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Sample records for extracted ion chromatograms

  1. OpenSlice: Quantitative data sharing from HyperPeaks to global ion chromatograms (GICs).

    Science.gov (United States)

    Askenazi, Manor; Fenyö, David

    2016-09-01

    Data sharing in the field of MS has advanced greatly thanks to innovations such as the standardized formats, data repositories, and publications guidelines. However, there is currently no data sharing mechanism that enables real-time data browsing and deep linking on a large scale: unrestricted data access (particularly at the quantitative level) ultimately requires the user to download a local copy of the relevant data files (e.g., in order to generate extracted ion chromatograms [XICs]). In this technical resource, we present a set of technologies (collectively termed OpenSlice) that enable the user to quantitatively query hundreds of hours of proteomics discovery data (i.e., nontargeted acquisition) in real time: the user is able to effectively generate XICs for arbitrary masses on the fly and across the entire dataset (so-called global ion chromatograms), interacting with the results through a very intuitive browser-based interface. A key design consideration underlying the OpenSlice approach is the notion that every aspect of the acquired data must be accessible through a RESTful uniform resource locator based application programming interface, up to and including individual chromatographic peaks (hence HyperPeaks). A publicly accessible demonstration of this technology based on the Clinical Proteomics Tumor Analysis Consortium CompRef dataset is made available at http://compref.fenyolab.org. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. An automated Pearson's correlation change classification (APC3) approach for GC/MS metabonomic data using total ion chromatograms (TICs).

    Science.gov (United States)

    Prakash, Bhaskaran David; Esuvaranathan, Kesavan; Ho, Paul C; Pasikanti, Kishore Kumar; Chan, Eric Chun Yong; Yap, Chun Wei

    2013-05-21

    A fully automated and computationally efficient Pearson's correlation change classification (APC3) approach is proposed and shown to have overall comparable performance with both an average accuracy and an average AUC of 0.89 ± 0.08 but is 3.9 to 7 times faster, easier to use and have low outlier susceptibility in contrast to other dimensional reduction and classification combinations using only the total ion chromatogram (TIC) intensities of GC/MS data. The use of only the TIC permits the possible application of APC3 to other metabonomic data such as LC/MS TICs or NMR spectra. A RapidMiner implementation is available for download at http://padel.nus.edu.sg/software/padelapc3.

  3. Combination of HPLC chromatogram and hypoglycemic effect identifies isoflavones as the principal active fraction of Belamcanda chinensis leaf extract in diabetes treatment.

    Science.gov (United States)

    Chen, Yan; Wu, Chong-Ming; Dai, Rong-Ji; Li, Liang; Yu, Yu-Hong; Li, Yan; Meng, Wei-Wei; Zhang, Liang; Zhang, Yongqian; Deng, Yu-Lin

    2011-02-15

    In previous study, we demonstrated the hypoglycemic effect of aqueous extract of Belamcanda chinensis leaves in rats. Here, we separated the aqueous extract of B. chinensis leaves and investigated the spectrum-effect relationships between HPLC chromatograms and hypoglycemic activities of different isolates from B. chinensis leaf extract. Sequential solvent extraction with petroleum ether, chloroform, acetic ester and n-butanol provided several isolates showing similar hypoglycemic activities, making it difficult to discriminate the active fractions. Stepwise elution through HP20 macroporous resin by water, 40% and 95% ethanol provided isolates with distinct hypoglycemic activities, representing a simple, rapid and efficient preparative separation method. Combination of HPLC chromatogram and pharmacological effect targeted a hypoglycemic activity-related region in HPLC chromatogram. Each peak in this region was analyzed by UV spectrum scan. Most of them were flavonoids in which tectoridin and swertisin were known flavonoids with anti-diabetic activities. In together, this work provides a general model of combination of HPLC chromatography and pharmacological effect to study the spectrum-effect relationships of aqueous extract from B. chinensis leaves, which can be used to find principle components of B. chinensis on pharmacological activity.

  4. Ion Beam Extraction by Discrete Ion Focusing

    DEFF Research Database (Denmark)

    2010-01-01

    An apparatus (900) and methods are disclosed for ion beam extraction. In an implementation, the apparatus includes a plasma source (or plasma) (802) and an ion extractor (804). The plasma source is adapted to generate ions and the ion extractor is immersed in the plasma source to extract a fraction...... of the generated ions. The ion extractor is surrounded by a space charge (810) formed at least in part by the extracted ions. The ion extractor includes a biased electrode (806) forming an interface with an insulator (808). The interface is customized to form a strongly curved potential distribution (812......) in the space-charge surrounding the ion extractor. The strongly curved potential distribution focuses the extracted ions towards an opening (814) on a surface of the biased electrode thereby resulting in an ion beam....

  5. A tool to evaluate correspondence between extraction ion chromatographic peaks and peptide-spectrum matches in shotgun proteomics experiments.

    Science.gov (United States)

    Ruse, Cristian I; Peacock, Samantha; Ghiban, Cornel; Rivera, Keith; Pappin, Darryl J; Leopold, Peter

    2013-08-01

    Chromatographed peptide signals form the basis of further data processing that eventually results in functional information derived from data-dependent bottom-up proteomics assays. We seek to rank LC/MS parent ions by the quality of their extracted ion chromatograms. Ranked extracted ion chromatograms act as an intuitive physical/chemical preselection filter to improve the quality of MS/MS fragment scans submitted for database search. We identify more than 4900 proteins when considering detector shifts of less than 7 ppm. High quality parent ions for which the database search yields no hits become candidates for subsequent unrestricted analysis for PTMs. Following this rational approach, we prioritize identification of more than 5000 spectrum matches from modified peptides and confirmed the presence of acetylaldehyde-modified His/Lys. We present a logical workflow that scores data-dependent selected ion chromatograms and leverage information about semianalytical LC/LC dimension prior to MS. Our method can be successfully used to identify unexpected modifications in peptides with excellent chromatography characteristics, independent of fragmentation pattern and activation methods. We illustrate analysis of ion chromatograms detected in two different modes by RF linear ion trap and electrostatic field orbitrap.

  6. Average mass scan of the total ion chromatograms: a new gas chromatography-mass spectrometry derived variable for fast and reliable multivariate statistical treatment of essential oil compositional data.

    Science.gov (United States)

    Radulović, Niko S; Blagojević, Polina D

    2013-08-02

    Plant volatiles have been repeatedly shown to provide valuable insight into the evolutionary relationships among plant taxa on various taxonomical levels. The number of variables available from GC-MS analyses of these plant metabolites usually represents a large data set. The comparison of such data sets requires the use of multivariate statistical analyses (MSA) but with several serious shortcomings. In order to make multivariate statistical comparison of essential oils more applicable, reliable and faster, this work was set to explore the suitability of a complementary use of relative abundances of m/z values of the average mass scan of the total GC chromatograms instead of the traditionally used variables-percentages (peak areas) of individual oil constituents. To achieve this, essential oils extracted from 12 different Artemisia species were analyzed using GC-FID and GC-MS. Almost 500 different constituents were successfully identified. Average mass scans of the total GC chromatograms (AMS) and chemical compositions (relative percentages) of the analyzed oils were separately compared using two MSA methods: agglomerative hierarchical cluster analysis and principal component analysis. This approach was applied to an additional set of essential oil compositional data (representatives of a number of different genera/families; data from the literature) using both types of variables. The obtained results strongly suggest that MSA of complex volatile mixtures, using the corresponding directly obtainable AMS, could be considered as a promising time saving tool for easy and reliable comparison purposes. The AMS approach gives comparable or even better results than the traditional method - it reflected the natural relationships between observations within both studied groups of oils.

  7. Identification of Hogwash Oil through Ion-Chromatogram%离子色谱法鉴别地沟油的应用研究

    Institute of Scientific and Technical Information of China (English)

    张咏; 李莹; 蔡春明

    2012-01-01

    The negative ion in the hogwash oil - adulterated edible oil was identified in both composition and quantity using IC method. The results showed that some acetate was detected in hogwash oil but none in qualified oil. A good linear relationship was found between the adulteration amount of hogwash oil and the acetate content. When the hogwash oil was added into qualified edible oil up to 5% ( wt), a characteristic peak of acetate would be obviously observed. Therefore the method would be effective in determining whether the oil was adulterated with hogwash oil.%利用离子色谱法测定地沟油样品水萃取液中阴离子组成及含量,从而定性分析食用油脂中是否掺杂地沟油.试验结果表明,在地沟油样品的水萃取液中检测出一定量的乙酸根离子,而在合格食用食物油中未检出;当食用植物油中掺杂5%(质量分数)以上的地沟油时,就能很明显在色谱图上观察到乙酸根离子的峰,并且其含量与地沟油的掺杂量呈线性增加.因此测定食用油水萃取液中阴离子的种类及含量是鉴别食用植物油是否掺混地沟油的重要检测依据.

  8. Negative ion beam extraction in ROBIN

    Energy Technology Data Exchange (ETDEWEB)

    Bansal, Gourab, E-mail: bansal@ipr.res.in [Institute for Plasma Research (IPR), Bhat, Gandhinagar, Gujarat 382428 (India); Gahlaut, Agrajit; Soni, Jignesh; Pandya, Kaushal; Parmar, Kanu G.; Pandey, Ravi; Vuppugalla, Mahesh; Prajapati, Bhavesh; Patel, Amee; Mistery, Hiren [Institute for Plasma Research (IPR), Bhat, Gandhinagar, Gujarat 382428 (India); Chakraborty, Arun; Bandyopadhyay, Mainak; Singh, Mahendrajit J.; Phukan, Arindam; Yadav, Ratnakar K.; Parmar, Deepak [ITER-India, Institute for Plasma Research, A-29, Sector 25, GIDC, Gandhinagar, Gujarat 380025 (India)

    2013-10-15

    Highlights: ► A RF based negative hydrogen ion beam test bed has been set up at IPR, India. ► Ion source has been successfully commissioned and three campaigns of plasma production have been carried out. ► Extraction system (35 kV) has been installed and commissioning has been initiated. Negative ion beam extraction is immediate milestone. -- Abstract: The RF based single driver −ve ion source experiment test bed ROBIN (Replica Of BATMAN like source in INDIA) has been set up at Institute for Plasma Research (IPR), India in a technical collaboration with IPP, Garching, Germany. A hydrogen plasma of density 5 × 10{sup 12} cm{sup −3} is expected in driver region of ROBIN by launching 100 kW RF power into the driver by 1 MHz RF generator. The cesiated source is expected to deliver a hydrogen negative ion beam of 10 A at 35 kV with a current density of 35 mA/cm{sup 2} as observed in BATMAN. In first phase operation of the ROBIN ion source, a hydrogen plasma has been successfully generated (without extraction system) by coupling 80 kW RF input power through a matching network with high power factor (cos θ > 0.8) and different plasma parameters have been measured using Langmuir probes and emission spectroscopy. The plasma density of 2.5 × 10{sup 11} cm{sup −3} has been measured in the extraction region of ROBIN. For negative hydrogen ion beam extraction in second phase operation, extraction system has been assembled and installed with ion source on the vacuum vessel. The source shall be first operated in volume mode for negative ion beam extraction. The commissioning of the source with high voltage power supply has been initiated.

  9. [GPC Fingerprint Chromatograms of Aloe vera Leaf Gel Polysaccharides].

    Science.gov (United States)

    Wang, Qiao-e; Xie, Dan; Qian, Jie; Dong, Yin-mao

    2015-10-01

    To establish the gel permeation chromatography (GPC) fingerprint chromatograms of polysaccharides in Aloe vera leaf gel from the same habitat (Beijing) and different habitats for evaluating the quality of Aloe vera leaf gel products commercially available and testing common adulterated substances. The samples were prepared by water-extraction and alcohol-precipitation method. GPC separation was performed on a Shodex SUGAR KS-805 (300 mm x 8.0 mm, 7 μm) column and a Shodex SUGAR KS-803 (300 mm x 8.0 mm, 6 μm) column at the temperature of 60 degrees C by eluting with 0.1 mol/L NaNO3 (containing 0.2 per thousand NaN) at a flow rate of 0.8 mL/min, the chromatographic effluent was detected by refractive index detector (RID) at the temperature of 50 degrees C. The common pattern of GPC fingerprint chromatograms was established and four common peaks were demarcated. The similarities of samples from the same habitat (Beijing) and different habitats were over 0.9. Taking the GPC fingerprint chromatograms for the qualified model, three commercially available aloe products were evaluated to be made of Aloe vera by the different manufacturing processes and four common adulterated substances of aloe polysaccharides were identified effectively. The method is simple and accurate with a good reproducibility, and it can be used for the identification and quality evaluation of Aloe vera leaf gel products.

  10. Fast ion extraction in laser isotope separation

    Energy Technology Data Exchange (ETDEWEB)

    Hazak, G.; Gell, Y.; Boneh, Y.; Goshen, S.

    1980-10-01

    An analysis of the E x B scheme for fast ion extraction in laser isotope separation is presented. Using an analytically solvable model and a numerical simulation we have found that the scheme can meet the rather severe time and space restrictions imposed by the large cross section for charge exchange.

  11. Applications of HPLC-MS in compound Ilex pubescens extract study

    Institute of Scientific and Technical Information of China (English)

    Yang Yunyun; Hongwei Chen; Zhong Ming; Ma Zhiling; Teng Jiuwei; Mu Dehai

    2006-01-01

    In this paper,high performance liquid chromatography(HPLC)along with mass spectrometry (MS)and HPLC along with a diode array detector(DAD)was used to study the compound flex pubescens extract.Two ionization techniques:electro spray ionization(ESI)and atmospheric pressure chemical ionization(APCI)were used in this work.The liquid chromatograms obtained by DAD,total ion chromatograms(TIC)from positive-and negative-ion ESI-MS and the positive-and negative-ion APCI-MS were compared.The liquid chromatograms obtained by TIC from ESI-MS provided more information on chromatographic peaks than those obtained by DAD or TIC from APCI-MS.It is suggested that the fingerprints of the compound Ilex pubescens extract should be provided by the liquid chromatograms obtained by DAD together with TIC from the negative-ion ESI-MS.The molecular weights of the nine main components in an HPLC-DAD chromatogram were determined by the corresponding positive-and negative-ion ESI and the positive-and negative-ion APCI mass spectra information.In the liquid chromatogram obtained by TIC from the negative-ion ESI-MS,the molecular weights of 23 main components were determined based on the corresponding positive-and negative-ion ESI mass spectra information.

  12. Calculation Of Extraction Optics For Ion System With Plazma Emitter

    CERN Document Server

    Frolov, B A

    2004-01-01

    The 2-D code for simulating of ion optics system of positive ion extraction from a plasma source is described. Example calculation of 100 kV optics for the extraction ion IHEP gun is presented. The trajectories of particles and emittance plots are resulted. The aberrations influ-ence strongly on ion optics for considered geometry.

  13. Neutralization principles for the Extraction and Transport of Ion Beams

    CERN Document Server

    Riege, H

    2000-01-01

    The strict application of conventional extraction techniques of ion beams from a plasma source is characterized by a natural intensity limit determined by space charge.The extracted current may be enhanced far beyond this limit by neutralizing the space charge of the extracted ions in the first extraction gap of the source with electrons injected from the opposite side. The transverse and longitudinal emittances of a neutralized ion beam, hence its brightness, are preserved. Results of beam compensation experiments, which have been carried out with a laser ion source, are resumed for proposing a general scheme of neutralizing ion sources and their adjacent low-energy beam transport channels with electron beams. Many technical applications of high-mass ion beam neutralization technology may be identified: the enhancement of ion source output for injection into high-intensity, low-and high-energy accelerators, or ion thrusters in space technology, for the neutral beams needed for plasma heating of magnetic conf...

  14. Extraction mechanism of monovalent ion-pairs by polyurethane foams.

    Science.gov (United States)

    Fong, P; Chow, A

    1992-07-01

    The extractability sequence of K(+) approximately Rb(+) > Cs(+) > Na(+) > Li(+) for the extraction with polyether foam suggests that the cation chelation mechanism might be operative. However, the same order was obtained for the extraction with 100% polypropylene oxide polyether foam which does not normally adopt a helical structure to form oxygen-rich cavities as easily or as effectively as polyethylene oxide to accommodate alkali metal ions. This result indicates that a hole-size/cation-diameter relationship may not be required for the high extraction of K(+). The extraction of alkali metal DPAs and hydroxides from methanol demonstrates the importance of the solvent effect. It indicates that the water-structure enforced ion-pairing (WSEIP) is the driving force for extraction of the ion-pairs. The extraction mechanism for ionic species can be described as an ion-pair extraction process. The overall effect of ion-pair formation in water and interaction of the extracted ions with foam appears to determine the extractability of the ions of the extractable ion-pair.

  15. Main magnetic focus ion source with the radial extraction of ions

    CERN Document Server

    Ovsyannikov, V P

    2015-01-01

    In the main magnetic focus ion source, atomic ions are produced in the local ion trap created by the rippled electron beam in focusing magnetic field. Here we present the novel modification of the room-temperature hand-size device, which allows the extraction of ions in the radial direction perpendicular to the electron beam across the magnetic field. The detected X-ray emission evidences the production of Ir$^{44+}$ and Ar$^{16+}$ ions. The ion source can operate as the ion trap for X-ray spectroscopy, as the ion source for the production of highly charged ions and also as the ion source of high brightness.

  16. Simulation of ion beam extraction and focusing system

    Institute of Scientific and Technical Information of China (English)

    B.A.Soliman; M.M.Abdelrahman; A.G.Helal; F.W.Abdelsalam

    2011-01-01

    The characteristics of ion beam extraction and focused to a volume as small as possible were investigated with the aid of computer code SIMION 3D version 7.This has been used to evaluate the extraction characteristics(accel-decel system)to generate an ion beam with low beam emittance and high brightness.The simulation process can provide a good study for optimizing the extraction and focusing system of the ion beam without any losses and transported to the required target.Also,a study of a simulation model for the extraction system of the ion source was used to describe the possible plasma boundary curvatures during the ion extraction that may be affected by the change in an extraction potential with a constant plasma density meniscus.

  17. Solid-liquid solvent extraction of metal ions

    Institute of Scientific and Technical Information of China (English)

    Bo Peng; Haiyan Fan; Jinzhang Gao

    2003-01-01

    An overview of extraction of some trace metal ions using molten solvent (low melting substance) during last two decadesis presented. The development of this technique since its inception is briefly traced. The comparison of extraction efficiency, thermo-dynamics and kinetics mainly involving extraction of rare earth ions between molten solvent extraction at high temperature and usualliquid-liquid extraction at room temperature are discussed in detail. The various parameters obtained from the previous and presentstudies such as equilibrium extraction constant Kex, pH1/2, thermodynamic and kinetic data are displayed in tabular form. Finally, thecurrent demands, disadvantages and future prospects are also evaluated.

  18. Simulation of ion beam injection and extraction in an EBIS

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, L., E-mail: zhao@far-tech.com; Kim, J. S. [FAR-TECH, Inc., San Diego, California 92121 (United States)

    2016-02-15

    An example simulation of Au+ charge breeding using FAR-TECH’s integrated EBIS (electron beam ion source) modeling toolset is presented with the emphasis on ion beam injection and extraction. The trajectories of injected ions are calculated with PBGUNS (particle beam gun simulation) self-consistently by including the space charges from both ions and electrons. The ion beam, starting with initial conditions within the 100% acceptance of the electron beam, is then tracked by EBIS-PIC (particle-in-cell EBIS simulation code). In the trap, the evolution of the ion charge state distribution is estimated by charge state estimator. The extraction of charge bred ions is simulated with PBGUNS. The simulations of the ion injections show significant ion space charge effects on beam capture efficiency and the ionization efficiency.

  19. Simulation of ion beam injection and extraction in an EBIS

    Science.gov (United States)

    Zhao, L.; Kim, J. S.

    2016-02-01

    An example simulation of Au+ charge breeding using FAR-TECH's integrated EBIS (electron beam ion source) modeling toolset is presented with the emphasis on ion beam injection and extraction. The trajectories of injected ions are calculated with PBGUNS (particle beam gun simulation) self-consistently by including the space charges from both ions and electrons. The ion beam, starting with initial conditions within the 100% acceptance of the electron beam, is then tracked by EBIS-PIC (particle-in-cell EBIS simulation code). In the trap, the evolution of the ion charge state distribution is estimated by charge state estimator. The extraction of charge bred ions is simulated with PBGUNS. The simulations of the ion injections show significant ion space charge effects on beam capture efficiency and the ionization efficiency.

  20. Gas Cromatography In Solar System Exploration:decoding Complex Chromatograms Recovered From Space Missions

    Science.gov (United States)

    Pietrogrande, M. C.; Tellini, I.; Dondi, F.; Felinger, A.; Sternberg, R.; Szopa, C.; Vidal-Madjar, C.

    GC plays a predominant role in solar system explorations: it has been applied to space research related to exobiology: i.e., Cassini-Huygens mission devoted to characterize chemical composition of TitanSs atmosphere [2], Rosetta mission to investigate the nucleus of comet p/Wirtamen (COSAC experiments) [1]. GC analysis of planetary atmosphere is a difficult analytical task because of the unknown and low level of an- alytes present in the sample, the high degree of automatization required, the strong constraints due to the flight (short analysis time, low power consumption, high accu- racy and reliability under extreme space conditions). In these circumstances the use of a signal processing procedure is practically mandatory to efficiently extract useful in- formation from the raw chromatogram ­ i.e. to decode the complex chromatogram to determine the number of components, the separation efficiency and the retention pat- tern. In this work a chemometric approach based on the Fourier analysis is applied to complex chromatograms related to space research: from the autocovariance function (ACVF) computed on the digitized chromatogram, the chromatographic parameters ­ number of components, peak shape parameters, retention pattern ­ can be estimated [3-7]. The procedure, originally developed for constant peak width [3], was extended to variable peak width [4], in order to describe chromatograms obtained in isother- mal conditions, i.e., analysis condition compatible with space flight constraints. The chemometric procedure was applied to chromatograms of standard mixtures repre- sentative of planetary atmospheres ­ hydrocarbons and oxygenated compounds with carbon atom number ranging from 2 to 8 ­ obtained in flight simulating conditions ­ isothermal or pseudo-isothermal conditions. Both the simplified graphic procedure, based on the assumption of constant peak width [3], and the complete approach de- veloped for variable peak width [4], were applied and the results

  1. Predicting ion flux uniformity at the ion extraction plate in a 3D ICP reactor

    Science.gov (United States)

    Roy, Abhra; Bhoj, Ananth

    2016-09-01

    In order to achieve better control in processing the wafer surface, the ion fluxes in a remote plasma system are often focused through one or more ion extraction plates between the main plasma chamber and the downstream wafer plane. The ion extraction plates are typically of showerhead pattern with multiple holes. The focus of this particular study is to predict the ion flux uniformity over the ion extraction plate for a full 3D inductively coupled discharge reactor model using Argon chemistry. We will use the commercial modeling tool, CFD-ACE +, which can address such a process involving gas flow, heat transfer, plasma physics, reaction chemistry and electromagnetics in a coupled fashion. The plasma characteristics in the chamber and uniformity of the ion fluxes at ion extraction plate are discussed. Parametric studies varying the geometrical dimensions and process conditions to determine the effect on ion flux uniformity are presented. The showerhead-like ion extraction plate will be modeled as a porous media with a specified porosity. Further, a spatially varying porosity of the ion extraction plate is used to simulate ion recombination in order to reduce the ion flux non-uniformity. The goal is to optimize the system maximizing the ion flux while maintaining the uniformity.

  2. A New Three-Dimensional Code for Simulation of Ion Beam Extraction: Ion Optics Simulator

    Institute of Scientific and Technical Information of China (English)

    JIN Dazhi; HUANG Tao; HU Quan; YANG Zhonghai

    2008-01-01

    A new thee-dimensional code, ion optics simulator (IOS), to simulate ion beam extraction is developed in visual C++ language. The theoretical model, the flowchart of code, and the results of calculation as an example are presented.

  3. Ion beam extraction from a matrix ECR plasma source by discrete ion-focusing effect

    DEFF Research Database (Denmark)

    Stamate, Eugen; Draghici, Mihai

    2010-01-01

    Positive or negative ion beams extracted from plasma are used in a large variety of surface functionalization techniques such as implantation, etching, surface activation, passivation or oxidation. Of particular importance is the surface treatment of materials sensitive to direct plasma exposure...... due to high heath fluxes, the controllability of the ion incidence angle, and charge accumulation when treating insulating materials. Despite of a large variety of plasma sources available for ion beam extraction, there is a clear need for new extraction mechanisms that can make available ion beams...... with high current densities that can treat surfaces placed adjacent to the extraction region. This work introduces a new phenomenology for ion beam extraction using the discrete ion-focusing effect associated with three-dimensional plasma-sheath-lenses [1, 2]. Experiments are performed in a matrix...

  4. Transport and extraction of radioactive ions stopped in superfluid helium

    CERN Document Server

    Huang Wan Xia; Gloos, K; Takahashi, N; Arutyunov, K; Pekola, J P; Äystö, J

    2003-01-01

    A new approach to convert a high energy beam to a low energy one, which is essential for the next generation radioactive ion beam facilities, has been proposed and tested at Jyvaeskylae, Finland. An open sup 2 sup 2 sup 3 Ra alpha-decay-recoil source has been used to produce radioactive ions in superfluid helium. The alpha spectra demonstrate that the recoiling sup 2 sup 1 sup 9 Rn ions have been extracted out of liquid helium. This first observation of the extraction of heavy positive ions across the superfluid helium surface was possible thanks to the high sensitivity of radioactivity detection. An efficiency of 36% was obtained for the ion extraction out of liquid helium.

  5. Grid-controlled extraction of pulsed ion beams

    Science.gov (United States)

    Humphries, S., Jr.; Burkhart, C.; Coffey, S.; Cooper, G.; Len, L. K.; Savage, M.; Woodall, D. M.; Rutkowski, H.; Oona, H.; Shurter, R.

    1986-03-01

    Experimental results are presented on a method for extracting well-focused ion beams from plasma sources with time-varying properties. An electrostatic grid was used to stop the flow of plasma electrons so that only ions entered the extraction gap. In this case, ion flow in the gap was controlled by space-charge effects as it would be with a thermionic ion source. Constant extracted current was observed even with large variations of source flux. An insulator spark source and a metal-vapor vacuum arc were used to generate pulsed ion beams. With a hydrocarbon spark, current densities of 44 mA/cm2 were achieved at 20-kV extractor voltage for an 8-μs pulse. With an aluminum-vapor arc, a current density of 15 mA/cm2 (0.3 A total) was measured for a 50-μs pulse.

  6. Grid-controlled extraction of pulsed ion beams

    Energy Technology Data Exchange (ETDEWEB)

    Humphries, S. Jr.; Burkhart, C.; Coffey, S.; Cooper, G.; Len, L.K.; Savage, M.; Woodall, D.M.; Rutkowski, H.; Oona, H.; Shurter, R.

    1986-03-15

    Experimental results are presented on a method for extracting well-focused ion beams from plasma sources with time-varying properties. An electrostatic grid was used to stop the flow of plasma electrons so that only ions entered the extraction gap. In this case, ion flow in the gap was controlled by space-charge effects as it would be with a thermionic ion source. Constant extracted current was observed even with large variations of source flux. An insulator spark source and a metal-vapor vacuum arc were used to generate pulsed ion beams. With a hydrocarbon spark, current densities of 44 mA/cm/sup 2/ were achieved at 20-kV extractor voltage for an 8-..mu..s pulse. With an aluminum-vapor arc, a current density of 15 mA/cm/sup 2/ (0.3 A total) was measured for a 50-..mu..s pulse.

  7. ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

    Science.gov (United States)

    A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

  8. ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

    Science.gov (United States)

    A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

  9. Determination of contents of 10-Hydroxycamptothecin in Camptotheca acuminata by high-performance liquid chromatogram

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The determination method of 10-hydroxycamptothecin in Camptotheca acuminata fruits by high-performance liquid chromatogram (HPLC) was studied. The HPLC analysis was performed on a HIQ sil C18(4.6×250 mm) column with mobile phase of acetonitrile-water (3:7, V:V), flow rate 1 mL@(min-1 and UV detective wavelength 266 nm. Extracting 10-hydroxycamptothecin by ultrasonic method from fruits of C. acuminata to prepare samples for analysis was systematically discussed. The optimal extraction condition was carried out by 60% alcohol solution at 60℃ for 50 minutes.

  10. Scattering extraction of ions at CRYRING for SEU testing

    CERN Document Server

    Novák, D; Klamra, W; Norlin, L O; Bagge, L; Kaellberg, A; Paál, A; Rensfelt, K G; Molnár, J

    1999-01-01

    A measuring station has been built at the CRYRING heavy ion accelerator to test the Single Event Upset (SEU) phenomena in working Static RAM circuits. The setup extracts the beam using Rutherford scattering and the ions are monitored with a BaF sub 2 scintillator. SEU measurements have been performed for standard bulk CMOS memory circuits.

  11. [Study on HPLC fingerprint chromatograms of Arisaematis Rhizoma].

    Science.gov (United States)

    Luo, Fen; Lu, Dan; Chi, Yumei; Wu, Hao; Yu, Hongli

    2011-12-01

    The fingerprint chromatograms of Arisaematis Rhizoma were established by HPLC. The analysis was performed on a Lichrospher C18 (4.6 mm x 200 mm, 5 microm) column with acetonitrile-water (containing 0.1% acetic acid) as mobile phase at a flow rate of 1.0 mL x min(-1). The detection wavelength was set at 270 nm, and the column temperature was 30 degrees C. The similarities of the fingerprint chromatograms were calculated over 0.9 between 11 batches of Arisaematis Rhizoma samples by analyzing 14 common peaks with adenosine as reference substance. However, their fingerprint chromatograms were significantly different from those of Pinellia pedatisecta and P. ternate. Adenine, hypoxanthine, xanthine, uridine, guanosine, adenosine, schaftoside, and isoschaftoside were identified by comparing the retention times and their ultraviolet spectra. The method is repeatable, exclusive and can be used for identification and evaluation of Arisaematis Rhizoma.

  12. Arsenic and selenium speciation in coal fly ash extracts by ion chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, B.P.; Miller, W.P. [University of Georgia, Aiken, SC (United States). Savannah River Ecology Lab.

    1998-10-01

    Ion chromatography (IC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) was used to determine As(III), As(V), Se(IV), and Se(VI) in aqueous extracts of coal fly ash. Because all species were fully resolved, the resulting chromatograms were obtained by summing signal intensities for m/z 75 + m/z 82. Absolute detection limits of 7.2, 87, 117 and 28 pg for As(III), Se(IV), Se(VI), and As(V) respectively, were obtained corresponding to 0.072, 0.868, 1.174, and 0.284 {mu} gl{sup -1} for 100 {mu} l injection volume. The technique was used to determine the speciation of As and Se in aqueous extracts of 24 coal fly ash samples including NIST SRM 1633 b. The predominant species were As(V) and Se(IV), with As(III) detected in two low pH fly ashes. Extraction of fly ashes at pH 5 altered the concentrations of total soluble As and Se but did not affect the predominant As and Se speciation.

  13. Simulation of ion beam extraction and focusing system

    Institute of Scientific and Technical Information of China (English)

    B. A. Soliman; M. M. Abdelrahman; A. G. Helal; F. W. Abdelsalam

    2011-01-01

    The characteristics of ion beam extraction and focused to a volume as small as possible were investigated with the aid of computer code SIMION 3D version 7. This has been used to evaluate the extraction characteristics (accel-decel system) to generate an

  14. On the microscopic mechanism of ion-extraction of a gridded ion propulsion thruster

    CERN Document Server

    Kirmse, Danny

    2013-01-01

    The following paper includes a physical microscopic particle-description of the phenomena and mechanisms that lead to the extraction of ions with the aim to generate thrust. This theoretical treatise arose from the intention to visualize the behavior of the involved particles under effect of the involved electrical fields. By this way, an underlying basis for experimental investigations of the work of an ion thruster should be formed. So a foundation was created, which explains the ion extracting and so thrust generating function of an ion thruster. The theoretical work was related to the Radio-frequency Ion Thruster (RIT). But the model worked out can be generalized for all thruster types that use electrostatic fields to extract positively charged ions.

  15. Analysis of the H- ion emissive surface in the extraction region of negative ion sources.

    Science.gov (United States)

    Kameyama, N; Fukuyama, T; Wada, S; Kuppel, S; Tsumori, K; Nakano, H; Hatayama, A; Miyamoto, K; Fukano, A; Bacal, M

    2012-02-01

    To understand the plasma characteristics in the extraction region of negative H(-) sources is very important for the optimization of H(-) extraction from the sources. The profile of plasma density and electrostatic potential in the extraction region with and without extraction grid voltage are analyzed with a 2D particle in cell modeling of the NIFS-RD H(-) sources. The simulation results make clear the physical process forming a double ion plasma layer (which consists only of positive H(+) and negative H(-) ions) recently observed in the Cs-seeded experiments of the NIFS-R&D source in the vicinity of the extraction hole and the plasma grid. The results also give a useful insight into the formation mechanism of the plasma meniscus and the H(-) extraction process for such double ion plasma.

  16. Extraction of ions and electrons from audio frequency plasma source

    Directory of Open Access Journals (Sweden)

    N. A. Haleem

    2016-09-01

    Full Text Available Herein, the extraction of high ion / electron current from an audio frequency (AF nitrogen gas discharge (10 – 100 kHz is studied and investigated. This system is featured by its small size (L= 20 cm and inner diameter = 3.4 cm and its capacitive discharge electrodes inside the tube and its high discharge pressure ∼ 0.3 Torr, without the need of high vacuum system or magnetic fields. The extraction system of ion/electron current from the plasma is a very simple electrode that allows self-beam focusing by adjusting its position from the source exit. The working discharge conditions were applied at a frequency from 10 to 100 kHz, power from 50 – 500 W and the gap distance between the plasma meniscus surface and the extractor electrode extending from 3 to 13 mm. The extracted ion/ electron current is found mainly dependent on the discharge power, the extraction gap width and the frequency of the audio supply. SIMION 3D program version 7.0 package is used to generate a simulation of ion trajectories as a reference to compare and to optimize the experimental extraction beam from the present audio frequency plasma source using identical operational conditions. The focal point as well the beam diameter at the collector area is deduced. The simulations showed a respectable agreement with the experimental results all together provide the optimizing basis of the extraction electrode construction and its parameters for beam production.

  17. Efficient ion beam extraction from a flowing plasma

    Energy Technology Data Exchange (ETDEWEB)

    Dembinski, M.; John, P.K.

    1979-10-01

    A moving plasma with directed flow velocities v larger than the ion acoustic speed c/sub s/ is used as a source of high-current ion beams in the 10--20-keV range of energies. Current densities up to 3 A/cm/sup 2/ are obtained at the plasma boundary which is an order of magnitude larger than the limiting value of Bohm current in a stationary plasma. The observed current densities were proportional to v, unlike the Bohm current densities which are proportional to ion acoustic speed. Total ion currents up to approx.100 A were extracted from the plasma through a two electrode extraction system. Simple geometric shaping of the electrodes enabled an 8-cm-diam beam to be focused to approx.7 mm.

  18. The role of space charge compensation for ion beam extraction and ion beam transport (invited)

    Energy Technology Data Exchange (ETDEWEB)

    Spädtke, Peter, E-mail: p.spaedtke@gsi.de [GSI Helmholtzzentrum für Schwerionenforschung GmbH (Germany)

    2014-02-15

    Depending on the specific type of ion source, the ion beam is extracted either from an electrode surface or from a plasma. There is always an interface between the (almost) space charge compensated ion source plasma, and the extraction region in which the full space charge is influencing the ion beam itself. After extraction, the ion beam is to be transported towards an accelerating structure in most cases. For lower intensities, this transport can be done without space charge compensation. However, if space charge is not negligible, the positive charge of the ion beam will attract electrons, which will compensate the space charge, at least partially. The final degree of Space Charge Compensation (SCC) will depend on different properties, like the ratio of generation rate of secondary particles and their loss rate, or the fact whether the ion beam is pulsed or continuous. In sections of the beam line, where the ion beam is drifting, a pure electrostatic plasma will develop, whereas in magnetic elements, these space charge compensating electrons become magnetized. The transport section will provide a series of different plasma conditions with different properties. Different measurement tools to investigate the degree of space charge compensation will be described, as well as computational methods for the simulation of ion beams with partial space charge compensation.

  19. A Study on the Ion Beam Extraction using Duo-PiGatron Ion source for Vertical Type Ion Beam Facility

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Bom Sok; Lee, Chan young; Lee, Jae Sang [KAERI, Daejeon (Korea, Republic of)

    2015-05-15

    In Korea Multipurpose Accelerator Complex (KOMAC), we have started ion beam service in the new beam utilization building since March this year. For various ion beam irradiation services, we are developed implanters such as metal (150keV/1mA), gaseous (200keV/5mA) and high current ion beam facility (20keV/150mA). One of the new one is a vertical type ion beam facility without acceleration tube (60keV/20mA) which is easy to install the sample. After the installation is complete, it is where you are studying the optimal ion beam extraction process. Detailed experimental results will be presented. Vertical Type Ion Beam Facility without acceleration tube of 60keV 20mA class was installed. We successfully extracted 60keV 20mA using Duo- PiGatron Ion source for Vertical Type Ion Beam Facility. Use the BPM and Faraday-cup, is being studied the optimum conditions of ion beam extraction.

  20. Simulation of H- ion source extraction systems for the Spallation Neutron Source with Ion Beam Simulator.

    Science.gov (United States)

    Kalvas, T; Welton, R F; Tarvainen, O; Han, B X; Stockli, M P

    2012-02-01

    A three-dimensional ion optical code IBSimu, which is being developed at the University of Jyväskylä, features positive and negative ion plasma extraction models and self-consistent space charge calculation. The code has been utilized for modeling the existing extraction system of the H(-) ion source of the Spallation Neutron Source. Simulation results are in good agreement with experimental data. A high-current extraction system with downstream electron dumping at intermediate energy has been designed. According to the simulations it provides lower emittance compared to the baseline system at H(-) currents exceeding 40 mA. A magnetic low energy beam transport section consisting of two solenoids has been designed to transport the beam from the alternative electrostatic extraction systems to the radio frequency quadrupole.

  1. Simulation of H- ion source extraction systems for the Spallation Neutron Source with Ion Beam Simulatora)

    Science.gov (United States)

    Kalvas, T.; Welton, R. F.; Tarvainen, O.; Han, B. X.; Stockli, M. P.

    2012-02-01

    A three-dimensional ion optical code IBSimu, which is being developed at the University of Jyväskylä, features positive and negative ion plasma extraction models and self-consistent space charge calculation. The code has been utilized for modeling the existing extraction system of the H- ion source of the Spallation Neutron Source. Simulation results are in good agreement with experimental data. A high-current extraction system with downstream electron dumping at intermediate energy has been designed. According to the simulations it provides lower emittance compared to the baseline system at H- currents exceeding 40 mA. A magnetic low energy beam transport section consisting of two solenoids has been designed to transport the beam from the alternative electrostatic extraction systems to the radio frequency quadrupole.

  2. Chromatogram Profiles and Cytotoxic Activity of Irradiated Mahkota Dewa (Phaleria Macrocarpa Scheff. Boerl Leaves

    Directory of Open Access Journals (Sweden)

    E. Katrin1

    2011-04-01

    Full Text Available Gamma irradiation has been used by the industries for preservation of herbal medicine, but it has not been studied the effect of gamma irradiation on their efficacy, especially their bioactivity as anticancer substances. The purpose of this research was to study the effect of gamma irradiation on the mahkota dewa leaves which has been claimed to contain potent anticancer substances. Maceration of dried mahkota dewa leaves successively with n-hexane, ethyl acetate, and ethanol gave crude extracts which the ethyl acetate was the most cytotoxic extract against leukemia L1210 cells with an inhibition concentration fifty (IC50 value of 10.3 µg/ml. Further separation of ethyl acetate extract by column chromatograph gave 7 fractions, and fraction 2 showed the most cytotoxic fraction exhibited the most cytotoxic extract against leukemia L1210 cells with an IC50 value of 1.9 µg/ml. Since, the fraction 2 of ethyl acetate extract was the most potent fraction, the irradiated samples were treated with the same procedure as treatment of fraction 2 from control sample. Cytotoxic activity test of fractions 2 from irradiated samples showed that the cytotoxic activity decreased depending on increasing of irradiation dose. Gamma irradiation dose up to 7.5 kGy on mahkota dewa leaves could decreased the cytotoxic activity of fraction 2 as the most cytotoxic-potential fraction against leukemia L1210 cells, but decreasing the cytotoxic activity has not exceeded the limit of the fraction declared inactive. So that the irradiation dose up to 7.5 kGy can be used for decontamination of bacteria and fungus/yeast without eliminating the cytotoxic activity. Gamma irradiation also caused changes in the thin layer chromatograph (TLC spots and HPLC chromatograms profiles of fraction 2 which was the most cytotoxic fraction in ethyl acetate extract of mahkota dewa leaves against leukemia L1210 cells. One of the main peaks (peak 1 on HPLC chromatograms decreased with increasing

  3. Extraction of copper ions by supercritical carbon dioxide

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Complexation combined with supercritical fluid extraction was used to extract Cu2+ in this study. The effects of pressure, temperature, volume of CO2 on the efficiency of extraction were systematically investigated. At the optimum condition a 57.32% recovery was achieved. Addition of suitable amount of methanol(v/v = 5 % ) to the supercritical CO2 can increase in the extraction of Cu2+ (72.69 %, RSD = 2.12 %, n = 3). And the recovery can further increase in the presence of non-ionic surfactant Triton X-100 because of its function of solubilization. Surfactant was first used in the extraction of metal ions in the present study, and the results are satisfied (90.52%, RSD=2.20%, n =3).

  4. Intensified extraction of ionized natural products by ion pair centrifugal partition extraction.

    Science.gov (United States)

    Hamzaoui, Mahmoud; Hubert, Jane; Hadj-Salem, Jamila; Richard, Bernard; Harakat, Dominique; Marchal, Luc; Foucault, Alain; Lavaud, Catherine; Renault, Jean-Hugues

    2011-08-05

    The potential of centrifugal partition extraction (CPE) combined with the ion-pair (IP) extraction mode to simultaneously extract and purify natural ionized saponins from licorice is presented in this work. The design of the instrument, a new laboratory-scale Fast Centrifugal Partition Extractor (FCPE300(®)), has evolved from centrifugal partition chromatography (CPC) columns, but with less cells of larger volume. Some hydrodynamic characteristics of the FCPE300(®) were highlighted by investigating the retention of the stationary phase under different flow rate conditions and for different biphasic solvent systems. A method based on the ion-pair extraction mode was developed to extract glycyrrhizin (GL), a biologically active ionic saponin naturally present in licorice (Glycyrrhiza glabra L., Fabaceae) roots. The extraction of GL was performed at a flow rate of 20 mL/min in the descending mode by using the biphasic solvent system ethyl acetate/n-butanol/water in the proportions 3/2/5 (v/v/v). Trioctylmethylammonium with chloride as a counter-ion (Al336(®)) was used as the anion extractant in the organic stationary phase and iodide, with potassium as counter-ion, was used as the displacer in the aqueous mobile phase. From 20 g of a crude extract of licorice roots, 2.2g of GL were recovered after 70 min, for a total process duration of 90 min. The combination of the centrifugal partition extractor with the ion-pair extraction mode (IP-CPE) offers promising perspectives for industrial applications in the field of natural product isolation or for the fractionation of natural complex mixtures.

  5. 数码扫描薄层色谱影像直接测定黄连提取物中4种生物碱含量%Quantitative Determination of Four Alkaloids in Extractive of Rhizoma Coptidis by Direct Digital Scanning of Thin Layer Chromatogram

    Institute of Scientific and Technical Information of China (English)

    郭隆钢; 孙帅; 谢培山; 徐新军; 王锐银

    2015-01-01

    目的:建立直接数码扫描薄层色谱的影像,利用计算机软件测定黄连提取物中巴马汀、小檗碱、表小檗碱、黄连碱含量的新方法。方法薄层色谱的制备:硅胶高效薄层板;展开剂为乙酸丁酯∶甲醇∶异丙醇∶氨水(25%~28%)=5∶2∶1.5∶1.2;定量操作获得荧光薄层色谱经摄像获取色谱的影像,经专业软件数码扫描,替代常规薄层色谱需采用薄层扫描仪定量的测定方法,利用获取的色谱中小檗碱、巴马汀、表小檗碱、黄连碱斑点的积分值,直接外标法同时测定含量。结果经精密度、准确度、重复性测试,结果符合方法学验证的技术要求。与液相色谱测定的数据比较完全具有可比性。结论用自编计算机软件(‘digiscan’)作为虚拟扫描仪进行数码扫描薄层色谱的影像(薄层色谱视觉数据的永久记录),通用软件Origin Pro积分,外标法计算含量,不需要昂贵的薄层色谱扫描仪,即可进行含量测定,通过黄连提取物中4种生物碱的含量测定,证明这一替代方法用于中药有效成分含量测定的可行性。本法最大优点是不需要昂贵的薄层扫描仪,依靠软件操作,薄层色谱的影像可长期保存,测定不受时间和地点的限制,检测成本效益高。符合中药指标成分含量测定的需求,有推广应用的价值,尤其适合生产企业的全程检验、新药研发过程检验及市场商品的检验。%Objective To establish a method of direct digital scanning of thin layer chromatogram integrated with professional software for quantitative determination of four alkaloids(palmatine, berberine, coptisine, epiberberine) in extractive of Rhizoma Coptidis. Methods Thin layer chromatography(TLC)was conducted on pre-coated Silica gel 60 high performance TLC plate, developing with the solvent system of n-butyl acetate, methanol, isopropanol and ammonia(25 %-28 %) in

  6. Effect of Coulomb collision on the negative ion extraction mechanism in negative ion sources

    Energy Technology Data Exchange (ETDEWEB)

    Goto, I., E-mail: goto@ppl.appi.keio.ac.jp; Nishioka, S.; Abe, S.; Hatayama, A. [Graduate School of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama 223-8522 (Japan); Miyamoto, K. [Naruto University of Education, 748 Nakashima, Takashima, Naruto-cho, Naruto-shi, Tokushima 772-8502 (Japan); Mattei, S.; Lettry, J. [CERN, 1211 Geneva 23 (Switzerland)

    2016-02-15

    To improve the H{sup −} ion beam optics, it is necessary to understand the energy relaxation process of surface produced H{sup −} ions in the extraction region of Cs seeded H{sup −} ion sources. Coulomb collisions of charged particles have been introduced to the 2D3V-PIC (two dimension in real space and three dimension in velocity space particle-in-cell) model for the H{sup −} extraction by using the binary collision model. Due to Coulomb collision, the lower energy part of the ion energy distribution function of H{sup −} ions has been greatly increased. The mean kinetic energy of the surface produced H{sup −} ions has been reduced to 0.65 eV from 1.5 eV. It has been suggested that the beam optics of the extracted H{sup −} ion beam is strongly affected by the energy relaxation process due to Coulomb collision.

  7. Massive parallel 3D PIC simulation of negative ion extraction

    Science.gov (United States)

    Revel, Adrien; Mochalskyy, Serhiy; Montellano, Ivar Mauricio; Wünderlich, Dirk; Fantz, Ursel; Minea, Tiberiu

    2017-09-01

    The 3D PIC-MCC code ONIX is dedicated to modeling Negative hydrogen/deuterium Ion (NI) extraction and co-extraction of electrons from radio-frequency driven, low pressure plasma sources. It provides valuable insight on the complex phenomena involved in the extraction process. In previous calculations, a mesh size larger than the Debye length was used, implying numerical electron heating. Important steps have been achieved in terms of computation performance and parallelization efficiency allowing successful massive parallel calculations (4096 cores), imperative to resolve the Debye length. In addition, the numerical algorithms have been improved in terms of grid treatment, i.e., the electric field near the complex geometry boundaries (plasma grid) is calculated more accurately. The revised model preserves the full 3D treatment, but can take advantage of a highly refined mesh. ONIX was used to investigate the role of the mesh size, the re-injection scheme for lost particles (extracted or wall absorbed), and the electron thermalization process on the calculated extracted current and plasma characteristics. It is demonstrated that all numerical schemes give the same NI current distribution for extracted ions. Concerning the electrons, the pair-injection technique is found well-adapted to simulate the sheath in front of the plasma grid.

  8. An improved extraction for the multicusp-type light ion-ion source apparatus

    Science.gov (United States)

    Reijonen, J.; Heikkinen, P.; Liukkonen, E.; ńrje, J.

    1998-02-01

    A new ion extraction system has been developed for use with the light ion source apparatus (LIISA) of the Accelerator Laboratory. The aim of the new extraction system is to have a more intense and better quality beam. For simulation of the beam behavior at the extraction region a computer code IGUNe has been used. The simulation shows that a simple triode extraction would be efficient enough to extract total beam intensities of around 5 mA at an extraction voltage of 10-15 kV. At the same time, with the carefully designed plasma electrode, the emittance could be decreased significantly from the original design. The new extraction was installed in May 1997 and the results have been encouraging. The transport efficiency of the extracted beam to the first Faraday cup (at a distance of 1.2 m) was 100% and the maximum proton current obtained was 2.0 mA. The maximum proton current in the cyclotron inflector is 1.0 mA, which is eight times larger than the previous record.

  9. Inferring short-range linkage information from sequencing chromatograms.

    Directory of Open Access Journals (Sweden)

    Bastian Beggel

    Full Text Available Direct Sanger sequencing of viral genome populations yields multiple ambiguous sequence positions. It is not straightforward to derive linkage information from sequencing chromatograms, which in turn hampers the correct interpretation of the sequence data. We present a method for determining the variants existing in a viral quasispecies in the case of two nearby ambiguous sequence positions by exploiting the effect of sequence context-dependent incorporation of dideoxynucleotides. The computational model was trained on data from sequencing chromatograms of clonal variants and was evaluated on two test sets of in vitro mixtures. The approach achieved high accuracies in identifying the mixture components of 97.4% on a test set in which the positions to be analyzed are only one base apart from each other, and of 84.5% on a test set in which the ambiguous positions are separated by three bases. In silico experiments suggest two major limitations of our approach in terms of accuracy. First, due to a basic limitation of Sanger sequencing, it is not possible to reliably detect minor variants with a relative frequency of no more than 10%. Second, the model cannot distinguish between mixtures of two or four clonal variants, if one of two sets of linear constraints is fulfilled. Furthermore, the approach requires repetitive sequencing of all variants that might be present in the mixture to be analyzed. Nevertheless, the effectiveness of our method on the two in vitro test sets shows that short-range linkage information of two ambiguous sequence positions can be inferred from Sanger sequencing chromatograms without any further assumptions on the mixture composition. Additionally, our model provides new insights into the established and widely used Sanger sequencing technology. The source code of our method is made available at http://bioinf.mpi-inf.mpg.de/publications/beggel/linkageinformation.zip.

  10. Complexation-induced supramolecular assembly drives metal-ion extraction.

    Science.gov (United States)

    Ellis, Ross J; Meridiano, Yannick; Muller, Julie; Berthon, Laurence; Guilbaud, Philippe; Zorz, Nicole; Antonio, Mark R; Demars, Thomas; Zemb, Thomas

    2014-09-26

    Combining experiment with theory reveals the role of self-assembly and complexation in metal-ion transfer through the water-oil interface. The coordinating metal salt Eu(NO3)3 was extracted from water into oil by a lipophilic neutral amphiphile. Molecular dynamics simulations were coupled to experimental spectroscopic and X-ray scattering techniques to investigate how local coordination interactions between the metal ion and ligands in the organic phase combine with long-range interactions to produce spontaneous changes in the solvent microstructure. Extraction of the Eu(3+)-3(NO3(-)) ion pairs involves incorporation of the "hard" metal complex into the core of "soft" aggregates. This seeds the formation of reverse micelles that draw the water and "free" amphiphile into nanoscale hydrophilic domains. The reverse micelles interact through attractive van der Waals interactions and coalesce into rod-shaped polynuclear Eu(III) -containing aggregates with metal centers bridged by nitrate. These preorganized hydrophilic domains, containing high densities of O-donor ligands and anions, provide improved Eu(III) solvation environments that help drive interfacial transfer, as is reflected by the increasing Eu(III) partitioning ratios (oil/aqueous) despite the organic phase approaching saturation. For the first time, this multiscale approach links metal-ion coordination with nanoscale structure to reveal the free-energy balance that drives the phase transfer of neutral metal salts.

  11. Ion Extraction from a Toroidal Electron Cyclotron Resonance Ion Source: a Numerical Feasibility Study

    Science.gov (United States)

    Caliri, Claudia; Volpe, Francesco; Gammino, Santo; Mascali, David

    2013-10-01

    Electron Cyclotron Resonance Ion Sources (ECRIS) are magnetic mirror plasmas of microwave-heated electrons and cold multi-charged ions. The ions are extracted from one end of the mirror and injected in accelerators for nuclear and particle physics studies, hadrontherapy, or neutral beam injection in fusion plasmas. ECRIS devices progressed to higher and higher ion currents and charge states by adopting stronger magnetic fields (beneficial for confinement) and proportionally higher ECR frequencies. Further improvements would require the attainment of ``triple products'' comparable with major fusion experiments. For this, we propose a new, toroidal rather than linear, ECRIS geometry, which would at the same time improve confinement and make better use of the magnetic field. Ion extraction is more complicated than from a linear device, but feasible, as our modeling indicates. Possible techniques involve charge-dependent drifts, divertors, specially designed magnetic fields and associated loss-cones, electrostatic and/or magnetic deflectors, or techniques used in accelerators to transfer particles from one storage ring or accelerator to the next. Here we present single-particle tracings assessing and comparing these extraction techniques.

  12. Ion beam extraction from a matrix ECR plasma source by discrete ion-focusing effect

    DEFF Research Database (Denmark)

    Stamate, Eugen; Draghici, Mihai

    2010-01-01

    Positive or negative ion beams extracted from plasma are used in a large variety of surface functionalization techniques such as implantation, etching, surface activation, passivation or oxidation. Of particular importance is the surface treatment of materials sensitive to direct plasma exposure ...

  13. Peak alignment and robust principal component analysis of gas chromatograms of fatty acid methyl esters and volatiles

    DEFF Research Database (Denmark)

    Frosch, Stina; Jørgensen, Bo

    2007-01-01

    Gas chromatograms of fatty acid methyl esters and of volatile lipid oxidation products from fish lipid extracts are analyzed by multivariate data analysis [principal component analysis (PCA)]. Peak alignment is necessary in order to include all sampled points of the chromatograms in the data set....... The ability of robust algorithms to deal with outlier problems, including both sample-wise and element-wise outliers, and the advantages and drawbacks of two robust PCA methods, robust PCA (ROBPCA) and robust singular value decomposition when analysing these GC data were investigated. The results show...... that the usage of ROPCA is advantageous, compared with traditional PCA, when analysing the entire profile of chromatographic data in cases of sub-optimally aligned data. It also demonstrates how choosing the most robust PCA (sample or element-wise) depends on the type of outliers present in the data set....

  14. Evaluation of ion current density distribution on an extraction electrode of a radio frequency ion thruster

    Science.gov (United States)

    Masherov, P.; Riaby, V.; Abgaryan, V.

    2017-01-01

    The radial distributions of ion current density on an ion extracting electrode of a radio frequency (RF) ion thruster (RIT) with an inductive plasma source were obtained using probe diagnostics of the RF xenon plasma. Measurements were carried out using a plane wall probe simulator and the VGPS-12 Probe System of Plasma Sensors Co. At xenon flow rate q  =  2 sccm plasma pressure was 2 · 10-3 Torr, incident RF generator power varied in the range P g  =  50-250 W with RF power absorbed by plasma up to P p  =  220 W. Ion current densities were determined using semi- and double-logarithmic probe characteristics by linear extrapolations of their ion branches to probe floating potentials. The same parameters were also measured in undisturbed plasma by a classic cylindrical probe. They exceeded plane probe data by more than two times, showing the effectiveness of plasma sheath reproduction of the RIT ion extracting electrode by the plane wall probe simulator. Slight non-uniformity of the resulting plasma distributions and simplified RIT model design showed that the studied device with flat antenna coil and ferrite core could be considered as a promising prospect for RITs of new generation.

  15. Advanced integrated solvent extraction and ion exchange systems

    Energy Technology Data Exchange (ETDEWEB)

    Horwitz, P. [Argonne National Lab., IL (United States)

    1996-10-01

    Advanced integrated solvent extraction (SX) and ion exchange (IX) systems are a series of novel SX and IX processes that extract and recover uranium and transuranics (TRUs) (neptunium, plutonium, americium) and fission products {sup 90}Sr, {sup 99}Tc, and {sup 137}Cs from acidic high-level liquid waste and that sorb and recover {sup 90}Sr, {sup 99}Tc, and {sup 137}Cs from alkaline supernatant high-level waste. Each system is based on the use of new selective liquid extractants or chromatographic materials. The purpose of the integrated SX and IX processes is to minimize the quantity of waste that must be vitrified and buried in a deep geologic repository by producing raffinates (from SX) and effluent streams (from IX) that will meet the specifications of Class A low-level waste.

  16. Nonlinear preprocessing method for detecting peaks from gas chromatograms

    Directory of Open Access Journals (Sweden)

    Min Hyeyoung

    2009-11-01

    Full Text Available Abstract Background The problem of locating valid peaks from data corrupted by noise frequently arises while analyzing experimental data. In various biological and chemical data analysis tasks, peak detection thus constitutes a critical preprocessing step that greatly affects downstream analysis and eventual quality of experiments. Many existing techniques require the users to adjust parameters by trial and error, which is error-prone, time-consuming and often leads to incorrect analysis results. Worse, conventional approaches tend to report an excessive number of false alarms by finding fictitious peaks generated by mere noise. Results We have designed a novel peak detection method that can significantly reduce parameter sensitivity, yet providing excellent peak detection performance and negligible false alarm rates from gas chromatographic data. The key feature of our new algorithm is the successive use of peak enhancement algorithms that are deliberately designed for a gradual improvement of peak detection quality. We tested our approach with real gas chromatograms as well as intentionally contaminated spectra that contain Gaussian or speckle-type noise. Conclusion Our results demonstrate that the proposed method can achieve near perfect peak detection performance while maintaining very small false alarm probabilities in case of gas chromatograms. Given the fact that biological signals appear in the form of peaks in various experimental data and that the propose method can easily be extended to such data, our approach will be a useful and robust tool that can help researchers highlight valid signals in their noisy measurements.

  17. Study of the negative ion extraction mechanism from a double-ion plasma in negative ion sources

    Energy Technology Data Exchange (ETDEWEB)

    Goto, I.; Nishioka, S.; Hatayama, A. [Graduate school of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama 223-8522 (Japan); Miyamoto, K. [Naruto University of Education, 748 Nakashima, Takashima, Naruto-cho, Naruto-shi, Tokushima 772-8502 (Japan)

    2015-04-08

    We have developed a 2D3V-PIC model of the extraction region, aiming to clarify the basic extraction mechanism of H{sup −} ions from the double-ion plasma in H{sup −} negative ion sources. The result shows the same tendency of the H{sup −} ion density n{sub H{sup −}} as that observed in the experiments, i.e.,n{sub H{sup −}} in the upstream region away from the plasma meniscus (H{sup −} emitting surface) has been reduced by applying the extraction voltage. At the same time, relatively slow temporal oscillation of the electric potential compared with the electron plasma frequency has been observed in the extraction region. Results of the systematic study using a 1D3V-PIC model with the uniform magnetic field confirm the result that the electrostatic oscillation is identified to be lower hybrid wave. The effect of this oscillation on the H{sup −} transport will be studied in the future.

  18. Use of semi-permeable membrane devices and solid-phase extraction for the wide-range screening of microcontaminants in surface water by GC-AED/MS

    NARCIS (Netherlands)

    Stee, van L.L.P.; Leonards, P.E.G.; Loon, van W.M.G.M.; Hendriks, A.J.; Maas, J.L.; Struijs, J.; Brinkman, U.A.T.

    2002-01-01

    An automated GC-MS-based screening method was developed for over 400 industrial, agrochemical and household chemicals. Extracted ion chromatograms were used and the method was aimed at creating a minimum number of false positives. The compound polarity range usually associated with solid-phase extra

  19. Use of semi-permeable membrane devices and solid-phase extraction for the wide-range screening of microcontaminants in surface water by GC-AED/MS

    NARCIS (Netherlands)

    Stee, van L.L.P.; Leonards, P.E.G.; Loon, van W.M.G.M.; Hendriks, A.J.; Maas, J.L.; Struijs, J.; Brinkman, U.A.T.

    2002-01-01

    An automated GC-MS-based screening method was developed for over 400 industrial, agrochemical and household chemicals. Extracted ion chromatograms were used and the method was aimed at creating a minimum number of false positives. The compound polarity range usually associated with solid-phase extra

  20. Negative ion production and beam extraction processes in a large ion source (invited)

    Energy Technology Data Exchange (ETDEWEB)

    Tsumori, K., E-mail: tsumori@nifs.ac.jp; Nakano, H.; Goto, M.; Nagaoka, K.; Osakabe, M.; Takeiri, Y.; Kaneko, O. [National Institute for Fusion Science, 322-6 Oroshi, Toki, Gifu 509-5292 (Japan); The Graduate University for Advanced Studies, Shonan Village, Hayama, Kanagawa 240-0193 (Japan); Ikeda, K.; Kisaki, M. [National Institute for Fusion Science, 322-6 Oroshi, Toki, Gifu 509-5292 (Japan); Geng, S. [The Graduate University for Advanced Studies, Shonan Village, Hayama, Kanagawa 240-0193 (Japan); Wada, M. [Graduate School of Science and Engineering, Doshisha University, Kyotanabe, Kyoto 610-0321 (Japan); Sasaki, K.; Nishiyama, S. [Division of Quantum Science and Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Serianni, G.; Agostinetti, P.; Sartori, E.; Brombin, M.; Veltri, P. [Plasma Engineering Group, Consorzio RFX, Corso Stati Uniti 4, 35127 Padova (Italy); Wimmer, C. [Max-Planck-Institut für Plasmaphysik, Bereich ITER-Technologie und -Diagnostik/N-NBI Boltzmannstr. 2, 85748 Garching (Germany)

    2016-02-15

    Recent research results on negative-ion-rich plasmas in a large negative ion source have been reviewed. Spatial density and flow distributions of negative hydrogen ions (H{sup −}) and positive hydrogen ions together with those of electrons are investigated with a 4-pin probe and a photodetachment (PD) signal of a Langmuir probe. The PD signal is converted to local H{sup −} density from signal calibration to a scanning cavity ring down PD measurement. Introduction of Cs changes the slope of plasma potential local distribution depending upon the plasma grid bias. A higher electron density H{sub 2} plasma locally shields the bias potential and behaves like a metallic free electron gas. On the other hand, the bias and extraction electric fields penetrate in a Cs-seeded electronegative plasma even when the electron density is similar. Electrons are transported by the penetrated electric fields from the driver region along and across the filter and electron deflection magnetic fields. Plasma ions exhibited a completely different response against the penetration of electric fields.

  1. An online peak extraction algorithm for ion mobility spectrometry data.

    Science.gov (United States)

    Kopczynski, Dominik; Rahmann, Sven

    2015-01-01

    Ion mobility (IM) spectrometry (IMS), coupled with multi-capillary columns (MCCs), has been gaining importance for biotechnological and medical applications because of its ability to detect and quantify volatile organic compounds (VOC) at low concentrations in the air or in exhaled breath at ambient pressure and temperature. Ongoing miniaturization of spectrometers creates the need for reliable data analysis on-the-fly in small embedded low-power devices. We present the first fully automated online peak extraction method for MCC/IMS measurements consisting of several thousand individual spectra. Each individual spectrum is processed as it arrives, removing the need to store the measurement before starting the analysis, as is currently the state of the art. Thus the analysis device can be an inexpensive low-power system such as the Raspberry Pi. The key idea is to extract one-dimensional peak models (with four parameters) from each spectrum and then merge these into peak chains and finally two-dimensional peak models. We describe the different algorithmic steps in detail and evaluate the online method against state-of-the-art peak extraction methods.

  2. Pixel-based analysis of comprehensive two-dimensional gas chromatograms (color plots) of petroleum

    DEFF Research Database (Denmark)

    Furbo, Søren; Hansen, Asger B.; Skov, Thomas;

    2014-01-01

    We demonstrate how to process comprehensive two-dimensional gas chromatograms (GC × GC chromatograms) to remove nonsample information (artifacts), including background and retention time shifts. We also demonstrate how this, combined with further reduction of the influence of irrelevant informati...

  3. Determination of antihyperglycemic biguanides in serum and urine using an ion-pair solid-phase extraction technique followed by HPLC-UV on a pentafluorophenylpropyl column and on an octadecyl column.

    Science.gov (United States)

    Tahara, Kayoko; Yonemoto, Ayumi; Yoshiyama, Yuji; Nakamura, Toshiya; Aizawa, Masaaki; Fujita, Yoshikuni; Nishikawa, Takashi

    2006-11-01

    An HPLC-UV method was established for the determination of metformin and buformin in biological fluids. Metformin was not retained on particles packed in conventional solid-phase extraction cartridges; in contrast, buformin was retained too firmly and not eluted with a solvent for recovery. However, both drugs were retained on particles that had been treated with an ion-pair reagent of heptanesulfonate or dodecylsulfate and recovered almost completely. The recovered fraction was subjected to HPLC on a pentafluorophenylpropyl column which was suitable for the determination of both biguanides in serum and in urine. Limits of quantitation were low enough for clinical use, and reproducibility was high with an RSD of 0.9-2.3%. HPLC on a conventional octadecyl column was suitable only for the determination of buformin in serum since interfering peaks appeared on the chromatograms of urine samples. The method was applied to analysis of some clinical specimens.

  4. Observation of doubly-charged ions of francium isotopes extracted from a gas cell

    Science.gov (United States)

    Schury, P.; Wada, M.; Ito, Y.; Kaji, D.; Haba, H.; Hirayama, Y.; Kimura, S.; Koura, H.; MacCormick, M.; Miyatake, H.; Moon, J. Y.; Morimoto, K.; Morita, K.; Murray, I.; Ozawa, A.; Rosenbusch, M.; Reponen, M.; Takamine, A.; Tanaka, T.; Watanabe, Y. X.; Wollnik, H.

    2017-09-01

    Various isotopes of Ac, Ra, Fr, and Rn were produced by fusion-evaporation reactions using a 48Ca beam. The energetic ions were stopped in and extracted from a helium gas cell. The extracted ions were identified using a multi-reflection time-of-fight mass spectrograph. In all cases, it was observed that the predominant charge state for the extracted ions, including the alkali Fr, was 2+.

  5. DNA sequence chromatogram browsing using JAVA and CORBA.

    Science.gov (United States)

    Parsons, J D; Buehler, E; Hillier, L

    1999-03-01

    DNA sequence chromatograms (traces) are the primary data source for all large-scale genomic and expressed sequence tags (ESTs) sequencing projects. Access to the sequencing trace assists many later analyses, for example contig assembly and polymorphism detection, but obtaining and using traces is problematic. Traces are not collected and published centrally, they are much larger than the base calls derived from them, and viewing them requires the interactivity of a local graphical client with local data. To provide efficient global access to DNA traces, we developed a client/server system based on flexible Java components integrated into other applications including an applet for use in a WWW browser and a stand-alone trace viewer. Client/server interaction is facilitated by CORBA middleware which provides a well-defined interface, a naming service, and location independence. [The software is packaged as a Jar file available from the following URL: http://www.ebi.ac.uk/jparsons. Links to working examples of the trace viewers can be found at http://corba.ebi.ac.uk/EST. All the Washington University mouse EST traces are available for browsing at the same URL.

  6. The extraction of negative carbon ions from a volume cusp ion source

    Science.gov (United States)

    Melanson, Stephane; Dehnel, Morgan; Potkins, Dave; McDonald, Hamish; Hollinger, Craig; Theroux, Joseph; Martin, Jeff; Stewart, Thomas; Jackle, Philip; Philpott, Chris; Jones, Tobin; Kalvas, Taneli; Tarvainen, Olli

    2017-08-01

    Acetylene and carbon dioxide gases are used in a filament-powered volume-cusp ion source to produce negative carbon ions for the purpose of carbon implantation for gettering applications. The beam was extracted to an energy of 25 keV and the composition was analyzed with a spectrometer system consisting of a 90° dipole magnet and a pair of slits. It is found that acetylene produces mostly C2- ions (up to 92 µA), while carbon dioxide produces mostly O- with only trace amounts of C-. Maximum C2- current was achieved with 400 W of arc power and, the beam current and composition were found to be highly dependent on the pressure in the source. The beam properties as a function of source settings are analyzed, and plasma properties are measured with a Langmuir probe. Finally, we describe testing of a new RF H- ion source, found to produce more than 6 mA of CW H- beam.

  7. Analysis of plasma distribution near the extraction region in surface produced negative ion sources.

    Science.gov (United States)

    Fukano, A; Hatayama, A

    2014-02-01

    In study of a negative ion source, it is important to understand the plasma characteristics near the extraction region. A recent experiment in the NIFS-R&D ion source has suggested that a "double ion plasma layer" which is a region consisting of hydrogen positive and negative ions exists near the plasma grid (PG). Density distribution of plasma near the extraction region is studied analytically. It is shown that the density distribution depends on an amount of the surface produced negative ions and the double ion plasma layer is formed near the PG surface for the case of strong surface production.

  8. Extraction characteristics of a low-energy ion beam system with a remote plasma chamber

    Energy Technology Data Exchange (ETDEWEB)

    Vasquez, M. R., E-mail: mrvasquez@coe.upd.edu.ph [Department of Mining, Metallurgical, and Materials Engineering, College of Engineering, University of the Philippines, Diliman, Quezon City 1101 (Philippines); Wada, M. [Graduate School of Science and Engineering, Doshisha University, Kyotanabe, Kyoto 610-0321 (Japan)

    2016-02-15

    Low-energy argon beams were extracted from a dual-chamber ion source system. The first chamber is a quartz cylinder where dense inductively coupled plasmas were produced using 13.56 MHz radio frequency (rf) power. The discharge was driven into an adjacent chamber which acts as a reservoir for ion beam extraction using a dual-electrode extractor configuration. Extraction of ions from the second chamber with energies in the 100 eV range was achieved while minimizing fluctuations induced by the rf signal. A custom-built retarding potential analyzer was used to analyze the effectiveness of ion beam transport using the remote plasma chamber. Well-defined beams were extracted between 60 and 100 V extraction potentials at 50–100 W rf powers. An increase in rf power resulted in an increase in average ion energy, increase in ion current density while the energy spread remains constant.

  9. Analytical and simulation studies for diode and triode ion beam extraction systems

    Institute of Scientific and Technical Information of China (English)

    M. M. Abdelrahman1; N. I. Basal; S. G. Zakhary

    2012-01-01

    This work is concerned with ion beam dynamics and compares the emittance to aberration ratios of two-and three-electrode extraction systems.The study is conducted with the aid of Version 7 of SIMION 3D ray-tracing software.The beam dependence on various parameters of the extraction systems is studied and the numerical results lead to qualitative conclusions.Ion beam characteristics using diode and triode extraction systems are investigated with the aid of the computer code SIMION 3 D,Version 7.0. The diode (two electrode extraction system) and triode (threeelectrode extraction,acceleration-deceleration system) extraction systems are designed and optimized with different geometric parameters of the electrode system,voltage applied to the extraction electrode,and plasma parameters inside the ion source chamber,as well as by the ion beam space charge.This work attempts to describe the importance of the acceleration-deceleration extraction system.It shows that besides an increase of the beam energy,the ion beam has lower emittance than the two-electrode extraction system.Ion beams of the highest quality are extracted whenever the half-angular divergence is minimum for which the perveance current intensity and the extraction gap have optimum value.Knowing the electron temperature of the plasma is necessary to determine plasma potential and the exact beam energy.

  10. Review on aggregation of acid extractants in solvent extraction of metal ions: remark on the general model

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    The aggregation behavior of various acid extractants in the solvent extraction systems of metal ions is re-examined and explained according to knowledge obtained in recent work. The conclusions are as follows. (1) Complexes formed by the extractants and metal ions can form reversed micelles in organic diluents, depending on the microstructures of the complexes. The dimers of the acid extractant cannot percolate to the metal-extractant aggregates, and the acid-salt complexes are always formed in the aggregates. The reversed micelles or the W/O microemulsions formed by different species cannot be associated with each other to form a unified aggregate. (2) In solvent extraction systems, hydration of the extractants and metal ions can be considered as the driving force of forming reversed micelles. (3) Information of the first approach to the insight of the bicontinuous microemulsion of NaDEHP shows that various components in the aqueous phase behave confined and very similar to the typical AOT/n-heptane W/O microemulsions. (4) In the extraction of lanthanide ions by the W/O microemulsion of sodium naphthenate, the saponification is a process of forming reversed micelle or W/O microemulsion, while the extraction step is a process of destroying reversed micelles or W/O microemulsion droplets.

  11. Self-consistent multicomponent plasma sheath theory for the extraction of H- ions (invited)

    Science.gov (United States)

    Becker, Reinard

    2004-05-01

    A self-consistent one-dimensional plasma sheath theory is presented to provide the basis for a correct numerical simulation of the extraction of volume produced H- ions. The plasma may consist not only of electrons and H- ions, but may also contain other positive ions such as protons, molecular ions and those of heavier elements, like cesium or tantalum. For the transition from the classical plasma sheath with a falling potential to the extraction region for H- ions with an increasing potential there exists the problem of a saddle point with adverse optical properties. This is eliminated by requiring sufficient space charge of H- ions near the extraction electrode. The formation of a virtual cathode in the extraction region by reflected positive ions is also taken into account. The integration of the Poisson equation in the extraction region establishes a criterion to avoid the creation of a nonphysical periodical sequence of potential maximums and minima. This criterion is an antithesis to the Bohm sheath criterion and has a corresponding interpretation: a virtual cathode in the extraction region can only be avoided, if the space charge of positive ions rapidly decreases. The acceptable range of parameters is thus reduced considerably. The resulting axial potential function is then used to derive the shape of the plasma wall electrode in the vicinity of the ion beam edge in order to obtain an aberration free beam boundary, this information being equivalent to the Pierce angle in the case of solid electron or ion emitters.

  12. Observation of burst frequency in extracted ECR ion current

    NARCIS (Netherlands)

    Taki, G. S.; Sarma, P. R.; Drentje, A. G.; Nakagawa, T.; Ray, P. K.; Bhandari, R. K.

    2007-01-01

    Earlier we reported an ion current jump which was observed at a fixed negative biased disc potential in the 6.4GHz ECR ion source at VECC, Kolkata. In a recent experiment with neon ions, we measured the time spectra of the ion current and observed the presence of a burst frequency in the kilohertz r

  13. Design of triode extraction system for a dual hollow cathode ion source

    Institute of Scientific and Technical Information of China (English)

    WANG Jing-Hui; ZHU Kun; ZHAO Wei-Jiang; LIU Ke-Xin

    2011-01-01

    A triode extraction system is designed for a dual hollow cathode ion source being developed at the Institute of Heavy Ion Physics,Peking University.Basic parameters of the plasma are selected after examining the operation principle of the ion source,then the triode extraction system is designed and optimized by using software PBGUNS (for Particle Beam GUN Simulations).The physical design of the system is given in this paper.

  14. Liquid-liquid extraction of metal ions by the 6-membered N-containing macrocycle hexacyclen.

    Science.gov (United States)

    Arpadjan, S; Mitewa, M; Bontchev, P R

    1987-11-01

    The nitrogen-containing analogue of 18-crown-6, 1,4,7,10,13,16-hexa-azaoctadecane (hexacyclen)] was studied as a reagent for complexation and extraction of some metal ions. It was found that with this reagent and methyl isobutyl ketone, metal ions such as silver(I), mercury(II), copper(II), platinum(II) and palladium(II) can be quantitatively extracted and separated from iron(III) and some other metal ions.

  15. Characterization of selenium species in biological extracts by enhanced ion-pair liquid chromatography with inductively coupled plasma-mass spectrometry and by referenced electrospray ionization-mass spectrometry

    Science.gov (United States)

    Kotrebai, Mihály; Bird, Susan M.; Tyson, Julian F.; Block, Eric; Uden, Peter C.

    1999-11-01

    Selenium is an essential nutrient for humans; selenium compounds catalyze intermediate metabolism reactions and inhibit the toxic effects of heavy metals such as arsenic, cadmium and mercury. Some extracts of selenium-enriched biological materials show cancer preventive effects, tentatively attributable to the biological functions of selenoamino acids. An improved ion pair chromatographic method with methodological enhancements for the separation, qualitative and quantitative determination of non-volatile selenium compounds extracted from different samples has been developed using ICP-MS as an element-selective detector. Separation power early in the chromatogram was increased to baseline separation in the standard mixture as a result of decreasing spray chamber size from 97 to 14 ml, and increasing trifluoracetic acid (TFA) concentration in the mobile phase from 0.1 to 0.6%. The former pH was restored by the addition of ammonia to the mobile phase, which also served to increase the column recovery of inorganic anions. Calibration curves for different selenoamino acids showed statistically different behavior. Biological sample extracts were characterized using HPLC-ICP-MS. Mass spectral behavior of selenoamino acids, using electrospray and ion trap technology with direct infusion and liquid chromatographic sample introduction, is also reported.

  16. Effective Extraction Mechanism of Volume-Produced Ions in the NIPPER I Device

    Directory of Open Access Journals (Sweden)

    Henry Ramos

    1993-12-01

    Full Text Available A mass spectrometer system is developed to extract and analyze hydrogen ions from a volume plasma hydrogen ion source. A 180° magnetic deflection-type mass analyzer is coupled to NIPPER I (National Institute of Physics Plasma Experimental Rig I, a negative ion source. Hydrogen plasma is produced from a low pressure gas (10-2 Torr with a transition of the glow discharge (254 volts, 75 mA to an arc plasma (78 volts, 14 amperes in a few seconds. The usually cylindrical plasma is converted into a sheet configuration using a pair of Sm-Co magnets. This optimizes ion current extraction by reducing (a the ion loss to the discharge anode and (b the decay of the ion current produced in the plasma. Negative hydrogen ions (H- are volume-produced by dissociative attachment of low energy electrons to highly vibrational excited hydrogen molecules.The extraction of H- ions from this volume source is optimized by the proper choice of apertures of the limiting electrodes and of the applied bias potential. A proper combination of extraction electrodes gives an optimum H- current extracted without the electrons. When one of the extraction electrodes is biased negatively near the value of the plasma floating potential, a maximum H- current is also obtained. The methods of effective extraction of H- are discussed.

  17. Solvent extraction, ion chromatography, and mass spectrometry of molybdenum isotopes.

    Science.gov (United States)

    Dauphas, N; Reisberg, L; Marty, B

    2001-06-01

    A procedure was developed that allows precise determination of molybdenum isotope abundances in natural samples. Purification of molybdenum was first achieved by solvent extraction using di(2-ethylhexyl) phosphate. Further separation of molybdenum from isobar nuclides was obtained by ion chromatography using AG1-X8 strongly basic anion exchanger. Finally, molybdenum isotopic composition was measured using a multiple collector inductively coupled plasma hexapole mass spectrometer. The abundances of molybdenum isotopes 92, 94, 95, 96, 97, 98, and 100 are 14.8428(510), 9.2498(157), 15.9303(133), 16.6787(37), 9.5534(83), 24.1346(394), and 9.6104(312) respectively, resulting in an atomic mass of 95.9304(45). After internal normalization for mass fractionation, no variation of the molybdenum isotopic composition is observed among terrestrial samples within a relative precision on the order of 0.00001-0.0001. This demonstrates the reliability of the method, which can be applied to searching for possible isotopic anomalies and mass fractionation.

  18. Advanced light ion source extraction system for a new electron cyclotron resonance ion source geometry at Saclay.

    Science.gov (United States)

    Delferrière, O; Gobin, R; Harrault, F; Nyckees, S; Sauce, Y; Tuske, O

    2012-02-01

    One of the main goal of intense light ion injector projects such as IPHI, IFMIF, or SPIRAL2, is to produce high current beams while keeping transverse emittance as low as possible. To prevent emittance growth induced in a dual solenoid low energy transfer line, its length has to be minimized. This can be performed with the advanced light ion source extraction system concept that we are developing: a new ECR 2.45 GHz type ion source based on the use of an additional low energy beam transport (LEBT) short length solenoid close to the extraction aperture to create the resonance in the plasma chamber. The geometry of the source has been considerably modified to allow easy maintenance of each component and to save space in front of the extraction. The source aims to be very flexible and to be able to extract high current ion beams at energy up to 100 kV. A specific experimental setup for this source is under installation on the BETSI test bench, to compare its performances with sources developed up to now in the laboratory, such as SILHI, IFMIF, or SPIRAL2 ECR sources. This original extraction source concept is presented, as well as electromagnetic simulations with OPERA-2D code. Ion beam extraction in space charge compensation regime with AXCEL, and beam dynamics simulation with SOLMAXP codes show the beam quality improvement at the end of the LEBT.

  19. Advanced light ion source extraction system for a new electron cyclotron resonance ion source geometry at Saclaya)

    Science.gov (United States)

    Delferrière, O.; Gobin, R.; Harrault, F.; Nyckees, S.; Sauce, Y.; Tuske, O.

    2012-02-01

    One of the main goal of intense light ion injector projects such as IPHI, IFMIF, or SPIRAL2, is to produce high current beams while keeping transverse emittance as low as possible. To prevent emittance growth induced in a dual solenoid low energy transfer line, its length has to be minimized. This can be performed with the advanced light ion source extraction system concept that we are developing: a new ECR 2.45 GHz type ion source based on the use of an additional low energy beam transport (LEBT) short length solenoid close to the extraction aperture to create the resonance in the plasma chamber. The geometry of the source has been considerably modified to allow easy maintenance of each component and to save space in front of the extraction. The source aims to be very flexible and to be able to extract high current ion beams at energy up to 100 kV. A specific experimental setup for this source is under installation on the BETSI test bench, to compare its performances with sources developed up to now in the laboratory, such as SILHI, IFMIF, or SPIRAL2 ECR sources. This original extraction source concept is presented, as well as electromagnetic simulations with OPERA-2D code. Ion beam extraction in space charge compensation regime with AXCEL, and beam dynamics simulation with SOLMAXP codes show the beam quality improvement at the end of the LEBT.

  20. Simulation of H{sup -} ion source extraction systems for the Spallation Neutron Source with Ion Beam Simulator

    Energy Technology Data Exchange (ETDEWEB)

    Kalvas, T.; Tarvainen, O. [Department of Physics, University of Jyvaeskylae, Jyvaeskylae (Finland); Welton, R. F.; Han, B. X.; Stockli, M. P. [Spallation Neutron Source, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

    2012-02-15

    A three-dimensional ion optical code IBSimu, which is being developed at University of Jyvaeskylae, features positive and negative ion plasma extraction models and self-consistent space charge calculation. The code has been utilized for modeling the existing extraction system of the H{sup -} ion source of the Spallation Neutron Source. Simulation results are in good agreement with experimental data. A high-current extraction system with downstream electron dumping at intermediate energy has been designed. According to the simulations it provides lower emittance compared to the baseline system at H{sup -} currents exceeding 40 mA. A magnetic low energy beam transport section consisting of two solenoids has been designed to transport the beam from the alternative electrostatic extraction systems to the radio frequency quadrupole.

  1. solid phase extraction of trace amounts of palladium ions using ...

    African Journals Online (AJOL)

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    hydroxybenzylidene)- ... applied to the determination of palladium ion in environmental samples. KEY WORDS: ... preparation tool and provides a method that is simple and safe to use. .... and recovery of ions was investigated under optimum conditions.

  2. Fingerprint chromatogram analysis of Pseudostellaria heterophylla (Miq.) Pax root by high performance liquid chromatography.

    Science.gov (United States)

    Han, Chao; Chen, Junhui; Chen, Bo; Lee, Frank Sen-Chun; Wang, Xiaoru

    2006-09-01

    A simple and reliable high performance liquid chromatographic (HPLC) method has been developed and validated for the fingerprinting of extracts from the root of Pseudostellaria heterophylla (Miq.) Pax. HPLC with gradient elution was performed on an authentic reference standard of powdered P. heterophylla (Miq.) Pax root and 11 plant samples of the root were collected from different geographic locations. The HPLC chromatograms have been standardized through the selection and identification of reference peaks and the normalization of retention times and peak intensities of all the common peaks. The standardized HPLC fingerprints show high stability and reproducibility, and thus can be used effectively for the screening analysis or quality assessment of the root or its derived products. Similarity index calculations based on cosine angle values or correlation methods have been performed on the HPLC fingerprints. As a group, the fingerprints of the P. heterophylla (Miq.) Pax samples studied are highly correlated with closely similar fingerprints. Within the group, the samples can be further divided into subgroups based on hierarchical clustering analysis (HCA). Sample grouping based on HCA coincides nicely with those based on the geographical origins of the samples. The HPLC fingerprinting techniques thus have high potential in authentication or source-tracing types of applications.

  3. Synchronized Analysis of FTIR Spectra and GCMS Chromatograms for Evaluation of the Thermally Degraded Vegetable Oils

    Science.gov (United States)

    Mohd Irwan Lu, Nurul Aida Lu; Samling, Benedict

    2014-01-01

    Fourier Transform Infrared (FTIR) and Gas Chromatography Mass Spectrometry (GCMS) are two common instruments used for analysis of edible oils. The output signal is often analysed on the software attached to the workstations. The processing software is usually individualised for a specific source. The output of GCMS cannot be analysed on the FTIR hence analysts often need to juggle between instruments when multiple techniques are employed. This could become exhaustive when a large dataset is involved. This paper reports a synchronised approach for analysis of signal from FTIR and GCMS. The algorithm is demonstrated on a dataset of edible oils to investigate the thermal degradation of seven types of edible oils treated at 100°C and 150°C. The synchronised routines identify peaks present in FTIR and GCMS spectra/chromatograms where the information is subsequently extracted onto peak tables for further analysis. In this study, it is found that palm based products and corn oils were relatively more stable with higher content of antioxidants tocopherols and squalene. As a conclusion, this approach allows simultaneous analysis of signal from multiple sources and samples enhancing the efficiency of the signal processing process. PMID:24563804

  4. An RF-only ion-funnel for extraction from high-pressure gases

    CERN Document Server

    Brunner, Thomas; Varentsov, Victor; Sabourov, Amanda; Gratta, Giorgio; Dilling, Jens; DeVoe, Ralph; Sinclair, David; Fairbank, William; Albert, Joshua B; Auty, David J; Barbeau, Phil S; Beck, Douglas; Benitez-Medina, Cesar; Breidenbach, Martin; Cao, Guofu F; Chambers, Christopher; Cleveland, Bruce; Coon, Matthew; Craycraft, Adam; Daniels, Timothy; Daugherty, Sean J; Didberidze, Tamar; Dolinski, Michelle J; Dunford, Matthew; Fabris, Lorenzo; Farine, Jacques; Feldmeier, Wolfhart; Fierlinger, Peter; Gornea, Razvan; Graham, Kevin; Heffner, Mike; Hughes, Mitchell; Jewell, Michael; Jiang, Xiaoshan S; Johnson, Tessa N; Johnston, Sereres; Karelin, Alexander; Kaufman, Lisa J; Killick, Ryan; Koffas, Thomas; Kravitz, Scott; Kruecken, Reiner; Kuchenkov, Alexey; Kumar, Krishna S; Leonard, Douglas S; Leonard, Francois; Licciardi, Caio; Lin, Yi-Hsuan H; Ling, Jiajie; MacLellan, Ryan; Marino, Michael G; Mong, Brian; Moore, David; Odian, Allen; Ostrovskiy, Igor; Ouellet, Christian; Piepke, Andreas; Pocar, Andrea; Retiere, Fabrice; Rowson, Peter C; Rozo, Maria P; Schubert, Alexis; Smith, Erica; Stekhanov, Victor; Tarka, Michal; Tolba, Tamer; Tosi, Delia; Twelker, Karl; Vuilleumier, Jean-Luc L; Walton, Josiah; Walton, Timothy; Weber, Manuel; Wen, Liangjian J; Wichoski, Ubi; Yang, Liang; Yen, Yung-Ruey

    2014-01-01

    An RF ion-funnel technique has been developed to extract ions from a high-pressure (10 bar) noble-gas environment into vacuum ($10^{-6}$ mbar). Detailed simulations have been performed and a prototype has been developed for the purpose of extracting $^{136}$Ba ions from Xe gas with high efficiency. With this prototype, ions have been extracted for the first time from high-pressure xenon gas and argon gas. Systematic studies have been carried out and compared to the simulations. This demonstration of extraction of ions with mass comparable to that of the gas generating the high-pressure into vacuum has applications to Ba tagging from a Xe-gas time-projection chamber (TPC) for double beta decay as well as to the general problem of recovering trace amounts of an ionized element in a heavy (m$>40$ u) carrier gas.

  5. Simulation of the CERN GTS-LHC ECR ion source extraction system with lead and argon ion beams

    CERN Document Server

    Toivanen, V; Küchler, D; Lombardi, A; Scrivens, R; Stafford-Haworth, J

    2014-01-01

    A comprehensive study of beam formation and beam transport has been initiated in order to improve the performance of the CERN heavy ion injector, Linac3. As part of this study, the ion beam extraction system of the CERN GTS-LHC 14.5 GHz Electron Cyclotron Resonance Ion Source (ECRIS) has been modelled with the ion optical code IBSimu. The simulations predict self-consistently the triangular and hollow beam structures which are often observed experimentally with ECRIS ion beams. The model is used to investigate the performance of the current extraction system and provides a basis for possible future improvements. In addition, the extraction simulation provides a more realistic representation of the initial beam properties for the beam transport simulations, which aim to identify the performance bottle necks along the Linac3 low energy beam transport. The results of beam extraction simulations with Pb and Ar ion beams from the GTS-LHC will be presented and compared with experimental observations.

  6. In situ analysis of the Martian soil by gas chromatography: decoding of complex chromatograms of organic molecules of exobiological interest.

    Science.gov (United States)

    Pietrogrande, M C; Zampolli, M G; Dondi, F; Szopa, C; Sternberg, R; Buch, A; Raulin, F

    2005-04-15

    Gas chromatography-mass spectrometry (GC-MS) will be used in future space exploration missions, in order to seek organic molecules at the surface of Mars, and especially potential chemical indicators of life. Carboxylic acids are among the most expected organic species at the surface of Mars, and they could be numerous in the analysed samples. For this reason, a chemometric method was applied to support the interpretation of chromatograms of carboxylic acid mixtures. The method is based on AutoCovariance Function (ACVF) in order to extract information on the sample--number and chemical structure of the components--and on separation performance. The procedure was applied to standard samples containing targeted compounds which are among the most expected to be present in the Martian soil: n-alkanoic and benzene dicarboxylic acids. ACVF was computed on the obtained chromatograms and plotted versus retention time: peaks of the ACVF plot can be related to specific molecular structures and are diagnostic for chemical identification of compounds.

  7. On the meniscus formation and the negative hydrogen ion extraction from ITER neutral beam injection relevant ion source

    Science.gov (United States)

    Mochalskyy, S.; Wünderlich, D.; Ruf, B.; Fantz, U.; Franzen, P.; Minea, T.

    2014-10-01

    The development of a large area (Asource,ITER = 0.9 × 2 m2) hydrogen negative ion (NI) source constitutes a crucial step in construction of the neutral beam injectors of the international fusion reactor ITER. To understand the plasma behaviour in the boundary layer close to the extraction system the 3D PIC MCC code ONIX is exploited. Direct cross checked analysis of the simulation and experimental results from the ITER-relevant BATMAN source testbed with a smaller area (Asource,BATMAN ≈ 0.32 × 0.59 m2) has been conducted for a low perveance beam, but for a full set of plasma parameters available. ONIX has been partially benchmarked by comparison to the results obtained using the commercial particle tracing code for positive ion extraction KOBRA3D. Very good agreement has been found in terms of meniscus position and its shape for simulations of different plasma densities. The influence of the initial plasma composition on the final meniscus structure was then investigated for NIs. As expected from the Child-Langmuir law, the results show that not only does the extraction potential play a crucial role on the meniscus formation, but also the initial plasma density and its electronegativity. For the given parameters, the calculated meniscus locates a few mm downstream of the plasma grid aperture provoking a direct NI extraction. Most of the surface produced NIs do not reach the plasma bulk, but move directly towards the extraction grid guided by the extraction field. Even for artificially increased electronegativity of the bulk plasma the extracted NI current from this region is low. This observation indicates a high relevance of the direct NI extraction. These calculations show that the extracted NI current from the bulk region is low even if a complete ion-ion plasma is assumed, meaning that direct extraction from surface produced ions should be present in order to obtain sufficiently high extracted NI current density. The calculated extracted currents, both ions

  8. Screening of Indian aphrodisiac ayurvedic/herbal healthcare products for adulteration with sildenafil, tadalafil and/or vardenafil using LC/PDA and extracted ion LC-MS/TOF.

    Science.gov (United States)

    Savaliya, Akash A; Shah, Ravi P; Prasad, Bhagwat; Singh, Saranjit

    2010-07-08

    Ayurvedic/herbal healthcare products are considered safe under the impression that they are derived from natural products. But recently, there have been several reports worldwide on the adulteration of synthetic PDE-5 inhibitors in aphrodisiac herbal formulations. Therefore, the objective of the present study was to explore the presence of synthetic PDE-5 inhibitors (sildenafil, tadalafil and/or vardenafil) in ayurvedic/herbal healthcare products sold in Indian market for aphrodisiac/related uses. In total, 85 herbal formulations (HFs) were included in the study. The formulations were extracted with methanol and subjected to centrifugation. The supernatant was analysed by HPLC and LC-MS/TOF. Early detection of the presence of sildenafil, tadalafil and vardenafil in the herbal samples was done by the study of extracted ion mass chromatograms at the m/z values of respective parent ions, and two prominent fragments of each. In case of sildenafil and tadalafil, adulteration was also detected by comparing the relative retention times (RR(T)) and UV spectra. Further substantiation was done through comparison of accurate mass spectra with those of the two available standards. Of the 85 HFs tested, only one was eventually found to be adulterated with sildenafil. The extent of adulterant in this sample was determined to the therapeutic dose in the formulation. The study thus indicates emergence of the problem of adulteration of Indian herbal products with PDE-5 inhibitors.

  9. Method for Continuous Monitoring of Electrospray Ion Formation

    Science.gov (United States)

    Metzler, Guille; Crathern, Susan; Bachmann, Lorin; Fernández-Metzler, Carmen; King, Richard

    2017-10-01

    A method for continuously monitoring the performance of electrospray ionization without the addition of hardware or chemistry to the system is demonstrated. In the method, which we refer to as SprayDx, cluster ions with solvent vapor natively formed by electrospray are followed throughout the collection of liquid chromatography-selected reaction monitoring data. The cluster ion extracted ion chromatograms report on the consistency of the ion formation and detection system. The data collected by the SprayDx method resemble the data collected for postcolumn infusion of analyte. The response of the cluster ions monitored reports on changes in the physical parameters of the ion source such as voltage and gas flow. SprayDx is also observed to report on ion suppression in a fashion very similar to a postcolumn infusion of analyte. We anticipate the method finding utility as a continuous readout on the performance of electrospray and other atmospheric pressure ionization processes. [Figure not available: see fulltext.

  10. Preliminary Simulation of Beam Extraction for the 28 GHz ECR Ion Source

    CERN Document Server

    Park, Bum-Sik; Choi, Seokjin

    2015-01-01

    The 28 GHz ECR(Electron Cyclotron Resonance) ion source is under development to supply various beams from proton to uranium at RISP(Rare Isotope Science Project). The superconducting magnet system for a 28 GHz ECR ion source consists of four solenoid coils and a saddle type sextupole. To meet the design requirement of ECR ion source, a numerical simulation was accomplished by using the KOBRA3-INP to optimize the extraction system which is the three dimensional ion optics code. The influence of the three dimensional magnetic field and the space charge effect was considered to extract the highly charged ion beam. In this paper, the design results of the extraction system were reported in detail.

  11. Transport and extraction of radioactive ions stopped in superfluid helium

    NARCIS (Netherlands)

    Huang, WX; Dendooven, P; Gloos, K; Takahashi, N; Arutyunov, K; Pekola, JP; Aysto, J

    2003-01-01

    A new approach to convert a high energy beam to a low energy one, which is essential for the next generation radioactive ion beam facilities, has been proposed and tested at Jyvaskyla, Finland. An open Ra-223 alpha-decay-recoil source has been used to produce radioactive ions in superfluid helium. T

  12. Identification of Trichoderma strains by image analysis of HPLC chromatograms

    DEFF Research Database (Denmark)

    Thrane, Ulf; Poulsen, S.B.; Nirenberg, H.I.

    2001-01-01

    Forty-four Trichoderma strains from water-damaged building materials or indoor dust were classified with chromatographic image analysis on full chromatographic matrices obtained by high performance liquid chromatography with UV detection of culture extracts. The classes were compared with morphol...

  13. Metal Ions Extraction with Glucose Derivatives as Chelating Reagents in Supercritical Carbon Dioxide

    Institute of Scientific and Technical Information of China (English)

    Guo Chen YANG; Hai Jian YANG

    2006-01-01

    A series of glucose derivatives have been used as chelating reagents to extract metal ions in supercritical carbon dioxide. With perfluoro-1-octanesulfonic acid tetraethylammonium salt as additive, glucose derivatives were selective for Sr2+ and Pb2+ extraction in supercritical carbon dioxide.

  14. Conceptual design of first toroidal electron cyclotron resonance ion source and modeling of ion extraction from it

    CERN Document Server

    Caliri, C; Volpe, F A

    2015-01-01

    Electron Cyclotron Resonance Ion Sources (ECRIS) progressed to higher and higher ion currents and charge states by adopting stronger magnetic fields (beneficial for confinement) and proportionally higher ECR frequencies. Further improvements would require the attainment of "triple products" of density, temperature and confinement time comparable with major fusion experiments. For this, we propose a new, toroidal rather than linear, ECRIS geometry, which would at the same time improve confinement and make better use of the magnetic field. Ion extraction is more complicated than from a linear device, but feasible, as our modelling suggests: single-particle tracings showed successful extraction by at least two techniques, making use respectively of a magnetic extractor and of ExB drifts. Additional techniques are briefly discussed.

  15. Empirical laws of particle extraction from single-grid source of bipolar ion-electron flow

    Energy Technology Data Exchange (ETDEWEB)

    Dudin, S. V. [Department of Physics and Technology, V.N. Karazin Kharkiv National University, Kurchatova Ave. 31, 61108 Kharkiv (Ukraine); Scientific Center of Physical Technologies, Svobody sq. 6, 61022 Kharkiv (Ukraine); Rafalskyi, D. V. [Scientific Center of Physical Technologies, Svobody sq. 6, 61022 Kharkiv (Ukraine)

    2012-11-15

    The present research is devoted to the problem of extraction grid choice for a single-grid source of bipolar ion-electron flow. The paper contains detailed reference information on ion and electron extraction characteristics of 10 different grids with broad range of parameters: aperture width (0.09-0.6 mm), grid transparency (0.19-0.51), thickness (0.036-0.5 mm), and with different aperture geometry. The grids with square, circular, and slit apertures were made with different technologies: laser cutting, welding, weaving, and electrolytic erosion. The general regularities of the ion and electron extraction from the single-grid source are experimentally researched for the cases of dc and RF extraction grid biasing. A conclusion has been made that the maximum extracted ion current at low ion energy (0-200 eV) does not significantly vary for all the grids and does not exceed half of the primary ion current from plasma multiplied by the optical grid transparency. The low-energy limit of efficient ion extraction has been discovered which cannot be overcome by the aperture narrowing. A conclusion is made that the RF extraction mode is superior for all the researched grids since it is characterized by higher extracted ion current at any acceleration voltage for any grid with much more simple and smooth extraction curves behavior in comparison to the dc case as well as absence of arcing, jumps, and hysteresis of the measured curves at any RF voltages. The unique ability of the RF biased single-grid source of simultaneous ion/electron emission has been studied. The measured maximal attainable ion beam current compensation ratio is always sufficiently higher than 1 and typically varies in the range 2-6. The results obtained in the present paper demonstrate prospective of the single-grid source in space thruster applications and in modern technologies, particularly for ion beam processing of wide bandgap semiconductor devices such as GaN and SiC transistors due to inherent

  16. POLY(AMINOMETHYLENEPHOSPHONIC ACID FOR SOLVENT EXTRACTION OF METAL IONS

    Directory of Open Access Journals (Sweden)

    M’hamed Kaid

    2011-09-01

    Full Text Available Diaminododecyltetramethylenetetraphosphonic acid (DADTMTPA has been investigated in liquid - liquid extraction of Zn (II and Cu (II in acetate media. The extraction of both cations was carried out in different media with the addition of CH3COONa, CH3COOH, HCl and H2SO4 at different pH values. The maximum extraction yield for copper is 70% after addition of 10 mg of sodium acetate and for zinc is 30% after addition of acetic acid at pHi = 5.5, in one step.

  17. Actinide ion extraction using room temperature ionic liquids: opportunities and challenges for nuclear fuel cycle applications.

    Science.gov (United States)

    Mohapatra, Prasanta Kumar

    2017-02-14

    Studies on the extraction of actinide ions from radioactive feeds have great relevance in nuclear fuel cycle activities, mainly in the back end processes focused on reprocessing and waste management. Room temperature ionic liquid (RTIL) based diluents are becoming increasingly popular due to factors such as more efficient extraction vis-à-vis molecular diluents, higher metal loading, higher radiation resistance, etc. The fascinating chemistry of the actinide ions in RTIL based solvent systems due to complex extraction mechanisms makes it a challenging area of research. By the suitable tuning of the cationic and anionic parts of the ionic liquids, their physical properties such as density, dielectric constant and viscosity can be changed which are considered key parameters in metal ion extraction. Aqueous solubility of the RTILs, which can lead to significant loss in the solvent inventory, can be avoided by appending the extractant moieties onto the ionic liquid. While the low vapour pressure and non-flammability of the ionic liquids make them appear as 'green' diluents, their aqueous solubility raises concerns of environmental hazards. The present article gives a summary of studies carried out on actinide ion extraction and presents perspectives of its applications in the nuclear fuel cycle. The article discusses various extractants used for actinide ion extraction and at many places, comparison is made vis-à-vis molecular diluents which includes the nature of the extracted species and the mechanism of extraction. Results of studies on rare earth elements are also included in view of their similarities with the trivalent minor actinides.

  18. Aqueous extraction of anions from coal and fly ash followed by ion-chromatographic determination

    Directory of Open Access Journals (Sweden)

    Tasić Aleksandra M.

    2016-01-01

    Full Text Available Three different techniques were applied for the aqueous extraction of anions from coal and fly ash: rotary mixer- and ultrasonic-assisted extraction with different duration time, and microwave-assisted extraction at different temperatures. Validation showed that the ion-chromatographic method was suitable for the analysis of anions in coal and fly ash extracts. The variations in the amounts of anions using different extraction times during rotary-assisted extraction were minimal for all investigated anions. The efficiency of ultrasound-assisted extraction of anions from coal depended on the sonication time and was highest at 30 min. The ultrasound-assisted extraction was less efficient for the extraction of anions from fly ash than rotary-assisted extraction. Increase of temperature in the microwave-assisted extraction had a positive effect on the amounts of all anions extracted from coal and sulphate from fly ash, while the amounts of fluoride and chloride in fly ash extracts decreased. The microwave-assisted extraction of coal at 150°C was compared with standard ASTM methods, and results were in good agreement only for chloride. Changes in the pH value and conductivity during ultrasound-assisted extraction were measured in order to explain changes on the surface of coal particles in contact with water and different processes that occur under environmental conditions. [Projekat Ministarstva nauke Republike Srbije, br. 172030, br. 176006 i br. III43009

  19. An improved transmutation method for quantitative determination of the components in multicomponent overlapping chromatograms.

    Science.gov (United States)

    Shao, Xueguang; Yu, Zhengliang; Ma, Chaoxiong

    2004-06-01

    An improved method is proposed for the quantitative determination of multicomponent overlapping chromatograms based on a known transmutation method. To overcome the main limitation of the transmutation method caused by the oscillation generated in the transmutation process, two techniques--wavelet transform smoothing and the cubic spline interpolation for reducing data points--were adopted, and a new criterion was also developed. By using the proposed algorithm, the oscillation can be suppressed effectively, and quantitative determination of the components in both the simulated and experimental overlapping chromatograms is successfully obtained.

  20. Identification of Trichoderma strains by image analysis of HPLC chromatograms

    DEFF Research Database (Denmark)

    Thrane, Ulf; Poulsen, S.B.; Nirenberg, H.I.

    2001-01-01

    Forty-four Trichoderma strains from water-damaged building materials or indoor dust were classified with chromatographic image analysis on full chromatographic matrices obtained by high performance liquid chromatography with UV detection of culture extracts. The classes were compared with morphol......Forty-four Trichoderma strains from water-damaged building materials or indoor dust were classified with chromatographic image analysis on full chromatographic matrices obtained by high performance liquid chromatography with UV detection of culture extracts. The classes were compared...... with morphological identification and rDNA sequence data, and for each class all strains were of the same identity. With all three techniques each strain - except one - was identified as the same species. These strains belonged to Trichoderma atroviride (nine strains), Trichoderma viride (three strains), Trichoderma...... harzianum (10 strains), Trichoderma citrinoviride (12 strains), and Trichoderma longibrachiatum (nine strains). The odd strain was identified as Trichoderma hamatum by morphology and rDNA sequencing. but not by image analysis as no reference strains of this species were included. It is concluded...

  1. Surface ion-imprinted amino-functionalized cellulosic cotton fibers for selective extraction of Cu(II) ions.

    Science.gov (United States)

    Monier, M; Ibrahim, Amr A; Metwally, M M; Badawy, D S

    2015-11-01

    Surface ion-imprinted amino-functionalized cellulosic fibers (Cu-ABZ) were manufactured for efficient selective adsorption of Cu(2+) ions. The chemical modification steps had been characterized utilizing elemental analysis; Fourier transforms infrared (FTIR) along with wide angle X-ray diffraction (XRD) spectroscopy. Also, the morphological structure of the ion-imprinted and the non-imprinted (NI-ABZ) fibers were visualized and compared with that of the native cotton fibers using scanning electron microscope (SEM). In addition, the coordination mode by which the Cu(2+) ions bonded to the active sites were examined by both FTIR and X-ray photo electron spectra (XPS). Both Cu-ABZ and NI-ABZ were implemented in batch experiments for optimizing the conditions by which the Cu(2+) ions can be selectively removal from aqueous medium and pH 5 was the optimum for the metal ion extraction. Moreover, the kinetics and isotherm studies revealed that the adsorption data fitted with pseudo-second-order kinetic and Langmuir models with estimated maximum adsorption capacity 93.6mg/g. Also, the reusability studies indicated that the prepared ion-imprinted adsorbent maintains more than 95% of its original activity after fifth generation cycle.

  2. Extraction of alginate biopolymer present in marine alga sargassum filipendula and bioadsorption of metallic ions

    Directory of Open Access Journals (Sweden)

    Sirlei Jaiana Kleinübing

    2013-04-01

    Full Text Available This paper studies the bioadsorption of Pb2+, Cu2+, Cd2+ and Zn2+ ions by marine alga Sargassum filipendula and by the alginate biopolymer extracted from this alga. The objective is to evaluate the importance of this biopolymer in removing different metallic ions by the marine alga S. filipendula. In the equilibrium study, the same affinity order was observed for both bioadsorbents: Pb2+ > Cu2+ > Zn2+ > Cd2+. For Pb2+ and Cu2+ ions when the alginate is isolated and acting as bioadsorbents, adsorption capacities greater than those found for the alga were observed, indicating that it is the main component responsible for the removal of metallic ions. For Zn2+ and Cd2+ ions, greater bioadsorption capacities were observed for the alga, indicating that other functional groups of the alga, such as sulfates and amino, are also important in the bioadsorption of these ions.

  3. STUDIES ON INOSINE EXTRACTION BY ION EXCHANGE METHOD

    Institute of Scientific and Technical Information of China (English)

    HuangXiwen; ShiFang; 等

    1998-01-01

    The adsorption characteristics of inosine from fermentation solution on anion exchange resin under the condition of different pH,resin type are investigated.Besides,the desorption conditions are studied under different temperature.The adsorption and desorption mechanism are described to obtain the optimum technological condition of inosine extraction.

  4. Automated multivariate analysis of comprehensive two-dimensional gas chromatograms of petroleum

    DEFF Research Database (Denmark)

    Skov, Søren Furbo

    of separated compounds makes the analysis of GCGC chromatograms tricky, as there are too much data for manual analysis , and automated analysis is not always trouble-free: Manual checking of the results is often necessary. In this work, I will investigate the possibility of another approach to analysis of GCGC...

  5. Uniform H(-) ion beam extraction in a large negative ion source with a tent-shaped magnetic filter.

    Science.gov (United States)

    Tobari, H; Hanada, M; Kashiwagi, M; Taniguchi, M; Umeda, N; Watanabe, K; Inoue, T; Sakamoto, K; Takado, N

    2008-02-01

    Based on previous studies on the spatial uniformity of the negative ion beam, the external magnetic filter was replaced to a novel tent-shaped magnetic filter in the JAEA 10 A negative ion source. The line-cusp field configuration on the source chamber was also changed to form a symmetric magnetic field like many of positive ion sources aiming at high proton yield. This magnetic field configuration allows fast electrons emitted from filament cathodes to rotate azimuthally inside the source chamber. The source configuration thus prevents localization of fast electrons due to their B x grad B drift in the filter field. As a result, the H(-) ion beam profile extracted from a wide region of 340 x 170 mm(2) showed reduction of standard deviation from 16% in the original to 7.9% with the tent filter. The negative ion source with the tent filter satisfied the requirement of the beam uniformity for a large negative ion source in the ITER neutral beam injection.

  6. Double einzel lens extraction for the JYFL 14 GHz ECR ion source designed with IBSimu

    Science.gov (United States)

    Toivanen, V.; Kalvas, T.; Koivisto, H.; Komppula, J.; Tarvainen, O.

    2013-05-01

    In order to improve the performance of the JYFL 14 GHz electron cyclotron resonance ion source (ECRIS) and initiate low energy beam transport (LEBT) upgrade at the University of Jyväskylä, Department of Physics (JYFL) accelerator laboratory, a new ion beam extraction system has been designed and installed. The development of the new extraction was performed with the ion optical code IBSimu, making it the first ECRIS extraction designed with the code. The measured performance of the new extraction is in good agreement with the simulations. Compared to the old extraction the new system provides improved beam quality, i.e. lower transverse emittance values and improved structure of beam profiles, and transmission efficiency of the LEBT and the JYFL K-130 cyclotron. For example, the transmission efficiencies of 40Ar8+ and 84Kr16+ beams have increased by 80 and 90%, respectively. The new extraction system is capable of handling higher beam currents than the old one, which has been demonstrated by extracting new 4He+ and 4He2+ record beam currents of 1.12 mA and 720 μA, exceeding the old records of the JYFL 14 GHz ECRIS by a factor of two.

  7. Solvent extraction-separation of La(III), Eu(III) and Er(III) ions from aqueous chloride medium using carbamoyl-carboxylic acid extractants

    Institute of Scientific and Technical Information of China (English)

    Reyhaneh Safarbali; Mohammad Reza Yaftian; Abbasali Zamani

    2016-01-01

    N,N-dibutyldiglycol amic acid (HLI) and N,N-dioctyldiglycol amic acid (HLI) were synthesized and characterized by con-ventional spectroscopic methods. These molecules were examined as extractants for extraction-separation of La(III), Eu(III) and Er(III), as representative ions of light, middle and heavy rare earths, from aqueous chloride solutions. The analysis of the extraction equilibria revealed that the extracted species of lanthanum and europium ions by both of the extractants had a 1:3 metal to ligand ratio. It was suggested that erbium ions were extracted into the organic phase via the formation of Er(LI or I)2Cl complexes. The effect of the organic diluents on the extraction-separation efficiency of the studied rare earths by HLI and HLI was investigated by comparing the results obtained in dichloromethane and carbon tetrachloride. Regardless to the diluent used, the order of selectivity presented by the investigated extractants was Er(III)>Eu(III)>La(III). It is noteworthy that, a significant enhancement in separation of the studied rare earths by the extractants was achieved in their competitive extraction experiments with respect to that obtained in single component extraction experiments. Applicability of the extractants for the removal of rare earth ions from spent Ni-MH batteries was tested by removal of La(III), Eu(III) and Er(III) ions from simulated leach solution of such batteries.

  8. Acid Extraction - Ion Exchange Recovery of Cinchona Alkaloids Process and Plant Development

    Science.gov (United States)

    1945-06-08

    farther and farther into the almost impenetrable rain forests of the Andes in search of drug- bearing bark. b. Labor and Transportation. In these...a certain percentage of the ion exchanger still bearing its hydrogen ion charge. As long as this situation exists, a certain amount of COp will...extraction medium. Hence, the contact time need be no greater than that re- quired to soften and disintegrate the gummy contents of the cell, plus

  9. QUANTITATIVE ION-PAIR EXTRACTION OF 4(5)-METHYLIMIDAZOLE FROM CARAMEL COLOR AND ITS DETERMINATION BY REVERSED-PHASE ION-PAIR LIQUID-CHROMATOGRAPHY

    DEFF Research Database (Denmark)

    Thomsen, Mohens; Willumsen, Dorthe

    1981-01-01

    A procedure for quantitative ion-pair extraction of 4(5)-methylimidazole from caramel colour using bis(2-ethylhexyl)phosphoric acid as ion-pairing agent has been developed. Furthermore, a reversed-phase ion-pair liquid chromatographic separation method has been established to analyse the content ...

  10. Measurements of an ion beam diameter extracted into air through a large-bore metal capillary

    Energy Technology Data Exchange (ETDEWEB)

    Hirano, Y.; Umigishi, M. [Graduate School of Humanities and Sciences, Nara Women’s University, Nara 630-8506 (Japan); Ishii, K.; Ogawa, H. [Department of Physics, Nara Women’s University, Nara 630-8506 (Japan)

    2015-07-01

    To extract an ion beam into air, the technique using a single macro-capillary has been paid attention. We have expanded the bore of the metal capillary up to 500 μm∅ inlet diameter to increase the beam intensity and have measured the intensity distributions of the extracted 3 MeV proton beam. Furthermore, we have tilted the capillary angle and measured the intensity distributions of the ion beam. In this article, we will present the experimental results together with the simulation which takes the tilt angles of the capillary into account.

  11. Generalization of the Child-Langmuir law to the alternate extraction of positive and negative ions

    Energy Technology Data Exchange (ETDEWEB)

    Lafleur, T., E-mail: trevor.lafleur@lpp.polytechnique.fr [Laboratoire de Physique des Plasmas, CNRS, Sorbonne Universités, UPMC Univ Paris 06, Univ Paris-Sud, Ecole Polytechnique, 91128 Palaiseau (France); ONERA-The French Aerospace Lab, 91120 Palaiseau (France); Aanesland, A. [Laboratoire de Physique des Plasmas, CNRS, Sorbonne Universités, UPMC Univ Paris 06, Univ Paris-Sud, Ecole Polytechnique, 91128 Palaiseau (France)

    2014-12-15

    Using a combined analytical and simulation approach, we investigate positive and negative ion extraction between two electrodes from an ion-ion plasma source. With a square voltage waveform applied to the electrodes, we obtain approximate analytical solutions for the time-averaged extracted current densities, which are given simply by: J{sub p}{sup ac}=[α−fL√((M{sub p})/(q{sub p}V{sub 0}) )]J{sub p}{sup dc}, and J{sub n}{sup ac}=[(1−α)−fL√((M{sub n})/(q{sub n}V{sub 0}) )]J{sub n}{sup dc}, where J{sup ac} is the time-averaged current density, α is the square waveform duty cycle, f is the frequency, L is the electrode gap length, M is the ion mass, q is the ion charge, V{sub 0} is the applied voltage amplitude, J{sup dc} is the dc extracted current density, and the subscripts p and n refer to positive and negative ions, respectively. In particular, if J{sup dc} is the dc space-charge limited current density, then these equations describe the square waveform generalization of the Child-Langmuir law.

  12. Ion Exchange Extraction of Boron from Aqueous Fluids by Amberlite IRA 743 Resin

    Institute of Scientific and Technical Information of China (English)

    肖应凯; 廖步勇; 刘卫国; 肖云; SWIHART,GeorgeH.

    2003-01-01

    The ion exchange characteristics d Amherlite IRA 743 resin for extracting boron from aqueous fluids have been investigated in detail. The results show that AmherHte IRA 743 resin, a boron specific ion exchange resin, can quantitatively extract boron as the B (OH)4- spedes from weakly basle solution. Some exchangeable anions such as CI- and SO42- are present, resulting in an increase in pH value of the loeded solution within the nan, and the boron in natural aqueous fluids with low nH is also extracted by Amberlite IRA 743 resin. However, the voiume of loaded solution must be restricted. The maximum voiume of loaded solution giving quantitative extraction of boron decreases for sample soh.,tiom of lower pH value. Warm HCI solution is more effective than room temperature HCI solution for eluting boron from Amberllte IRA 743 resin.

  13. Extraction of alginate biopolymer present in marine alga sargassum filipendula and bioadsorption of metallic ions

    OpenAIRE

    Sirlei Jaiana Kleinübing; Frederico Gai; Caroline Bertagnolli; Meuris Gurgel Carlos da Silva

    2013-01-01

    This paper studies the bioadsorption of Pb2+, Cu2+, Cd2+ and Zn2+ ions by marine alga Sargassum filipendula and by the alginate biopolymer extracted from this alga. The objective is to evaluate the importance of this biopolymer in removing different metallic ions by the marine alga S. filipendula. In the equilibrium study, the same affinity order was observed for both bioadsorbents: Pb2+ > Cu2+ > Zn2+ > Cd2+. For Pb2+ and Cu2+ ions when the alginate is isolated and acting as bioadsorbents, ad...

  14. Computer simulation of 2-D and 3-D ion beam extraction and acceleration

    Energy Technology Data Exchange (ETDEWEB)

    Ido, Shunji; Nakajima, Yuji [Saitama Univ., Urawa (Japan). Faculty of Engineering

    1997-03-01

    The two-dimensional code and the three-dimensional code have been developed to study the physical features of the ion beams in the extraction and acceleration stages. By using the two-dimensional code, the design of first electrode(plasma grid) is examined in regard to the beam divergence. In the computational studies by using the three-dimensional code, the axis-off model of ion beam is investigated. It is found that the deflection angle of ion beam is proportional to the gap displacement of the electrodes. (author)

  15. Extractive Spectrophotometric Determination of Fluconazole by Ion-pair Complex Formation with Bromocresol Green

    Institute of Scientific and Technical Information of China (English)

    JALALI,Fahimeh; RAJABI,Mohammad J.

    2007-01-01

    An extraction-spectrophotometric method for the determination of trace amounts of fluconazole was described.Fluconazole was effectively extracted as a 1 : 1 ion-pair complex with bromocresole green (BCG) at pH 3.0 into chloroform, followed by spectrophotometric determination at 420 nm. Beer's law was obeyed over the range of 4-procedure was applied to the determination of fluconazole in pharmaceutical preparations as well as its recovery from a blood serum sample.

  16. Producing multicharged fullerene ion beam extracted from the second stage of tandem-type ECRIS

    Energy Technology Data Exchange (ETDEWEB)

    Nagaya, Tomoki, E-mail: nagaya@nf.eie.eng.osaka-u.ac.jp; Nishiokada, Takuya; Hagino, Shogo; Otsuka, Takuro; Sato, Fuminobu; Kato, Yushi [Graduate School of Engineering, Osaka University, 2-1 Yamada-oka, Suita-shi, Osaka 565-0871 (Japan); Uchida, Takashi [Graduate School of Interdisciplinary New Science, Toyo University, 2100, Kujirai, Kawagoe-shi, Saitama 350-8585 (Japan); Bio-Nano Electronics Research Centre, Toyo University, 2100, Kujirai, Kawagoe-shi, Saitama 350-8585 (Japan); Muramatsu, Masayuki; Kitagawa, Atsushi [National Institute of Radiological Sciences (NIRS), 4-9-1 Anagawa, Inage-ku, Chiba-shi, Chiba 263-8555 (Japan); Yoshida, Yoshikazu [Graduate School of Interdisciplinary New Science, Toyo University, 2100, Kujirai, Kawagoe-shi, Saitama 350-8585 (Japan); Faculty of Science and Engineering, Toyo University, 2100, Kujirai, Kawagoe-shi, Saitama 350-8585 (Japan)

    2016-02-15

    We have been constructing the tandem-type electron cyclotron resonance ion source (ECRIS). Two ion sources of the tandem-type ECRIS are possible to generate plasma individually, and they also confined individual ion species by each different plasma parameter. Hence, it is considered to be suitable for new materials production. As the first step, we try to produce and extract multicharged C{sub 60} ions by supplying pure C{sub 60} vapor in the second stage plasma because our main target is producing the endohedral fullerenes. We developed a new evaporator to supply fullerene vapor, and we succeeded in observation about multicharged C{sub 60} ion beam in tandem-type ECRIS for the first time.

  17. Design of a low voltage, high current extraction system for the ITER Ion Source

    Science.gov (United States)

    Agostinetti, P.; Antoni, V.; Cavenago, M.; de Esch, H. P. L.; Fubiani, G.; Marcuzzi, D.; Petrenko, S.; Pilan, N.; Rigato, W.; Serianni, G.; Singh, M.; Sonato, P.; Veltri, P.; Zaccaria, P.

    2009-03-01

    A Test Facility is planned to be built in Padova to assemble and test the Neutral Beam Injector for ITER. In the same Test Facility the Ion Source will be tested in a dedicated facility planned to operate in parallel to the main 1 MV facility. Purpose of the full size Ion Source is to optimize the Ion Source performance by maximizing the extracted negative ion current density and its spatial uniformity and by minimizing the ratio of co-extracted electrons. In this contribution the design of the extractor and accelerator grids for a 100 kV, 60 A system is presented. The trajectories of the negative ions, calculated with the SLACCAD code [1], have been benchmarked by a new 2D code (BYPO [2]) which solves in a self consistent way the electric fields in presence of electric charge and magnetic fields. The energy flux intercepted by the grids is estimated by using the Montecarlo code EAMCC [3] and the grids designed according to the constraints set by the permanent magnets and by the cooling channels. The interaction of backstreaming ions due to the ionization process with the grids and the Ion Source backplate is investigated and its impact on the project and performance discussed.

  18. Extraction design and low energy beam transport optimization of space charge dominated multispecies ion beam sources

    Science.gov (United States)

    Delferrière, O.; De Menezes, D.

    2004-05-01

    In all accelerator projects, the low energy part of the accelerator has to be carefully optimized to match the beam characteristic requirements of the higher energy parts. Since 1994 with the beginning of the Injector of Protons for High Intensity (IPHI) project and Source of Light Ions with High Intensities (SILHI) electron cyclotron resonance (ECR) ion source development at CEA/Saclay, we are using a set of two-dimensional (2D) codes for extraction system optimization (AXCEL, OPERA-2D) and beam transport (MULTIPART). The 95 keV SILHI extraction system optimization has largely increased the extracted current, and improved the beam line transmission. From these good results, a 130 mA D+ extraction system for the International Fusion Material Irradiation Facility project has been designed in the same way as SILHI one. We are also now involved in the SPIRAL 2 project for the building of a 40 keV D+ ECR ion source, continuously tunable from 0.1 to 5 mA, for which a special four-electrode extraction system has been studied. In this article we will describe the 2D design process and present the different extraction geometries and beam characteristics. Simulation results of SILHI H+ beam emittance will be compared with experimental measurements.

  19. Portable test bench for the studies concerning ion sources and ion beam extraction and focusing systems; Banco de pruebas portatil para el estudio de fuentes de iones y de la extraccion y enfoque del haz de iones

    Energy Technology Data Exchange (ETDEWEB)

    Cordero Lopez, F.

    1961-07-01

    A portable test bench is described, which was designed to check ion sources, ion beam extraction and focusing systems before its use in a 600 KeV Cockcroft-Walton accelerator. The vacuum possibilities of the system are specially analyzed in connection with its particular use. The whole can be considered as a portable accelerator of low energy (50 keV). (Author)

  20. Stream mesocosm response sensitivities to simulated ion stress in produced waters from resource extraction activities

    Science.gov (United States)

    To increase the ecological relevance of laboratory exposures intent on determining species sensitivity to ion stress from resource extraction activities we have conducted several stream mesocosm dosing studies that pair single-species and community-level responses in-situ and all...

  1. Extracting the Electron-Ion Temperature Relaxation Rate from Ion Stopping Experiments

    Science.gov (United States)

    Grabowski, Paul E.; Frenje, Johan A.; Benedict, Lorin X.

    2016-10-01

    Direct measurement of i-e equilibration rates at ICF-relevant conditions is a big challenge, as it is difficult to differentiate from other sinks and sources of energy, such as heat conduction and pdV work. Another method is to use information from ion stopping experiments. Such experiments at the OMEGA laser have made precision energy loss measurements of fusion products at these conditions. Combined with the multimonochromatic x-ray imager technique, which gives temporally and spatially resolved electron temperature and density, we have a robust stopping experiment. We propose to use such stopping measurements to assess the i-e temperature relaxation rate, since both processes involve energy exchange between electrons and ions. We require that the fusion products are 1) much faster than the thermal ions so that i-i collisions are negligible compared to i-e collisions and 2) slower than the thermal electrons so that the stopping obeys a linear friction law. Then the Coulomb logarithms associated with ion stopping and i-e temperature relaxation rate are identical and a measurement of the former provides the latter. Prepared by LLNL under Contract DE-AC52-07NA27344.

  2. Solvent extraction of trivalent lanthanoid ions with N,N`-dimethyl-N,N`-diphenyl-3-oxapentanediamide

    Energy Technology Data Exchange (ETDEWEB)

    Narita, H.; Tachimori, S. [Separation Chemistry Lab., Japan Atomic Energy Research Inst., Ibaraki (Japan)]|[Ibaraki Univ., Bunkyo (Japan); Yaita, T.; Tamura, K. [Ibaraki Univ., Bunkyo (Japan)

    1998-12-31

    The extraction of trivalent lanthanoid ions from nitric acid and hydrochloric acid solutions by N,N`-dimethyl-N,N`-diphenyl-3-oxapentanediamide, DMDPhOPDA, was investigated. The distribution ratios in the nitric acid system were much higher than those in the hydrochloric acid system. In the nitric acid system, the dependencies of the distribution ratios on nitric acid and DMDPhOPDA concentrations showed a difference between lighter and heavier lanthanoid ions. The plots of the number of DMDPhOPDA molecules in the extracted species obtained from slope analysis in 4 mol dm{sup -3} nitric acid versus the ionic radius of trivalent lanthanoid ions exhibited a significant change around the middle of the lanthanoids (S-shape). The distribution ratios in the nitric acid system increased with an increase in the atomic number, while those in the HCl system decreased. (orig.)

  3. Bohai crude oil identification by gas chromatogram fingerprinting quantitative analysis coupled with cluster analysis

    Institute of Scientific and Technical Information of China (English)

    SUN Peiyan; BAO Mutai; GAO Zhenhui; LI Mei; ZHAO Yuhui; WANG Xinping; ZHOU Qing; WANG Xiulin

    2006-01-01

    By gas chromatogram, six crude oils fingerprinting distributed in four oilfields and four oil platforms were analyzed and the corresponding normal paraffin hydrocarbon (including pristane and phytane) concentration was obtained by the internal standard method. The normal paraffin hydrocarbon distribution patterns of six crude oils were built and compared. The cluster analysis on the normal paraffin hydrocarbon concentration was conducted for classification and some ratios of oils were used for oils comparison. The results indicated: there was a clear difference within different crude oils in different oil fields and a small difference between the crude oils in the same oil platform. The normal paraffin hydrocarbon distribution pattern and ratios, as well as the cluster analysis on the normal paraffin hydrocarbon concentration can have a better differentiation result for the crude oils with small difference than the original gas chromatogram.

  4. Aggregation and metal ion extraction properties of novel, silicon-substituted alkylenediphosphonic acids.

    Energy Technology Data Exchange (ETDEWEB)

    McAlister, D. R.; Dietz, M. L.; Chiarizia, R.; Herlinger, A. W.

    2001-05-10

    In conjunction with efforts to develop novel actinide extractants exhibiting solubility in supercritical carbon dioxide, the effect of adding silicon-based functionalities to diphosphonic acids has been investigated. Specifically, a series of silyl-substituted diphosphonic acids has been prepared and characterized, and their aggregation and metal ion extraction properties compared with alkyl-substituted diphosphonic acids, reagents previously demonstrated to be effective extractants of actinides from acidic aqueous media into various organic solvents. In addition, the influence of the number of methylene groups bridging the phosphorus atoms of the diphosphonic acids on their extraction behavior has been investigated. Variations in the extraction behavior of the compounds arising from differences in the number of bridging methylene groups have been shown to be attributable to a combination of factors, in particular, the aggregation state of the ligand, the size of the chelate rings formed upon complexation, the basicity of the phosphoryl group and the relative acidities of the ligands.

  5. Optimization and numerical simulation for the extraction system of the H- multicusp ion source

    Science.gov (United States)

    Hosseinzadeh, M.; Afarideh, H.

    2014-05-01

    A new ion source has been designed and manufactured for the CYCLONE30 accelerator, which has a much advanced performance compared with the original. It is expected that the newly designed ion source extraction system will transport a very large percentage of the beam without deteriorating the beam optics, which is designed to deliver an H- beam at 30 keV. The accelerator assembly consists of three circular aperture electrodes made of copper. The simulation study was focused on finding parameter sets that raise the beam perveance as large as possible and which reduce the beam divergence as low as possible. Ion beams of the highest quality are extracted whenever the half-angular divergence is minimum, for which the perveance current intensity and the extraction gap have optimum values. The triode extraction system is designed and optimized by using CST software (for Particle Beam Simulations). The physical design of the extraction system is given in this paper. From the simulation results, it is concluded that it is possible to achieve this goal by decreasing the thickness of the plasma electrode, shortening the first gap, and adjusting the acceleration electrode voltage.

  6. [Determination of residual aluminium Ion in Huoxiang Zhengqi pellets by GFAAS with EDTA complexation extraction].

    Science.gov (United States)

    Wang, Xue-Na; Ran, Cong-Cong; Li, Qing-Lian; Du, Chao-Hui; Jiang, Ye

    2015-06-01

    To establish an EDTA complexation extraction pretreatment combining with GFAAS method for the determination of residual aluminium ion in Huoxiang zhengqi pellets without digestive treatment, systematical investigation was made on sample preparation, and EDTA was used for the complexation extraction of residual aluminium ion in samples. The pH, concentration and volume of extraction solution, the temperature and time of microwave extraction, and graphite furnace temperature program were investigated. The results were compared with the microwave digestion. It was showed that, 0.1 g of sample weight was added in 20 mL 0.05 mol x L(-1) EDTA solution (pH 3.5), followed by heating at 150 degrees C for 10 min in the microwave extraction device. The determination of GFAAS was performed at optimized detection wavelength (257.4 nm) as well as graphite furnace temperature program, the detection limits and quantification limits were 2.37 μg x L(-1) and 7.89 μg x L(-1), respectively. The precision (RSD) was less than 2.3%. The average recovery was 96.9% -101%. The present method is easy, rapid and accurate for the determination of residual aluminium ion in Huoxiang zhengqi pellets.

  7. Data mining of plasma peptide chromatograms for biomarkers of air contaminant exposures

    Directory of Open Access Journals (Sweden)

    Vincent Renaud

    2008-01-01

    Full Text Available Abstract Background Interrogation of chromatographic data for biomarker discovery becomes a tedious task due to stochastic variability in retention times arising from solvent and column performance. The difficulty is further compounded when the effects of exposure (e.g. to environmental contaminants and biological variability result in varying numbers and intensities of peaks among chromatograms. Results We developed a software tool to correct the stochastic time shifts in chromatographic data through iterative selection of landmark peaks and isometric interpolation to improve alignment of all chromatographic peaks. To illustrate application of the tool, plasma peptides from Fischer rats exposed for 4 h to clean air or Ottawa urban particles (EHC-93 were separated by HPLC with autofluorescence detection, and the retention time shifts between chromatograms were corrected (dewarped. Both dewarped and non-dewarped datasets were then mined for models containing peptide peaks that best discriminate among the treatment groups using ClinproTools™. In general, models generated by dewarped datasets were able to better classify test sample chromatograms into either clean air or EHC-93 exposure groups, and 0 or 24 h post-recovery time groups. Peak areas of peptides in a model that produced the best discrimination of treatment groups were analyzed by two-way ANOVA with exposure (clean air, EHC-93 and recovery time (0 h, 24 h as factors. Statistically significant (p Conclusion Our software tool provides a simple and portable approach for alignment of chromatograms with complex, bi-directional retention time shifts prior to data mining. Reliable biomarker discovery can be achieved through chromatographic dewarping using our software followed by pattern recognition by commercial data mining applications.

  8. Negative ion extraction via particle simulation for fusion: critical assessment of recent contributions

    Science.gov (United States)

    Garrigues, L.; Fubiani, G.; Boeuf, J. P.

    2017-01-01

    Particle-in-cell (PIC) models have been extensively used in the last few years to describe negative ion extraction for neutral beam injection applications. We show that some of these models have been employed in conditions far from the requirements of particle simulations and that questionable conclusions about negative ion extraction, not supported by experimental evidence, have been obtained. We present a critical analysis of the method that has led to these conclusions and propose directions toward a more accurate and realistic description of negative ion extraction. We show in particular that, as expected in PIC simulations, mesh convergence is reached only if the grid spacing is on the order of or smaller than the minimum Debye length in the simulation domain, and that strong aberrations in the extracted beam are observed if this constraint is not respected. The method of injection of charged particles in the simulated plasma is also discussed, and we show that some injection methods used in the literature lead to unphysical results.

  9. Satellite Lithium-Ion Battery Remaining Cycle Life Prediction with Novel Indirect Health Indicator Extraction

    Directory of Open Access Journals (Sweden)

    Haitao Liao

    2013-07-01

    Full Text Available Prognostics and remaining useful life (RUL estimation for lithium-ion batteries play an important role in intelligent battery management systems (BMS. The capacity is often used as the fade indicator for estimating the remaining cycle life of a lithium-ion battery. For spacecraft requiring high reliability and long lifetime, in-orbit RUL estimation and reliability verification on ground should be carefully addressed. However, it is quite challenging to monitor and estimate the capacity of a lithium-ion battery on-line in satellite applications. In this work, a novel health indicator (HI is extracted from the operating parameters of a lithium-ion battery to quantify battery degradation. Moreover, the Grey Correlation Analysis (GCA is utilized to evaluate the similarities between the extracted HI and the battery’s capacity. The result illustrates the effectiveness of using this new HI for fading indication. Furthermore, we propose an optimized ensemble monotonic echo state networks (En_MONESN algorithm, in which the monotonic constraint is introduced to improve the adaptivity of degradation trend estimation, and ensemble learning is integrated to achieve high stability and precision of RUL prediction. Experiments with actual testing data show the efficiency of our proposed method in RUL estimation and degradation modeling for the satellite lithium-ion battery application.

  10. Extractive Spectrophotometric Determination of Bismuth(III in Water Using Some Ion Pairing Reagents

    Directory of Open Access Journals (Sweden)

    Abdulaziz S. Bashammakh

    2011-01-01

    Full Text Available Two novel and low cost liquid-liquid extraction methods for the separation of bismuth(III at trace level from aqueous medium have been developed. The two methods were based upon the formation of yellow colored ternary complex ion associates of tetraiodobismuth(III complex anion, BiI4- with the ion-pairing reagent 2,3,5-tetraphenyltetrazoliumchloride (Tz+.Cl– and 1, 10 phenanthroline (Phen in sulfuric acid medium. The effect of various parameters e.g. pH, organic solvent, shaking time, etc. on the preconcentration of bismuth(III from the aqueous media by the reagent was investigated. The developed colored complex ion associates [Tz+.BiI4-] and [Phen+.BiI4-] were extracted quantitatively into acetone-chloroform (1:1v/v and methyliso- butylketone (MIBK, respectively. The compositions of the formed complex ion associates [Tz+.BiI4-] and [Phen+.BiI4-] were determined by the Job's method at 500 and 490 nm, respectively. The plots of bismuth(III concentration (0-17 μg mL-1 versus absorbance of the associates at 500 and 490 nm were linear with good correlation coefficient (R2=0.998. The developed method of the ion associate [Tz+.BiI4-] two methods was applied successfully for the analysis of bismuth in water.

  11. Technical note: Efficiency of total demineralization and ion-exchange column for DNA extraction from bone.

    Science.gov (United States)

    Seo, Seung Bum; Zhang, Aihua; Kim, Hye Yeon; Yi, Jin A; Lee, Hye Young; Shin, Dong Hoon; Lee, Soong Deok

    2010-01-01

    We investigated whether a combination of recently introduced methods, total demineralization and ion-exchange columns, would increase DNA recovery from old bone. Ten bone samples taken after a burial period of approximately 60 years were used in this study. Bone powder was digested using total or incomplete demineralization. DNA was extracted by the standard organic method. The DNA extract was purified with ion-exchange columns or QIAquick spin columns. The efficiency of different DNA extraction methods was compared in terms of DNA concentration, inhibitors generated by real-time PCR, and conventional STR typing results. The mean DNA concentration using the total demineralization method is approximately 3 times higher than that using the incomplete demineralization method. For DNA purification, the method using QIAquick spin columns appeared to yield approximately double the DNA than the method using ion-exchange columns. Furthermore, 2 out of 10 samples showed higher levels of inhibition with C(T) values of IPC > or =30 cycles when using only ion-exchange columns. In STR results, total demineralization yielded more locus profiles by 4.2 loci than incomplete demineralization, and QIAquick spin columns also yielded more locus profiles by 3.5 loci than ion-exchange columns. Total demineralization of bone powder significantly increased DNA yield and improved STR typing results. However, the use of ion-exchange columns was not efficient when compared with the method using QIAquick spin columns. It is suggested that the combination of total demineralization and QIAquick spin columns lead to greatly improved STR typing results.

  12. Extraction of Alkali Ions Investigated by Conductometric and pH Measurements

    Directory of Open Access Journals (Sweden)

    L. Kalvoda

    2006-01-01

    Full Text Available Extraction of alkali ions from aqueous solutions of chlorides and hydroxides into a lipophilic liquid membrane composed of tetraethyl p-tert-butylcalix[4]arene tetraacetate (TBT solution in hexane was investigated by means of measurements of changes in the electrolytic conductivity and pH-value of the aqueous solution. Hydrolysis of the TBT ionophore resulting in the release of the ethyl groups was proposed as the main reaction process, leading to disturbance of the known preference of TBT for sodium ions

  13. High extraction ability of 1,3-dialkynyl calixarene towards mercury(Ⅱ) ion

    Institute of Scientific and Technical Information of China (English)

    Lin Bo Gong; Shu Ling Gong; Qin Zheng; Xiong Li; Yuan Yin Chen

    2007-01-01

    The reaction of 1,3-dipropyn-2-yloxycalix[4]arene with mercury(Ⅱ) acetate could give mercury-containing alkynyl calixarene polymer. The extraction behavior of 1,3-dipropyn-2-yl-oxycalix[4]arene towards mercury(H) ion was examined. When the mole ratio of Hg2+/calixarene was 1∶1, the extractive percent can reach to 99.1%, and the extraction capacity was up to 431 mg/g. It could also decrease the Hg2+ concentration from 5 to 0.85 mg/L, which was only 17% of the national standard of effluent and satisfied the national standard of drinking water. The extraction process included chemical reaction.

  14. Extraction of radioactive positive ions across the surface of superfluid helium : A new method to produce cold radioactive nuclear beams

    NARCIS (Netherlands)

    Huang, WX; Dendooven, P; Gloos, K; Takahashi, N; Pekola, JP; Aysto, J

    2003-01-01

    Alpha-decay recoils Rn-219 were stopped in superfluid helium and positive ions were extracted by electric field into the vapour phase. This first quantitative observation of extraction was successfully conducted using highly sensitive radioactivity detection. The efficiency for extraction across the

  15. Effect of high ionic strength on the extraction of uranium(VI ions

    Directory of Open Access Journals (Sweden)

    M.K. Nazal

    2014-01-01

    Full Text Available Preparation and characterization of didodecylphosphoric acid (HDDPA as an extractant in toluene was carried. Mass spectroscopy showed that the monomer peak at 457.4 amu [M–Na+] is double that of the dimer at 891.9 amu [M–M–Na+] and the monomer molecules concentration dominate the dimer molecules in toluene. HDDPA was used as an extractant for the extraction of U(VI ion from perchlorate and nitrate media that have ionic strength (1.00, 3.00, 5.00, 7.00 M. The effect of HDDPA concentration, pcH, ionic strength of supporting electrolytes, and temperature in the range 15–45 °C on the extraction process have been studied. The stoichiometry of the extraction of U(VI ion, the free energy change (ΔG, the enthalpy change (ΔH, the entropy change (ΔS, and Kex at different ionic strength have been calculated. The formula of the complexes, which were formed has been established to be UO2(X(R2(HR2 at pcH equal 2.00 and UO2(X(R2(HR2 and UO2(X(R2 at pcH = 1.00, where (X isClO4- orNO3- and (HR2 is didodecylphosphoric acid monomer, (R2 is the deprotonated didodecylphosphoric acid, where R is the dodecyl group.

  16. Ion suppression in the determination of clenbuterol in urine by solid-phase extraction atmospheric pressure chemical ionisation ion-trap mass spectrometry

    NARCIS (Netherlands)

    van Hout, M.W.J.; Niederlander, H.A G; de Zeeuw, R.A.; de Jong, G.J.

    2003-01-01

    Ion suppression effects were observed during the determination of clenbuterol in urine with solid-phase extraction/multiple-stage ion-trap mass spectrometry (SPE/MS3), despite the use of atmospheric pressure chemical ionisation. During SPE, a polymeric stationary phase (polydivinylbenzene) was appli

  17. Analysis of ion dynamics and peak shapes for delayed extraction time-of-flight mass spectrometers

    Science.gov (United States)

    Collado, V. M.; Ponciano, C. R.; Fernandez-Lima, F. A.; da Silveira, E. F.

    2004-06-01

    The dependence of time-of-flight (TOF) peak shapes on time-dependent extraction electric fields is studied theoretically. Conditions for time focusing are analyzed both analytically and numerically for double-acceleration-region TOF spectrometers. Expressions for the spectrometer mass resolution and for the critical delay time are deduced. Effects due to a leakage field in the first acceleration region are shown to be relevant under certain conditions. TOF peak shape simulations for the delayed extraction method are performed for emitted ions presenting a Maxwellian initial energy distribution. Calculations are compared to experimental results of Cs+ emission due to CsI laser ablation.

  18. Studies of the beam extraction system of the GTS-LHC electron cyclotron resonance ion source at CERN.

    Science.gov (United States)

    Toivanen, V; Küchler, D

    2016-02-01

    The 14.5 GHz GTS-LHC Electron Cyclotron Resonance Ion Source (ECRIS) provides multiply charged heavy ion beams for the CERN experimental program. The GTS-LHC beam formation has been studied extensively with lead, argon, and xenon beams with varied beam extraction conditions using the ion optical code IBSimu. The simulation model predicts self-consistently the formation of triangular and hollow beam structures which are often associated with ECRIS ion beams, as well as beam loss patterns which match the observed beam induced markings in the extraction region. These studies provide a better understanding of the properties of the extracted beams and a way to diagnose the extraction system performance and limitations, which is otherwise challenging due to the lack of direct diagnostics in this region and the limited availability of the ion source for development work.

  19. Studies of the beam extraction system of the GTS-LHC electron cyclotron resonance ion source at CERN

    Energy Technology Data Exchange (ETDEWEB)

    Toivanen, V., E-mail: ville.aleksi.toivanen@cern.ch; Küchler, D. [European Organization for Nuclear Research (CERN), 1211 Geneva 23 (Switzerland)

    2016-02-15

    The 14.5 GHz GTS-LHC Electron Cyclotron Resonance Ion Source (ECRIS) provides multiply charged heavy ion beams for the CERN experimental program. The GTS-LHC beam formation has been studied extensively with lead, argon, and xenon beams with varied beam extraction conditions using the ion optical code IBSimu. The simulation model predicts self-consistently the formation of triangular and hollow beam structures which are often associated with ECRIS ion beams, as well as beam loss patterns which match the observed beam induced markings in the extraction region. These studies provide a better understanding of the properties of the extracted beams and a way to diagnose the extraction system performance and limitations, which is otherwise challenging due to the lack of direct diagnostics in this region and the limited availability of the ion source for development work.

  20. Studies of the beam extraction system of the GTS-LHC electron cyclotron resonance ion source at CERN

    Science.gov (United States)

    Toivanen, V.; Küchler, D.

    2016-02-01

    The 14.5 GHz GTS-LHC Electron Cyclotron Resonance Ion Source (ECRIS) provides multiply charged heavy ion beams for the CERN experimental program. The GTS-LHC beam formation has been studied extensively with lead, argon, and xenon beams with varied beam extraction conditions using the ion optical code IBSimu. The simulation model predicts self-consistently the formation of triangular and hollow beam structures which are often associated with ECRIS ion beams, as well as beam loss patterns which match the observed beam induced markings in the extraction region. These studies provide a better understanding of the properties of the extracted beams and a way to diagnose the extraction system performance and limitations, which is otherwise challenging due to the lack of direct diagnostics in this region and the limited availability of the ion source for development work.

  1. Effect of impurity ions on preparation of novel saponifier for rare earth extraction

    Institute of Scientific and Technical Information of China (English)

    肖燕飞; 冯宗玉; 黄小卫; 黄莉; 徐旸; 侯永可; 王猛

    2013-01-01

    Magnesium bicarbonate, prepared by the carbonation of magnesium hydroxide slurry, was used as a novel saponifier to eliminate the ammonia nitrogen pollution in the rare earth extraction separation process. The effect of impurity ions introduced by system on the carbonation reaction of magnesium hydroxide was studied in the work. The results showed that the presence of Ca2+could lead to side reactions so as to reduce the conversion rate of magnesium hydroxide, and a small number of rare earth ions would have great influence on the carbonation reaction. What’s more, there was no influence on carbonation reaction with the low concen-tration of Na+or Mg2+, the conversion rate of magnesium hydroxide could reach above 96%. This paper showed a practical theory which could provide scientific guidance for the preparation of novel saponifier in rare earth extraction separation process.

  2. Extraction of high-intensity ion beams from a laser plasma by a pulsed spherical diode

    Directory of Open Access Journals (Sweden)

    Yoshiyuki Oguri

    2005-06-01

    Full Text Available High-current Cu^{+} ion beams were extracted from a laser-produced plasma using a pulsed high-voltage multiaperture diode driven by an induction cavity. The amplitude and the duration of the extraction voltage were 130 kV and 450 ns, respectively. During the extraction, explosive beam divergence due to the strong space-charge force was suppressed by the focusing action of the gap between concentric hemispheres. Modulation of the extracted beam flux due to the plasma prefill in the gap has been eliminated by using a biased control grid put on the anode holes. By means of this extraction scheme we obtained a rectangular beam pulse with a rise time as short as ≈100  ns. The beam current behind the cathode was limited to ≈0.1   A, owing to space-charge effects, as well as to poor geometrical transmission through the cathode sphere. From the measurement of the extracted beam current density distribution along the beam axis and the beam profile measurement, we found a beam waist slightly downstream of the spherical center of the diode structure. The measured beam behavior was consistent with numerical results obtained via a 3D particle code. No serious degradation of the beam emittance was observed for the grid-controlled extraction scheme.

  3. Parameter Extraction and Characteristics Study for Manganese-Type Lithium-Ion Battery

    OpenAIRE

    Somakettarin, Natthawuth; Funaki, Tsuyoshi

    2016-01-01

    In this paper, we propose the battery transient response model and parameter extraction method for studying the dynamic behaviors of Manganese-type Lithium-Ion battery. The background knowledge of the battery structure and its operating principle are also concluded. Several aspects of operating conditions, such as charging and discharging operations, environments of terminal currents and temperatures, are considered through the experiments for understanding the battery behaviors.  The charact...

  4. Modeling of plasma transport and negative ion extraction in a magnetized radio-frequency plasma source

    Science.gov (United States)

    Fubiani, G.; Garrigues, L.; Hagelaar, G.; Kohen, N.; Boeuf, J. P.

    2017-01-01

    Negative ion sources for fusion are high densities plasma sources in large discharge volumes. There are many challenges in the modeling of these sources, due to numerical constraints associated with the high plasma density, to the coupling between plasma and neutral transport and chemistry, the presence of a magnetic filter, and the extraction of negative ions. In this paper we present recent results concerning these different aspects. Emphasis is put on the modeling approach and on the methods and approximations. The models are not fully predictive and not complete as would be engineering codes but they are used to identify the basic principles and to better understand the physics of the negative ion sources.

  5. Decontamination of Metal Ions in Soil by Supercritical CO{sub 2} Extraction with Catecholamine Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jihye; Kim, Hakwon; Park, Kwangheon [Kyunghee University, Yongin (Korea, Republic of)

    2015-10-15

    The role of fuel cladding and reactor vessels is to help prevent the leakage of radioactive materials, including the fission products. However, if these shielding materials are damaged by a severe disaster such as the Fukushima Accident, radioactive materials could leak outside of a power plant site. Indeed, after the Fukushima Accident, radioactive materials have been detected in air and water samples. The air and water pollution lead to soil pollution, which is particularly difficult to decontaminate, as soil pollution has several types that vary according to the characteristics of a pollutant or its area. The existing decontamination methods generate a secondary waste owing to use of chemical toxicity solvents. It is also disadvantageous due to the additional cost of handling them. Therefore, new effective decontamination methods that reduce the use of toxicity solvents are necessary. For example, using supercritical CO{sub 2} has been studied as a new decontamination method. This study examines the method of decontaminating metallic ions inside of the soil using supercritical CO{sub 2} and a catecholamine compound. This study examined the effects of extracting metallic ions inside the soil using supercritical CO{sub 2} and catecholamine as the ligand. Based on these results, it is evident that when only the extraction agent was used, there was no extraction effect and that only when the ligand, co-ligand, and additive were used together was there an extraction effect. Following this, the optimal extraction-agent ratio was confirmed using varying amounts of extraction agents. The most effective extraction ratio of ligand to co-ligand was 1:2 in E-9 when 0.3 ml of H{sub 2}O were added.

  6. Beam extraction from a laser-driven multicharged ion source (abstract)

    Science.gov (United States)

    Anderson, O. A.; Logan, B. Grant

    1998-02-01

    A newly proposed type of multicharged ion source has several potential advantages over existing types and a number of useful applications. The basic principle is that multiphoton absorption in an intense uniform laser focus can give multiple charge states of high purity (Ref. Reference 1). Thus, charge state separation downstream is simplified or made unnecessary. Another advantage is that large currents (hundreds of amperes) can be extracted. This type of source could be used for heavy-ion fusion drivers (see Ref. Reference 1) or storage rings. There are also industrial application such as materials processing. We describe conceptual design studies for several specific cases. For example, we discuss extraction and focusing of a 4.1 MV, 144 A beam of Xe16+ ions from an expanding plasma created by an intense laser. The maximum duration of the beam pulse is determined by the total charge in the plasma, while the practical pulse length is determined by the range of plasma radii over which good beam optics can be achieved. The initially diverging beam can be refocused to a small radius or made parallel by a combination of electrostatic and solenoid focusing. Our design studies are carried out first with an envelope code to determine the proper focusing parameters and then with a self-consistent particle code to optimize the beam quality. We present results from both codes and discuss several applications of this type of ion source.

  7. Separation and quantitation of methenamine in urine by ion-pair extraction.

    Science.gov (United States)

    Strom, J G; Jun, H W

    1986-04-01

    An ion-pair extraction technique is described for separating methenamine, a urinary tract antibacterial agent, from formaldehyde in human urine samples. Separation conditions are developed from extraction constants for the methenamine-bromocresol green ion-pair. The technique involves adsorption of the ion-pair onto a silica cartridge and elution with methylene chloride:1-pentanol (95:5). Methenamine is freed from the ion-pair by the addition of excess tetrabutylammonium iodide and converted to formaldehyde (determined spectrophotometrically) by reaction with ammonia and acetylacetone. Linear standard plots were obtained from urine containing methenamine which was diluted to 10-160 micrograms/mL. The lower limit of detection was 6 micrograms/mL of methenamine. Absolute recovery from urine was greater than or equal to 94.5%. The precision (CV) of detection of methenamine in the presence of formaldehyde was less than 2%, and less than or equal to 4.5% for the detection of formaldehyde in the presence of methenamine. No interferences were noted. The applicability of the method was demonstrated by analysis of human urine levels of both methenamine and formaldehyde following oral administration of a methenamine salt to a volunteer.

  8. Bach Adsorption Study for the Extraction of Silver Ions by Hydrazone Compounds from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Abdussalam Salhin Mohamad Ali

    2012-01-01

    Full Text Available Sorbent materials based on a hydrazone Schiff base compound, C14H11BrN4O4, were prepared either by immobilizing the ligand into sol-gel (SG1 or bonding to silica (SG2. The sorbent materials were characterized by FT-IR, EDX, SEM, TEM, and TGA. The sorption characteristics of a matrix of eight transition metal ions (Ag+, Cu2+, Co2+, Ni2+, Fe3+, Pb2+, Zn2+, and Mn2+ using batch method were studied. Several key parameters that affected the extraction efficiency such as pH, contact time, metal ions concentration, and gel size (for SGl were investigated and optimized. Under the optimized conditions, the physically immobilized hydrazone sorbent (SG1 exhibits highest selectivity towards Ag+ ions, while the chemically bonded hydrazone sorbent (SG2 exhibits high extraction for all metal ions tested. However, for practical applications such as the removal and preconcentration of Ag+, the physically immobilized sorbent (SG1 is preferred.

  9. Ba-ion extraction from a high pressure Xe gas for double-beta decay studies with EXO

    CERN Document Server

    Brunner, T; Sabourov, A; Varentsov, V L; Gratta, G; Sinclair, D

    2013-01-01

    An experimental setup is being developed to extract Ba ions from a high-pressure Xe gas environment. It aims to transport Ba ions from 10 bar Xe to vacuum conditions. The setup utilizes a converging-diverging nozzle in combination with a radio-frequency (RF) funnel to move Ba ions into vacuum through the pressure drop of several orders of magnitude. This technique is intended to be used in a future multi-ton detector investigating double-beta decay in $^{136}$Xe. Efficient extraction and detection of Ba ions, the decay product of Xe, would allow for a background-free measurement of the $^{136}$Xe double-beta decay.

  10. Signal processing using sparse derivatives with applications to chromatograms and ECG

    Science.gov (United States)

    Ning, Xiaoran

    In this thesis, we investigate the sparsity exist in the derivative domain. Particularly, we focus on the type of signals which posses up to Mth (M > 0) order sparse derivatives. Efforts are put on formulating proper penalty functions and optimization problems to capture properties related to sparse derivatives, searching for fast, computationally efficient solvers. Also the effectiveness of these algorithms are applied to two real world applications. In the first application, we provide an algorithm which jointly addresses the problems of chromatogram baseline correction and noise reduction. The series of chromatogram peaks are modeled as sparse with sparse derivatives, and the baseline is modeled as a low-pass signal. A convex optimization problem is formulated so as to encapsulate these non-parametric models. To account for the positivity of chromatogram peaks, an asymmetric penalty function is also utilized with symmetric penalty functions. A robust, computationally efficient, iterative algorithm is developed that is guaranteed to converge to the unique optimal solution. The approach, termed Baseline Estimation And Denoising with Sparsity (BEADS), is evaluated and compared with two state-of-the-art methods using both simulated and real chromatogram data. Promising result is obtained. In the second application, a novel Electrocardiography (ECG) enhancement algorithm is designed also based on sparse derivatives. In the real medical environment, ECG signals are often contaminated by various kinds of noise or artifacts, for example, morphological changes due to motion artifact, non-stationary noise due to muscular contraction (EMG), etc. Some of these contaminations severely affect the usefulness of ECG signals, especially when computer aided algorithms are utilized. By solving the proposed convex l1 optimization problem, artifacts are reduced by modeling the clean ECG signal as a sum of two signals whose second and third-order derivatives (differences) are sparse

  11. Proton and Pb ion beam extraction experiments with bent crystals at the CERN-SPS

    CERN Document Server

    Elsener, K; Klem, J T; CERN. Geneva. SPS and LEP Division

    1997-01-01

    Extraction of particle beams from the CERN-SPS using bent silicon crystals is described. A summary of the early results is given. Emphasis is on the recent experiments, in particular on the energy dependence of proton extraction at 14, 120 and 270 GeV. 'U-shaped' crystals of different thickness and with a different miscut angle have been compared at 120 GeV. Non-linear excitation of the beam was used in one experiment, with the aim to achieve larger impact parameters - the results show a particular behaviour in the tails of the beam. Finally, the first experimental result on extraction of a 22 TeV fully stripped Pb ion beam with a bent crystal is also described.

  12. Improvement of the cloud point extraction of uranyl ions by the addition of ionic liquids.

    Science.gov (United States)

    Gao, Song; Sun, Taoxiang; Chen, Qingde; Shen, Xinghai

    2013-12-15

    The cloud point extraction (CPE) of uranyl ions by different kinds of extractants in Triton X-114 (TX-114) micellar solution was investigated upon the addition of ionic liquids (ILs) with various anions, i.e., bromide (Br(-)), tetrafluoroborate (BF4(-)), hexafluorophosphate (PF6(-)) and bis[(trifluoromethyl)sulfonyl]imide (NTf2(-)). A significant increase of the extraction efficiency was found on the addition of NTf2(-) based ILs when using neutral extractant tri-octylphosphine oxide (TOPO), and the extraction efficiency kept high at both nearly neutral and high acidity. However, the CPE with acidic extractants, e.g., bis(2-ethylhexyl) phosphoric acid (HDEHP) and 8-hydroxyquinoline (8-HQ) which are only effective at nearly neutral condition, was not improved by ILs. The results of zeta potential and (19)F NMR measurements indicated that the anion NTf2(-) penetrated into the TX-114 micelles and was enriched in the surfactant-rich phase during the CPE process. Meanwhile, NTf2(-) may act as a counterion in the CPE of UO2(2+) by TOPO. Furthermore, the addition of IL increased the separation factor of UO2(2+) and La(3+), which implied that in the micelle TOPO, NTf2(-) and NO3(-) established a soft template for UO2(2+). Therefore, the combination of CPE and IL provided a supramolecular recognition to concentrate UO2(2+) efficiently and selectively.

  13. CHROMATOGATE: A TOOL FOR DETECTING BASE MIS-CALLS IN MULTIPLE SEQUENCE ALIGNMENTS BY SEMI-AUTOMATIC CHROMATOGRAM INSPECTION

    Directory of Open Access Journals (Sweden)

    Nikolaos Alachiotis

    2013-03-01

    Full Text Available Automated DNA sequencers generate chromatograms that contain raw sequencing data. They also generate data that translates the chromatograms into molecular sequences of A, C, G, T, or N (undetermined characters. Since chromatogram translation programs frequently introduce errors, a manual inspection of the generated sequence data is required. As sequence numbers and lengths increase, visual inspection and manual correction of chromatograms and corresponding sequences on a per-peak and per-nucleotide basis becomes an error-prone, time-consuming, and tedious process. Here, we introduce ChromatoGate (CG, an open-source software that accelerates and partially automates the inspection of chromatograms and the detection of sequencing errors for bidirectional sequencing runs. To provide users full control over the error correction process, a fully automated error correction algorithm has not been implemented. Initially, the program scans a given multiple sequence alignment (MSA for potential sequencing errors, assuming that each polymorphic site in the alignment may be attributed to a sequencing error with a certain probability. The guided MSA assembly procedure in ChromatoGate detects chromatogram peaks of all characters in an alignment that lead to polymorphic sites, given a user-defined threshold. The threshold value represents the sensitivity of the sequencing error detection mechanism. After this pre-filtering, the user only needs to inspect a small number of peaks in every chromatogram to correct sequencing errors. Finally, we show that correcting sequencing errors is important, because population genetic and phylogenetic inferences can be misled by MSAs with uncorrected mis-calls. Our experiments indicate that estimates of population mutation rates can be affected two- to three-fold by uncorrected errors.

  14. Optimization of the beam extraction systems for the Linac4 H{sup −} ion source

    Energy Technology Data Exchange (ETDEWEB)

    Fink, D. A.; Lettry, J.; Scrivens, R.; Steyaert, D. [CERN, 1211 Geneva 23 (Switzerland); Midttun, Ø. [University of Oslo, P.O. Box 1048, 0316 Oslo (Norway); CERN, 1211 Geneva 23 (Switzerland); Valerio-Lizarraga, C. A. [Departamento de Investigación en Fisica, Universidad de Sonora, Hermosillo (Mexico); CERN, 1211 Geneva 23 (Switzerland)

    2015-04-08

    The development of the Linac 4 and its integration into CERN’s acceleration complex is part of the foreseen luminosity upgrade of the Large Hadron Collider (LHC). The goal is to inject a 160 MeV H{sup −} beam into the CERN PS Booster (PSB) in order to increase the beam brightness by a factor of 2 compared to the 50 MeV proton linac, Linac 2, that is currently in operation. The requirements for the ion source are a 45 keV H{sup −} beam of 80 mA intensity, 2 Hz repetition rate and 0.5 ms pulse length within a normalized rms-emittance of 0.25 mm· mrad. The previously installed beam extraction system has been designed for an H{sup −} ion beam intensity of 20 mA produced by an RF-volume source with an electron to H{sup −} ratio of up to 50. For the required intensity upgrades of the Linac4 ion source, a new beam extraction system is being produced and tested; it is optimized for a cesiated surface RF-source with a nominal beam current of 40 mA and an electron to H{sup −} ratio of 4. The simulations, based on the IBSIMU code, are presented. At the Brookhaven National Laboratory (BNL), a peak beam current of more than 100 mA was demonstrated with a magnetron H{sup −} source at an energy of 35 keV and a repetition rate of 2 Hz. A new extraction system is required to operate at an energy of 45 keV; simulation of a two stage extraction system dedicated to the magnetron is presented.

  15. Optimization of the beam extraction systems for the Linac4 H- ion source

    Science.gov (United States)

    Fink, D. A.; Lettry, J.; Midttun, Ø.; Scrivens, R.; Steyaert, D.; Valerio-Lizarraga, C. A.

    2015-04-01

    The development of the Linac 4 and its integration into CERN's acceleration complex is part of the foreseen luminosity upgrade of the Large Hadron Collider (LHC). The goal is to inject a 160 MeV H- beam into the CERN PS Booster (PSB) in order to increase the beam brightness by a factor of 2 compared to the 50 MeV proton linac, Linac 2, that is currently in operation. The requirements for the ion source are a 45 keV H- beam of 80 mA intensity, 2 Hz repetition rate and 0.5 ms pulse length within a normalized rms-emittance of 0.25 mm. mrad. The previously installed beam extraction system has been designed for an H- ion beam intensity of 20 mA produced by an RF-volume source with an electron to H- ratio of up to 50. For the required intensity upgrades of the Linac4 ion source, a new beam extraction system is being produced and tested; it is optimized for a cesiated surface RF-source with a nominal beam current of 40 mA and an electron to H- ratio of 4. The simulations, based on the IBSIMU code, are presented. At the Brookhaven National Laboratory (BNL), a peak beam current of more than 100 mA was demonstrated with a magnetron H- source at an energy of 35 keV and a repetition rate of 2 Hz. A new extraction system is required to operate at an energy of 45 keV; simulation of a two stage extraction system dedicated to the magnetron is presented.

  16. Comparison of ONIX simulation results with experimental data from the BATMAN testbed for the study of negative ion extraction

    Science.gov (United States)

    Mochalskyy, Serhiy; Fantz, Ursel; Wünderlich, Dirk; Minea, Tiberiu

    2016-10-01

    The development of negative ion (NI) sources for the ITER neutral beam injector is strongly accompanied by modelling activities. The ONIX (Orsay Negative Ion eXtraction) code simulates the formation and extraction of negative hydrogen ions and co-extracted electrons produced in caesiated sources. In this paper the 3D geometry of the BATMAN extraction system, and the source characteristics such as the extraction and bias potential, and the 3D magnetic field were integrated in the model. Calculations were performed using plasma parameters experimentally obtained on BATMAN. The comparison of the ONIX calculated extracted NI density with the experimental results suggests that predictive calculations of the extraction of NIs are possible. The results show that for an ideal status of the Cs conditioning the extracted hydrogen NI current density could reach ~30 mA cm-2 at 10 kV and ~20 mA cm-2 at 5 kV extraction potential, with an electron/NI current density ratio of about 1, as measured in the experiments under the same plasma and source conditions. The dependency of the extracted NI current on the NI density in the bulk plasma region from both the modeling and the experiment was investigated. The separate distributions composing the NI beam originating from the plasma bulk region and the PG surface are presented for different NI plasma volume densities and NI emission rates from the plasma grid (PG) wall, respectively. The extracted current from the NIs produced at the Cs covered PG surface, initially moving towards the bulk plasma and then being bent towards the extraction surfaces, is lower compared to the extracted NI current from directly extracted surface produced ions.

  17. Rice straw modified by click reaction for selective extraction of noble metal ions.

    Science.gov (United States)

    Wang, Jingjing; Wei, Jun; Li, Juan

    2015-02-01

    Rice straw was modified by azide-alkyne click reaction in order to realize selective extraction of noble metal ions. The ability of the modified straw to adsorb Pd(2+) and Pt(4+) was assessed using a batch adsorption technique. It was found that the sorption equilibrium could be reached within 1h and the adsorption capacity increased with temperature for both Pd(2+) and Pt(4+). The maximum sorption capacities for Pd(2+) and Pt(4+) were respectively attained in 1.0 and 0.1 mol/L HCl. The modified straw showed excellent selectivity for noble metal ions in comparison to the pristine straw. In addition, the modified straw was examined as a column packing material for extraction of noble metal ions. It was indicated that 1.0 mL/min was the best flow rate for Pd(2+) and Pt(4+). The modified straw could be repeatedly used for 10 times without any significant loss in the initial binding affinity. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. DNA degradation by aqueous extract of Aloe vera in the presence of copper ions.

    Science.gov (United States)

    Naqvi, Shoa; Ullah, M F; Hadi, S M

    2010-06-01

    The plant Aloe vera has long been used in medicine, as dietary supplements and for cosmetic purposes. Aloe vera extracts are a rich source of polyphenols, such as aloin and aloe emodin and have shown a wide range of pharmacological properties, including anti-inflammatory and anti-cancer properties. The bioactive component aloe emodin has been reported to induce apoptosis in various cancer cell lines. Many of the biological activities of Aloe vera have been attributed to its antioxidant properties. However, most plant-derived polyphenols that are also present in Aloe vera may exhibit pro-oxidant properties either alone or in the presence of transition metals, such as copper. Previous reports from this laboratory have implicated the pro-oxidant action as one of the mechanisms for their anti-cancer properties. In the present paper, we show that aqueous extract of Aloe vera is also able to cause DNA degradation in the presence of copper ions. Further, the extract is also able to reduce Cu(II) to Cu(I) and generate reactive oxygen species, such as superoxide anion and hydroxyl radicals in a dose-dependent manner, which correlates with ability of the extract to cause DNA breakage. Thus, the study shows that in addition to antioxidant activity, Aloe vera extract also possess pro-oxidant properties, leading to oxidative DNA breakage.

  19. submitter Light Extraction From Scintillating Crystals Enhanced by Photonic Crystal Structures Patterned by Focused Ion Beam

    CERN Document Server

    Modrzynski, Pawel; Knapitsch, Arno; Kunicki, Piotr; Lecoq, Paul; Moczala, Magdalena; Papakonstantinou, Ioannis; Auffray, Etiennette

    2016-01-01

    “Photonic Crystals (PhC)” have been used in a variety of fields as a structure for improving the light extraction efficiency from materials with high index of refraction. In previous work we already showed the light extraction improvement of several PhC covered LYSO crystals in computer simulations and practical measurements. In this work, new samples are made using different materials and techniques which allows further efficiency improvements. For rapid prototyping of PhC patterns on scintillators we tested a new method using “Focused Ion Beam (FIB)” patterning. The FIB machine is a device similar to a “Scanning Electron Microscope (SEM)”, but it uses ions (mainly gallium) instead of electrons for the imaging of the samples' surface. The additional feature of FIB devices is the option of surface patterning in nano-scale which was exploited for our samples. Three samples using FIB patterning have been produced. One of them is a direct patterning of the extraction face of a 0.8×0.8×10 $mm^3$ LYS...

  20. Studies of extraction and transport system for highly charged ion beam of 18 GHz superconducting electron cyclotron resonance ion source at Research Center for Nuclear Physics.

    Science.gov (United States)

    Yorita, T; Hatanaka, K; Fukuda, M; Ueda, H; Yasuda, Y; Morinobu, S; Tamii, A; Kamakura, K

    2014-02-01

    An 18 GHz superconducting electron cyclotron resonance ion source is installed to increase beam currents and to extend the variety of ions especially for highly charged heavy ions which can be accelerated by cyclotrons of Research Center for Nuclear Physics (RCNP), Osaka University. The beam production developments of several ions from B to Xe have been already done [T. Yorita, K. Hatanaka, M. Fukuda, M. Kibayashi, S. Morinobu, H.Okamura, and A. Tamii, Rev. Sci. Instrum. 79, 02A311 (2008) and T. Yorita, K. Hatanaka, M. Fukuda, M. Kibayashi, S. Morinobu, H.Okamura, and A. Tamii, Rev. Sci. Instrum. 81, 02A332 (2010)] and the further studies for those beam extraction and its transport have been done in order to increase the beam current more. The plasma electrode, extraction electrode, and einzel lens are modified. Especially extraction electrode can be applied minus voltage for the beam extraction and it works well to improve the extracted beam current. The extraction voltage dependences of transmission and emittance also have been studied for beam current improvement which is injected into azimuthally varying field cyclotron at RCNP.

  1. Studies of extraction and transport system for highly charged ion beam of 18 GHz superconducting electron cyclotron resonance ion source at Research Center for Nuclear Physics

    Science.gov (United States)

    Yorita, T.; Hatanaka, K.; Fukuda, M.; Ueda, H.; Yasuda, Y.; Morinobu, S.; Tamii, A.; Kamakura, K.

    2014-02-01

    An 18 GHz superconducting electron cyclotron resonance ion source is installed to increase beam currents and to extend the variety of ions especially for highly charged heavy ions which can be accelerated by cyclotrons of Research Center for Nuclear Physics (RCNP), Osaka University. The beam production developments of several ions from B to Xe have been already done [T. Yorita, K. Hatanaka, M. Fukuda, M. Kibayashi, S. Morinobu, H.Okamura, and A. Tamii, Rev. Sci. Instrum. 79, 02A311 (2008) and T. Yorita, K. Hatanaka, M. Fukuda, M. Kibayashi, S. Morinobu, H.Okamura, and A. Tamii, Rev. Sci. Instrum. 81, 02A332 (2010)] and the further studies for those beam extraction and its transport have been done in order to increase the beam current more. The plasma electrode, extraction electrode, and einzel lens are modified. Especially extraction electrode can be applied minus voltage for the beam extraction and it works well to improve the extracted beam current. The extraction voltage dependences of transmission and emittance also have been studied for beam current improvement which is injected into azimuthally varying field cyclotron at RCNP.

  2. Studies of extraction and transport system for highly charged ion beam of 18 GHz superconducting electron cyclotron resonance ion source at Research Center for Nuclear Physics

    Energy Technology Data Exchange (ETDEWEB)

    Yorita, T., E-mail: yorita@rcnp.osaka-u.ac.jp; Hatanaka, K.; Fukuda, M.; Ueda, H.; Yasuda, Y.; Morinobu, S.; Tamii, A.; Kamakura, K. [Research Center for Nuclear Physics (RCNP), Osaka University, Osaka 567-0047 (Japan)

    2014-02-15

    An 18 GHz superconducting electron cyclotron resonance ion source is installed to increase beam currents and to extend the variety of ions especially for highly charged heavy ions which can be accelerated by cyclotrons of Research Center for Nuclear Physics (RCNP), Osaka University. The beam production developments of several ions from B to Xe have been already done [T. Yorita, K. Hatanaka, M. Fukuda, M. Kibayashi, S. Morinobu, H.Okamura, and A. Tamii, Rev. Sci. Instrum. 79, 02A311 (2008) and T. Yorita, K. Hatanaka, M. Fukuda, M. Kibayashi, S. Morinobu, H.Okamura, and A. Tamii, Rev. Sci. Instrum. 81, 02A332 (2010)] and the further studies for those beam extraction and its transport have been done in order to increase the beam current more. The plasma electrode, extraction electrode, and einzel lens are modified. Especially extraction electrode can be applied minus voltage for the beam extraction and it works well to improve the extracted beam current. The extraction voltage dependences of transmission and emittance also have been studied for beam current improvement which is injected into azimuthally varying field cyclotron at RCNP.

  3. Organic acids and inorganic anions in Bayer liquors by ion chromatography after solid-phase extraction

    Institute of Scientific and Technical Information of China (English)

    ZHONG Fu-jin; CHEN Xiao-qing; ZHANG Shu-chao; LI Yue-ping

    2007-01-01

    A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate,glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.

  4. Chemical Extraction Preparation of Delithiated Cathode Materials of Li-ion Battery

    Institute of Scientific and Technical Information of China (English)

    YAN Shijian; ZHANG Mingang; CHAI Yuesheng; TIAN Wenhuai

    2009-01-01

    A method of conventional chemical reaction to prepare delithiated cathode materials of Li-ion battery was introduced.The cathode material of Li-ion battery was mixed with oxidizing agent Na_2S_2O_8 in water solution,and the solution was stirred continuously to make the chemical re-action proceed sufficiently,then the reaction product was filtered and finally the insoluble delithiated cathode material was obtained.A series of tests were conducted to verify the composition,crystal structure and electrochemical property of the delithiated cathode materials were all desirable.This method overcomes the shortcomings of battery charging preparation and chemical extraction prepa-ration employing other oxidizing agents.

  5. Ion Exchange and Solvent Extraction: Supramolecular Aspects of Solvent Exchange Volume 21

    Energy Technology Data Exchange (ETDEWEB)

    Gloe, Karsten [Technischen Universität Dresden; Tasker, Peter A [ORNL; Oshima, Tatsuya [University of Miyazaki; Watarai, Hitoshi [Institute for NanoScience Design at Osaka University; Nilsson, Mikael [University of California, Irvine

    2013-01-01

    Preface The theme of supramolecular chemistry (SC), entailing the organization of multiple species through noncovalent interactions, has permeated virtually all aspects of chemical endeavor over the past several decades. Given that the observed behavior of discrete molecular species depends upon their weak interactions with one another and with matrix components, one would have to conclude that SC must indeed form part of the fabric of chemistry itself. A vast literature now serves to categorize SC phenomena within a body of consistent terminology. The word supramolecular itself appears in the titles of dozens of books, several journals, and a dedicated encyclopedia. Not surprisingly, the theme of SC also permeates the field of solvent extraction (SX), inspiring the framework for this volume of Ion Exchange and Solvent Extraction. It is attempted in the six chapters of this volume to identify both how supramolecular behavior occurs and is studied in the context of SX and how SC is influencing the current direction of SX. Researchers and practitioners have long dealt with supramolecular interactions in SX. Indeed, the use of polar extractant molecules in nonpolar media virtually assures that aggregative interactions will dominate the solution behavior of SX. Analytical chemists working in the 1930s to the 1950s with simple mono- and bidentate chelating ligands as extractants noted that extraction of metal ions obeyed complicated mass-action equilibria involving complex stoichiometries. As chemists and engineers developed processes for nuclear and hydrometallurgical applications in the 1950s and 1960s, the preference for aliphatic diluents only enhanced the complexity and supramolecular nature of extraction chemistry. Use of physical techniques such as light scattering and vapor-pressure measurements together with various spectroscopic methods revealed organic-phase aggregates from well-defined dimers to small aggregates containing a few extractant molecules to large

  6. Preliminary results of the ion extraction simulations applied to the MONO1000 and SUPERSHyPIE electron cyclotron resonance ion sources.

    Science.gov (United States)

    Pierret, C; Maunoury, L; Biri, S; Pacquet, J Y; Tuske, O; Delferriere, O

    2008-02-01

    The goal of this article is to present simulations on the extraction from an electron cyclotron resonance ion source (ECRIS). The aim of this work is to find out an extraction system, which allows one to reduce the emittances and to increase the current of the extracted ion beam at the focal point of the analyzing dipole. But first, we should locate the correct software which is able to reproduce the specific physics of an ion beam. To perform the simulations, the following softwares have been tested: SIMION 3D, AXCEL, CPO 3D, and especially, for the magnetic field calculation, MATHEMATICA coupled with the RADIA module. Emittance calculations have been done with two types of ECRIS: one with a hexapole and one without a hexapole, and the difference will be discussed.

  7. Preliminary results of the ion extraction simulations applied to the MONO1000 and SUPERSHyPIE electron cyclotron resonance ion sourcesa)

    Science.gov (United States)

    Pierret, C.; Maunoury, L.; Biri, S.; Pacquet, J. Y.; Tuske, O.; Delferriere, O.

    2008-02-01

    The goal of this article is to present simulations on the extraction from an electron cyclotron resonance ion source (ECRIS). The aim of this work is to find out an extraction system, which allows one to reduce the emittances and to increase the current of the extracted ion beam at the focal point of the analyzing dipole. But first, we should locate the correct software which is able to reproduce the specific physics of an ion beam. To perform the simulations, the following softwares have been tested: SIMION 3D, AXCEL, CPO 3D, and especially, for the magnetic field calculation, MATHEMATICA coupled with the RADIA module. Emittance calculations have been done with two types of ECRIS: one with a hexapole and one without a hexapole, and the difference will be discussed.

  8. Extraction of 22 TeV/c Lead Ions from the CERN SPS using a Bent Silicon Crystal

    Science.gov (United States)

    Herr, W.; Elsener, K.; Fidecaro, G.; Gyr, M.; Klem, J.; Weisse, E.

    1997-05-01

    The extraction of protons from the halo of a circulating beam has been repeatedly demonstrated at the SPS. In a recent experiment a coasting lead ion beam was available at a momentum of 270 GeV/c/Z corresponding to a total momentum of 22 TeV/c per ion and the possibility to extract ultrarelativistic lead ions with a bent crystal could be demonstrated for the first time. We present the experimental challenges, the measurements performed during this experiment and the first results.

  9. Optimized Extraction of H– by Three-Electrode Faraday Cup System in Magnetized Sheet Plasma Ion Source

    Directory of Open Access Journals (Sweden)

    M. S. Fernandez

    2003-06-01

    Full Text Available A locally designed rectangular parallelepiped, three-electrode Faraday cup system has been developed.Its design incorporates the capability of simultaneous extraction and deposition of the H– ions on substrates.The device functions to attain prescribed selectivity conditions of extracted ions, with controlled energies,for deposition or adsorption. It has been proven to detect the ions at filter bias voltage of 13.61 V with acurrent density of 5.3 A/m2 that is relatively higher than reported (Abate & Ramos, 2000.

  10. Determination of nitrate in lettuce by ion chromatography after microwave water extraction

    Directory of Open Access Journals (Sweden)

    Humberto Brevilato Novaes

    2009-01-01

    Full Text Available Lettuce is worldwide known as the most important vegetable. In this context, most farmers are searching new techniques for best quality products including hydropony. However, nitrate is of great concern, since it has a negative impact on human metabolism. The main objective of the present work was to evaluate the nitrate content of lettuce produced by conventional and hydroponic systems. The determination was conducted by ion chromatography and a new method of extraction was tested using microwave oven digestion. The results indicated that nitrate level produced in the conventional system was lower than in the hydroponic system.

  11. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  12. Investigation on the extraction of strontium ions from aqueous phase using crown ether-ionic liquid systems

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    The extraction of strontium ions using DCH18C6 as the extractant and various ionic liquids(ILs) as solvents has been investigated.The distribution ratio of Sr2+ can reach as high as 103 under certain conditions,much larger than that in DCH18C6/n-octanol system.The extraction capacity depends greatly on the structure of ionic liquids.In Ils-based extraction systems,the extraction efficiency of strontium ions is reduced by increasing the concentration of nitric acid and can also be influenced directly by the presence of Na+ and K+ in the aqueous phase.It is confirmed that the extraction proceeds mainly via a cation-exchange mechanism.

  13. Investigation on the extraction of strontium ions from aqueous phase using crown ether-ionic liquid systems

    Institute of Scientific and Technical Information of China (English)

    XU Chao; SHEN XingHai; CHEN QingDe; GAO HongCheng

    2009-01-01

    The extraction of strontium ions using DCH18C6 as the extractant and various ionic liquids (Ils) as solvents has been investigated.The distribution ratio of Sr~(2+) can reach as high as 10~3 under certain conditions,much larger than that in DCH18C6/n-octanol system.The extraction capacity depends greatly on the structure of ionic liquids.In Ils-based extraction systems,the extraction efficiency of strontium ions is reduced by increasing the concentration of nitric acid and can also be influenced directly by the presence of Na~+ and K~+ in the aqueous phase.It is confirmed that the extraction proceeds mainly via a cation-exchange mechanism.

  14. Combined effects of sugarcane bagasse extract and Zinc(II) ions on the growth and bioaccumulation properties of yeast isolates.

    OpenAIRE

    Geetanjali Basak; CHARUMATHI D; NILANJANA DAS

    2011-01-01

    Bioaccumulation of zinc(II) ions by yeast isolates viz. Candida rugosa and Cryptococcus laurentii was investigated in different growth media. Both the isolates showed maximum bioaccumulation of zinc(II) in the medium prepared from sugarcane bagasse extract. The growth and zinc(II) bioaccumulation properties of yeasts in sugar cane bagasse extract were tested as a function of pH, temperature and initial metal concentrations. The combined effects of sugar extracted from bagasse and initial zinc...

  15. Complex-forming organic ligands in cloud-point extraction of metal ions: a review.

    Science.gov (United States)

    Pytlakowska, K; Kozik, V; Dabioch, M

    2013-06-15

    Cloud-point extraction (CPE), an easy, safe, environmentally friendly, rapid and inexpensive methodology for preconcentration and separation of trace metals from aqueous solutions has recently become an attractive area of research and an alternative to liquid-liquid extraction. Moreover, it provides results comparable to those obtained with other separation techniques and has a greater potential to be explored in improving detection limits and other analytical characteristics over other methods. A few reviews have been published covering different aspects of the CPE procedure and its relevant applications, such as the phenomenon of clouding, the application in the extraction of trace inorganic and organic materials, as well as pesticides and protein substrates from different sources, or incorporation of CPE into an FIA system. This review focuses on general properties of the most frequently used organic ligands in cloud-point extraction and on literature data (from 2000 to 2012) concerning the use of modern techniques in determination of metal ions' content in various materials. The article is divided according to the class of organic ligands to be used in CPE.

  16. Selective metal ion extraction for multiple ion liquid-liquid exchange reactions. Progress report, DE-AS02-79ER 10406. A001

    Energy Technology Data Exchange (ETDEWEB)

    Tavlarides, L.L.

    1980-01-01

    The first phase of selecting a model binary system to study was completed. The system selected is Cu(II), Fe(III) acid sulfate solutions extracted by ..beta..-alkenyl 8-hydroxy quinoline (Kelex 100) in xylene. Maximum copper extraction occurs in less than 5 minutes at 30 to 50/sup 0/C. Thermodynamic chemical equilibrium studies with the Fe(III) ion indicate that the ionic charge of the extracted ion is +3 over a limited pH and concentration range. A simplified equilibrium model did not fit the experimental data. A chemical equilibrium model for the aqueous phase was developed. Kinetic studies on the liquid jet recycle reactor are underway. The model proposed to analyze simultaneous extraction of Cu(II) and Fe(III) in a stirred tank extractor was reduced to a set of two nonlinear algebraic equations for idealized kinetic expressions.

  17. Single element of the matrix source of negative hydrogen ions: Measurements of the extracted currents combined with diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Yordanov, D., E-mail: yordanov@phys.uni-sofia.bg; Lishev, St.; Shivarova, A. [Faculty of Physics, Sofia University, BG-1164 Sofia (Bulgaria)

    2016-02-15

    Combining measurements of the extracted currents with probe and laser-photodetachment diagnostics, the study is an extension of recent tests of factors and gas-discharge conditions stimulating the extraction of volume produced negative ions. The experiment is in a single element of a rf source with the design of a matrix of small-radius inductively driven discharges. The results are for the electron and negative-ion densities, for the plasma potential and for the electronegativity in the vicinity of the plasma electrode as well as for the currents of the extracted negative ions and electrons. The plasma-electrode bias and the rf power have been varied. Necessity of a high bias to the plasma electrode and stable linear increase of the extracted currents with the rf power are the main conclusions.

  18. Removal of Heavy Metal Ions by using Calcium Carbonate Extracted from Starfish Treated by Protease and Amylase

    Directory of Open Access Journals (Sweden)

    Kyong-Soo Hong

    2011-10-01

    Full Text Available CaCO3 extracted from starfish by using the commercial protein lyase having α-amylase, β-amylase, and protease is applied to remove heavy metal ions. The extracted CaCO3 shows excellent characteristics in removing heavy metal ions such as Cu2+, Cd2+, Pb2+, and Cr6+ compared with conventional materials such as crab shells, sawdust, and activated carbon except for removing Zn2+. SEM images reveal that the extracted CaCO33 has a good morphology and porosity. We characterize the removal efficiencies of the extracted CaCO3 for the heavy metal ions according to the concentrations, pH, temperatures, and conditions of empty bed contact times.

  19. Asparagus cochinchinensis Extract Alleviates Metal Ion-Induced Gut Injury in Drosophila: An In Silico Analysis of Potential Active Constituents

    Directory of Open Access Journals (Sweden)

    Weiyu Zhang

    2016-01-01

    Full Text Available Metal ions and sulfate are components of atmospheric pollutants that have diverse ways of entering the human body. We used Drosophila as a model to investigate the effect of Asparagus cochinchinensis (A. cochinchinensis extracts on the gut and characterized gut homeostasis following the ingestion of metal ions (copper, zinc, and aluminum. In this study, we found that the aqueous A. cochinchinensis extract increased the survival rate, decreased epithelial cell death, and attenuated metal ion-induced gut morphological changes in flies following chronic exposure to metal ions. In addition, we screened out, by network pharmacology, six natural products (NPs that could serve as putative active components of A. cochinchinensis that prevented gut injury. Altogether, the results of our study provide evidence that A. cochinchinensis might be an effective phytomedicine for the treatment of metal ion-induced gut injury.

  20. Radiolytic stability of some recently developed ion exchange and extraction chromatographic resins containing diphosphonic acid groups

    Energy Technology Data Exchange (ETDEWEB)

    Chiarizia, R.; Horwitz, E.P.

    2000-01-01

    The effect of {sup 60}Co irradiation on the Diphonix{trademark}, Diphosil and Diphonix-CS chelating ion exchange resins, and on two Dipex{trademark} extraction chromatographic resins containing the P,P{prime}-di(2-ethylhexyl) methanediphosphonic acid (H{sub 2}DEH[MDP]) impregnated in the pores of a polymeric support (Dipex-1) and of silica (Dipex-2), respectively, has been investigated. The resins have been irradiated while in contact with HNO{sub 3} (Diphonix, Diphosil and Dipex resins) or NaOH (Diphonix-DS resin) up to an absorbed dose of about 200 Mrad. As a probe of the resin radiolytic degradation, metal uptake (both equilibrium and kinetics) and capacity measurements have been performed. Results show that the Diphonix-CS resin properties are practically unaffected by irradiation under the experimental conditions used in this work. The Diphonix, Diphosil, and especially the Dipex resins suffer substantial capacity losses, but their affinity for actinide ions is not seriously compromised. On the other hand, the kinetics of metal uptake by the silica based Diphosil and Dipex-2 resins becomes substantially slower indicating that, from a radiolytic degradation standpoint, polymeric materials perform better than silica as supports for H{sub 2}DEH[MDP] containing extraction chromatographic resins.

  1. Interstitial and Interlayer Ion Diffusion Geometry Extraction in Graphitic Nanosphere Battery Materials

    Energy Technology Data Exchange (ETDEWEB)

    Gyulassy, Attila; Knoll, Aaron; Lau, Kah Chun; Wang, Bei; Bremer, Peer-Timo; Papka, Michael E.; Curtiss, Larry A.; Pascucci, Valerio

    2016-01-01

    Large-scale molecular dynamics (MD) simulations are commonly used for simulating the synthesis and ion diffusion of battery materials. A good battery anode material is determined by its capacity to store ion or other diffusers. However, modeling of ion diffusion dynamics and transport properties at large length and long time scales would be impossible with current MD codes. To analyze the fundamental properties of these materials, therefore, we turn to geometric and topological analysis of their structure. In this paper, we apply a novel technique inspired by discrete Morse theory to the Delaunay triangulation of the simulated geometry of a thermally annealed carbon nanosphere. We utilize our computed structures to drive further geometric analysis to extract the interstitial diffusion structure as a single mesh. Our results provide a new approach to analyze the geometry of the simulated carbon nanosphere, and new insights into the role of carbon defect size and distribution in determining the charge capacity and charge dynamics of these carbon based battery materials.

  2. Ability of freshwater fish to extract oxygen at different hydrogen-ion concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Wiebe, A.H.; McGavock, A.M.; Fuller, A.C.; Markus, H.C.

    1934-01-01

    Pruthi's observations on the stickleback at pH 3.1 have been confirmed for the stickleback as well as several other species of fresh-water fish. Pruthi's criticism of the work of Powers is invalid within the pH range to which the fish are acclimated. The initial oxygen has either no effect on the lethal oxygen or the effect is in the opposite direction from that suggested by Pruthi. Outside of the pH range normal to the species in question the lethal oxygen is dependent in a large measure on the initial oxygen. Several species of freshwater fish--largemouth blackbass, smallmouth blackbass, white crappie, yellow perch, rainbow trout, as well as the goldfish and green sunfish--have the ability to extract oxygen from the water at low oxygen tensions equally well over a fairly wide range of hydrogen-ion concentration. The bluegill has a somewhat narrower range of toleration. The two species of minnow--steel-colored and bluntnose--tolerate a markedly narrower range of difference in hydrogen-ion concentration as shown by the lethal oxygen. The ability of fish to extract oxygen from the water at low pressure depends more or less on the hydrogen-ion concentration of water. The results obtained in this investigation confirm the studies on pH tolerance of fish previously published. These results also confirm the observations that in highly alkaline water fish require a higher concentration of oxygen to survive.

  3. Extraction of copper(II) ions from aqueous solutions with a methimazole-based ionic liquid.

    Science.gov (United States)

    Reyna-González, Juan M; Torriero, Angel A J; Siriwardana, Amal I; Burgar, Iko M; Bond, Alan M

    2010-09-15

    The recently synthesized ionic liquid (IL) 2-butylthiolonium bis(trifluoromethanesulfonyl)amide, [mimSBu][NTf(2)], has been used for the extraction of copper(II) from aqueous solution. The pH of the aqueous phase decreases upon addition of [mimSBu](+), which is attributed to partial release of the hydrogen attached to the N(3) nitrogen atom of the imidazolium ring. The presence of sparingly soluble water in [mimSBu][NTf(2)] also is required in solvent extraction studies to promote the incorporation of Cu(II) into the [mimSBu][NTf(2)] ionic liquid phase. The labile copper(II) system formed by interacting with both the water and the IL cation component has been characterized by cyclic voltammetry as well as UV-vis, Raman, and (1)H, (13)C, and (15)N NMR spectroscopies. The extraction process does not require the addition of a complexing agent or pH control of the aqueous phase. [mimSBu][NTf(2)] can be recovered from the labile copper-water-IL interacting system by washing with a strong acid. High selectivity of copper(II) extraction is achieved relative to that of other divalent cobalt(II), iron(II), and nickel(II) transition-metal cations. The course of microextraction of Cu(2+) from aqueous media into the [mimSBu][NTf(2)] IL phase was monitored in situ by cyclic voltammetry using a well-defined process in which specific interaction with copper is believed to switch from the ionic liquid cation component, [mimSBu], to the [NTf(2)] anion during the course of electrochemical reduction from Cu(II) to Cu(I). The microextraction-voltammetry technique provides a fast and convenient method to determine whether an IL is able to extract electroactive metal ions from an aqueous solution.

  4. Extraction of negative charges from an ion source: Transition from an electron repelling to an electron attracting plasma close to the extraction surface

    Science.gov (United States)

    Wimmer, Christian; Fantz, Ursel

    2016-08-01

    Large-scale sources for negative hydrogen ions, capable of delivering an extracted ion current of several ten amperes, are a key component of the neutral beam injection system of the upcoming ITER fusion device. Since the created heat load of the inevitably co-extracted electrons after magnetic separation from the extracted beam limits their tolerable amount, special care must be taken for the reduction of co-extracted electrons—in particular, in deuterium operation, where the larger amount of co-extracted electrons often limits the source performance. By biasing the plasma grid (PG, first grid of the extraction system) positively with respect to the source body, the plasma sheath in front of the PG can be changed from an electron repelling towards an electron attracting sheath. In this way, the flux of charged particles onto the PG can be varied, thus changing the bias current and inverse to it the amount of co-extracted electrons. The PG bias affects also the flux of surface-produced H - towards the plasma volume as well as the plasma symmetry in front of the plasma grid, strongly influenced by an E → × B → drift. The influence of varying PG sheath potential profile on the plasma drift, the negative hydrogen ion density, and the source performance at the prototype H - source is presented, comparing hydrogen and deuterium operation. The transition in the PG sheath profile takes place in both isotopes, with a minimum of co-extracted electrons formed in case of the electron attracting PG sheath. The co-extracted electron density in deuterium operation is higher than in hydrogen operation, which is accompanied by an increased plasma density in deuterium.

  5. Beam size reduction of a several hundred-keV compact ion microbeam system by improving the extraction condition in an ion source

    Energy Technology Data Exchange (ETDEWEB)

    Ishii, Yasuyuki; Ohkubo, Takeru; Kamiya, Tomihiro; Saitoh, Yuichi

    2015-04-01

    A several hundred-keV compact ion microbeam system with a three-stage acceleration lens has been developed to form an ion beam of several micrometers in diameter. In a previous study of the Ohkubo et al. (2013) and Ishii et al. (2014), a hydrogen beam of 143 keV having 17 μm diameter was experimentally formed using such a microbeam system. It was demonstrated that a three-stage acceleration lens functioned as a focusing lens and indicated that the beam diameter (hereinafter referred to as the “beam size”) depended on the extraction voltage to generate the ion beam and the vacuum pressure in the extraction space in a plasma-type ion source. In this study, the hydrogen beam sizes were experimentally measured at 130 keV as functions of the extraction voltage and vacuum pressure to form the beam size with several micrometers in diameter. These two relationships showed that beam sizes were reduced in the extraction voltage range of 400–500 V and when the vacuum pressure was lowered to a minimum value of 5.33 × 10{sup −5} Pa. In addition, the result showed that the beam size was dominantly influenced by the vacuum pressure. Consequently, a hydrogen beam 5.8 μm in diameter was formed experimentally—the smallest beam yet obtained.

  6. Amyloid β Ion Channels in a Membrane Comprising Brain Total Lipid Extracts.

    Science.gov (United States)

    Lee, Joon; Kim, Young Hun; T Arce, Fernando; Gillman, Alan L; Jang, Hyunbum; Kagan, Bruce L; Nussinov, Ruth; Yang, Jerry; Lal, Ratnesh

    2017-02-20

    Amyloid β (Aβ) oligomers are the predominant toxic species in the pathology of Alzheimer's disease. The prevailing mechanism for toxicity by Aβ oligomers includes ionic homeostasis destabilization in neuronal cells by forming ion channels. These channel structures have been previously studied in model lipid bilayers. In order to gain further insight into the interaction of Aβ oligomers with natural membrane compositions, we have examined the structures and conductivities of Aβ oligomers in a membrane composed of brain total lipid extract (BTLE). We utilized two complementary techniques: atomic force microscopy (AFM) and black lipid membrane (BLM) electrical recording. Our results indicate that Aβ1-42 forms ion channel structures in BTLE membranes, accompanied by a heterogeneous population of ionic current fluctuations. Notably, the observed current events generated by Aβ1-42 peptides in BTLE membranes possess different characteristics compared to current events generated by the presence of Aβ1-42 in model membranes comprising a 1:1 mixture of DOPS and POPE lipids. Oligomers of the truncated Aβ fragment Aβ17-42 (p3) exhibited similar ion conductivity behavior as Aβ1-42 in BTLE membranes. However, the observed macroscopic ion flux across the BTLE membranes induced by Aβ1-42 pores was larger than for p3 pores. Our analysis of structure and conductance of oligomeric Aβ pores in a natural lipid membrane closely mimics the in vivo cellular environment suggesting that Aβ pores could potentially accelerate the loss of ionic homeostasis and cellular abnormalities. Hence, these pore structures may serve as a target for drug development and therapeutic strategies for AD treatment.

  7. Partial alkali-metal ion extraction from K0.8(Li0.27Ti1.73)O4 using PTFE as an extraction reagent.

    Science.gov (United States)

    Ozawa, Tadashi C; Sasaki, Takayoshi

    2014-10-21

    The alkali-metal ion extraction ability of an inert material, polytetrafluoroethylene (PTFE; empirical formula CF2), was clarified by characterizing a partially alkali-metal ion-extracted layered compound, K0.8(Li0.27Ti1.73)O4. Washing K0.8(Li0.27Ti1.73)O4 in water extracts only 44% of the interlayer K(+) and no intralayer Li(+); on the other hand, 53% of the interlayer K(+) and approximately 10% of the intralayer Li(+) ions were extracted from K0.8(Li0.27Ti1.73)O4 by the reaction with PTFE at 350 °C under flowing Ar. A systematic decrease in the lattice parameters a and c along the intralayer directions and an increase in b along the interlayer direction were observed, consistent with the alkali-metal ion deintercalation amount as a function of the reaction temperatures and the reacted PTFE amounts. After the reaction with K0.8(Li0.27Ti1.73)O4 : CF2 = 1 : 0.6 in mol, the lattice parameter b increased to 1.5607(3) nm from 1.5522(2) of the pristine K0.8(Li0.27Ti1.73)O4, and this change in the lattice parameter was approximately one order of magnitude larger than those in a and c.

  8. Synthesis and application of ion-imprinted polymer for extraction and pre-concentration of iron ions in environmental water and food samples.

    Science.gov (United States)

    Roushani, Mahmoud; Beygi, Tahereh Musa; Saedi, Zahra

    2016-01-15

    In this work, a novel Fe(III) ion imprinted polymer as a sorbent for extraction of iron ions from different samples was synthesized. Precipitation of thermal copolymerization was used for preparation of polymeric sorbent. In this technique, methacrylic acid, ethylene glycoldimethacrylate, 2,2'-azobisisobutyronitrile and (DHBPT)2 {(DHBPT)2=3,6-bis (3,5-dimethyl-1-H-pyrzol-1-yl)-1,2-dihydro-1,2,4,5-tetrazine)} were used as monomer, cross-linker, initiator and ligand, respectively, in the presence of Fe(III) ions and ethanol as a porogenic solvent. Moreover, control polymer (NIP) particles were similarly prepared without the Fe(III) ions. XRD, FT-IR, SEM and nitrogen adsorption-desorption techniques have been used to characterization of these prepared polymeric samples. Iron ion imprinted polymer particles, abbreviated as Fe(III)-IIP, were leached with 50 mL of HCl (50% (v/v)). Absorption capacity for ion imprinted polymer was calculated about 40.41 mg·g(-1). Per-concentration of iron ion was investigated as a function of pH, weight of IIP, adsorption and desorption times, and volumes of sample. FAAS technique was used to determination of Fe(III) ion in the foods and waters samples.

  9. Direct 16S rRNA gene sequencing of polymicrobial culture-negative samples with analysis of mixed chromatograms

    DEFF Research Database (Denmark)

    Hartmeyer, Gitte N; Justesen, Ulrik S

    2010-01-01

    Two cases involving polymicrobial culture-negative samples were investigated by 16S rRNA gene sequencing, with analysis of mixed chromatograms. Fusobacterium necrophorum, Prevotella intermedia and Streptococcus constellatus were identified from pleural fluid in a patient with Lemierre's syndrome...

  10. Recent Progress in the Development of Supercritical Carbon Dioxide-Soluble Metal Ion Extractants: Aggregation, Extraction, and Solubility Properties of Silicon-Substituted Alkylenediphosphonic Acids

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, Mark L.; McAlister, Daniel R.; Stepinski, Dominique C.; Zalupski, Peter R.; Dzilawa, Julie A.; Barrans, Richard E.; Hess, J.N.; Rubas, Audris V.; Chiarizia, Renato; Lubbers, Christopher M.; Scurto, Aaron M.; Brennecke, Joan F.; Herlinger, Albert W.

    2003-09-11

    Partially esterified alkylenediphosphonic acids (DPAs) have been shown to be effective reagents for the extraction of actinide ions from acidic aqueous solution into conventional organic solvents. Efforts to employ these compounds in supercritical fluid extraction have been hampered by their modest solubility in unmodified supercritical carbon dioxide (SC-CO2). In an effort to design DPAs that are soluble in SC-CO2, a variety of silicon-substituted alkylenediphosphonic acids have been prepared and characterized, and their behavior compared with that of conventional alkyl-substituted reagents. Silicon substitution is shown to enhance the CO2-philicity of the reagents, while other structural features, in particular, the number of methylene groups bridging the phosphorus atoms of the extractant, are shown to exert a significant influence on their aggregation and extraction properties. The identification of DPAs combining desirable extraction properties with adequate solubility in SC-CO2 is shown to be facilitated by the application of molecular connectivity indices.

  11. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  12. Continuous protein recovery from whey using liquid-solid circulating fluidized bed ion-exchange extraction.

    Science.gov (United States)

    Lan, Qingdao; Bassi, Amarjeet; Zhu, Jing-Xu Jesse; Margaritis, Argyrios

    2002-04-20

    A liquid-solid circulating fluidized bed (LSCFB) continuous ion-exchange extraction system has been investigated for total protein recovery from whey solutions under various operating conditions. The effectiveness of a dynamic seal was evaluated between the riser and the downcomer, and the best conditions for the establishment of this seal were established. Start-up studies indicated that the system is robust and stable. Under optimal conditions, a productivity of 8.2 g of total protein removed per hour per kilogram of resin was achieved with a protein removal efficiency of 78.4%. However, higher overall protein recovery of up to 90% was also achieved under other conditions, with lower protein concentration in the effluent and a lower overall productivity.

  13. Characterization of a metastable neon beam extracted from a commercial RF ion source

    CERN Document Server

    Ohayon, B; Ron, G

    2015-01-01

    We have used a commercial RF ion-source to extract a beam of metastable neon atoms. The source was easily incorporated into our existing system and was operative within a day of installation. The metastable velocity distribution, flux, flow, and efficiency were investigated for different RF powers and pressures, and an optimum was found at a flux density of $2\\times10^{12}\\,$atoms/s/sr. To obtain an accurate measurement of the amount of metastable atoms leaving the source, we insert a Faraday cup in the beam line and quench some of them using a weak $633\\,$nm laser beam. In order to determine how much of the beam was quenched before reaching our detector, we devised a simple model for the quenching transition and investigated it for different laser powers. This detection method can be easily adapted to other noble gas atoms.

  14. Upgrade of the beam extraction system of the GTS-LHC electron cyclotron resonance ion source at CERN.

    Science.gov (United States)

    Toivanen, V; Bellodi, G; Dimov, V; Küchler, D; Lombardi, A M; Maintrot, M

    2016-02-01

    Linac3 is the first accelerator in the heavy ion injector chain of the Large Hadron Collider (LHC), providing multiply charged heavy ion beams for the CERN experimental program. The ion beams are produced with GTS-LHC, a 14.5 GHz electron cyclotron resonance ion source, operated in afterglow mode. Improvement of the GTS-LHC beam formation and beam transport along Linac3 is part of the upgrade program of the injector chain in preparation for the future high luminosity LHC. A mismatch between the ion beam properties in the ion source extraction region and the acceptance of the following Low Energy Beam Transport (LEBT) section has been identified as one of the factors limiting the Linac3 performance. The installation of a new focusing element, an einzel lens, into the GTS-LHC extraction region is foreseen as a part of the Linac3 upgrade, as well as a redesign of the first section of the LEBT. Details of the upgrade and results of a beam dynamics study of the extraction region and LEBT modifications will be presented.

  15. Calix[4]pyrrole derivative: recognition of fluoride and mercury ions and extracting properties of the receptor-based new material.

    Science.gov (United States)

    de Namor, Angela F Danil; Khalife, Rasha

    2008-12-11

    A calix[4]pyrrole derivative, namely, meso-tetramethyl tetrakis (4-phenoxy methyl ketone) calix[4]pyrrole, 1, was synthesized and structurally (1H NMR) and thermodynamically characterized. The complexing properties of this receptor with a wide variety of anions and cations in dipolar aprotic media (acetonitrile, propylene carbonate, and dimethyl sulfoxide) were investigated through 1H NMR and conductance studies. The former technique was used to assess whether or not complexation occurs and if so to identify the active sites of interaction of 1 with ions. The composition of the complexes was established by conductance measurements. It was found that in dipolar aprotic solvents, 1 interacts only with two polluting ions (fluoride and mercury). The complexation thermodynamics of 1 and these ions in these solvents is reported. The medium effect on the binding process involving the fluoride ion is discussed taking into account the solvation properties of reactants and the product. Complexes of moderate stability are found. Given that this is an important factor to consider for the recycling of the loaded material in extraction processes, 1 was treated with formaldehyde in basic medium leading to the production of a calix[4]pyrrole based material able to extract fluoride and mercury (II) ions from water. Thus the optimum conditions for the extraction of these ions from aqueous solutions were established. The material is easily recyclable using an organic acid. Final conclusions are given.

  16. Upgrade of the beam extraction system of the GTS-LHC electron cyclotron resonance ion source at CERN

    Science.gov (United States)

    Toivanen, V.; Bellodi, G.; Dimov, V.; Küchler, D.; Lombardi, A. M.; Maintrot, M.

    2016-02-01

    Linac3 is the first accelerator in the heavy ion injector chain of the Large Hadron Collider (LHC), providing multiply charged heavy ion beams for the CERN experimental program. The ion beams are produced with GTS-LHC, a 14.5 GHz electron cyclotron resonance ion source, operated in afterglow mode. Improvement of the GTS-LHC beam formation and beam transport along Linac3 is part of the upgrade program of the injector chain in preparation for the future high luminosity LHC. A mismatch between the ion beam properties in the ion source extraction region and the acceptance of the following Low Energy Beam Transport (LEBT) section has been identified as one of the factors limiting the Linac3 performance. The installation of a new focusing element, an einzel lens, into the GTS-LHC extraction region is foreseen as a part of the Linac3 upgrade, as well as a redesign of the first section of the LEBT. Details of the upgrade and results of a beam dynamics study of the extraction region and LEBT modifications will be presented.

  17. Numerical modeling of the Linac4 negative ion source extraction region by 3D PIC-MCC code ONIX

    CERN Document Server

    Mochalskyy, S; Minea, T; Lifschitz, AF; Schmitzer, C; Midttun, O; Steyaert, D

    2013-01-01

    At CERN, a high performance negative ion (NI) source is required for the 160 MeV H- linear accelerator Linac4. The source is planned to produce 80 mA of H- with an emittance of 0.25 mm mradN-RMS which is technically and scientifically very challenging. The optimization of the NI source requires a deep understanding of the underling physics concerning the production and extraction of the negative ions. The extraction mechanism from the negative ion source is complex involving a magnetic filter in order to cool down electrons’ temperature. The ONIX (Orsay Negative Ion eXtraction) code is used to address this problem. The ONIX is a selfconsistent 3D electrostatic code using Particles-in-Cell Monte Carlo Collisions (PIC-MCC) approach. It was written to handle the complex boundary conditions between plasma, source walls, and beam formation at the extraction hole. Both, the positive extraction potential (25kV) and the magnetic field map are taken from the experimental set-up, in construction at CERN. This contrib...

  18. Code-to-code benchmark tests for 3D simulation models dedicated to the extraction region in negative ion sources

    Science.gov (United States)

    Nishioka, S.; Mochalskyy, S.; Taccogna, F.; Hatayama, A.; Fantz, U.; Minelli, P.

    2017-08-01

    The development of the kinetic particle model for the extraction region in negative hydrogen ion sources is indispensable and helpful to clarify the H- beam extraction physics. Recently, various 3D kinetic particle codes have been developed to study the extraction mechanism. Direct comparison between each other has not yet been done. Therefore, we have carried out a code-to-code benchmark activity to validate our codes. In the present study, the progress in this benchmark activity is summarized. At present, the reasonable agreement with the result by each code have been obtained using realistic plasma parameters at least for the following items; (1) Potential profile in the case of the vacuum condition (2) Temporal evolution of extracted current densities and profiles of electric potential in the case of the plasma consisting of only electrons and positive ions.

  19. Comparative evaluation of actinide ion uptake by polymer inclusion membranes containing TODGA as the carrier extractant.

    Science.gov (United States)

    Mahanty, B N; Raut, D R; Mohapatra, P K; Das, D K; Behere, P G; Afzal, Md

    2014-06-30

    Polymer inclusion membranes (PIM) containing TODGA (N,N,N',N'-tetra-n-octyl diglycolamide) were evaluated for the separation of actinide ions such as Am(3+), Pu(4+), UO2(2+) and Th(4+) from acidic feeds. The PIMs were prepared using cellulose triacetate (CTA) as the polymer matrix and 2-nitrophenyloctyl ether (NPOE) as the plasticizer along with the diglycolamide carrier extractants and were characterized by conventional techniques such as XRD, thermal analysis and AFM. The PIM composition was optimized by a series of studies which involved variation in the CTA, NPOE and carrier concentration which suggested 58% TODGA, 30% NPOE and 12% CTA to be optimum. The uptake studies were carried out using feed solutions containing varying concentrations of nitric acid and showed the trend: Am(3+)>Pu(4+)>Th(4+)>UO2(2+). Transport studies were carried out in a two-compartment cell where nitric acid concentration the feed was varied (1-3M) while the receiver compartment contained alpha-hydroxy-iso-butyric acid (AHIBA). The actinide ion transport efficiencies with TODGA containing PIMs followed the same trend as seen in the uptake studies. The AFM patterns of the PIMs changed when loaded with Eu(3+) carrier (used as a surrogate for Am(3+)) while the regenerated membranes have displayed comparable morphologies. Diffusion coefficient values were experimentally obtained from the transport studies and were found to be 8.89×10(-8) cm(2)/s for Am(3+) transport.

  20. A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

    Science.gov (United States)

    Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

    2016-02-01

    It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure.

  1. Extraction of tetra-oxo anions into a hydrophobic, ionic liquid-based solvent without concomitant ion exchange.

    Energy Technology Data Exchange (ETDEWEB)

    Stepinski, D. C.; Vandegrift, G. F.; Shkrob, I. A.; Wishart, J. F.; Kerr, K.; Dietz, M. L.; Qadah, D. T. D.; Garvey, S. L.; BNL; Univ. of Wisconsin at Milwaukee

    2010-06-16

    Hydrophobic ionic liquids (IL) have the potential to simplify certain separations by serving as both an extraction solvent and an electrolyte for subsequent electrochemical reductions. While IL-based solvents are known to be efficient media for metal ion extraction, separations employing these solvents are frequently complicated by the loss of constituent IL ions to the aqueous phase, resulting in deteriorating performance. In this study, we have examined the extraction of pertechnetate and related tetra-oxo anions from aqueous solutions into IL-based solvents incorporating tetraalkylphosphonium bis[(trifluoromethyl)sulfonyl]imide and a crown ether. In contrast to various previously studied IL-based cation extraction systems, facile anion extraction without significant transfer of the IL ions to the aqueous phase has been observed. In addition, the solvents exhibit high distribution ratios (100-500 for pertechnetate), significant electrical conductivity (>100 ?S/cm), and a wide (4 V) electrochemical window. The results suggest that these solvents may provide the basis for improved approaches to the extraction and recovery of a variety of anions.

  2. Extraction of Tetra-oxo Anions into a Hydrophobic, Ionic Liquid-Based Solvent Without Concomitant Ion Exchange

    Energy Technology Data Exchange (ETDEWEB)

    Stepinski, D.C.; Wishart, J.; Vandegrift, III, G.F.; Shkrob, I.A.; Kerr, K.; Dietz, M.L.; Qadah, D.T.D.; Garvey, S.L.

    2010-06-10

    Hydrophobic ionic liquids (IL) have the potential to simplify certain separations by serving as both an extraction solvent and an electrolyte for subsequent electrochemical reductions. While IL-based solvents are known to be efficient media for metal ion extraction, separations employing these solvents are frequently complicated by the loss of constituent IL ions to the aqueous phase, resulting in deteriorating performance. In this study, we have examined the extraction of pertechnetate and related tetra-oxo anions from aqueous solutions into IL-based solvents incorporating tetraalkylphosphonium bis[(trifluoromethyl)sulfonyl]imide and a crown ether. In contrast to various previously studied IL-based cation extraction systems, facile anion extraction without significant transfer of the IL ions to the aqueous phase has been observed. In addition, the solvents exhibit high distribution ratios (100-500 for pertechnetate), significant electrical conductivity (>100 {micro}S/cm), and a wide ({approx}4 V) electrochemical window. The results suggest that these solvents may provide the basis for improved approaches to the extraction and recovery of a variety of anions.

  3. Characteristics of a betatron core for extraction in a proton-ion medical synchrotron

    CERN Document Server

    Badano, L

    1997-01-01

    Medical synchrotrons for radiation therapy require a very stable extraction of the beam over a period of about one second. The techniques for applying resonant extraction to achieve this long spill can be classified into two groups, those that move the resonance and those that move the beam. The latter has the great advantage of keeping all lattice functions, and hence the resonance conditions, constant. The present report examines the possibility of using a betatron core to accelerate the waiting ion beam by induction into the resonance. The working principle, the proposed characteristics and the expected performances of this device are discussed. The betatron core is a smooth high-inductance device compared to the small quadrupole lenses that are normally used to move the resonance and is therefore better suited to delivering a very smooth spill. The large stored energy in a betatron core compared to a small quadrupole is also a safety feature since it responds less quickly to transients that could send lar...

  4. Recovery of metal values from spent lithium-ion batteries with chemical deposition and solvent extraction

    Science.gov (United States)

    Nan, Junmin; Han, Dongmei; Zuo, Xiaoxi

    This paper describes a new recycling process of metal values from spent lithium-ion batteries (LIBs). After the dismantling of the spent batteries steel crusts, the leaching of battery internal substances with alkaline solution and the dissolving of the residues with H 2SO 4 solution were carried out. Then mass cobalt was chemically deposited as oxalate, and Acorga M5640 and Cyanex272 extracted the small quantities of copper and cobalt, respectively. Lithium was recovered as deposition of lithium carbonate. It is shown that about 90% cobalt was deposited as oxalate with less than 0.5% impurities, and Acorga M5640 and Cyanex272 were efficient and selective for the extraction of copper and cobalt in sulfate solution. Over 98% of the copper and 97% of the cobalt was recovered in the given process. In addition, the waste solution was treated innocuously, and LiCoO 2 positive electrode material with good electrochemical performance was also synthesized by using the recovered compounds of cobalt and lithium as precursors. The process is feasible for the recycling of spent LIBs in scale-up.

  5. [LC-LTQ-Orbitrap analysis on chemical constituents in Scrophulariae Radix extract and their metabolites in rat plasma].

    Science.gov (United States)

    Xu, Duo-Duo; Pang, Huan-Huan; Jiang, Mei-Fang; Jian, Wei-Jie; Wang, Qin-Hui; Sun, Lu; Dong, Zi-Yi; Huang, Jian-Mei

    2016-02-01

    Chemical constituents in extract of Scrophulariae Radix and their metabolites in rat plasma after oral administration were identified by HPLC-LTQ-Orbitrap. Samples were separated by a Venusil MP C₁₈ column using a binary gradient elution. The information on the total ion chromatogram, the extraction chromatogram and the mass spectrogram in a negative mode were synthetically analyzed by comparing the retention time, MS and MS/MS spectra with literature data and some of reference standards to conduct a qualitative study on constituents of Radix Scrophulariae extract in vivo and in vitro. Totally 37 compounds from Scrophularia ningpoensis extract were detected including 12 iridoid glycosides, 20 phenylpropanoids and 5 unknown compounds. In vivo, harpagide, harpagoside and angoroside C were confirmed to enter into the blood in prototype forms. Besides, another 2 prototype compounds and 2 metabolites were detected in rat plasma after oral administration of S. ningpoensis extract. The results are beneficial for the determination of bioactive substances of S. ningpoensis and significant for further studies on S. ningpoensis. Copyright© by the Chinese Pharmaceutical Association.

  6. Determination of chloride in brazilian crude oils by ion chromatography after extraction induced by emulsion breaking.

    Science.gov (United States)

    Robaina, Nicolle F; Feiteira, Fernanda N; Cassella, Alessandra R; Cassella, Ricardo J

    2016-08-01

    The present paper reports on the development of a novel extraction induced by emulsion breaking (EIEB) method for the determination of chloride in crude oils. The proposed method was based on the formation and breaking of oil-in-water emulsions with the samples and the consequential transference of the highly water-soluble chloride to the aqueous phase during emulsion breaking, which was achieved by centrifugation. The determination of chloride in the extracts was performed by ion chromatography (IC) with conductivity detection. Several parameters (oil phase:aqueous phase ratio, crude oil:mineral oil ratio, shaking time and type and concentration of surfactant) that could affect the performance of the method were evaluated. Total extraction of chloride from samples could be achieved when 1.0g of oil phase (0.5g of sample+0.5g of mineral oil) was emulsified in 5mL of a 2.5% (m/v) solution of Triton X-114. The obtained emulsion was shaken for 60min and broken by centrifugation for 5min at 5000rpm. The separated aqueous phase was collected, filtered and diluted before analysis by IC. Under these conditions, the limit of detection was 0.5μgg(-1) NaCl and the limit of quantification was 1.6μgg(-1) NaCl. We applied the method to the determination of chloride in six Brazilian crude oils and the results did not differ statistically from those obtained by the ASTM D6470 method when the paired Student-t-test, at 95% confidence level, was applied.

  7. Synthesis of novel calix[4]crown telomers and selective extraction of cesium ions

    Institute of Scientific and Technical Information of China (English)

    Hai Bing Li; Yuan Yin Chen; De Jun Xiong; Jun Yan Zhan; Cui Ping Han

    2007-01-01

    p-tert-Butylcalix[4]diazacrown-4 telomer, which contains hard and soft ion binding sites, was synthesized. It exhibited high selectivity toward cesium ions. The binding sites may complex alkali metal ions selectively.

  8. Aggressive dereplication using UHPLC-DAD-QTOF: screening extracts for up to 3000 fungal secondary metabolites.

    Science.gov (United States)

    Klitgaard, Andreas; Iversen, Anita; Andersen, Mikael R; Larsen, Thomas O; Frisvad, Jens Christian; Nielsen, Kristian Fog

    2014-03-01

    In natural-product drug discovery, finding new compounds is the main task, and thus fast dereplication of known compounds is essential. This is usually performed by manual liquid chromatography-ultraviolet (LC-UV) or visible light-mass spectroscopy (Vis-MS) interpretation of detected peaks, often assisted by automated identification of previously identified compounds. We used a 15 min high-performance liquid chromatography-diode array detection (UHPLC-DAD)-high-resolution MS method (electrospray ionization (ESI)(+) or ESI(-)), followed by 10-60 s of automated data analysis for up to 3000 relevant elemental compositions. By overlaying automatically generated extracted-ion chromatograms from detected compounds on the base peak chromatogram, all major potentially novel peaks could be visualized. Peaks corresponding to compounds available as reference standards, previously identified compounds, and major contaminants from solvents, media, filters etc. were labeled to differentiate these from compounds only identified by elemental composition. This enabled fast manual evaluation of both known peaks and potential novel-compound peaks, by manual verification of: the adduct pattern, UV-Vis, retention time compared with log D, co-identified biosynthetic related compounds, and elution order. System performance, including adduct patterns, in-source fragmentation, and ion-cooler bias, was investigated on reference standards, and the overall method was used on extracts of Aspergillus carbonarius and Penicillium melanoconidium, revealing new nitrogen-containing biomarkers for both species.

  9. Preliminary results concerning the simulation of beam profiles from extracted ion current distributions for mini-STRIKE

    Energy Technology Data Exchange (ETDEWEB)

    Agostinetti, P., E-mail: piero.agostinetti@igi.cnr.it; Serianni, G.; Veltri, P. [Consorzio RFX (CNR, ENEA, INFN, Università di Padova, Acciaierie Venete SpA), Corso Stati Uniti 4, 35127 Padova (Italy); Giacomin, M. [Physics Department, Università di Padova, via F. Marzolo 8, 35131 Padova (Italy); Bonomo, F.; Schiesko, L. [Max-Planck-Institut für Plasmaphysik, Boltzmannstrasse 2, D-85748 Garching (Germany)

    2016-02-15

    The Radio Frequency (RF) negative hydrogen ion source prototype has been chosen for the ITER neutral beam injectors due to its optimal performances and easier maintenance demonstrated at Max-Planck-Institut für Plasmaphysik, Garching in hydrogen and deuterium. One of the key information to better understand the operating behavior of the RF ion sources is the extracted negative ion current density distribution. This distribution—influenced by several factors like source geometry, particle drifts inside the source, cesium distribution, and layout of cesium ovens—is not straightforward to be evaluated. The main outcome of the present contribution is the development of a minimization method to estimate the extracted current distribution using the footprint of the beam recorded with mini-STRIKE (Short-Time Retractable Instrumented Kalorimeter). To accomplish this, a series of four computational models have been set up, where the output of a model is the input of the following one. These models compute the optics of the ion beam, evaluate the distribution of the heat deposited on the mini-STRIKE diagnostic calorimeter, and finally give an estimate of the temperature distribution on the back of mini-STRIKE. Several iterations with different extracted current profiles are necessary to give an estimate of the profile most compatible with the experimental data. A first test of the application of the method to the BAvarian Test Machine for Negative ions beam is given.

  10. Synthesis and application of ion-imprinted polymer nanoparticles for the extraction and preconcentration of copper ions in environmental water samples.

    Science.gov (United States)

    Roushani, Mahmoud; Abbasi, Shahryar; Khani, Hossein

    2015-04-01

    Novel Cu(II) ion-imprinted polymers (Cu-IIP) nanoparticles were prepared by using Cu(II) ion-thiosemicarbazide complex as the template molecule and methacrylic acid, ethylene glycol dimethacrylate (EGDMA), and 2,2'azobisisobutyronitrile (AIBN) as the functional monomer, cross-linker, and the radical initiator, respectively. The synthesized polymer nanoparticles were characterized by using infrared spectroscopy (IR), thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and scanning electron microscopic (SEM) techniques. Some parameters such as pH, weight of the polymer, adsorption time, elution time, eluent type, and eluent volume which affect the extraction efficiency of the polymer were studied. In the proposed method, the maximum sorbent capacity of the ion-imprinted polymer was calculated to be 38.8 mg g(-1). The preconcentration factor, relative standard deviation, and limit of detection of the method were found to be 80, 1.7%, and 0.003 μg mL(-1), respectively. The prepared ion-imprinted polymer nanoparticles have an increased selectivity toward Cu(II) ions over a range of competing metal ions with the same charge and similar ionic radius. The method was applied to the determination of ultra trace levels of Cu2+ in environmental water samples with satisfactory results.

  11. Deflection and Extraction of Pb Ions up to 33 TeV/c by a Bent Silicon Crystal

    Energy Technology Data Exchange (ETDEWEB)

    Arduini, G.; Biino, C.; Clement, M.; Cornelis, K.; Doble, N.; Elsener, K.; Ferioli, G.; Fidecaro, G.; Gatignon, L.; Grafstroem, P.; Gyr, M.; Herr, W.; Klem, J.; Mikkelsen, U.; Weisse, E. [SL Division, CERN, CH-1211 Geneva 23 (Switzerland); Mo/ller, S.P.; Uggerho/j, E. [ISA, Aarhus University (Denmark); Taratin, A. [JINR, Dubna (Russia); Freund, A. [ESRF, Grenoble (France); Keppler, P.; Major, J. [MPI fuer Metallforschung, Stuttgart (Germany)

    1997-11-01

    The first results from an experiment to deflect a beam of fully stripped, ultrarelativistic Pb{sup 82+} ions of 400 GeV/c per unit of charge, equivalent to 33 TeV/c , by means of a bent crystal are reported. Deflection efficiencies are as high as 14{percent}, in agreement with theoretical estimates. In a second experiment a bent crystal was used to extract 270 GeV/c -per-charge Pb{sup 82+} (22 TeV/c) ions from a coasting beam in the CERN-SPS, and a high extraction efficiency of up to 10{percent} was found. These represent the first measurements to demonstrate applications of bent crystals in high energy heavy ion beams. {copyright} {ital 1997} {ital The American Physical Society}

  12. Deflection and Extraction of Pb Ions up to 33 TeV/c by a Bent Silicon Crystal

    Science.gov (United States)

    Arduini, G.; Biino, C.; Clément, M.; Cornelis, K.; Doble, N.; Elsener, K.; Ferioli, G.; Fidecaro, G.; Gatignon, L.; Grafström, P.; Gyr, M.; Herr, W.; Klem, J.; Mikkelsen, U.; Weisse, E.; Møller, S. P.; Uggerhøj, E.; Taratin, A.; Freund, A.; Keppler, P.; Major, J.

    1997-11-01

    The first results from an experiment to deflect a beam of fully stripped, ultrarelativistic Pb82+ ions of 400 GeV/c per unit of charge, equivalent to 33 TeV/c, by means of a bent crystal are reported. Deflection efficiencies are as high as 14%, in agreement with theoretical estimates. In a second experiment a bent crystal was used to extract 270 GeV/c-per-charge Pb82+ \\(22 TeV/c\\) ions from a coasting beam in the CERN-SPS, and a high extraction efficiency of up to 10% was found. These represent the first measurements to demonstrate applications of bent crystals in high energy heavy ion beams.

  13. Deflection and extraction of Pb ions up to 33 TeV/c by a bent silicon crystal

    CERN Document Server

    Arduini, Gianluigi; Clément, M; Cornelis, Karel; Doble, Niels T; Elsener, K; Ferioli, G; Fidecaro, Giuseppe; Freund, A; Gatignon, L; Grafström, P; Gyr, Marcel; Herr, Werner; Keppler, P; Klem, J T; Major, J V; Mikkelsen, U; Møller, S P; Taratin, A M; Uggerhøj, Erik; Weisse, E

    1997-01-01

    The first results from an experiment to deflect a beam of fully stripped, ulta-relativistic Pb ions of 400 GeV/c per unit of charge, equivalent to 33 TeV/c, by means of a bent crystal are reported. Deflection efficiencies are as high as 14%, in agreement with theoretical predictions. In a second experiment a bent crsytal was used to extract 270 GeV/c per charge Pb82+ (22 TeV/c) ions from a coasting beam in the CERN-SPS, and a high extraction efficiency of up to 10% was found. These represent the first measurements to demonstrate applications of bent crystals in high energy heavy ion beams.

  14. Concentration of zinc ions in perchlorate medium by a menbrane-gel using an acid extractant (DEHPA

    Directory of Open Access Journals (Sweden)

    Belhadji L.

    2013-07-01

    Full Text Available Recent decades, it is an awareness of the importance of ecological balance in the environment, balances threatened by industrial pollution. A new spirit presides we seek to minimize pollution of receiving waters. The present work is to study the liquid-gel-extraction of zinc ions in perchlorate medium by an acid extractant: the di (ethyl-2 hexyl phosphorique acid, or DEHPA. Two types of polymers were used as supports of solvent extraction: a polybutadiene rubber cross-linked respectively with 0.1% dicumyl peroxide and 0.4% dicumyl peroxide, vulcanized at 160°C, one is most cross-linked than the other. The liquid-gel extraction is based on the principles of the liquid-liquid extraction.

  15. Improved beam extraction for a negative hydrogen ion source for the LHC injector chain upgrade, Linac4

    CERN Document Server

    Midttun, Øystein; Scrivens, Richard

    In the scope of an upgrade of the injector chain of CERN’s accelerator complex, a new linear accelerator, Linac4, is under construction. This accelerator will replace the existing 50 MeV proton linac, Linac2. By increasing the beam energy to 160 MeV, Linac4 makes it possible to double the brightness in the PSB, and ultimately increase the luminosity in the LHC. Linac4 will accelerate beams of negative hydrogen (H-) to be injected into the PSB by multi-turn, charge exchange injection. The ion source was initially based on the non-caesiated RF-volume source from DESY. However, the beam extraction from this source could not handle the 45 keV beam energy required by the RFQ. A new beam extraction system has therefore been designed, via IBSimu simulations [1], to extract and transport the H- ion beam respecting the Linac4 requirements. Key features of the extraction system is a tuneable puller voltage to adapt the extraction field to the ion and electron beam currents, and a magnetized Einzel lens to dump the co...

  16. Liquid-liquid extraction of ion-association complexes of cobalt(II-4-(2-pyridylazoresorcinol with ditetrazolium salts

    Directory of Open Access Journals (Sweden)

    Divarova Vidka V.

    2015-01-01

    Full Text Available The formation and liquid-liquid extraction of ion-association complexes between Co(II-4-(2-Pyridylazoresorcinol (PAR anionic chelates and cations of three ditetrazolium chlorides were studied: Blue Tetrazolium chloride (BTC, Neotetrazolium chloride (NTC and Nitro Blue Tetrazolium chloride (NBT. The optimum conditions for the formation and solvent extraction of the ion-association comlpex chelates were determined. It has been found that in the systems of Co(II-PAR-DTS, the reactants are reacted in molar ratios 1:2:1 and the general formula of complexes was suggested. The extraction equilibria were investigated and quantitatively characterized by the equilibrium constants and the recovery factors. The analytical characteristics of the complexes were calculated.

  17. Study on the HPLC Characteristic Chromatogram of Pheretima%地龙的HPLC特征图谱研究

    Institute of Scientific and Technical Information of China (English)

    黄帅; 徐风; 杨平; 杨雪雁; 刘广学; 尚明英; 王璇; 蔡少青

    2015-01-01

    OBJECTIVE:To establish the HPLC characteristic chromatogram of pheretima,and compare the differences of the main ingredient contents of Guangdong pheretima and Shanghai pheretima and the chromatogram differences among pheretima and 3 other animal drugs. METHODS:Pheretima HPLC characteristic chromatogram method was adopted to determine the characteris-tic chromatograms of 16 Guangdong pheretima,8 Shanghai pheretima,3 eupolyphaga,3 hirudo and 3 catharsius. Similarity evalua-tion and t test were used to analyze the differences of chromatogram data of 5 animal drugs. RESULTS:The established HPLC char-acteristic chromatogram method firstly identified 11 common characteristic peaks,including 6 nucleosides,4 nucleobase and 1 ami-no acid;and it could be used for the identification of pheretima from eupolyphaga,hirudo and catharsius;the differences of main ingredient contents in the characteristic chromatogram of Guangdong pheretima and Shanghai pheretima were firstly studied. The contents of xanthine and adenosine in Guangdong pheretima were higher than Shanghai pheretima,while the contents of uridine, guanosine and 2′-deoxy guanosine in Shanghai pheretima were higher than Guangdong pheretima. A new index S,calculated by these 5 constituents,was successfully applied to distinguish the 2 kinds of pheretima. CONCLUSIONS:The characteristic chro-matogram can be used for the identification of pheretima,and can provide reference for the pharmacodynamic differences study of Guangdong pheretima and Shanghai pheretima.%目的:建立地龙的高效液相色谱(HPLC)特征图谱,比较广地龙与沪地龙的主要成分含量差异以及地龙与3种其他动物药的图谱差异。方法:采用地龙HPLC特征图谱法,测定了16份广地龙、8份沪地龙、3份土鳖虫、3份水蛭与3份蜣螂虫的特征图谱,采用相似度评价与t检验对这5种动物药的图谱数据进行差异分析。结果:本研究建立了地龙药材的HPLC特

  18. Kinetic and equilibrium studies of the removal of cadmium ions from acidic chloride solutions by hydrophobic pyridinecarboxamide extractants

    Energy Technology Data Exchange (ETDEWEB)

    Borowiak-Resterna, Aleksandra [Institute of Chemical Technology and Engineering, Poznan University of Technology, Pl. Marii Sklodowskiej-Curie 2, 60-965 Poznan (Poland); Cierpiszewski, Ryszard [Poznan University of Economics, Faculty of Commodity Science, al. Niepodleglosci 10, 61-875 Poznan (Poland); Prochaska, Krystyna, E-mail: Krystyna.Prochaska@put.poznan.pl [Institute of Chemical Technology and Engineering, Poznan University of Technology, Pl. Marii Sklodowskiej-Curie 2, 60-965 Poznan (Poland)

    2010-07-15

    Liquid-liquid extraction of cadmium(II) from acidic chloride solutions was carried out with alkyl derivatives of pyridinecarboxamide in toluene with addition of 2-ethylhexan-1-ol as modifier. Equilibrium as well as kinetic studies was performed. The kinetic studies of a Cd(II) extraction process were carried out with a Lewis cell having a constant interfacial area. Cadmium(II) concentration in the aqueous phases was determined by atomic absorption spectroscopy (Varian SPECTR AA800). The results of equilibrium experiments showed that cadmium(II) was quantitatively extracted with N,N-dihexylpyridine-3-carboxamide whereas the derivative N,N-dihexylpyridine-2-carboxamide was not able to transfer Cd(II) ions from the aqueous phase to the organic one. Thus, the kinetics of extraction and the initial extraction rate were examined only in the systems with N,N-dihexylpyridine-3-carboxamide. The obtained experimental data as well as the calculated values of mass transfer coefficients suggest that the investigated process of extraction of Cd(II) by means of pyridinecarboxamide as extractant occurs in the mixed diffusion-kinetic region. Moreover, the results of adsorption studies indicated that the extraction of Cd(II) with a hydrophobic extractant should be considered as an interfacial process.

  19. Green synthesis of silver nanoparticles using Carica Papaya fruit extract under sunlight irradiation and their colorimetric detection of mercury ions

    Science.gov (United States)

    Firdaus, M.; Andriana, S.; Elvinawati; Alwi, W.; Swistoro, E.; Ruyani, A.; Sundaryono, A.

    2017-04-01

    We have successfully synthesized silver nanoparticles (AgNPs) by using aqueous extract of papaya (Carica papaya) fruit as bioreductant under sunlight irradiation without additional capping agent. Characterizations were done using UV-Visible spectrophotometry and Fourier Transform Infrared Spectroscopy (FTIR). The synthesized AgNPs have yellowish-brown color with surface plasmon resonance peak at 410 nm. Good selectivity of the AgNPs towards hazardous heavy metal of mercury ions in aqueous solution has been developed as a green environmental sensor. The presence of Hg(II) ions in the mixture changed the yellowish-brown color of AgNPs to colorless due to oxidation of Ag(O) in AgNPs to Ag(I) ions. Effect of samples matrix such as alkali metal, alkaline earth metal and transition metal ions were evaluated.

  20. Multi-element pre-concentration of heavy metal ions by solid phase extraction on Chromosorb 108

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Art and Science, Department of Chemistry, 38039 Kayseri (Turkey)]. E-mail: soylak@erciyes.edu.tr; Elci, Latif [Pamukkale University, Faculty of Art and Science, Department of Chemistry, 20020 Denizli (Turkey)

    2005-08-29

    A multi-element preconcentration procedure for solid phase extraction on Chromosorb 108 as bathocuproinedisulfonic acid chelates and flame atomic absorption spectrometric determinations of some heavy metal ions in environmental samples is proposed in the present work. The influences of analytical parameters including pH of the aqueous solution, amounts of reagents, flow rates of sample and eluent solutions, sample volume etc. on the quantitative recoveries of copper, cadmium, lead, zinc, manganese, iron, chromium, nickel and cobalt ions were investigated. The effects of concomitant ions on the retentions of the analytes were also examined. The presented preconcentration procedure was applied to the determination of metal ions in reference standard materials (NRCC-SLRS 4 Riverine Water, SRM 1515 Apple leaves and GBW 07605 Tea) and some real samples including tap and river water, red wine, rice, black tea and honey.

  1. Development of a pepper-pot emittance meter for diagnostics of low-energy multiply charged heavy ion beams extracted from an ECR ion source

    Energy Technology Data Exchange (ETDEWEB)

    Nagatomo, T., E-mail: nagatomo@riken.jp; Kase, M.; Kamigaito, O.; Nakagawa, T. [Nishina Center for Accelerator Based Science, RIKEN, Wako, Saitama 351-0198 (Japan); Tzoganis, V. [Nishina Center for Accelerator Based Science, RIKEN, Wako, Saitama 351-0198 (Japan); Cockcroft Institute, Daresbury, Warrington WA4 4AD (United Kingdom); Department of Physics, University of Liverpool, Liverpool, Merseyside L69 3BX (United Kingdom)

    2016-02-15

    Several fluorescent materials were tested for use in the imaging screen of a pepper-pot emittance meter that is suitable for investigating the beam dynamics of multiply charged heavy ions extracted from an ECR ion source. SiO{sub 2} (quartz), KBr, Eu-doped CaF{sub 2}, and Tl-doped CsI crystals were first irradiated with 6.52-keV protons to determine the effects of radiation damage on their fluorescence emission properties. For such a low-energy proton beam, only the quartz was found to be a suitable fluorescent material, since the other materials suffered a decay in fluorescence intensity with irradiation time. Subsequently, quartz was irradiated with heavy {sup 12}C{sup 4+}, {sup 16}O{sup 4+}, and {sup 40}Ar{sup 11+} ions, but it was found that the fluorescence intensity decreased too rapidly to measure the emittance of these heavy-ion beams. These results suggest that a different energy loss mechanism occurs for heavier ions and for protons.

  2. Development of a pepper-pot emittance meter for diagnostics of low-energy multiply charged heavy ion beams extracted from an ECR ion source

    Science.gov (United States)

    Nagatomo, T.; Tzoganis, V.; Kase, M.; Kamigaito, O.; Nakagawa, T.

    2016-02-01

    Several fluorescent materials were tested for use in the imaging screen of a pepper-pot emittance meter that is suitable for investigating the beam dynamics of multiply charged heavy ions extracted from an ECR ion source. SiO2 (quartz), KBr, Eu-doped CaF2, and Tl-doped CsI crystals were first irradiated with 6.52-keV protons to determine the effects of radiation damage on their fluorescence emission properties. For such a low-energy proton beam, only the quartz was found to be a suitable fluorescent material, since the other materials suffered a decay in fluorescence intensity with irradiation time. Subsequently, quartz was irradiated with heavy 12C4+, 16O4+, and 40Ar11+ ions, but it was found that the fluorescence intensity decreased too rapidly to measure the emittance of these heavy-ion beams. These results suggest that a different energy loss mechanism occurs for heavier ions and for protons.

  3. Recovery of cobalt from spent lithium-ion batteries using supercritical carbon dioxide extraction.

    Science.gov (United States)

    Bertuol, Daniel A; Machado, Caroline M; Silva, Mariana L; Calgaro, Camila O; Dotto, Guilherme L; Tanabe, Eduardo H

    2016-05-01

    Continuing technological development decreases the useful lifetime of electronic equipment, resulting in the generation of waste and the need for new and more efficient recycling processes. The objective of this work is to study the effectiveness of supercritical fluids for the leaching of cobalt contained in lithium-ion batteries (LIBs). For comparative purposes, leaching tests are performed with supercritical CO2 and co-solvents, as well as under conventional conditions. In both cases, sulfuric acid and H2O2 are used as reagents. The solution obtained from the supercritical leaching is processed using electrowinning in order to recover the cobalt. The results show that at atmospheric pressure, cobalt leaching is favored by increasing the amount of H2O2 (from 0 to 8% v/v). The use of supercritical conditions enable extraction of more than 95wt% of the cobalt, with reduction of the reaction time from 60min (the time employed in leaching at atmospheric pressure) to 5min, and a reduction in the concentration of H2O2 required from 8 to 4% (v/v). Electrowinning using a leach solution achieve a current efficiency of 96% and a deposit with cobalt concentration of 99.5wt%.

  4. Bulk matter evolution and extraction of jet transport parameter in heavy-ion collisions at RHIC

    CERN Document Server

    Chen, Xiao-Fang; Wang, Enke; Wang, Xin-Nian; Xu, Zhe

    2010-01-01

    Within the picture of jet quenching induced by multiple parton scattering and gluon bremsstrahlung, medium modification of parton fragmentation functions and therefore the suppression of large transverse momentum hadron spectra are controlled by both the value and the space-time profile of the jet transport parameter along the jet propagation path. Experimental data on single hadron suppression in high-energy heavy-ion collisions at the RHIC energy are analyzed within the higher-twist (HT) approach to the medium modified fragmentation functions and the next-to-leading order (NLO) perturbative QCD (pQCD) parton model. Assuming that the jet transport parameter $\\hat q$ is proportional to the particle number density in both QGP and hadronic phase, experimental data on jet quenching in deeply inelastic scattering (DIS) off nuclear targets can provide guidance on $\\hat q_{h}$ in the hot hadronic matter. One can then study the dependence of extracted initial value of jet quenching parameter $\\hat q_{0}$ at initial ...

  5. SEQUENTIAL EXTRACTION OF PHOSPHORUS BY MEHLICH-1 AND ION EXCHANGE RESIN FROM B HORIZONS OF FERRIC AND PERFERRIC LATOSOLS (OXISOLS

    Directory of Open Access Journals (Sweden)

    Danilo de Lima Camêlo

    2015-08-01

    Full Text Available In general, Latosols have low levels of available P, however, the influence of the parent material seems to be decisive in defining the pool and predominant form of P in these soils. This study evaluated P availability by extraction with Mehlich-1 (M-1 and Ion Exchange Resin (IER, from samples of B horizons of Ferric and Perferric Latosols developed from different parent materials. To this end, in addition to the physical and chemical characterization of soils, 10 sequential extractions were performed with M-1 and IER from samples of B horizons (depth between 0.8 and 1.0 m. Total contents of Ca, P, Fe, Al, and Ti were determined after digestion with nitric, hydrofluoric and perchloric acids. The effects of sequential P extractions on Fe oxides were also evaluated from the analyses of dithionite-citrate-bicarbonate and ammonium acid oxalate. The high similarity between contents of P accumulated after sequential extractions with M-1 and IER in soils developed on tuffite indicated a predominance of P-Ca. Higher contents of P after a single IER extraction show greater efficiency in P removal from highly weathered soils, as from the Latosols studied here. The P contents also show the high sensitivity of extractant M-1 in highly buffered soils. Furthermore, a single extraction with extractant M-1 or IER is not sufficient to estimate the amount of labile P in these soils.

  6. Synthesis and application of novel ion-imprinted polymer coated magnetic multi-walled carbon nanotubes for selective solid phase extraction of lead(II) ions

    Energy Technology Data Exchange (ETDEWEB)

    Fayazi, Maryam, E-mail: maryam.fayazi@yahoo.com [Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Researchers Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Taher, Mohammad Ali [Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Department of Environment, Institute of Science and High Technology and Environmental Sciences, Graduate University of Advanced Technology, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Ghanei-Motlagh, Masoud, E-mail: m.ghaneimotlagh@yahoo.com [Young Researchers Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2016-03-01

    In this study, novel magnetic ion-imprinted polymer (MIIP) nanoparticles were utilized for the sensitive and selective detection of Pb(II) ions by graphite furnace atomic absorption spectrometry (GFAAS). The Pb(II)-imprinted polymer was synthesized by using 4-vinylpyridine (4VP) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,3,5,6-tetra(2-pyridyl) pyrazine (TPPZ) as the chelating agent and magnetic multi-walled carbon nanotubes (MMWCNTs) as the carrier. The synthesized MIIP materials were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). Various analytical parameters such as extraction and desorption time, eluent type and concentration, pH and sample volume were systematically examined. The selectivity of MIIP sorbent for Pb(II) ions in the presence of some cations was also evaluated. The limit of detection (LOD, 3S{sub b}) and the relative standard deviation (RSD, n = 8, c = 25 ng L{sup −1}) were found to be 2.4 ng L{sup −1} and 5.6%, respectively. The maximum sorption capacity of the MIIP for Pb(II) was found to be 48.1 mg g{sup −1}. Finally, the proposed analytical procedure was successfully applied to monitoring lead in human hair and water samples with satisfactory results for the spiked samples. - Highlights: • A selective and sensitive method based on MSPE-GFAAS was proposed. • The MIIP nanoparticles were characterized using FE-SEM, XRD, VSM and FT-IR techniques. • The synthesized MIIP material is efficient at extracting lead ions. • The method was applied to determine lead ions in several real samples.

  7. Feasibility of corona discharge ion mobility spectrometry for direct analysis of samples extracted by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Jafari, Mohammad T; Riahi, Farhad

    2014-05-23

    The capability of corona discharge ionization ion mobility spectrometry (CD-IMS) for direct analysis of the samples extracted by dispersive liquid-liquid microextraction (DLLME) was investigated and evaluated, for the first time. To that end, an appropriate new injection port was designed and constructed, resulting in possibility of direct injection of the known sample volume, without tedious sample preparation steps (e.g. derivatization, solvent evaporation, and re-solving in another solvent…). Malathion as a test compound was extracted from different matrices by a rapid and convenient DLLME method. The positive ion mobility spectra of the extracted malathion were obtained after direct injection of carbon tetrachloride or methanol solutions. The analyte responses were compared and the statistical results revealed the feasibility of direct analysis of the extracted samples in carbon tetrachloride, resulting in a convenient methodology. The coupled method of DLLME-CD-IMS was exhaustively validated in terms of sensitivity, dynamic range, recovery, and enrichment factor. Finally, various real samples of apple, river and underground water were analyzed, all verifying the feasibility and success of the proposed method for the easy extraction of the analyte using DLLME separation before the direct analysis by CD-IMS.

  8. Solvent extraction of rare earth ions from nitrate media with new extractant di-(2,3-dimethylbutyl)-phosphinic acid

    Institute of Scientific and Technical Information of China (English)

    王俊莲; 陈广; 徐盛明; 尹祉力; 张覃

    2016-01-01

    As a relatively new extractant, di-(2,3-dimethylbutyl)-phosphinic acid (HYY-2) is more efficient to separate heavy rare earths Tm/Yb/Lu than Cyanex 272 and P507. In this paper, HYY-2 was synthesized in our lab, and the extraction equilibrium, ther-modynamics and stripping acidity for La, Gd and Y, which stood for light rare earth elements (REE), middle REE and heavy REE respectively, from nitrate media with this extractant were investigated. Meanwhile, extraction ability, capacity and stripping acidity of HYY-2 were investigated and compared with those of Cyanex 272 and P507. The separation performance for rare earth element cou-ples Gd/Eu and Er/Ywere also studied. Compared to Cyanex 272, it possessed higher extraction capacity; while compared with P507, it has lower stripping acidity. The maximumβGd/Eu 1.46 occurred at pHequilibrium=2.78 and the maximumβEr/Y was 1.47 when pHequilibrium= 2.01.

  9. Evaluation of the method of electrochemical extraction of chlorides ions for the rehabilitation of concrete structures with reinforcement corrosion problems

    Directory of Open Access Journals (Sweden)

    Monteiro, E.

    2003-12-01

    Full Text Available The present work evaluates the method of electrochemical extraction of chloride ions for the rehabilitation of corroded concrete structures. The influence of the concrete cover and the water-to-cement ratio in the efficiency of the method was studied by determining the initial and the final chloride content. Electrochemical impedance spectroscopy and the corrosion potential were used to monitor the reinforcement electrochemical behavior during the chloride extraction. The test results verify that this method successfully extracted chloride ions like it was previous reported in the literature. On average, this method removed 77% of the content of initial chloride ions at a distance of 0.5 cm from the surface and 50% of the content of initial chloride ions near de rebars.

    El actual trabajo evalúa el método de extracción electroquímica de cloruros para la rehabilitación de estructuras de hormigón corroídas. La influencia del espesor de recubrimiento y de la relación agua/cemento en la eficacia del método fue estudiada determinando el contenido inicial y final de cloruros. La técnica de impedancia electroquímica y el potencial de la corrosión fueron utilizados para la monitorización del comportamiento electroquímico del refuerzo durante la extracción de cloruros. Los resultados de los ensayos verificaron que este método extrajo con éxito cloruros, tal y como fue divulgado previamente en la literatura. Como promedio, este método extrajo el 77% del contenido de iones iniciales de cloruros a una distancia de 0,5 centímetros de la superficie, y el 50% del contenido de cloruros cerca de las armaduras.

  10. Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from Radio Frequency plasma) experiment: tests in BATMAN (BAvarian Test Machine for Negative ions).

    Science.gov (United States)

    Brombin, M; Spolaore, M; Serianni, G; Pomaro, N; Taliercio, C; Dalla Palma, M; Pasqualotto, R; Schiesko, L

    2014-11-01

    A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors' holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

  11. Langmuir probes for SPIDER (source for the production of ions of deuterium extracted from radio frequency plasma) experiment: Tests in BATMAN (Bavarian test machine for negative ions)

    Energy Technology Data Exchange (ETDEWEB)

    Brombin, M., E-mail: matteo.brombin@igi.cnr.it; Spolaore, M.; Serianni, G.; Pomaro, N.; Taliercio, C.; Palma, M. Dalla; Pasqualotto, R. [Consorzio RFX, Corso Stati Uniti 4, I-35127 Padova (Italy); Schiesko, L. [Max-Planck-Institut für Plasmaphysik, Boltzmannstr. 2, 85748 Garching (Germany)

    2014-11-15

    A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors’ holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

  12. Langmuir probes for SPIDER (source for the production of ions of deuterium extracted from radio frequency plasma) experiment: Tests in BATMAN (Bavarian test machine for negative ions)

    Science.gov (United States)

    Brombin, M.; Spolaore, M.; Serianni, G.; Pomaro, N.; Taliercio, C.; Palma, M. Dalla; Pasqualotto, R.; Schiesko, L.

    2014-11-01

    A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors' holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

  13. IonLab. A remote-controlled experiment for academic and vocational education and training on extraction chromatography and ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Schulz, Wolfgang; Fournier, Claudia; Vahlbruch, Jan-Willem; Walther, Clemens [Leibniz Univ., Hannover (Germany). Inst. for Radioecology and Radiation Protection (IRS)

    2016-07-01

    As a major contribution to modern web-based education and training in nuclear chemistry we have built and operated a remote-controlled experiment - IonLab - as part of the integrated EUFP7 project CINCHII. The setup is suitable for teaching basics on extraction chromatography and ion exchange using radionuclides. We describe separation of the beta emitting nuclides Sr-90 and Y-90 followed by radiometric detection, but the experiment is easily adapted to other separation schemes. This approach is aimed at institutions in academic or vocational education who need to convey the skills of handling radioactive (or otherwise dangerous, e.g. biotoxic) substances without appropriately licensed laboratory space for teaching. This camera-monitored remote controlled lab experiment has proved to be much closer to a real hands-on training and superior to a mere computer simulation.

  14. Solid phase extraction of Cu2+, Ni2+, and Co2+ ions by a new magnetic nano-composite: excellent reactivity combined with facile extraction and determination.

    Science.gov (United States)

    Azizi, Parastou; Golshekan, Mostafa; Shariati, Shahab; Rahchamani, Jalal

    2015-04-01

    In the present study, silica magnetite mesoporous nanoparticles functionalized with a new chelating agent were synthesized and introduced as a magnetic solid phase for preconcentration of trace amounts of Cu2+, Ni2+, and Co2+ ions from aqueous solutions. Briefly, MCM-41 mesoporous-coated magnetite nano-particles (MMNPs) with particle size lower than 15 nm were synthesized via chemical co-precipitation methods. Then, N-(4-methoxysalicylidene)-4,5-dinitro-1,2-phenylenediamine (HL) as a new chelating agent was synthesized and used for surface modification of mesoporous magnetic solid phase by dispersive liquid-liquid functionalization (DLLF) as a new rapid method to form HL functionalized mesoporous magnetite nanoparticles (MMNPs─HL). The structure and morphology of prepared sorbent were characterized by FT-IR, XRD, VSM, and TEM. Finally, the prepared nanoparticles were utilized for preconcentration of Cu2+, Ni2+, and Co2+ ions prior to determination by atomic absorption spectrophotometery. The calibration graph was obtained under the optimized conditions with linear dynamic range of 1.0-300 μg L(-1) and correlation coefficient (r2) of 0.998. The detection limits of this method for cobalt, nickel, and copper ions were 0.03, 0.03, and 0.04 ng/mL, respectively. Finally, the method was successfully applied to the extraction and determination of the analyte ions in natural waters and reference plant samples.

  15. Influence of the ionic liquid cation on the solvent extraction of trivalent rare-earth ions by mixtures of Cyanex 923 and ionic liquids.

    Science.gov (United States)

    Rout, Alok; Binnemans, Koen

    2015-01-21

    Trivalent rare-earth ions were extracted from nitric acid medium by the neutral phosphine oxide extractant Cyanex 923 into ionic liquid phases containing the bis(trifluoromethylsulfonyl)imide anion. Five different cations were considered: 1-butyl-3-methylimidazolium, 1-decyl-3-methylimidazolium, methyltributylammonium, methyltrioctylammonium and trihexyl(tetradecyl)phosphonium. The extraction behavior of neodymium(iii) was investigated as a function of various parameters: pH, extractant concentration, concentration of the neodymium(iii) ion in the aqueous feed and concentration of the salting-out agent. The loading capacity of the ionic liquid phase was studied. The extraction efficiency increased with increasing pH of the aqueous feed solution. The extraction occurred for all ionic liquids via an ion-exchange mechanism and the extraction efficiency could be related to the solubility of the ionic liquid cation in the aqueous phase: high distribution ratios for hydrophilic cations and low ones for hydrophobic cations. Addition of nitrate ions to the aqueous phase resulted in an increase in extraction efficiency for ionic liquids with hydrophobic cations due to extraction of neutral complexes. Neodymium(iii) could be stripped from the ionic liquid phase by 0.5-1.0 M nitric acid solutions and the extracting phase could be reused. The extractability of other rare earths present in the mixture was compared for the five ionic liquids.

  16. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Ghaedi, M; Shokrollahi, A; Ahmadi, F; Rajabi, H R; Soylak, M

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L(-1) HNO(3) nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO(3), bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL(-1) for Cu(2+), Co(2+) and Ni(2+) along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu(2+), Ni(2+) and Co(2+), respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  17. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, M. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Shokrollahi, A.; Ahmadi, F.; Rajabi, H.R. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, M. [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L{sup -1} HNO{sub 3} nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO{sub 3}, bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL{sup -1} for Cu{sup 2+}, Co{sup 2+} and Ni{sup 2+} along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu{sup 2+}, Ni{sup 2+} and Co{sup 2+}, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  18. Spectrophotometric determination of traces of iodide by liquid-liquid extraction of Brilliant Green-iodide ion pair

    Energy Technology Data Exchange (ETDEWEB)

    Niazi, S.B.; Mozammil, Mohammad (Bahauddin Zakariya University, Multan (Pakistan). Department of Chemistry)

    1991-11-05

    Iodide in natural waters at the 10{sup -6} M level is determined spectrophotometrically as the Brilliant Green-iodide ion pair. Iodide is the first oxidized to iodide with hydrogen peroxide-sulphuric acid to separate it from other chemical species and extracted into carbon tetrachloride. It is then extracted back into aqueous medium by its reduction with sodium thiosulphate and stabilized as the ion pair with Brilliant Green. At pH 7 the ion pair is extracted into chloroform and the absorbance is measured at 625 nm against chloroform. A linear calibration graph is obtained over the range 5x10{sup -7}-3.5x10{sup -6} M iodide with a relative standard deviation of 0.38 % at the 2x10{sup -6} M iodide level. The apparent molar absorptivity for iodide is 3.0x10{sup 5} l mol{sup -1} cm{sup -1}. (author). 11 refs.; 4 figs.; 2 tabs.

  19. [Determination of nonylphenol in wastewater by solid phase extraction gas chromatography mass spectrometry and multi-selective ions].

    Science.gov (United States)

    Hao, Rui-Xia; Liang, Peng; Zhao, Man; Wang, Jun-An; Zhou, Yu-Wen

    2006-11-01

    Nonylphenol (NP) having endocrine disrupter activity is an ultra trace component in sewage and reuse wastewater. There are many NP isomers in the wastewater because nonyl structure is different. The background impurity of the samples is very complex with many other components. So it is difficulty for quantitative analysis of NP in the samples. About seventy sewages and recycled wastewater samples were measured for the content of NP isomer mixtures by solid-phase extraction-gas chromatography-mass spectrometry and multi-selected ions monitoring (shortened as SPE-GC-MS-SIM). The results show that hydrophilic-lipophilic-equilibrium solid-phase extraction pole has selective adsorption for NP, so that the samples can be concentrated from 50 to 200 times. The five kinds of mass spectrum ions, i. e. 107, 121, 135, 149, 163, have higher abundance and distinct character. The sum of five selected ion monitoring (sigmaSIM) is from 54.4 to 73 percent of the total ion current for NP, which can accurately represent different NP isomers. Quantitative analysis base on the spectral integralof the sigmaSIM chromatograph can eliminate interference with background signal and ensure selectivity, accuracy and precision ofthe method.

  20. DETERMINATION OF FLUORIDE IN HIGHLY SALINATED WATERS BY ION CHROMATOGRAPHY METHOD WITH USE OF SOLID PHASE EXTRACTION FOR SAMPLE PREPARATION

    Directory of Open Access Journals (Sweden)

    Beata Kostka

    2014-10-01

    Full Text Available Solid phase extraction (SPE is one of the most popular methods of matrix elimination in determination of anions by ion chromatography. Possibility of using cartridges containing a cation-exchange resin in the Ag+ and Na+ forms for determination of fluoride in the presence of very high concentration of chloride in mine waters was described in this paper. A Dionex ICS-2500 ion chromatograph was used for separation of anions in gradient elution using IonPac AS19 (4x250 mm separation column along with generated KOH eluent. Fluoride after separation was determined by conductivity detector with suppression. The investigations performed on mine waters (conductivity in the range 12 700 μS/cm–155 000 μS/cm and synthetic brine (38 820 mg/L Cl- and 3 408 mg/L SO4 2- confirmed usefulness of cartridges containing a cation-exchange resin for minimizing matrix influence on results of fluoride determination. The ion chromatography method accompanied by solid phase extraction for sample preparation proved to be very useful for determination of fluoride in highly salinated waters (i.e. mine waters because of low detection limit (0,02 mg/L, good precision (< 2,5 % and accuracy (recovery 91 % – 104 %.

  1. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

    Science.gov (United States)

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-01

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

  2. Comparison of gravimetry and hydrolysis/derivatization/gas chromatography-mass spectrometry for quantitative analysis of fat from standard reference infant formula powder using supercritical fluid extraction.

    Science.gov (United States)

    Ashraf-Khorassani, M; Ude, M; Doane-Weideman, T; Tomczak, J; Taylor, L T

    2002-03-27

    This paper describes a comparative study of the gravimetric versus hydrolysis/derivatization/gas chromatography-mass spectrometry determination of fat in infant formula. Fat was extracted using supercritical carbon dioxide modified with a small amount of ethanol, the extract was weighed, and the total fat was determined gravimetrically. Subsequently, another sample of the supercritical fluid fat extract was hydrolyzed to yield free fatty acids, which were converted to their methyl ester derivatives (FAMEs). Quantification was performed by GC-MS. NIST Standard Reference Material (SRM-1846) was used to validate both fat determination methods. Results showed that the gravimetric average percent fat was 26.86%, whereas the GC-MS method yielded 24.64%. Some peaks were detected in the ion chromatogram from the GC-MS that were identified as nonfatty acids such as aldehydes, which may account for the higher percentage fat measured as weight of extract rather than measured as FAMEs expressed as triglycerides.

  3. Selective metal-ion extraction for multiple-ion liquid-liquid exchange reactions. Final report, June 1, 1979-May 31, 1982

    Energy Technology Data Exchange (ETDEWEB)

    Tavlarides, L.L.

    1982-01-29

    This research in hydrometallurgical solvent extraction is to develop a fundamental means to predict selectivity during simultaneous solvent extraction of multiple metal ions when the kinetic rates and thermodynamic equilibria both do not favor the desired metal. To this end the chemical kinetics and thermodynamic chemical equilibria models for the system copper-iron-acid sulfate solutions extracted by ..beta..-alkenyl-8-hydroxy quinoline in xylene are studied. These models can be employed with appropriate design equations to predict selectivity factors for two phase contactors. The work completed and in progress during the first half of the third funding period is on chemical equilibria studies for the iron-acid-sulfate-..beta..-alkenyl-8-hydroxy quinoline-xylene system. An aqueous phase ionic equilibrium model is available which can be used to calculate concentration of various Fe(III) ionic species present. Iron extraction data were obtained using both the AKUFVE, a high intensity stirrer with an in line centrifugal separator, and a shaker bath apparatus. Analysis of the data to determine a thermodynamic equilibrium model is in progress.

  4. Optimization of LiCoO2 powder extraction process from cathodes of lithium-ion batteries by chemical dissolution

    Directory of Open Access Journals (Sweden)

    Lucas Evangelista Sita

    2015-05-01

    Full Text Available A chemical process has been applied to extract LiCoO2 powder from cathodes of spent lithium-ion batteries by dissolution of the binder that agglutinate the powder particle each other as well to the Al collector surface. As solvents dimethylformamide (DMF and N-methyilpirrolidone (NMP were employed and the variables, cathode area, solution temperature, ultrasound bath power and solution stirring were chosen to optimize the extraction process. NMP solutions presented best results for powder extraction than DMF solutions. At 100 oC and under mechanical stirring or low power ultrasound bath NMP solution optimizes the binder dissolution. Powder extractions under DMF solutions are slow and an increase in the powder extraction efficiency was observed for crushed cathodes on solutions under ultrasound bath, at medium power. Filtration processes can separate the decanted LiCoO2 powder extracted upon DMF dissolution while the powder in suspension in the NMP solutions is separated by centrifugation techniques.

  5. Electro-driven extraction of inorganic anions from water samples and water miscible organic solvents and analysis by ion chromatography.

    Science.gov (United States)

    Nojavan, Saeed; Bidarmanesh, Tina; Memarzadeh, Farkhondeh; Chalavi, Soheila

    2014-09-01

    A simple electromembrane extraction (EME) procedure combined with ion chromatography (IC) was developed to quantify inorganic anions in different pure water samples and water miscible organic solvents. The parameters affecting extraction performance, such as supported liquid membrane (SLM) solvent, extraction time, pH of donor and acceptor solutions, and extraction voltage were optimized. The optimized EME conditions were as follows: 1-heptanol was used as the SLM solvent, the extraction time was 10 min, pHs of the acceptor and donor solutions were 10 and 7, respectively, and the extraction voltage was 15 V. The mobile phase used for IC was a combination of 1.8 mM sodium carbonate and 1.7 mM sodium bicarbonate. Under these optimized conditions, all anions had enrichment factors ranging from 67 to 117 with RSDs between 7.3 and 13.5% (n = 5). Good linearity values ranging from 2 to 1200 ng/mL with coefficients of determination (R(2) ) between 0.987 and 0.999 were obtained. The LODs of the EME-IC method ranged from 0.6 to 7.5 ng/mL. The developed method was applied to different samples to evaluate the feasibility of the method for real applications.

  6. An ion-imprinted polymer for the selective extraction of mercury(II ...

    African Journals Online (AJOL)

    2011-02-16

    Feb 16, 2011 ... A double-imprinted polymer exhibiting high sensitivity for mercury(II) in aqueous solution is ... In recent years the release of various harmful heavy metal ions ..... both of the competing ions have the same charge, have com-.

  7. Synthesis and application of novel ion-imprinted polymer coated magnetic multi-walled carbon nanotubes for selective solid phase extraction of lead(II) ions.

    Science.gov (United States)

    Fayazi, Maryam; Taher, Mohammad Ali; Afzali, Daryoush; Mostafavi, Ali; Ghanei-Motlagh, Masoud

    2016-03-01

    In this study, novel magnetic ion-imprinted polymer (MIIP) nanoparticles were utilized for the sensitive and selective detection of Pb(II) ions by graphite furnace atomic absorption spectrometry (GFAAS). The Pb(II)-imprinted polymer was synthesized by using 4-vinylpyridine (4VP) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,3,5,6-tetra(2-pyridyl) pyrazine (TPPZ) as the chelating agent and magnetic multi-walled carbon nanotubes (MMWCNTs) as the carrier. The synthesized MIIP materials were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). Various analytical parameters such as extraction and desorption time, eluent type and concentration, pH and sample volume were systematically examined. The selectivity of MIIP sorbent for Pb(II) ions in the presence of some cations was also evaluated. The limit of detection (LOD, 3S(b)) and the relative standard deviation (RSD, n=8, c=25 ng L(-1)) were found to be 2.4 ng L(-1) and 5.6%, respectively. The maximum sorption capacity of the MIIP for Pb(II) was found to be 48.1 mg g(-1). Finally, the proposed analytical procedure was successfully applied to monitoring lead in human hair and water samples with satisfactory results for the spiked samples.

  8. ChromatoGate: A Tool for Detecting Base Mis-Calls in Multiple Sequence Alignments by Semi-Automatic Chromatogram Inspection

    Directory of Open Access Journals (Sweden)

    Alexandros Stamatakis

    2013-03-01

    Full Text Available Automated DNA sequencers generate chromatograms that contain raw sequencing data. They also generate data that translates the chromatograms into molecular sequences of A, C, G, T, or N (undetermined characters. Since chromatogram translation programs frequently introduce errors, a manual inspection of the generated sequence data is required. As sequence numbers and lengths increase, visual inspection and manual correction of chromatograms and corresponding sequences on a per-peak and per-nucleotide basis becomes an error-prone, time-consuming, and tedious process. Here, we introduce ChromatoGate (CG, an open-source software that accelerates and partially automates the inspection of chromatograms and the detection of sequencing errors for bidirectional sequencing runs. To provide users full control over the error correction process, a fully automated error correction algorithm has not been implemented. Initially, the program scans a given multiple sequence alignment (MSA for potential sequencing errors, assuming that each polymorphic site in the alignment may be attributed to a sequencing error with a certain probability. The guided MSA assembly procedure in ChromatoGate detects chromatogram peaks of all characters in an alignment that lead to polymorphic sites, given a user-defined threshold. The threshold value represents the sensitivity of the sequencing error detection mechanism. After this pre-filtering, the user only needs to inspect a small number of peaks in every chromatogram to correct sequencing errors. Finally, we show that correcting sequencing errors is important, because population genetic and phylogenetic inferences can be misled by MSAs with uncorrected mis-calls. Our experiments indicate that estimates of population mutation rates can be affected two- to three-fold by uncorrected errors.

  9. Fundamental studies of the plasma extraction and ion beam formation processes in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Niu, Hongsen

    1995-02-10

    The fundamental and practical aspects are described for extracting ions from atmospheric pressure plasma sources into an analytical mass spectrometer. Methodologies and basic concepts of inductively coupled plasma mass spectrometry (ICP-MS) are emphasized in the discussion, including ion source, sampling interface, supersonic expansion, slumming process, ion optics and beam focusing, and vacuum considerations. Some new developments and innovative designs are introduced. The plasma extraction process in ICP-MS was investigated by Langmuir measurements in the region between the skimmer and first ion lens. Electron temperature (T{sub e}) is in the range 2000--11000 K and changes with probe position inside an aerosol gas flow. Electron density (n{sub e}) is in the range 10{sup 8}--10{sup 10} {sup {minus}cm }at the skimmer tip and drops abruptly to 10{sup 6}--10{sup 8} cm{sup {minus}3} near the skimmer tip and drops abruptly to 10{sup 6}--10{sup 8} cm{sup {minus}3} downstream further behind the skimmer. Electron density in the beam leaving the skimmer also depends on water loading and on the presence and mass of matrix elements. Axially resolved distributions of electron number-density and electron temperature were obtained to characterize the ion beam at a variety of plasma operating conditions. The electron density dropped by a factor of 101 along the centerline between the sampler and skimmer cones in the first stage and continued to drop by factors of 10{sup 4}--10{sup 5} downstream of skimmer to the entrance of ion lens. The electron density in the beam expansion behind sampler cone exhibited a 1/z{sup 2} intensity fall-off (z is the axial position). An second beam expansion originated from the skimmer entrance, and the beam flow underwent with another 1/z{sup 2} fall-off behind the skimmer. Skimmer interactions play an important role in plasma extraction in the ICP-MS instrument.

  10. Layer-by-layer encapsulated nano-emulsion of ionic liquid loaded with functional material for extraction of Cd(2+) ions from aqueous solutions.

    Science.gov (United States)

    Elizarova, Iuliia S; Luckham, Paul F

    2017-04-01

    Ionic liquids can serve as an environmentally-friendly replacement for solvents in emulsions, therefore they are considered suitable to be used as an emulsified medium for various active materials one of which are extractors of metal ions. Increasing the extraction efficiency is considered to be one of the key objectives when working with such extraction systems. One way to improve the extraction efficiency is to increase the contact area between the extractant and the working ionic solution. This can be accomplished by creating a nano-emulsion of ionic liquid containing such an extractant. Since emulsification of ionic liquid is not always possible in the sample itself, there is a necessity of creating a stable emulsion that can be added externally and on demand to samples from which metal ions need to be extracted. We propose a method of fabrication of a highly-stable extractant-loaded ionic liquid-in-water nano-emulsion via a low-energy phase reversal emulsification followed by continuous layer-by-layer polyelectrolyte deposition process to encapsulate the nano-emulsion and enhance the emulsion stability. Such a multilayered stabilized nano-emulsion was tested for extraction of Cd(2+) and Ca(2+) ions in order to determine its extraction efficiency and selectivity. It was found to be effective in the extraction of Cd(2+) ions with near 100% cadmium removal, as well as being selective since no Ca(2+) ions were extracted. The encapsulated emulsion was removed from samples post-extraction using two methods - filtration and magnetic separation, both of which were shown to be viable under different circumstances - larger and mechanically stronger capsules could be removed by filtration, however magnetic separation worked better for both smaller and bigger capsules. The long-term stability of nano-emulsion was also tested being a very important characteristic for its proposed use: it was found to be highly stable after four months of storage time.

  11. Evaluation of extraction procedures for the ion chromatographic determination of arsenic species in plant materials.

    Science.gov (United States)

    Schmidt, A C; Reisser, W; Mattusch, J; Popp, P; Wennrich, R

    2000-08-11

    The determination of arsenic species in plants grown on contaminated sediments and soils is important in order to understand the uptake, transfer and accumulation processes of arsenic. For the separation and detection of arsenic species, hyphenated techniques can be applied successfully in many cases. A lack of investigations exists in the handling (e.g., sampling, pre-treatment and extraction) of redox- and chemically labile arsenic species prior to analysis. This paper presents an application of pressurized liquid extraction (PLE) using water as the solvent for the effective extraction of arsenic species from freshly harvested plants. The method was optimized with respect to extraction time, number of extraction steps and temperature. The thermal stability of the inorganic and organic arsenic species under PLE conditions (60-180 degrees C) was tested. The adaptation of the proposed extraction method to freeze-dried, fine-grained material was limited because of the insufficient reproducibility in some cases.

  12. Measurements of an ion beam diameter extracted into air through a glass capillary

    Energy Technology Data Exchange (ETDEWEB)

    Fujita, Natsuko, E-mail: fujita.natsuko@jaea.go.jp [Graduate School of Humanities and Sciences, Nara Women’s University, Nara, 630 8506 (Japan); Yamaki, Atsuko [Graduate School of Humanities and Sciences, Nara Women’s University, Nara, 630 8506 (Japan); Ishii, Kunikazu; Ogawa, Hidemi [Department of Physics, Nara Women’s University, Nara, 630 8506 (Japan)

    2013-11-15

    To establish techniques for in-air materials analysis using a glass capillary, we studied the beam distribution extracted in air as a function of the distance between the exit of the capillary and the target. We measured three-dimensional intensity distributions of the extracted beams, and compared the observed results with the model calculation. The comparison showed that the glass capillary technique is designed to reduce a divergence of the beam extracted into the air by a beam-focusing effect.

  13. Radiation effects on hydrophobic ionic liquid [C4mim][NTf2] during extraction of strontium ions.

    Science.gov (United States)

    Yuan, Liyong; Peng, Jing; Xu, Ling; Zhai, Maolin; Li, Jiuqiang; Wei, Genshuan

    2009-07-02

    The applications of room-temperature ionic liquids (RTILs) in separation of high level radioactive nuclides demand a comprehensive knowledge of the stability and metal ion extraction of RTILs under radiation. Herein, we assessed the influence of gamma-irradiation on the [C(4)mim][NTf(2)]-based extraction system, where [C(4)mim](+) is 1-butyl-3-methylimidazolium and [NTf(2)](-) is bis(trifluoromethylsulfonyl)imide, by solvent extraction of Sr(2+) using irradiated [C(4)mim][NTf(2)] in combination with dicyclohexyl-18-crown-6 (DCH18C6). It was found that the degree of extraction for Sr(2+) from water to irradiated [C(4)mim][NTf(2)] decreased compared with that to unirradiated [C(4)mim][NTf(2)], and the decrement enhanced obviously with increasing dose. NMR spectroscopic probe analysis revealed the formation of acids during irradiation of [C(4)mim][NTf(2)]. The decrease of Sr(2+) partitioning in irradiated [C(4)mim][NTf(2)] is attributed to the competition between H(+) with Sr(2+) to interact with DCH18C6. Accordingly, washing irradiated [C(4)mim][NTf(2)] with water gives a simple way of ionic liquid recycling. Furthermore, the degree of extraction for Sr(2+) from 3 mol.L(-1) nitric acid solution to [C(4)mim][NTf(2)] is independent of the irradiation of [C(4)mim][NTf(2)] since the amount of the radiation-generated H(+) is negligible in such a high acidic solution.

  14. Transport of yttrium metal ions through fibers supported liquid membrane solvent extraction

    Institute of Scientific and Technical Information of China (English)

    A.G.Gaikwad; A.M.Rajput

    2010-01-01

    A novel idea of transport of yttrium(Ⅲ) metal ions through fibers supported liquid membrane in two stage processes namely source to membrane and membrane to receiving phase has been proposed.The fibers supported liquid membrane was impregnated with different concentrations carrier.The experimental variables explored were concentration of yttrium(Ⅲ) ions,pH of source phase,PC-88A concentration in membrane phase,acid concentration in receiving phase and stirring speed.The pre-concentration of yttrium(Ⅲ) ions ...

  15. Preconcentration and determination of zinc and lead ions by a combination of cloud point extraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, H. [Chemistry Department, Payamenore University, Shiraz (Iran); Shokrollahi, A.; Zahedi, M. [Chemistry Department, Yasouj University, Yasouj (Iran); Niknam, K. [Chemistry Department, Persian Gulf University, Bushehr (Iran); Soylak, M. [Chemistry Department, University of Erciyes, Kayseri (Turkey); Ghaedi, M.

    2009-04-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead(II) and zinc(II). After complexation with 3-[(4-bromophenyl) (1-H-inden-3-yl)methyl]-1 H-indene (BPIMI), the analytes were quantitatively extracted to a phase rich in Triton X-114 after centrifugation. Methanol acidified with 1 mol/L HNO{sub 3} was added to the surfactant rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of bis((1H-benzo [d] imidazol-2yl)ethyl)sulfane, Triton X-114, pH and amount of surfactant were all optimized. Detection limits (3 SDb/m) of 2.5 and 1.6 ng/mL for Pb{sup 2+} and Zn{sup 2+} along with preconcentration factors of 30 and an enrichment factor of 32 and 48 for Pb{sup 2+}and Zn {sup 2+} ions were obtained, respectively. The proposed cloud point extraction was been successfully applied for the determination of these ions in real samples with complicated matrices such as food and soil samples, with high efficiency. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  16. Cloud point extraction and flame atomic absorption spectrometry combination for copper(II) ion in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: ashokrollahi@mail.yu.ac.ir; Ghaedi, Mehrorang [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Hossaini, Omid; Khanjari, Narges [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-12-30

    A cloud point extraction procedure was presented for the preconcentration of copper(II) ion in various samples. After complexation by 4-(phenyl diazenyl) benzene-1,3-diamine (PDBDM) (chrysoidine), copper(II) ions were quantitatively recovered in Triton X-114 after centrifugation. 0.5 ml of methanol acidified with 1.0 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The influence of analytical parameters including ligand, Triton X-114 and HNO{sub 3} concentrations, bath temperature, heating time, centrifuge rate and time were optimized. The effect of the matrix ions on the recovery of copper(II) ions was investigated. The detection limit (3S.D.{sub b}/m, n = 10) of 0.6 ng mL{sup -1} along with preconcentration factor of 30 and enrichment factor of 41.1 with R.S.D. of 1.0% for Cu was achieved. The proposed procedure was applied to the analysis of various environmental and biological samples.

  17. Ion-pair mediated transport of small model peptides in liquid phase micro extraction under acidic conditions.

    Science.gov (United States)

    Reubsaet, J Léon E; Paulsen, Jonas V

    2005-02-01

    This paper discusses the behaviour of five small model peptides in a three phase (aqueous donor-organic-aqueous acceptor) liquid phase micro extraction system in relation to their physico-chemical properties (charge, hydrophobicity). It is proved that for all peptides transport over the organic phase is mediated by aliphatic sulphonic acids. Heptane-1-sulphonic acid gave the best overall recoveries. It appeared that peptides with hydrophobic properties (IPI) and a high number of positive charges (KYK) show good recoveries and are enriched in the acceptor phase. Variation in the pH (1.6-4.4) of the donor phase shows that there are peptide-dependent optimal pH-values for their recovery. Increasing pH in the acceptor phase shows that in most cases the recovery decreases due to decreased ion-pair mediated membrane transport. For KYK the partition between the organic phase and the aqueous acceptor-phase is also driven by the solubility in the aqueous acceptor phase. Increase of the ion strength of the acceptor phase did not affect the recovery of the peptides. Except for KYK, which showed decreased recovery when the ion strength increased. Another finding is that delocalisation of positive charge causes bad recovery, probably due to incomplete ion-pair-peptide complex formation.

  18. Satellite Lithium-Ion Battery Remaining Cycle Life Prediction with Novel Indirect Health Indicator Extraction

    OpenAIRE

    Haitao Liao; Wei Xie; Yu Peng; Datong Liu; Hong Wang

    2013-01-01

    Prognostics and remaining useful life (RUL) estimation for lithium-ion batteries play an important role in intelligent battery management systems (BMS). The capacity is often used as the fade indicator for estimating the remaining cycle life of a lithium-ion battery. For spacecraft requiring high reliability and long lifetime, in-orbit RUL estimation and reliability verification on ground should be carefully addressed. However, it is quite challenging to monitor and estimate the capacity of a...

  19. Optimization and adsorption kinetic studies of aqueous manganese ion removal using chitin extracted from shells of edible Philippine crabs

    Science.gov (United States)

    Quimque, Mark Tristan J.; Jimenez, Marvin C.; Acas, Meg Ina S.; Indoc, Danrelle Keth L.; Gomez, Enjelyn C.; Tabuñag, Jenny Syl D.

    2017-01-01

    Manganese is a common contaminant in drinking water along with other metal pollutants. This paper investigates the use of chitin, extracted from crab shells obtained as restaurant throwaway, as an adsorbent in removing manganese ions from aqueous medium. In particular, this aims to optimize the adsorption parameters and look into the kinetics of the process. The adsorption experiments done in this study employed the batch equilibration method. In the optimization, the following parameters were considered: pH and concentration of Mn (II) sorbate solution, particle size and dosage of adsorbent chitin, and adsorbent-adsorbate contact time. At the optimal condition, the order of the adsorption reaction was estimated using kinetic models which describes the process best. It was found out that the adsorption of aqueous Mn (II) ions onto chitin obeys the pseudo-second order model. This model assumes that the adsorption occurred via chemisorption

  20. Capillary ion chromatography-mass spectrometry for simultaneous determination of glucosylglycerol and sucrose in intracellular extracts of cyanobacteria.

    Science.gov (United States)

    Fa, Yun; Liang, Wenhui; Cui, He; Duan, Yangkai; Yang, Menglong; Gao, Jun; Liu, Huizhou

    2015-09-15

    A capillary ion chromatography-mass spectrometry (MS) method was proposed to determine glucosylglycerol (GG), sucrose, and five other carbohydrates. MS conditions and make-up flow parameters were optimized. This method is accurate and sensitive for simultaneous analysis of carbohydrates, with mean correlation coefficients of determination greater than 0.99, relative standard deviation of 0.91-2.81% for eight replicates, and average spiked recoveries of 97.3-104.9%. Limits of detection of sodium adduct were obtained with MS detection in selected ion mode for GG (0.006mg/L), sucrose (0.02mg/L), and other carbohydrates (0.03mg/L). This method was successfully applied to determine GG and sucrose in intracellular extracts of salt-stressed cyanobacteria.

  1. Injection and extraction computer control system HIRFL-SSC The HIRFL-SSC is stated for Heavy Ion Research Facility of Lanzhou-Separated Sector Cyclotron

    CERN Document Server

    Zhang Wei; Chen Yun; Zhang Xia; Hu Jian Jun; Xu Xing Ming

    2002-01-01

    The injection and extraction computer control system of HIRFL-SSC (Heavy Ion Research Facility of Lanzhou-Separated Sector Cyclotron) have been introduced. Software is described briefly. Hardware structure is mainly presented. The computer control system realize that the adjustment of injection and extraction can done by PC and operate interface is Windows style. The system can make the adjustment convenient and veracious

  2. Experimental studies of a microsecond plasma opening switch in the positive polarity regime with inductive load/extraction ion diode

    Science.gov (United States)

    Bystritskii, V. M.; Lisitsyn, I. V.; Sinebryukhov, V. A.; Volkov, S. N.; Krasik, Ya. E.

    1992-06-01

    Systematic studies of the microsecond plasma opening switch (MPOS) operation in the positive polarity of its inner electrode with an inductive load/B-applied ion diode of the extraction type at a level of 0.3 TW of dissipated power were performed at the DOUBLE generator (300 kA, 480 kV, 1 μs). The detailed measurements of ion flow parameters in the conductive phase of the MPOS showed the considerable enhancement of the ion current amplitude over the thermal flow limit (3-10 times) which is coupled with a significant decrease of electron conductivity in the MPOS across its self-magnetic field. The positive polarity MPOS operation proved to be more critical to the stored current amplitudes and geometry of the electrodes in comparison with the negative polarity case. This fact resulted in limitations of satisfactory performance of the MPOS involving short high-voltage pulse duration, low stored current amplitudes, and a narrow region of acceptable electrode diameters. The variation of the diode anode-cathode (AC) gap provided a sensitive control of the MPOS + magnetically insulated diode (MID) system, which displayed very strong coupling, resulting in clamping of the output voltage in a wide region of diode impedances. The early long-duration (<300 ns) high-voltage (50-200 kV) prepulse improves plasma production at the anode of the MID prior to the application of the main pulse. The optimal performance of the MPOS+MID system was realized at the level of ZMPOS/ZMID = 2.5. The energy of the extracted high-power ion beam made up 3.5 kJ, its power being 120 GW with 40% efficiency of energy transfer from MPOS to the MID.

  3. Comparison of volatile constituents extracted from model grape juice and model wine by stir bar sorptive extraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Caven-Quantrill, Darren J; Buglass, Alan J

    2011-02-18

    A stir bar sorptive extraction (SBSE) method coupled with gas chromatography-mass spectrometry was optimised for the analysis of volatile components of a model wine, based on a previously optimised method used for analysis of the same components in model grape juice. The presence of ethanol in the model wine sample matrix resulted in decreased sensitivity of the method toward most of the volatile constituents. Mean percent relative recoveries and reproducibilities (%CV) were 22.8% and 7.1%, respectively, compared with 28.4% and 8.5% for model grape juice. The mean limit of detection (LoD) ratio (juice:wine) was 0.25. Similar sensitivities for the two sample matrices using this method were achieved by changing the split ratio from 20:1 (grape juice) to 5:1 (wine), giving a mean limit of detection ratio (juice:wine) of 1.0, thus allowing direct comparison of chromatograms of volatile components in the two matrices. This enabled direct comparisons of grape juices and the wines derived from them by alcoholic yeast fermentation. The influence of ethanol concentration in the range 9-15% on method sensitivity is discussed, using an overlay of the total ion chromatograms. The use of a gas saver device for the 5:1 split ratio analysis of desorbed model wine aroma compounds is discussed in terms of preventing extraneous reaction of sorbent and stationary phases with air during analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Removal of Radioactive Nuclides by Multi-Functional Microcapsules Enclosing Inorganic Ion-Exchangers and Organic Extractants

    Energy Technology Data Exchange (ETDEWEB)

    Mimura, H.; Akiba, K.; Onodera, Y.

    2002-02-26

    The microcapsules enclosing two kinds of functional materials, inorganic ion-exchangers and organic extractants, were prepared by taking advantage of the high immobilization ability of alginate gel polymer. The fine powders of inorganic ion-exchanger and oil drops of extractant were kneaded with sodium alginate (NaALG) solution and the kneaded sol readily gelled in a salt solution of CaCl2, BaCl2 or HCl to form spherical gel particles. The uptake properties of various nuclides, 137Cs, 85Sr, 60Co, 88Y, 152Eu and 241Am, for thirty-four specimens of microcapsules in the presence of 10-1-10-4 M HNO3 were evaluated by the batch method. The distribution coefficient (Kd) of Cs+ above 103 cm3/g was obtained for the microcapsules enclosing CuFC or AMP. The Kd of Sr2+ around 102 cm3/g was obtained for the microcapsules containing clinoptilolite, antimonic acid, zeolite A, zeolite X or titanic acid. The microcapsules enclosing DEHPA exhibited relatively large Kd values of trivalent metal ions above 103 cm3/g; for example, the Kd values of Cs+, Sr2+, Co2+, Y3+, Eu3+ and Am3+ for a favorable microcapsule (CuFC/clinoptilolite/DEHPA/CaALG) were 1.1x104, 7.5x10, 1.1x10, 1.0x104, 1.4x104, 3.4x103 cm3/g, respectively. The uptake rates of Cs+, Y3+, Eu3+ and Am3+ for this microcapsule were rather fast; the uptake percentage above 90% was obtained after 19 h-shaking and the uptake equilibrium was attained within 1 d. The AMP/CaALG exhibited high uptake ability for Cs+ even after irradiation of 188 kGy, and DEHPA/CaALG microcapsule had similar Kd values of Cs+, Sr2+, Co2+, Y3+, Eu3+ and Am3+ ions before and after irradiation. The microcapsules with various shapes such as spherical, columnar, fibrous and filmy forms were easily prepared by changing the way of dipping kneaded sol into gelling salt solution. The microcapsules enclosing inorganic ion-exchangers and extractants have a potential possibility for the simultaneous removal of various radioactive nuclides from waste solutions.

  5. The Rate of Decolorization of a Radical Ion Reagent Was Used to Determine the Phenolic Content of Various Food Extracts

    Directory of Open Access Journals (Sweden)

    Arthur Bradley

    2013-01-01

    Full Text Available Polyphenols are among the most valuable and widely studied food components. In the laboratory, they are readily extractable with aqueous alcohol. An aliquot rapidly decolorizes a measured portion of ABTS, a stable deep blue radical ion. The semilog plot of light absorption versus time is typically a straight line, and an immediately evident slope provides rapid classification in terms of gallic acid equivalents. Experimental data are presented to show general agreement with the literature. The disproportionate concentration of antioxidant in the skins and peels of fruits, vegetables, and nuts is given special attention.

  6. Upgraded millimeter-wave interferometer for measuring the electron density during the beam extraction in the negative ion source

    Science.gov (United States)

    Tokuzawa, T.; Kisaki, M.; Nagaoka, K.; Tsumori, K.; Ito, Y.; Ikeda, K.; Nakano, H.; Osakabe, M.; Takeiri, Y.; Kaneko, O.

    2016-11-01

    The upgraded millimeter-wave interferometer with the frequency of 70 GHz is installed on a large-scaled negative ion source. Measurable line-averaged electron density is from 2 × 1015 to 3 × 1018 m-3 in front of the plasma grid. Several improvements such as the change to shorter wavelength probing with low noise, the installation of special ordered horn antenna, the signal modulation for a high accuracy digital phase detection, the insertion of insulator, and so on, are carried out for the measurement during the beam extraction by applying high voltage. The line-averaged electron density is successfully measured and it is found that it increases linearly with the arc power and drops suddenly at the beam extraction.

  7. Synthesis, Structure and Ion Extraction Properties of Novel Monooxa-diselkylene-1,ω-dioxy Substituted Calix[4]arene Derivatives

    Institute of Scientific and Technical Information of China (English)

    QIN Da-Bin; ZENG Xian-Shun; XU Feng-Bo; LI Qing-Shan; ZHANG Zheng-Zhi

    2006-01-01

    Novel macrocyclic monooxa-diselkylene-1,ω-dioxy substituted calix[4]arene derivatives 1a-5a were synthesized by the reaction of calix[4]arene dibromides 1-5 with the disodium salt of bis(2-selenylethyl)ether in the yields between 28% and 64%. Their structures were characterized by proton and carbon NMR spectra. X-Ray structure analysis of 1a further confirmed the cone conformation of compounds 1a-5a. An interesting host-guest complex of 1a with dichloromethane via CH/π and Cl/π interactions was elucidated. Extraction experiments showed that these novel monooxa-diselkylene-1,ω-dioxy substituted calix[4]arene derivatives 1a-5a had strong extraction ability towards mercury ion. The interaction of Hg2+with the calix ligand has also been investigated by 1H NMR titration.

  8. Co-extraction of egg white proteins using ion-exchange chromatography from ovomucin-removed egg whites.

    Science.gov (United States)

    Omana, Dileep A; Wang, Jiapei; Wu, Jianping

    2010-07-01

    Efficient isolation of egg white components is desired due to its potential uses. Existing methods mainly targeted on one specific protein; an attempt has been made in the study to co-extract all the valuable egg white components in a continuous process. Ovomucin was first isolated by our newly developed two-step method; the resultant supernatant obtained after ovomucin isolation was used as the starting material for ion-exchange chromatography. Anion-exchange chromatography of 100 mM supernatant yielded a flow-through fraction and three other fractions representing ovotransferrin, ovalbumin and flavoproteins. The flow-through fraction was further separated into ovoinhibitor, lysozyme, ovotransferrin and an unidentified fraction which represents 4% of total egg white proteins. Chromatographic separation of 500 mM supernatant resulted in fractions representing lysozyme, ovotransferrin and ovalbumin. This co-extraction protocol represents a global recovery of 71.0% proteins.

  9. ECR离子源引出束流周期性波动研究%Observation of Burst Frequency in Extracted ECR Ion Current

    Institute of Scientific and Technical Information of China (English)

    G.S.Taki; P.R.Sarma; A.G.Drentje; T.Nakagawa; P.K.Ray; R.K.Bhandari

    2007-01-01

    Earlier we reported an ion current jump which was observed at a fixed negative biased disc potential in the 6.4GHz ECR ion source at VECC,Kolkata.In a recent experiment with neon ions.we measured the time spectra of the ion current and observed the presence of a burst frequency in the kilohertz range.This frequency shows a correlated jump with the ion current jump described above.Another interesting feature is that the observed burst frequency shows a good linear correlation with the extracted ion current.The higher the ion current,the higher is the burst frequency.This means that current per burst is a constant factor;when there are more number of bursts,the current also increases.

  10. Ion-pair cloud-point extraction: a new method for the determination of water-soluble vitamins in plasma and urine.

    Science.gov (United States)

    Heydari, Rouhollah; Elyasi, Najmeh S

    2014-10-01

    A novel, simple, and effective ion-pair cloud-point extraction coupled with a gradient high-performance liquid chromatography method was developed for determination of thiamine (vitamin B1 ), niacinamide (vitamin B3 ), pyridoxine (vitamin B6 ), and riboflavin (vitamin B2 ) in plasma and urine samples. The extraction and separation of vitamins were achieved based on an ion-pair formation approach between these ionizable analytes and 1-heptanesulfonic acid sodium salt as an ion-pairing agent. Influential variables on the ion-pair cloud-point extraction efficiency, such as the ion-pairing agent concentration, ionic strength, pH, volume of Triton X-100, extraction temperature, and incubation time have been fully evaluated and optimized. Water-soluble vitamins were successfully extracted by 1-heptanesulfonic acid sodium salt (0.2% w/v) as ion-pairing agent with Triton X-100 (4% w/v) as surfactant phase at 50°C for 10 min. The calibration curves showed good linearity (r(2) > 0.9916) and precision in the concentration ranges of 1-50 μg/mL for thiamine and niacinamide, 5-100 μg/mL for pyridoxine, and 0.5-20 μg/mL for riboflavin. The recoveries were in the range of 78.0-88.0% with relative standard deviations ranging from 6.2 to 8.2%.

  11. Utilizing ion-pairing hydrophilic interaction chromatography solid phase extraction for efficient glycopeptide enrichment in glycoproteomics

    DEFF Research Database (Denmark)

    Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter;

    2010-01-01

    Glycopeptide enrichment is a prerequisite to enable structural characterization of protein glycosylation in glycoproteomics. Here we present an improved method for glycopeptide enrichment based on zwitter-ionic hydrophilic interaction chromatography solid phase extraction (ZIC-HILIC SPE...

  12. A study on prevention of an electric discharge at an extraction electrode of an electron cyclotron resonance ion source for cancer therapy

    Energy Technology Data Exchange (ETDEWEB)

    Kishii, Y., E-mail: Ando.Yasuto@ct.MitsubishiElectric.co.jp; Kawasaki, S. [Energy Systems Center, Mitsubishi Electric Corporation, 1-1-2 Wadasaki-cho, Hyogo-ku, Kobe 652-8555 (Japan); Kitagawa, A.; Muramatsu, M. [National Institute of Radiological Sciences, 4-9-1 Anagawa, Inage, Chiba 263-8555 (Japan); Uchida, T. [Bio-Nano Electronics Research Center, Toyo University, 2100 Kujirai, Kawagoe 350-8585 (Japan); Graduate School of Interdisciplinary New Science, Toyo University, 2100 Kujirai, Kawagoe 350-8585 (Japan)

    2014-02-15

    A compact ECR ion source has utilized for carbon radiotherapy. In order to increase beam intensity with higher electric field at the extraction electrode and be better ion supply stability for long periods, electric geometry and surface conditions of an extraction electrode have been studied. Focusing attention on black deposited substances on the extraction electrode, which were observed around the extraction electrode after long-term use, the relation between black deposited substances and the electrical insulation property is investigated. The black deposited substances were inspected for the thickness of deposit, surface roughness, structural arrangement examined using Raman spectroscopy, and characteristics of electric discharge in a test bench, which was set up to simulate the ECR ion source.

  13. Optimization of sodium extraction from soil by using a central composite design (CCD and determination of soil sodium content by ion selective electrodes

    Directory of Open Access Journals (Sweden)

    Sevinç Karadağ

    2016-04-01

    Full Text Available Rapid determination of sodium (Na ions in soil samples using ion selective electrodes (ISE was investigated in this study. The compatibility of ISEs with soil extraction solution is a challenging subject as various effects such as pH, ionic strength and other interferences have to be considered as well as efficiency of the extraction solution. Because almost every type of sodium salt is soluble in water, and the pH of water is suitable for ISE studies, it was chosen as the soil extractant. Firstly, the extraction parameters were optimized by using a central composite design (CCD, secondly thirty agricultural soil samples were extracted with water and the extracts were measured by Na-ISE in a previously developed flow system. The results were compared with ion chromatography (IC as the reference method, and the regression analysis between IC and ISE results yielded a high correlation (R² = 0.9408. It was concluded that, ion selective electrodes can be used with water as an extraction solution for rapid determination of sodium in soil samples.

  14. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/....

  15. Solid phase extraction and determination of sub-ppb levels of hazardous Hg2+ ions.

    Science.gov (United States)

    Shamsipur, Mojtaba; Shokrollahi, Ardeshir; Sharghi, Hashem; Eskandari, Mohammad Mehdi

    2005-01-31

    A simple, rapid and reliable method has been developed to selectively separate and concentrate ultra trace amounts of mercury(II) ions from aqueous samples for its highly sensitive measurement by cold vapor atomic absorption spectrometry (CV-AAS). The Hg(2+) ions were adsorbed selectively and quantitatively during the passage of aqueous samples through octadecyl silica membrane disks modified by isopropyl 2-[(isopropoxycarbothiolyl)disulfanyl]ethane thioate (IIDE). The retained Hg(2+) ions were then stripped from the disk with minimal amounts of 0.5 M hydrobromic acid (two 8 ml portions) as eluent, and determined by CV-AAS. The break-through volume of the method is greater than 3000 ml, which results in enrichment factors >150. Maximum capacity of the membrane disks modified with 10mg of the ligand was found to be 350+/-30 microg of mercury(II), and the limit of detection is 0.005 ng ml(-1). The effect of various cationic interferences on the recovery of mercury in binary mixtures was studied. The method was applied to the recovery of Hg(2+) ions from different synthetic and tap water samples, as well as the determination of mercury in human hair samples.

  16. Near Discharge Cathode Assembly Plasma Potential Measurements in a 30-cm NSTAR Type Ion Engine During Beam Extraction

    Science.gov (United States)

    Herman, Daniel A.; Gallimore, Alec D.

    2006-01-01

    Floating emissive probe plasma potential data are presented over a two-dimensional array of locations in the near Discharge Cathode Assembly (DCA) region of a 30-cm diameter ring-cusp ion thruster. Discharge plasma data are presented with beam extraction at throttling conditions comparable to the NASA TH Levels 8, 12, and 15. The operating conditions of the Extended Life Test (ELT) of the Deep Space One (DS1) flight spare ion engine, where anomalous discharge keeper erosion occurred, were TH 8 and TH 12 consequently they are of specific interest in investigating discharge keeper erosion phenomena. The data do not validate the presence of a potential hill plasma structure downstream of the DCA, which has been proposed as a possible erosion mechanism. The data are comparable in magnitude to data taken by other researchers in ring-cusp electron-bombardment ion thrusters. The plasma potential structures are insensitive to thruster throttling level with a minimum as low as 14 V measured at the DCA exit plane and increasing gradually in the axial direction. A sharp increase in plasma potential to the bulk discharge value of 26 to 28 volts, roughly 10 mm radially from DCA centerline, was observed. Plasma potential measurements indicate a low-potential plume structure that is roughly 20 mm in diameter emanating from the discharge cathode that may be attributed to a free-standing plasma double layer.

  17. Ion current extracted from a self ignition plasma around the target immersed in a pulsed rf ICP methane plasma

    Science.gov (United States)

    Tanaka, Takeshi; Watanabe, Satoshi; Mizuno, Giichiro; Takagi, Toshinori; Yoshida, Mitsuhiro; Horibe, Hiroshi; Yukimura, Ken

    2003-05-01

    When a pulsed voltage is applied to a target immersed in plasma, the surrounding medium of the target is self-ignited under an appropriate discharge condition. For a three-dimensional substrate, ion implantation and deposition of the plasma species are promising to be uniformly attained by the self-ignition plasma. A retained dose of conformal ion implantation may increase with the self-ignition plasma generated in the target-immersed plasma. Ion are extracted from both the target-immersed plasma and the self-ignition plasma. In this research, a stainless steel target with a diameter of 140 mm and a thickness of 18 mm was immersed in a pulsed inductively coupled methane plasma to which a pulse voltage of -400 V to -10 kV with a width of 12 μs was repeatedly applied. The self-ignition plasma was generated at the voltage higher than about -1.2 kV. It was found that the shape of the current waveform changes by varying the applied voltage due to the change of the current from the self-ignition plasma.

  18. Control of a large vacuum wave precursor on the SABRE voltage adder MITL and extraction ion diode

    Science.gov (United States)

    Cuneo, M. E.; Hanson, D. L.; Poukey, J. W.; Menge, P. R.; Savage, M. E.; Smith, J. R.; Bernard, M. A.

    SABRE is a ten-cavity magnetically insulated voltage adder (6MV, 300 kA) used to study ion beam production in high voltage extraction applied-B ion diodes. Observations indicate that the machine power initially propagates in a large-amplitude vacuum wave prior to electron emission. This vacuum wave 'precursor' has an important impact on the turn-on and impedance history of ion diodes. Some typical precursor characteristics are shown using transmission line, diode, and beam current and voltage data and are compared to TWOQUICK simulations. Two techniques are under investigation to control the precursor and its effects on diode performance. A plasma opening switch (POS) has been used to erode the precursor. Field enhancing inserts are also planned to decrease the macroscopic field required for electron emission from the cathode. This will limit the distance over which vacuum and insulated waves separate by propagation at different velocities. Experimental data from the POS technique and TWOQUICK simulations of the insert technique are presented and discussed.

  19. In Vitro Ion Chelating, Antioxidative Mechanism of Extracts from Fruits and Barks of Tetrapleura tetraptera and Their Protective Effects against Fenton Mediated Toxicity of Metal Ions on Liver Homogenates

    Directory of Open Access Journals (Sweden)

    Bruno Moukette Moukette

    2015-01-01

    Full Text Available The aim of the present study was to investigate the antioxidant activity and protective potential of T. tetraptera extracts against ion toxicity. The antioxidant activity of the extracts was investigated spectrophotometrically against several radicals (1,1-diphenyl-2-picrylhydrazyl (DPPH•, 2,2′-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid (ABTS•, hydroxyl radical (HO•, and nitric oxide (NO•, followed by the ferric reducing power, total phenols, flavonoid, and flavonol contents. The effects of the extracts on catalase (CAT, superoxide dismutase (SOD, and peroxidase activities were also determined using the standard methods as well as the polyphenol profile using HPLC. The results showed that the hydroethanolic extract of T. tetraptera (CFH has the lowest IC50 value with the DPPH, ABTS, OH, and NO radicals. The same extract also exhibited the significantly higher level of total phenols (37.24 ± 2.00 CAE/g dried extract; flavonoids (11.36 ± 1.88 QE/g dried extract; and flavonols contents (3.95 ± 0.39 QE/g dried extract. The HPLC profile of T. tetraptera revealed that eugenol (958.81 ± 00 mg/g DW, quercetin (353.78 ± 00 mg/g DW, and rutin (210.54 ± 00 mg/g DW were higher in the fruit than the bark extracts. In conclusion, extracts from T. tetraptera may act as a protector against oxidative mediated ion toxicity.

  20. Selective cloud point extraction and graphite furnace atomic absorption spectrometric determination of molybdenum (VI) ion in seawater samples

    Energy Technology Data Exchange (ETDEWEB)

    Filik, Hayati, E-mail: filik@istanbul.edu.tr [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey); Cengel, Tayfun; Apak, Resat [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)

    2009-09-30

    A cloud point extraction process using the nonionic surfactant Triton X-114 to extract molybdenum from aqueous solutions was investigated. The method is based on the complexation reaction of Mo(VI) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarine: QA) and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by graphite furnace atomic absorption spectrometry (GFAAS). The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature, incubation and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the limit of detection (LOD) for Mo(VI) was 7.0 ng L{sup -1} with an preconcentration factor of {approx}25 when 10 mL of sample solution was preconcentrated to 0.4 mL. The proposed method (with extraction) showed linear calibration within the range 0.03-0.6 {mu}g L{sup -1}. The relative standard deviation (RSD) was found to be 3.7% (C{sub Mo(VI)} = 0.05 {mu}g L{sup -1}, n = 5) for pure standard solutions, whereas RSD for the recoveries from real samples ranged between 2 and 8% (mean RSD = 3.9%). The method was applied to the determination of Mo(VI) in seawater and tap water samples with a recovery for the spiked samples in the range of 98-103%. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. In order to verify the accuracy of the method, a certified reference water sample was analysed and the results obtained were in good agreement with the certified values.

  1. Determination of trace labile copper in environmental waters by magnetic nanoparticle solid phase extraction and high-performance chelation ion chromatography.

    Science.gov (United States)

    Wei, Z; Sandron, S; Townsend, A T; Nesterenko, P N; Paull, B

    2015-04-01

    Cobalt magnetic nanoparticles surface functionalised with iminodiacetic acid were evaluated as a nano-particulate solid phase extraction absorbent for copper ions (Cu(2+)) from environmental water samples. Using an external magnetic field, the collector nanoparticles could be separated from the aqueous phase, and adsorbed ions simply decomplexed using dilute HNO3. Effects of pH, buffer concentration, sample and sorbent volume, extraction equilibrium time, and interfering ion concentration on extraction efficiency were investigated. Optimal conditions were then applied to the extraction of Cu(2+) ions from natural water samples, prior to their quantitation using high-performance chelation ion chromatography. The limits of detection (LOD) of the combined extraction and chromatographic method were ~0.1 ng ml(-1), based upon a 100-fold preconcentration factor (chromatographic performance; LOD=9.2 ng ml(-1) Cu(2+)), analytical linear range from 20 to 5000 ng mL(-1), and relative standard deviations=4.9% (c=1000 ng ml(-1), n=7). Accuracy and precision of the combined approach was verified using a certified reference standard estuarine water sample (SLEW-2) and comparison of sample determinations with sector field inductively coupled plasma mass spectrometry. Recoveries from the addition of Cu(2+) to impacted estuarine and rain water samples were 103.5% and 108.5%, respectively. Coastal seawater samples, both with and without prior UV irradiation and dissolved organic matter removal were also investigated using the new methodology. The effect of DOM concentration on copper availability was demonstrated.

  2. Investigation of different extraction procedures for the determination of major and trace elements in coal by ICP-AES and ion chromatography

    Directory of Open Access Journals (Sweden)

    Tasić Aleksandra M.

    2016-01-01

    Full Text Available This paper presents the extraction of major and trace elements from a coal sample, in deionized water, by using three different extraction techniques. Rotary mixing and ultrasonic extraction were examined for different extraction times, while the microwave assisted extraction was performed at different temperatures. Metal concentrations (Na, K, Ca, Mg, Al, Fe, Mn, Be, Cd, Co, Cr, Hg, As, Ni, Se, Sb and Pb in a solution were determined by employing the inductively coupled plasma atomic emission spectrometry; whereas the results obtained for Na, K, Ca and Mg were compared employing ion chromatography. Comparing the rotary and ultrasonic-assisted extraction it is shown that the former is more efficient for the determination of Fe, Na and Pb, whereas the latter one has proven more efficient for the determination of Co and Cr ions. Microwave-assisted extraction has proven the most efficient method for any elements tested in coal. In addition, sequential extraction of elements was done using microwave digestion. The results of sequential extraction experiments indicated associations of investigated elements with a mineral phase and organic matrix. Sequential extraction provided information on possible leaching of As, Cd, Co, Cr, Ni, Pb, Fe and Mn in environmental conditions. [Projekat Ministarstva nauke Republike Srbije, br. 172030

  3. Characterisation of polyacetylenes isolated from carrot (Daucus carota) extracts by negative ion tandem mass spectrometry.

    Science.gov (United States)

    Rai, Dilip K; Brunton, Nigel P; Koidis, Anastasios; Rawson, Ashish; McLoughlin, Padraig; Griffiths, William J

    2011-08-15

    The potential use of negative electrospray ionisation mass spectrometry (ESI-MS) in the characterisation of the three polyacetylenes common in carrots (Daucus carota) has been assessed. The MS scans have demonstrated that the polyacetylenes undergo a modest degree of in-source decomposition in the negative ionisation mode while the positive ionisation mode has shown predominantly sodiated ions and no [M+H](+) ions. Tandem mass spectrometric (MS/MS) studies have shown that the polyacetylenes follow two distinct fragmentation pathways: one that involves cleavage of the C3-C4 bond and the other with cleavage of the C7-C8 bond. The cleavage of the C7-C8 bond generated product ions m/z 105.0 for falcarinol, m/z 105/107.0 for falcarindiol, m/z 147.0/149.1 for falcarindiol-3-acetate. In addition to these product ions, the transitions m/z 243.2 → 187.1 (falcarinol), m/z 259.2 → 203.1 (falcarindiol), m/z 301.2 → 255.2/203.1 (falcarindiol-3-acetate), mostly from the C3-C4 bond cleavage, can form the basis of multiple reaction monitoring (MRM)-quantitative methods which are poorly represented in the literature. The 'MS(3) ' experimental data confirmed a less pronounced homolytic cleavage site between the C11-C12 bond in the falcarinol-type polacetylenes. The optimised liquid chromatography (LC)/MS conditions have achieved a baseline chromatographic separation of the three polyacetylenes investigated within 40 min total run-time.

  4. Ion-pair assisted extraction followed by (1)H NMR determination of biogenic amines in food and biological matrices.

    Science.gov (United States)

    Chatzimitakos, T; Exarchou, V; Ordoudi, S A; Fiamegos, Y; Stalikas, C

    2016-07-01

    A selective method for the extraction and determination of six biogenic amines (BAs) by NMR is presented. Briefly, BAs are extracted into an organic solvent via the use of an ion pairing agent, followed by a back extraction in D2O in order to acquire the (1)H NMR spectra. The method is studied with respect to the critical experimental parameters and is successfully applied to selected food substrates (dark chocolate, banana, gouda cheese) and biological samples (urine and blood plasma) signifying its potential as an alternative tool for BAs determination. Accurate and precise results are consistently achieved with all matrixes studied. The calculated limits of detection and limits of quantitation were found to be in the ranges 0.05-0.13μg/mL and 0.14-0.38μg/mL, respectively, for biological samples while for food samples they were in the ranges 2.25-6.25μg/g and 6.75-18.7μg/g, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Separation of boron from borated paraffin wax by pyrohydrolysis and alkali extraction methods and its determination using ion chromatography.

    Science.gov (United States)

    Raut, Vaibhavi Vishwajeet; Jeyakumar, Subbiah; Shah, Dipti Jayesh; Thakur, Uday Kumar; Tomar, Bhupendra Singh; Ramakumar, Karanam Lakshminarayana

    2015-01-01

    A method based on the pyrohydrolysis extraction of boron and its quantification with ion chromatography was proposed for paraffin waxes borated with H3BO3 and B4C. The optimum pyrohydrolysis conditions were identified. Wax samples were mixed with U3O8, which prevents the sample from flare up, and also accelerates the extraction of boron. Pyrohydrolysis was carried out with moist O2 at 950°C for 60 and 90 min for wax with H3BO3 and wax with B4C, respectively. Two simple methods of separation based on alkali extraction and melting wax in alkali were also developed exclusively for wax with H3BO3. In all the separations, the recovery of B was above 98%. During IC separation, B was separated as boron-mannitol anion complex. Linear calibration was obtained it between 0.1 and 50 ppm of B, and LOD was calculated as 5 ppb (S/N = 3). The reproducibility was better than 5% (RSD).

  6. Ion-exchange molecularly imprinted polymer for the extraction of negatively charged acesulfame from wastewater samples.

    Science.gov (United States)

    Zarejousheghani, Mashaalah; Schrader, Steffi; Möder, Monika; Lorenz, Pierre; Borsdorf, Helko

    2015-09-11

    Acesulfame is a known indicator that is used to identify the introduction of domestic wastewater into water systems. It is negatively charged and highly water-soluble at environmental pH values. In this study, a molecularly imprinted polymer (MIP) was synthesized for negatively charged acesulfame and successfully applied for the selective solid phase extraction (SPE) of acesulfame from influent and effluent wastewater samples. (Vinylbenzyl)trimethylammonium chloride (VBTA) was used as a novel phase transfer reagent, which enhanced the solubility of negatively charged acesulfame in the organic solvent (porogen) and served as a functional monomer in MIP synthesis. Different molecularly imprinted polymers were synthesized to optimize the extraction capability of acesulfame. The different materials were evaluated using equilibrium rebinding experiments, selectivity experiments and scanning electron microscopy (SEM). The most efficient MIP was used in a molecularly imprinted-solid phase extraction (MISPE) protocol to extract acesulfame from wastewater samples. Using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis, detection and quantification limits were achieved at 0.12μgL(-1) and 0.35μgL(-1), respectively. Certain cross selectivity for the chemical compounds containing negatively charged sulfonamide functional group was observed during selectivity experiments.

  7. Synthesis and characterisation of nano structure lead (II) ion-imprinted polymer as a new sorbent for selective extraction and preconcentration of ultra trace amounts of lead ions from vegetables, rice, and fish samples.

    Science.gov (United States)

    Behbahani, Mohammad; Bagheri, Akbar; Taghizadeh, Mohsen; Salarian, Mani; Sadeghi, Omid; Adlnasab, Laleh; Jalali, Kobra

    2013-06-01

    This paper describes the preparation of new Pb(II)-imprinted polymeric particles using 2-vinylpyridine as a functional monomer, ethylene glycol dimethacrylate as the cross-linker, 2,2'- azobisisobutyronitrile as the initiator, diphenylcarbazone as the ligand, acetonitril as the solvent, and Pb(NO(3))(2) as the template ion, through bulk polymerisation technique. The imprinted lead ions were removed from the polymeric matrix using 5 mL of HCl (2 mol.L(-1)) as the eluting solvent. The lead ion concentration was determined by flame atomic absorption spectrometry. Optimum pH for maximum sorption was obtained at 6.0. Sorption and desorption of Pb(II) ions on the IIP particles were quite fast and achieved fully over 5 min. In the proposed method, the maximum sorbent capacity of the ion-imprinted polymer was calculated to be 75.4 mg g(-1). The preconcentration factor, relative standard deviation, and limit of detection of the method were found to be 245, 2.1%, and 0.42 ng mL(-1), respectively. The prepared ion-imprinted polymer particles have an increased selectivity toward Pb(II) ions over a range of competing metal ions with the same charge and similar ionic radius. This ion-imprinted polymer is an efficient solid phase for extraction and preconcentration of lead ions in complex matrixes. For proving that the proposed method is reliable, a wide range of food samples with different and complex matrixes was used.

  8. Determination of the extraction efficiency for $^{233}$U source $\\alpha$-recoil ions from the MLL buffer-gas stopping cell

    CERN Document Server

    von der Wense, Lars; Laatiaoui, Mustapha; Thirolf, Peter G

    2016-01-01

    Following the $\\alpha$ decay of $^{233}$U, $^{229}$Th recoil ions are shown to be extracted in a significant amount from the MLL buffer-gas stopping cell. The produced recoil ions and subsequent daughter nuclei are mass purified with the help of a customized quadrupole mass spectrometer. The combined extraction and mass-purification efficiency for $^{229}$Th$^{3+}$ is determined via MCP-based measurements and via the direct detection of the $^{229}$Th $\\alpha$ decay. A large value of $(10\\pm2)$\\% for the combined extraction and mass-purification efficiency of $^{229}$Th$^{3+}$ is obtained at a mass resolution of about 1 u/e. In addition to $^{229}$Th, also other $\\alpha$-recoil ions of the $^{233,232}$U decay chains are addressed.

  9. Spectrophotometeric determination of trace amounts of Al3+ ion in water samples after cloud point extraction using quinizarin as a complexing agent.

    Science.gov (United States)

    Shokrollahi, Ardeshir; Aghaei, Roghayeh

    2014-02-01

    In this study, cloud point extraction was used for the preconcentration of Al(3+) ion after the complex formation with 1,4-dihydroxy-9,10-anthraquinone (Quinizarin [QUIN]), and subsequent analysis by spectrophotometeric method, using Triton X-114 as surfactant. The optimal extraction and reaction conditions were studied (i.e., pH = 5.5, 0.1 mM QUIN, Triton X-114 = 0.1% (w/v)), and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and enrichment factors) were obtained. Linearity was obeyed in the range of 3.33-166.67 ng ml(-1) of Al(3+) ion. The detection limit of the method was 2.09 ng ml(-1) for Al(3+) ion. The interference effect of some anions and cations was also tested. The method was applied to determine Al(3+) ion in water samples.

  10. Multiple testing issues in discriminating compound-related peaks and chromatograms from high frequency noise, spikes and solvent-based nois in LC-MS data sets

    NARCIS (Netherlands)

    Nyangoma, S.O.; Van Kampen, A.A.; Reijmers, T.H.; Govorukhina, N.I; van der Zee, A.G.; Billingham, I.J; Bischoff, Rainer; Jansen, R.C.

    2007-01-01

    Multiple testing issues in discriminating compound-related peaks and chromatograms from high frequency noise, spikes and solvent-based noise in LC-MS data sets.Nyangoma SO, van Kampen AA, Reijmers TH, Govorukhina NI, van der Zee AG, Billingham LJ, Bischoff R, Jansen RC. University of Birmingham. Liq

  11. Identification of fermentation inhibitors in wood hydrolyzates and removal of inhibitors by ion exchange and liquid-liquid extraction

    Science.gov (United States)

    Luo, Caidian

    1998-12-01

    Common methods employed in the ethanol production from biomass consist of chemical or enzymatic degradation of biomass into sugars and then fermentation of sugars into ethanol or other chemicals. However, some degradation products severely inhibit the fermentation processes and substantially reduce the efficiency of ethanol production. How to remove inhibitors from the reaction product mixture and increase the production efficiency are critical in the commercialization of any processes of energy from biomass. The present study has investigated anion exchange and liquid-liquid extraction as potential methods for inhibitor removal. An analytical method has been developed to identify the fermentation inhibitors in a hydrolyzate. The majority of inhibitors present in hybrid poplar hydrolyzate have positively been identified. Ion exchange with weak basic Dowex-MWA-1 resin has been proved to be an effective mean to remove fermentation inhibitors from hybrid poplar hydrolyzate and significantly increase the fermentation productivity. Extraction with n-butanol might be a preferred way to remove inhibitors from wood hydrolyzates and improve the fermentability of sugars in the hydrolyzates. n-Butanol also removes some glucose, mannose and xylose from the hydrolyzate. Inhibitor identification reveals that lignin and sugar degradation compounds including both aromatic and aliphatic aldehydes and carboxylic acids formed in hydrolysis, plus fatty acids and other components from wood extractives are major fermentation inhibitors in Sacchromyces cerevisiae fermentation. There are 35 components identified as fermentation inhibitors. Among them, 4-hydroxy benzoic acid, 3,4-dihydroxy benzoic acid, syringic acid, syringaldehyde, and ferulic acid are among the most abundant aromatic inhibitors in hybrid poplar hydrolyzate. The conversion of aldehyde groups into carboxylic acid groups in the nitric acid catalyzed hydrolysis reduces the toxicity of the hydrolyzate. A wide spectrum of

  12. Recording ion channels across soy-extracted lecithin bilayer generated by water-soluble quantum dots

    Science.gov (United States)

    Sarma, Runjun; Mohanta, Dambarudhar

    2014-02-01

    We report on the quantum dot (QD)-induced ion channels across a soya-derived lecithin bilayer supported on a laser drilled of ~100 μm aperture of cellulose acetate substrate that separates two electrolytic chambers. Adequate current bursts were observed when the bilayer was subjected to a gating voltage. The voltage-dependent current fluctuation, across the bilayer, was attributed to the insertion of ~20 nm sized water-soluble CdSe QDs, forming nanopores due to their spontaneous aggregation. Apart from a closed state, the first observable conductance levels were found as 6.3 and 11 nS, as for the respective biasing voltages of -10 and -20 mV. The highest observable conductance states, at corresponding voltages were ~14.3 and 21.1 nS. Considering two simplified models, we predict that the non-spherical pores (dnspore) can be a better approximation over spherical nanopores (dspore) for exhibiting a definite conductance level. At times, even dnspore ≤ 4dspore and that the non-spherical nanopores were associated with a smaller No. of QDs than the case for spherical nanopores, for a definite conductance state. It seems like the current events are partly stochastic, possibly due to thermal effects on the aggregated QDs that would form nanopores. The dwell time of the states was predicted in the range of 384-411 μs. The ion channel mechanism in natural phospholipid bilayers over artificial ones will provide a closer account to understand ion transport mechanism in live cells and signaling activity including labelling with fluorescent QDs.

  13. KINETICS OF YTTERBIUM ION EXTRACTION BY CA-12 AT THE LIQUID-LIQUID INTERFACE

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    IntroductionExtractants of the carboxylic acid type, althoughnot as widely used as their organophosphoruscounterparts, have found some application in thehydrometallursical processing of base metals. Forexample, they have been employed in the separationo f copper from nickel and cobalt, the removal ofimpurities from cobalt electrolytes, the sepndion ofyttrium and the rare-each metals, the co-eXtraction ofcobalt and nickel, and the recovery of gallium andindiumll].CA-12(see-octylphenoxy acetic acid) is a newe...

  14. Extraction of metals from metal ion-catechol-quaternary base systems.

    Science.gov (United States)

    Vrchlabský, M; Sommer, L

    1968-09-01

    Methods are given for the extraction of iron(III), molybdenum(VI), titanium(IV), niobium(V), vanadium(IV), uranium(VI) and tungsten(VI) as ternary complexes with catechol and a quaternary cation such as n-butyltriphenylphosphonium, n-propyltriphenylphosphonium, tetraphenylarsonium, cetylpyridinium, cetyltrimethylammonium and 2,3,5-triphenyltetrazolium, the solvent being chloroform. By use of masking agents and pH control, some of these elements can be separated from each other by this means.

  15. Characteristics of the negative ion beam extracted from an LBL multicusp volume source

    Energy Technology Data Exchange (ETDEWEB)

    Debiak, T.W.; Solensten, L.; Sredniawski, J.J.; Ng, Y.C.; Heuer, R. (Grumman Corporation, Bethpage, New York 11714 (US))

    1990-01-01

    This work encompasses a study of the beam position, profile, and emittance of a Lawrence Berkeley Lab (LBL) multicusp volume source. The study includes a comparison of different extraction geometries with single- and multiple-hole apertures. Our work is currently based on single-gap extraction and acceleration. These experiments are the first of a planned series of studies with various extractor geometries. The beam profile full width at half-maximum ranged from 5.7 to 10.2 mm at a position 69 mm from the emission aperture. Measurements of profile and position in the vertical direction indicate that the beam is significantly bent in the direction expected due to the field of the electron separation magnet. Phase space contour plots in the horizontal plane have been obtained for circular extraction apertures with a diameter of 1.0 and 2.0 mm, and a multiple-hole aperture with an overall diameter of 2.46 mm. Emittances were calculated to be as low as 0.0010 {pi} cm mrad for the 1-mm aperture and 0.0014 {pi} cm mrad for the 2-mm aperture. Emittances are not reported for the multiple-hole aperture due to the shape of the phase space contours; however, analysis of the data is in progress to provide a meaningful comparison of the single-hole and multiple-hole beam characteristics.

  16. The influence of extraction procedure on ion concentrations in sediment pore water

    Science.gov (United States)

    Winger, P.V.; Lasier, P.J.; Jackson, B.P.

    1998-01-01

    Sediment pore water has the potential to yield important information on sediment quality, but the influence of isolation procedures on the chemistry and toxicity are not completely known and consensus on methods used for the isolation from sediment has not been reached. To provide additional insight into the influence of collection procedures on pore water chemistry, anion (filtered only) and cation concentrations were measured in filtered and unfiltered pore water isolated from four sediments using three different procedures: dialysis, centrifugation and vacuum. Peepers were constructed using 24-cell culture plates and cellulose membranes, and vacuum extractors consisted of fused-glass air stones attached with airline tubing to 60cc syringes. Centrifugation was accomplished at two speeds (2,500 and 10,000 x g) for 30 min in a refrigerated centrifuge maintained at 4?C. Only minor differences in chemical characteristics and cation and anion concentrations were found among the different collecting methods with differences being sediment specific. Filtering of the pore water did not appreciably reduce major cation concentrations, but trace metals (Cu and Pb) were markedly reduced. Although the extraction methods evaluated produced pore waters of similar chemistries, the vacuum extractor provided the following advantages over the other methods: (1) ease of extraction, (2) volumes of pore water isolated, (3) minimal preparation time and (4) least time required for extraction of pore water from multiple samples at one time.

  17. The relationship between visible light emission and species fraction of the hydrogen ion beams extracted from 2.45 GHz microwave discharge

    CERN Document Server

    Cortázar, O D; Tarvainen, O; Kalvas, T; Koivisto, H

    2015-01-01

    The relationship between Balmer-α and Fulcher-band emissions with extracted H +, H+2 , and H+3 ions is demonstrated for a 2.45 GHz microwave discharge. Ion mass spectra and optical measurements of Balmer-α and Fulcher-band emissions have been obtained with a Wien Filter having an optical view-port on the plasma chamber axis. The beam of approximately 1 mA is analyzed for different plasma conditions simultaneously with the measurement of light emissions both with temporal resolution. The use of visible light emissions as a valuable diagnostic tool for monitoring the species fraction of the extracted beams is proposed.

  18. Study of electron current extraction from a radio frequency plasma cathode designed as a neutralizer for ion source applications

    Energy Technology Data Exchange (ETDEWEB)

    Jahanbakhsh, Sina, E-mail: sinajahanbakhsh@gmail.com; Satir, Mert; Celik, Murat [Department of Mechanical Engineering, Bogazici University, Istanbul 34342 (Turkey)

    2016-02-15

    Plasma cathodes are insert free devices that are developed to be employed as electron sources in electric propulsion and ion source applications as practical alternatives to more commonly used hollow cathodes. Inductively coupled plasma cathodes, or Radio Frequency (RF) plasma cathodes, are introduced in recent years. Because of its compact geometry, and simple and efficient plasma generation, RF plasma source is considered to be suitable for plasma cathode applications. In this study, numerous RF plasma cathodes have been designed and manufactured. Experimental measurements have been conducted to study the effects of geometric and operational parameters. Experimental results of this study show that the plasma generation and electron extraction characteristics of the RF plasma cathode device strongly depend on the geometric parameters such as chamber diameter, chamber length, orifice diameter, orifice length, as well as the operational parameters such as RF power and gas mass flow rate.

  19. Fluorous ionic liquids as solvents for the liquid-liquid extraction of metal ions by macrocyclic polyethers.

    Science.gov (United States)

    Heitzman, Holly; Young, Blake A; Rausch, David J; Rickert, Paul; Stepinski, Dominique C; Dietz, Mark L

    2006-04-15

    The predominant mode of strontium ion transfer from aqueous nitrate media into a series of 1-fluoroalkyl-3-methylimidazolium bis[(trifluoromethylsulfonyl)]imides containing dicyclohexano-18-crown-6 (DCH18C6) is shown to shift from cation exchange to strontium nitrato-crown ether complex partitioning as the length of the fluoroalkyl substituent is increased. Fluoroalkyl substituents are shown to be only slightly more effective than their non-fluorous analogs at inducing this shift. At the same time, the fluorinated ionic liquids (ILs) yield strontium distribution ratios as much as an order of magnitude lower than the corresponding 1-alkyl-3-methylimidazolium (C(n)mim(+)) salts. Fluorous ILs thus appear to offer no compelling advantages over C(n)mim(+) ionic liquids as extraction solvents.

  20. Graphene-Based Materials as Solid Phase Extraction Sorbent for Trace Metal Ions, Organic Compounds, and Biological Sample Preparation.

    Science.gov (United States)

    Ibrahim, Wan Aini Wan; Nodeh, Hamid Rashidi; Sanagi, Mohd Marsin

    2016-07-03

    Graphene is a new carbon-based material that is of interest in separation science. Graphene has extraordinary properties including nano size, high surface area, thermal and chemical stability, and excellent adsorption affinity to pollutants. Its adsorption mechanisms are through non-covalent interactions (π-π stacking, electrostatic interactions, and H-bonding) for organic compounds and covalent interactions for metal ions. These properties have led to graphene-based material becoming a desirable adsorbent in a popular sample preparation technique known as solid phase extraction (SPE). Numerous studies have been published on graphene applications in recent years, but few review papers have focused on its applications in analytical chemistry. This article focuses on recent preconcentration of trace elements, organic compounds, and biological species using SPE-based graphene, graphene oxide, and their modified forms. Solid phase microextraction and micro SPE (µSPE) methods based on graphene are discussed.

  1. Surface modified magnetic Fe{sub 3}O{sub 4} nanoparticles as a selective sorbent for solid phase extraction of uranyl ions from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Sadeghi, Susan, E-mail: ssadeghi@birjand.ac.ir [Department of Chemistry, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of); Azhdari, Hoda [Department of Chemistry, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of); Arabi, Hadi [Magnetism and Superconducting Research Lab, Department of Physics, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of); Moghaddam, Ali Zeraatkar [Department of Chemistry, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer A new sorbent based on functionalized magnetite nanoparticles with quercetin is reported. Black-Right-Pointing-Pointer The quercetin based magnetic nanoparticles could be used as a sorbent to remove toxic uranyl ions from water samples. Black-Right-Pointing-Pointer The sorbent provides a rapidly and easy separation of uranyl ions only by using a permanent magnet. Black-Right-Pointing-Pointer This technique is considered more efficient separation compared to conventional filtering or centrifuging methods for the removing of the sorbent. - Abstract: In this study, silica-coated magnetic nanoparticles modified with quercetin were synthesized by a sol-gel method. These magnetic nanoparticles were assessed as a new solid phase sorbent for extraction of uranyl ions from aqueous solutions. The crystal and chemical structures and magnetic property of the new sorbent were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectrophotometer (FT-IR), and vibration sample magnetometer (VSM). The experimental parameters affecting the extraction efficiency of uranyl ions from aqueous solutions using the synthesized sorbent were optimized by means of the response surface methodology. The adsorption equilibrium of uranyl ions onto the sorbent was explained by Langmuir isotherm and maximum monolayer adsorption capacity was found 12.33 mg/g. The synthesized sorbent was applied to extraction of uranyl ions from different water samples.

  2. 低压离子色谱法分析茶水中的无机离子%ANALYSIS OF INORGANIC IONS IN TEA EXTRACTS BY LOW-PRESSURE ION CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    张新申; 廖峰; 罗世元

    2001-01-01

    The low-pressure ion chromatography has been developed for the determination of the concentration of Na+、NH+4、K+、Ca2+、Mg2+、Cl-、SO2-4 and PO3-4 in the extracts of flower tea、red tea and green tea.Calibrations were linear (r2>0.996) for eight ions,with RSDs of less than 2%.The recovery of the method was between 95~106% for these ions and the lowest detection limit was less than 1.0×10-6g/ml,Results indicate that the developed low-pressure ion chromatography assay is fine and accurate for determination of the inorganic ions in the tea eluent.

  3. Extraction and Analysis of Disperse Dyes from Colored Polyester Single Fibers Using Liquid Chromatography/Linear Ion Trap Tandem Mass Spectrometry.

    Science.gov (United States)

    Kato, Takao; Suzuki, Yasuhiro; Handa, Makoto

    2016-01-01

    Nine disperse dyes extracted from colored polyester threads and single fibers of manufactory-supplied textiles by using centrifugal filtration were analyzed using liquid chromatography/linear ion trap tandem mass spectrometry (LC/LIT-MS(n)). Based on diode array detector data, dimethylformamide (DMF) was found to be a more effective extraction solvent than acetonitrile/water (4:3, v/v) or methanol/water (1:1, v/v) mixtures. The precursor, [M+H](+) ions, were detected for the dyes extracted using DMF. The MS(2) and MS(3) spectra also matched those of the standard disperse dyes. Without relying on comparison clothes, disperse dyes extracted from the single fibers (5 mm in length) were successfully identified by LC/LIT-MS(n) and the custom-built database.

  4. Design, manufacture and factory testing of the Ion Source and Extraction Power Supplies for the SPIDER experiment

    Energy Technology Data Exchange (ETDEWEB)

    Bigi, Marco, E-mail: marco.bigi@igi.cnr.it [Consorzio RFX (CNR, ENEA, INFN, Università di Padova, Acciaierie Venete SpA), Corso Stati Uniti 4, 35127 Padova (Italy); Rinaldi, Luigi [OCEM Energy Technology, Via della Solidarietà 2/1, 40056 Valsamoggia (località Crespellano), Bologna (Italy); Simon, Muriel [Fusion for Energy, Josep Pla 2, 08019 Barcelona (Spain); Sita, Luca; Taddia, Giuseppe; Carrozza, Saverino [OCEM Energy Technology, Via della Solidarietà 2/1, 40056 Valsamoggia (località Crespellano), Bologna (Italy); Decamps, Hans [ITER Organization, Route de Vinon sur Verdon, 13115 Saint Paul lez Durance (France); Luchetta, Adriano [Consorzio RFX (CNR, ENEA, INFN, Università di Padova, Acciaierie Venete SpA), Corso Stati Uniti 4, 35127 Padova (Italy); Meddour, Abdelraouf [HIMMELWERK Hoch- und Mittelfrequenzanlagen GmbH, Jopestr. 10, 72072 Tübingen (Germany); Moressa, Modesto [Consorzio RFX (CNR, ENEA, INFN, Università di Padova, Acciaierie Venete SpA), Corso Stati Uniti 4, 35127 Padova (Italy); Morri, Cristiano; Musile Tanzi, Antonio [OCEM Energy Technology, Via della Solidarietà 2/1, 40056 Valsamoggia (località Crespellano), Bologna (Italy); Recchia, Mauro [Consorzio RFX (CNR, ENEA, INFN, Università di Padova, Acciaierie Venete SpA), Corso Stati Uniti 4, 35127 Padova (Italy); Wagner, Uwe [HIMMELWERK Hoch- und Mittelfrequenzanlagen GmbH, Jopestr. 10, 72072 Tübingen (Germany); Zamengo, Andrea; Toigo, Vanni [Consorzio RFX (CNR, ENEA, INFN, Università di Padova, Acciaierie Venete SpA), Corso Stati Uniti 4, 35127 Padova (Italy)

    2015-10-15

    Highlights: • 5 MVA ion source power supplies effectively integrated in 150 m{sup 2} Faraday cage. • Load protection and performance requirements met of custom design high voltage power supplies. • 200 kW tetrode oscillator with 200 kHz frequency range successfully tested. - Abstract: The SPIDER experiment, currently under construction at the Neutral Beam Test Facility in Padua, Italy, is a full-size prototype of the ion source for the ITER Neutral Beam Injectors. The Ion Source and Extraction Power Supplies (ISEPS) for SPIDER are supplied by OCEM Energy Technology s.r.l. (OCEM) under a procurement contract with Fusion for Energy (F4E) covering also the units required for MITICA and ITER injectors. The detailed design of SPIDER ISEPS was finalized in 2011 and manufacture of most components completed by end 2013. The Factory Acceptance Tests took place early 2014. ISEPS, with an overall power rating of 5 MVA, form a heterogeneous set of items including solid state power converters and 1 MHz radiofrequency generators of 200 kW output power. The paper presents the main features of the detailed design developed by OCEM, focusing in particular on the high output voltage pulse step modulators, the high output current resonant converters, the radiofrequency generators by HIMMELWERK GmbH and the architecture and implementation of the complex control system. Details are given on non-standard factory tests verifying the insulation requirements specific to this application. Performance of ISEPS during the factory acceptance tests is described, with emphasis on demonstration of the load protection requirements, a crucial point for all neutral beam power supplies. Finally, key dates of SPIDER ISEPS installation and site testing schedule are provided.

  5. Adsorption of saponin compound in Carica papaya leaves extract using weakly basic ion exchanger resin

    Science.gov (United States)

    Abidin, Noraziani Zainal; Janam, Anathasia; Zubairi, Saiful Irwan

    2016-11-01

    Adsorption of saponin compound in papaya leaves juice extract using Amberlite® IRA-67 resin was not reported in previous studies. In this research, Amberlite® IRA-67 was used to determine the amount of saponin that can be adsorbed using different weights of dry resin (0.1 g and 0.5 g). Peleg model was used to determine the maximum yield of saponin (43.67 mg) and the exhaustive time (5.7 days) prior to a preliminary resin-saponin adsorption study. After adsorption process, there was no significant difference (p>0.05) in total saponin content (mg) for sample treated with 0.1 g (3.79 ± 0.55 mg) and sample treated with 0.5 g (3.43 ± 0.51 mg) dry weight resin. Long-term kinetic adsorption of resin-saponin method (>24 hours) should be conducted to obtain optimum freed saponin extract. Besides that, sample treated with 0.1 g dry weight resin had high free radical scavenging value of 50.33 ± 2.74% compared to sample treated with 0.5 g dry weight resin that had low free radical scavenging value of 24.54 ± 1.66% dry weights. Total saponin content (mg), total phenolic content (mg GAE) and free radical scavenging activity (%) was investigated to determine the interaction of those compounds with Amberlite® IRA-67. The RP-HPLC analysis using ursolic acid as standard at 203 nm showed no peak even though ursolic acid was one of the saponin components that was ubiquitous in plant kingdom. The absence of peak was due to weak solubility of ursolic acid in water and since it was only soluble in solvent with moderate polarity. The Pearson's correlation coefficient for total saponin content (mg) versus total phenolic content (mg GAE) and radical scavenging activity (%) were +0.959 and +0.807. Positive values showed that whenever there was an increase in saponin content (mg), the phenolic content (mg GAE) and radical scavenging activity (%) would also increase. However, as the resin-saponin adsorption was carried out, there was a significant decrease of radical scavenging activity

  6. Use of semi-permeable membrane devices and solid-phase extraction for the wide-range screening of microcontaminants in surface water by GC-AED/MS.

    Science.gov (United States)

    van Stee, Leo L P; Leonards, Pim E G; van Loon, Willem M G M; Hendriks, A Jan; Maas, Johanna L; Struijs, Jaap; Brinkman, Udo A Th

    2002-11-01

    An automated GC-MS-based screening method was developed for over 400 industrial, agrochemical and household chemicals. Extracted ion chromatograms were used and the method was aimed at creating a minimum number of false positives. The compound polarity range usually associated with solid-phase extraction was extended to include very apolar, bioaccumulative, compounds by using the complementary semi-permeable membrane device technique. Real-life samples were taken at four locations in the main Dutch river systems and one in an agricultural area. Some 150 compounds were detected in the low-ng/l to low-microg/l range. Next to the target compounds, several brominated and chlorinated non-target compounds were detected by means of GC with atomic emission detection and tentatively identified using mass spectral library searching.

  7. Extraction and Characterization of Phenolic Compounds from Rose Hip (Rosa canina L. Using Liquid Chromatography Coupled with Electrospray Ionization - Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Andreea STĂNILĂ

    2015-12-01

    Full Text Available Wild berry are a rich of natural compounds which provide them high antioxidant potential. The compounds which provide them these proprieties are known to be vitamins, flavonoids, anthocyanins and phenolic acids. The aim of this study was to extract and characterize bioactive compounds from rose hip (Rosa canina L. currently found in Romania. A qualitative high-performance liquid chromatography coupled with electrospray ionization mass spectrometric (ESI-MS detection in positive ion mode has been used to identify phenolic compounds from rose hip crude extract. The chromatograms revealed the presence of a large number of compounds (19, identified and grouped as phenolic acids and flavones/ols, flavan-3-ols and also anthocyanins. Based on obtained results these berries can be highly recommended as part of our diet. Also this finding represents a contribution to the chemical characterization of phenolic profile of rose hip.

  8. Metal ion determination by flame atomic absorption spectrometry through reagentless coacervate phase separation-extraction into lamellar vesicles.

    Science.gov (United States)

    Giokas, Dimosthenis L; Tsogas, George Z; Vlessidis, Athanasios G; Karayannis, Miltiades I

    2004-03-01

    The phase separation of lamellar vesicles of anionic surfactants in aqueous solutions and its application as a novel liquid coacervate extraction procedure was examined. Solutions of lauric acid sodium salt separate into two phases in the presence of alkaline earth metals and a water miscible cosurfactant. It is proven that the surfactant phase is built of a perplexed network of multilamellar vesicles consisting of densely packed bilayers. Several factors affecting the formation of this new phase as well as its analytical utility in the preconcentration of metallic ions were assessed on the basis of better exploitation of this new nonspecific extraction technique. In essence, although the procedure to arrive at the optimum conditions seems laborious, the delivered method is straightforward, alleviating the requirement for prereaction with a complexing agent and highly reproducible under the optimum experimental conditions. As an analytical demonstration, the method was successfully applied to the determination of Cd(2+) and Zn(2+) in natural waters. Recoveries were higher than 95%, and detection limits as low as 3 microg L(-)(1) were accomplished by preconcentrating only 10 mL of sample volume in the presence of 0.45% (w/v) anionic surfactant.

  9. Source fabrication and lifetime for Li+ ion beams extracted from alumino-silicate sources

    Energy Technology Data Exchange (ETDEWEB)

    Roy, Prabir K.; Greenway, Wayne G.; Kwan, Joe W.

    2012-04-01

    A space-charge-limited beam with current densities (J) exceeding 1 mA/cm2 have been measured from lithium alumino-silicate ion sources at a temperature of ~1275 °C. At higher extraction voltages, the source appears to become emission limited with J ≥ 1.5 mA/cm2, and J increases weakly with the applied voltage. A 6.35 mm diameter source with an alumino-silicate coating, ≤0.25 mm thick, has a measured lifetime of ~40 h at ~1275 °C, when pulsed at 0.05 Hz and with pulse length of ~6 μs each. At this rate, the source lifetime was independent of the actual beam charge extracted due to the loss of neutral atoms at high temperature. Finally, the source lifetime increases with the amount of alumino-silicate coated on the emitting surface, and may also be further extended if the temperature is reduced between pulses.

  10. Source fabrication and lifetime for Li+ ion beams extracted from alumino-silicate sources

    Energy Technology Data Exchange (ETDEWEB)

    Roy, Prabir K.; Greenway, Wayne G.; Kwan, Joe W

    2012-03-05

    A space-charge-limited beam with current densities (J) exceeding 1 mA/cm2 have been measured from lithium alumino-silicate ion sources at a temperature of ~1275 °C. At higher extraction voltages, the source appears to become emission limited with J ≥ 1.5 mA/cm2, and J increases weakly with the applied voltage. A 6.35 mm diameter source with an alumino-silicate coating, ≤0.25 mm thick, has a measured lifetime of ~40 h at ~1275 °C, when pulsed at 0.05 Hz and with pulse length of ~6 μs each. At this rate, the source lifetime was independent of the actual beam charge extracted due to the loss of neutral atoms at high temperature. Finally, the source lifetime increases with the amount of alumino-silicate coated on the emitting surface, and may also be further extended if the temperature is reduced between pulses.

  11. A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.

    Science.gov (United States)

    Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

    2013-11-15

    A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 μg/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Determination of penicillin G in milk samples using its effect on cloud point extraction of triiodide ion.

    Science.gov (United States)

    Pourreza, Nahid; Fat'hi, Mohammad Reza; Hatami, Ali

    2014-01-01

    A cloud point extraction (CPE) method for determination of trace amounts of penicillin G by spectrophotometry based on its effect on the triiodide ion (I3(-)) has been developed. Penicillin G is converted to the corresponding penicilloic acid by carrying out hydrolysis with sodium hydroxide solution, and treatment with acid yields D-penicillamine that is oxidized quantitatively by iodine to give rise to a disulfide. The 13- remaining in the solution is extracted into the surfactant Triton X-100, and the difference between absorbance of the working solution in the presence and absence of penicillin G is proportional to the amount of penicillin G. The effects of different variables, such as concentrations of sodium hydroxide, hydrochloric acid, surfactant, and I3(-) and the temperature and incubation time on the CPE were studied. The calibration graph was linear in the range of 50-1250 microg/L, and the LOD was 38 microg/L (n = 10). The RSD for 10 replicate determinations of 1000 microg/L of penicillin G was 1.0%. The method was applied to the determination of penicillin G in milk samples.

  13. Appropriate choice of collision-induced dissociation energy for qualitative analysis of notoginsenosides based on liquid chromatography hybrid ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Guang-Ji; Fu, Han-Xu; Xiao, Jing-Cheng; Ye, Wei; Rao, Tai; Shao, Yu-Hao; Kang, Dian; Xie, Lin; Liang, Yan

    2016-04-01

    Liquid chromatography hybrid ion trap/time-of-flight mass spectrometry possessesd both the MS(n) ability of ion trap and the excellent resolution of a time-of-flight, and has been widely used to identify drug metabolites and determine trace multi-components for in natural products. Collision energy, one of the most important factors in acquiring MS(n) information, could be set freely in the range of 10%-400%. Herein, notoginsenosides were chosen as model compounds to build a novel methodology for the collision energy optimization. Firstly, the fragmental patterns of the representatives for the authentic standards of protopanaxadiol-type and protopanaxatriol-type notoginsenosides authentic standards were obtained based on accurate MS(2) and MS(3) measurements via liquid chromatography hybrid ion trap/time-of-flight mass spectrometry. Then the extracted ion chromatograms of characteristic product ions of notoginsenosides in Panax Notoginseng Extract, which were produced under a series of collision energies and, were compared to screen out the optimum collision energies values for MS(2) and MS(3). The results demonstrated that the qualitative capability of liquid chromatography hybrid ion trap/time-of-flight mass spectrometry was greatly influenced by collision energies, and 50% of MS(2) collision energy was found to produce the highest collision-induced dissociation efficiency for notoginsenosides. BesidesAddtionally, the highest collision-induced dissociation efficiency appeared when the collision energy was set at 75% in the MS(3) stage.

  14. Robust alignment of chromatograms by statistically analyzing the shifts matrix generated by moving window fast Fourier transform cross-correlation.

    Science.gov (United States)

    Zhang, Mingjing; Wen, Ming; Zhang, Zhi-Min; Lu, Hongmei; Liang, Yizeng; Zhan, Dejian

    2015-03-01

    Retention time shift is one of the most challenging problems during the preprocessing of massive chromatographic datasets. Here, an improved version of the moving window fast Fourier transform cross-correlation algorithm is presented to perform nonlinear and robust alignment of chromatograms by analyzing the shifts matrix generated by moving window procedure. The shifts matrix in retention time can be estimated by fast Fourier transform cross-correlation with a moving window procedure. The refined shift of each scan point can be obtained by calculating the mode of corresponding column of the shifts matrix. This version is simple, but more effective and robust than the previously published moving window fast Fourier transform cross-correlation method. It can handle nonlinear retention time shift robustly if proper window size has been selected. The window size is the only one parameter needed to adjust and optimize. The properties of the proposed method are investigated by comparison with the previous moving window fast Fourier transform cross-correlation and recursive alignment by fast Fourier transform using chromatographic datasets. The pattern recognition results of a gas chromatography mass spectrometry dataset of metabolic syndrome can be improved significantly after preprocessing by this method. Furthermore, the proposed method is available as an open source package at https://github.com/zmzhang/MWFFT2.

  15. Cupric ion reducing antioxidant capacity assay for food antioxidants: vitamins, polyphenolics, and flavonoids in food extracts.

    Science.gov (United States)

    Apak, Reşat; Güçlü, Kubilay; Ozyürek, Mustafa; Bektas Oğlu, Burcu; Bener, Mustafa

    2008-01-01

    Antioxidants are health beneficial compounds through their combat with reactive oxygen and nitrogen species and free radicals that may cause tissue damage leading to various diseases. This work reports the development of a simple and widely applicable antioxidant capacity index for dietary polyphenols, vitamins C and E, and plasma antioxidants utilizing the copper(II)-neocuproine (Cu(II)-Nc) reagent as the chromogenic oxidizing agent. This novel method based on an electron-transfer mechanism was named by our research group as 'cupric reducing antioxidant capacity', abbreviated as the CUPRAC method. The method is comprised of mixing the antioxidant solution with aqueous copper(II) chloride, alcoholic neocuproine, and ammonium acetate aqueous buffer at pH 7, and subsequently measuring the developed absorbance at 450 nm after 30 min. Since the color development is fast for compounds like ascorbic acid, gallic acid, and quercetin but slow for naringin and naringenin, the latter compounds are assayed after incubation at 50 degrees C on a water bath for 20 min. The flavonoid glycosides are hydrolyzed to their corresponding aglycones by refluxing in 1.2 M: HCl-containing 50% MeOH so as to exert maximal reducing power towards Cu(II)-Nc. The CUPRAC antioxidant capacities of synthetic mixtures are equal to the sum of individual capacities of antioxidant constituents, indicating lack of chemical deviations from Beer's law. Tests on antioxidant polyphenols demonstrate that the highest CUPRAC capacities are observed for epicatechin gallate, epigallocatechin gallate, quercetin, fisetin, epigallocatechin, catechin, and caffeic acid in this order, in accord with the number and position of the -OH groups as well the conjugation level of the molecule. The parallelism of the linear calibration curves of pure antioxidants in water and in a given complex matrix (plant extract) demonstrates that there are no chemical interactions of interferent nature among the solution constituents

  16. EFFECT OF DE-tert-BUTYLATION AND FUNCTIONALIZATION WITH AMINE GROUPS AT THE UPPER RIM OF p-tert-BUTYLCALIX[4]ARENE TO THE EXTRACTABILITY FOR Cr3+, Cd2+ and Pb2+ IONS

    Directory of Open Access Journals (Sweden)

    Firdaus Firdaus

    2010-06-01

    Full Text Available The effects to the extractability forwards Cr3+, Cd2+, and Pb2+ ions of de-tert-butylation and functionalization with amine groups at the upper rim of p-tert-butylcalix[4]arene had been studied by applied the p-tert-butylcalix[4]arene (1, tetrahydroxycalix[4]arene (2, and p-(aminobutoxycalixarene (3 compounds as extractants for the heavy metals ions. The extraction involved optimise of three parameters, i.e. pH, time, and concentration of extractants. The extraction degrees of the heavy metals ions at optimum conditions were compared each other to decide the effects. Compound 1 showed high extractability to Cr3+ and Pb2+ ions over Cd2+ ion, but compound 2 as the debutylated product of compound 1 showed low extractability to the all of the heavy metals ions. Compound 3 as product of etherification with butyl groups of the lower rim followed functionalization with amine groups of the upper rim of compound 1 showed high extractability to Pb2+, but low to Cr3+ and Cd2+. Pursuant to the facts it was concluded that debutylation of compound 1 to compound 2 causing decrease drastically of extractability to the heavy metals ions; functionalization of the upper with amine groups as ionophore (compound 3 causing increase of the extractability to Pb2+ ion and decrease of the extractability to Cr3+ with increasing of separation factor value β(Pb2+/Cr3+ from 1.74 by compound 1 to 48.00 by compound 3. By slope analysis, the extracted species and mechanisms of the extractions have been confirmed.   Keywords: p-tert-butylcalix[4]arene, debutylation, p-(aminobutoxycalix[4]arene, extractability, heavy metals, extraction mechanisms.

  17. Simultaneous detection of trace metal ions in water by solid phase extraction spectroscopy combined with multivariate calibration.

    Science.gov (United States)

    Wang, Lei; Cao, Peng; Li, Wei; Tong, Peijin; Zhang, Xiaofang; Du, Yiping

    2016-04-15

    Solid Phase Extraction Spectroscopy (SPES) developed in this paper is a technique to measure spectrum directly on the solid phase material where the analytes are concentrated in SPE process. Membrane enrichment and UV-Visible spectroscopy were utilized to fulfill SPES, and multivariate calibration method of partial least squares (PLS) was used to simultaneously detect the concentrations of trace cobalt (II) and zinc (II) in water samples. The proposed method is simple, sensitive and selective. The complexes of analyte ions were collected on the cellulose acetate membranes via membrane filtration after the complexation reaction with 1-2-pyridylazo 2-naphthol (PAN). The spectra of the membranes which contained the complexes of metal ions and PAN were measured directly without eluting. The analytical conditions including pH, reaction time, sample volume, the amount of PAN, and flow rates were optimized. Nonionic surfactant Brij-30 was absorbed on the membranes prior to SPES to modify the membranes for improving the enrichment and spectrum measurement. The interference from other ions to the determination was investigated. Under the optimal condition, the absorbance was linearly related to the concentration at the range of 0.1-3.0 μg/L and 0.1-2.0 μg/L, with the correlation coefficients (R(2)) of 0.9977 and 0.9951 for Co (II) and Zn (II), respectively. The limits of detection were 0.066 μg/L for cobalt (II) and 0.104 μg/L for zinc (II). PLS regression with leave-one-out cross-validation was utilized to build models to detect cobalt (II) and zinc (II) in drinking water samples simultaneously. The correlation coefficient between ion concentration and spectrum of calibration set and independent prediction set were 1.0000 and 0.9974 for cobalt (II) and 1.0000 and 0.9956 for zinc (II). For cobalt (II) and zinc (II), the errors of the prediction set were in the range 0.0406-0.1353 μg/L and 0.0025-0.1884 μg/L. Copyright © 2016. Published by Elsevier B.V.

  18. Extraction of Li and Co from Li-ion Batteries by Chemical Methods

    Science.gov (United States)

    Guzolu, Jafar Sharrivar; Gharabaghi, Mahdi; Mobin, Mohammad; Alilo, Hojat

    2016-05-01

    In this work a process involving ultrasonic washing and leaching and precipitation was used to recover Li and Co from spent Li-ion batteries. Ultrasonic washing was used to reduce energy consumption and pollution whereas hydrochloric acid was used as leaching reagent. 98 % of Li and nearly 99 % of Co were obtained under optimum condition of 5 M hydrochloric acid solution, temperature of 95 °C, reaction time of 70 min, and solid-liquid ratio of 10 g/L. In this process at first nickel, copper, iron, aluminum, cobalt, and manganese were precipitated from leaching solution using sodium hydroxide at pH f 12.5 and reaction time of 1 h and temperature was 55 °C and all metal recoveries were more than 99 %. In the precipitation experiments, lithium loss was only 18.34 %. In the next stage, white lithium carbonate was precipitated by addition of saturated sodium carbonate solution to the left filtrate from first precipitation step. The purity of the recovered powder of lithium was 95 %.

  19. Modified Bentonite with Dithizone as Nano Clay Mineral Adsorbent for Solid Phase Extraction of Silver Ions

    Directory of Open Access Journals (Sweden)

    Farid Shakerian

    2016-09-01

    Full Text Available In this work, a simple flow injection system incorporating a microcolumn of immobilized dithizone on bentonite coated with cetyltrimethylammonium bromide was combined with flame atomic absorption spectrometry (FAAS for on-line separation/preconcentration and determination of trace amounts of silver in water. Dithizone was physically immobilized on the surfactant coated bentonite particles and was used as the adsorbent in the preparation of microcolumn. Silver ions were deposited by processing a standard or sample solution of analyte in the pH range of 3–9 through the microcolumn. Injection of 250 µL of thiourea (0.4 mol L−1, pH = 5.0 served to elute the retained species to the FAAS. The capacity of the adsorbent under working conditions was found to be 7.2 mg of silver per gram of adsorbent. Processing a water sample volume of 30 mL resulted in an enrichment factor of 116. The method was successfully applied to the determination of silver in different natural waters and a certified reference material. This work is licensed under a Creative Commons Attribution 4.0 International License.

  20. Extraction of Li and Co from Li-ion Batteries by Chemical Methods

    Science.gov (United States)

    Guzolu, Jafar Sharrivar; Gharabaghi, Mahdi; Mobin, Mohammad; Alilo, Hojat

    2017-04-01

    In this work a process involving ultrasonic washing and leaching and precipitation was used to recover Li and Co from spent Li-ion batteries. Ultrasonic washing was used to reduce energy consumption and pollution whereas hydrochloric acid was used as leaching reagent. 98 % of Li and nearly 99 % of Co were obtained under optimum condition of 5 M hydrochloric acid solution, temperature of 95 °C, reaction time of 70 min, and solid-liquid ratio of 10 g/L. In this process at first nickel, copper, iron, aluminum, cobalt, and manganese were precipitated from leaching solution using sodium hydroxide at pH f 12.5 and reaction time of 1 h and temperature was 55 °C and all metal recoveries were more than 99 %. In the precipitation experiments, lithium loss was only 18.34 %. In the next stage, white lithium carbonate was precipitated by addition of saturated sodium carbonate solution to the left filtrate from first precipitation step. The purity of the recovered powder of lithium was 95 %.

  1. Technical note: removal of metal ion inhibition encountered during DNA extraction and amplification of copper-preserved archaeological bone using size exclusion chromatography.

    Science.gov (United States)

    Matheson, Carney D; Marion, Travis E; Hayter, Shana; Esau, Neal; Fratpietro, Renee; Vernon, Kim K

    2009-10-01

    A novel technique for the removal of metal ions inhibiting DNA extraction and PCR of archaeological bone extracts is presented using size exclusion chromatography. Two case studies, involving copper inhibition, demonstrate the effective removal of metal ion inhibition. Light microscopy, SEM, elemental analysis, and genetic analysis were used to demonstrate the effective removal of metal ions from samples that previously exhibited molecular inhibition. This research identifies that copper can cause inhibition of DNA polymerase during DNA amplification. The use of size exclusion chromatography as an additional purification step before DNA amplification from degraded bone samples successfully removes metal ions and other inhibitors, for the analysis of archaeological bone. The biochemistry of inhibition is explored through chemical and enzymatic extraction methodology on archaeological material. We demonstrate a simple purification technique that provides a high yield of purified DNA (>95%) that can be used to address most types of inhibition commonly associated with the analysis of degraded archaeological and forensic samples. We present a new opportunity for the molecular analysis of archaeological samples preserved in the presence of metal ions, such as copper, which have previously yielded no DNA results.

  2. Ion Chromatography as an Alternative to Standard Methods for Analysis of Macro-nutrients in Mehlich 1 Extracts of Unfertilized Forest Soils

    Science.gov (United States)

    Joseph B. Fischer; James H. Miller

    2004-01-01

    This study evaluates ion chromatography (IC) as an alternative to atomic absorption (AA) and inductively-coupled plasma spectromctry (ICP) for analysis of potassium (K), magnesium (Mg), and calcium (Ca), and and as an alternative to antimonylmolybdate colorimetry and ICP for analysis of phosphorus (P) macro-nutrients in Mehlich 1 extracts. Soils typical of pine forests...

  3. Characterization and Utilization of Tannin Extract for the Selective Adsorption of Ni (II Ions from Water

    Directory of Open Access Journals (Sweden)

    Priya Meethale Kunnambath

    2015-01-01

    Full Text Available The current paper studies the preparation of a new tannin gel from Acacia nilotica for water purification and waste water remediation. Design of experiments is used for optimizing the tannin gel using tannin extract (Taguchi method with formaldehyde in the assistance of microwave (TGAN by the help of iodine number. The feasible combinations were tested in the removal of nickel from simulated and river water. In this study, the effect of adsorbent dosage, pH, and initial metal concentration on Ni (II biosorption on modified Acacia nilotica tannin gel (TGAN was investigated. Tannin gel was characterized by SEM, FTIR, XRD, and EDAX. The kinetic data was tested using pseudo-first-order, pseudo-second-order, and intraparticle diffusion model. The results suggested that the pseudo-second-order model (R2 > 0.998 was the best choice among all the kinetic models describing the adsorption behavior of Ni (II onto TGAN. Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich adsorption models were used to represent the equilibrium data. The best interpretation for the experimental data was given by the Langmuir isotherm and the maximum adsorption capacity 250 mg g−1 of Ni (II was obtained at pH 5.04 at 296 K. Adsorption of Ni (II onto TGAN is confirmed qualitatively by the use of atomic absorption spectroscopy. The BOD and COD values are considerably reduced after adsorption.

  4. Unique ion filter: a data reduction tool for GC/MS data preprocessing prior to chemometric analysis.

    Science.gov (United States)

    Adutwum, L A; Harynuk, J J

    2014-08-01

    Using raw GC/MS data as the X-block for chemometric modeling has the potential to provide better classification models for complex samples when compared to using the total ion current (TIC), extracted ion chromatograms/profiles (EIC/EIP), or integrated peak tables. However, the abundance of raw GC/MS data necessitates some form of data reduction/feature selection to remove the variables containing primarily noise from the data set. Several algorithms for feature selection exist; however, due to the extreme number of variables (10(6)-10(8) variables per chromatogram), the feature selection time can be prolonged and computationally expensive. Herein, we present a new prefilter for automated data reduction of GC/MS data prior to feature selection. This tool, termed unique ion filter (UIF), is a module that can be added after chromatographic alignment and prior to any subsequent feature selection algorithm. The UIF objectively reduces the number of irrelevant or redundant variables in raw GC/MS data, while preserving potentially relevant analytical information. In the m/z dimension, data are reduced from a full spectrum to a handful of unique ions for each chromatographic peak. In the time dimension, data are reduced to only a handful of scans around each peak apex. UIF was applied to a data set of GC/MS data for a variety of gasoline samples to be classified using partial least-squares discriminant analysis (PLS-DA) according to octane rating. It was also applied to a series of chromatograms from casework fire debris analysis to be classified on the basis of whether or not signatures of gasoline were detected. By reducing the overall population of candidate variables subjected to subsequent variable selection, the UIF reduced the total feature selection time for which a perfect classification of all validation data was achieved from 373 to 9 min (98% reduction in computing time). Additionally, the significant reduction in included variables resulted in a concomitant

  5. PIXiE: An Algorithm for Automated Ion Mobility Arrival Time Extraction and Collision Cross Section Calculation using Global Data Association

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Jian; Casey, Cameron P.; Zheng, Xueyun; Ibrahim, Yehia M.; Wilkins, Christopher S.; Renslow, Ryan S.; Thomas, Dennis G.; Payne, Samuel H.; Monroe, Matthew E.; Smith, Richard D.; Teeguarden, Justin G.; Baker, Erin M.; Metz, Thomas O.

    2017-05-15

    Motivation: Drift tube ion mobility spectrometry (DTIMS) is increasingly implemented in high throughput omics workflows, and new informatics approaches are necessary for processing the associated data. To automatically extract arrival times for molecules measured by DTIMS coupled with mass spectrometry and compute their associated collisional cross sections (CCS) we created the PNNL Ion Mobility Cross Section Extractor (PIXiE). The primary application presented for this algorithm is the extraction of information necessary to create a reference library containing accu-rate masses, DTIMS arrival times and CCSs for use in high throughput omics analyses. Results: We demonstrate the utility of this approach by automatically extracting arrival times and calculating the associated CCSs for a set of endogenous metabolites and xenobiotics. The PIXiE-generated CCS values were identical to those calculated by hand and within error of those calcu-lated using commercially available instrument vendor software.

  6. A new ion imprinted polymer based on Ru(III)-thiobarbituric acid complex for solid phase extraction of ruthenium(III) prior to its determination by ETAAS.

    Science.gov (United States)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

    2014-01-01

    A new ruthenium ion imprinted polymer was prepared from the Ru(III) 2-thiobarbituric acid complex (the template), methacrylic acid or acrylamide (the functional monomers), and ethylene glycol dimethacrylate (the cross-linking agent) using 2,2'-azobisisobutyronitrile as the radical initiator. The ion imprinted polymer was characterized and used as a selective sorbent for the solid phase extraction of Ru(III) ions. The effects of type of functional monomer, sample volume, solution pH and flow rate on the extraction efficiency were studied in the dynamic mode. Ru(III) ion was quantitatively retained on the sorbents in the pH range from 3.5 to 10, and can be eluted with 4 mol L(-1) aqueous ammonia. The affinity of Ru(III) for the ion imprinted polymer based on the acrylamide monomer is weaker than that for the polymer based on the methacrylic acid monomer, which therefore was used in interference studies and in analytical applications. Following extraction of Ru(III) ions with the imprint and their subsequent elution from the polymer with aqueous ammonia, Ru(III) was detected by electrothermal atomic absorption spectrometry with a detection limit of 0.21 ng mL(-1). The method was successfully applied to the determination of trace amounts of Ru(III) in water, waste, road dust and platinum ore (CRM SARM 76) with a reproducibility (expressed as RSD) below 6.4 %. FigureThe new ion imprinted polymer was prepared and used for the separation of ruthenium from water and most complex environmental samples, such as road dust and platinum ore (CRM SARM 76) prior ETAAS determination.

  7. 强流ECR离子源引出系统研究%Study on Extraction System for High Current ECR Ion Source

    Institute of Scientific and Technical Information of China (English)

    王云; 张文慧; 张子民; 张雪珍; 刘占稳; 陈志; 赵红卫; 赵阳阳; 孙良亭; 杨尧; 钱程; 武启; 马鸿义

    2013-01-01

      为了提高强流ECR离子源的引出束流品质,分别设计了1#和2#引出系统,利用束流引出模拟软件PBGUNS对1#和2#引出系统进行了质子束流引出与传输的模拟计算,结合实际测得的发射度数据分析引出系统,发现2#引出系统比1#引出系统引出束流品质高。对ECR离子源引出系统的电势等位线分布等参数引起的球差进行了简单数学推导及MATLAB绘图,并结合1#和2#引出系统束流相图模拟结果证明了球差会使引出束流品质有效发射度增长,通过适当加大电极孔径可改善束流聚焦情况,得到了束流光学聚焦较好的束流引出系统设计。%  To improve the quality of extracted ion beam from a high current ECR ion source, 1# and 2# extraction systems were designed and tested. The PBGUNS code was used to simulate the 1# and 2# extraction systems of proton ion beam. The emittance measurement results with the two different extraction systems were compared and analyzed with the simulation, the conclusion that more high quality beam extracted from 2# system than 1# system was got. The formula derivation of ECR ion source extraction system spherical aberration and MATLAB drawing was done by the analyzing on the distribution of extraction field equipotentials, effective emittance increasing caused by spherical aberration was proved by 1# and 2# extraction systems beam phase space simulation result, beam focusing would be improved if electrode hole size increasing appropriately and a general concept on good optics focusing of ion beam extraction system was proposed finally.

  8. Quality representation of Yuanzhi (Radix Polygalae)based on characteristic chromatograms of drug-like effective components of Kai Xin San-Yuanzhi%基于开心散-远志类药有效组分特征图谱的远志质量表征研究

    Institute of Scientific and Technical Information of China (English)

    姜艳艳; 戴莹; 巴寅颖; 刘洋; 张硕峰; 畅洪昇; 吕航; 闫陶; 石任兵

    2011-01-01

    目的 筛选开心散一远志关联的类药有效组分,建立基于类药有效组分的远志特征图谱,进行远志质量表征研究.方法SD大鼠,采用东莨菪碱造模致记忆障碍,灌胃给予‘开心散提取物后,制备含药血清,测定HPLC特征图谱.在相同的色谱条件下测定远志提取物的HPLC特征图谱,并以保留时间为主要指标,与开心散提取物HPLC特征图谱进行对比分析,采用对照品添加法,鉴定特征色谱峰.结果筛选出远志类药有效组分,建立了远志类药有效组分特征图谱,鉴定了其中4个特征化学成分,分别为西伯利亚糖As、西伯利亚糖A6.远志咄酮Ⅲ和3,6’.二芥子酰基蔗糖,并建立了开心散和远志特征图谱之间的关联关系,进而基于类药有效组分筛选结果,建立了基于开心散类药有效组分的远志特征图谱质量表征方法.结论所建立的质量表征方法科学、合理、可行,为建立体现中药及复方有效物质基础特点的质量控制方法体系的构建提供研究思路与方法学.%Objective To screen the drug-like effective components related to Kai Xin San-Yuanzhi (Radix Polygalae), establish the characteristic chromatograms of Yuanzhi based on drug-like effective components, and study the quality representation of Yuanzhi. Methods The model of dysmnesia was established by using scopolamine in SD rats, and then the rats were given intragastrically the extract of Kai Xin San for collecting medicinal serum and determining HPLC characteristic chromatograms. With the same chromatographic condition, the HPLC characteristic chromatogram of Yuanzhi extract was determined, and compared with that of extract of Kai Xin San taken retention time as a major index. The characteristic chromatographic peaks were identified by using reference addition method. Results The drug-like effective components of Yuanzhi were screened and the characteristic chromatogram wasestablished. There were 4 characteristic

  9. Self-focusing of a high current density ion beam extracted with concave electrodes in a low energy region around 150 eV

    Energy Technology Data Exchange (ETDEWEB)

    Hirano, Y., E-mail: y.hirano@aist.go.jp [Innovative Plasma Technologies Group, National Institute of Advanced Industrial Science and Technology (AIST), Ibaraki (Japan); Laboratory of Physics, College of Science and Technologies, Nihon University, Tokyo (Japan); Kiyama, S.; Koguchi, H. [Innovative Plasma Technologies Group, National Institute of Advanced Industrial Science and Technology (AIST), Ibaraki (Japan); Sakakita, H. [Innovative Plasma Technologies Group, National Institute of Advanced Industrial Science and Technology (AIST), Ibaraki (Japan); Department of Engineering Mechanics and Energy, University of Tsukuba, Ibaraki (Japan)

    2014-02-15

    Spontaneous self-focusing of ion beam with high current density (J{sub c} ∼ 2 mA/cm{sup 2}, I{sub b} ∼ 65 mA) in low energy region (∼150 eV) is observed in a hydrogen ion beam extracted from an ordinary bucket type ion source with three electrodes having concave shape (acceleration, deceleration, and grounded electrodes). The focusing appears abruptly in the beam energy region over ∼135–150 eV, and the J{sub c} jumps up from 0.7 to 2 mA/cm{sup 2}. Simultaneously a strong electron flow also appears in the beam region. The electron flow has almost the same current density. Probably these electrons compensate the ion space charge and suppress the beam divergence.

  10. Hexavalent chromium recovery by liquid–liquid extraction with 2-octylaminopyridine from acidic chloride media and its sequential separation from other heavy toxic metal ions

    Directory of Open Access Journals (Sweden)

    C.P. Mane

    2016-11-01

    Full Text Available A systematic study of extraction of chromium(VI with 2-octylaminopyridine (2-OAP in xylene at room temperature has been conducted. Quantitative extraction of chromium(VI was observed in the 0.4–0.8 M concentration range of hydrochloric acid. From the extracted complex species in the organic phase, chromium(VI was back extracted with 7 N ammonia (3 × 10 mL, and was determined by spectrophotometric method. Various parameters such as 2-OAP concentration, equilibrium period, effect of various diluents, aqueous: organic volume ratio, acidity and diverse ions were studied. The extraction reaction proceeds with ion-pair formation and the stoichiometry of extracted species was found to be [(2OAPH+ CrO3Cl−](org. The separation and determination of chromium(VI from associated and toxic metals in binary, ternary and multicomponent mixture were carried out. The method permits the sequential separation of chromium(VI from other toxic metals and has been used to separate and determine chromium(VI from alloys, and effluent water samples from tannery industries.

  11. Control control control: a reassessment and comparison of GenBank and chromatogram mtDNA sequence variation in Baltic grey seals (Halichoerus grypus.

    Directory of Open Access Journals (Sweden)

    Katharina Fietz

    Full Text Available Genetic data can provide a powerful tool for those interested in the biology, management and conservation of wildlife, but also lead to erroneous conclusions if appropriate controls are not taken at all steps of the analytical process. This particularly applies to data deposited in public repositories such as GenBank, whose utility relies heavily on the assumption of high data quality. Here we report on an in-depth reassessment and comparison of GenBank and chromatogram mtDNA sequence data generated in a previous study of Baltic grey seals. By re-editing the original chromatogram data we found that approximately 40% of the grey seal mtDNA haplotype sequences posted in GenBank contained errors. The re-analysis of the edited chromatogram data yielded overall similar results and conclusions as the original study. However, a significantly different outcome was observed when using the uncorrected dataset based on the GenBank haplotypes. We therefore suggest disregarding the existing GenBank data and instead using the correct haplotypes reported here. Our study serves as an illustrative example reiterating the importance of quality control through every step of a research project, from data generation to interpretation and submission to an online repository. Errors conducted in any step may lead to biased results and conclusions, and could impact management decisions.

  12. 故障变压器油色谱分析及解决方案%Chromatogram Analysis of Transformer Oil in Transformer with Problems and its Solutions

    Institute of Scientific and Technical Information of China (English)

    房小花

    2014-01-01

    分析了一例变压器故障产生的原因并给出解决方案。利用油色谱分析法(即色谱分析)分析了变压器故障产生的原因,此方法可以定期对运行中的变压器进行诊断分析,不仅有较大的经济效益,而且精度高、可靠性好,判断变压器的内部故障并找出解决方法,对现场产生故障的变压器的故障分析、判断和修理具有现实的意义。%Based on the analysis of a case of transformer fault and bringing forward solution, analyzing chromatogram of transformer oil was introduced to looking for the reason of transformer fault. The method can be used for diagnosing and analyzing running transformer regularly, which not only have great economic benefits, but high precision and better reliability. To determine internal fault of transformer through chromatogram analysis and to find out the solution has real meaning for making analysis, judgment and how to repair fault transformer on site through chromatogram analysis of transformer oil.

  13. The synthesis of (N 2O 2S 2)-Schiff base ligands and investigation of their ion extraction capability from aqueous media

    Science.gov (United States)

    Zoubi, Wail A. L.; Kandil, Farouk; Chebani, Mohamad Khaled

    2011-09-01

    Two new Schiff bases (I) and (II) containing nitrogen-sulfur-oxygen donor atoms were designed and synthesized in a multi-step reaction sequence. The Schiff base (I) was used in solvent extraction of metal chlorides such as Cu 2+ and Cr 3+ as well as metal picrates such as Hg 2+ and UO 22+ from aqueous phase to the organic phase. The influences of the parameter functions, such as pH, solvent, ionic strength of aqueous phase, aqueous to organic phase and concentration of the extractant were investigated to shed light on their chemical extracting properties upon the extractability of metal ions. The effect of chloroform, dichloromethane and nitrobenzene as organic solvents over the metal chlorides extraction was investigated at 25 ± 0.1 °C by using flame atomic absorption and the result is that the ability of extraction in solvents as follows: C 6H 5NO 2 > CHCl 3 > CH 2Cl 2 and the compositions of the extracted species have been determined. The metal picrate extraction was investigated at 25 ± 0.1 °C by using UV-visible spectrometry. As well that the extraction of picrates metal such as UO 22+ and Hg 2+ with Schiff base(I) in absence and presence of 2-(2-aminoethyl) pyridine was investigated in chloroform. The extraction results revealed the presence of neutral donors 2-(2-aminoethyl) pyridine shifts the extraction percentage curves towards higher pH region, indicating a synergistic effect of this donors on extraction of UO 22+ and Hg 2+ by the studied Schiff base (I).

  14. Strain accommodation and potential hysteresis of LiFePO 4 cathodes during lithium ion insertion/extraction

    Science.gov (United States)

    Zhu, Yujie; Wang, Chunsheng

    Equilibrium potential hysteresis of electrode materials refers to the phenomenon that discharge equilibrium potential is lower than charge equilibrium potential. It is induced by the strain accommodation energy of phase transformation. Taking LiFePO 4 as an example, the equilibrium potential hysteresis and accommodation energy of two LiFePO 4 with different particle sizes were characterized using galvanostatic intermittent titration technique (GITT), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) methods. The LiFePO 4 sample with 40 nm particle size has lower accommodation energy than that of 100 nm LiFePO 4, which is due to a narrower miscibility gap and smaller potential hysteresis of 40 nm LiFePO 4 comparing to 100 nm LiFePO 4. The phase transformation of LiFePO 4 occurs only at potential levels above delithiation (charge) equilibrium potential and below lithiation (discharge) equilibrium potential. No phase transformation occurs when charge/discharge is limited in the potential hysteresis range, i.e. LiFePO 4 behaves like a solid solution in the potential hysteresis range. A reliable EIS can only be obtained when it is performed at the center of potential hysteresis and the potential amplitude does not exceed the range of equilibrium potential hysteresis. The analysis on strain accommodation and potential hysteresis of LiFePO 4 cathodes during Li ion insertion/extraction is also suitable for other phase transformation electrodes.

  15. +Facile extraction of azide in sartan drugs using magnetized anion-exchange metal-organic frameworks prior to ion chromatography.

    Science.gov (United States)

    Zhang, Sainan; Han, Peipei; Xia, Yan

    2017-09-08

    Quaternary amine functionalized metal-organic framework MIL-101(Cr) (MIL-101(Cr)-NMe3) was prepared as the sorbent for the magnetic solid-phase extraction (MSPE) of azide from sartan drugs before ion chromatography determination. Magnetization of MIL-101-NMe3 were achieved concurrently by adding MIL-101-NMe3 and Fe3O4@SiO2 to the sample solution under ultrasonication. The prepared Fe3O4@SiO2/MIL-101-NMe3 gave the adsorption capacity of 37.5mgg(-1). The developed method had a detection limit of 0.24μgL(-1) and quantitation limit of 0.79μgL(-1) for azide. The relative standard deviations for the intra-day retention time and peak area were 0.52% and 0.36% (n=5), respectively. The developed method was successfully applied for the determination of azide in sartan drugs with the recoveries from 96.5% to 100.5%. Copyright © 2017. Published by Elsevier B.V.

  16. Identification and characterization of supercritical fluid extracts of Rhizoma Chuanxiong by high performance liquid chromatography ion trap mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Teng Jiuwei; Chen Hongwei; Li Deliang; Luo Andong

    2006-01-01

    The main constituents,senkyunolide A,Zligustilide,neocnidilide,3-butylphthalide,and ligustilide dimers,in supercritical CO2 fluid extracts of Rhizoma Chuanxiong,a popular Chinese traditional medicine,have been identified and characterized by high performance liquid chromatography tandem mass spectrometry.Separations were carded out on an Agilent (ECLIPSE XDB) C18 analytical column by gradient elution with 0.25% acetic acid and methanol (containing 0.25% acetic acid).An Agilent 1100 series LC/MSD XCT system was operated under positive ESI and auto MS/MS modes for mass spectrometric analysis.Collision-induced dissociation (CID) fragmentations of these phthalides have been investigated and elucidated.Phthalides have primarily undergone two ESI CID pathways:side-chain cleavage with losses of alkenes and ring-opening with eliminations of H2O followed by losses of CO.Direct neutral loss of CO has not been observed.Sodium adduct ions have demonstrated completely different CID pathways.

  17. Novel polymer inclusion membranes containing T2EHDGA as carrier extractant for actinide ion uptake from acidic feeds

    Energy Technology Data Exchange (ETDEWEB)

    Mahanty, Bholanath; Das, Dillip Kumar; Behere, Praveen Gajanan; Afzal, Mohammad [Bhabha Atomic Research Centre, Tarapur, Maharashtra (India). Advanced Fuel Fabrication Facility; Mohapatra, Prasanta Kumar; Raut, Dhaval Ramakant [Bhabha Atomic Research Centre, Trombay, Mumbai (India). Radiochemistry Div.

    2015-06-01

    Polymer inclusion membranes (PIM) containing N,N,N',N'-tetra(2-ethylhexyl) diglycolamide (T2EHDGA) were evaluated for the separation of actinide ions such as Am{sup 3+}, Pu{sup 4+}, UO{sub 2}{sup 2+} and Th{sup 4+} from acidic feeds. The PIMs were prepared using cellulose triacetate (CTA) as the polymer matrix, 2-nitrophenyloctyl ether (NPOE) as the plasticizer and T2EHDGA as the carrier extractant and the optimized membrane composition was found to be 68.4% T2EHDGA, 17.9% NPOE and 13.7% CTA which resulted in 74% Am{sup 3+} uptake at 1 M HNO{sub 3} in 2 h. The uptake studies were carried out using feed solutions containing varying concentrations of nitric acid (0.5-3.0 M) and showed the trend: Pu{sup 4+} > Am{sup 3+} > Th{sup 4+} > UO{sub 2}{sup 2+}. Quantitative stripping (> 99%) of the sorbed Am{sup 3+} was possible using a solution containing 0.01 M EDTA at pH 3.0. Reusability studies indicated deterioration of the PIM on continuous use.

  18. Enhanced Retention of Chelating Reagents in Octadecylsilyl Silica Phase by Interaction with Residual Silanol Groups in Solid Phase Extraction of Divalent Metal Ions.

    Science.gov (United States)

    Ohmuro, Satoshi; Fujii, Kan; Yasui, Takashi; Takada, Kazutake; Yuchi, Akio; Kokusen, Hisao

    2016-01-01

    Solid-phase extraction (SPE) of divalent metal ions with a lipophilic and potentially divalent hexadentate chelating reagent (H2L), with which octadecylsilyl silica (ODS), was impregnated with was studied to gain more insight into and develop the potential of this methodology. This is the first time to demonstrate that this reagent as well as other common nitrogen-containing reagents were retained both by adsorption due to hydrogen bonding between nitrogen atoms of the reagent and residual silanol groups in the ODS phase and by simple distribution into the hydrophobic space. An appreciably large amount of this reagent could be retained by the adsorption mechanism even with a relatively thin loading solution. The divalent metal ions of Mn(2+), Co(2+) and Zn(2+) were extracted as 1:1 neutral complexes ([ML]), while Ni(2+) and Cu(2+) as ion-pairs of 1:1 cationic complex ([MHL](+)) with anion in SPE with H2L. The extractability and selectivity were substantially the same as that in liquid-liquid extraction.

  19. Solid phase extraction and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic nanoporous silica

    Energy Technology Data Exchange (ETDEWEB)

    Omidi, Fariborz [Department of Occupational Health Engineering, School of Public Health, Shahroud University of Medical Sciences, Shahroud (Iran, Islamic Republic of); Behbahani, Mohammad, E-mail: mohammadbehbahai89@yahoo.com [Department of Chemistry, Shahid Beheshti University, Evin, Tehran (Iran, Islamic Republic of); Kalate Bojdi, Majid [Faculty of Chemistry, Kharazmi (Tarbiat Moallem) University, Tehran (Iran, Islamic Republic of); Shahtaheri, Seyed Jamaleddin [Department of Occupational Health Engineering, School of Public Health and Institute for Environmental Research, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of)

    2015-12-01

    A new method has been developed for trace separation/preconcentration of cadmium ions using pyridine-functionalized magnetic nanoporous silica material (called Py-Fe{sub 3}O{sub 4}@MCM-41) as a new magnetic sorbent and their determination by flame atomic absorption spectrometry (FAAS). The Py-Fe{sub 3}O{sub 4}@MCM-41 sorbent was characterized by thermogravimetric analysis, differential thermal analysis, transmission electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The modified Fe{sub 3}O{sub 4}@MCM-41 can be easily separated from an aqueous solution by applying an external magnetic field. Effects of pH, amount of functionalized Fe{sub 3}O{sub 4}@MCM-41, extraction time, type and quantity of eluent, desorption time, and interfering ions on the extraction efficiency were evaluated and optimized. Under the optimized conditions, the detection limit and relative standard deviation was 0.04 μg L{sup –1} and 2.9%, respectively and the maximum adsorption capacity of the synthesized sorbent for cadmium ions was 154 mg g{sup −1}. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, rice, onion, carrot, lettuce, parsley, basil, tap water, river water and seawater with satisfactory results. - Highlights: • The introducing of modified magnetic mesoporous silica as a novel magnetic sorbent. • Trace monitoring of cadmium ions. • The limit of detection (LOD) by the proposed solid phase extraction method was 0.04 ng mL{sup −1} for the cadmium ions. • High surface areas and magnetic characteristic of the sorbent. • Maximum adsorption capacity of the sorbent was 154 mg g{sup −1}.

  20. Ultrasound-assisted low-density solvent dispersive liquid-liquid extraction for the determination of alkanolamines and alkylamines in cosmetics with ion chromatography.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke; Zhong, Xiuhua; Luo, Zhibin; Zhu, Binghui

    2013-10-15

    A new one-step sample preparation technique termed ultrasound-assisted low-density solvent dispersive liquid-liquid extraction (UA-LDS-DLLE) coupled with ion chromatography (IC) was developed for the determination of three alkanolamines and two alkylamines in complex samples. Sample matrices were rapidly dissolved and dispersed to form cloudy solutions by using two solvents, where target analytes were transferred into acid solutions, while liposoluble substances were dissolved in cyclohexane. The obtained extracts could be used directly for injection analysis without any additional purification because the potential matrix interferences had been effectively eliminated in extraction process. The extraction efficiency could be markedly enhanced and the extraction could be quickly accomplished within 13 min under the synergistic effects of ultrasound radiation, vibration and heating. Various parameters influencing extraction efficiency were evaluated using orthogonal array experimental design. The extraction performance of the approach was demonstrated for the determination of target analytes in 15 commercial cosmetics covering very different matrices. Linearity ranges of 0.3-50 mg L(-1) and limits of detection varying from 0.072 to 0.12 mg L(-1) were achieved. The recoveries ranged from 86.9-108.5% with the relative standard deviations (RSDs) of 1.2-6.2%. The method was proved to be a simple and effective extraction technique that provided an attractive alternative to the analysis of trace amounts of target analytes in large numbers of cosmetics. Copyright © 2013. Published by Elsevier B.V.

  1. Chelating agent free solid phase extraction (CAF-SPE) method for separation and/or preconcentration of iron(III) ions

    OpenAIRE

    for, Chelating agent free solid phase extract

    2014-01-01

    This paper presents a chelating agent free solid phase extraction (CAF-SPE) method for the separation and/or preconcentration of trace iron(III) ions. This method is based on the sorption of Fe(III) ions without using any chelating agent onto Amberlyst 36 resin. A good relative standard deviation (3%), high recovery (>95%), high enrichment factor (100), and low detection limit (0.32 m g L-1) were obtained. The adsorption capacity of resin was 117 mg g-1 for iron(III). The me...

  2. 三七破壁饮片指纹图谱研究%Study on HPLC Fingerprint Chromatograms of Cell Wall-Broken Decoction Pieces of Notoginseng

    Institute of Scientific and Technical Information of China (English)

    陈炜璇; 刘敏; 严萍; 詹若挺; 陈蔚文; 成金乐

    2012-01-01

    Objective: To establish the HPLC fingerprint chromatograms of crude Notoginseng, cell wall-broken powder and cell wall-broken decoction pieces of Notoginseng and provide evidence for quality control of cell wall-broken decoction pieces of Notoginseng. Methods:The HPLC procedure was performed on the chromatographic column of Hypersil ODS2 ,and the mobile phase was aceto-nitrile and water in gradient elution with the flow velocity of 1. 0 mL/min. The detection wavelength was 203 nm and the column temperature was 25 ℃. The chromatograms was analyzed with the software of "similarity evaluation system for chromatographic fingerprint of TCM". Results:Eight common peaks were pinpointed from the chromatograms of different batches of crude Notoginseng, cell-broken powder and cell-broken decoction pieces, the similarities of the chromatograms were all larger than 0. 9. Conclusion: The method of the HPLC fingerprint chromatogram is of good precision, reproducibility and stability, which is suitable for quality control of cell wall-broken decoction pieces of Notoginseng.%目的:建立三七药材、破壁粉体和破壁饮片的HPLC指纹图谱,为三七破壁饮片的质量控制提供依据.方法:采用高效液相色谱法,Hypersil ODS2色谱柱,流动相:乙腈-水(梯度洗脱),流速:1.0 mL/min,检测波长:203nm,柱温:25℃.采用“中药色谱指纹图谱相似度评价系统”软件对图谱进行分析处理.结果:三七药材、破壁粉体和破壁饮片皂苷类成分指纹图谱标定8个共有峰,三七药材、破壁粉体和破壁饮片之间相似度均大于0.9.结论:建立的HPLC指纹图谱方法具有良好的精密度、重复性和稳定性,适用于三七破壁饮片的质量控制.

  3. Determination of sulfonamide antibiotics and metabolites in liver, muscle and kidney samples by pressurized liquid extraction or ultrasound-assisted extraction followed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry (HPLC-QqLIT-MS/MS).

    Science.gov (United States)

    Hoff, Rodrigo Barcellos; Pizzolato, Tânia Mara; Peralba, Maria do Carmo Ruaro; Díaz-Cruz, M Silvia; Barceló, Damià

    2015-03-01

    Sulfonamides are widely used in human and veterinary medicine. The presence of sulfonamides residues in food is an issue of great concern. Throughout the present work, a method for the targeted analysis of 16 sulfonamides and metabolites residue in liver of several species has been developed and validated. Extraction and clean-up has been statistically optimized using central composite design experiments. Two extraction methods have been developed, validated and compared: i) pressurized liquid extraction, in which samples were defatted with hexane and subsequently extracted with acetonitrile and ii) ultrasound-assisted extraction with acetonitrile and further liquid-liquid extraction with hexane. Extracts have been analyzed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry. Validation procedure has been based on the Commission Decision 2002/657/EC and included the assessment of parameters such as decision limit (CCα), detection capability (CCβ), sensitivity, selectivity, accuracy and precision. Method׳s performance has been satisfactory, with CCα values within the range of 111.2-161.4 µg kg(-1), limits of detection of 10 µg kg(-1) and accuracy values around 100% for all compounds.

  4. Electron Beam Ion Sources

    OpenAIRE

    Zschornacka, G.; Schmidt, M.; Thorn, A.

    2014-01-01

    Electron beam ion sources (EBISs) are ion sources that work based on the principle of electron impact ionization, allowing the production of very highly charged ions. The ions produced can be extracted as a DC ion beam as well as ion pulses of different time structures. In comparison to most of the other known ion sources, EBISs feature ion beams with very good beam emittances and a low energy spread. Furthermore, EBISs are excellent sources of photons (X-rays, ultraviolet, extreme ultraviole...

  5. Rapid quantification of four major bioactive alkaloids in Corydalis decumbens (Thunb.) Pers. by pressurised liquid extraction combined with liquid chromatography-triple quadrupole linear ion trap mass spectrometry.

    Science.gov (United States)

    Shen, Yan; Han, Chao; Jiang, Yongxiang; Zhou, Xiujin; Zhu, Zhenou; Lei, Xinxiang

    2011-05-30

    A new method based on pressurised liquid extraction (PLE) followed by liquid chromatography-triple quadrupole linear ion trap mass spectrometry (LC-QTrap-MS) analysis has been developed for the identification and quantification of four major alkaloids in extracts of Corydalis decumbens (Thunb.) Pers. PLE extractions were performed using 90% ethanol; temperature was set at 100°C and pressure at 1500 psi. HPLC analysis was performed on a Waters XBridge™ C(18) column (150 mm × 2.1mm i.d., 3.5 μm) eluted by a mobile phase of acetonitrile and 0.2% acetic acid. Data acquisition was carried out in multiple reaction monitoring transitions (MRMs) mode, monitoring two MRM transitions to ensure an accurate identification of target compounds in the samples. Additional identification and confirmation of target compounds were performed using the enhanced product ion modus (EPI) of the linear ion trap. The novel LC-QTrap-MS platform offers the best sensitivity and specificity for characterization and quantitative determination of the four alkaloids in C. decumbens (Thunb.) Pers. and fulfils the quality criteria for routine laboratory application.

  6. Appropriate use of the particle-in-cell method in low temperature plasmas: Application to the simulation of negative ion extraction

    Science.gov (United States)

    Garrigues, L.; Fubiani, G.; Boeuf, J. P.

    2016-12-01

    The Particle-In-Cell Monte Carlo Collision (PIC MCC) method has been used by different authors in the last ten years to describe negative ion extraction in the context of neutral beam injection for fusion. Questionable results on the intensity and profile of the extracted negative ion beamlets have been presented in several recently published papers. Using a standard explicit PIC MCC method, we show that these results are due to a non-compliance with the constraints of the numerical method (grid spacing, number of particles per cell) and to a non-physical generation of the simulated plasma. We discuss in detail the conditions of mesh convergence and plasma generation and show that the results can significantly deviate from the correct solution and lead to unphysical features when the constraints inherent to the method are not strictly fulfilled. This paper illustrates the importance of verification in any plasma simulation. Since the results presented in this paper have been obtained with careful verification of the method, we propose them as benchmarks for future comparisons between different simulation codes for negative ion extraction.

  7. Trace monitoring of silver ions in food and water samples by flame atomic absorption spectrophotometry after preconcentration with solvent-assisted dispersive solid phase extraction.

    Science.gov (United States)

    Omidi, Fariborz; Behbahani, Mohammad; Shahtaheri, Seyed Jamaleddin; Salimi, Sara

    2015-06-01

    In this research, a new sample treatment technique termed solvent-assisted dispersive solid phase extraction (SADSPE) was developed. The new method was based on the dispersion of the sorbent into the sample to maximize the contact surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by injecting a mixture solution of the sorbent and disperser solvent into the aqueous sample. Thereby, a cloudy solution formed. The cloudy solution resulted from the dispersion of the fine particles of the sorbent in the bulk aqueous sample. After extraction, the cloudy solution was centrifuged and the enriched analytes in the sediment phase dissolved in ethanol and determined by FAAS. Under the optimized conditions, the detection limit for silver ions was 0.8 μg L(-1). The relative standard deviations for six separate extraction experiments for determination of 5 and 200 μg L(-1) of silver ions was 3.4 and 3.1 %. The preconcentration factor was found to be 61.7. SADSPE was successfully applied for trace determination of silver ions in water and food samples.

  8. Solid phase extraction and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic nanoporous silica

    Science.gov (United States)

    Omidi, Fariborz; Behbahani, Mohammad; Kalate Bojdi, Majid; Shahtaheri, Seyed Jamaleddin

    2015-12-01

    A new method has been developed for trace separation/preconcentration of cadmium ions using pyridine-functionalized magnetic nanoporous silica material (called Py-Fe3O4@MCM-41) as a new magnetic sorbent and their determination by flame atomic absorption spectrometry (FAAS). The Py-Fe3O4@MCM-41 sorbent was characterized by thermogravimetric analysis, differential thermal analysis, transmission electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The modified Fe3O4@MCM-41 can be easily separated from an aqueous solution by applying an external magnetic field. Effects of pH, amount of functionalized Fe3O4@MCM-41, extraction time, type and quantity of eluent, desorption time, and interfering ions on the extraction efficiency were evaluated and optimized. Under the optimized conditions, the detection limit and relative standard deviation was 0.04 μg L-1 and 2.9%, respectively and the maximum adsorption capacity of the synthesized sorbent for cadmium ions was 154 mg g-1. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, rice, onion, carrot, lettuce, parsley, basil, tap water, river water and seawater with satisfactory results.

  9. Extraction methods for the removal of phospholipids and other endogenous material from a biological fluid.

    Science.gov (United States)

    Michopoulos, F; Edge, A M; Hui, Y-T; Liddicoat, T; Theodoridis, G; Wilson, I D

    2011-12-01

    A comparison of three different sample preparation techniques for the analysis of plasma samples has been investigated to highlight the effect that these approaches have on the removal of endogenous material. The three techniques under investigation are: SPE, support assisted liquid-liquid extraction and nonspecific solvent-based protein precipitation. Comparisons are made on the practicalities of each approach and to allow a semiquantitative assessment between the effectiveness of these different techniques the relative amounts of phospholipids present within the sample are analyzed. Total ion chromatograms are also obtained to further study the effects of different extraction techniques in the removal of endogenous components from a biological matrix. Both of these approaches provide a very coarse measure of the cleanliness of the extracts and demonstrate that support assisted liquid-liquid extraction and an optimized SPE approach remove a greater amount of endogenous material. This study highlights the importance of sample preparation in removing endogenous material, which may have a detrimental effect on the performance of a bioanalytical assay.

  10. Multiresidue pesticide analysis of ginseng powders using acetonitrile- or acetone-based extraction, solid-phase extraction cleanup, and gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS).

    Science.gov (United States)

    Wong, Jon W; Zhang, Kai; Tech, Katherine; Hayward, Douglas G; Krynitsky, Alexander J; Cassias, Irene; Schenck, Frank J; Banerjee, Kaushik; Dasgupta, Soma; Brown, Don

    2010-05-26

    A multiresidue method for the analysis of 168 pesticides in dried powdered ginseng has been developed using acetonitrile or acetone mixture (acetone/cyclohexane/ethyl acetate, 2:1:1 v/v/v) extraction, solid-phase extraction (SPE) cleanup with octyl-bonded silica (C(8)), graphitized carbon black/primary-secondary amine (GCB/PSA) sorbents and toluene, and capillary gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS). The geometric mean limits of quantitation (LOQs) were 53 and 6 microg/kg for the acetonitrile extraction and 48 and 7 microg/kg for the acetone-based extraction for GC-MS/SIM and GC-MS/MS, respectively. Mean percent recoveries and standard deviations from the ginseng fortified at 25, 100, and 500 microg/kg using GC-MS/SIM were 87 +/- 10, 88 +/- 8, and 86 +/- 10% from acetonitrile extracts and 88 +/- 13, 88 +/- 12, and 88 +/- 14% from acetone mixture extracts, respectively. The mean percent recoveries from the ginseng at the 25, 100, and 500 microg/kg levels using GC-MS/MS were 83 +/- 19, 90 +/- 13, and 89 +/- 11% from acetonitrile extracts and 98 +/- 20, 91 +/- 13, and 88 +/- 14% from acetone extracts, respectively. Twelve dried ginseng products were found to contain one or more of the following pesticides and their metabolites: BHCs (benzene hexachlorides, alpha-, beta-, gamma-, and delta-), chlorothalonil, chlorpyrifos, DDT (dichlorodiphenyl trichloroethane), dacthal, diazinon, iprodione, quintozene, and procymidone ranging from 4000 microg/kg. No significant differences were found between the two extraction solvents, and GC-MS/MS was found to be more specific and sensitive than GC-MS/SIM. The procedures described were shown to be effective in screening, identifying, confirming, and quantitating pesticides in commercial ginseng products.

  11. Experimental study and simulation of the extraction conditions of a multicharged ion beam from an electron cyclotron resonance source; Etude experimentale et simulation des conditions d`extraction d`un faisceau d`ions multicharges d`une source a resonance cyclotronique electronique

    Energy Technology Data Exchange (ETDEWEB)

    Mandin, J.

    1996-12-17

    This thesis concerns the beam extraction studies of ECR Ion Sources for the SPIRAL project at GANIL (France). The optical properties (i.e. the emittances) of the radioactive ion beam production source is a crucial point in this project. We performed emittance measurements with a very high transport efficiency and developed a computer code for simulating the extraction and transport conditions. This simulation takes into account all the parameters acting on the extraction process: the characteristics of the ions and electrons emitted by the plasma, their space and energy distributions, the space charge, the magnetic filed of the source and the accelerating electric field. We explained the evolution of the emittances for two different types of ECR Ion Source. The simulation-experiment comparison showed us that the magnetic field and the intrinsic energy of the ions seem to be the most important parameters for explaining the overall emittance behaviour of the ECRIS. We precise their values and comment them. (author). 530refs.

  12. Cloud Point Extraction and Determination of Silver Ion in Real Sample using Bis((1H-benzo[d ]imidazol-2ylmethylsulfane

    Directory of Open Access Journals (Sweden)

    Farshid Ahmadi

    2011-01-01

    Full Text Available Bis((1H-benzo[d]imidazol-2ylmethylsulfane (BHIS was used as a complexing agent in cloud point extraction for the first time and applied for selective pre-concentration of trace amounts of silver. The method is based on the extraction of silver at pH 8.0 by using non-ionic surfactant T-X114 and bis((1H-benzo[d]imidazol-2ylmethylsulfane as a chelating agent. The adopted concentrations for BHIS, Triton X-114 and HNO3, bath temperature, centrifuge rate and time were optimized. Detection limits (3SDb/m of 1.7 along with enrichment factor of 39 for silver ion was achieved. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed method was successfully applied to the ultra-trace determination of silver in real samples.

  13. Di-ionizable p-tert-butylcalix[4]arene-1,2-crown-3 ligands in cone and 1,2-alternate conformations: synthesis and metal ion extraction.

    Science.gov (United States)

    Zhang, Dongmei; Cao, Xiaodan; Purkiss, David W; Bartsch, Richard A

    2007-04-21

    Novel di-ionizable p-tert-butylcalix[4]arene-1,2-crown-3 ligands in cone and 1,2-alternate conformations were prepared as potential metal ion extractants. Selective bridging of proximal hydroxyl groups of the calix[4]arene platform by a crown-3 polyether unit was achieved under Mitsunobu reaction conditions. In addition to the carboxylic acid group, the acidity tunable N-(X)sulfonyl oxyacetamide functions [OCH(2)C(O)NHSO(2)X] with X group variation from methyl to phenyl to p-nitrophenyl to trifluomethyl were used as the proton-ionizable groups. Conformations and regioselectivities of the new ligands were established by (1)H and (13)C NMR spectroscopy. Competitive solvent extractions of alkali metal cations and of alkaline earth metal cations from aqueous solutions into chloroform were performed, as were single species extractions of lead(ii) and mercury(ii).

  14. Sodium dodecyl sulfate coated γ-alumina support modified by a new Schiff base for solid phase extraction and flame-AAS determination of lead and copper ions

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2013-01-01

    Full Text Available A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb2+ and Cu2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS-coated γ-alumina modified with bis(2-hydroxy acetophenone-1,6-hexanediimine (BHAH ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS. The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb2+ or Cu2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu2+ was 7.9 µg L-1 with a relative standard deviation of 1.67%, while that for Pb2+ was 6.4 µg L-1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.

  15. Identification of alkyl dimethylbenzylammonium surfactants in water samples by solid-phase extraction followed by ion trap LC/MS and LC/MS/MS

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2001-01-01

    A novel methodology was developed for the determination of alkyl (C12, C14, and C16) dimethylbenzylammonium chloride (benzalkonium chloride or BAC, Chemical Abstract Service number: 8001-54-5) in water samples. This method is based on solid-phase extraction (SPE) using polymeric cartridges, followed by high-performance liquid chromatography/ion trap mass spectrometry (LC/MS) and tandem mass spectrometry(MS/MS) detection, equipped with an electrospray interface in positive ion mode. Chromatographic separation was achieved for three BAC homologues by using a C18 column and a gradient of acetonitrile/10 millimolar aqueous ammonium formate. Total method recoveries were higher than 71% in different water matrices. The main ions observed by LC/MS were at mass-to-charge ratios (m/z) of 304, 332, and 360, which correspond to the molecular ions of the C12, C14, and C16 alkyl BAC, respectively. The unequivocal structural identification of these compounds in water samples was performed by LC/MS/MS after isolation and subsequent fragmentation of each molecular ion. The main fragmentation observed for the three different homologues corresponded to the loss of the toluyl group in the chemical structure, which leads to the fragment ions at m/z 212, 240, and 268 and a tropylium ion, characteristic of all homologues, at m/z 91. Detection limits for the methodology developed in this work were in the low nanogram-per-liter range. Concentration levels of BAC - ranging from 1.2 to 36.6 micrograms per liter - were found in surface-water samples collected downstream from different wastewater-treatment discharges, thus indicating its input and persistence through the wastewater-treatment process.

  16. Selective extraction and release using (EDTA-Ni)-layered double hydroxide coupled with catalytic oxidation of 3,3',5,5'-tetramethylbenzidine for sensitive detection of copper ion.

    Science.gov (United States)

    Tang, Sheng; Chang, Yuepeng; Chia, Guo Hui; Lee, Hian Kee

    2015-07-23

    Copper is an important heavy metal in various biological processes. Many methods have been developed for detecting of copper ions (Cu(2+)) in aqueous samples. However, an easy, cheap, selective and sensitive method is still desired. In this study, a selective extraction-release-catalysis approach has been developed for sensitive detection of copper ion. Ethylenediaminetetraacetic acid (EDTA) chelated with nickel ion (Ni(2+)) were intercalated in a layered double hydroxide via a co-precipitation reaction. The product was subsequently applied as sorbent in dispersive solid-phase extraction for the enrichment of Cu(2+) at pH 6. Since Cu(2+) has a stronger complex formation constant with EDTA, Ni(2+) exchanged with Cu(2+) selectively. The resulting sorbent containing Cu(2+) was transferred to catalyze the 3,3',5,5'-tetramethylbenzidine oxidation reaction, since Cu(2+) could be released by the sorbent effectively and has high catalytic ability for the reaction. Blue light emitted from the oxidation product was measured by ultraviolet-visible spectrophotometry for the determination of Cu(2+). The extraction temperature, extraction time, and catalysis time were optimized. The results showed that this method provided a low limit of detection of 10nM, a wide linear range (0.05-100μM) and good linearity (r(2)=0.9977). The optimized conditions were applied to environmental water samples. Using Cu(2+) as an example, this work provided a new and interesting approach for the convenient and efficient detection of metal cations in aqueous samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Novel Pb2+ ion imprinted polymers based on ionic interaction via synergy of dual functional monomers for selective solid-phase extraction of Pb2+ in water samples.

    Science.gov (United States)

    Cai, Xiaoqiang; Li, Jinhua; Zhang, Zhong; Yang, Fangfang; Dong, Ruichen; Chen, Lingxin

    2014-01-08

    A novel kind of Pb(2+) ion imprinted polymers (IIPs) was prepared based on ionic interactions via the synergy of dual functional monomers of methacrylic acid and vinyl pyridine for selective solid-phase extraction (SPE) of Pb(2+) in water samples. Suspension polymerization was employed for the formation of template Pb(2+)/monomer complex by self-assembly in the presence of ethylene glycol dimethacrylate cross-linker. The resulted Pb(2+) IIPs showed fast kinetics, high binding capacity, and the adsorption processes obeyed intraparticle diffusion kinetics and Langmuir isotherm models. The IIPs displayed excellent selectivity toward Pb(2+) over other metal ions such as Cu(2+), Cd(2+), Zn(2+), and Mn(2+) with selective coefficients above 30, as well as high anti-interference ability for Pb(2+) confronting with common coexisting various ions. Through 10 adsorption-desorption cycles, the reusable IIPs exhibited a good recoverability with the standard error within 5%. These features suggested the IIPs were ideal candidates for extraction and removal of Pb(2+) ions. Consequently, the IIPs were utilized as SPE sorbents and related parameters were optimized. An excellent linearity was presented in the range of 0.2-50 μg L(-1) (R(2) = 0.9998), as well as the limits of detection and quantification were achieved of 0.06 and 0.19 μg L(-1), respectively. A good repeatability was obtained with the relative standard deviation of 2.8%. Furthermore, real water samples were successfully analyzed and satisfactory recoveries varying from 95.5 to 104.6% were attained. The IIPs-SPE demonstrated potential application perspectives for rapid and high-effective cleanup and enrichment of trace Pb(2+) ions in complicated matrices.

  18. Solvent extraction of the ion-pairs of chromium(VI) and molybdenum(VI) with trioctylmethylammonium chloride and benzyldimethylcetylammonium chloride.

    Science.gov (United States)

    Ohashi, K; Shikina, K; Nagatsu, H; Ito, I; Yamamoto, K

    1984-11-01

    The number of capriquat molecules per chromium(VI) atom in the chromate-capriquat ion-association complex has been found to be between one and two. The distribution ratio in the extraction of chromium(VI) with capriquat is dependent on the dielectric constant of the organic solvent, with a minimum at a dielectric constant of about 8. The absorption spectra of the ion-pair extracted into cyclohexane, carbon tetrachloride, benzene and n-butanol are very similar to that of chromate in aqueous solution. The absorption spectra of the chromium(VI)-capriquat extracts in these organic solvents gradually change to an absorption spectrum similar to that of HCrO(4)(-) in aqueous solution. Chromium(VI)-capriquat extracted into chloroform and 1,2-dichloroethane gives absorption spectra similar to that of HCrO(4)(-)in aqueous medium. The chromium(VI)-capriquat species extracted into 1,2-dichloroethane may be (Q(+))(2).CrO(4)(2-)(H(2)O)(n). In contrast, chromium(VI) is extracted with capriquat into the other organic solvents from ammoniacal medium as a mixture of (Q(+))(2).CrO(4)(2-)(H(2)O)(n) and Q(+).NH(4)(+).CrO(4)(2-)(H(2)O)(n). The spectral change is ascribed to the change of the extracted species from (Q(+))(2).CrO(4)(2-)(H(2)O)(n) and Q(+)NH(4)(+).CrO(4)(-)(H(2)O)(n) to Q(+).HCrO(4)(2-)(H(2)O)(n-1). The chromium(VI)-zephiramine species extracted is formulated as (Q(+), NH(4)(+))(2)CrO(4)(2-)(H(2)O)(n).(Q(+).Cl(-))(m). Molybdenum(VI) is extracted with capriquat into the same organic solvents as a mixture of (Q(+))(2).MoO(4)(2-)(H(2)O)(n) and Q(+).NH(4)(+).MoO(4)(2-).(H(2)O)(n).

  19. A novel lead imprinted polymer as the selective solid phase for extraction and trace detection of lead ions by flame atomic absorption spectrophotometry: Synthesis, characterization and analytical application

    Directory of Open Access Journals (Sweden)

    Homeira Ebrahimzadeh

    2017-05-01

    Full Text Available A novel ion imprinted polymer as the selective solid phase combined with flame atomic absorption spectrometry (FAAS was applied for preconcentration and determination of lead in real samples. In the first step, Pb(II-IIP was synthesized by copolymerization of 2-vinyl pyridine as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, 2,2-azobisisobutyronitrile as the initiator that imprinted with Pb(II as the template ion, 2-amino pyridine as the ligand. Subsequently, the imprinted Pb(II was completely removed by leaching the dried and powdered imprinted polymer with HCl (2 mol L−1. This polymer was characterized by Fourier Transform Infrared (FT-IR spectrometer. The effect of different variables on the extraction efficiency such as type and volume of eluent for extraction, solution’s pH for adsorption, sorption and desorption times was evaluated. Under the optimum conditions: type of eluent, HCl (2 mol L−1; volume of eluent, 5 mL; solution’s pH for sorption, 5; sorption time, 90 min; desorption time, 125 min and breakthrough volume of 750 mL were obtained. Preconcentration factor of the method was about 150. The limit of detection was obtained 0.75 μg L−1 and a dynamic linear range (DLR of 3–150 μg L−1 was found. The maximum sorption retention capacity of Pb(II ions on the imprinted polymer was 85.6 mg g−1. The prepared ion-imprinted polymer particles have an increased selectivity toward Pb(II ions over a range of competing metal ions with the same charge and similar ionic radius. Performance of the present method was evaluated for extraction and determination of Pb(II in water samples at microgram per liter concentration and satisfactory results were obtained (RSD = 2.7%.

  20. Quantitative determination of sotolon, maltol and free furaneol in wine by solid-phase extraction and gas chromatography-ion-trap mass spectrometry.

    Science.gov (United States)

    Ferreira, Vicente; Jarauta, Idoia; López, Ricardo; Cacho, Juan

    2003-08-22

    A method for the analytical determination of sotolon [4,5-dimethyl-3-hydroxy-2(5H)-furanone], maltol [3-hydroxy-2-methyl-4H-pyran-4-one] and free furaneol [2,5-dimethyl-4-hydroxy-3(2H)-furanone] in wine has been developed. The analytes are extracted from 50 ml of wine in a solid-phase extraction cartridge filled with 800 mg of LiChrolut EN resins. Interferences are removed with 15 ml of a pentane-dichloromethane (20:1) solution, and analytes are recovered with 6 ml of dichloromethane. The extract is concentrated up to 0.1 ml and analyzed by GC-ion trap MS. Maltol and sotolon were determined by selected ion storage of ions in the m/z ranges 120-153 and 79-95, using the ions m/z 126 and 83 for quantitation, respectively. Furaneol was determined by non-resonant fragmentation of the m/z 128 mother ion and subsequent analysis of the m/z 81 ion. The detection limits of the method are in all cases between 0.5 and 1 microg l(-1), well below the olfactory thresholds of the compounds. The precision of the method is in the 4-5% range for levels in wine around 20 microg l(-1). Linearity holds at least up to 400 microg l(-1), and is satisfactory in all cases. The recoveries of maltol and sotolon are constant (70 and 64%, respectively) and do not depend on the type of wine. On the contrary, in the case of furaneol, red wines show constant and high recoveries (97%), while the recoveries on white wines range between 30 and 80%. Different experiments showed that this behavior is probably due to the existence of complexes formed between furaneol and sulphur dioxide or catechols. Sensory experiments confirmed that the complexed forms found in white wines are not perceived by orthonasal olfaction, and that the furaneol determined by the method can be considered as the free and odor-active fraction.

  1. Detailed beam and plasma measurements on the vessel for extraction and source plasma analyses (VESPA) Penning H{sup −} ion source

    Energy Technology Data Exchange (ETDEWEB)

    Lawrie, S. R., E-mail: scott.lawrie@stfc.ac.uk [STFC ISIS Pulsed Spallation Neutron and Muon Facility, Rutherford Appleton Laboratory, Harwell, Oxford (United Kingdom); John Adams Institute of Accelerator Science, University of Oxford, Oxford (United Kingdom); Faircloth, D. C.; Letchford, A. P.; Whitehead, M. O.; Wood, T. [STFC ISIS Pulsed Spallation Neutron and Muon Facility, Rutherford Appleton Laboratory, Harwell, Oxford (United Kingdom)

    2016-02-15

    A vessel for extraction and source plasma analyses (VESPA) is operational at the Rutherford Appleton Laboratory (RAL). This project supports and guides the overall ion source R&D effort for the ISIS spallation neutron and muon facility at RAL. The VESPA produces 100 mA of pulsed H{sup −} beam, but perveance scans indicate that the source is production-limited at extraction voltages above 12 kV unless the arc current is increased. A high resolution optical monochromator is used to measure plasma properties using argon as a diagnostic gas. The atomic hydrogen temperature increases linearly with arc current, up to 2.8 eV for 50 A; whereas the electron temperature has a slight linear decrease toward 2.2 eV. The gas density is 10{sup 21} m{sup −3}, whilst the electron density is two orders of magnitude lower. Densities follow square root relationships with arc current, with gas density decreasing whilst electron (and hence ion) density increases. Stopping and range of ions in matter calculations prove that operating a high current arc with an argon admixture is extremely difficult because cathode-coated cesium is heavily sputtered by argon.

  2. Online Capacity Estimation of Lithium-Ion Batteries Based on Novel Feature Extraction and Adaptive Multi-Kernel Relevance Vector Machine

    Directory of Open Access Journals (Sweden)

    Yang Zhang

    2015-11-01

    Full Text Available Prognostics is necessary to ensure the reliability and safety of lithium-ion batteries for hybrid electric vehicles or satellites. This process can be achieved by capacity estimation, which is a direct fading indicator for assessing the state of health of a battery. However, the capacity of a lithium-ion battery onboard is difficult to monitor. This paper presents a data-driven approach for online capacity estimation. First, six novel features are extracted from cyclic charge/discharge cycles and used as indirect health indicators. An adaptive multi-kernel relevance machine (MKRVM based on accelerated particle swarm optimization algorithm is used to determine the optimal parameters of MKRVM and characterize the relationship between extracted features and battery capacity. The overall estimation process comprises offline and online stages. A supervised learning step in the offline stage is established for model verification to ensure the generalizability of MKRVM for online application. Cross-validation is further conducted to validate the performance of the proposed model. Experiment and comparison results show the effectiveness, accuracy, efficiency, and robustness of the proposed approach for online capacity estimation of lithium-ion batteries.

  3. An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

    NARCIS (Netherlands)

    Peters, S.; Kaal, E.; Horsting, I.; Janssen, H.-G.

    2012-01-01

    A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing ‘Micro-extraction in packed sorbent’ (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve

  4. Carboxylated graphene oxide/polyvinyl chloride as solid-phase extraction sorbent combined with ion chromatography for the determination of sulfonamides in cosmetics.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke; Luo, Zhibin; Liu, Zhe; Shao, Yijuan; He, Wanwen; Deng, Jianchao; Luo, Xingling

    2015-08-12

    A carboxylated graphene oxide/polyvinyl chloride (CGO/PVC) material was prepared as a sorbent for the selective extraction of sulphonamides from complex sample. After being dispersed in buffer solution, sample was transferred into the prefabricated solid-phase extraction (SPE) column, which integrated extraction and cleanup into one single-step. A multi-response optimization based on the Box-Behnken design was used to optimize factors affecting extraction efficiency. Compared with the commonly commercial sorbents including MCX, WCX and C18, CGO/PVC hybrid material had higher extraction selectivity and capacity to sulphonamides. The limits of detection and quantification for seven target compounds were in the range of 3.4-7.1 μg/L and 11.4-23.7 μg/L, respectively. The self-assembly SPE cartridge was successfully used to enrich seven analytes in anti-acne cosmetics prior to ion chromatography detection with good recoveries of 87.8-102.0% and relative standard deviations of 1.2-6.4%, implying that this method was suitable for routine analysis of cosmetics. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. PIXiE: an algorithm for automated ion mobility arrival time extraction and collision cross section calculation using global data association.

    Science.gov (United States)

    Ma, Jian; Casey, Cameron P; Zheng, Xueyun; Ibrahim, Yehia M; Wilkins, Christopher S; Renslow, Ryan S; Thomas, Dennis G; Payne, Samuel H; Monroe, Matthew E; Smith, Richard D; Teeguarden, Justin G; Baker, Erin S; Metz, Thomas O

    2017-09-01

    Drift tube ion mobility spectrometry coupled with mass spectrometry (DTIMS-MS) is increasingly implemented in high throughput omics workflows, and new informatics approaches are necessary for processing the associated data. To automatically extract arrival times for molecules measured by DTIMS at multiple electric fields and compute their associated collisional cross sections (CCS), we created the PNNL Ion Mobility Cross Section Extractor (PIXiE). The primary application presented for this algorithm is the extraction of data that can then be used to create a reference library of experimental CCS values for use in high throughput omics analyses. We demonstrate the utility of this approach by automatically extracting arrival times and calculating the associated CCSs for a set of endogenous metabolites and xenobiotics. The PIXiE-generated CCS values were within error of those calculated using commercially available instrument vendor software. PIXiE is an open-source tool, freely available on Github. The documentation, source code of the software, and a GUI can be found at https://github.com/PNNL-Comp-Mass-Spec/PIXiE and the source code of the backend workflow library used by PIXiE can be found at https://github.com/PNNL-Comp-Mass-Spec/IMS-Informed-Library . erin.baker@pnnl.gov or thomas.metz@pnnl.gov. Supplementary data are available at Bioinformatics online.

  6. Enhanced light extraction efficiency of chip-on board light-emitting diodes through micro-lens array fabricated by ion wind

    Science.gov (United States)

    Chu, Jingcao; Lei, Xiang; Wu, Jiading; Peng, Yang; Liu, Sheng; Yang, Qian; Zheng, Huai

    2017-03-01

    Low light extraction efficiency (LEE) is a key challenge of chip-on board (COB) packaging light-emitting diodes (LEDs). In this paper, a facile preparation of micro-lens array was proposed based on the ion wind patterning. The geometries and sizes of the micro-lens arrays were controlled through adjusting the voltage parameter of the ion wind generation. Consequently, the micro-lens array with the diameter of 180 μm and the gap distance of 15 μm has been fabricated. Benefitting from this micro-lens array, the LEE of COB packaging LEDs was enhanced by 9%. This facile fabrication of micro-lens array would be a promising method to improve the LEE of COB packaging LEDs.

  7. Thermal and electrostatic simulations of the diagnostic calorimeter for the source for production of ion of deuterium extracted from RF plasma beam.

    Science.gov (United States)

    Serianni, G; Dalla Palma, M; De Muri, M; Fasolo, D; Pasqualotto, R; Pomaro, N; Rizzolo, A; Tollin, M

    2012-02-01

    To study and optimise negative ion production for the ITER neutral beam injectors, a test facility is under construction in Padova with the aim of testing beam characteristics and to verify the source proper operation. The instrumented calorimeter STRIKE (short-time retractable instrumented kalorimeter experiment) is being developed to characterise the SPIDER (Source for Production of Ion of Deuterium Extracted from RF plasma) beam during short operations. The paper presents an investigation of the response of STRIKE measurement systems. It results that biasing is necessary to cope with the influence of secondary electrons on current measurements; moreover, despite the discretisation of the recorded thermal patterns introduced by the pixels of thermal cameras, a sufficient spatial resolution is expected.

  8. Using the Orbit Tracking Code Z3CYCLONE to Predict the Beam Produced by a Cold Cathode PIG Ion Source for Cyclotrons under DC Extraction

    CERN Document Server

    Forringer, Edward

    2005-01-01

    Experimental measurements of the emittance and luminosity of beams produced by a cold-cathode Phillips Ionization Guage (PIG) ion source for cyclotrons under dc extraction are reviewed. (The source being studied is of the same style as ones that will be used in a series of 250 MeV proton cyclotrons being constructed for cancer therapy by ACCEL Inst, Gmbh, of Bergisch Gladbach, Germany.) The concepts of 'plasma boundary' and 'plasma temperature' are presented as a useful set of parameters for describing the initial conditions used in computational orbit tracking. Experimental results for r-pr and z-pz emittance are compared to predictions from the MSU orbit tracking code Z3CYCLONE with results indicating that the code is able to predict the beam produced by these ion sources with adequate accuracy such that construction of actual cyclotrons can proceed with reasonably prudent confidence that the cyclotron will perform as predicted.

  9. Quantification of Tetramethylenedisulfotetramine (TETS) in Various Food Matrices by Solid Phase Extraction Liquid ChromatographyIon Trap Mass Spectrometry

    Science.gov (United States)

    2017-04-01

    used to deliberately contaminate food or water . TETS is not absorbed through the skin; the most common route of exposure is ingestion of...TETS in various complex food matrices. TETS is a relatively persistent environmental contaminant due to its high stability in water . This extraction...QUANTIFICATION OF TETRAMETHYLENEDISULFOTETRAMINE (TETS) IN VARIOUS FOOD MATRICES BY SOLID-PHASE EXTRACTION

  10. Antibacterial activity of the lactoperoxidase system combined with edible Laminaria hot-water extract as a source of halide ions.

    Science.gov (United States)

    Shin, Kouichirou; Nakano, Manabu; Yamauchi, Koji; Toida, Tomohiro; Iwatsuki, Keiji

    2012-01-01

    Hot-water extracts prepared from nine out of 12 samples of dried edible Laminaria reduced the viable numbers of Aggregatibacter actinomycetemcomitans, Staphylococcus aureus, and Esherichia coli below the detection limit after incubation for 5 min when combined with lactoperoxidase, glucose oxidase, and glucose. Some extracts showed higher bactericidal activity and a higher OI(-) concentration in the assay mixture after ultrafiltration.

  11. On-line coupling of solid-phase extraction with mass spectrometry for the analysis of biological samples. II. Determination of clenbuterol in urine using multiple-stage mass spectrometry in an ion-trap mass spectrometer

    NARCIS (Netherlands)

    van Hout, MWJ; Hofland, CM; Niederlander, HAG; de Jong, GJ

    2000-01-01

    Solid-phase extraction (SPE) was coupled to ion-trap mass spectrometry to determine clenbuterol in urine. For SPE a cartridge exchanger was used and, after extraction, the eluate was directly introduced into the mass spectrometer, For two types of cartridges, i.e. C-18 and polydivinylbenzene (PDVB),

  12. Characterization of cigarette tobacco by direct electrospray ionization-ion trap mass spectrometry (ESI-ITMS) analysis of the aqueous extract--a novel and simple approach.

    Science.gov (United States)

    Ng, Lay-Keow; Lafontaine, Pierre; Vanier, Micheline

    2004-12-01

    In support of the efforts to combat smuggling, as well as illegal sale and distribution of cigarettes, an analytical approach for the characterization of tobacco has been proposed and evaluated. It involves aqueous extraction of the filler tobaccos followed by direct analysis of the extracts by electrospray ionization-ion trap mass spectrometry (ESI-ITMS) in the negative mode. Typically, the deprotonated ions, [M - H](-), of organic acids (malic, citric, caffeic, quinic acid) and polyphenols (chlorogenic acid, rutin, scopoletin) were detected. MS/MS spectra of the ion at m/z 191, which is the [M - H](-) of quinic acid, citric acid, and scopoletin, and a fragment ion of chlorogenic acid were acquired. Significant differences in the MS and MS/MS spectra were observed between counterfeit samples and the corresponding authentic brand name cigarettes. Analysis of 25 commercial cigarettes showed that straight Virginia blends were readily distinguished from the blended products containing different tobacco types (Virginia, burley, and Oriental). The former exhibited consistently higher relative abundances of m/z 353 (chlorogenic acid) to m/z 133 (malic acid) in the MS spectra (0.9-1.2 vs 0.4-0.6) and higher intensity ratios of m/z 176 (scopoletin) to m/z 173 (0.4-0.8 vs 0.1-0.3) and of m/z 127 (quinic acid) to m/z 173 (0.7-1.0 vs 0.3-0.5) in the MS/MS spectra. Evidence is presented to demonstrate that the spectral differences were related not only to the tobacco type (Virginia, burley and Oriental) but also to the tobacco part (stem, lamina) used in the manufacture of the cigarettes.

  13. Naturally occurring glucosinolates in plant extracts of rocket salad (Eruca sativa L.) identified by liquid chromatography coupled with negative ion electrospray ionization and quadrupole ion-trap mass spectrometry.

    Science.gov (United States)

    Cataldi, Tommaso R I; Rubino, Alessandra; Lelario, Filomena; Bufo, Sabino A

    2007-01-01

    A method for the comprehensive profiling of intact glucosinolates (GLSs), major and minor, occurring in leaves and seeds of rocket salad (Eruca sativa L.) is presented using optimized reversed-phase liquid chromatography (RP-LC) with electrospray ionization (ESI) ion trap mass spectrometry (ITMS). ESI-ITMS in the negative mode was confirmed to be very suitable to analyze these compounds in crude extracts. After extraction from the plant material with methanol/water (70:30 v/v) at 70 degrees C, the analytes of interest were separated on a C18 column using an eluent acidified with formic acid (0.1%) and modified with acetonitrile. All the GLSs found in leaves of rocket salad gave good signals corresponding to the deprotonated precursor ion, [M-H]-. Although the mass spectra also exhibited an analytically important non-covalent adduct ion at [2M-H]-, the structures of glucosinolates were confirmed by extensive sequential MS analysis, thereby substantially improving the identification of unknown compounds. The results obtained not only revealed in leaves of E. sativa at least twelve species of GLSs including seven aliphatic compounds (glucoraphanin with [M-H]- at m/z ratio of 436, glucoerucin at m/z 420, 4-mercaptobutyl-GLS at m/z 406, progoitrin/epiprogoitrin at m/z 388, sinigrin at m/z 358, 4-methylpentyl- and n-hexyl-GLS at m/z 402) and three indole glucosinolates (i.e., three N-heterocyclic compounds: 4-hydroxyglucobrassicin and 5-hydroxyglucobrassicin at m/z 463, and 4-methoxy-glucobrassicin at m/z 477), but also two structurally related compounds containing one intermolecular disulfide linkage (4-(beta-D-glucopyranosyldisulfanyl)butyl-GLS at m/z 600 and a dimeric 4-mercaptobutyl-GLS at m/z 811). This latter symmetric disulfide was previously considered as an artefact formed during extraction of GLSs from vegetative tissues. Glucosinolates were detected in the leaves with a wide range of contents (10-200 micromol/g) and a great variation in the composition. Only

  14. Development of a system for monitoring the shape, position, and intensity of the extracted relativistic ion beam at the Nuclotron-M accelerator complex at JINR

    Science.gov (United States)

    Vasilev, S. E.; Vishnevskiy, A. V.; Kadykov, M. G.; Makankin, A. M.; Tyutyunnikov, S. I.; Shurygin, A. A.

    2014-11-01

    Test samples of detectors and electronics for them constructed for the purpose of monitoring the "intense" relativistic ion beams extracted from the accelerator of the Nuclotron-M accelerator complex in real time are described. The system was tested in a series of acceleration runs with deuteron beams with an intensity of up to 1010 1/s and beams of carbon nuclei. The system allows one to perform multiple measurements of the two-dimensional distribution of the beam intensity in the plane perpendicular to it and the beam position in this plane during the beam dump and measure the two-dimensional distribution of the target irradiation dose after each beam dump.

  15. Exploiting 1,2,3-Triazolium Ionic Liquids for Synthesis of Tryptanthrin and Chemoselective Extraction of Copper(II Ions and Histidine-Containing Peptides

    Directory of Open Access Journals (Sweden)

    Hsin-Yi Li

    2016-10-01

    Full Text Available Based on a common structural core of 4,5,6,7-tetrahydro[1,2,3]triazolo[1,5-a]pyridine, a number of bicyclic triazolium ionic liquids 1–3 were designed and successfully prepared. In our hands, this optimized synthesis of ionic liquids 1 and 2 requires no chromatographic separation. Also in this work, ionic liquids 1, 2 were shown to be efficient ionic solvents for fast synthesis of tryptanthrin natural product. Furthermore, a new affinity ionic liquid 3 was tailor-synthesized and displayed its effectiveness in chemoselective extraction of both Cu(II ions and, for the first time, histidine-containing peptides.

  16. Exploiting 1,2,3-Triazolium Ionic Liquids for Synthesis of Tryptanthrin and Chemoselective Extraction of Copper(II) Ions and Histidine-Containing Peptides.

    Science.gov (United States)

    Li, Hsin-Yi; Chen, Chien-Yuan; Cheng, Hui-Ting; Chu, Yen-Ho

    2016-10-13

    Based on a common structural core of 4,5,6,7-tetrahydro[1,2,3]triazolo[1,5-a]pyridine, a number of bicyclic triazolium ionic liquids 1-3 were designed and successfully prepared. In our hands, this optimized synthesis of ionic liquids 1 and 2 requires no chromatographic separation. Also in this work, ionic liquids 1, 2 were shown to be efficient ionic solvents for fast synthesis of tryptanthrin natural product. Furthermore, a new affinity ionic liquid 3 was tailor-synthesized and displayed its effectiveness in chemoselective extraction of both Cu(II) ions and, for the first time, histidine-containing peptides.

  17. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 2: migration from paperboard into dry foods: interpretation of chromatograms.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    Mineral oil hydrocarbons are complex as well as varying mixtures and produce correspondingly complex chromatograms (on-line HPLC-GC-FID as described in Part 1): mostly humps of unresolved components are obtained, sometimes with sharp peaks on top. Chromatograms may also contain peaks of hydrocarbons from other sources which need to be subtracted from the mineral oil components. The review focuses on the interpretation and integration of chromatograms related to food contamination by mineral oil from paperboard boxes (off-set printing inks and recycled fibers), if possible distinguishing between various sources of mineral oil. Typical chromatograms are shown for relevant components and interferences as well as food samples encountered on the market. Details are pointed out which may provide relevant information. Integration is shown for examples of paperboard packaging materials as well as various foods. Finally the uncertainty of the analysis and limit of quantitation are discussed for specific examples. They primarily result from the interpretation of the chromatogram, manually placing the baseline and cuts for taking off extraneous components. Without previous enrichment, the limit of quantitation is between around 0.1 mg/kg for foods with a low fat content and 2.5 mg/kg for fats and oils. The measurement uncertainty can be kept clearly below 20% for most samples.

  18. Liquid-liquid extraction of metal ions, DFT and TD-DFT analysis of some 1,2,4-triazole Schiff Bases with high selectivity for Pb(II) and Fe(II)

    Science.gov (United States)

    Khoutoul, Mohamed; Lamsayah, Morad; Al-blewi, Fawzia F.; Rezki, Nadjet; Aouad, Mohamed Reda; Mouslim, Messali; Touzani, Rachid

    2016-06-01

    Liquid-liquid extraction of metal ions using some 1,2,4-triazole Schiff base derivatives as new extractants was studied. Fe2+, Zn2+, Cu2+, Co2+, Cd2+ and Pb2+ were extracted from the aqueous phase into the organic phase and the extractability for each metal ion was determined by atomic absorption. Interestingly, a competitive extraction was also investigated and then examined at different pH in order to explore the effect of the different substituent groups on metal extraction. Accordingly, high selectivity towards Fe2+ (90.1%) and Pb2+ (94.3%) provided respectively by the presence of electron withdrawing group and electron donor group was attained. In addition, geometry optimizations of the ground and excited-states of the ligands in order to get better insight into the geometry and the electronic structure were carried out by means of DFT and TD-DFT calculations.

  19. Suitability of selective pressurized liquid extraction combined with gas chromatography-ion-trap tandem mass spectrometry for the analysis of polybrominated diphenyl ethers.

    Science.gov (United States)

    Losada, S; Parera, J; Abalos, M; Abad, E; Santos, F J; Galceran, M T

    2010-09-23

    A one-step extraction and clean-up method using pressurized liquid extraction (PLE) (selective PLE) combined with gas chromatography-ion-trap tandem mass spectrometry (GC-ITMS-MS) was evaluated for the analysis of polybrominated diphenyl ethers (from tri- to hepta-PBDEs) at low concentrations in fish and shellfish samples. To this end, the performance of an on-line PLE extraction/clean-up method and of a classical Soxhlet extraction and clean-up method using a multi-layer modified silica column were compared. The two sample treatment methods provided similar results, although an important reduction in the sample treatment time (40 min per sample) was achieved using the selective PLE method. In addition, the suitability of the PLE combined with GC-ITMS-MS method was evaluated by comparing the results obtained in the analysis of fish samples with those obtained by gas chromatography-high resolution mass spectrometry (GC-HRMS). Good agreement between both techniques was obtained with differences between the mean values of less than 16%. The selective PLE method coupled to GC-ITMS-MS produced accurate results for PBDE determination with low limits of detection (1.0-16.8 pg g(-1) wet weight) and quantification (3.1-51 pg g(-1) wet weight) as well as good precision (RSD<16%). This method has been applied to the analysis of PBDEs in fish and shellfish samples collected at fish markets in Catalonia (NE Spain).

  20. Speciation analysis of arsenic in prenatal and children's dietary supplements using microwave-enhanced extraction and ion chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Wolle, Mesay M; Rahman, G M Mizanur; Kingston, H M Skip; Pamuku, Matt

    2014-03-25

    A study was conducted to develop a microwave-enhanced extraction method for the determination of arsenic species in prenatal and children's dietary supplements prepared from plant materials. The method was optimized by evaluating the efficiency of various solutions previously used to extract arsenic from the types of plant materials used in the dietary supplement formulations. A multivitamin standard reference material (NIST SRM 3280) and a prenatal supplement sample were analyzed in the method optimization. The identified optimum conditions were 0.25 g of sample, 5 mL of 0.3 mol L(-1) orthophosphoric acid (H3PO4) and microwave heating at 90 °C for 30 min. The extracted arsenic was speciated by cation exchange ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP-MS). The method detection limit (MDL) for the arsenic species was in the range 2-8 ng g(-1). Ten widely consumed prenatal and children's dietary supplements were analyzed using the optimized protocol. The supplements were found to have total arsenic in the concentration range 59-531 ng g(-1). The extraction procedure recovered 61-92% of the arsenic from the supplements. All the supplementary products were found to contain arsenite (As(3+)) and dimethylarsinic acid (DMA). Arsenate (As(5+)) was found in two of the supplements, and an unknown specie of arsenic was detected in one product. The results of the analysis were validated using mass balance by comparing the sum of the extracted and non-extracted arsenic with the total concentration of the element in the corresponding samples.

  1. Observing Effects of Calcium/Magnesium Ions and pH Value on the Self-Assembly of Extracted Swine Tendon Collagen by Atomic Force Microscopy

    Directory of Open Access Journals (Sweden)

    Xuan Song

    2017-01-01

    Full Text Available Self-assembly of extracted collagen from swine trotter tendon under different conditions was firstly observed using atomic force microscopy; then the effects of collagen concentration, pH value, and metal ions to the topography of the collagen assembly were analyzed with the height images and section analysis data. Collagen assembly under 0.1 M, 0.2 M, 0.3 M CaCl2, and MgCl2 solutions in different pH values showed significant differences (P < 0.05 in the topographical properties including height, width, and roughness. With the concentration being increased, the width of collagen decreased significantly (P < 0.05. The width of collagen fibers was first increased significantly (P < 0.05 and then decreased with the increasing of pH. The collagen was assembled with network structure on the mica in solution with Ca2+ ions. However, it had shown uniformed fibrous structure with Mg2+ ions on the new cleaved mica sheet. In addition, the width of collagen fibrous was 31~58 nm in solution with Mg2+ but 21~50 nm in Ca2+ solution. The self-assembly collagen displayed various potential abilities to construct fibers or membrane on mica surfaces with Ca2+ ions and Mg2+ irons. Besides, the result of collagen self-assembly had shown more relations among solution pH value, metal ions, and collagen molecular concentration, which will provide useful information on the control of collagen self-assembly in tissue engineering and food packaging engineering.

  2. Silica chemically bonded N-propyl kriptofix 21 and 22 with immobilized palladium nanoparticles for solid phase extraction and preconcentration of some metal ions

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, Mehrorang, E-mail: m_ghaedi@mail.yu.ac.ir [Chemistry Department, Yasouj University, Yasouj, 75914-353 (Iran, Islamic Republic of); Niknam, Khodabakhsh, E-mail: niknam@pgu.ac.ir [Chemistry Department, Faculty of Sciences, Persian Gulf University, Bushehr, 75169 (Iran, Islamic Republic of); Zamani, Saeed; Abasi Larki, Habib [Chemistry Department, Islamic Azad University, Omidiyeh Branch, Omidiyeh (Iran, Islamic Republic of); Roosta, Mostafa [Chemistry Department, Yasouj University, Yasouj, 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2013-08-01

    Silica gel chemically bonded N-propyl kriptofix 21 (SBNPK 21) and N-propyl kriptofix 22 (SBNPK 22) and subsequently immobilized with palladium nanoparticles (PNP-SBNPK 21 and PNP-SBNPK 22) to produce two new complexing lipophilic materials. Then these novel sorbents were applied for the enrichment of some metal ions and their subsequent determination by flame atomic absorption spectroscopy (FAAS). The influences of the variables including pH, amount of solid phase, sample flow rate, eluent conditions and sample volume on the metal ion recoveries were investigated. The detection limit of proposed method was in the interval 2.1–2.3 and 1.7–2.8 ng mL{sup −1} for PNP-SBNPK 21 and PNP-SBNPK 22 respectively, while the preconcentration factor was 80 for two sorbents. The relative standard deviations of recoveries were between 1.23–1.31 and 1.28–1.49 for PNP-SBNPK 21 and PNP-SBNPK 22 respectively. The method has high sorption-preconcentration efficiency even in the presence of various interfering ions. Due to the reasonable selectivity of proposed method, the relative standard deviation of recoveries of all understudied metal ions in some complicated matrices was less than 3.0%. Highlights: • Highly selective sorbents for solid phase extraction were synthesized. • The method has been successfully applied for the determination of trace metals ions. • Excellent properties of the sorbent have been illustrated in detail.

  3. Usage of X-ray absorption spectroscopy and extractive fractionation in studies of the Cu (II and Zn (II ions in soils

    Directory of Open Access Journals (Sweden)

    Dina Nevidomskaya

    2014-12-01

    Full Text Available XANES spectroscopy is an effective method for the study of bonds between metals and soil components. The study of structural organization in different soil samples and soil phases saturated with Cu2+ and Zn2+ ions by using XANES allowed determining the mechanism of their interaction with soil phases and all the chemical bindings taken place in the course of this process. Changes in the structure of the metal ion, in particular breakdown of the symmetry of electron orbits of atoms, take place due to interaction with soil components. Application of this method demonstrated that the state of copper and zinc introduced in chernozem as oxides did not change after one year of incubation. Copper is absorbed after being introduced as soluble salts, and copper ions are incorporated in the octahedral and tetrahedral sites of minerals and bonded with humic materials at the expense of covalent bond and the formation of coordination humate copper complexes. Zinc included into octahedric structures of layered minerals and hydro(oxides can be inner-and outer-sphere adsorbed. It is shown that the action of the metal bound to soil components becomes weakened in case of increasing the Cu and Zn load (from 2000 to 10000 mg/kg especially applied in the form of soluble salts. Extractive fractionation of metal compounds in chernozem samples, artificially contaminated with copper and zinc salts serves as evidence of absorbing the applied Cu2+ ions by the soil organic matter and Zn2+ ions – by silicates, carbonates, and Fe-Mn oxides.

  4. Rapid analysis of pesticide residues in drinking water samples by dispersive solid-phase extraction based on multiwalled carbon nanotubes and pulse glow discharge ion source ion mobility spectrometry.

    Science.gov (United States)

    Zou, Nan; Gu, Kejia; Liu, Shaowen; Hou, Yanbing; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

    2016-03-01

    An analytical method based on dispersive solid-phase extraction with a multiwalled carbon nanotubes sorbent coupled with positive pulse glow discharge ion mobility spectrometry was developed for analysis of 30 pesticide residues in drinking water samples. Reduced ion mobilities and the mass-mobility correlation of 30 pesticides were measured. The pesticides were divided into five groups to verify the separation capability of pulse glow discharge in mobility spectrometry. The extraction conditions such as desorption solvent, ionic strength, conditions of adsorption and desorption, the amounts of multiwalled carbon nanotubes, and solution pH were optimized. The enrichment factors of pesticides were 5.4- to 48.7-fold (theoretical enrichment factor was 50-fold). The detection limits of pesticides were 0.01∼0.77 μg/kg. The linear range was 0.005-0.2 mg/L for pesticide standard solutions, with determination coefficients from 0.9616 to 0.9999. The method was applied for the analysis of practical and spiked drinking water samples. All results were confirmed by high-performance liquid chromatography with tandem mass spectrometry. The proposed method was proven to be a commendably rapid screening qualitative and semiquantitative technique for the analysis of pesticide residues in drinking water samples on site.

  5. A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

    2003-01-01

    A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

  6. Characterization of Anthocyanins in Perilla frutescens var. acuta Extract by Advanced UPLC-ESI-IT-TOF-MSn Method and Their Anticancer Bioactivity.

    Science.gov (United States)

    He, Yan-Kang; Yao, You-Yuan; Chang, Ya-Ning

    2015-05-19

    The anthocyanin extract from a domestic Perilla cultivar (Perilla frutescens var. acuta) were isolated and characterized with high mass accuracy and multi-dimensional fragmentation by means of ultra-performance liquid chromatography (UPLC) and electrospray ionization-ion trap-time of flight mass spectrometry analysis (ESI-IT-TOF-MSn). The new developed and applied LC-MS method focused on in-depth screening of anthocyanin compounds with similar structures which also provided a new approach of anthocyanin characterization without the use of external standards. Selective detection of interested anthocyanins was achieved utilizing extracted ion chromatogram (EIC) analysis, while MSn spectra were recorded to allow identification of the anthocyanin based on characteristic fragmentation patterns. Seven anthocyanins including one feruloyl (Cyanidin 3-O-feruloylglucoside-5-O-glucoside), two caffeoyl (Cyanidin 3-O-caffeoylglucoside-5-O-glucoside, Cyanidin 3-O-caffeoylglucoside-5-O-malonylglucoside) and four coumaroyl substituted anthocyanins (Cis-shisonin, Malonyl-cis-shisonin, Shisonin, and Malonyl-shisonin) were identified. Annexin-V FITC/PI flow cytometric assay was performed to analyze the influence of anthocyanin extract of P. frutescens var. acuta on cell apoptosis. The results suggested that Perilla anthocyanins can induce Hela cell apoptosis by a dose dependent manner.

  7. Characterization of Anthocyanins in Perilla frutescens var. acuta Extract by Advanced UPLC-ESI-IT-TOF-MSn Method and Their Anticancer Bioactivity

    Directory of Open Access Journals (Sweden)

    Yan-Kang He

    2015-05-01

    Full Text Available The anthocyanin extract from a domestic Perilla cultivar (Perilla frutescens var. acuta were isolated and characterized with high mass accuracy and multi-dimensional fragmentation by means of ultra-performance liquid chromatography (UPLC and electrospray ionization-ion trap-time of flight mass spectrometry analysis (ESI-IT-TOF-MSn. The new developed and applied LC-MS method focused on in-depth screening of anthocyanin compounds with similar structures which also provided a new approach of anthocyanin characterization without the use of external standards. Selective detection of interested anthocyanins was achieved utilizing extracted ion chromatogram (EIC analysis, while MSn spectra were recorded to allow identification of the anthocyanin based on characteristic fragmentation patterns. Seven anthocyanins including one feruloyl (Cyanidin 3-O-feruloylglucoside-5-O-glucoside, two caffeoyl (Cyanidin 3-O-caffeoylglucoside-5-O-glucoside, Cyanidin 3-O-caffeoylglucoside-5-O-malonylglucoside and four coumaroyl substituted anthocyanins (Cis-shisonin, Malonyl-cis-shisonin, Shisonin, and Malonyl-shisonin were identified. Annexin-V FITC/PI flow cytometric assay was performed to analyze the influence of anthocyanin extract of P. frutescens var. acuta on cell apoptosis. The results suggested that Perilla anthocyanins can induce Hela cell apoptosis by a dose dependent manner.

  8. Effet des extractibles sur la durabilité naturelle du duramen de cyprès

    OpenAIRE

    Mohareb, Ahmed; Sirmah, Peter; Desharnais, Lyne; Dumarçay, Stéphane; Pétrissans,Mathieu; Gérardin, Philippe

    2010-01-01

    International audience; Identification of extractives present in Cupressus lusitanica heartwood has been conducted using GC-MS analyses. The chromatogram of toluene/ethanol extracts indicated the presence of large amounts of benzaldehyde and numerous terpenic compounds such as cedrol, agathadiol, epimanool, bornyl acetate, α-cedrene and β-cedrene.* The effect of these extractives on the natural durability of cypress wood was investigated on heart wood blocks exposed to pure culture of Poria p...

  9. Selenium metabolomics in yeast using complementary reversed-phase/hydrophilic ion interaction (HILIC) liquid chromatography-electrospray hybrid quadrupole trap/Orbitrap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Arnaudguilhem, C.; Bierla, K.; Ouerdane, L.; Preud' homme, H. [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-inorganique et Environnement, UMR 5254, Helioparc, 2, Av. Pr. Angot, 64053 Pau (France); Yiannikouris, A. [Alltech Inc., 3031 Catnip Hill Pike, Nicholasville, KY (United States); Lobinski, R., E-mail: ryszard.lobinski@univ-pau.fr [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-inorganique et Environnement, UMR 5254, Helioparc, 2, Av. Pr. Angot, 64053 Pau (France); Chair of Analytical Chemistry, Warsaw University of Technology, 00-664 Warszawa (Poland)

    2012-12-13

    Highlights: Black-Right-Pointing-Pointer The use of bimodal chromatographic separation enlarged amount of compounds identified. Black-Right-Pointing-Pointer The method allowed the largest scale ever (>60 compounds) speciation analysis of selenium metabolites in Se-rich yeast. Black-Right-Pointing-Pointer The estimated concentration of compounds was given. - Abstract: A high efficiency chromatographic separation on a porous graphitic carbon stationary phase was developed for a large-scale separation of selenium metabolites in Se-rich yeast prior to their identification by electrospray hybrid quadrupole trap/Orbitrap mass spectrometry (Orbitrap MS{sup n}). The reversed-phase (RP) separation mode offered distinctly higher separation efficiency than the hydrophilic ion interaction (HILIC) mode. The latter was nevertheless complementary and useful to validate the detection of several compounds. The method allowed the detection of 64 metabolites including 30 Se-Se or Se-S conjugates (3 triple S/Se/S ones) and 14 selenoethers. 21 previously unreported metabolites were detected on the basis of the selenium isotopic pattern usually matched with the sub-ppm mass accuracy. 9 of these metabolites were subsequently identified using the multi-stage high mass accuracy (<5 ppm) mass spectrometry. The identified metabolites (and their groups) were quantified on-line by ICP-MS fitted with a frequency-matching generator allowing a quasi-uniform response over the large (20-90%) acetonitrile mobile phase concentration range. The morphology of HPLC-ICP-MS chromatograms was remarkably similar to that of HPLC multi-ion extracted ESI-MS chromatograms. The detection limits obtained by ICP MS and ESI MS were 1 and 2 ppb, respectively.

  10. On-line solid phase extraction using ion-pair microparticles combined with ICP-OES for the simultaneous preconcentration and determination of uranium and thorium

    Energy Technology Data Exchange (ETDEWEB)

    Yousefi, Seyed Reza; Zolfonoun, Ehsan [Nuclear Science and Technology Research Institute, Tehran (Iran, Islamic Republic of). NFCRS

    2016-07-01

    In this work, after on-line and in-situ solid phase extraction technique was used for the extraction and preconcentration of uranium and thorium from aqueous samples prior to inductively coupled plasma optical emission spectrometry (ICP-OES) determination. In this method, sodium hexafluorophosphate (as an ion-pairing agent) was added to the sample solution containing the cationic surfactant (dodecyltrimethylammonium bromide) and the complexing agent (dibenzoylmethane). A cloudy solution was formed as a result of formation of an ion pair between surfactant and hexafluorophosphate. The solid microparticles were passed through a microcolumn filter and the adsorbed microparticles were subsequently eluted with acid, which was directly introduced into the ICP-OES nebulizer. The main variables affecting the pre-concentration and determination steps of uranium and thorium were studied and optimized. Under the optimum conditions, the enhancement factors of 97 and 95 and the detection limits of 0.52 and 0.21 μg L{sup -1} were obtained for uranium and thorium, respectively.

  11. 一台14GHz CAPRICE型ECR离子源的束流引出%Ion Beam Extracted from a 14GHz ECRIS of CAPRICE Type

    Institute of Scientific and Technical Information of China (English)

    P.Sp(a)dtke; R.Lang; J.M(a)der; J.Roβbach; K.Tinschert; J.Stetson

    2007-01-01

    An ion beam extracted from an ECRIS suffers from the inhomogeneous distribution of cold electrons within the minimum B configuration,necessary to confine the plasma.Especially for higher ion currents,the space charge force is not negligible any more,and because of the nonlinear force,emittance growth will occur.Measurements of the profile and the emittance of the beam directly behind the source show the complicated correlation between extraction voltage and plasma density.The emittance has been measured with a pepper pot device to account for the inhomogeneous azimuthal distribution of the beam.These results indicate that further information about the profile is required.To visualize the beam profile a tantalum foil with a thickness of 20μm has been used for an electrical beam power between 10 and 50W.Looking on the back side of the foil with a CCD camera it is possible to record the profile in real time.As a more sensitive diagnostic tool viewing targets made from BaF has been used.Three dimensional computer simulations have been used to identify the reason for the structures,observed in measurements.

  12. Determination of melamine in milk and dairy products by microchip-based high-field asymmetric ion mobility spectrometry combined with solid-phase extraction.

    Science.gov (United States)

    Zhao, Wei-jun; Wang, Yonghuan; Li, Juan; Li, Ling-feng; Wang, Qi; Han, Ke; Zhang, Yuang; Li, Xin; Li, Peng; Luo, Jikui; Wang, Xiaozhi

    2015-12-01

    This article presents a method for sensitive, fast and quantitative determination of melamine in milk and dairy products using high-field asymmetric ion mobility spectrometry (FAIMS). The solid-phase extraction (SPE) technology was used for purification after the sample was extracted by organic solvents, and followed by the analysis of FAIMS. The measurement parameters and variables that affect the FAIMS detection have been investigated, and optimum conditions have been obtained as follows: the carrier gas flow rate is 1.6 L min(-1), the headspace sampler temperature is 150 °C, the pressure is 1 atm, and the humidity is 2.0 g m(-3). The results showed that the SPE-FAIMS method can detect melamine in samples with a concentration down to 0.1 mg kg(-1). The ion intensity has a linear relationship with melamine concentration in the range from 0.3 mg L(-1) to 25 mg L(-1), with a good linearity of 0.9975. The limits of detection (LOD) and limits of quantification (LOQ) are 0.1 mg kg(-1) and 0.3 mg kg(-1) in milk and dairy products, respectively, and the relative standard deviation is less than 8.0%. The results demonstrated that FAIMS has great potential as a powerful tool for food analysis and safety inspection.

  13. Extractive spectrophotometric determination of sulphonamide drugs in pure and pharmaceutical preparations through ion-pair formation with molybdenum(V thiocyanate in acidic medium

    Directory of Open Access Journals (Sweden)

    Faten A. Nour El-Dien

    2010-07-01

    Full Text Available A simple and sensitive extraction-spectrophotometric method is described for the determination of sulfonamide drugs, namely sulphamethoxazole, sulphaguanidine, sulphaquinoxaline, sulphametrole and sulphadimidine, in both pure form and in the dosage forms available in Egyptian markets. The method is based on ion-pair formation between the sulphonamides and Mo(V-thiocyanate inorganic complex in a sulphuric acid medium followed by extraction of the coloured ion-pairs with 1,2-dichloroethane. The optimum conditions are established. The method permits the determination of sulphonamide drugs over the concentration range of 5–50 μg ml−1. The Sandell sensitivity (S, molar absorptivity, correlation coefficient and regression equations, and limits of detection (LOD and quantification (LOQ are calculated. The law values of standard deviation (0.09–0.38 and relative standard deviation (0.10–0.550 reflect the accuracy and precision of the proposed method. The method is applicable for the assay of the investigated drugs in different dosage forms and the results are in good agreement with those obtained by the official pharmacopeial method.

  14. High performance liquid chromatography for the simultaneous analysis of penicillin residues in beef and milk using ion-paired extraction and binary water-acetonitrile mixture.

    Science.gov (United States)

    Kukusamude, Chunyapuk; Burakham, Rodjana; Chailapakul, Orawon; Srijaranai, Supalax

    2012-04-15

    An ion-paired extraction (IPE) has been developed for the analysis of penicillin antibiotics (penicillin G, oxacillin and cloxacillin) in beef and milk samples using tetrabutylammonium bromide (TBABr) as ion-pairing agent and binary water-acetonitrile as extractant. The factors affecting the IPE efficiency were optimized including solution pH, volume of acetonitrile (ACN), concentration of TBABr and electrolyte salt (NH(4))(2)SO(4). The optimum IPE conditions were 10 mmol L(-1) phosphate buffer pH 8, 2 mL of ACN, 6 mmol L(-1) of TBABr and 2.5 mL of saturated ammonium sulfate. Under the HPLC condition: an Xbridge™ C18 reversed-phase column, isocratic elution of 5 mmol L(-1) phosphate buffer (pH 6.6) and acetonitrile (75:25, v/v) and a flow rate of 1 mL min(-1), with UV detection at 215 nm, the separation of three penicillins was achieved within 10 min. Under the selected optimum conditions, the enhancement of 21-53 folds compared to that without preconcentration and limits of detection (LODs) of 1-2 ng mL(-1) were obtained. Good reproducibility was achieved with RSDpenicillin residues in beef and milk with LOD lower than the maximum residue limits.

  15. Capillary electrophoresis coupled with inductively coupled mass spectrometry as an alternative to cloud point extraction based methods for rapid quantification of silver ions and surface coated silver nanoparticles.

    Science.gov (United States)

    Qu, Haiou; Mudalige, Thilak K; Linder, Sean W

    2016-01-15

    Speciation and accurate quantification of ionic silver and metallic silver nanoparticles are critical to investigate silver toxicity and to determine the shelf-life of products that contain nano silver under various storage conditions. We developed a rapid method for quantification of silver ions and silver nanoparticles using capillary electrophoresis (CE) interfaced with inductively-coupled plasma mass spectrometry (ICPMS). The addition of 2-mercaptopropionylglycine (tiopronin) to the background electrolyte was used to facilitate the chromatographic separation of ionic silver and maintain the oxidation state of silver. The obtained limits of detection were 0.05 μg kg(-1) of silver nanoparticles and 0.03 μg kg(-1) of ionic silver. Nanoparticles of varied sizes (10-110 nm) with different surface coating, including citrate acid, lipoic acid, polyvinylpyrrolidone and bovine serum albumin (BSA) were successfully analyzed. Particularly good recoveries (>93%) were obtained for both ionic silver and silver nanoparticle in the presence of excess amount of BSA. The method was further tested with six commercially available dietary supplements which varied in concentration and matrix components. The summed values of silver ions and silver nanoparticles correlated well with the total silver concentration determined by ICPMS after acid digestion. This method can serve as an alternative to cloud point extraction technique when the extraction efficiency for protein coated nanoparticles is low.

  16. X-ray fluorescence analysis of trace metal ions following a preconcentration of metal-diethyldithiocarbamate complexes by homogeneous liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, Atsushi; Igarashi, Shukuro; Ueki, Yasuo [Ibaraki Univ., Hitachi (Japan). Faculty of Engineering; Yamaguchi, Hitoshi [National Research Inst. for Metals, Ibaraki (Japan)

    2000-11-01

    A homogeneous liquid-liquid extraction method for 36 metal ions with diethyldithiocarbamate was studied. As a result, 11 metal ions were extracted as metal-chelates. Under the experimental conditions, the maximum concentration factor was 500 (i.e., 0.1 mL of sedimented liquid phase was produced from 50 mL of aqueous phase). Moreover, the proposed method was utilized as a preconcentration method for X-ray fluorescence analysis of these metals. The recovery of each metal was ca. 97-100%. All calibration curves were linear over the range of 5.0 x 10{sup -7} mol L{sup -1} to 1.0 x 10{sup -5} mol L{sup -1}. The detection limits were at the 10{sup -8} mol L{sup -1} levels and the relative standard deviations were below 5% (5 determinations). When the proposed method was used for the determination of contaminants in a synthetic sample (Al-based alloy model) and of components in an Au-Pd alloy, the results were satisfactory. (orig.)

  17. Ion-ion reactions for charge reduction of biopolymer at atmospheric pressure ambient

    Institute of Scientific and Technical Information of China (English)

    Yue Ming Zhou; Jian Hua Ding; Xie Zhang; Huan Wen Chen

    2007-01-01

    Extractive electrospray ionization source (EESI) was adapted for ion-ion reaction, which was demonstrated by using a linear quadrupole ion trap mass spectrometer for the first ion-ion reaction of biopolymers in the atmospheric pressure ambient.

  18. Solid phase extraction and determination of sub-ppb levels of hazardous Hg{sup 2+} ions

    Energy Technology Data Exchange (ETDEWEB)

    Shamsipur, Mojtaba [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of)]. E-mail: mshamsipur@yahoo.com; Shokrollahi, Ardeshir [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Sharghi, Hashem [Department of Chemistry, Shiraz University, Shiraz (Iran, Islamic Republic of); Eskandari, Mohammad Mehdi [Department of Chemistry, Shiraz University, Shiraz (Iran, Islamic Republic of)

    2005-01-31

    A simple, rapid and reliable method has been developed to selectively separate and concentrate ultra trace amounts of mercury(II) ions from aqueous samples for its highly sensitive measurement by cold vapor atomic absorption spectrometry (CV-AAS). The Hg{sup 2+} ions were adsorbed selectively and quantitatively during the passage of aqueous samples through octadecyl silica membrane disks modified by isopropyl 2-[(isopropoxycarbothiolyl)disulfanyl]ethane thioate (IIDE). The retained Hg{sup 2+} ions were then stripped from the disk with minimal amounts of 0.5 M hydrobromic acid (two 8 ml portions) as eluent, and determined by CV-AAS. The break-through volume of the method is greater than 3000 ml, which results in enrichment factors >150. Maximum capacity of the membrane disks modified with 10 mg of the ligand was found to be 350 {+-} 30 {mu}g of mercury(II), and the limit of detection is 0.005 ng ml{sup -1}. The effect of various cationic interferences on the recovery of mercury in binary mixtures was studied. The method was applied to the recovery of Hg{sup 2+} ions from different synthetic and tap water samples, as well as the determination of mercury in human hair samples.

  19. Clean-up of cereal extracts for gas chromatography-tandem quadrupole mass spectrometry pesticide residues analysis using primary secondary amine and C18

    DEFF Research Database (Denmark)

    Herrmann, Susan Strange; Poulsen, Mette Erecius

    2015-01-01

    The level of co-extracted matrix in wheat and oat extracts obtained by the QuEChERS method (EN 15662) is high and the occurrence of free fatty acids generates a major matrix peak in TIC chromatograms (rt. 13-22min). Matrix can compromise the analytical performance in pesticide analysis using GC...

  20. Analysis of accumulation, extractability, and metabolization of five different phenylarsenic compounds in plants by ion chromatography with mass spectrometric detection and by atomic emission spectroscopy.

    Science.gov (United States)

    Schmidt, Anne-Christine; Kutschera, Kristin; Mattusch, Jürgen; Otto, Matthias

    2008-12-01

    Phenylated arsenic compounds occur as highly toxic contaminants in former military areas where they were formed as degradation products of chemical warfare agents. Some phenylarsenic compounds such as roxarsone and aminophenylarsonic acids were applied as food additive and veterinary drugs in stock-breeding and therefore pose an environmental risk in agricultural used sites. Very few data exist in the literature concerning uptake and effects of phenylarsenic compounds in plants growing on contaminated soils. In this study, the accumulation, extractability, and metabolization of five different phenylarsenic compounds, phenylarsonic acid, p- and o-aminophenylarsonic acid, phenylarsine oxide, and 3-nitro-4-hydroxyphenylarsonic acid called roxarsone, by the terrestrial plant Tropaeolum majus were investigated. Ion chromatography coupled to inductively coupled plasma mass spectrometry was used to differentiate these arsenic compounds, and inductively coupled plasma atomic emission spectroscopy was used for total arsenic quantification. All compounds considered were taken up by the roots and transferred to stalks, leaves, and flowers. The strongest accumulation was observed for unsubstituted phenylarsonic acid followed by its trivalent analogue phenylarsine oxide that was mostly oxidized in soil whereas the amino- or nitro- and hydroxy-substituted phenylarsonic acids were accumulated to a smaller degree. The highest extraction yield of 90% for ground leaf material was achieved by 0.1M phosphate buffer, pH 7.7, in a two-step extraction with a total extraction time of 24h. The extraction of higher amounts of arsenic (50-70% of total arsenic present in leaves depending on arsenic species application) from non-ground intact leaves with deionized water in comparison with the buffer (20-40% of total arsenic) is ascribed to osmotic effects. The arsenic species analysis revealed a cleavage of the amino groups from the phenyl ring for plants treated with aminophenylarsonic acids

  1. Screening and selective quantification of illicit drugs in wastewater by mixed-mode solid-phase extraction and quadrupole-time-of-flight liquid chromatography-mass spectrometry.

    Science.gov (United States)

    González-Mariño, Iria; Quintana, José Benito; Rodríguez, Isaac; González-Díez, Marta; Cela, Rafael

    2012-02-07

    For the first time, a mixed-mode solid-phase extraction with fractionation of basic analytes from neutral and acidic species during cartridge elution and liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) was combined for the quantitative determination of 24 illicit drugs and metabolites in urban sewage samples. The effects of several sample preparation and instrumental parameters in the sensitivity and selectivity of the quantitative method are thoroughly discussed. Under final working conditions, recoveries above 63% and 82% were attained for all species in raw and treated sewage, respectively; whereas, the limits of quantification of the method, defined for a signal-to-noise of 10 (S/N = 10), ranged from 2 to 50 ng L(-1). Sequential elution of mixed-mode cartridges allowed a significant reduction of matrix effects observed during electrospray ionization of basic drugs versus those measured for hydrophilic balance reversed-phase sorbents and the same mixed-mode polymer without fractionated elution. Analysis of raw wastewater samples confirmed the ubiquity of cocaine (COC), benzoylecgonine (BE), and 11-nor-9-carboxy-Δ(9)-tetrahydrocannabinol (THCCOOH) in this matrix. The capability of the above methodology to identify new illicit drugs and/or metabolites in sewage samples is also discussed. With this aim, a two step strategy is proposed. First, high-resolution MS chromatograms, acquired throughout each chromatographic run, are automatically searched against an in-house built database, a reduced list of candidate drugs is generated, and the corresponding extracted ion chromatograms are obtained. In a further LC run, the tandem mass spectrometry (MS/MS) spectra of unknown peaks are acquired using different collision energies and compared with those existing in public libraries, or interpreted, to assign the unknown peak to one of the previously selected candidates.

  2. A novel solid-phase extraction for the concentration of sweeteners in water and analysis by ion-pair liquid chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Gan, Zhiwei; Sun, Hongwen; Wang, Ruonan; Feng, Biting

    2013-01-25

    A highly sensitive method for the simultaneous trace (ng/L) quantification of seven commonly used artificial sweeteners in a variety of water samples using solid-phase extraction and ion-pair high-performance liquid chromatography (HPLC) triple quadrupole mass spectrometer with an electrospray ionization source (ESI-MS) in negative ion multiple reaction monitoring mode was developed. Ten solid phase extraction (SPE) cartridges were tested to evaluate their applicability for the pre-concentration of the analytes, and their loading and eluting parameters were optimized. Satisfactory recoveries (77-99%) of all of the studied sweeteners were obtained using a Poly-Sery PWAX cartridge with 25 mM sodium acetate solution (pH 4) as wash buffer and methanol containing 1mM tris (hydroxymethyl) amino methane (TRIS) as eluent. The method is sound and does not require pH adjustment or buffering of water samples. The HPLC separation was performed on an Athena C18-WP column with water and acetonitrile, both containing 5mM ammonium acetate and 1mM TRIS as mobile phases, in gradient elution mode. The linearity, precision, and accuracy of the method were evaluated, and good reproducibility was obtained. Method quantification limits varied between 0.4 and 7.5 ng/L for different water samples. The post-extraction spike method was applied to assess matrix effects, and quantification was achieved using internal standard calibration to overcome the unavoidable matrix effects during ESI-MS analysis. The method was applied to the analysis of thirteen water samples from Tianjin, China, including wastewater, tap water, surface water, and groundwater. The method described here is time-saving, accurate and precise, and is suitable for monitoring artificial sweeteners in different water matrices.

  3. Determination of the extractive capacity of para-tert butyl calix[8]arene octa-phosphinoylated towards uranyl ions from an aqueous-acidic-salty medium; Determinacion de la capacidad extractiva del p-ter-butilocalix[8]areno octa-fosfinoilado hacia iones uranilo de un medio acuo-acido salino

    Energy Technology Data Exchange (ETDEWEB)

    Serrano V, E. C.

    2011-07-01

    The extraction properties of octa-phosphinoylated para-tert butyl calix[8]arene (prepared in the laboratory) in chloroform towards uranyl ions from an aqueous-acidic-salty medium (HNO{sub 3}-3.5 NaNO{sub 3}) containing uranyl nitrate salt, was investigated. Two spectroscopic techniques UV/Vis and Luminescence were used for this study. The latter permitted analyze the fluorescence from the uranyl ions influenced by the surrounding medium. Both permitted to learn about the power of this calixarene as extractant towards the mentioned ions. Its extraction ability or capability using this calixarene at 5.91 x 10{sup -4} M towards the uranyl ions was 400% as determined by UV/Vis while fluorescence revealed 100% of uranyl ion extraction. A closed analysis of the results obtained by using these techniques revealed that the stoichiometry of the main extracted species was 1calixarene:2 uranyl ions. The loading capacity of the calixarene ligand towards the uranyl ions was also investigated using both techniques. UV/Vis resulted to be inadequate for quantifying exactly the loading capacity of the calixarene whereas luminescence was excellent indeed, using a 5.91 x 10{sup -4} M calixarene concentration, its loading capacity was 0.157 M of free uranyl ions from 0.161 M of uranyl ions present in the aqueous-acidic-salty medium. The extracts from the ability and capacity studies were concentrated to dryness, purified and the dried extracts were analyzed by infrared and neutron activation analysis. By these techniques it was demonstrated that during the extraction of the uranyl ions by the calixarene ligand they form thermodynamically and kinetically stable complexes, since in the solid state, the 1:2, calixarene; uranyl ions stoichiometry was kept with the minimum formula: (UO{sub 2}){sub 2}B{sub 8}bL{sup 8}(NO{sub 3}){sub 4}(H{sub 2}O){sub 4}CHCl{sub 3}(CH{sub 3}OH){sub 3} the methanol molecules come from its purification. It is proposed that B{sub 8}bL{sup 8} calixarene in

  4. Studies of ion-imprinted polymers for solid-phase extraction of ruthenium from environmental samples before its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zambrzycka, Elzbieta; Roszko, Dorota; Lesniewska, Barbara; Wilczewska, Agnieszka Z.; Godlewska-Zylkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2011-07-15

    The examination of the effect of interfering ions on the analytical signal of ruthenium measured by electrothermal atomic absorption spectrometry was initially performed in this work. The complexes of ruthenium(III) with thiosemicarbazide (TSd) and acetaldehyde thiosemicarbazone (AcTSn) were prepared and imprinted in polymeric network. The ion-imprinted polymers were synthesized by copolymerization of methacrylic acid, as functional monomer and ethylene glycol dimethacrylate, as crosslinking agent in the presence of 2,2-azobisisobutyronitrile as initiator. The effects of sample volume, pH, and flow rate on the extraction of analyte were studied in dynamic mode. The optimum pH for quantitative retention of ruthenium on each of the studied sorbents was 7.5 {+-} 0.5. The elution of analyte was completed with 0.2 mol L{sup -1} thiourea in 0.2 mol L{sup -1} HCl. The effect of matrix ions on ruthenium(III) separation process was studied. The analytical performance of the Ru-TSd polymer in the presence of competing ions was better than Ru-AcTSn polymer, considering recovery of analyte, reproducibility of results, selectivity coefficients, and sorbent capacity. The detection limit of the proposed method (0.16 ng mL{sup -1} on Ru-TSd and 0.25 ng mL{sup -1} on Ru-AcTSn) is lower in comparison with the previously published methods. The developed separation method was successfully applied to the determination of trace amounts of ruthenium in spiked water samples, sludge, grass, and human hair.

  5. Selective dispersive micro solid-phase extraction using oxidized multiwalled carbon nanotubes modified with 1,10-phenanthroline for preconcentration of lead ions.

    Science.gov (United States)

    Feist, Barbara

    2016-10-15

    A dispersive micro solid phase extraction (DMSPE) method for the selective preconcentration of trace lead ions on oxidized multiwalled carbon nanotubes (ox-MWCNTs) with complexing reagent 1,10-phenanthroline is presented. Flame and electrothermal atomic absorption spectrometry (F-AAS, ET-AAS) were used for detection. The influence of several parameters such as pH, amount of sorbent and 1,10-phenanthroline, stirring time, concentration and volume of eluent, sample flow rate and sample volume was examined using batch procedures. Moreover, effects of inorganic matrix on recovery of the determined elements were studied. The experiment shows that foreign ions did not influence on recovery of the determined element. The method characterized by high selectivity toward Pb(II) ions. Lead ions can be quantitatively retained at pH 7 from sample volume up to 400mL and then eluent completely with 2mL of 0.5molL(-1)HNO3. The detection limits of Pb was 0.26μgL(-1) for F-AAS and 6.4ngL(-1) for ET-AAS. The recovery of the method for the determined lead was better than 97% with relative standard deviation lower than 3.0%. The preconcentration factor was 200 for F-AAS and 100 for ET-AAS. The maximum adsorption capacity of the adsorbent was found to be about 350mgg(-1). The method was applied for determination of Pb in fish samples with good results. Accuracy of the method was verified using certified reference material DOLT-3 and ERM-BB186.

  6. Determination of aminophenols and phenol in hair colorants by ultrasound-assisted solid-phase dispersion extraction coupled with ion chromatography.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke; Wu, Rong; Zhu, Binghui; Luo, Zhibin

    2014-08-01

    A simple and reliable ultrasound-assisted solid-phase dispersion extraction coupled with ion chromatography was developed for the determination of aminophenols and phenol. The highly viscous hair colorant was dispersed in solvents using anhydrous sodium sulfite having dual functions of dispersant and antioxidant. The use of anhydrous sodium sulfite did not change the sample volume because it could completely dissolve in solution after matrix dispersion. The extraction and cleanup were combined in one single step for simplifying operation. The extraction process could be rapidly accomplished within 9 min with high sample throughput under the synergistic effects of vibration, ultrasound, and heating. Satisfactory linearity was observed with correlation coefficients higher than 0.9992, and the limits of detection varied from 0.02 to 0.09 mg/L. The applicability of the proposed method was demonstrated by measuring the concentrations of aminophenols and phenol in 32 different commercial hair color products. The recoveries ranged from 86.4-101.2% with the relative standard deviations in the range of 0.52-4.3%. The method offers an attractive alternative for the analysis of trace phenols in complex matrices.

  7. Preparation of a core-shell magnetic ion-imprinted polymer via a sol-gel process for selective extraction of Cu(II) from herbal medicines.

    Science.gov (United States)

    He, Huan; Xiao, Deli; He, Jia; Li, Hui; He, Hua; Dai, Hao; Peng, Jun

    2014-05-21

    A novel magnetic surface ion-imprinted polymer (c-MMWCNTs-SiO2-IIP) was synthesized for the first time using magnetic CNTs/Fe3O4 composites (c-MMWCNTs) as the core, 3-ammonium propyltriethoxysilane (APTES) as the functional monomer, tetraethylorthosilicate (TEOS) as the cross-linker and Cu(II) as the template. c-MMWCNTs-SiO2-IIP was evaluated for selective extraction of Cu(II) from herbal medicines via a magnetic solid phase extraction (M-SPE) procedure. One factor affecting the separation and preconcentration of the target heavy metal was pH. Under the optimized experimental conditions, the adsorption kinetics and adsorption capacity of c-MMWCNTs-SiO2-IIP toward Cu(II) were estimated. The results indicated that the adsorption mechanism corresponds to a pseudo-second order adsorption process, with a correlation coefficient (R(2)) of 0.985 and a maximum adsorption capacity of 42.2 mg g(-1). The relative selectivity factor (β) values of Cu(II)/Zn(II) and Cu(II)/Pb(II) were 38.5 and 34.5, respectively. c-MMWCNTs-SiO2-IIP, combined with flame atomic absorption spectrometry, was successfully applied in the extraction and detection of Cu(II) in herbal medicine, with high recoveries ranging from 95.6% to 108.4%.

  8. Two solid-phase recycling method for basic ionic liquid [C4mim]Ac by macroporous resin and ion exchange resin from Schisandra chinensis fruits extract.

    Science.gov (United States)

    Ma, Chun-hui; Zu, Yuan-gang; Yang, Lei; Li, Jian

    2015-01-22

    In this study, two solid-phase recycling method for basic ionic liquid (IL) 1-butyl-3-methylimidazolium acetate ([C4mim]Ac) were studied through a digestion extraction system of extracting biphenyl cyclooctene lignans from Schisandra chinensis. The RP-HPLC detection method for [C4mim]Ac was established in order to investigate the recovery efficiency of IL. The recycling method of [C4mim]Ac is divided into two steps, the first step was the separation of lignans from the IL solution containing HPD 5000 macroporous resin, the recovery efficiency and purity of [C4mim]Ac achieved were 97.8% and 67.7%, respectively. This method cannot only separate the lignans from [C4mim]Ac solution, also improve the purity of lignans, the absorption rate of lignans in [C4mim]Ac solution was found to be higher (69.2%) than that in ethanol solution (57.7%). The second step was the purification of [C4mim]Ac by the SK1B strong acid ion exchange resin, an [C4mim]Ac recovery efficiency of 55.9% and the purity higher than 90% were achieved. Additionally, [C4mim]Ac as solvent extraction of lignans from S. chinensis was optimized, the hydrolysis temperature was 90°C and the hydrolysis time was 2h.

  9. Production of citric acid using its extraction wastewater treated by anaerobic digestion and ion exchange in an integrated citric acid-methane fermentation process.

    Science.gov (United States)

    Xu, Jian; Chen, Yang-Qiu; Zhang, Hong-Jian; Tang, Lei; Wang, Ke; Zhang, Jian-Hua; Chen, Xu-Sheng; Mao, Zhong-Gui

    2014-08-01

    In order to solve the problem of extraction wastewater pollution in citric acid industry, an integrated citric acid-methane fermentation process is proposed in this study. Extraction wastewater was treated by mesophilic anaerobic digestion and then used to make mash for the next batch of citric acid fermentation. The recycling process was done for seven batches. Citric acid production (82.4 g/L on average) decreased by 34.1 % in the recycling batches (2nd-7th) compared with the first batch. And the residual reducing sugar exceeded 40 g/L on average in the recycling batches. Pigment substances, acetic acid, ammonium, and metal ions in anaerobic digestion effluent (ADE) were considered to be the inhibitors, and their effects on the fermentation were studied. Results indicated that ammonium, Na(+) and K(+) in the ADE significantly inhibited citric acid fermentation. Therefore, the ADE was treated by acidic cation exchange resin prior to reuse to make mash for citric acid fermentation. The recycling process was performed for ten batches, and citric acid productions in the recycling batches were 126.6 g/L on average, increasing by 1.7 % compared with the first batch. This process could eliminate extraction wastewater discharge and reduce water resource consumption.

  10. Synthesis and Characterization of Polystyrene-Supported Piperazine-Substituted Triazoles by CuAAC and First Evaluation for Metal Ion Extraction

    Directory of Open Access Journals (Sweden)

    Riadh Slimi

    2016-05-01

    Full Text Available The goal of this work was to synthesize substituted polystyrene for metal extraction and/or depollution by introduction of substituted piperazines as chelatants starting from Merrifield polymer. After transformation of Merrifield’s resin in azidomethyl polystyrene, click-chemistry using copper (I-catalyzed Huisgen’s reaction (CuAAC was performed to prepare different polymers grafted with 1,4-triazoles bearing the piperazines, containing an alkyne as the other counterpart in the CuAAC. The polymers were then first tested for their efficiency to remove various metal ions from neutral aqueous solutions (Fe3+, Ni2+, Cu2+, Zn2+ and Pb2+. The polymers were found to extract Ni2+ and Zn2+ with low efficiencies ≤40%. For Fe3+ and Cu2+, the average extraction was around 80%, and for Pb2+ around 50%. The global selectivity for these polymers was found to be in the order of Fe3+ ≥ Cu2+ > Pb2+ >> Ni2+ > Zn2+.

  11. Solid-phase extraction of copper, iron and zinc ions on Bacillus thuringiensis israelensis loaded on Dowex optipore V-493

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa; Melek, Esra [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Chemistry Department, 38039 Kayseri (Turkey)], E-mail: msoylak@gmail.com

    2008-11-30

    Bacillus thuringiensis israelensis loaded on Dowex optipore V-493 as new adsorbent for the separation-preconcentration of heavy metal ions has been proposed. The analytical conditions for the quantitative recoveries of copper(II), iron(III) and zinc(II) including pH, amounts of adsorbent, sample volume, etc. were investigated. The influences of alkaline and earth alkaline ions were also reported. The recovery values for the analytes are generally higher than 95%. The preconcentration factor was 37. The limit of detections of the analyte ions (k = 3, N = 21) were 1.14 {mu}g L{sup -1} for copper, 2.01 {mu}g L{sup -1} for iron and 0.14 {mu}g L{sup -1} for zinc. The relative standard deviations of the determinations were found to be lower than 9%. The procedure was validated by analyzing copper, iron and zinc contents in two certified reference materials, NRCC-SLRS-4 Riverine water and NIST SRM 1515 Apple leaves. Agreements between the obtained results and the certified values were achieved. The developed preconcentration method was applied in the flame atomic absorption spectrometric determination of copper, iron and zinc in several samples including a multivitamin-multimineral tablet, dialysis solutions, natural waters and some food samples.

  12. Quantification of Art v 1 and Act c 1 being major allergens of mugwort pollen and kiwi fruit extracts in mass-units by ion-exchange HPLC-UV method.

    Science.gov (United States)

    Blanusa, Milan; Perovic, Iva; Popovic, Milica; Polovic, Natalija; Burazer, Lidija; Milovanovic, Mina; Gavrovic-Jankulovic, Marija; Jankov, Ratko; Cirkovic Velickovic, Tanja

    2007-10-01

    A simple ion-exchange HPLC-UV method was developed for determination of major allergens from mugwort pollen and kiwi fruit extracts in mass-units. The separation of Art v 1 and Act c 1 from other components in the extracts was achieved in one step. The extinction coefficients used in the study were theoretically determined and compared to the extinction coefficients determined by gravimetry. We also reported a close correlation of the major allergen contents with the overall allergenic potency of the extracts determined by inhibition ELISA. This method could be a useful tool for standardization of allergenic extracts for clinical use.

  13. Extraction, Separation, and Identification of Phenolic Compounds in Virgin Olive Oil by HPLC-DAD and HPLC-MS

    Science.gov (United States)

    Tasioula-Margari, Maria; Tsabolatidou, Eleftheria

    2015-01-01

    The aim of this study was to evaluate the recovery of individual phenolic compounds extracted from virgin olive oil (VOO), from different Greek olive varieties. Sufficient recoveries (90%) of all individual phenolic compounds were obtained using methanol as an extraction solvent, acetonitrile for residue solubilization, and two washing steps with hexane. Moreover, in order to elucidate structural characteristics of phenolic compounds in VOO, high performance liquid chromatography with a diode array detector (HPLC-DAD) at 280 and 340 nm and HPLC coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS) in the negative-ion mode were performed. The most abundant phenolic compounds were oleuropein derivatives with m/z 319 and 377 and ligstroside derivatives with m/z 303, 361. Lignans, such as 1-acetoxypinoresinol and pinoresinol were also present in substantial quantities in the phenolic fraction. However, pinoresinol was co-eluted with dialdehydic form of ligstroside aglycone (DAFLA) and it was not possible to be quantified separately. The phenolic extracts, obtained from different VOO samples, yielded similar HPLC profiles. Differences, however, were observed in the last part of the chromatogram, corresponding to isomers of the aldehydic form of ligstroside aglycone. Oxidized phenolic products, originating from secoiridoids, were also detected. PMID:26783843

  14. Extraction, Separation, and Identification of Phenolic Compounds in Virgin Olive Oil by HPLC-DAD and HPLC-MS

    Directory of Open Access Journals (Sweden)

    Maria Tasioula-Margari

    2015-08-01

    Full Text Available The aim of this study was to evaluate the recovery of individual phenolic compounds extracted from virgin olive oil (VOO, from different Greek olive varieties. Sufficient recoveries (90% of all individual phenolic compounds were obtained using methanol as an extraction solvent, acetonitrile for residue solubilization, and two washing steps with hexane. Moreover, in order to elucidate structural characteristics of phenolic compounds in VOO, high performance liquid chromatography with a diode array detector (HPLC-DAD at 280 and 340 nm and HPLC coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS in the negative-ion mode were performed. The most abundant phenolic compounds were oleuropein derivatives with m/z 319 and 377 and ligstroside derivatives with m/z 303, 361. Lignans, such as 1-acetoxypinoresinol and pinoresinol were also present in substantial quantities in the phenolic fraction. However, pinoresinol was co-eluted with dialdehydic form of ligstroside aglycone (DAFLA and it was not possible to be quantified separately. The phenolic extracts, obtained from different VOO samples, yielded similar HPLC profiles. Differences, however, were observed in the last part of the chromatogram, corresponding to isomers of the aldehydic form of ligstroside aglycone. Oxidized phenolic products, originating from secoiridoids, were also detected.

  15. Extraction, Separation, and Identification of Phenolic Compounds in Virgin Olive Oil by HPLC-DAD and HPLC-MS.

    Science.gov (United States)

    Tasioula-Margari, Maria; Tsabolatidou, Eleftheria

    2015-08-13

    The aim of this study was to evaluate the recovery of individual phenolic compounds extracted from virgin olive oil (VOO), from different Greek olive varieties. Sufficient recoveries (90%) of all individual phenolic compounds were obtained using methanol as an extraction solvent, acetonitrile for residue solubilization, and two washing steps with hexane. Moreover, in order to elucidate structural characteristics of phenolic compounds in VOO, high performance liquid chromatography with a diode array detector (HPLC-DAD) at 280 and 340 nm and HPLC coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS) in the negative-ion mode were performed. The most abundant phenolic compounds were oleuropein derivatives with m/z 319 and 377 and ligstroside derivatives with m/z 303, 361. Lignans, such as 1-acetoxypinoresinol and pinoresinol were also present in substantial quantities in the phenolic fraction. However, pinoresinol was co-eluted with dialdehydic form of ligstroside aglycone (DAFLA) and it was not possible to be quantified separately. The phenolic extracts, obtained from different VOO samples, yielded similar HPLC profiles. Differences, however, were observed in the last part of the chromatogram, corresponding to isomers of the aldehydic form of ligstroside aglycone. Oxidized phenolic products, originating from secoiridoids, were also detected.

  16. Determination of ricin by nano liquid chromatography/mass spectrometry after extraction using lactose-immobilized monolithic silica spin column.

    Science.gov (United States)

    Kanamori-Kataoka, Mieko; Kato, Haruhito; Uzawa, Hirotaka; Ohta, Shigenori; Takei, Yoshiyuki; Furuno, Masahiro; Seto, Yasuo

    2011-08-01

    Ricin is a glycosylated proteinous toxin that is registered as toxic substance by Chemical Weapons convention. Current detection methods can result in false negatives and/or positives, and their criteria are not based on the identification of the protein amino acid sequences. In this study, lactose-immobilized monolithic silica extraction followed by tryptic digestion and liquid chromatography/mass spectrometry (LC/MS) was developed as a method for rapid and accurate determination of ricin. Lactose, which was immobilized on monolithic silica, was used as a capture ligand for ricin extraction from the sample solution, and the silica was supported in a disk-packed spin column. Recovery of ricin was more than 40%. After extraction, the extract was digested with trypsin and analyzed by LC/MS. The accurate masses of molecular ions and MS/MS spectra of the separated peptide peaks were measured by Fourier transform-MS and linear iontrap-MS, respectively. Six peptides, which were derived from the ricin A-(m/z 537.8, 448.8 and 586.8) and B-chains (m/z 701.3, 647.8 and 616.8), were chosen as marker peptides for the identification of ricin. Among these marker peptides, two peptides were ricin-specific. This method was applied to the determination of ricin from crude samples. The monolithic silica extraction removed most contaminant peaks from the total ion chromatogram of the sample, and the six marker peptides were clearly detected by LC/MS. It takes about 5 h for detection and identification of more than 8 ng/ml of ricin through the whole handling, and this procedure will be able to deal with the terrorism using chemical weapon.

  17. Supercritical carbon dioxide extraction of electrolyte from spent lithium ion batteries and its characterization by gas chromatography with chemical ionization

    Science.gov (United States)

    Mönnighoff, Xaver; Friesen, Alex; Konersmann, Benedikt; Horsthemke, Fabian; Grützke, Martin; Winter, Martin; Nowak, Sascha

    2017-06-01

    The aging products of the electrolyte from a commercially available state-of-the-art 18650-type cell were investigated. During long term cycling a huge difference in their performance and lifetime at different temperatures was observed. By interpretation of a strong capacity fading of cells cycled at 20 °C compared to cells cycled at 45 °C a temperature depending aging mechanism was determined. To investigate the influence of the electrolyte on this fading, the electrolyte was extracted by supercritical fluid extraction (SFE) and then analyzed by gas chromatography (GC) with electron impact (EI) ionization and mass selective detection. To obtain more information with regard to the identification of unknown decomposition products further analysis with positive chemical ionization (PCI) and negative chemical ionization (NCI) was performed. 17 different volatile organic aging products were detected and identified. So far, seven of them were not yet known in literature and several formation pathways were postulated taking previously published literature into account.

  18. Ion exchange equilibria in simultaneous extraction of platinum(II, IV) and rhodium(III) from hydrochloric solutions

    Science.gov (United States)

    Mel'nikov, A. M.; Kononova, O. N.; Pavlenko, N. I.; Krylov, A. S.

    2012-06-01

    Regularities of sorption extraction of platinum(II, IV) and rhodium(III) by anion exchangers of various physical and chemical structure in the presence of hydrochloric media were studied. It is established that AM-2B, Purolite A 500, and Purolite S 985 ionites adsorb complex anions of platinum metals employing mixed mechanism. A high affinity of the studied anionites for the studied complex anions of platinum and rhodium is established.

  19. Purification of gamma-amino butyric acid (GABA) from fermentation of defatted rice bran extract by using ion exchange resin

    Science.gov (United States)

    Tuan Nha, Vi; Phung, Le Thi Kim; Dat, Lai Quoc

    2017-09-01

    Rice bran is one of the significant byproducts of rice processing with 10 %w/w of constitution of whole rice grain. It is rich in nutrient compounds, including glutamic acid. Thus, it could be utilized for the fermentation with Lactobateria for synthesis of GABA, a valuable bioactive for antihypertensive effects. However, the concentration and purity of GABA in fermentation broth of defatted rice bran extract is low for production of GABA drug. This research focused on the purification of GABA from the fermentation broth of defatted rice bran extract by using cation exchange resin. The results indicate that, the adsorption isotherm of GABA by Purelite C100 showed the good agreement with Freundlich model, with high adsorption capacity. The effects of pH and concentration of NaCl in eluent on the elution were also investigated. The obtained results show that, at the operating conditions of elution as follows: pH 6.5, 0.8 M of NaCl in eluent, 0.43 of bed volume; concentration of GABA in accumulative eluent, the purity and recovery yield of GABA were 743.8 ppm, 44.0% and 84.2%, respectively. Results imply that, it is feasible to apply cation exchange resin for purification of GABA from fermentation broth of defatted rice bran extract.

  20. Prediction of Radix Astragali Immunomodulatory Effect of CD80 Expression from Chromatograms by Quantitative Pattern-Activity Relationship

    Directory of Open Access Journals (Sweden)

    Michelle Chun-har Ng

    2017-01-01

    Full Text Available The current use of a single chemical component as the representative quality control marker of herbal food supplement is inadequate. In this CD80-Quantitative-Pattern-Activity-Relationship (QPAR study, we built a bioactivity predictive model that can be applicable for complex mixtures. Through integrating the chemical fingerprinting profiles of the immunomodulating herb Radix Astragali (RA extracts, and their related biological data of immunological marker CD80 expression on dendritic cells, a chemometric model using the Elastic Net Partial Least Square (EN-PLS algorithm was established. The EN-PLS algorithm increased the biological predictive capability with lower value of RMSEP (11.66 and higher values of Rp2 (0.55 when compared to the standard PLS model. This CD80-QPAR platform provides a useful predictive model for unknown RA extract’s bioactivities using the chemical fingerprint inputs. Furthermore, this bioactivity prediction platform facilitates identification of key bioactivity-related chemical components within complex mixtures for future drug discovery and understanding of the batch-to-batch consistency for quality clinical trials.

  1. 负氢潘宁型离子源的束流引出测量%Beam extraction measurement of negative hydrogen Penning ion source

    Institute of Scientific and Technical Information of China (English)

    王韬; 杨振; 董攀; 龙继东; 李勤; 何小中; 张开志

    2012-01-01

    Negative hydrogen (H-) ion beam extraction measurement experiment was conducted in the Penning ion source developed by Institute of Fluid Physics. The single electrode, double electrode and tri-electrode extraction methods were applied for the preliminary experiment. The experimental beam intensities are much higher than the theoretical calculation result of space charge limited flow. Thus, we present a new method called beam measurement of electrical shielding box. This paper describes the basic principle of dc beam measurement of electrical shielding box method, the CST numerical simulation of the beam trajectory and the experimental results of beam measurement extraction. Employing the "V3.2 law" of space charge limited flow to fit curve, the beam current will reach 4 niA when the extraction voltage is loaded to 40 kV.%在中国工程物理研究院流体物理研究所自行研制的负氢潘宁型离子源上进行负氢束流引出测量实验,采用单电极、双电极、三电极束流引出测量方法进行初步束流引出测量,束流强度的实验测量结果远远高于空间限制流的理论计算值.因此,提出一种电屏蔽盒的直流束流引出测量方法.阐述了电屏蔽盒直流束流引出测量的基本方法、束流轨迹的CST数值模拟以及束流引出测量实验结果.研究表明:引出电压为2kV,引出间隙为3mm,磁感应强度为0.435 T时,得到较为精确的负氢束流引出强度约100 μA.通过空间电荷限制流的“V3-2定律”进行拟合,推算得到引出电压为40 kV时,负氢束流强度约达到4 mA.

  2. Determination of trace nitrite ion by spectrophotometry with cloud point extraction%浊点萃取-分光光度法测定痕量NO2-

    Institute of Scientific and Technical Information of China (English)

    王红艳; 代如梅; 王聪

    2012-01-01

    A new method for the determination of trace nitrite ion by spectrometry after cloud point extraction was proposed. With sulfanilic acid and a-naphthylamine as complexing agents, nonionic surfactant TritonX-100 as an extractant, enrichment, separation and detection of trace NO2- was achieved by using visible absorption spectroscopy. The effects of solution acidity, reagent dosage, balance time, equilibrium temperature, interfering ions on the effect of cloud point extraction were discussed, and the optimal experimental conditions were as follows; 2. 0 mL of 5% TritonX-100, 85℃, 10 min, 0. 3 mL of sulfanilic acid and a-naphthylamine, 0. 5 mL of 0. 1 mol/L sulfuric acid solution. Under the optimum conditions, the complex formed by sulfanilic acid, a-naphthylamine and NO2 was extracted into the surfactant TritonX-100 phase which was separated from water phase. The method is simple, accurate, efficient, and it has high selectivity, high sensitivity characteristics of determining trace NO2- in water samples.%建立了浊点萃取-分光光度法测定痕量NO2-根的方法.以对氨基苯磺酸和α-萘胺为络合剂,非离子型表面活性剂TritonX-100为萃取剂,富集、分离水样中痕量NO2-,采用可见吸收光谱法进行检测.研究了溶液的酸度、试剂用量、平衡时间、平衡温度、干扰离子对浊点萃取效果的影响,并得到最佳实验条件:5%的TritonX-100用量2.0mL、平衡温度85℃、平衡时间10min、对氨基苯磺酸和α-萘胺均为0.3mL、0.1mol/LH2SO4溶液0.5mL.在最佳实验条件下,对氨基苯磺酸、α-萘胺和NO2-生成的络合物被萃取到TritonX-100表面活性剂相并与水相分开.该方法适用于环境水样中痕量NO2-的测定.

  3. 色谱标气气瓶摇匀装置的研制与应用%Development and application of shaking up device for chromatogram standard gas cylinder

    Institute of Scientific and Technical Information of China (English)

    马鑫

    2012-01-01

    针对现有色谱标定试验存在的问题,分析了气瓶是否摇匀对色谱仪器标定试验成功率的影响及存在的安全隐患,研制了色谱标气气瓶摇匀装置。应用结果表明:新型色谱标气气瓶摇匀装置操作灵活、使用简单、安全可靠,从根本上杜绝了气瓶摔坏或爆炸的可能性,提高了标定试验成功率,从规范化、安全化的角度保证了色谱试验顺利进行。%In view of the existing problems of gas chromatogram demarcation test, analyzes the influence of gas not shaking up on success rate of chromatogram demarcation test and the hidden danger in safety, develops a new type of shaking up device for chromatogram standard gas cylinder. The application result shows that the new type of shaking up device for chromatogram standard gas cylinder has the characteristic of flexible operatin, simple to use, safety and trustiness, fundamentally eliminate the cylinder breaken or exploding, improves the success rate of the demarcation test, ensure chromatography test to make successfully from the aspect of standardization and security.

  4. Ultra-high performance liquid chromatography with linear ion trap-Orbitrap hybrid mass spectrometry combined with a systematic strategy based on fragment ions for the rapid separation and characterization of components in Stellera chamaejasme extracts.

    Science.gov (United States)

    Wang, Zhixin; Qu, Yang; Wang, Li; Zhang, Xiaozhe; Xiao, Hongbin

    2016-04-01

    Stellera chamaejasme, a famous toxic herb, has been used in traditional Chinese medicine to treat various diseases. For decades, increasing attention in modern pharmacological studies has been drawn to S. chamaejasme because of its potential anti-tumor, anti-virus, and anti-fungus activities. However, due to the intrinsic complexity of chemical constitutes, hardly any investigations formed an overall recognition for the chemical profiles of this herb. In this study, a rapid and sensitive ultra-high performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry method was developed to characterize the chemical components of S. chamaejasme extracts. Based on optimized ultra-high performance liquid chromatography and mass spectrometry conditions and systematic fragment ions-based strategy, a total of 47 components including flavones, diterpenes, coumarins, and lignans were simultaneously detected and identified or tentatively identified for the first time. The MS(n) fragmentation patterns of all the characterized compounds in positive or negative electrospray ionization modes were also explored and summarized. These results provided essential data for further pharmacological research on S. chamaejasme. Moreover, the method was demonstrated to be an efficient tool for rapid qualitative analysis of secondary metabolites from natural resources.

  5. Key technology of extraction power based on CSNS ion source%CSNS离子源引出电源关键技术研究

    Institute of Scientific and Technical Information of China (English)

    李海波; 沈莉; 周国仲; 翟军

    2015-01-01

    详细分析了中国散裂中子源(China Spallation Neutron Source, CSNS)直线加速器前端离子源引出电源工作原理,针对设计指标要求,提出了一种由40个功率MOSFET管串联组成的高压调制电路方案。在引出脉冲电源系统中对多个MOS管串联存在的问题,包括MOS管串联均压、保护电路、MOS管驱动信号一致性等关键问题进行了分析研究,并给出了有效的解决办法。最后在一台输入为AC220V、脉冲幅值25 kV、脉冲电流600 mA、平均功率为375 W输出的试验样机上验证了理论分析的正确性。经测试,实验结果表明离子源引出脉冲电源满足各项设计指标要求。%Background: The performance of the ion source of China Spallation Neutron Source (CSNS) starting point directly determines the success or the failure of the CSNS project, and the extracted power plays a key role in the ion source. Purpose: This study aims to resolve the critical issues including the MOS tube over-voltage, MOS tube protection circuit and the consistency of driving signal in the multiple MOS tubes working in serial structures. Methods: A high voltage modulation circuit schemed by 40 MOSFET power tubes is designed to inter-connect in series to the obtain high-voltage pulse. A high-frequency transformer of 40 secondary groups is applied to solve MOS tube consistency of driving signal issue with the same resistance in MOSFET drain source to protect MOS tube is not damaged.Results: The correctness of a prototype ion-extraction power supply of AC220V input and output average power of 375 W is verified by theoretical analysis. The experimental results show that the power supply outputs peak pulse voltage of 25 kV, with pulse width of 900μs pulse current of 600 mA, pulse jitter of 15 ns. The repetition rate is 25 Hz, and the pulse rise time is 200 ns.Conclusion: The power supply meets the requirements for ion source extraction of the negative hydrogen and lays the

  6. Analysis of ecstasy in oral fluid by ion mobility spectrometry and infrared spectroscopy after liquid-liquid extraction.

    Science.gov (United States)

    Armenta, Sergio; Garrigues, Salvador; de la Guardia, Miguel; Brassier, Judit; Alcalà, Manel; Blanco, Marcelo

    2015-03-06

    We developed and evaluated two different strategies for determining abuse drugs based on (i) the analysis of saliva by ion mobility spectrometry (IMS) after thermal desorption and (ii) the joint use of IMS and infrared (IR) spectroscopy after liquid-liquid microextraction (LLME) to enable the sensitivity-enhanced detection and double confirmation of ecstasy (MDMA) abuse. Both strategies proved effective for the intended purpose. Analysing saliva by IMS after thermal desorption, which provides a limit of detection (LOD) of 160μgL(-1), requires adding 0.2M acetic acid to the sample and using the truncated negative second derivative of the ion mobility spectrum. The joint use of IMS and IR spectroscopy after LLME provides an LOD of 11μgL(-1) with the former technique and 800μgL(-1) with the latter, in addition to a limit of confirmation (LOC) of 1.5mgL(-1). Using IMS after thermal desorption simplifies the operational procedure, and using it jointly with IR spectroscopy after LLME allows double confirmation of MDMA abuse with two techniques based on different principles (viz., IMS drift times and IR spectra). Also, it affords on-site analyses, albeit at a lower throughput.

  7. Simple extraction method and gas chromatography-mass spectrometry in the selective ion monitoring mode for the determination of phenols in wine.

    Science.gov (United States)

    Minuti, Lucio; Pellegrino, Roberto Maria; Tesei, Ilaria

    2006-05-12

    The concentrations of 22 components of wine, including most of those that have been shown to possess significant biological properties, have been determined by a fast and simple analytical method based on gas chromatography with mass spectrometric detection in the selective ion monitoring mode (GC/MS-SIM). The procedure involves an easy liquid-liquid extraction and derivatization methods of flavanols, phenols and carboxylic acid, using a very small wine volume. The average recovery (Rcv) ranged from 73 to 107% and linear regression coefficients (r(2)) were in a range of 0.981or=0.999. The GC/MS-SIM technique gives good specificity and sensitivity, and can therefore be suitable for routine monitoring of the concentration of individual phenolic antioxidants during winemaking and the aging process.

  8. Assessing ligand selectivity for uranium over vanadium ions to aid in the discovery of superior adsorbents for extraction of UO2(2+) from seawater.

    Science.gov (United States)

    Ivanov, Alexander S; Bryantsev, Vyacheslav S

    2016-06-28

    Uranium is used as the basic fuel for nuclear power plants, which generate significant amounts of electricity and have life cycle carbon emissions that are as low as renewable energy sources. However, the extraction of this valuable energy commodity from the ground remains controversial, mainly because of environmental and health impacts. Alternatively, seawater offers an enormous uranium resource that may be tapped at minimal environmental cost. Nowadays, amidoxime polymers are the most widely utilized sorbent materials for large-scale extraction of uranium from seawater, but they are not perfectly selective for uranyl, UO2(2+). In particular, the competition between UO2(2+) and VO(2+)/VO2(+) cations poses a significant challenge to the efficient mining of UO2(2+). Thus, screening and rational design of more selective ligands must be accomplished. One of the key components in achieving this goal is the establishment of computational techniques capable of assessing ligand selectivity trends. Here, we report an approach based on quantum chemical calculations that achieves high accuracy in reproducing experimental aqueous stability constants for VO(2+)/VO2(+) complexes with ten different oxygen donor ligands. The predictive power of the developed computational protocol is demonstrated for amidoxime-type ligands, providing greater insights into new design strategies for the development of the next generation of adsorbents with high selectivity toward UO2(2+) over VO(2+)/VO2(+) ions. Importantly, the results of calculations suggest that alkylation of amidoxime moieties present in poly(acrylamidoxime) sorbents can be a potential route to better discrimination between the uranyl and competing vanadium ions in seawater.

  9. Determination of non-ionic polyethoxylated surfactants in wastewater and river water by mixed hemimicelle extraction and liquid chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Cantero, Manuel; Rubio, Soledad; Pérez-Bendito, Dolores

    2005-03-04

    The capability of hemimicelles-based solid phase extraction (SPE)/liquid chromatography/atmospheric pressure chemical ionisation in positive mode, ion trap mass spectrometry (LC/(APCl+-IT)-MS) for the concentration, separation and quantitation of non-ionic surfactants has been investigated. Concentration was based on the formation of mixed aggregates of analytes [alkylphenol ethoxylates (APE, octyl and nonyl) and alkyl ethoxylates (AE, C12-C16)] with the anionic surfactant sodium dodecyl sulphate (SDS) that is adsorbed on alumina. Parameters affecting SPE were investigated on the basis that hemimicelles are dynamic entities in equilibrium with the aqueous phase. The performance of ion trap mass spectrometry for MS and MS/MS quantitation of non-ionic homologues was assessed. Recoveries of analytes from wastewater influent and effluent and river water samples ranged between 91 and 98% and were found independent on the length of the alkyl chain under the optimised conditions. Anionic surfactants did not interfere to the levels found in environmental samples. The detection limits ranged between 14 and 111 ng/l for wastewater influent, 10 and 40 for wastewater effluent and 4 and 35 for river water, after concentration of 250, 500 and 750 ml of sample, respectively. The approach was applied to the determination of AE and APE in influent and effluent samples from four wastewater treatment plants and four river samples. The concentrations of individual non-ionic surfactants found ranged between 0.3 and 373 microg/l.

  10. Green Electrochemical Process Solid-Oxide Oxygen-Ion-Conducting Membrane (SOM): Direct Extraction of Ti-Fe Alloys from Natural Ilmenite

    Science.gov (United States)

    Lu, Xionggang; Zou, Xingli; Li, Chonghe; Zhong, Qingdong; Ding, Weizhong; Zhou, Zhongfu

    2012-06-01

    The direct electrochemical extraction of Ti-Fe alloys from natural ilmenite (FeTiO3) in molten CaCl2 is reported in this article. The sintered porous pellet of natural ilmenite acted as the cathode of the electrochemical system, and the carbon-saturated liquid tin contained in a solid-oxide oxygen-ion-conducting membrane (SOM) tube served as the anode of the electrolytic cell. The electrochemical process was carried out at 3.8 V, under 1223 K and 1273 K (950 °C and 1000 °C). Oxygen was ionized continuously from the cathode and discharged at the anode; solid porous Ti-Fe alloys were obtained at the cathode. The electro-deoxidation procedure of the ilmenite was characterized by analyzing partially electro-deoxidized samples taken periodically throughout the electro-deoxidation process. The findings of this study are as follows: (1) The electro-deoxidation process followed these steps: Fe2TiO5 → FeTiO3 → Fe2TiO4 → Fe, Ti (and/or Ti-Fe alloys); and TiO2 → CaTiO3 → Ti; and (2) two types of particle growth pattern are observed in the experiments. The first pattern is characterized with particle fusion and second pattern is interconnection of particles to form porous structure. A microhole oxygen-ion-migration model is suggested based on the experimental evidence.

  11. Extractive spectrophotometric determination of five selected drugs by ion-pair complex formation with bromothymol blue in pure form and pharmaceutical preparations

    Directory of Open Access Journals (Sweden)

    Sneha G. Nair

    2015-12-01

    Full Text Available Simple, precise, selective, and expeditious spectrophotometric methods have been developed for the determination of itopride (ITO, midodrine (MID, diclofenac (DIC, mesalamine (MES, and sumatriptan (SUM in their pure form as well as in pharmaceutical preparations. The method was based on ion-pair complex formation between the drugs and anionic dye, bromothymol blue in an acidic medium (pH 2.0–4.0. The yellow colored complexes formed were quantitatively extracted into chloroform and measured at 411, 410, 413, 412, and 414 nm wavelength for ITO, MID, DIC, MES, and SUM, respectively. Beer’s law was obeyed in the concentration range of 3.0–30 µg/mL for ITO, 1.0–20 µg/mL for MID, 1.5–40 µg/mL for DIC, 1.2–12 µg/mL for MES, and 0.5–15 µg/mL for SUM. The stoichiometry of the complexes formed between the drugs and the dye was 1:1 as determined by Job’s method of continuous variation. The association constant (KIP of the ion-pair complexes formed was evaluated using Benesi–Hildebrand equation. Limit of detection, limit of quantification, and Sandell’s sensitivity of the methods were also estimated. The proposed methods were successfully employed for the determination of these drugs in their pharmaceutical dosage forms.

  12. Extraction of metal ions using chemically modified silica gel covalently bonded with 4,4'-diaminodiphenylether and 4,4'-diaminodiphenylsulfone-salicylaldehyde Schiff bases.

    Science.gov (United States)

    Dey, R K; Jha, Usha; Singh, A C; Samal, S; Ray, Alok R

    2006-08-01

    Two new chelating materials (Si-DDE-o-HB, and Si-DDS-o-HB) were synthesized by modifying the activated silica gel phase with Schiff bases of 4,4'-diaminodiphenylether (DDE)/4,4'-diaminodiphenylsulfone (DDS) and o-hydroxybenzaldehyde (o-HB). The synthesized materials were characterized by FTIR and BET surface area measurement techniques. The extraction of metal ions such as Zn2+, Mn2+ and Cr3+ by the chelating material Si-DDE-o-HB was found to be higher than that by Si-DDS-o-HB. The order of metal sorption was found to be Zn2+ > Mn2+ > Cr3+. The correlation coefficients for Freundlich and Langmuir adsorption isotherms were compared for the sorption of Zn2+ onto the chelating material. The loading and elution of the metal ion solution was examined at optimum pH 7.5 and 0.5 cm3 min-1 flow rate of the solution using a column technique. The preconcentration factor for the elution of Zn2+ using dilute HNO3 was found to be 66.2 with a breakthrough volume of 15 cm3. The data obtained for the preconcentration of Zn2+ by the column technique suggested that the material Si-DDE-o-HB can find industrial applications.

  13. Combining peak- and chromatogram-based retention time alignment algorithms for multiple chromatography-mass spectrometry datasets

    Directory of Open Access Journals (Sweden)

    Hoffmann Nils

    2012-08-01

    Full Text Available Abstract Background Modern analytical methods in biology and chemistry use separation techniques coupled to sensitive detectors, such as gas chromatography-mass spectrometry (GC-MS and liquid chromatography-mass spectrometry (LC-MS. These hyphenated methods provide high-dimensional data. Comparing such data manually to find corresponding signals is a laborious task, as each experiment usually consists of thousands of individual scans, each containing hundreds or even thousands of distinct signals. In order to allow for successful identification of metabolites or proteins within such data, especially in the context of metabolomics and proteomics, an accurate alignment and matching of corresponding features between two or more experiments is required. Such a matching algorithm should capture fluctuations in the chromatographic system which lead to non-linear distortions on the time axis, as well as systematic changes in recorded intensities. Many different algorithms for the retention time alignment of GC-MS and LC-MS data have been proposed and published, but all of them focus either on aligning previously extracted peak features or on aligning and comparing the complete raw data containing all available features. Results In this paper we introduce two algorithms for retention time alignment of multiple GC-MS datasets: multiple alignment by bidirectional best hits peak assignment and cluster extension (BIPACE and center-star multiple alignment by pairwise partitioned dynamic time warping (CeMAPP-DTW. We show how the similarity-based peak group matching method BIPACE may be used for multiple alignment calculation individually and how it can be used as a preprocessing step for the pairwise alignments performed by CeMAPP-DTW. We evaluate the algorithms individually and in combination on a previously published small GC-MS dataset studying the Leishmania parasite and on a larger GC-MS dataset studying grains of wheat (Triticum aestivum. Conclusions We

  14. Extract-filter-shoot liquid chromatography with mass spectrometry for the analysis of vitamin D2 in a powdered supplement capsule and standard reference material 3280.

    Science.gov (United States)

    Byrdwell, William Craig

    2014-08-01

    An "extract-filter-shoot" method for the analysis of vitamin D2, ergocalciferol, in a dry powdered dietary supplement capsule containing rice flour excipient and in a National Institute of Standards and Technology standard reference material 3280 is reported. Quantification of vitamin D2 was done by atmospheric pressure chemical ionization mass spectrometry using selected ion monitoring, two transitions of selected reaction monitoring, and extracted ion chromatograms from full scans. UV detection was used for the quantification of Vitamin D2 in the dry powder capsule, whereas interfering species rendered UV detection unreliable for standard reference material 3280. Average values for standard reference material 3280 ranged from 8.27 ± 0.58 to 8.33 ± 0.57 μg/g using internal standard calibration and response factor approaches, compared to the previous National Institute of Standards and Technology internal value for vitamin D2 of 8.78 ± 0.11 μg/g, and the recently updated reference value of 8.6 ± 2.6 μg/g. The powdered supplement capsule was found to contain 28.19 ± 0.35 to 28.67 ± 0.90 μg/capsule for a capsule labeled to contain 25.00 μg. The triacylglycerol composition of the rice flour excipient in the powdered supplement capsule determined by atmospheric pressure chemical ionization mass spectrometry is also reported.

  15. Spectrophotometric determination of low levels arsenic species in beverages after ion-pairing vortex-assisted cloud-point extraction with acridine red.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan; Kır, Ufuk

    2016-01-01

    A new, low-cost, micellar-sensitive and selective spectrophotometric method was developed for the determination of inorganic arsenic (As) species in beverage samples. Vortex-assisted cloud-point extraction (VA-CPE) was used for the efficient pre-concentration of As(V) in the selected samples. The method is based on selective and sensitive ion-pairing of As(V) with acridine red (ARH(+)) in the presence of pyrogallol and sequential extraction into the micellar phase of Triton X-45 at pH 6.0. Under the optimised conditions, the calibration curve was highly linear in the range of 0.8-280 µg l(-1) for As(V). The limits of detection and quantification of the method were 0.25 and 0.83 µg l(-1), respectively. The method was successfully applied to the determination of trace As in the pre-treated and digested samples under microwave and ultrasonic power. As(V) and total As levels in the samples were spectrophotometrically determined after pre-concentration with VA-CPE at 494 nm before and after oxidation with acidic KMnO4. The As(III) levels were calculated from the difference between As(V) and total As levels. The accuracy of the method was demonstrated by analysis of two certified reference materials (CRMs) where the measured values for As were statistically within the 95% confidence limit for the certified values.

  16. 2-Alkylcyclobutanones as markers for irradiated foodstuffs. III. Improvement of the field of application on the EN 1785 method by using silver ion chromatography

    NARCIS (Netherlands)

    Ndiaye, B; Horvatovich, P; Miesch, M; Hasselmann, C; Marchioni, E

    1999-01-01

    The inclusion of a purification step by silver ion chromatography in the EN 1785 analytical protocol for 2-alkylcyclobutanones (validated by the European Committee for Standardization for the detection of ionizing radiation treatment) has considerably improved the quality of the chromatograms obtain

  17. Solid phase extraction using silica gel modified with murexide for preconcentration of uranium (VI) ions from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Sadeghi, S. [Department of Chemistry, Faculty of Science, Birjand University, Birjand (Iran, Islamic Republic of)], E-mail: ssadeghi@birjand.ac.ir; Sheikhzadeh, E. [Department of Chemistry, Faculty of Science, Birjand University, Birjand (Iran, Islamic Republic of)

    2009-04-30

    Murexide was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane (APMS) to produce the new sorbent. A solid phase extraction method using the new sorbent has been developed to separate and concentrate trace amount of uranium (VI) from aqueous samples for the measurement by spectrophotometry method using Arsenazo III reagent. The influences of some analytical parameters on the quantitative recoveries of the analyte were investigated both in batch and column methods. Quantitative recovery of U(VI) was achieved by stripping with 0.1 mol L{sup -1} HCl. The maximum sorption capacity of the modified silica gel was 1.13 mmol g{sup -1} U(VI). A high preconcentration factor value of 400 with a lower limit of detection of 1 {mu}g L{sup -1} was obtained for U(VI). The practical applicability of the developed sorbent was examined using synthetic and real samples such as sea/ground water samples.

  18. Solid phase extraction using silica gel modified with murexide for preconcentration of uranium (VI) ions from water samples.

    Science.gov (United States)

    Sadeghi, S; Sheikhzadeh, E

    2009-04-30

    Murexide was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane (APMS) to produce the new sorbent. A solid phase extraction method using the new sorbent has been developed to separate and concentrate trace amount of uranium (VI) from aqueous samples for the measurement by spectrophotometry method using Arsenazo III reagent. The influences of some analytical parameters on the quantitative recoveries of the analyte were investigated both in batch and column methods. Quantitative recovery of U(VI) was achieved by stripping with 0.1 mol L(-1) HCl. The maximum sorption capacity of the modified silica gel was 1.13 mmol g(-1) U(VI). A high preconcentration factor value of 400 with a lower limit of detection of 1 microg L(-1) was obtained for U(VI). The practical applicability of the developed sorbent was examined using synthetic and real samples such as sea/ground water samples.

  19. Kinetic simulation of complex decomposition as a tool for the ion chromatographic determination of elemental speciation of less inert metal ions.

    Science.gov (United States)

    Winter, Christian; Seubert, Andreas

    2016-01-15

    Species decomposition is an often occurring artefact during the chromatographic determination of elemental speciation. The decomposition follows a simple path to lower coordinated compounds. Therefore a simulation is developed for those decomposition reactions. The simulation separates the isochronal processes of the separation itself and the ongoing reaction and delivers thermodynamic and kinetic information about the species present in the original sample. This shifts the boundaries of separation based elemental speciation to less inert metal ions which are typically not analyzable by this approach. The less inert gallium monooxalato complex [GaOx](+) is used as example for testing the simulation software as this complex decomposes only to Ga(3+) and both species are retained on cation exchange columns. We extracted thermodynamic and kinetic information from flow rate experiments by the analysis of the peak areas in the chromatogram. The results show that some of our assumptions such as the irreversibility under the applied chromatographic conditions are not ultimately true, but good accordance of simulation and measured data was achieved.

  20. Uranyl ion extraction with conventional PUREX/TRUEX ligands assessed by electroanalytical chemistry at micro liquid/liquid interfaces.

    Science.gov (United States)

    Stockmann, Tom J; Ding, Zhifeng

    2011-10-01

    The facilitated ion transfer (FIT) of uranyl or dioxouranium (UO(2)(2+)) was studied electrochemically using a micro interface between two immiscible electrolytic solutions (micro-ITIES) in order to evaluate the complexation stoichiometry and complexation constants (β) of two widely used ligands in spent fuel reprocessing: tributylphosphate (TBP) and octyl(phenyl)-N,N-diisobutylcarbamoylmethyl-phosphine oxide (CMPO). For the first time, discrete interfacial complexation reaction steps of varying uranyl to the two ligands ratios were resolved using the micro-ITIES hosted at the tip of a 25 μm diameter glass capillary. Two stoichiometries for UO(2)NO(3)TBP(n)(+) were determined including n = 3 and 4 with β values of 3.2 × 10(11) and 3.9 × 10(13), respectively. Subsequently, three distinct complexation reactions of CMPO with UO(2)(2+) were discovered corresponding to UO(2)NO(3)CMPO(2)(+), UO(2)NO(3)CMPO(3)(+), and UO(2)CMPO(5)(2+) whose respective complexation constants were determined to be 8.0 × 10(11), 8.8 × 10(14), and 6.5 × 10(32). The participation of nitrate anions in these complexation reactions is also discussed.

  1. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    Science.gov (United States)

    Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

    1995-01-01

    A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time.

  2. Comparative proteomic analysis of the response to silver ions and yeast extract in Salvia miltiorrhiza hairy root cultures.

    Science.gov (United States)

    Wang, Yajun; Shen, Ye; Shen, Zhuo; Zhao, Le; Ning, Deli; Jiang, Chao; Zhao, Rong; Huang, Luqi

    2016-10-01

    Biotic and abiotic stresses can inhibit plant growth, resulting in losses of crop productivity. However, moderate adverse stress can promote the accumulation of valuable natural products in medicinal plants. Elucidating the underlying molecular mechanisms thus might help optimize the variety of available plant medicinal materials and improve their quality. In this study, Salvia miltiorrhiza hairy root cultures were employed as an in vitro model of the Chinese herb Danshen. A comparative proteomic analysis using 2-dimensional gel electrophoresis and MALDI-TOF-MS was performed. By comparing the gel images of groups exposed to the stress of yeast extract (YE) combined with Ag(+) and controls, 64 proteins were identified that showed significant changes in protein abundance for at least one time point after treatment. According to analysis based on the KEGG and related physiological experimental verification, it was found that YE and Ag(+) stress induced a burst of reactive oxygen species and activated the Ca(2+)/calmodulin signaling pathway. Expression of immune-suppressive proteins increased. Epidermal cells underwent programmed cell death. Energy metabolism was enhanced and carbon metabolism shifted to favor the production of secondary metabolites such as lignin, tanshinone and salvianolic acids. The tanshinone and salvianolic acids were deposited on the collapsed epidermal cells forming a physicochemical barrier. The defense proteins and these natural products together enhanced the stress resistance of the plants. Since higher levels of natural products represent good quality in medicinal materials, this study sheds new light on quality formation mechanisms of medicinal plants and will hopefully encourage further research on how the planting environment affects the efficacy of herbal medicines.

  3. Assignment of Milk Fat Fatty Acid Propyl Esters by GC-FID Analysis with the Aid of Ag-ion Solid-phase Extraction.

    Science.gov (United States)

    Sasaki, Ryo; Umezawa, Masatoshi; Tsukahara, Satoru; Ishiguro, Takashi; Sato, Shinichi; Watanabe, Yomi

    2015-01-01

    The recovery of short-chain fatty acids (FAs) in milk fat (MF) is improved when the analysis of the FA composition of MF by gas chromatography (GC) is conducted with the propyl or butyl ester derivatives, instead of the methyl esters. However, this approach complicates the detection of minor FAs, such as the minor positional isomers of 16:1, which represent <0.2% of the total content. In addition, the standards of these minor esters are not commercially available. In this study, with the aim to identify minor FAs, the fatty acid propyl esters (FAPEs) of MF were fractionated by Ag-ion solid phase extraction (Ag(+)-SPE) and analyzed by GC using a DB-23 capillary column. FAPEs were successfully fractionated mainly according to the degree of unsaturation by adjusting the elution conditions of the Ag(+)-SPE, and the minor FAPEs were easily determined without the aid of standard compounds. For example, by comparison of the GC profile of the saturated Ag(+)-SPE fraction with that of the original MF, minor FAs, such as iso-, anteiso-, and saturated FAs of 15:0 and 17:0, were expected to be eluted in this order. In addition, 16:1 propyl ester was co-eluted with iso 17:0 propyl ester under the GC conditions used in this study, as confirmed by the detection of the corresponding molecular ions (296 and 312, respectively) by GC-MS. Moreover, 9c,11t-conjugated linoleic acid was found to elute between 18:3 and 20:0. To the best of our knowledge, this is the first report suggesting that the peak observed before that of cis-12:1 corresponds to trans-12:1. In conclusion, Ag(+)-SPE fractionation of FAPEs contributed to the identification of minor FAs in MF without the use of standard compounds.

  4. A simple assay for the simultaneous determination of human plasma albendazole and albendazole sulfoxide levels by high performance liquid chromatography in tandem mass spectrometry with solid-phase extraction.

    Science.gov (United States)

    Wojnicz, Aneta; Cabaleiro-Ocampo, Teresa; Román-Martínez, Manuel; Ochoa-Mazarro, Dolores; Abad-Santos, Francisco; Ruiz-Nuño, Ana

    2013-11-15

    A simple, reproducible and fast (4 min chromatogram) method of liquid chromatography in tandem with mass spectrometry (LC/MS-MS) was developed to determine simultaneously the plasma levels of albendazole (ABZ) and its metabolite albendazole sulfoxide (ABZOX) for pharmacokinetic and clinical analysis. Each plasma sample was extracted by solid phase extraction (SPE) using phenacetin as internal standard (IS). The extracted sample was eluted with a Zorbax XDB-CN column using an isocratic method. The mobile phase consisting of water with 1% acetic acid (40%, A) and MeOH (60%, B), was used at a flow rate of 1 mL/min. ABZ and ABZOX were detected and identified by mass spectrometry with electrospray ionization (ESI) in the positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 5-1000 ng/mL for ABZ and 10-1500 ng/mL (full validation) or 10-5000 ng/mL (partial validation) for ABZOX, with 5 and 10 ng/mL lower limit of quantification (LLOQ) for ABZ and ABZOX, respectively. The tests of accuracy and precision, matrix effect, extraction recovery and stability of the samples for both ABZ and ABZOX did not deviate more than 20% for the LLOQ and no more than 15% for other quality controls (QCs), according to regulatory agencies.

  5. Collision-induced dissociation pathways of yeast sphingolipids and their molecular profiling in total lipid extracts: a study by quadrupole TOF and linear ion trap-orbitrap mass spectrometry

    DEFF Research Database (Denmark)

    Ejsing, Christer S.; Moehring, Thomas; Bahr, Ute

    2006-01-01

    and the long chain base moieties in individual molecular species. By selecting m/z of class-specific fragment ions for multiple precursor ion scanning, we profiled yeast sphingolipids in total lipid extracts on a QqTOF mass spectrometer. Thus, a combination of QqTOF and LTQ Orbitrap mass spectrometry lends......TOF) instrument produced fragments of inositol-containing head groups, which were specific for each lipid class. MS(n) analysis performed on a hybrid linear ion trap-orbitrap (LTQ Orbitrap) mass spectrometer with better than 3 ppm mass accuracy identified fragment ions specific for the amide-linked fatty acid...... itself to rapid, comprehensive and structure-specific profiling of the molecular composition of sphingolipids and glycerophospholipids in important model organisms, such as fungi and plants....

  6. Trace level determination of beta-blockers in waste waters by highly selective molecularly imprinted polymers extraction followed by liquid chromatography-quadrupole-linear ion trap mass spectrometry.

    Science.gov (United States)

    Gros, Meritxell; Pizzolato, Tânia-Mara; Petrović, Mira; de Alda, Maria José López; Barceló, Damià

    2008-05-02

    This paper describes the development of an analytical methodology to determine eight beta-blockers in waste waters using molecularly imprinted polymers (MIPs) as extraction and pre-concentration material, followed by liquid chromatography-quadrupole-linear ion trap mass spectrometry (LC-QqLIT MS). The advantages offered by MIPs, in terms of selectivity and specificity, were compared with the most commonly polymeric materials used (the lipophilic-hydrophilic balanced Oasis HLB cartridges). Even though recoveries achieved with both sorbents were similar, ranging from 50 to 110% for sewage treatment plant (STP) effluent and 40-110 for STP influent, respectively, MIPs provided lower method detection limits than Oasis HLB, due to their specificity for target analytes and closely related analogues. Method detection limits (MDL) achieved using MIPs ranged from 0.2 to 6.4 ng/L for STP effluent and from 0.4 to 6.5 ng/L for STP influent. To highlight the advantages of MIPs against conventional polymeric cartridges, a detailed matrix effects study as well as cross reactivity tests were performed. For the latter purpose, the extraction efficiency of some pharmaceuticals and pesticides belonging to different therapeutic classes was assessed. LC-QqLIT MS, used for quantification and confirmation, proved to be a powerful analytical tool, as instrumental detection limits (IDL) achieved ranged from 0.2 to 2.7 pg injected (in multiple reaction monitoring mode (MRM)). In addition the inclusion of high sensitive MS/MS scans for each compound when working in Information Dependent Acquisition mode (IDA) provided extra confirmation for unequivocal identification of target compounds in complex environmental matrices.

  7. Study on specific chromatogram of rosmarinus officinalis by HPCE%迷迭香的毛细管电泳特征图谱的研究

    Institute of Scientific and Technical Information of China (English)

    高静; 王辉; 王士伟; 邓光辉

    2013-01-01

    目的:建立了迷迭香水溶性成分的毛细管电泳特征图谱.方法:以20 mmol·L-1硼砂(pH =9.50)为背景电解质溶液,运行电压12 kV,紫外检测波长300 nm,重力进样时间5 s(高度10 cm),对不同产地迷迭香进行检测.结果:按电泳峰共有率fi≥90%为依据,确定10个不同产地迷迭香的毛细管电泳指纹峰为11个,各产地迷迭香的毛细管电泳特征图谱与对照毛细管电泳特征图谱的相似度较好.在不同时间对样品进行测定,各特征峰的相对迁移时间的RSD小于5.0%,相对峰面积的RSD在2.7%~8.0%之间,结果表明样品在36 h内稳定.结论:该方法简便准确,为迷迭香的质量控制提供了有效的手段.%Objective: To establish the specific chromatogram of water - soluble constituents of rosmarinus officina-lis by capillary electrophoresis. Methods:Twenty mmol · L-1 borax(pH =9. 50) was used as background electrolyte, and operation voltage of 12 kV was applied. UV - detection was adopted at the wavelength of 300 nm. Samples were introduced at a height of 10 cm for 5 s. Result: Samples of rosmarinus officinalis from 10 different origins were selected for analysis. Based on the value of rate of common electrophoretic peaks fi≥90% ,a set of electrophoretic fingerprint atlas of 11 peaks was determined for flavones in rosmarinus officinalis samples from 10 different areas. Good similarities between the electrophoretic specific chromatogram of the samples and the standards were obtained. Relative standard deviation among the values of relative migration times of various specific peaks obtained at different time points of sample introduction was less than 5.0% ,and values of RSD's for the relative peak areas were in the range from 2.7% to 8.0%. The results obtained proved that the sample was stable within 36 h. Conclusion:The method is simple and accurate,which could be an effective method for the quality control of rosmarinus officinalis.

  8. Nanobeam production with the multicusp ion source

    Science.gov (United States)

    Lee, Y.; Ji, Q.; Leung, K. N.; Zahir, N.

    2000-02-01

    A 1.8-cm-diam multicusp ion source to be used for focused ion beam applications has been tested for Xe, He, Ne, Ar, and Kr ions. The extractable ion and electron currents were measured. The extractable ion current is similar for all these ion species except for Ne+, but the extractable electron current behaves quite differently. The multicusp ion source will be used with a combined extractor-collimator electrode system that can provide a few hundred nA of Xe+ or Kr+ ions. Ion optics computation indicates that these beams can be further focused with an electrostatic column to a beam spot size of ˜100 nm.

  9. Visual colorimetry for trace antimony(V) by ion-pair solid-phase extraction with bis[2-(5-chloro-2-pyridylazo)-5-diethylaminophenolato]cobalt(III) on a PTFE type membrane filter.

    Science.gov (United States)

    Mizuguchi, Hitoshi; Matsuda, Yuki; Mori, Takehito; Uehara, Atsushi; Ishikawa, Yuta; Endo, Masatoshi; Shida, Junichi

    2008-02-01

    A new visual colorimetry for trace antimony(V) based on ion-pair solid-phase extraction to a PTFE-type membrane filter with bis[2-(5-chloro-2-pyridylazo)-5-diethylaminophenolato]cobalt(III) ion ([Co(5-Cl-PADAP)(2)](+)) has been developed. Experiments showed that hexachloroantimonate(V) ion (SbCl(6)(-)) was adsorbed with [Co(5-Cl-PADAP)(2)](+) to the front surface of the PTFE filter. The adsorption of antimony(V) ion was promoted by the addition of lithium chloride as a source of chloride ion. The excess reagent of [Co(5-Cl-PADAP)(2)](+) was eluted by rinsing with a 10 wt% methanol aqueous solution. In this case, the slow rate of the hydrolysis reaction of SbCl(6)(-) and the difference of the hydrophobicity of the ion pairs were important for adsorption and separation with a PTFE-type membrane filter. The antimony(V) concentration was determined through a visual comparison with a standard series. The visual detection limit was 0.10 microg. The calibration curve assessed with the reflection spectrometric responses at 580 nm was linear in the concentration range of 0.10 - 1.2 microg (r = 0.996). The proposed method has been applied to the determination of sub-microgram levels of antimony(V) ion in water samples.

  10. Evaluation of Ion Exchange and Sorbing Materials for Their Adsorption/Desorption Performane towards Anthocyanins, Total Phenolics, and Sugars from a Grape Pomace Extract

    Directory of Open Access Journals (Sweden)

    Evangelos D. Trikas

    2017-03-01

    Full Text Available Byproducts of winery industries are treated, in many cases, as useless wastes constituting not only a major disposal problem but also not providing any additional profit to the industries. However, these byproducts could be utilized as a source of various phenolic compounds, such as anthocyanins, that could be used as nutraceuticals or natural colorants. Nine materials were tested and evaluated for their ability to retain and elute anthocyanins, total phenolics, and sugars from a grape pomace extract. The materials tested were the ion exchange Amberlite IRA 400 Cl−, Lewatit TP 208 and Lewatit TP 260, and the sorbing Chromosorb G-HP, Amberite XAD 2, Zeocros CA 150, Chemviron Carbon, Oasis HLB (hydrophilic-lipophilic balance and Isolute C8 end-capped (EC. The two materials with the higher anthocyanins recovery rate, Oasis HLB and Isolute C8 (EC, were further examined for their anthocyanin capacities which were calculated as 5.76 mg·cm−3 and 3.06 mg·cm−3 respectively. Furthermore, their behavior pattern towards anthocyanins of various molecular weights was investigated using a liquid chromatography coupled with mass spectrometry (LC-PDA-MS system.

  11. Helium ion microscopy and ultra-high-resolution scanning electron microscopy analysis of membrane-extracted cells reveals novel characteristics of the cytoskeleton of Giardia intestinalis.

    Science.gov (United States)

    Gadelha, Ana Paula Rocha; Benchimol, Marlene; de Souza, Wanderley

    2015-06-01

    Giardia intestinalis presents a complex microtubular cytoskeleton formed by specialized structures, such as the adhesive disk, four pairs of flagella, the funis and the median body. The ultrastructural organization of the Giardia cytoskeleton has been analyzed using different microscopic techniques, including high-resolution scanning electron microscopy. Recent advances in scanning microscopy technology have opened a new venue for the characterization of cellular structures and include scanning probe microscopy techniques such as ultra-high-resolution scanning electron microscopy (UHRSEM) and helium ion microscopy (HIM). Here, we studied the organization of the cytoskeleton of G. intestinalis trophozoites using UHRSEM and HIM in membrane-extracted cells. The results revealed a number of new cytoskeletal elements associated with the lateral crest and the dorsal surface of the parasite. The fine structure of the banded collar was also observed. The marginal plates were seen linked to a network of filaments, which were continuous with filaments parallel to the main cell axis. Cytoplasmic filaments that supported the internal structures were seen by the first time. Using anti-actin antibody, we observed a labeling in these filamentous structures. Taken together, these data revealed new surface characteristics of the cytoskeleton of G. intestinalis and may contribute to an improved understanding of the structural organization of trophozoites.

  12. Preparation and characterization of magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) nanocomposite for vortex assisted magnetic solid phase extraction of some metal ions.

    Science.gov (United States)

    Khan, Mansoor; Yilmaz, Erkan; Sevinc, Basak; Sahmetlioglu, Ertugrul; Shah, Jasmin; Jan, Muhammad Rasul; Soylak, Mustafa

    2016-01-01

    Magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) (MGO-DVB-VA) was synthesized and used for magnetic solid phase extraction of Pb(II), Cd(II), Cu(II), Ni(II) and Co(II) prior to their determination by flame atomic absorption spectroscopy. The adsorbent surface functional group was characterized by using FT-IR and Raman spectroscopy. XRD pattern was used to determine the layers of GO. Surface morphology and elemental composition of the adsorbent were evaluated by using SEM and EDX analysis. Various parameters, effecting adsorption efficiency like initial solution pH, adsorbent dose, type and volume of eluent, volume of sample and diverse ions effects were optimized. The preconcentration factor (PF) is 40 for all the metals and the limits of detection for Pb, Cd, Cu, Ni and Co are in the range of 0.37-2.39 µg L(-1) and relative standard deviation below 3.1%. The method was validated by using the method for certified reference materials (Tobacco Leaves (INCT-OBTL-5), Tomato Leaves (1573a), Certified Water (SPS-ww2) and Certified Water (TMDA 64-2)). The method was successfully applied for natural water and food samples.

  13. Application of cloud point extraction-atomic spectrometry in the speciation analysis of metal ions%浊点萃取-原子光谱法在金属离子形态分析中的应用

    Institute of Scientific and Technical Information of China (English)

    杨利宁; 赵玲玲; 陈建荣

    2012-01-01

    Cloud point extraction, an environment friendly liquid-liquid extraction technology had been applied to trace metal determination extensively. It was reviewed the application of cloud point extraction coupled with atomic spectrometry in determination of the different forms of ions in recent years. The principle of cloud point extraction was also introduced briefly.%简要介绍了浊点萃取的原理及其与原子光谱技术的联用,综述了近十年来应用浊点萃取法分离富集、原子光谱法测定多种金属离子不同形态含量的进展,对浊点萃取与光谱法联用在测定不同形态金属离子含量方面的发展进行了展望.

  14. Study on chromatographic fingerprint of sarcandra glabra (Thunb.) by microwave-assisted extraction coupled to HPLC/DAD

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was...

  15. Efficiency of a miniaturized silica monolithic cartridge in reducing matrix ions as demonstrated in the simultaneous extraction of morphine and codeine from urine samples for quantification with liquid chromatography-tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Nema, T; Chan, E C Y; Ho, P C

    2011-09-01

    Presence of matrix ions could negatively affect the sensitivity and selectivity of liquid chromatography-tandem mass spectrometer (LC-MS/MS). In this study, the efficiency of a miniaturized silica monolithic cartridge in reducing matrix ions was demonstrated in the simultaneous extraction of morphine and codeine from urine samples for quantification with LC-MS. The miniaturized silica monolith with hydroxyl groups present on the largely exposed surface area function as a weak cation exchanger for solid phase extraction (SPE). The miniaturized silica cartridge in 1 cm diameter and 0.5 cm length was housed in a 2-ml syringe fixed over a SPE vacuum manifold for extraction. The cleaning effectiveness of the cartridge was confirmed by osmometer, atomic absorption spectrometer, LC-MS and GC-TOFMS. The drugs were efficiently extracted from urine samples with recoveries ranging from 86% to 114%. The extracted analytes, after concentration and reconstitution, were quantified using LC-MS/MS. The limits of detection for morphine and codeine were 2 ng/ml and 1 ng/mL, respectively. The relative standard deviations of measurements ranged from 3% to 12%. The monolithic sorbent offered good linearity with correlation coefficients > 0.99, over a concentration range of 50-500 ng/ml. The silica monolithic cartridge was found to be more robust than the particle-based packed sorbent and also the commercial cartridge with regards to its recyclability and repeated usage with minimal loss in efficiency. Our study demonstrated the efficiency of the miniaturized silica monolith for removal of matrix ions and extraction of drugs of abuse in urinary screening.

  16. Extraction of pure components from overlapped signals in gas chromatography-mass spectrometry (GC-MS

    Directory of Open Access Journals (Sweden)

    Likić Vladimir A

    2009-10-01

    Full Text Available Abstract Gas chromatography-mass spectrometry (GC-MS is a widely used analytical technique for the identification and quantification of trace chemicals in complex mixtures. When complex samples are analyzed by GC-MS it is common to observe co-elution of two or more components, resulting in an overlap of signal peaks observed in the total ion chromatogram. In such situations manual signal analysis is often the most reliable means for the extraction of pure component signals; however, a systematic manual analysis over a number of samples is both tedious and prone to error. In the past 30 years a number of computational approaches were proposed to assist in the process of the extraction of pure signals from co-eluting GC-MS components. This includes empirical methods, comparison with library spectra, eigenvalue analysis, regression and others. However, to date no approach has been recognized as best, nor accepted as standard. This situation hampers general GC-MS capabilities, and in particular has implications for the development of robust, high-throughput GC-MS analytical protocols required in metabolic profiling and biomarker discovery. Here we first discuss the nature of GC-MS data, and then review some of the approaches proposed for the extraction of pure signals from co-eluting components. We summarize and classify different approaches to this problem, and examine why so many approaches proposed in the past have failed to live up to their full promise. Finally, we give some thoughts on the future developments in this field, and suggest that the progress in general computing capabilities attained in the past two decades has opened new horizons for tackling this important problem.

  17. Determination of Chromium(III), Chromium(VI), and Chromium(III) acetylacetonate in water by ion-exchange disk extraction/metal furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kamakura, Nao, E-mail: minnie04_tb@yahoo.co.jp; Inui, Tetsuo; Kitano, Masaru; Nakamura, Toshihiro

    2014-03-01

    A new method for the separate determination of Chromium(III) (Cr(III)), Chromium(VI) (Cr(VI)), and Cr(III) acetylacetonate (Cr(acac){sub 3}) in water was developed using a cation-exchange extraction disk (CED) and an anion-exchange extraction disk (AED) combined with metal furnace atomic absorption spectrometry (MFAAS). A 100-mL water sample was adjusted to pH 5.6 and passed through the CED placed on the AED. Cr(acac){sub 3} and Cr(III) were adsorbed on the CED, and Cr(VI) was adsorbed on the AED. The adsorbed Cr(acac){sub 3} was eluted with 50 mL of carbon tetrachloride, followed by the elution of Cr(III) with 50 mL of 3 mol L{sup −1} nitric acid. Cr(VI) was eluted with 50 mL of 3 mol L{sup −1} nitric acid. The chemical species of Cr eluted from the CED with carbon tetrachloride was identified as Cr(acac){sub 3} using infrared spectroscopy. The eluate of Cr(acac){sub 3} was diluted to 100 mL with carbon tetrachloride, and those of Cr(III) and Cr(VI) were diluted to 100 mL with deionized water. All of the solutions were subsequently analyzed by MFAAS. The calibration curve for the Cr(acac){sub 3} aqueous solutions exhibited good linearity in the range of 0.1 to 1 ng. The detection limit of Cr, which corresponded to three times the standard deviation (n = 10) of the blank values, was 20 pg. The recovery test for Cr(III), Cr(VI), and Cr(acac){sub 3} exhibited desirable results (96.0%–107%) when 5 μg of each species (50 μg L{sup −1}) was added to 100 mL water samples (i.e., tap water, rainwater, and bottled drinking water). In a humic acid solution, Cr(acac){sub 3} was quantitatively recovered (103%), but Cr(III) and Cr(VI) exhibited poor recoveries (i.e., 84.8% and 78.4%, respectively). - Highlights: • A determination method of Cr(III), Cr(VI), and Cr(III) acetylacetonate in water was developed. • The combination of ion-exchange resin disks with metal furnace AAS was used. • No effect of humic acid on the recovery of Cr(III) acetylacetonate was

  18. Multiwalled carbon nanotubes as a solid-phase extraction adsorbent for the determination of three barbiturates in pork by ion trap gas chromatography-tandem mass spectrometry (GC/MS/MS) following microwave assisted derivatization

    Energy Technology Data Exchange (ETDEWEB)

    Zhao Haixiang [College of Science, China Agricultural University, Beijing 100094 (China); Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China); Department of Basic Agricultural Science, Hebei North College, Zhangjiakou Hebei 075131 (China); Wang Liping [College of Science, China Agricultural University, Beijing 100094 (China); Qiu Yueming [Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China); Zhou Zhiqiang [College of Science, China Agricultural University, Beijing 100094 (China)]. E-mail: zqzhou@cau.edu.cn; Zhong Weike [Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China); Li Xiang [Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China)

    2007-03-14

    A new method was developed for the rapid screening and confirmation analysis of barbital, amobarbital and phenobarbital residues in pork by gas chromatography-tandem mass spectrometry (GC/MS/MS) with ion trap MSD. The residual barbiturates in pork were extracted by ultrasonic extraction, cleaned up on a multiwalled carbon nanotubes (MWCNTs) packed solid phase extraction (SPE) cartridge and applied acetone-ethyl acetate (3:7, v/v) mixture as eluting solvent and derivatized with CH{sub 3}I under microwave irradiation. The methylated barbiturates were separated on a TR-5MS capillary column and detected with an ion trap mass detector. Electron impact ion source (EI) operating MS/MS mode was adopted for identification and external standard method was employed for quantification. One precursor ion m/z 169 was selected for analysis of barbital and amobarbital and m/z 232 was selected for phenobarbital. The product ions were obtained under 1.0 V excitation voltage. Good linearities (linear coefficient R > 0.99) were obtained at the range of 0.5-50 {mu}g kg{sup -1}. Limit of detection (LOD) of barbital was 0.2 {mu}g kg{sup -1} and that of amobarbital and phenobarbital were both 0.1 {mu}g kg{sup -1} (S/N {>=} 3). Limit of quatification (LOQ) was 0.5 {mu}g kg{sup -1} for three barbiturates (S/N {>=} 10). Satisfying recoveries ranging from 75% to 96% of the three barbiturates spiked in pork were obtained, with relative standard deviations (R.S.D.) in the range of 2.1-7.8%.

  19. Assessment of capillary anion exchange ion chromatography tandem mass spectrometry for the quantitative profiling of the phosphometabolome and organic acids in biological extracts.

    Science.gov (United States)

    Kvitvang, Hans F N; Kristiansen, Kåre A; Bruheim, Per

    2014-11-28

    Metabolic profiling has become an important tool in biological research, and the chromatographic separation of metabolites coupled with mass spectrometric detection is the most frequently used approach for such studies. The establishment of robust chromatographic methods for comprehensive coverage of the anionic metabolite pool is especially challenging. In this study, the development of a capillary ion exchange chromatography (capIC) - negative ESI tandem mass spectrometry (MS/MS) workflow for the quantitative profiling of the phosphometabolome (e.g., sugar phosphates and nucleotides) is presented. The chromatographic separation and MS/MS conditions were optimized, and the precision of repetitive injections and accuracy in terms of error percentage to true concentration were assessed. The precision is excellent for a capillary flow system with an average CV% of 8.5% for a 50-fmol standard injection and in the lower 2.4-4.4% range for higher concentrations (500-7,500 fmol). The limit of detection (LOD) ranges from 1 to 100 nM (5-500 fmol injected on column), and the limit of quantitation (LOQ) ranges from 1 to 500 nM (5-2,500 fmol injected on column). A fast gradient method with the injection of 50% methanol in water between analytical samples is needed to eliminate carry-over and ensure optimal re-equilibration of the column. Finally, the quantitative applicability of the system was tested on real biological matrices using the constant-volume standard addition method (SAM). Extracts of the human kidney Hek293 cell line were spiked with increasing concentrations of standards to determine the concentration of each metabolite in the sample. Forty-four metabolites were detected with an average uncertainty of 4.1%. Thus, the capIC-MS/MS method exhibits excellent selectivity, sensitivity and precision for the quantitative profiling of the phosphometabolome.

  20. Effect Analysis of Plasma Density on Ion Beam Extracted by Grid System%等离子体密度对栅极系统束流影响分析

    Institute of Scientific and Technical Information of China (English)

    贾艳辉; 李忠明; 张天平; 李娟

    2012-01-01

    Present analyses on the ion beam of the grid system do not take account the plasma density in discharger chamber. Ion beam extraction was simulated by the particle in cell (PIC) method. The electric field was calculated by the finite differential method (FDM), and the ion particles were accelerated by the leap-frog method. With Chinese 20-centimeter Xe ion thruster, the electric potential and ion beam distributions in the center and brim aperture of grid system were obtained. The results show that the ion beam extracted by the center aperture has better focus property and smaller divergence angle than that of the brim ion beam. However, the saddle point potential of the center aperture is 24. 8V, higher than that of the brim. Hence, the plasma density in discharger chamber has an important effect on the ion beam extraction, and electron back-streaming phenomena take place on the center position of grid system firstly.%针对现有离子推力器栅极系统束流引出分析中未考虑放电室等离子体密度均匀性影响的不足,基于数值方法对该问题进行了研究.采用单元内粒子(Particle In Cell,PIC)方法对栅极系统束流引出进行了数值模拟.PIC方法中电场求解采用有限差分方法,离子加速方法采用跳蛙格式.以国产20 cm Xe离子推力器作为算例,计算得到了栅极中心和边缘孔引出束流离子和电场的分布.结果显示栅极中心孔相对边缘孔束流聚焦性好,束流发散角小,但中心孔轴线的鞍点电势较边缘孔高24.8V.因此,放电室等离子体密度分布对束流引出具有重要影响,电子返流现象最先出现在栅极中心位置.

  1. Electron Beam Ion Sources

    CERN Document Server

    Zschornacka, G.; Thorn, A.

    2013-12-16

    Electron beam ion sources (EBISs) are ion sources that work based on the principle of electron impact ionization, allowing the production of very highly charged ions. The ions produced can be extracted as a DC ion beam as well as ion pulses of different time structures. In comparison to most of the other known ion sources, EBISs feature ion beams with very good beam emittances and a low energy spread. Furthermore, EBISs are excellent sources of photons (X-rays, ultraviolet, extreme ultraviolet, visible light) from highly charged ions. This chapter gives an overview of EBIS physics, the principle of operation, and the known technical solutions. Using examples, the performance of EBISs as well as their applications in various fields of basic research, technology and medicine are discussed.

  2. Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    Science.gov (United States)

    Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

    1992-01-01

    A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

  3. Thin-layer Chromatographic (TLC) Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

    OpenAIRE

    Kagan, Isabelle A.; Flythe, Michael D.

    2014-01-01

    A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth. The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken wit...

  4. Hot-water and solid-phase extraction of fluorescent whitening agents in paper materials and infant clothes followed by unequivocal determination with ion-pair chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Chen, Hsin-Chang; Ding, Wang-Hsien

    2006-03-10

    A comprehensive method for the determination of four stilbene-type disulfonate and one distyrylbiphenyl-type fluorescent whitening agents (FWAs) in paper materials (napkin and paper tissue) and infant clothes was developed. FWAs were extracted from paper material and cloth samples using a hot-water extraction, and the aqueous extracts were then preconcentrated with the newly developed Oasis WAX (mixed-mode of weak anion exchange and reversed-phase sorbent) solid-phase extraction cartridge. The analytes were unequivocal determined by ion pair chromatography coupled with negative electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS-MS), applying a di-n-hexyl-ammonium acetate (DHAA) as the ion-pairing reagent in mobile phase. Limits of quantitation (LOQ) were established between 0.2 and 0.9 ng/g in 2 g of samples. Recovery of five FWAs in spiked commercial samples was between 42 and 95% and RSD (n = 3) ranging from 2 to 11%. The method was finally applied to commercial samples, showing that two stilbene-type disulfonates were predominant FWAs detected in napkin and infant cloth samples.

  5. Estimation of mercury speciation in soil standard reference materials with different extraction methods by ion chromatography coupled with ICP-MS.

    Science.gov (United States)

    Park, Misun; Yoon, Hyeon; Yoon, Cheolho; Yu, Jae-Young

    2011-01-01

    Analytical methods for the speciation of mercury, based on microwave extraction and sonication extraction, have been tested to determine the inorganic mercury and methyl mercury contents in two standard soil reference materials: SRM 2710 Montana Soil and BCR 580 estuarine sediment. Prior to applying the speciation extraction methods, the mineral compositions were analyzed via XRD analysis, with SRM 2710 shown to be composed mostly of aluminum silicate minerals, while carbonate minerals were the major constituent in BCR 580. Two extraction methods, microwave and sonication, were tested for the analysis and recovery efficiency of total mercury. The accuracy and efficiency of each extraction method was also compared. In the analysis of total mercury, the microwave extraction method, with using methanol and HCl as extractants, was better for SRM2710, while the application of the sonication extraction method was more efficient for the calcite-based BCR 580. The results showed good separation and recovery efficiencies, with values reaching 100% of those estimated. The sonication method was selected for the speciation of mercury, especially in BCR 580. An extraction solution comprising of a 1:1 mixture of methanol and HCl was used for the sonication extraction of BCR 580, with the resulting extractants analyzed by IC-HG-ICP-MS for methyl mercury and inorganic mercury. As a simple, rapid, sensitive, and accurate method, sonication extraction was found to be satisfactory.

  6. Bevalac extraction

    Energy Technology Data Exchange (ETDEWEB)

    Kalnins, J.G.; Krebs, G.; Tekawa, M.; Cowles, D.; Byrne, T.

    1992-02-01

    This report will describe some of the general features of the Bevatron extraction system, primarily the dependence of the beam parameters and extraction magnet currents on the Bevalac field. The extraction magnets considered are: PFW, XPl, XP2, XS1, XS2, XM1, XM2, XM3, XQ3A and X03B. This study is based on 84 past tunes (from 1987 to the present) of various ions (p,He,O,Ne,Si,S,Ar,Ca,Ti,Fe,Nb,La,Au and U), for Bevalac fields from 1.749 to 12.575 kG, where all tunes included a complete set of beam line wire chamber pictures. The circulating beam intensity inside the Bevalac is measured with Beam Induction Electrodes (BIE) in the South Tangent Tank. The extracted beam intensity is usually measured with the Secondary Emission Monitor (SEM) in the F1-Box. For most of the tunes the extraction efficiency, as given by the SEM/BIE ratio, was not recorded in the MCR Log Book, but plotting the available Log Book data as a function of the Bevalac field, see Fig.9, we find that the extraction efficiency is typically between 30->60% with feedback spill.

  7. Nuclear magnetic resonance and liquid chromatography-mass spectrometry combined with an incompleted separation strategy for identifying the natural products in crude extract

    Energy Technology Data Exchange (ETDEWEB)

    Dai Dongmei; He Jiuming [Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, 1 Xian Nong Tan Street, Beijing 100050 (China); Sun Ruixiang [Institute of Computing Technology, Chinese Academy of Sciences, Beijing 100080 (China); Zhang Ruiping [Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, 1 Xian Nong Tan Street, Beijing 100050 (China); Aisa, Haji Akber [Xinjiang Technological Institute of Physics and Chemistry, Chinese Academy of Sciences, Urumqi 830011 (China); Abliz, Zeper [Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, 1 Xian Nong Tan Street, Beijing 100050 (China)], E-mail: zeper@imm.ac.cn

    2009-01-26

    NMR and LC-MS combined with an incompleted separation strategy were proposed to the simultaneous structure identification of natural products in crude extracts, and a novel method termed as NMR/LC-MS parallel dynamic spectroscopy (NMR/LC-MS PDS) was developed to discover the intrinsic correlation between retention time (Rt), mass/charge (m/z) and chemical shift ({delta}) data of the same constituent from mixture spectra by the co-analysis of parallelly visualized multispectroscopic datasets from LC-MS and {sup 1}H NMR. The extracted ion chromatogram (XIC) and {sup 1}H NMR signals deriving from the same individual constituent were correlated through fraction ranges and intensity changing profiles in NMR/LC-MS PDS spectrum due to the signal amplitude co-variation resulted from the concentration variation of constituents in a series of incompletely separated fractions. NMR/LC-MS PDS was applied to identify 12 constituents in an active herbal extract including flavonol glycosides, which was separated into a series of fractions by flash column chromatography. The complementary spectral information of the same individual constituent in the crude extract was discovered simultaneously from mixture spectra. Especially, two groups of co-eluted isomers were identified successfully. The results demonstrated that NMR/LC-MS PDS combined with the incompleted separation strategy achieved the similar function of on-line LC-NMR-MS analysis in off-line mode and had the potential for simplifying and accelerating the analytical routes for structure identification of constituents in herbs or their active extracts.

  8. 补中益气丸中氨基酸类成分指纹图谱%Fingerprint Chromatogram of Amino Acids Compounds Analysis in Different Brands Buzhongyiqi Pills

    Institute of Scientific and Technical Information of China (English)

    柯雪红; 花汝凤; 陈锦富; 杨小催; 陈为

    2012-01-01

    Objective; To analyze the fingerprint chromatogram of amino acids compounds in different brands Buzhongyiqi pills and offer reference to distinguishing them. Method; By 6-aminoqtiinoly-Af-hydroxysuccinimdyl carbamate ( AQC) according to pre-column derivatization HPLC method to establish the fingerprint chromatogram of amino acids compounds, distilling the digital info of fingerprint chromatogram and analyzing with SPSS. Result; nine co-peaks on the HPLC fingerprints of Buzhongyiqi pills were indicated. The results of similarity analysis were 0. 8-1.00. Conclusion; This method is available for quality evalution and can control the quality of BuzhongYiqi pills.%目的:对5个不同药厂生产的20批补中益气丸氨基酸类成分指纹图谱进行比较研究.方法:以柱前衍生化HPLC,测定不同药厂补中益气丸氨基酸类成分指纹图谱,提取指纹图谱数字化信息,采用相似度分析、聚类分析等多种统计方法分析不同药厂产品特征.结果:不同药厂补中益气丸氨基酸类成分指纹图谱中有9个共有峰,相似度在0.8 ~1.00;A药厂样品中氨基酸类成分较多,指纹图谱特征与标准汤剂指纹图谱相似度最高.结论:方法稳定、可靠、重复性好,为区分不同药厂补中益气丸提供参考.

  9. Computer-assisted multi-segment gradient optimization in ion chromatography.

    Science.gov (United States)

    Tyteca, Eva; Park, Soo Hyun; Shellie, Robert A; Haddad, Paul R; Desmet, Gert

    2015-02-13

    This study reports simulation and optimization of ion chromatography separations using multi-segment gradient elution. First, an analytical expression for the gradient retention factor under these complex elution profiles was derived. This allows a rapid retention time prediction calculations under different gradient conditions, during computer-assisted method development. Next, these analytical expressions were implemented in an in-house written Matlab(®) routine that searches for the optimal (multi-segment) gradient conditions, either via a four-segment grid search or via the recently proposed one-segment-per-component search, in which the slope is adjusted after the elution of each individual component. Evaluation of the retention time simulation and optimization approaches was performed on a mixture of 18 inorganic anions and different subsets with varying number of compounds. The two considered multi-segment gradient optimization searches resulted in similar proposed gradient profiles, and corresponding chromatograms. Moreover, the resultant chromatograms were clearly superior to the chromatograms obtained from the best simple linear gradient profiles, found via a fine grid search. The proposed approach is useful for automated method development in ion chromatography in which complex elution profiles are often used to increase the separation power.

  10. Solid-phase extraction followed by liquid chromatography quadrupole time-of-flight tandem mass spectrometry for the selective determination of fungicides in wine samples.

    Science.gov (United States)

    Fontana, A R; Rodríguez, I; Ramil, M; Altamirano, J C; Cela, R

    2011-04-22

    In this work, a reliable and selective procedure for the determination of thirteen fungicides in red and white wine samples is proposed. Solid-phase extraction (SPE) and liquid chromatography (LC) tandem mass spectrometry (MS/MS), based on a hybrid quadrupole time-of-flight (QTOF) system, were used as sample preparation and determination techniques, respectively. Extraction and purification of target analytes was carried out simultaneously by using a reversed-phase Oasis HLB (200mg) SPE cartridge combined with acetonitrile as elution solvent. Fungicides were determined operating the electrospray source in the positive ionization mode, with MS/MS conditions adjusted to obtain at least two intense product ions per compound, or registering two transitions per species when a single product was noticed. High selective MS/MS chromatograms were extracted using a mass window of 20 ppms for each product ion. Considering external calibration as quantification technique, the overall recoveries (accuracy) of the procedure ranged between 81% and 114% for red and white wine samples (10-20 mL), spiked at different concentrations between 5 and 100 ng mL(-1). Relative standard deviations of the above data stayed below 12% and the limits of quantification (LOQs) of the method, calculated for 10 mL of wine, varied between 0.1 ng mL(-1) for cyprodinil (CYP) and 0.7 ng mL(-1) for myclobutanil (MYC). The optimized method was applied to seventeen commercial wines produced in Spain and obtained from local supermarkets. Nine fungicides were determined, at levels above the LOQs of the method, in the above samples. The maximum concentrations and the highest occurrence frequencies corresponded to metalaxyl (MET) and iprovalicarb (IPR). Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Quality Evaluation of Scrophulariae Slices Based on HPLC Specific Chromatogram%高效液相色谱法特征图谱用于玄参饮片的质量评价

    Institute of Scientific and Technical Information of China (English)

    朱月月; 付静; 聂诗明

    2015-01-01

    目的:建立玄参饮片的高效液相色谱法( HPLC)特征图谱,为玄参饮片的质量评价提供依据。方法采用高效液相色谱法,以C18(250mm ×4.6mm,5μm)为色谱柱,甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,以道地优质玄参为建模样本,建立玄参饮片的HPLC标准特征图谱。结果该特征图谱具18个共有特征峰。其中安格洛苷-C、肉桂酸和哈巴俄苷的色谱峰得到很好的分离,新产药材加工的13批饮片相似度均>0.95,其质量较好;23批市售饮片相似度有较大差别,存在较大质量差异。结论建立的玄参饮片HPLC标准特征图谱特征峰数量多,色谱信息量大,有助于玄参饮片的质量评价。%s:Objective To establish the HPLC specific chromatogram of Scrophulariae slices for quality evaluation.Methods The HPLC specific chromatogram of Scrophulariae slices was developed.Diamansil C18 (250mm ×4.6mm ×5μm) was adopted;The mobile phase was the mixture of methanol and 0.1%formic acid water with a gradient mode;The HPLC specific chromatogram of Scrophulariae slices was determinedbyusinghigh-qualitygeoherbsasthemodelingsample.Results 18co-possessingpeakswereselected;Thepeaksofangelo glycoside-C, cinnamic acid and harpagoside were detached clearly;The similarities of 13 batches of new produced Scrophulariae slices were higher than 0.95;The similarities of 23 batches of Scrophulariae slices on sale differed greatly.Conclusion The HPLC specific chromato-gram of Scrophulariae slices includes quantities of characteristic peaks and information, which contribute to the quality evaluation of Scrophu-lariae slices.

  12. Identification of Metabolites of 6′-Hydroxy-3,4,5,2′,4′-pentamethoxychalcone in Rats by a Combination of Ultra-High-Performance Liquid Chromatography with Linear Ion Trap-Orbitrap Mass Spectrometry Based on Multiple Data Processing Techniques

    Directory of Open Access Journals (Sweden)

    Siyi Liu

    2016-09-01

    Full Text Available In this study, an efficient strategy was established using ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap MS to profile the in vivo metabolic fate of 6′-hydroxy-3,4,5,2′,4′-pentamethoxychalcone (PTC in rat urine and feces. The UHPLC-LTQ-Orbitrap method combines the high trapping capacity and MSn scanning function of the linear ion trap along with accurate mass measurements within 5 ppm and a resolving power of up to 30,000 over a wider dynamic range compared to many other mass spectrometers. In order to reduce the potential interferences of endogenous substances, the post-acquisition processing method including high-resolution extracted ion chromatogram (HREIC and multiple mass defect filters (MMDF were developed for metabolite detection. As a result, a total of 60 and 35 metabolites were detected in the urine and feces, respectively. The corresponding in vivo reactions such as methylation, hydroxylation, hydrogenation, decarbonylation, demethylation, dehydration, methylation, demethoxylation, sulfate conjugation, glucuronide conjugation, and their composite reactions were all detected in this study. The result on PTC metabolites significantly expanded the understanding of its pharmacological effects, and could be targets for future studies on the important chemical constituents from herbal medicines.

  13. Ion sources for ion implantation technology (invited)

    Energy Technology Data Exchange (ETDEWEB)

    Sakai, Shigeki, E-mail: sakai-shigeki@nissin.co.jp; Hamamoto, Nariaki; Inouchi, Yutaka; Umisedo, Sei; Miyamoto, Naoki [Nissin Ion Equipment co., ltd, 575 Kuze-Tonoshiro-cho Minami-ku, Kyoto 601-8205 (Japan)

    2014-02-15

    Ion sources for ion implantation are introduced. The technique is applied not only to large scale integration (LSI) devices but also to flat panel display. For LSI fabrication, ion source scheduled maintenance cycle is most important. For CMOS image sensor devices, metal contamination at implanted wafer is most important. On the other hand, to fabricate miniaturized devices, cluster ion implantation has been proposed to make shallow PN junction. While for power devices such as silicon carbide, aluminum ion is required. For doping processes of LCD fabrication, a large ion source is required. The extraction area is about 150 cm × 10 cm, and the beam uniformity is important as well as the total target beam current.

  14. Coupling of multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction with pulse glow discharge-ion mobility spectrometry for analysis of triazine herbicides in water and soil samples.

    Science.gov (United States)

    Zou, Nan; Yuan, Chunhao; Liu, Shaowen; Han, Yongtao; Li, Yanjie; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

    2016-07-29

    An analytical method based on stir bar sorptive extraction (SBSE) coupled with pulse glow discharge-ion mobility spectrometry (PGD-IMS) was developed for analysis of three triazine pesticide residues in water and soil samples. An injection port with sealing device and stir bars hold device were designed and constructed to directly position the SBSE fiber including the extracted samples into the heating device, making desorption and detection of analytes proceeded simultaneously. The extraction conditions such as SBSE solid phase material, extraction time, extraction temperature, pH value and salt concentration were optimized. Mixture of MWCNTs-COOH and PDMS were shown to be effective in enriching the triazines. The LODs and LOQs of three triazines were found to be 0.006-0.015μgkg(-1) and 0.02-0.05μgkg(-1), and the linear range was 0.05-10μgL(-1) with determination coefficients from 0.9987 to 0.9993. The SBSE-PGD-IMS method was environmentally friendly without organic solvent consumption in the entire experimental procedures, and it was demonstrated to be a commendable rapid analysis technique for analysis of triazine pesticide residues in environmental samples on site. The proposed method was applied for the analysis of real ground water, surface water and soil samples.

  15. Extraction of Pectin from Ginkgo Biloba L. Shells by Ion-exchange Method%离子交换法提取银杏壳中果胶工艺研究

    Institute of Scientific and Technical Information of China (English)

    顾焰波; 仇菲; 汤小芳; 常晓垒

    2015-01-01

    The pectin of ginkgo biloba L. shells were extracted by ion-exchange method. The influent of single factors and orthogo-nal tests on the yield of pectin were studied. The results showed that the appropriate technical conditions were as followed: cation exchange resins 7%, pH 2.0, the extraction temperature 85℃, the extraction time 2h,the ratio of material to extraction solution 1g/20mL. Under the process conditions, the extract yield of pectin was 4.85%.%采用离子交换法对银杏壳中果胶进行提取.通过单因素试验和正交试验探讨了提取过程中各因素对果胶得率的影响,结果表明适宜工艺条件为:离子交换树脂用量7%,pH 2.0,提取温度85℃,提取时间2h,料液比1:20(g:mL).在此工艺条件下,果胶得率为4.85%.

  16. Operator care and eco-concerned development of a fast, facile and economical assay for basic nitrogenous drugs based on simplified ion-pair mini-scale extraction using safer solvent combined with drop-based spectrophotometry.

    Science.gov (United States)

    Plianwong, Samarwadee; Sripattanaporn, Areerut; Waewsa-nga, Kwanrutai; Buacheen, Parin; Opanasopit, Praneet; Ngawhirunpat, Tanasait; Rojanarata, Theerasak

    2012-08-30

    A fast, facile, and economical assay for basic nitrogenous drugs has been developed based on the mini-scale extraction of the drug-dye ion pair complex combined with the use of safe-for-analyst and eco-friendlier organic extractant and drop-based micro-spectrophotometry. Instead of using large volume devices, the extraction was simply carried out in typical 1.5 mL microcentrifuge tubes along with the use of micropipettes for accurate transfer of liquids, vortex mixer for efficient partitioning of solutes and benchtop centrifuge for rapid phase separation. In the last step, back-extraction was performed by using the microvolume of acidic solution in order to concentrate the colored species into a confined aqueous microdrop and to keep the analyst away from unwanted contact and inhalation of organic solvents during the quantitation step which was achieved by using cuvetteless UV-vis micro-spectrophotometry without any prior dilutions. Using chlorpheniramine maleate as a representative analyte and n-butyl acetate as a less toxic and non-ozone depleting extractant, the miniaturized method was less laborious and much faster. It was accurate, precise and insensitive to the interferences from common excipients. Notably, it gave the assay results of drug in tablets and oral solution comparable to the large-scale pharmacopeial method while the consumption of organic solvents and the release of wastes were lowered by 200-400 folds.

  17. A Multicusp Ion Source for Radioactive Ion Beams

    Science.gov (United States)

    Wutte, D.; Freedman, S.; Gough, R.; Lee, Y.; Leitner, M.; Leung, K. N.; Lyneis, C.; Picard, D. S.; Sun, L.; Williams, M. D.; Xie, Z. Q.

    1997-05-01

    In order to produce a radioactive ion beam of (14)O+, a 10-cm-diameter, 13.56 MHz radio frequency (rf) driven multicusp ion source is now being developed at Lawrence Berkeley National Laboratory. In this paper we describe the specific ion source design and the basic ion source characteristics using Ar, Xe and a 90types of measurements have been performed: extractable ion current, ion species distributions, gas efficiency, axial energy spread and ion beam emittance measurements. The source can generate ion current densities of approximately 60 mA/cm2 . In addition the design of the ion beam extraction/transport system for the actual experimental setup for the radioactive beam line will be presented.

  18. Successive extraction of As(V), Cu(II) and P(V) ions from water using spent coffee powder as renewable bioadsorbents

    OpenAIRE

    Linlin Hao; Peng Wang; Suresh Valiyaveettil

    2017-01-01

    For the first time, renewable and easy accessible pre-bleached spent coffee powder coated with polyethylenimine (PEI) and ferric ions (Coffee-PEI-Fe) was used for the successive adsorption of As(V), Cu(II) and P(V) ions from spiked water samples. Fully characterized coffee-PEI-Fe was employed for batch mode experiments. Kinetic regression analysis showed that the adsorption processes of As(V) and P(V) anions follows a pseudo-second-order model, while the adsorption of Cu(II) ions fit with a p...

  19. Hexavalent chromium recovery by liquid–liquid extraction with 2-octylaminopyridine from acidic chloride media and its sequential separation from other heavy toxic metal ions

    OpenAIRE

    C.P. Mane; S.V. Mahamuni; S. S. Kolekar; Han, S. H.; M. A. ANUSE

    2016-01-01

    A systematic study of extraction of chromium(VI) with 2-octylaminopyridine (2-OAP) in xylene at room temperature has been conducted. Quantitative extraction of chromium(VI) was observed in the 0.4–0.8 M concentration range of hydrochloric acid. From the extracted complex species in the organic phase, chromium(VI) was back extracted with 7 N ammonia (3 × 10 mL), and was determined by spectrophotometric method. Various parameters such as 2-OAP concentration, equilibrium period, effect of variou...

  20. Application of a thiourea-containing task-specific ionic liquid for the solid-phase extraction cleanup of lead ions from red lipstick, pine leaves, and water samples.

    Science.gov (United States)

    Saljooqi, Asma; Shamspur, Tayebeh; Mohamadi, Maryam; Mostafavi, Ali

    2014-07-01

    Here, task-specific ionic liquid solid-phase extraction is proposed for the first time. In this approach, a thiourea-functionalized ionic liquid is immobilized on the solid sorbent, multiwalled carbon nanotubes. These modified nanotubes packed into a solid-phase extraction column are used for the selective extraction and preconcentration of ultra-trace amounts of lead(II) from aqueous samples prior to electrothermal atomic absorption spectroscopy determination. The thiourea functional groups act as chelating agents for lead ions retaining them and so, give the selectivity to the sorbent. Elution of the retained ions can be performed using an acidic thiourea solution. The effects of experimental parameters including pH of the aqueous solution, type and amount of eluent, and the flow rates of sample and eluent solutions on the separation efficiency are investigated. The linear dependence of absorbance of lead on its concentration in the initial solution is in the range of 0.5-40.0 ng/mL with the detection limit of 0.13 ng/mL (3(Sb)/m, n = 10). The proposed method is applicable to the analysis of red lipstick, pine leaves, and water samples for their lead contents. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. 浊点萃取技术在金属离子形态分析中的应用%Application of Cloud Point Extraction in Speciation Analysis of Metal Ions

    Institute of Scientific and Technical Information of China (English)

    陈建国; 金献忠; 陈少鸿

    2011-01-01

    A review on the recent progress of application of cloud point extraction in speciation analysis was presented,pertaining especially to two aspects: ① the metal ions with various species were determined after sequential extraction under different conditions;② the metal ions with various species were simultaneously extracted,then separated by chromatography and determined online(34 ref.cited).%综述了近年来浊点萃取分离富集方法在金属离子形态分析中的应用,包括以下两个方面:①通过控制萃取条件对不同形态金属离子进行顺序萃取,实现不同形态金属离子的分别测定;②将不同形态的金属离子同时萃取后,浓缩相经色谱分离在线测定(引用文献34篇)。

  2. Determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxyethylamphetamine, and 3,4-methylenedioxymethamphetamine in urine by online solid-phase extraction and ion-pairing liquid chromatography with detection by electrospray tandem mass spectrometry.

    Science.gov (United States)

    Wu, Ti-Yu; Fuh, Ming-Ren

    2005-01-01

    A method using an online solid-phase extraction (SPE) and ion-pairing liquid chromatography with electrospray tandem mass spectrometry (LC/ES-MS/MS) was developed for determination of amphetamine (Amp), methamphetamine (mAmp), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA), and 3,4-methylenedioxymethamphetamine (MDMA) in urine samples. A SPE cartridge column with both hydrophilic and lipophilic functions was utilized for online extraction. A reversed-phase C18 LC column was employed for LC separation and MS/MS was used for detection. Trifluoroacetic acid was added to the mobile phase as an ion-pairing reagent. This method was fully automated and the extraction and analysis procedures were controlled by a six-port switch valve. Recoveries ranging from 85-101% were measured. Good linear ranges (10-500 ng/mL) for Amp and mAmp were determined. For MDA, MDMA and MDEA, dual linear ranges were obtained from 5-100 and 100-500 ng/mL, respectively. The detection limit of each analytical compound, based on a signal-to-noise ratio of 3, ranged from 1-3 ng/mL. The applicability of this newly developed method was examined by analyzing several urine samples from drug users. Good agreement was obtained between the results from this method and a literature GC/MS method.

  3. Preliminary Phytochemical screening and HPTLC Studies of Extracts of Dried Rhizomes of Aspidium cicutarium

    Directory of Open Access Journals (Sweden)

    Maushumi Kulkarni

    2013-09-01

    Full Text Available Objective: Many herbal formulations are widely used in Ayurveda since ancient times. However it is not possible to attribute their pharmacological activity to a particular phytoconstituent present in the extract unless thorough phytochemical investigation is carried out. The present study aims at phytochemical screening of methanolic and aqueous extracts of rhizomes of Aspidium cicutarium Family Dyropteridaceae. The powdered dried rhizome was subjected to initial studies to determine the physical constants. Results: Extracts were made and subjected to various chemical tests and showed presence of steroids, flavonoids, saponins. Further investigation of the extracts by HPTLC is an attempt to deduce the varied composition of methanolic and aqueous extract of Aspidium cicutarium. The chromatogram shows presence of multiple peaks which indicate diverse composition of extract. Conclusion: Further detailed investigations of the extracts can be helpful in making formulations of these extracts so that they can successfully and safely be used to treat some diseases.

  4. Successive extraction of As(V), Cu(II) and P(V) ions from water using spent coffee powder as renewable bioadsorbents.

    Science.gov (United States)

    Hao, Linlin; Wang, Peng; Valiyaveettil, Suresh

    2017-02-21

    For the first time, renewable and easy accessible pre-bleached spent coffee powder coated with polyethylenimine (PEI) and ferric ions (Coffee-PEI-Fe) was used for the successive adsorption of As(V), Cu(II) and P(V) ions from spiked water samples. Fully characterized coffee-PEI-Fe was employed for batch mode experiments. Kinetic regression analysis showed that the adsorption processes of As(V) and P(V) anions follows a pseudo-second-order model, while the adsorption of Cu(II) ions fit with a pseudo-first-order model. The maximum adsorption capacities estimated by Langmuir model for As(V), Cu(II) and P(V) ions were 83.3, 200.1, and 50.2 mg/g, respectively. The simulated results revealed that the internal diffusion is the rate-determining step for the adsorptions of As(V) and Cu(II) ions, while film diffusion is the mass transfer resistance for the adsorption of P(V) ions on the surface of coffee-PEI-Fe. The successive adsorptions of adsorbates were achieved through electrostatic attraction between adsorbent surface and adsorbates. The dynamic column adsorption behavior of the adsorbent was described by Thomas model, which showed a good agreement with the experimental values (qexp). The results presented in this paper could be used for developing efficient adsorbent from renewable materials for water purification.

  5. Successive extraction of As(V), Cu(II) and P(V) ions from water using spent coffee powder as renewable bioadsorbents

    Science.gov (United States)

    Hao, Linlin; Wang, Peng; Valiyaveettil, Suresh

    2017-02-01

    For the first time, renewable and easy accessible pre-bleached spent coffee powder coated with polyethylenimine (PEI) and ferric ions (Coffee-PEI-Fe) was used for the successive adsorption of As(V), Cu(II) and P(V) ions from spiked water samples. Fully characterized coffee-PEI-Fe was employed for batch mode experiments. Kinetic regression analysis showed that the adsorption processes of As(V) and P(V) anions follows a pseudo-second-order model, while the adsorption of Cu(II) ions fit with a pseudo-first-order model. The maximum adsorption capacities estimated by Langmuir model for As(V), Cu(II) and P(V) ions were 83.3, 200.1, and 50.2 mg/g, respectively. The simulated results revealed that the internal diffusion is the rate-determining step for the adsorptions of As(V) and Cu(II) ions, while film diffusion is the mass transfer resistance for the adsorption of P(V) ions on the surface of coffee-PEI-Fe. The successive adsorptions of adsorbates were achieved through electrostatic attraction between adsorbent surface and adsorbates. The dynamic column adsorption behavior of the adsorbent was described by Thomas model, which showed a good agreement with the experimental values (qexp). The results presented in this paper could be used for developing efficient adsorbent from renewable materials for water purification.

  6. Pyrazine-functionalized calix[4]arenes: synthesis by palladium-catalyzed cross-coupling with phosphorus pronucleophiles and metal ion extraction properties

    NARCIS (Netherlands)

    Nikishkin, N.; Huskens, Jurriaan; Ansari, S.A.; Mohapatra, P.K.; Verboom, Willem

    2013-01-01

    A series of pyrazine-based calix[4]arene extractants was prepared by a stepwise functionalization, comprising palladium-catalyzed exhaustive cross-coupling of di- and tetrasubstituted calix[4]arenes bearing chloropyrazine moieties. The extraction behavior of the synthesized ligands was studied on

  7. Detergent extraction of herpes simplex virus type 1 glycoprotein D by zwitterionic and non-ionic detergents and purification by ion-exchange high-performance liquid chromatography

    NARCIS (Netherlands)

    Welling-Wester, S; Feijlbrief, M; Koedijk, DGAM; Welling, GW

    1998-01-01

    Detergents (surfactants) are the key reagents in the extraction and purification of integral membrane proteins. Zwitterionic and non-ionic detergents were used for the extraction of recombinant glycoprotein D (gD-1) of herpes simplex virus type 1 (HSV-1) from insect cells infected with recombinant b

  8. Hyphenating size-exclusion chromatography with electrospray mass spectrometry; using on-line liquid-liquid extraction to study the lipid composition of lipoprotein particles.

    Science.gov (United States)

    Osei, Michael; Griffin, Julian L; Koulman, Albert

    2015-11-15

    Lipoproteins belong to the most commonly measured clinical biochemical parameters. Lipidomics is an orthogonal approach and aims to profile the individual lipid molecules that jointly form the lipoprotein particles. However, in the first step of the extraction of lipid molecules from serum, an organic solvent is used leading to dissociation of the lipoproteins. Thus far it has been impossible to combine lipidomics and lipoprotein analysis in one analytical system. Human plasma was diluted in phosphate-buffered saline (PBS) and injected onto a Superose 6 PC 3.2 column with PBS as a mobile phase to separate lipoproteins. The eluent was led to a Syrris FLLEX module, which also received CHCl3 /MeOH (3:1). The two phases were mixed and subsequently separated using a Teflon membrane in an especially designed pressurized flow chamber. The organic phase was led to a standard electrospray source of an Orbitrap mass spectrometer. Size-exclusion chromatography (SEC) has been commonly applied to separate lipoproteins and is considered a practical alternative to ultracentrifugation. Through the on-line liquid-liquid extraction method it becomes possible to obtained detailed mass spectra of lipids across different lipoprotein fractions. The extracted ion chromatograms of specific lipid signals showed their distribution against the size of lipoprotein particles. The application of on-line liquid-liquid extraction allows for the continuous electrospray-based mass spectral analysis of SEC eluent, providing the detailed lipid composition of lipoprotein particles separated by size. This approach provides new possibilities for the study of the biochemistry of lipoproteins. © 2015 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd.

  9. Effect of para-substituents on alkaline earth metal ion extraction by proton di-ionizable calix[4]arene-crown-6 ligands in cone, partial-cone and 1,3-alternate conformations.

    Science.gov (United States)

    Zhou, Hui; Liu, Dazhan; Gega, Jerzy; Surowiec, Kazimierz; Purkiss, David W; Bartsch, Richard A

    2007-01-21

    Two carboxylic acid or N-(X)sulfonyl carboxamide groups were incorporated into calix[4]arene-crown-6 compounds to afford di-ionizable ligands for use in divalent metal ion separations. Acidities of the N-(X)sulfonyl carboxamide groups were tuned by variation of the electron-withdrawing properties of X. Cone, partial-cone and 1,3-alternate conformations were obtained by different synthetic strategies and their structures verified by NMR spectroscopy. Competitive solvent extractions of alkaline earth metal cations from aqueous solutions into chloroform were performed and the results compared with those reported previously for di-ionizable p-tert-butylcalix[4]arene-crown-6 analogues to probe the influence of the para-substituent on the calix[4]arene scaffold on extraction selectivity and efficiency.

  10. Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

    Science.gov (United States)

    Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

    2016-08-12

    A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples.

  11. Batch and fixed-bed column studies for biosorption of Zn(II) ions onto pongamia oil cake (Pongamia pinnata) from biodiesel oil extraction.

    Science.gov (United States)

    Shanmugaprakash, M; Sivakumar, V

    2015-12-01

    The present work, analyzes the potential of defatted pongamia oil cake (DPOC) for the biosorption of Zn(II) ions from aqueous solutions in the both batch and column mode. Batch experiments were conducted to evaluate the optimal pH, effect of adsorbent dosage, initial Zn(II) ions concentration and contact time. The biosorption equilibrium and kinetics data for Zn(II) ions onto the DPOC were studied in detail, using several models, among all it was found to be that, Freundlich and the second-order model explained the equilibrium data well. The calculated thermodynamic parameters had shown that the biosorption of Zn(II) ions was exothermic and spontaneous in nature. Batch desorption studies showed that the maximum Zn(II) recovery occurred, using 0.1 M EDTA. The Bed Depth Service Time (BDST) and the Thomas model was successfull