual and perennial weeds. Its principal metabolite in soils and waters is the Aminomethyl-Phosphonic Acid (AMPA) formed by micro organism's action. This herbicide is used in Colombia in high doses to illegal crops eradication of coca and Amapola and like natural accelerator in sugar cane, constituting an environmental and social problem for the country, being necessary the evaluation of glyphosate residues in different matrices. This study describes the validation of the analytical methodology for the simultaneous determination of glyphosate and its metabolite AMPA in waters of some Colombian regions. The experimental procedure pointed out two main steps: the first one was a cleaning, extraction and concentration step by solid phase extraction; the second step is the separation, identification and quantification of the compounds by High Performance Liquid Chromatography (HPLC) with post-column derivation and fluorescence detection. The results of the validation show that the methodology is specific, selective, precise and robust with linear calibration curve in the linear range between 10 and 750 μg/L, with limits of detection of 0.8 μg/L and limits of quantification of 2 μg/L for the two analyses. The recoveries are in the order of 73% for glyphosate and 70% for AMPA. More over analysis results are presented for water samples of some country regions where glyphosate is applied in different doses with different purposes, finding residues of the herbicide and its metabolite in concentrations above the allowed values in drinking waters for pesticides of toxicology category IV, like the glyphosate, according with the Colombian legislation

  5. Nanostructured palladium tailored via carbonyl chemical route towards oxygen reduction reaction

    International Nuclear Information System (INIS)

    Luo, Y.; Mora-Hernández, J.M.; Estudillo-Wong, L.A.; Arce-Estrada, E.M.; Alonso-Vante, N.

    2015-01-01

    Graphical Abstract: Mass-depending morphologies of nanostructured Palladium obtained via the carbonyl chemical route. Display Omitted -- Highlights: •Mass-depending morphology was observed in nanostructured palladium supported on carbon prepared by the carbonyl chemical route. •The Morphological effect of carbon supported Pd was investigated towards ORR. -- Abstract: Carbon supported palladium nanostructures were synthesized via the carbonyl chemical route. Compared with nanostructured platinum, prepared via carbonyl chemical route, Pd nanomaterials showed mass-loading morphology, whereas particle size and morphology of Pt nanostructures was constant. The oxygen reduction reaction (ORR) on nanostructured Pd, with different morphology in both acid and alkaline medium was investigated. A relationship, based on X-ray diffraction structural analysis pattern, transmission electron microscope, with the Pd morphological effect on ORR activity was identified

  6. γ-Diimine palladium(II based complexes mediated polymerization of methyl methacrylate

    Directory of Open Access Journals (Sweden)

    Mahmoud Sunjuk

    2017-02-01

    Full Text Available The synthesis of new palladium(II complexes of the type [Pd(A–NC–ph–CN–ACl2] (4a–e (A = cyclohexyl (a, 2-isoprpropyl (b, pyrenyl (c, naphthyl (d, and 2,6-diisopropyl (e is described. The isolated γ-diimine ligands and their corresponding palladium(II complexes were characterized by their physical properties, elemental analysis, 1H NMR-, 13C NMR, and infrared spectroscopy. The palladium(II complexes (4a–e were employed successfully as catalysts for atom transfer radical polymerization (ATRP of methyl methacrylate (MMA in the presence of ethyl-2-bromoisobutyrate (EBIB as initiator at 90 °C. Polymerization with these catalyst systems afforded polymers with low molecular weight distribution (Mw/Mn and syndio-rich atactic poly (MMA with relatively higher [rr] diads.

  7. Study on a multi-component palladium alloy membrane for the fusion fuel cycle

    International Nuclear Information System (INIS)

    Yoshida, Hiroshi; Okuno, Kenji; Nagasaki, Takanori; Noda, Kenji; Ishii, Yoshinobu; Takeshita, Hidefumi.

    1985-11-01

    A feasibility study on the material integrity with respect to the hydride formation and helium damage of the palladium alloy membrane was performed for an application of the palladium diffuser to a fusion fuel cleanup process. This study was conducted under the Japan/US Fusion Cooperation Program. Experimental works on the crystallography, hydrogen solubility and 3 He release characteristics were carried out with a multi-component palladium alloy(Pd-25Ag.Au.Ru). The excellent hydrogen permeability and mechanical properties of the membrane made of this alloy had been confirmed by authors' previous study. Based on the present study, this alloy membrane has high resistivity to the hydrogen embrittlement, and swelling and fracture due to the helium bubble formation under the practical operating conditions of the diffuser. (author)

  8. A dataset for preparing pristine graphene-palladium nanocomposites using swollen liquid crystal templates

    Science.gov (United States)

    Vats, Tripti; Siril, Prem Felix

    2017-12-01

    Pristine graphene (G) has not received much attention as a catalyst support, presumably due to its relative inertness as compared to reduced graphene oxide (RGO). In the present work, we used swollen liquid crystals (SLCs) as nano-reactors for graphene-palladium nanocomposites synthesis. The 'soft' confinement of SLCs directs the growth of palladium (Pd) nanoparticles over the G sheets. In this dataset we include all the parameters and details of different techniques used for the characterization of G, SLCs and synthesized G-Pd nanocomposites. The synthesized G-palladium nanocomposites (Pd-G) exhibited improved catalytic activity compared with Pd-RGO and Pd nanoparticles, in the hydrogenation of nitrophenols and C-C coupling reactions.

  9. Preparation of Palladium/Silver-Coated Polyimide Nanotubes: Flexible, Electrically Conductive Fibers.

    Science.gov (United States)

    Kong, Lushi; Rui, Guanchun; Wang, Guangyu; Huang, Rundong; Li, Ran; Yu, Jiajie; Qi, Shengli; Wu, Dezhen

    2017-11-02

    A simple and practical method for coating palladium/silver nanoparticles on polyimide (PI) nanotubes is developed. The key steps involved in the process are silver ion exchange/reduction and displacement reactions between silver and palladium ions. With the addition of silver, the conductivity of the PI nanotubes is greatly enhanced. Further, the polyimide nanotubes with a dense, homogeneous coating of palladium nanoparticles remain flexible after heat treatment and show the possibility for use as highly efficient catalysts. The approach developed here is applicable for coating various noble metals on a wide range of polymer matrices, and can be used for obtaining polyimide nanotubes with metal loaded on both the inner and outer surface.

  10. Preparation of Palladium/Silver-Coated Polyimide Nanotubes: Flexible, Electrically Conductive Fibers

    Directory of Open Access Journals (Sweden)

    Lushi Kong

    2017-11-01

    Full Text Available A simple and practical method for coating palladium/silver nanoparticles on polyimide (PI nanotubes is developed. The key steps involved in the process are silver ion exchange/reduction and displacement reactions between silver and palladium ions. With the addition of silver, the conductivity of the PI nanotubes is greatly enhanced. Further, the polyimide nanotubes with a dense, homogeneous coating of palladium nanoparticles remain flexible after heat treatment and show the possibility for use as highly efficient catalysts. The approach developed here is applicable for coating various noble metals on a wide range of polymer matrices, and can be used for obtaining polyimide nanotubes with metal loaded on both the inner and outer surface.

  11. Low Temperature Steam Methane Reforming Over Ni Based Catalytic Membrane Prepared by Electroless Palladium Plating.

    Science.gov (United States)

    Lee, Sang Moon; Hong, Sung Chang; Kim, Sung Su

    2018-09-01

    A Pd/Ni-YSZ porous membrane with different palladium loadings and hydrazine as a reducing reagent was prepared by electroless plating and evaluated for the steam methane reforming activity. The steam-reforming activity of a Ni-YSZ porous membrane was greatly increased by the deposition of 4 g/L palladium in the low-temperature range (600 °C). With an increasing amount of reducing reagent, the Pd clusters were well dispersed on the Ni-YSZ surface and were uniform in size (∼500 nm). The Pd/Ni-YSZ catalytic porous membrane prepared by 1 of Pd/hydrazine ratio possessed an abundant amount of metallic Pd. The optimal palladium loadings and Pd/hydrazine ratio increased the catalytic activity in both the steam-reforming reaction and the Pd dispersion.

  12. A Confirmatory Method Based on HPLC-MS/MS for the Detection and Quantification of Residue of Tetracyclines in Nonmedicated Feed

    Directory of Open Access Journals (Sweden)

    Rosa E. Gavilán

    2016-01-01

    Full Text Available The Commission Regulation 574/2011/EC set up maximum levels of coccidiostats and histomonostats in nonmedicated feed as a consequence of carry-over during manufacturing. Carry-over takes place from medicated to nonmedicated feed during feed production. Similar contamination could also occur for other pharmaceuticals such as tetracyclines, a group of antibiotics commonly employed in food production animal. The objective of this work is to present a simple and fast method for the simultaneous detection of four tetracyclines (chlortetracycline, doxycycline, oxytetracycline, and tetracycline in nontarget feed at a μg/kg level. Validation of the method was performed according to the guideline included in the Commission Decision 2002/657/EC for official method. The validated method was successfully applied to 50 feed samples collected from different milk farms and 25 samples obtained from feed manufacturers. While oxytetracycline was the tetracycline most frequently detected, chlortetracycline was the analyte measured at the highest concentration 15.14 mg/Kg. From 75 nonmedicated feed analysed 15% resulted to be positive for the presence of one tetracycline.

  13. On-site monitoring of Hebei Spirit oil spill by fluorometric detection of oil residues in coastal waters off Taean, Korea

    Energy Technology Data Exchange (ETDEWEB)

    Kim, M.; Yim, U.H.; Hong, S.H.; Jung, J.H.; Won, J.; An, J.; Choi, H.W.; Shim, W.J. [Korea Ocean Research and Development Inst., Geoje (Korea, Republic of)

    2009-07-01

    This paper discussed activities conducted to monitor a crude oil spill that contaminated over 70 km of the western Korean coastline. Contamination levels and temporal variations of dissolved and dispersed oils in sea and pore water at 40 beaches were monitored using a portable fluorimeter for 10 months after the spill. More than 980 samples from the heavily-impacted Mallipo Beach area were analyzed. The analysis showed that oil concentrations in the sea water were as high as 16,600 {mu}g/L directly after the spill, and decreased to below the Korean marine water quality standard of 10 {mu}g/L at most sites 10 months after the spill. However, the oil content in pore water remained high, with levels of up to 2,320 {mu}g/L for the first few months following the spill. Higher oil contamination levels were observed at some sites for up to 10 months after the spill. Results of the study suggested that oil in pore water persisted in confined areas along the coastline. Results from the fluorescence detection technique were then compared with traditional gas chromatography (GC) techniques of total petroleum hydrocarbon analysis. It was concluded that fluorescence detection was capable of generating accurate results more quickly and cost-effectively than traditional GC techniques. 22 refs., 7 figs.

  14. Antiplasmodial activity of eco-friendly synthesized palladium nanoparticles using Eclipta prostrata extract against Plasmodium berghei in Swiss albino mice.

    Science.gov (United States)

    Rajakumar, Govindasamy; Rahuman, Abdul Abdul; Chung, Ill-Min; Kirthi, Arivarasan Vishnu; Marimuthu, Sampath; Anbarasan, Karunanithi

    2015-04-01

    Malaria is an infectious disease caused by the Plasmodium parasite that continues to be a health issue for humans. It is one of the most common pathogenic factors of morbidity and mortality. Palladium nanoparticles (Pd NPs) have been used as target antimicrobial compounds, as a catalyst to manufacture pharmaceuticals, degrade harmful environmental pollutants, and as sensors for the detection of various analyses. The aim of this study was to investigate the antiplasmodial activity of synthesized Pd NPs by using leaf aqueous extract of Eclipta prostrata against Plasmodium berghei in Swiss albino mice. The synthesized Pd NPs were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR), Scanning electron microscopy (SEM) with Energy dispersive X-ray spectroscopy (EDX), and High-resolution transmission electron microscope (HRTEM) with the Selected area (electron) diffraction (SAED). The XRD peaks appeared at 35.61°, 44.27°, 56.40°, and 74.51°, which correspond to (111), (200), (220), and (311) planes for palladium, respectively. The FTIR spectra that were carried out to identify the potential biomolecule of synthesized Pd NPs showed the peaks at 3361, 1540, 1399, 1257, 1049, and 659 in the region of 4000-500 cm(-1). The SEM images showed aggregation of NPs with an average size of 63 ± 1.4. The HRTEM images of the precipitated solid phase obtained after termination of the reaction of E. prostrata aqueous leaf extract were in the range from 18 to 64 nm with an average size of 27 ± 1.3 nm. The in vivo antiplasmodial assay was carried out as per Peters' 4-day suppressive test, and the synthesized Pd NP-treated mice group showed reduction of parasitemia by 78.13% with an inhibitory concentration (IC)50 value of 16.44 mg/kg/body weight. The growth inhibition of E. prostrata aqueous leaf extract, palladium acetate, and synthesized Pd NPs showed the IC20, IC50, and IC90 values of 1.90, 10.29, and 64.11; 4.49, 9.84, and 23.04; and 4.34, 8

  15. Recovery of nonradioactive palladium and rhodium from high-level radioactive wastes

    International Nuclear Information System (INIS)

    McDuffie, H.F.

    1979-01-01

    A possible method for recovering significant quantities of nonradioactive palladium from fission-product wastes requires essentially complete separation of the fission-product (radioactive) palladium from fission-product ruthenium. After the decay of 106 Ru via 106 Rh to 106 Pd, this nonradioactive palladium is recovered for normal commercial use. The U.S. production of palladium has never been above 1000 kg per year vs consumption of about 46,000 kg per year. Most of the supply comes from Russia and South Africa. It has been estimated that a 400-GW(e) nuclear reactor economy will make available 2000 kg per year of 106 Ru at reactor fuel discharge. A substantial increase might be achieved if plutonium were recycled as fissionable material because of the higher yields of the 106 chain from plutonium. A literature search has uncovered support for three promising approaches to the required separation of palladium from ruthenium: (1) recrystallization from solution in bismuth or in zinc; (2) selective precipitation of a titanium--ruthenium intermetallic compound from bismuth, followed by precipitation of a zinc--palladium intermetallic compound; and (3) dissolution in molten magnesium followed by partitioning between molten magnesium and a molten uranium-5 wt % chromium eutectic at a temperature above 870 0 C. Liquid-liquid extraction appears to be the most promising method from a technological point of view, although intermetallic compound formation is much more interesting chemically. Recovery of some nonradioactive 103 Rh may be possible by liquid-liquid extraction of the fuel before the decay of the 39.8-d 103 Ru has gone substantially to completion. Demonstration of the practicality of these separations will contribute a positive factor to the evaluation of resumption in the United States of nuclear fuel reprocessing and plutonium recycle in light-water-moderated reactors

  16. Influence of residual stress on diffusion-induced bending in bilayered microcantilever sensors

    International Nuclear Information System (INIS)

    Xuan Fuzhen; Shao Shanshan; Wang Zhengdong; Tu Shantung

    2010-01-01

    The influence of residual stress on diffusion-induced bending in bilayered microcantilever sensors has been analyzed under the framework of thermodynamic theory and Fick's second law. A self-consistent diffusion equation involving the coupling effects of residual stress and diffusion-induced stress is developed. Effects of thickness ratio, modulus ratio, diffusivity ratio and residual stress gradient of film and substrate on the curvature of bilayered cantilever are then discussed with the help of finite difference method. Results reveal that the curvature of bilayered cantilever increases with decreasing the diffusivity ratio and modulus ratio of substrate to film at a given time. Case study of the polysilicon/palladium hydrogen sensor has been finally carried out using the above developed bending theory.

  17. Validation of the System One RemStar Auto A-Flex for Obstructive Sleep Apnea Treatment and Detection of Residual Apnea-Hypopnea Index

    DEFF Research Database (Denmark)

    Gagnadoux, Frédéric; Pevernagie, Dirk; Jennum, Poul

    2017-01-01

    the performance of the System One RemStar Auto A-Flex (Philips Respironics, Murrysville, PA, USA) automatically adjusted positive airway pressure (APAP) mode to manually titrated, fixed pressure CPAP and to validate the device's breathing event detection capabilities against attended in-laboratory PSG. METHODS......: Sixty-one patients investigated in five centers for moderate to severe obstructive sleep apnea between May 2012 and June 2013 were invited to participate. Participants underwent two full-night attended polysomnograms in random order with manually titrated, fixed pressure CPAP versus APAP. RESULTS: Fifty......-three participants with a mean apnea-hypopnea index (AHI) of 45.9 ± 23 completed two sleep studies and were included in the analysis. There were significant but not clinically relevant differences between APAP and CPAP respectively: Apnea index [1.0 (2.8 ± 0.8), median (mean ± standard deviation)] versus [1.8 (5...

  18. Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

    Science.gov (United States)

    Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

    2018-03-30

    Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Morphology of one-time coated palladium-alumina composite membrane prepared by sol-gel process and electroless plating technique

    Science.gov (United States)

    Sari, R.; Dewi, R.; Pardi; Hakim, L.; Diana, S.

    2018-03-01

    Palladium coated porous alumina ceramic membrane tube was obtained using a combination of sol-gel process and electroless plating technique. The thickness, structure and composition of palladium-alumina composite membrane were analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM). Palladium particle size was 6.18 to 7.64 nm. Palladium membrane with thickness of approximately 301.5 to 815.1 nm was formed at the outer surface of the alumina layer. EDX data confirmed the formation of palladium-alumina membrane containing 45% of palladium. From this research it shows the combination of sol-gel process and electroless plating technique with one-time coating can produce a homogeneous and smoother palladium nano layer film on alumina substrate.

  20. Method for palladium activating molybdenum metallized features on a ceramic substrate

    International Nuclear Information System (INIS)

    Kumar, A.H.; Schwartz, B.

    1985-01-01

    A molybdenum or tungsten metallurgical pattern is formed on or in a dielectric green sheet. Palladium, nickel, platinum or rhodium is coated on a layer of polyvinyl butyral which is carried on a polyester film. The metal layer of this assembly is laminated to a dielectric green sheet which carries the molybdenum or tungsten metallurgy. The polyester film is stripped off. The resulting assembly is sintered to a fired structure, whereby the polyvinyl butyral is volatilized off and the palladium, nickel, platinum or rhodium is alloyed with the molybdenum or tungsten metallurgy to provide a densified metallurgy whose surface is free of glass

  1. Fabrication of Polybenzimidazole/Palladium Nanoparticles Hollow Fiber Membranes for Hydrogen Purification

    KAUST Repository

    Villalobos, Luis Francisco

    2017-09-13

    A novel scheme to fabricate polybenzimidazole (PBI) hollow fiber membranes with a thin skin loaded with fully dispersed palladium nanoparticles is proposed for the first time. Palladium is added to the membrane during the spinning process in the form of ions that coordinate to the imidazole groups of the polymer. This is attractive for membrane production because agglomeration of nanoparticles is minimized and the high-cost metal is incorporated in only the selective layer—where it is required. Pd-containing membranes achieve three orders of magnitude higher H2 permeances and a twofold improvement in H2/CO2 selectivity compared to pure PBI hollow fiber membranes.

  2. Palladium-catalysed arylation of acetoacetate esters to yield 2-arylacetic acid esters

    CSIR Research Space (South Africa)

    Zeevaart, JG

    2004-05-24

    Full Text Available , was developed simultaneously by Hart- wig and Buchwald.5 Typically the tert-butyl ester of propionic acid is treated with an aryl halide (bromide or chloride) in the presence of a strong base, palladium and a bulky phosphine ligand or a bulky imidazolinium CO2t... novel palladium- catalysed conditions for the arylation of acetoacetate esters resulting in the formation of 2-arylacetic acid esters. When we attempted the arylation of tert-butyl aceto- acetate 1a with bromobenzene 2a using mild reaction conditions (K3...

  3. Neutron activation determination of gold and palladium using extraction by organic sulfides

    International Nuclear Information System (INIS)

    Gil'berg, Eh.N.; Torgov, V.G.; Verevkin, G.V.; AN SSSR, Novosibirsk. Inst. Neorganicheskoj Khimii)

    1978-01-01

    Compared are methods of gold determination in standard rock samples of the USA National Geological Service: a) extraction by solutions of dioctylsulfide and oil sulfides from irradiated samples; b) preliminary extraction by the above solfides with the following extract radiation; c) the method of isotope dilution with substoichiometry extraction. A possibility is studied to determine palladium in the sulfide extract with gold using the NaI(Tl) thin crystal scintillators. It is established that joint palladium and gold extraction permits to determine them in many natural products simultaneously

  4. Watermelon rind-mediated green synthesis of noble palladium nanoparticles: catalytic application

    Science.gov (United States)

    Lakshmipathy, R.; Palakshi Reddy, B.; Sarada, N. C.; Chidambaram, K.; Khadeer Pasha, Sk.

    2015-02-01

    The present study reports the feasibility of synthesis of palladium nanoparticles (Pd NPs) by watermelon rind. The aqueous extract prepared from watermelon rind, an agro waste, was evaluated as capping and reducing agent for biosynthesis of palladium nanoparticles. The formation of Pd NPs was visually monitored with change in color from pale yellow to dark brown and later monitored with UV-Vis spectroscopy. The synthesized Pd NPs were further characterized by XRD, FTIR, DLS, AFM and TEM techniques. The synthesized Pd NPs were employed in Suzuki coupling reaction as catalyst. The results reveal that watermelon rind, an agro waste, is capable of synthesizing spherical-shaped Pd NPs with catalytic activity.

  5. Efficiency of Al2O3 supported palladium sorbents in the process of hydrogen isotope exchange

    International Nuclear Information System (INIS)

    Andreev, B.M.; Perevezentsev, A.N.; Yasenkov, V.I.

    1981-01-01

    It is found that in the hydrogen-palladium system while applying the metal to aluminium oxide a considerable increase of the heterogeneous hydrogen isotopic exchange rate is observed due to the increase of its specific surface at 167-298 K temperatures and 350-500 Torr hydrogen pressures. It is shown that in the process of thermal treatment of the supported palladium sorbent resulting in reconstruction of the carrier porous structure, as well as in increasing the metal crystal size, the change of the stage, limiting the isotopic exchange process, occurs. The values of the rate and energy of activation of the hydrogen isotopic exchange are presented [ru

  6. Insights into functional-group-tolerant polymerization catalysis with phosphine-sulfonamide palladium (II) complexes

    KAUST Repository

    Jian, Zhongbao; Falivene, Laura; Wucher, Philipp; Roesle, Philipp; Caporaso, Lucia; Cavallo, Luigi; Gç ttker-Schnetmann, Inigo; Mecking, Stefan

    2014-01-01

    Two series of cationic palladium(II) methyl complexes {[(2-MeOC6H4)2PC6H4SO2NHC6H3(2,6-R1,R2)]PdMe}2[A]2 (X1+-A: R1=R2=H: H1+-A; R1=R2=CH(CH3)2: DIPP1+-A; R1=H, R2=CF3: CF31+-A; A=BF4 or SbF6) and neutral palladium(II) methyl complexes {[(2-MeOC6H4

  7. Progress in excess of power experiments with electrochemical loading of deuterium in palladium

    International Nuclear Information System (INIS)

    Violante, V.; Moretti, S.; Bertolotti, M.

    2006-01-01

    A research activity has been carried out, during the last 3 years, in the field of triggering anomalous heat effects in palladium deuteride. An enhancement of the excess of power reproducibility in deuterated palladium was obtained by using He-Ne Laser irradiation during electrochemical loading. A preliminary correlation between excess of energy and 4 He concentration increasing above the background was found. The continuation of the experimental program confirmed that Laser triggering produce an interesting gain of reproducibility. An upgrade of the experimental set-up has been realized. (author)

  8. [Development of residual voltage testing equipment].

    Science.gov (United States)

    Zeng, Xiaohui; Wu, Mingjun; Cao, Li; He, Jinyi; Deng, Zhensheng

    2014-07-01

    For the existing measurement methods of residual voltage which can't turn the power off at peak voltage exactly and simultaneously display waveforms, a new residual voltage detection method is put forward in this paper. First, the zero point of the power supply is detected with zero cross detection circuit and is inputted to a single-chip microcomputer in the form of pulse signal. Secend, when the zero point delays to the peak voltage, the single-chip microcomputer sends control signal to power off the relay. At last, the waveform of the residual voltage is displayed on a principal computer or oscilloscope. The experimental results show that the device designed in this paper can turn the power off at peak voltage and is able to accurately display the voltage waveform immediately after power off and the standard deviation of the residual voltage is less than 0.2 V at exactly one second and later.

  9. Simplified flow cytometric assay to detect minimal residual disease in childhood with acute lymphoblastic leukemia Detecção de doença residual mínima em crianças com leucemia linfoblástica aguda por citometria de fluxo

    Directory of Open Access Journals (Sweden)

    Elizabete Delbuono

    2008-08-01

    Full Text Available The detection of minimal residual disease (MRD is an important prognostic factor in childhood acute lymphoblastic leukemia (ALL providing crucial information on the response to treatment and risk of relapse. However, the high cost of these techniques restricts their use in countries with limited resources. Thus, we prospectively studied the use of flow cytometry (FC with a simplified 3-color assay and a limited antibody panel to detect MRD in the bone marrow (BM and peripheral blood (PB of children with ALL. BM and PB samples from 40 children with ALL were analyzed on days (d 14 and 28 during induction and in weeks 24-30 of maintenance therapy. Detectable MRD was defined as > 0.01% cells expressing the aberrant immunophenotype as characterized at diagnosis among total events in the sample. A total of 87% of the patients had an aberrant immunophenotype at diagnosis. On d14, 56% of the BM and 43% of the PB samples had detectable MRD. On d28, this decreased to 45% and 31%, respectively. The percentage of cells with the aberrant phenotype was similar in both BM and PB in T-ALL but about 10 times higher in the BM of patients with B-cell-precursor ALL. Moreover, MRD was detected in the BM of patients in complete morphological remission (44% on d14 and 39% on d28. MRD was not significantly associated to gender, age, initial white blood cell count or cell lineage. This FC assay is feasible, affordable and readily applicable to detect MRD in centers with limited resources.A detecção de doença residual mínima (DRM é um importante fator prognóstico na leucemia linfóide aguda (LLA infantil e fornece informações sobre a resposta ao tratamento e o risco de recaída. Entretanto, os altos custos das técnicas utilizadas limitam seu uso nos países em desenvolvimento. Desta forma, realizamos um estudo prospectivo para avaliar a citometria de fluxo (CF, utilizando três fluorescências e um painel limitado de anticorpos monoclonais, como método de detec

  10. Resíduos de anabolizantes na produção animal: importância e métodos de detecção Anabolic residues in livestock prodution: relevancy and detection methods

    Directory of Open Access Journals (Sweden)

    Keila Maria Roncato Duarte

    2002-08-01

    Full Text Available Com o desenvolvimento da indústria farmacêutica e o conseqüente surgimento de novas substâncias promotoras do crescimento animal, o setor agropecuário necessita de tecnologias cada vez mais eficientes e sensíveis para detectar possíveis resíduos deixados por este vasto número de substâncias anabolizantes, principalmente esteróides com atividades estrogênicas, androgênicas e progestogênicas. Tais substâncias, quando presentes na carne, gordura, ovos, entre outros, podem ser detectadas e quantificadas por uma série de métodos, dentre os quais, descrevemos os cromatográficos, baseados principalmente em cromatografia gasosa acoplada à espectrometria de massa (CG-EM, cromatografia líquida de alta eficiência (CLAE, cromatografia em camada delgada de alta eficiência (CCDAE e os métodos imunológicos, como radioomunoensaio (RIA e ensaio imunoenzimático (ELISA. Estes métodos têm como vantagens o elevado número de amostras que podem ser analisadas por período de tempo, aliadas à alta sensibilidade na detecção de resíduos.With the development of the pharmaceutical industry, and consequently appearance of new substances which promote animal growth, the agricultural sector needs technologies more and more efficient and sensitive to detect possible residues left by this vast number of anabolic substances, mainly steroids with estrogenic, androgenic and progesterogenics activities. Such substances, when present in meat, fat, and eggs among others, can be detected and quantified by a series of methods, among the ones which we described the chromatographic methods, based mainly on gaseous chromatography coupled to the mass espectrometry (CG-MS, high performance liquid chromatography (HPLC, thin layer chromatography (HPTLC and the immunological methods, as radioimmunoassay (RIA and enzyme linked immunosorbent assay (ELISA. These methods have as advantages the high number of samples that can be analyzed by period of time, toghether

  11. MIL-101(Cr)@GO for dispersive micro-solid-phase extraction of pharmaceutical residue in chicken breast used in microwave-assisted coupling with HPLC-MS/MS detection.

    Science.gov (United States)

    Wang, Yudan; Dai, Xinpeng; He, Xi; Chen, Lin; Hou, Xiaohong

    2017-10-25

    In this work, MIL-101(Cr)@GO (Graphite Oxide) was synthesized using a hydrothermal synthesis method and was applied as a dispersive micro-solid-phase extraction (D-μ-SPE) sorbent for the efficient concentration of four residual drugs (metronidazole, MNZ; tinidazole, TNZ; chloramphenicol, CAP; sulfamethoxazole, SMX). Meanwhile, the extraction process was optimized by combining it with microwave-assisted extraction. Factors affecting the D-μ-SPE efficiency, such as selection of sorbent materials, pH of the sample solution, salting-out effect, amount of used material, extraction time, desorption solvent and desorption time, were studied. Under the optimal extraction conditions, the linearity ranged from 10 to 1000ngkg -1 and 1-100ngkg -1 (r 2 ≥0.9928) for the target analytes. The limits of detection were between 0.08 and 1.02ngkg -1 , and the limits of quantitation were between 0.26 and 3.40ngkg -1 . Additionally, the developed method also exhibited good precision (RSD≤2.5%), repeatability (RSD≤4.3%), high recoveries (88.9%-102.3%) and low matrix effects (78.2%-95.1%). The proposed method proved to be an efficient and reliable approach for the determination of the analytes. Finally, we successfully detected the four drugs in chicken breast. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Sol-gel synthesized of nanocomposite palladium-alumina ceramic membrane for H{sub 2} permeability: Preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, A.L.; Mustafa, N.N.N. [School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, Seri Ampangan, 14300 Nibong Tebal, Penang (Malaysia)

    2007-08-15

    Palladium-alumina membrane with mesopore and narrow pore size distribution was prepared by the sol-gel method. Effect of the finely dispersed metal on the microstructure and the characteristic properties of the palladium-alumina membrane were investigated. Observations were made on membrane weight loss, morphology, pore structure, pore size, surface area, pore surface fractal and membrane's crystal structure. Autosorb analysis, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared (FTIR) analysis were employed in the membrane characterization. Autosorb analysis found that, BET surface area decreased and pore size of the membrane increased with the increasing of calcinations temperature (500-1100{sup o}C) and with the increasing of palladium amount in the membrane. FTIR and TG/DTA analysis show that the suitable temperature for calcinations of palladium-alumina membrane is at 700{sup o}C. Palladium metals are highly dispersed at calcinations temperature of 700{sup o}C as observed by TEM analysis. The fine crystallinity of the palladium and {gamma}-alumina phase was obtained after calcined at 700{sup o}C. The SEM morphology shows a smooth and free crack layer of palladium-alumina membrane after repeating the process of dipping, drying and calcinations at temperature of 700{sup o}C. The membrane also successfully coated with a good adhesion on support. The thickness of the final membrane layer was estimated as 9{mu} m. (author)

  13. Enhancing the performance of single-chambered microbial fuel cell using manganese/palladium and zirconium/palladium composite cathode catalysts.

    Science.gov (United States)

    Jadhav, Dipak A; Deshpande, Parag A; Ghangrekar, Makarand M

    2017-08-01

    Application of ZrO 2 , MnO 2 , palladium, palladium-substituted-zirconium oxide (Zr 0.98 Pd 0.02 O 2 ) and palladium-substituted-manganese oxide (Mn 0.98 Pd 0.02 O 2 ) cathode catalysts in a single-chambered microbial fuel cell (MFC) was explored. The highest power generation (1.28W/m 3 ) was achieved in MFC with Mn 0.98 Pd 0.02 O 2 catalyst, which was higher than that with MnO 2 (0.58W/m 3 ) alone; whereas, MFC having Zr 0.98 Pd 0.02 O 2 catalyzed cathode and non-catalyzed cathode produced powers of 1.02 and 0.23W/m 3 , respectively. Also, low-cost zirconium-palladium-composite showed better catalytic activity and capacitance over ZrO 2 with 20A/m 3 current production and demonstrated its suitability for MFC applications. Cyclic voltammetry analyses showed higher well-defined redox peaks in composite catalysts (Mn/Zr-Pd-C) over other catalyzed MFCs containing MnO 2 or ZrO 2 . Electrochemical behaviour of composite catalysts on cathode showed higher availability of adsorption sites for oxygen reduction and, hence, enhanced the rate of cathodic reactions. Thus, Mn/Zr-Pd-C-based composite catalysts exhibited superior cathodic performance and could be proposed as alternatives to costly Pd-catalyst for field applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Touch-down reverse transcriptase-PCR detection of IgV(H) rearrangement and Sybr-Green-based real-time RT-PCR quantitation of minimal residual disease in patients with chronic lymphocytic leukemia.

    Science.gov (United States)

    Peková, Sona; Marková, Jana; Pajer, Petr; Dvorák, Michal; Cetkovský, Petr; Schwarz, Jirí

    2005-01-01

    Patients with chronic lymphocytic leukemia (CLL) can relapse even after aggressive therapy and autografts. It is commonly assumed that to prevent relapse the level of minimal residual disease (MRD) should be as low as possible. To evaluate MRD, highly sensitive quantitative assays are needed. The aim of the study was to develop a robust and sensitive method for detection of the clonal immunoglobulin heavy-chain variable (IgV(H)) rearrangement in CLL and to introduce a highly sensitive and specific methodology for MRD monitoring in patients with CLL who undergo intensive treatment. As a prerequisite for MRD detection, touch-down reverse transcriptase (RT)-PCR using degenerate primers were used for the diagnostic identification of (H) gene rearrangement(s). For quantitative MRD detection in 18 patients, we employed a real-time RT-PCR assay (RQ-PCR) making use of patient-specific primers and the cost-saving Sybr-Green reporter dye (SG). For precise calibration of RQ-PCR, patient-specific IgV(H) sequences were cloned. Touch-down RT-PCR with degenerate primers allowed the successful detection of IgV(H) clonal rearrangement(s) in 252 of 257 (98.1%) diagnostic samples. Biallelic rearrangements were found in 27 of 252 (10.7%) cases. Degenerate primers used for the identification of clonal expansion at diagnosis were not sensitive enough for MRD detection. In contrast, our RQ-PCR assay using patient-specific primers and SG reached the sensitivity of 10(-)(6). We demonstrated MRD in each patient tested, including four of four patients in complete remission following autologous hematopoietic stem cell transplantation (HSCT) and three of three following allogeneic 'mini'-HSCT. Increments in MRD might herald relapse; aggressive chemotherapy could induce molecular remission. Our touch-down RT-PCR has higher efficiency to detect clonal IgV(H) rearrangements including the biallelic ones. MRD quantitation of IgV(H) expression using SG-based RQ-PCR represents a highly specific

  15. Synergistic dual activation catalysis by palladium nanoparticles for epoxide ring opening with phenols.

    Science.gov (United States)

    Seth, Kapileswar; Roy, Sudipta Raha; Pipaliya, Bhavin V; Chakraborti, Asit K

    2013-07-04

    Synergistic dual activation catalysis has been devised for epoxide phenolysis wherein palladium nanoparticles induce electrophilic activation via coordination with the epoxide oxygen followed by nucleophilic activation through anion-π interaction with the aromatic ring of the phenol, and water (reaction medium) also renders assistance through 'epoxide-phenol' dual activation.

  16. REMOVAL OF NICKEL(II) AND PALLADIUM(II) FROM SURFACE ...

    African Journals Online (AJOL)

    Preferred Customer

    Nickel is widely used in electroplating, in the manufacture of Ni-Cd batteries, in rods for arc welding, in pigments for ... Palladium has an extensive use in electrical industry as grids for ... It is also used as catalytic converter in motor vehicles.

  17. Thin film platinum–palladium thermocouples for gas turbine engine applications

    Energy Technology Data Exchange (ETDEWEB)

    Tougas, Ian M.; Gregory, Otto J., E-mail: gregory@egr.uri.edu

    2013-07-31

    Thin film platinum:palladium thermocouples were fabricated on alumina and mullite surfaces using radio frequency sputtering and characterized after high temperature exposure to oxidizing environments. The thermoelectric output, hysteresis, and drift of these sensors were measured at temperatures up to 1100 °C. Auger electron spectroscopy was used to follow the extent of oxidation in each thermocouple leg and interdiffusion at the metallurgical junction. Minimal oxidation of the platinum and palladium thermoelements was observed after high temperature exposure, but considerable dewetting and faceting of the films were observed in scanning electron microscopy. An Arrhenius temperature dependence on the drift rate was observed and later attributed to microstructural changes during thermal cycling. The thin film thermocouples, however, did exhibit excellent stability at 1000 °C with drift rates comparable to commercial type-K wire thermocouples. Based on these results, platinum:palladium thin film thermocouples have considerable potential for use in the hot sections of gas turbine engines. - Highlights: • Stable thin film platinum:palladium thermocouples for gas turbine engines • Little oxidation but significant microstructural changes from thermal cycling • Minimal hysteresis during repeated thermal cycling • Drift comparable to commercial wire thermocouples.

  18. Green synthesis of palladium nanoparticles with carboxymethyl cellulose for degradation of azo-dyes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Gang; Li, Yun; Wang, Zhengdong; Liu, Huihong, E-mail: huihongliu@126.com

    2017-02-01

    Palladium nanoparticles (PdNPs) were synthesized through friendly environmental method using PdCl{sub 2} and carboxymethyl cellulose (CMC) in an aqueous solution (pH 6) at controlled water bath (80 °C) for 30 min. CMC functioned as both reducing and stabilizing agent. The characterization through high resolution-transmission electron microscopic (HRTEM) and X-ray Fluorescence Spectrometry (XRF) inferred that the as-synthesized PdNPs were spherical in shape with a face cubic crystal (FCC) structure. The results from dynamic light scattering (DLS) suggested the PdNPs had the narrow size distribution with an average size of 2.5 nm. The negative zeta potential (−52.6 mV) kept the as-synthesized PdNPs stable more than one year. The PdNPs showed the excellent catalytic activity by reducing degradation of azo-dyes, such as p-Aminoazobenzene, acid red 66, acid orange 7, scarlet 3G and reactive yellow 179, in the present of sodium borohydride. - Highlights: • Green synthesis of palladium nanoparticles using carboxymethyl cellulose. • The synthesis of palladium nanoparticles were performed easily. • Carboxymethyl cellulose acts as both reducing and stabilization agents. • The as-synthesized palladium nanoparticles show excellent catalytic activity.

  19. Reversible, high molecular weight palladium and platinum coordination polymers based on phosphorus ligands

    NARCIS (Netherlands)

    Paulusse, J.M.J.; Huijbers, J.P.J.; Sijbesma, R.P.

    2005-01-01

    A general strategy for the preparation and characterization of high molecular weight coordination polymers based on bifunctional phosphorus ligands and palladium or platinum dichloride is described. Metal-to-ligand stoichiometry is of key importance for the formation of linear coordination polymers

  20. Reversible, High Molecular Weight Palladium and Platinum Coordination Polymers Based on Phosphorus Ligands

    NARCIS (Netherlands)

    Paulusse, Jos Marie Johannes; Huijbers, Jeroen P.J.; Sijbesma, Rint P.

    2005-01-01

    A general strategy for the preparation and characterization of high molecular weight coordination polymers based on bifunctional phosphorus ligands and palladium or platinum dichloride is described. Metal-to-ligand stoichiometry is of key importance for the formation of linear coordination polymers

  1. PALLADIUM-FACILITATED ELECTROLYTIC DECHLORINATION OF 2-CHLOROBIPHENYL USING A GRANULAR-GRAPHITE ELECTRODE.

    Science.gov (United States)

    Palladium-assisted electrocatalytic dechlorination of 2-chlorobiphenyl (2-Cl BP) in aqueous solutions was conducted in a membrane-separated electrochemical reactor with granular-graphite packed electrodes. The dechlorination took place at a granular-graphite cathode while Pd was ...

  2. Chalcogen-containing oxazolines in the palladium-catalyzed asymmetric allylic alkylation

    Directory of Open Access Journals (Sweden)

    Braga Antonio L.

    2006-01-01

    Full Text Available A comparative study about the ability of chiral chalcogen-containing oxazolines to act as chiral ligands in the palladium-catalyzed allylic alkylation of rac-1,3-diphenyl-2-propenyl acetate with dimethyl malonate is reported. Differences in the catalytic performance are observed with sulfur, selenium and tellurium analogues.

  3. Halide-Enhanced Catalytic Activity of Palladium Nanoparticles Comes at the Expense of Catalyst Recovery

    Directory of Open Access Journals (Sweden)

    Azzedine Bouleghlimat

    2017-09-01

    Full Text Available In this communication, we present studies of the oxidative homocoupling of arylboronic acids catalyzed by immobilised palladium nanoparticles in aqueous solution. This reaction is of significant interest because it shares a key transmetallation step with the well-known Suzuki-Miyaura cross-coupling reaction. Additives can have significant effects on catalysis, both in terms of reaction mechanism and recovery of catalytic species, and our aim was to study the effect of added halides on catalytic efficiency and catalyst recovery. Using kinetic studies, we have shown that added halides (added as NaCl and NaBr can increase the catalytic activity of the palladium nanoparticles more than 10-fold, allowing reactions to be completed in less than half a day at 30 °C. However, this increased activity comes at the expense of catalyst recovery. The results are in agreement with a reaction mechanism in which, under conditions involving high concentrations of chloride or bromide, palladium leaching plays an important role. Considering the evidence for analogous reactions occurring on the surface of palladium nanoparticles under different reaction conditions, we conclude that additives can exert a significant effect on the mechanism of reactions catalyzed by nanoparticles, including switching from a surface reaction to a solution reaction. The possibility of this switch in mechanism may also be the cause for the disagreement on this topic in the literature.

  4. Electrochemical behavior of fission palladium in 1-butyl-3-methylimidazolium chloride

    Energy Technology Data Exchange (ETDEWEB)

    Jayakumar, M.; Venkatesan, K.A.; Srinivasan, T.G. [Fuel Chemistry Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India)

    2007-08-01

    Electrochemical behavior of palladium (II) chloride in 1-butyl-3-methylimidazolium chloride has been investigated by various electrochemical transient techniques using glassy carbon working electrode at different temperatures (343-373 K). Cyclic voltammogram consisted of a prominent reduction wave at -0.61 V (vs. Pd) due to the reduction of Pd(II) to Pd, and two oxidation waves at -0.26 and 0.31 V. A nucleation loop is observed at -0.53 V. The diffusion coefficient of palladium (II) in bmimCl ({proportional_to}10{sup -7} cm{sup 2}/s) was determined and the energy of activation (63 kJ/mol) was deduced from the cyclic voltammograms at various temperatures. Nucleation and growth of palladium on glassy carbon working electrode has been investigated by chronoamperometry and chronopotentiometry. The growth and decay of chronocurrents measured for palladium deposition has been found to follow the instantaneous nucleation model with three-dimensional growth of nuclei. The surface morphology of the deposit obtained at various applied potentials revealed the formation of dendrites immediately after nucleation and spread in all the directions with time. (author)

  5. Alternative products to carbazoles in the oxidation of diphenylamines with palladium (II) acetate

    OpenAIRE

    Raposo, M. Manuela M.; Campos, Ana M. F. Oliveira; Shannon, Patrick V. R.

    1997-01-01

    Although simple diphenylamines are conveniently oxidised with Palladium (II) acetate to give carbazoles, for more complex examples, carbazoles are minor products amongst many. CRUP (Portugal). British Council - Treaty of Windsor Programme. Junta Nacional de Investigação Científica e Tecnológica.

  6. Oxidative addition of aryl chlorides to monoligated palladium(0): A DFT-SCRF study

    DEFF Research Database (Denmark)

    Ahlquist, Mårten Sten Gösta; Norrby, Per-Ola

    2007-01-01

    Oxidative addition of aryl chlorides to palladium has been investigated by hybrid density functional theory methods (B3LYP), including a continuum model describing the solvent implicitly. A series of para-substituted aryl chlorides were studied to see the influence of electronic effects...

  7. Definition of the size of nanoclusters of silver and palladium in carbon fiber

    International Nuclear Information System (INIS)

    Volobuev, V.S.; Bashmakov, I.A.; Lukashevich, S.M.; Tolkacheva, E.A.; Tikhonova, T.F.; Lukashevich, M.G.; Kaputskij, F.N.

    2008-01-01

    Size of palladium and silver nanoclusters is carbon matrix prepared by heart treatment of metal-polymer precursor has been determined by means of XR diffractions study. It was shown that the cluster size increases with increasing annealing temperature from 700 to 900 degree Celsius by factor two. No structuring of carbon matrix was observed under clusters forming. (authors)

  8. Sensitization to palladium and nickel in Europe and the relationship with oral disease and dental alloys

    NARCIS (Netherlands)

    Muris, J.; Goossens, A.; Gonçalo, M.; Bircher, A.J.; Giménez-Arnau, A.; Foti, C.; Rustemeyer, T.; Feilzer, A.J.; Kleverlaan, C.J.

    2015-01-01

    Background The role of palladium and nickel sensitization in oral disease and dermatitis is not fully understood. Objectives To investigate whether sensitization to these metals was associated with exposure to dental alloys and oral and skin complaints/symptoms in a European multicentre study.

  9. Controlled deposition of palladium nanodendrites on the tips of gold nanorods and their enhanced catalytic activity.

    Science.gov (United States)

    Su, Gaoxing; Jiang, Huaqiao; Zhu, Hongyan; Lv, Jing-Jing; Yang, Guohai; Yan, Bing; Zhu, Jun-Jie

    2017-08-31

    Plasmonic Au-Pd nanostructures have drawn significant attention for use in heterogeneous catalysis. In this study, palladium nanodendrite-tipped gold nanorods (PdND-T-AuNRs) were subjected to a facile fabrication under mild reaction conditions. The palladium amounts on the two tips were tunable. In the preparation of PdND-T-AuNRs, dense capped AuNRs, a low reaction temperature, and suitable stabilizing agents were identified as critical reaction parameters for controlling palladium nanodendrites deposited on both ends of AuNRs. After overgrowth with palladium nanodendrites, the longitudinal surface plasmonic resonance peaks of PdND-T-AuNRs were red-shifted from 810 nm to 980 nm. The electrocatalytic activity of PdND-T-AuNRs for ethanol oxidation was examined, which was a bit weaker than that of cuboid core-shell Au-Pd nanodendrites; however, PdND-T-AuNRs were more stable in ethanol electrooxidation. Moreover, the photocatalytic activity of PdND-T-AuNRs for Suzuki cross-coupling reactions was investigated. At room temperature, nearly 100% yield was obtained under laser irradiation. The results can further enhance our capability of fine-tuning the optical, electronic, and catalytic properties of the bimetallic Au-Pd nanostructures.

  10. Sonogashira Coupling Reaction with Palladium Powder and Potassium Fluoride in Methanol

    Institute of Scientific and Technical Information of China (English)

    王磊; 李品华

    2003-01-01

    A Sonogashira coupling reaction of aromatic halides with terminal alkynes in the presence of palladium powder,potassium fluoride,cuprous iodide and triphenylphosphine in methanol,giving the corresponding coupling products aryl alkynes in good to excellent yiekls,was investigated.

  11. Palladium-catalyzed aerobic oxidative cross-coupling of arylhydrazines with terminal alkynes.

    Science.gov (United States)

    Zhao, Yingwei; Song, Qiuling

    2015-09-04

    The palladium-catalyzed Sonogashira-type aerobic oxidative coupling of arylhydrazines with terminal alkynes via C-N bond cleavage has been developed; internal alkynes were afforded with a broad substrate scope. This reaction proceeds under copper- and base-free conditions with molecular oxygen as the sole oxidant and nitrogen and water as the only by-products.

  12. Practical and General Palladium-Catalyzed Synthesis of Ketones from Internal Olefins

    KAUST Repository

    Morandi, Bill; Wickens, Zachary K.; Grubbs, Robert H.

    2013-01-01

    Make it simple! A convenient and general palladium-catalyzed oxidation of internal olefins to ketones is reported. The transformation occurs at room temperature and shows wide substrate scope. Applications to the oxidation of seed-oil derivatives and a bioactive natural product (see scheme) are described, as well as intriguing mechanistic features.

  13. Reactivation of a Palladium Catalyst during Glucose Oxidation by Molecular Oxygen

    Czech Academy of Sciences Publication Activity Database

    Gogová, Zuzana; Hanika, Jiří

    2009-01-01

    Roč. 63, č. 5 (2009), s. 520-526 ISSN 0366-6352 R&D Projects: GA ČR(CZ) GD203/08/H032 Institutional research plan: CEZ:AV0Z40720504 Keywords : glucose * palladium catalyst * deactivation Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 0.791, year: 2009

  14. Metal Palladium Dispersed Inside Macroporous Ion-Exchange Resins: Textural Characterization and Accessibility to Gaseou Reactants

    Czech Academy of Sciences Publication Activity Database

    Biffis, A.; Jeřábek, Karel; D'Archivio, A. A.; Galantini, L.; Corain, B.

    2000-01-01

    Roč. 130, - (2000), s. 2327-2332 ISSN 0167-2991. [International Congress on Catalysis /12./. Granada, 09.07.2000-14.07.2000] Institutional research plan: CEZ:AV0Z4072921 Keywords : metal palladium * dispersed * ion-exchange resins Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 0.513, year: 2000

  15. Practical and General Palladium-Catalyzed Synthesis of Ketones from Internal Olefins

    KAUST Repository

    Morandi, Bill

    2013-01-16

    Make it simple! A convenient and general palladium-catalyzed oxidation of internal olefins to ketones is reported. The transformation occurs at room temperature and shows wide substrate scope. Applications to the oxidation of seed-oil derivatives and a bioactive natural product (see scheme) are described, as well as intriguing mechanistic features.

  16. Palladium-Catalysed Direct Cross-Coupling of Organolithium Reagents with Aryl and Vinyl Triflates

    NARCIS (Netherlands)

    Vila, Carlos; Hornillos, Valentin; Giannerini, Massimo; Fananas-Mastral, Martin; Feringa, Bernard L.

    2014-01-01

    Carbon-Carbon Bond Formation Carbon-carbon bond formation by the cross-coupling of highly reactive organolithium reagents is a major challenge. Recently, it was demonstrated that palladium catalysts are able to couple organic halides with various organolithium species under mild conditions in a

  17. Palladium-catalysed direct cross-coupling of secondary alkyllithium reagents

    NARCIS (Netherlands)

    Vila, Carlos; Giannerini, Massimo; Hornillos, Valentin; Fananas-Mastral, Martin; Feringa, Ben L.

    2014-01-01

    Palladium-catalysed cross-coupling of secondary C(sp(3)) organometallic reagents has been a long-standing challenge in organic synthesis, due to the problems associated with undesired isomerisation or the formation of reduction products. Based on our recently developed catalytic C-C bond formation

  18. Preparation of fluorinated biaryls through direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates

    KAUST Repository

    Fang, Xin

    2013-07-01

    The direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates gave the desired products of fluorinated biaryls in good to excellent yields. A diverse set of important functional groups including methoxy, aldehyde, ester, nitro and halide can be well tolerated in the protocol. © 2013 Elsevier B.V. All rights reserved.

  19. Silver-palladium catalysts for the direct synthesis of hydrogen peroxide

    Science.gov (United States)

    Khan, Zainab; Dummer, Nicholas F.; Edwards, Jennifer K.

    2017-11-01

    A series of bimetallic silver-palladium catalysts supported on titania were prepared by wet impregnation and assessed for the direct synthesis of hydrogen peroxide, and its subsequent side reactions. The addition of silver to a palladium catalyst was found to significantly decrease hydrogen peroxide productivity and hydrogenation, but crucially increase the rate of decomposition. The decomposition product, which is predominantly hydroxyl radicals, can be used to decrease bacterial colonies. The interaction between silver and palladium was characterized using scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and temperature programmed reduction (TPR). The results of the TPR and XPS indicated the formation of a silver-palladium alloy. The optimal 1% Ag-4% Pd/TiO2 bimetallic catalyst was able to produce approximately 200 ppm of H2O2 in 30 min. The findings demonstrate that AgPd/TiO2 catalysts are active for the synthesis of hydrogen peroxide and its subsequent decomposition to reactive oxygen species. The catalysts are promising for use in wastewater treatment as they combine the disinfectant properties of silver, hydrogen peroxide production and subsequent decomposition. This article is part of a discussion meeting issue 'Providing sustainable catalytic solutions for a rapidly changing world'.

  20. Bulk and Surface Structures of Palladium-Modified Copper-Zinc Oxides ex Hydroxycarbonate Precursors

    NARCIS (Netherlands)

    López Granados, M.; Melián-Cabrera, I.; Fierro, J.L.G.

    2002-01-01

    (Pd)-Cu-Zn ex hydroxycarbonate precursors were prepared and characterized by several bulk and surface techniques. A palladium-free Cu-Zn precursor (CZ) was prepared by coprecipitation. Two Pd-Cu-Zn samples were prepared by coprecipitation (PCZ-CP) and sequential precipitation (PCZ-SP). It is shown

  1. Synthesis of Nitriles via Palladium-Catalyzed Water Shuffling from Amides to Acetonitrile

    OpenAIRE

    Zhang, Wandi; Haskins, Christopher W.; Yang, Yang; Dai, Mingji

    2014-01-01

    Palladium-catalyzed synthesis of nitriles from amides has been described. Two similar, but complementary reaction conditions have been identified to convert various amides including α,β,γ,δ-unsaturated amides, cinnamides, aromatic amides and alkyl amides to the corresponding nitriles in good to excellent yield.

  2. Synthesis of nitriles via palladium-catalyzed water shuffling from amides to acetonitrile.

    Science.gov (United States)

    Zhang, Wandi; Haskins, Christopher W; Yang, Yang; Dai, Mingji

    2014-12-07

    Palladium-catalyzed synthesis of nitriles from amides has been described. Two similar, but complementary reaction conditions have been identified to convert various amides including α,β,γ,δ-unsaturated amides, cinnamides, aromatic amides and alkyl amides to the corresponding nitriles in good to excellent yield.

  3. Palladium(II)-catalyzed ortho-olefination of arenes applying sulfoxides as remote directing groups.

    Science.gov (United States)

    Wang, Binjie; Shen, Chuang; Yao, Jinzhong; Yin, Hong; Zhang, Yuhong

    2014-01-03

    A novel palladium-catalyzed ortho-C(sp(2))-H olefination protocol has been developed by the use of sulfoxide as the directing group. Importantly, relatively remote coordination can be accessed to achieve the ortho olefination of benzyl, 2-arylethyl, and 3-arylpropenyl sulfoxide substrates, and the olefinated sulfoxide can be easily transformed to other functionalities.

  4. Palladium Hydride Promoted Stereoselective Isomerization of Unactivated Di(exo)methylenes to Endocyclic Dienes

    OpenAIRE

    Jung, Michael E.; Lee, Gloria S.; Pham, Hung V.; Houk, K. N.

    2014-01-01

    The exomethylenes of 2,6-disubstituted bicyclo[3.3.1]nonan-9-ones 2 are readily isomerized over a palladium catalyst under an atmosphere of hydrogen to predominantly form the isomer 3 with C 2 symmetry with very little formation of the analogous product with C s symmetry. A hydrogen source is essential to effect the rearrangement.

  5. Memory effects in palladium-catalyzed allylic Alkylations of 2-cyclohexen-1-yl acetate

    DEFF Research Database (Denmark)

    Svensen, Nina; Fristrup, Peter; Tanner, David Ackland

    2007-01-01

    The objective of this work was to characterize the enantiospecificity of the allylic alkylation of enantioenriched 2-cyclohexen-1-yl acetate with the enolate ion of dimethyl malonate catalyzed by unsymmetrical palladium catalysts. The precatalysts employed were (eta(3)-allyl)PdLCl, where L...

  6. Assembling strategy to synthesize palladium modified kaolin nanocomposites with different morphologies

    OpenAIRE

    Li, Xiaoyu; Ouyang, Jing; Zhou, Yonghua; Yang, Huaming

    2015-01-01

    Nanocomposites of aluminosilicate minerals, kaolins (kaolinite and halloysite) with natural different morphologies assembling with palladium (Pd) nanoparticles have been successfully synthesized through strong electrostatic adsorption and chemical bonding after surface modification with 3-aminopropyl triethoxysilane (APTES). Meanwhile, the influence of different morphologies supports on catalytic hydrogenation properties was explored. The surface concentration of amino groups on the kaolins w...

  7. Preparation of palladium nanoparticles on alumina surface by chemical co-precipitation method and catalytic applications

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Avvaru Praveen; Kumar, B. Prem; Kumar, A.B.V. Kiran; Huy, Bui The [Department of Chemistry, Changwon National University, Changwon 641-773 (Korea, Republic of); Lee, Yong-Ill, E-mail: yilee@changwon.ac.kr [Department of Chemistry, Changwon National University, Changwon 641-773 (Korea, Republic of)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer Facile synthesis of palladium nanoparticles on alumina surface. Black-Right-Pointing-Pointer The surface morphology and properties of the nanocrystalline powders were characterized. Black-Right-Pointing-Pointer The catalytic activities of palladium nanoparticles were investigated. - Abstract: The present work reports a chemical co-precipitation process to synthesize palladium (Pd) nanoparticles using alumina as a supporting material. The optimized temperature for the formation of nanocrystalline palladium was found to be 600 Degree-Sign C. The X-ray diffraction (XRD) and Raman spectroscopy were used to study the chemical nature of the Pd in alumina matrix. The surface morphology and properties of the nanocrystalline powders were examined using thermogravimetric analysis (TG-DTA), XRD, Raman spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM). The calcinations in different atmospheres including in the inert medium forms the pure nano Pd{sup 0} while in the atmospheric air indicates the existence pure Pd{sup 0} along with PdO nanoparticles. The catalytic activities of the as-synthesized nanocrystalline Pd nanoparticles in the alumina matrix were investigated in Suzuki coupling, Hiyama cross-coupling, alkene and alkyne hydrogenation, and aerobic oxidation reactions.

  8. Micromachined Dense Palladium Electrodes for Thin-film Solid Acid Fuel Cells

    NARCIS (Netherlands)

    Unnikrishnan, S.

    2009-01-01

    This thesis paves the way towards the microfabrication of a solid acid electrolyte based fuel cell (µSAFC), which has a membrane electrode assembly (MEA) consisting of a thin-film of water soluble electrolyte encapsulated between two dense palladium electrode membranes. This project work

  9. A Palladium-Catalyzed Vinylcyclopropane (3 + 2) Cycloaddition Approach to the Melodinus Alkaloids

    KAUST Repository

    Goldberg, Alexander F. G.

    2011-08-19

    A palladium-catalyzed (3+2) cycloaddition of a vinylcyclopropane and a β-nitrostyrene is employed to rapidly assemble the cyclopentane core of the Melodinus alkaloids. The ABCD ring system of the natural product family is prepared in six steps from commercially available materials.

  10. GREEN SYNTHESIS OF SILVER AND PALLADIUM NANOPARTICLES AT ROOM TEMPERATURE USING COFFEE AND TEA EXTRACT

    Science.gov (United States)

    An extremely simple green approach that generates bulk quantities of nanocrystals of noble metals such as silver (Ag) and palladium (Pd) using coffee and tea extract at room temperature is described. The single-pot method uses no surfactant, capping agent, and/or template. The ob...

  11. DTDGA impregnated XAD-16 beads for separation and recovery of palladium from acidic wastes

    International Nuclear Information System (INIS)

    Singh, Krishan Kant; Kanagare, Anant B.; Bairwa, K.K.; Manmohan Kumar; Bajaj, Parma N.; Ruhela, Ritesh; Singh, Ajoy K.; Hubli, Rajendra C.

    2014-01-01

    In the present study DTDGA extractant impregnated XAD16 polymeric beads (DTDGA- XAD16) were synthesized by wet chemical method and the beads were characterized by various techniques viz. FT-IR, Optical microscopy, SEM and TGA. The DTDGA-XAD 16 beads were evaluated for separation and recovery of palladium from high level waste solutions (HLW)

  12. Analysis of antibiotic residues in foodstuffs in Tunisia: The tetracyclines, quinolones, and Sulphonamides

    International Nuclear Information System (INIS)

    Rezgui, Adel

    2009-01-01

    The first part of the work was to detect antibiotic residues in animal nutriment: chicken, fish, eggs and milk, by methods of screening. The second part covered the development of a new kit for the detection of antibiotic residues. (Author)

  13. Characterization of intracellular palladium nanoparticles synthesized by Desulfovibrio desulfuricans and Bacillus benzeovorans

    Energy Technology Data Exchange (ETDEWEB)

    Omajali, Jacob B., E-mail: JBO037@bham.ac.uk, E-mail: jbomajali@gmail.com; Mikheenko, Iryna P. [University of Birmingham, Unit of Functional Bionanomaterials, School of Biosciences, Institute of Microbiology and Infection (United Kingdom); Merroun, Mohamed L. [University of Granada, Department of Microbiology, Faculty of Sciences (Spain); Wood, Joseph [University of Birmingham, School of Chemical Engineering (United Kingdom); Macaskie, Lynne E. [University of Birmingham, Unit of Functional Bionanomaterials, School of Biosciences, Institute of Microbiology and Infection (United Kingdom)

    2015-06-15

    Early studies have focused on the synthesis of palladium nanoparticles within the periplasmic layer or on the outer membrane of Desulfovibrio desulfuricans and on the S-layer protein of Bacillus sphaericus. However, it has remained unclear whether the synthesis of palladium nanoparticles also takes place in the bacterial cell cytoplasm. This study reports the use of high-resolution scanning transmission electron microscopy with a high-angle annular dark field detector and energy dispersive X-ray spectrometry attachment to investigate the intracellular synthesis of palladium nanoparticles (Pd NPs). We show the intracellular synthesis of Pd NPs within cells of two anaerobic strains of D. desulfuricans and an aerobic strain of B. benzeovorans using hydrogen and formate as electron donors. The Pd nanoparticles were small and largely monodispersed, between 0.2 and 8 nm, occasionally from 9 to 12 nm with occasional larger nanoparticles. With D. desulfuricans NCIMB 8307 (but not D. desulfuricans NCIMB 8326) and with B. benzeovorans NCIMB 12555, the NPs were larger when made at the expense of formate, co-localizing with phosphate in the latter, and were crystalline, but were amorphous when made with H{sub 2,} with no phosphorus association. The intracellular Pd nanoparticles were mainly icosahedrons with surfaces comprising {111} facets and about 5 % distortion when compared with that of bulk palladium. The particles were more concentrated in the cell cytoplasm than the cell wall, outer membrane, or periplasm. We provide new evidence for synthesis of palladium nanoparticles within the cytoplasm of bacteria, which were confirmed to maintain cellular integrity during this synthesis.

  14. Conducting polymer-coated, palladium-functionalized multi-walled carbon nanotubes for the electrochemical sensing of hydroxylamine

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Eunhee; Ahmed, Mohammad Shamsuddin; You, Jung-Min; Kim, Seul Ki; Jeon, Seungwon, E-mail: swjeon@chonnam.ac.kr

    2012-08-31

    Electrochemical sensors of hydroxylamine were fabricated on glassy carbon electrodes (GCEs) by the electropolymerization of 3,4-ethylenedioxypyrrole (EDOP) and 3,4-ethylenedioxythiophene (EDOT) on palladium (Pd) nanoparticles attached to thiolated multi-walled carbon nanotubes (MWCNTs), denoted as PEDOP/MWCNT-Pd/GCE and PEDOT/MWCNT-Pd/GCE. The sensors were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy. They showed strong catalytic activity toward the oxidation of hydroxylamine. Cyclic voltammetry and amperometry were used to characterize the sensors' performances. The detection limits of hydroxylamine by PEDOP/MWCNT-Pd/GCE and PEDOT/MWCNT-Pd/GCE were 0.22 and 0.24 {mu}M (S/N = 3), respectively. The sensors' sensitivity, selectivity, and stability were also investigated. - Highlights: Black-Right-Pointing-Pointer Multi-wall carbon nanotubes-Pd nanoparticles (MWCNT-Pd) based electrodes. Black-Right-Pointing-Pointer Electropolymerized electrodes by poly3,4-ethylenedioxythiophene(PEDOT). Black-Right-Pointing-Pointer PEDOT/MWCNT-Pd has a low detection limit of 0.24 Micro-Sign M for hydroxylamine. Black-Right-Pointing-Pointer PEDOT/MWCNT-Pd exhibits a wide linear range from 1 Micro-Sign M to 6 mM hydroxylamine. Black-Right-Pointing-Pointer The resulting sensor shows fast response and good stability.

  15. Residual gas analysis

    International Nuclear Information System (INIS)

    Berecz, I.

    1982-01-01

    Determination of the residual gas composition in vacuum systems by a special mass spectrometric method was presented. The quadrupole mass spectrometer (QMS) and its application in thin film technology was discussed. Results, partial pressure versus time curves as well as the line spectra of the residual gases in case of the vaporization of a Ti-Pd-Au alloy were demonstrated together with the possible construction schemes of QMS residual gas analysers. (Sz.J.)

  16. Soluble Polymer-supported Synthesis of Indoles via Palladium-mediat -ed Heteroannulation of Terminal Alkynes with o-Iodoanilines

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A soluble polymer-supported synthesis of indoles via palladium-mediated hetero- annulation of terminal alkynes with o-iodoanilines has been described. The protocol provides a useful tool for constructing combinatorial indole libraries.

  17. Stereoselective synthesis of tricyclic compounds by intramolecular palladium-catalyzed addition of aryl iodides to carbonyl groups

    Directory of Open Access Journals (Sweden)

    Jakub Saadi

    2016-06-01

    Full Text Available Starting from γ-ketoesters with an o-iodobenzyl group we studied a palladium-catalyzed cyclization process that stereoselectively led to bi- and tricyclic compounds in moderate to excellent yields. Four X-ray crystal structure analyses unequivocally defined the structure of crucial cyclization products. The relative configuration of the precursor compounds is essentially transferred to that of the products and the formed hydroxy group in the newly generated cyclohexane ring is consistently in trans-arrangement with respect to the methoxycarbonyl group. A transition-state model is proposed to explain the observed stereochemical outcome. This palladium-catalyzed Barbier-type reaction requires a reduction of palladium(II back to palladium(0 which is apparently achieved by the present triethylamine.

  18. Camphyl-based α-diimine palladium complexes: highly efficient precatalysts for direct arylation of thiazoles in open-air.

    Science.gov (United States)

    Chen, Fu-Min; Lu, Dong-Dong; Hu, Li-Qun; Huang, Ju; Liu, Feng-Shou

    2017-07-21

    Based on the strategy of the development of phosphine-free palladium-catalyzed direct C-H arylation, a series of camphyl-based α-diimine palladium complexes bearing sterically bulky substituents were synthesized and characterized. The palladium complexes were applied for the cross-coupling of thiazole derivatives with aryl bromides. The effect of the sterically bulky substituent on the N-aryl moiety as well as the reaction conditions was screened. Under the optimal protocols, a wide range of aryl bromides can be smoothly coupled with thiazoles in good to excellent yields in the presence of a low palladium loading of 0.2 mol% under open-air conditions.

  19. Myocardial blood flow rate and capillary permeability for 99mTc-DTPA in patients with angiographically normal coronary arteries. Evaluation of the single-injection, residue detection method with intracoronary indicator bolus injection and the use of a mobile gamma camera

    DEFF Research Database (Denmark)

    Svendsen, Jesper Hastrup; Kelbaek, H; Efsen, F

    1994-01-01

    The aims of the present study were to quantitate myocardial perfusion and capillary permeability in the human heart by means of the single-injection, residue detection method using a mobile gamma camera. With this method, the intravascular mean transit time and the capillary extraction fraction (E...

  20. Impact of a second FDG PET scan before adjuvant therapy for the early detection of residual/relapsing tumours in high-risk patients with oral cavity cancer and pathological extracapsular spread

    Energy Technology Data Exchange (ETDEWEB)

    Liao, Chun-Ta; Huang, Shiang-Fu; Chen, I-How; Kang, Chung-Jan [Chang Gung Memorial Hospital and Chang Gung University, Department of Otorhinolaryngology, Head and Neck Surgery, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Fan, Kang-Hsing; Lin, Chien-Yu [Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Department of Radiation Oncology, Taoyuan (China); Wang, Hung-Ming [Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Department of Medical Oncology, Taoyuan (China); Ng, Shu-Hang [Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Department of Diagnostic Radiology, Taoyuan (China); Hsueh, Chuen; Lee, Li-Yu [Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Department of Pathology, Taoyuan (China); Lin, Chih-Hung [Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Department of Plastic and Reconstructive Surgery, Taoyuan (China); Yen, Tzu-Chen [Chang Gung Memorial Hospital and Chang Gung University, Head and Neck Oncology Group, Taoyuan (China); Chang Gung Memorial Hospital and Chang Gung University, Department of Nuclear Medicine and Molecular Imaging Center, Taoyuan (China)

    2012-06-15

    Extracapsular spread (ECS) to the cervical lymph nodes is a major adverse prognostic factor in oral cavity squamous cell carcinoma (OSCC). We prospectively examined the value of FDG PET immediately before postoperative radiotherapy/concurrent chemoradiotherapy (pre-RT/CCRT PET) to detect residual/relapsing disease in the early postsurgical follow-up period in high-risk OSCC patients with ECS. We examined 183 high-risk OSCC patients with ECS who underwent preoperative FDG PET/CT for staging purposes. Of these patients, 29 underwent a second pre-RT/CCRT FDG PET/CT scan. The clinical utility of the second FDG PET/CT was examined using Kaplan-Meier curve analysis. Patients who underwent the second FDG PET/CT scan had baseline clinicopathological characteristics similar to those who did not undergo a second scan. Of the patients who underwent the second scan, seven (24 %) had unexpected, newly discovered lesions. Five eventually died of the disease, and two had no evidence of recurrence after a change in RT field and dose. In an event-based analysis at 2 months, rates of neck control (6/29 vs. 6/154, p = 0.001), distant metastases (3/29 vs. 4/154, p = 0.046), and disease-free survival (7/29 vs. 10/154, p = 0.003) were significantly higher in patients who received a second PET scan than in those who did not. The second pre-RT/CCRT PET scan was of particular benefit for detecting new lesions in OSCC patients with both ECS and lymph node standardized uptake value (SUV) of {>=}5.2 in the first PET scan. The present findings support the clinical value of pre-RT/CCRT FDG PET for defining treatment strategy in OSCC patients with both ECS and high nodal SUV, even when FDG PET had already been performed during the initial staging work-up. (orig.)