WorldWideScience

Sample records for two-dimensional ion chromatography

  1. Determination of γ-hydroxybutyrate in human urine samples by ion exclusion and ion exchange two-dimensional chromatography system.

    Science.gov (United States)

    Liu, Junwei; Deng, Zhifen; Zhu, Zuoyi; Wang, Yong; Wang, Guoqing; Sun, Yu-An; Zhu, Yan

    2017-12-15

    A two-dimensional ion chromatography system was developed for the determination of γ-hydroxybutyrate (GHB) in human urine samples. Ion exclusion chromatography was used in the first dimensional separation for elimination of urine matrices and detection of GHB above 10mgL -1 , ion exchange chromatography was used in the second dimensional separation via column-switching technique for detection of GHB above 0.08mgL -1 . Under the optimized chromatographic conditions, the ion exclusion and ion exchange chromatography separation system exhibited satisfactory repeatability (RSDchromatography system was convenient and practical for the determination of GHB in human urine samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

    NARCIS (Netherlands)

    Brudin, S.S.; Shellie, R.A.; Haddad, P.R.; Schoenmakers, P.J.

    2010-01-01

    In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

  3. Optimizing separations in online comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

    2018-01-01

    Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

  4. Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

    Science.gov (United States)

    Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

    2017-12-29

    Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Theories to support method development in comprehensive two-dimensional liquid chromatography - A review

    NARCIS (Netherlands)

    Bedani, F.; Schoenmakers, P.J.; Janssen, H.-G.

    2012-01-01

    On-line comprehensive two-dimensional liquid chromatography techniques promise to resolve samples that current one-dimensional liquid chromatography methods cannot adequately deal with. To make full use of the potential of two-dimensional liquid chromatography, optimization is required. Optimization

  6. Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

    Science.gov (United States)

    Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

    2016-01-01

    Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Two-dimensional boundary-value problem for ion-ion diffusion

    International Nuclear Information System (INIS)

    Tuszewski, M.; Lichtenberg, A.J.

    1977-01-01

    Like-particle diffusion is usually negligible compared with unlike-particle diffusion because it is two orders higher in spatial derivatives. When the ratio of the ion gyroradius to the plasma transverse dimension is of the order of the fourth root of the mass ratio, previous one-dimensional analysis indicated that like-particle diffusion is significant. A two-dimensional boundary-value problem for ion-ion diffusion is investigated. Numerical solutions are found with models for which the nonlinear partial differential equation reduces to an ordinary fourth-order differential equation. These solutions indicate that the ion-ion losses are higher by a factor of six for a slab geometry, and by a factor of four for circular geometry, than estimated from dimensional analysis. The solutions are applied to a multiple mirror experiment stabilized with a quadrupole magnetic field which generates highly elliptical flux surfaces. It is found that the ion-ion losses dominate the electron-ion losses and that these classical radial losses contribute to a significant decrease of plasma lifetime, in qualitiative agreement with the experimental results

  8. Bayesian approach for peak detection in two-dimensional chromatography

    NARCIS (Netherlands)

    Vivó-Truyols, G.

    2012-01-01

    A new method for peak detection in two-dimensional chromatography is presented. In a first step, the method starts with a conventional one-dimensional peak detection algorithm to detect modulated peaks. In a second step, a sophisticated algorithm is constructed to decide which of the individual

  9. Quantitation of triacylglycerols in edible oils by off-line comprehensive two-dimensional liquid chromatography-atmospheric pressure chemical ionization mass spectrometry using a single column.

    Science.gov (United States)

    Wei, Fang; Hu, Na; Lv, Xin; Dong, Xu-Yan; Chen, Hong

    2015-07-24

    In this investigation, off-line comprehensive two-dimensional liquid chromatography-atmospheric pressure chemical ionization mass spectrometry using a single column has been applied for the identification and quantification of triacylglycerols in edible oils. A novel mixed-mode phenyl-hexyl chromatographic column was employed in this off-line two-dimensional separation system. The phenyl-hexyl column combined the features of traditional C18 and silver-ion columns, which could provide hydrophobic interactions with triacylglycerols under acetonitrile conditions and can offer π-π interactions with triacylglycerols under methanol conditions. When compared with traditional off-line comprehensive two-dimensional liquid chromatography employing two different chromatographic columns (C18 and silver-ion column) and using elution solvents comprised of two phases (reversed-phase/normal-phase) for triacylglycerols separation, the novel off-line comprehensive two-dimensional liquid chromatography using a single column can be achieved by simply altering the mobile phase between acetonitrile and methanol, which exhibited a much higher selectivity for the separation of triacylglycerols with great efficiency and rapid speed. In addition, an approach based on the use of response factor with atmospheric pressure chemical ionization mass spectrometry has been developed for triacylglycerols quantification. Due to the differences between saturated and unsaturated acyl chains, the use of response factors significantly improves the quantitation of triacylglycerols. This two-dimensional liquid chromatography-mass spectrometry system was successfully applied for the profiling of triacylglycerols in soybean oils, peanut oils and lord oils. A total of 68 triacylglycerols including 40 triacylglycerols in soybean oils, 50 triacylglycerols in peanut oils and 44 triacylglycerols in lord oils have been identified and quantified. The liquid chromatography-mass spectrometry data were analyzed

  10. Two-Dimensional Liquid Chromatography Analysis of Polystyrene/Polybutadiene Block Copolymers.

    Science.gov (United States)

    Lee, Sanghoon; Choi, Heejae; Chang, Taihyun; Staal, Bastiaan

    2018-05-15

    A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (Styrolux) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene- block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition, and chain architecture. While individual LC analysis, including size exclusion chromatography, interaction chromatography, or liquid chromatography at critical condition, is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homopolystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

  11. Offline coupling of high-speed counter-current chromatography and gas chromatography/mass spectrometry generates a two-dimensional plot of toxaphene components.

    Science.gov (United States)

    Kapp, Thomas; Vetter, Walter

    2009-11-20

    High-speed counter-current chromatography (HSCCC), a separation technique based solely on the partitioning of solutes between two immiscible liquid phases, was applied for the fractionation of technical toxaphene, an organochlorine pesticide which consists of a complex mixture of structurally closely related compounds. A solvent system (n-hexane/methanol/water 34:24:1, v/v/v) was developed which allowed to separate compounds of technical toxaphene (CTTs) with excellent retention of the stationary phase (S(f) = 88%). Subsequent analysis of all HSCCC fractions by gas chromatography coupled to electron-capture negative ion mass spectrometry (GC/ECNI-MS) provided a wealth of information regarding separation characteristics of HSCCC and the composition of technical toxaphene. The visualization of the large amount of data obtained from the offline two-dimensional HSCCC-GC/ECNI-MS experiment was facilitated by the creation of a two-dimensional (2D) contour plot. The contour plot not only provided an excellent overview of the HSCCC separation progress, it also illustrated the differences in selectivity between HSCCC and GC. The results of this proof-of-concept study showed that the 2D chromatographic approach involving HSCCC facilitated the separation of CTTs that coelute in unidimensional GC. Furthermore, the creation of 2D contour plots may provide a useful means of enhancing data visualization for other offline two-dimensional separations.

  12. Overview of online two-dimensional liquid chromatography based on cell membrane chromatography for screening target components from traditional Chinese medicines.

    Science.gov (United States)

    Muhammad, Saqib; Han, Shengli; Xie, Xiaoyu; Wang, Sicen; Aziz, Muhammad Majid

    2017-01-01

    Cell membrane chromatography is a simple, specific, and time-saving technique for studying drug-receptor interactions, screening of active components from complex mixtures, and quality control of traditional Chinese medicines. However, the short column life, low sensitivity, low column efficiency (so cannot resolve satisfactorily mixture of compounds), low peak capacity, and inefficient in structure identification were bottleneck in its application. Combinations of cell membrane chromatography with multidimensional chromatography such as two-dimensional liquid chromatography and high sensitivity detectors like mass have significantly reduced many of the above-mentioned shortcomings. This paper provides an overview of the current advances in online two-dimensional-based cell membrane chromatography for screening target components from traditional Chinese medicines with particular emphasis on the instrumentation, preparation of cell membrane stationary phase, advantages, and disadvantages compared to alternative approaches. The last section of the review summarizes the applications of the online two-dimensional high-performance liquid chromatography based cell membrane chromatography reported since its emergence to date (2010-June 2016). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Optimizing separations in online comprehensive two‐dimensional liquid chromatography

    Science.gov (United States)

    Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2017-01-01

    Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high‐molecular‐weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one‐dimensional liquid chromatography, two‐dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two‐dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two‐dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two‐dimensional liquid chromatography separations. PMID:29027363

  15. Tunable secondary dimension selectivity in comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Mommers, J.; Pluimakers, G.; Knooren, J.; Dutriez, T.; van der Wal, S.

    2013-01-01

    In this paper two tunable two-dimensional gas chromatography setups are compared and described in which the secondary dimension consists of two different capillary columns coupled in series. In the first setup the selectivity of the second dimension can be tuned by adjusting the effective column

  16. Two-dimensional ion chromatography for the separation of ionic organophosphates generated in thermally decomposed lithium hexafluorophosphate-based lithium ion battery electrolytes.

    Science.gov (United States)

    Kraft, Vadim; Grützke, Martin; Weber, Waldemar; Menzel, Jennifer; Wiemers-Meyer, Simon; Winter, Martin; Nowak, Sascha

    2015-08-28

    A two-dimensional ion chromatography (IC/IC) technique with heart-cutting mode for the separation of ionic organophosphates was developed. These analytes are generated during thermal degradation of three different commercially available Selectilyte™ lithium ion battery electrolytes. The composition of the investigated electrolytes is based on 1M lithium hexafluorophosphate (LiPF6) dissolved in ethylene carbonate/dimethyl carbonate (50:50wt%, LP30), ethylene carbonate/diethyl carbonate (50:50wt%, LP40) and ethylene carbonate/ethyl methyl carbonate (50:50wt%, LP50). The organophosphates were pre-separated from PF6(-) anion on the low capacity A Supp 4 column, which was eluted with a gradient step containing acetonitrile. The fraction containing analytes was retarded on a pre-concentration column and after that transferred to the high capacity columns, where the separation was performed isocratically. Different stationary phases and eluents were applied on the 2nd dimension for the investigation of retention times, whereas the highly promising results were obtained with a high capacitive A Supp 10 column. The organophosphates generated in LP30 and LP40 electrolytes could be separated by application of an aqueous NaOH eluent providing fast analysis time within 35min. For the separation of the organophosphates of LP50 electrolyte due to its complexity a NaOH eluent containing a mixture of methanol/H2O was necessary. In addition, the developed two dimensional IC method was hyphenated to an inductively coupled plasma mass spectrometer (ICP-MS) using aqueous NaOH without organic modifiers. This proof of principle measurement was carried out for future quantitative investigation regarding the concentration of the ionic organophosphates. Furthermore, the chemical stability of several ionic organophosphates in water and acetonitrile at room temperature over a period of 10h was investigated. In both solvents no decomposition of the investigated analytes was observed and

  17. Two-dimensional ion effects in relativistic diodes

    International Nuclear Information System (INIS)

    Poukey, J.W.

    1975-01-01

    In relativistic diodes, ions are emitted from the anode plasma. The effects and properties of these ions are studied via a two-dimensional particle simulation code. The space charge of these ions enhances the electron emission, and this additional current (including that of the ions, themselves) aids in obtaining superpinched electron beams for use in pellet fusion studies. (U.S.)

  18. Comprehensive two-dimensional gas chromatography applied to illicit drug analysis.

    Science.gov (United States)

    Mitrevski, Blagoj; Wynne, Paul; Marriott, Philip J

    2011-11-01

    Multidimensional gas chromatography (MDGC), and especially its latest incarnation--comprehensive two-dimensional gas chromatography (GC × GC)--have proved advantageous over and above classic one-dimensional gas chromatography (1D GC) in many areas of analysis by offering improved peak capacity, often enhanced sensitivity and, especially in the case of GC × GC, the unique feature of 'structured' chromatograms. This article reviews recent advances in MDGC and GC × GC in drug analysis with special focus on ecstasy, heroin and cocaine profiling. Although 1D GC is still the method of choice for drug profiling in most laboratories because of its simplicity and instrument availability, GC × GC is a tempting proposition for this purpose because of its ability to generate a higher net information content. Effluent refocusing due to the modulation (compression) process, combined with the separation on two 'orthogonal' columns, results in more components being well resolved and therefore being analytically and statistically useful to the profile. The spread of the components in the two-dimensional plots is strongly dependent on the extent of retention 'orthogonality' (i.e. the extent to which the two phases possess different or independent retention mechanisms towards sample constituents) between the two columns. The benefits of 'information-driven' drug profiling, where more points of reference are usually required for sample differentiation, are discussed. In addition, several limitations in application of MDGC in drug profiling, including data acquisition rate, column temperature limit, column phase orthogonality and chiral separation, are considered and discussed. Although the review focuses on the articles published in the last decade, a brief chronological preview of the profiling methods used throughout the last three decades is given.

  19. A four dimensional separation method based on continuous heart-cutting gas chromatography with ion mobility and high resolution mass spectrometry.

    Science.gov (United States)

    Lipok, Christian; Hippler, Jörg; Schmitz, Oliver J

    2018-02-09

    A two-dimensional GC (2D-GC) method was developed and coupled to an ion mobility-high resolution mass spectrometer, which enables the separation of complex samples in four dimensions (2D-GC, ion mobilility spectrometry and mass spectrometry). This approach works as a continuous multiheart-cutting GC-system (GC+GC), using a long modulation time of 20s, which allows the complete transfer of most of the first dimension peaks to the second dimension column without fractionation, in comparison to comprehensive two-dimensional gas chromatography (GCxGC). Hence, each compound delivers only one peak in the second dimension, which simplifies the data handling even when ion mobility spectrometry as a third and mass spectrometry as a fourth dimension are introduced. The analysis of a plant extract from Calendula officinales shows the separation power of this four dimensional separation method. The introduction of ion mobility spectrometry provides an additional separation dimension and allows to determine collision cross sections (CCS) of the analytes as a further physicochemical constant supporting the identification. A CCS database with more than 800 standard substances including drug-like compounds and pesticides was used for CCS data base search in this work. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Purification of lignans from Fructus Arctii using off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography.

    Science.gov (United States)

    Yang, Bichao; Xin, Huaxia; Wang, Feier; Cai, Jianfeng; Liu, Yanfang; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-08-01

    As a common traditional Chinese medicine, Fructus Arctii has important clinical medical values. Its main components are lignans, which are difficult to separate and analyze because of the complex composition, similar chemical structures, and close properties. In this study, an off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method, as well as an effective sample pretreatment method based on hydrophilic interaction chromatography material, was developed to enrich the minor lignan fractions and obtain high-purity compounds. In total, 12 high-purity compounds were isolated from Fructus Arctii. Their structures were identified by using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy, which showed that all were lignans and that most of them were isomers. The results demonstrated the effective off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method for the purification of lignans from Fructus Arctii. The separation protocol established here will be beneficial for the separation of complex samples from other kinds of natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

    Science.gov (United States)

    Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

    2014-03-01

    In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  2. Using Ion Exchange Chromatography to Separate and Quantify Complex Ions

    Science.gov (United States)

    Johnson, Brian J.

    2014-01-01

    Ion exchange chromatography is an important technique in the separation of charged species, particularly in biological, inorganic, and environmental samples. In this experiment, students are supplied with a mixture of two substitution-inert complex ions. They separate the complexes by ion exchange chromatography using a "flash"…

  3. Two-dimensional liquid chromatography consisting of twelve second-dimension columns for comprehensive analysis of intact proteins.

    Science.gov (United States)

    Ren, Jiangtao; Beckner, Matthew A; Lynch, Kyle B; Chen, Huang; Zhu, Zaifang; Yang, Yu; Chen, Apeng; Qiao, Zhenzhen; Liu, Shaorong; Lu, Joann J

    2018-05-15

    A comprehensive two-dimensional liquid chromatography (LCxLC) system consisting of twelve columns in the second dimension was developed for comprehensive analysis of intact proteins in complex biological samples. The system consisted of an ion-exchange column in the first dimension and the twelve reverse-phase columns in the second dimension; all thirteen columns were monolithic and prepared inside 250 µm i.d. capillaries. These columns were assembled together through the use of three valves and an innovative configuration. The effluent from the first dimension was continuously fractionated and sequentially transferred into the twelve second-dimension columns, while the second-dimension separations were carried out in a series of batches (six columns per batch). This LCxLC system was tested first using standard proteins followed by real-world samples from E. coli. Baseline separation was observed for eleven standard proteins and hundreds of peaks were observed for the real-world sample analysis. Two-dimensional liquid chromatography, often considered as an effective tool for mapping proteins, is seen as laborious and time-consuming when configured offline. Our online LCxLC system with increased second-dimension columns promises to provide a solution to overcome these hindrances. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. Two-dimensional analysis of trapped-ion eigenmodes

    International Nuclear Information System (INIS)

    Marchand, R.; Tang, W.M.; Rewoldt, G.

    1979-11-01

    A fully two-dimensional eigenmode analysis of the trapped-ion instability in axisymmetric toroidal geometry is presented. The calculations also takes into account the basic dynamics associated with other low frequency modes such as the trapped-electron instability and the ion-temperature-gradient instability. The poloidal structure of the mode is taken into account by Fourier expanding the perturbed electrostatic potential, PHI, in theta

  5. Quantitative analysis of target components by comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Mispelaar, V.G. van; Tas, A.C.; Smilde, A.K.; Schoenmakers, P.J.; Asten, A.C. van

    2003-01-01

    Quantitative analysis using comprehensive two-dimensional (2D) gas chromatography (GC) is still rarely reported. This is largely due to a lack of suitable software. The objective of the present study is to generate quantitative results from a large GC x GC data set, consisting of 32 chromatograms.

  6. Bayesian approach for peak detection in two-dimensional chromatography.

    Science.gov (United States)

    Vivó-Truyols, Gabriel

    2012-03-20

    A new method for peak detection in two-dimensional chromatography is presented. In a first step, the method starts with a conventional one-dimensional peak detection algorithm to detect modulated peaks. In a second step, a sophisticated algorithm is constructed to decide which of the individual one-dimensional peaks have been originated from the same compound and should then be arranged in a two-dimensional peak. The merging algorithm is based on Bayesian inference. The user sets prior information about certain parameters (e.g., second-dimension retention time variability, first-dimension band broadening, chromatographic noise). On the basis of these priors, the algorithm calculates the probability of myriads of peak arrangements (i.e., ways of merging one-dimensional peaks), finding which of them holds the highest value. Uncertainty in each parameter can be accounted by adapting conveniently its probability distribution function, which in turn may change the final decision of the most probable peak arrangement. It has been demonstrated that the Bayesian approach presented in this paper follows the chromatographers' intuition. The algorithm has been applied and tested with LC × LC and GC × GC data and takes around 1 min to process chromatograms with several thousands of peaks.

  7. Folding two dimensional crystals by swift heavy ion irradiation

    International Nuclear Information System (INIS)

    Ochedowski, Oliver; Bukowska, Hanna; Freire Soler, Victor M.; Brökers, Lara; Ban-d'Etat, Brigitte; Lebius, Henning; Schleberger, Marika

    2014-01-01

    Ion irradiation of graphene, the showcase model of two dimensional crystals, has been successfully applied to induce various modifications in the graphene crystal. One of these modifications is the formation of origami like foldings in graphene which are created by swift heavy ion irradiation under glancing incidence angle. These foldings can be applied to locally alter the physical properties of graphene like mechanical strength or chemical reactivity. In this work we show that the formation of foldings in two dimensional crystals is not restricted to graphene but can be applied for other materials like MoS 2 and hexagonal BN as well. Further we show that chemical vapour deposited graphene forms foldings after swift heavy ion irradiation while chemical vapour deposited MoS 2 does not

  8. Profiling analysis of low molecular weight heparins by multiple heart-cutting two dimensional chromatography with quadruple time-of-flight mass spectrometry.

    Science.gov (United States)

    Ouyang, Yilan; Zeng, Yangyang; Rong, Yinxiu; Song, Yue; Shi, Lv; Chen, Bo; Yang, Xinlei; Xu, Naiyu; Linhardt, Robert J; Zhang, Zhenqing

    2015-09-01

    Low molecular weight heparins (LMWHs) are polydisperse and microheterogenous mixtures of polysaccharides used as anticoagulant drugs. Profiling analysis is important for obtaining deeper insights into the structure of LMWHs. Previous oligosaccharide mapping methods are relatively low resolution and are unable to show an entire picture of the structural complexity of LMWHs. In the current study a profiling method was developed relying on multiple heart-cutting, two-dimensional, ultrahigh performance liquid chromatography with quadruple time-of-flight mass spectrometry. This represents an efficient, automated, and robust approach for profiling LMWHs. Using size-exclusion chromatography and ion-pairing reversed-phase chromatography in a two-dimensional separation, LMW components of different sizes and LMW components of the same size but with different charges and polarities can be resolved, providing a more complete picture of a LMWH. Structural information on each component was then obtained with quadrupole time-of-flight mass spectrometry. More than 80 and 120 oligosaccharides were observed and unambiguously assigned from the LMWHs, nadroparin and enoxaparin, respectively. This method might be useful for quality control of LMWHs and as a powerful tool for heparin-related glycomics.

  9. Nanoparticle Analysis by Online Comprehensive Two-Dimensional Liquid Chromatography combining Hydrodynamic Chromatography and Size-Exclusion Chromatography with Intermediate Sample Transformation

    Science.gov (United States)

    2017-01-01

    Polymeric nanoparticles have become indispensable in modern society with a wide array of applications ranging from waterborne coatings to drug-carrier-delivery systems. While a large range of techniques exist to determine a multitude of properties of these particles, relating physicochemical properties of the particle to the chemical structure of the intrinsic polymers is still challenging. A novel, highly orthogonal separation system based on comprehensive two-dimensional liquid chromatography (LC × LC) has been developed. The system combines hydrodynamic chromatography (HDC) in the first-dimension to separate the particles based on their size, with ultrahigh-performance size-exclusion chromatography (SEC) in the second dimension to separate the constituting polymer molecules according to their hydrodynamic radius for each of 80 to 100 separated fractions. A chip-based mixer is incorporated to transform the sample by dissolving the separated nanoparticles from the first-dimension online in tetrahydrofuran. The polymer bands are then focused using stationary-phase-assisted modulation to enhance sensitivity, and the water from the first-dimension eluent is largely eliminated to allow interaction-free SEC. Using the developed system, the combined two-dimensional distribution of the particle-size and the molecular-size of a mixture of various polystyrene (PS) and polyacrylate (PACR) nanoparticles has been obtained within 60 min. PMID:28745485

  10. Comprehensive two-dimensional gas chromatography for the analysis of organohalogenated micro-contaminants

    NARCIS (Netherlands)

    Korytar, P.; Haglund, P.; Boer, de J.; Brinkman, U.A.Th.

    2006-01-01

    We explain the principles of comprehensive two-dimensional gas chromatography (GC × GC), and discuss key instrumental aspects - with emphasis on column combinations and mass spectrometric detection. As the main item of interest, we review the potential of GC × GC for the analysis of

  11. Folding two dimensional crystals by swift heavy ion irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Ochedowski, Oliver; Bukowska, Hanna [Fakultät für Physik and CENIDE, Universität Duisburg-Essen, D-47048 Duisburg (Germany); Freire Soler, Victor M. [Fakultät für Physik and CENIDE, Universität Duisburg-Essen, D-47048 Duisburg (Germany); Departament de Fisica Aplicada i Optica, Universitat de Barcelona, E08028 Barcelona (Spain); Brökers, Lara [Fakultät für Physik and CENIDE, Universität Duisburg-Essen, D-47048 Duisburg (Germany); Ban-d' Etat, Brigitte; Lebius, Henning [CIMAP (CEA-CNRS-ENSICAEN-UCBN), 14070 Caen Cedex 5 (France); Schleberger, Marika, E-mail: marika.schleberger@uni-due.de [Fakultät für Physik and CENIDE, Universität Duisburg-Essen, D-47048 Duisburg (Germany)

    2014-12-01

    Ion irradiation of graphene, the showcase model of two dimensional crystals, has been successfully applied to induce various modifications in the graphene crystal. One of these modifications is the formation of origami like foldings in graphene which are created by swift heavy ion irradiation under glancing incidence angle. These foldings can be applied to locally alter the physical properties of graphene like mechanical strength or chemical reactivity. In this work we show that the formation of foldings in two dimensional crystals is not restricted to graphene but can be applied for other materials like MoS{sub 2} and hexagonal BN as well. Further we show that chemical vapour deposited graphene forms foldings after swift heavy ion irradiation while chemical vapour deposited MoS{sub 2} does not.

  12. Assessing the detectability of antioxidants in two-dimensional high-performance liquid chromatography.

    Science.gov (United States)

    Bassanese, Danielle N; Conlan, Xavier A; Barnett, Neil W; Stevenson, Paul G

    2015-05-01

    This paper explores the analytical figures of merit of two-dimensional high-performance liquid chromatography for the separation of antioxidant standards. The cumulative two-dimensional high-performance liquid chromatography peak area was calculated for 11 antioxidants by two different methods--the areas reported by the control software and by fitting the data with a Gaussian model; these methods were evaluated for precision and sensitivity. Both methods demonstrated excellent precision in regards to retention time in the second dimension (%RSD below 1.16%) and cumulative second dimension peak area (%RSD below 3.73% from the instrument software and 5.87% for the Gaussian method). Combining areas reported by the high-performance liquid chromatographic control software displayed superior limits of detection, in the order of 1 × 10(-6) M, almost an order of magnitude lower than the Gaussian method for some analytes. The introduction of the countergradient eliminated the strong solvent mismatch between dimensions, leading to a much improved peak shape and better detection limits for quantification. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Trends in data processing of comprehensive two-dimensional chromatography: state of the art.

    Science.gov (United States)

    Matos, João T V; Duarte, Regina M B O; Duarte, Armando C

    2012-12-01

    The operation of advanced chromatographic systems, namely comprehensive two-dimensional (2D) chromatography coupled to multidimensional detectors, allows achieving a great deal of data that need special care to be processed in order to characterize and quantify as much as possible the analytes under study. The aim of this review is to identify the main trends, research needs and gaps on the techniques for data processing of multidimensional data sets obtained from comprehensive 2D chromatography. The following topics have been identified as the most promising for new developments in the near future: data acquisition and handling, peak detection and quantification, measurement of overlapping of 2D peaks, and data analysis software for 2D chromatography. The rational supporting most of the data processing techniques is based on the generalization of one-dimensional (1D) chromatography although algorithms, such as the inverted watershed algorithm, use the 2D chromatographic data as such. However, for processing more complex N-way data there is a need for using more sophisticated techniques. Apart from using other concepts from 1D chromatography, which have not been tested for 2D chromatography, there is still room for new improvements and developments in algorithms and software for dealing with 2D comprehensive chromatographic data. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Comparative analysis of peak-detection techniques for comprehensive two-dimensional chromatography.

    Science.gov (United States)

    Latha, Indu; Reichenbach, Stephen E; Tao, Qingping

    2011-09-23

    Comprehensive two-dimensional gas chromatography (GC×GC) is a powerful technology for separating complex samples. The typical goal of GC×GC peak detection is to aggregate data points of analyte peaks based on their retention times and intensities. Two techniques commonly used for two-dimensional peak detection are the two-step algorithm and the watershed algorithm. A recent study [4] compared the performance of the two-step and watershed algorithms for GC×GC data with retention-time shifts in the second-column separations. In that analysis, the peak retention-time shifts were corrected while applying the two-step algorithm but the watershed algorithm was applied without shift correction. The results indicated that the watershed algorithm has a higher probability of erroneously splitting a single two-dimensional peak than the two-step approach. This paper reconsiders the analysis by comparing peak-detection performance for resolved peaks after correcting retention-time shifts for both the two-step and watershed algorithms. Simulations with wide-ranging conditions indicate that when shift correction is employed with both algorithms, the watershed algorithm detects resolved peaks with greater accuracy than the two-step method. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Trimodal Mixed Mode Chromatography That Enables Efficient Offline Two-Dimensional Peptide Fractionation for Proteome Analysis.

    Science.gov (United States)

    Yu, Peng; Petzoldt, Svenja; Wilhelm, Mathias; Zolg, Daniel Paul; Zheng, Runsheng; Sun, Xuefei; Liu, Xiaodong; Schneider, Günter; Huhmer, Andreas; Kuster, Bernhard

    2017-09-05

    Offline two-dimensional chromatography is a common means to achieve deep proteome coverage. To reduce sample complexity and dynamic range and to utilize mass spectrometer (MS) time efficiently, high chromatographic resolution of and good orthogonality between the two dimensions are needed. Ion exchange and high pH reversed phase chromatography are often used for this purpose. However, the former requires desalting to be MS-compatible, and the latter requires fraction pooling to create orthogonality. Here, we report an alternative first-dimension separation technique using a commercial trimodal phase incorporating polar embedded reversed phase, weak anion exchange, and strong cation exchange material. The column is capable of retaining polar and nonpolar peptides alike without noticeable breakthrough. It allows separating ordinary and TMT-labeled peptides under mild acidic conditions using an acetonitrile gradient. The direct MS compatibility of solvents and good orthogonality to online coupled C18 columns enable a straightforward workflow without fraction pooling and desalting while showing comparable performance to the other techniques. The method scales from low to high microgram sample quantity and is amenable to full automation. To demonstrate practical utility, we analyzed the proteomes of 10 human pancreatic cancer cell lines to a depth of >8,700 quantified proteins.

  16. Comprehensive two-dimensional liquid chromatography with on-line Fourier-transform-infrared-spectroscopy detection for the characterization of copolymers

    NARCIS (Netherlands)

    Kok, S.J.; Hankemeier, T.; Schoenmakers, P.J.

    2005-01-01

    The on-line coupling of comprehensive two-dimensional liquid chromatography (liquid chromatography × size-exclusion chromatography, LC × SEC) and infrared (IR) spectroscopy has been realized by means of an IR flow cell. The system has been assessed by the functional-group analysis of a series of

  17. Qualitative and quantitative two-dimensional thin-layer chromatography/high performance liquid chromatography/diode-array/electrospray-ionization-time-of-flight mass spectrometry of cholinesterase inhibitors.

    Science.gov (United States)

    Mroczek, Tomasz

    2016-09-10

    Recently launched thin-layer chromatography-mass spectrometry (TLC-MS) interface enabling extraction of compounds directly from TLC plates into MS ion source was unusually extended into two-dimensional thin-layer chromatography/high performance liquid chromatography (2D, TLC/HPLC) system by its a direct connection to a rapid resolution 50×2.1mm, I.D. C18 column compartment followed by detection by diode array (DAD) and electrospray ionisation time-of-flight mass spectrometry (ESI-TOF-MS). In this way, even not separated bands of complicated mixtures of natural compounds could be analysed structurally, only within 1-2min after development of TLC plates. In comparison to typically applied TLC-MS interface, no ion suppression for acidic mobile phases was observed. Also, substantial increase in ESI-TOF-MS sensitivities and quality of spectra, were noticed. It has been utilised in combination with TLC- based bioautographic approaches of acetylcholinesterase (AChE) inhibitors, However, it can be also applied in any other procedures related to bioactivity (e.g. 2,2-Diphenyl-1-picryl-hydrazyl-DPPH screen test for radicals). This system has been also used for determination of half maximal inhibitory concentration (IC50 values) of the active inhibitor-galanthamine, as an example. Moreover, AChE inhibitory potencies of some of purified plant extracts, never studied before, have been quantitatively measured. This is first report of usage such the 2D TLC/HPLC/MS system both for qualitative and quantitative evaluation of cholinesterase inhibitors in biological matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Separation and analysis of phenolic acids from Salvia miltiorrhiza and its related preparations by off-line two-dimensional hydrophilic interaction chromatography×reversed-phase liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Sun, Wanyang; Tong, Ling; Miao, Jingzhuo; Huang, Jingyi; Li, Dongxiang; Li, Yunfei; Xiao, Hongting; Sun, Henry; Bi, Kaishun

    2016-01-29

    Salvia miltiorrhiza (SM) is one of the most widely used Traditional Chinese Medicine. Active constituents of SM mainly contain hydrophilic phenolic acids (PAs) and lipophilic tanshinones. However, due to the existing of multiple ester bonds and unsaturated bonds in the structures, PAs have numerous chemical conversion products. Many of them are so low-abundant that hard to be separated using conventional methods. In this study, an off-line two-dimensional liquid chromatography (2D-LC) method was developed to separate PAs in SM and its related preparations. In the first dimension, samples were fractionated by hydrophilic interaction chromatography (HILIC) (Acchrom×Amide, 4.6×250mm, 5μm) mainly based on the hydrogen bonding effects. The fractions were then separated on reversed-phase liquid chromatography (RP-LC) (Acquity HSS T3, 2.1×50mm, 1.7μm) according to hydrophobicity. For the selective identification of PAs, diode array detector (DAD) and electrospray ionization tandem ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) were employed. Practical and effective peak capacities of all the samples were greater than 2046 and 1130, respectively, with the orthogonalities ranged from 69.7% to 92.8%, which indicated the high efficiency and versatility of this method. By utilizing the data post-processing techniques, including mass defect filter, neutral loss filter and product ion filter, a total of 265 compounds comprising 196 potentially new PAs were tentatively characterized. Twelve kinds of derivatives, mainly including glycosylated compounds, O-alkylated compounds, condensed compounds and hydrolyzed compounds, constituted the novelty of the newly identified PAs. The HILIC×RP-LC/TOF-MS system expanded our understanding on PAs of S. miltiorrhiza and its related preparations, which could also benefit the separation and characterization of polar constituents in complicated herbal extracts. Copyright © 2016. Published by Elsevier B.V.

  19. Ion distributions in a two-dimensional reconnection field geometry

    International Nuclear Information System (INIS)

    Curran, D.B.; Goertz, C.K.; Whelan, T.A.

    1987-01-01

    ISEE observations have shown trapped ion distributions in the magnetosphere along with streaming ion distributions in the magnetosheath. The more energetic ion beams are found to exist further away from the magnetopause than lower-energy ion beams. In order to understand these properties of the data, we have taken a simple two-dimensional reconnection model which contains a neutral line and an azimuthal electric field and compared its predictions with the experimental data of September 8, 1978. Our model explains trapped particles in the magnetosphere due to nonadiabatic mirroring in the magnetosheath and streaming ions in the magnetosheath due to energization at the magnetopause. The model also shows the higher-energy ions extending further into the magnetosheath, away from the magnetopause than the lower-energy ions. This suggests the ion data of September 8, 1978 are consistent with a reconnection geometry. Copyright American Geophysical Union 1987

  20. Pulsed flow modulation two-dimensional comprehensive gas chromatography-tandem mass spectrometry with supersonic molecular beams.

    Science.gov (United States)

    Poliak, Marina; Fialkov, Alexander B; Amirav, Aviv

    2008-11-07

    Pulsed flow modulation (PFM) two-dimensional comprehensive gas chromatography (GC x GC) was combined with quadrupole-based mass spectrometry (MS) via a supersonic molecular beam (SMB) interface using a triple-quadrupole system as the base platform, which enabled tandem mass spectrometry (MS-MS). PFM is a simple GC x GC modulator that does not consume cryogenic gases while providing tunable second GC x GC column injection time for enabling the use of quadrupole-based mass spectrometry regardless its limited scanning speed. The 20-ml/min second column flow rate involved with PFM is handled, splitless, by the SMB interface without affecting the sensitivity. The combinations of PFM GC x GC-MS with SMB and PFM GC x GC-MS-MS with SMB were explored with the analysis of diazinon and permethrin in coriander. PFM GC x GC-MS with SMB is characterized by enhanced molecular ion and tailing-free fast ion source response time. It enables universal pesticide analysis with full scan and data analysis with reconstructed single ion monitoring on the enhanced molecular ion and another prominent high mass fragment ion. The elimination of the third fragment ion used in standard three ions method results in significantly reduced matrix interference. GC x GC-MS with SMB improves the GC separation, and thereby our ability for sample identification using libraries. GC-MS-MS with SMB provides better reduction (elimination) of matrix interference than GC x GC-MS. However, it is a target method, which is not always applicable. GC x GC-MS-MS does not seem to further reduce matrix interferences over GC-MS-MS and unlike GC x GC-MS, it is incompatible with library identification, but it is beneficial to have both GC x GC and MS-MS capabilities in the same system.

  1. Two-dimensional liquid chromatography

    DEFF Research Database (Denmark)

    Græsbøll, Rune

    -dimensional separation space. Optimization of gradients in online RP×RP is more difficult than in normal HPLC as a result of the increased number of parameters and their influence on each other. Modeling the coverage of the compounds across the two-dimensional chromatogram as a result of a change in gradients could...... be used for optimization purposes, and reduce the time spend on optimization. In this thesis (chapter 6), and manuscript B, a measure of the coverage of the compounds in the twodimensional separation space is defined. It is then shown that this measure can be modeled for changes in the gradient in both...

  2. Chromium Speciation Analysis by Ion Chromatography Coupled ...

    African Journals Online (AJOL)

    Two methods coupling ion chromatography with inductively coupled plasma - optical emission spectroscopy (ICP-OES) were developed for the simultaneous separation and determination of Cr(III) and Cr(VI) species. In the first method, anion chromatography with sodium bicarbonate/carbonate solution as the eluent was ...

  3. [Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography- reversed-phase liquid chromatography].

    Science.gov (United States)

    Jia, Youmei; Cai, Jianfeng; Xin, Huaxia; Feng, Jiatao; Fu, Yanhui; Fu, Qing; Jin, Yu

    2017-06-08

    A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography (Pre-2D-HILIC/RPLC) method was established to separate and purify the components in Trachelospermum jasminoides . The pigments and strongly polar components were removed from the crude extract after the active carbon decolorization and solid phase extraction processes. A Click XIon column (250 mm×20 mm, 10 μm) was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC. Finally, 15 fractions were collected under UV-triggered mode. In the second dimensional RPLC, a C18 column (250 mm×20 mm, 5 μm) was selected and water-acetonitrile was used as mobile phases. As a result, 14 compounds with high purity were obtained, which were further identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). Finally, 11 lignan compounds and three flavonoid compounds were obtained. The method has a good orthogonality, and can improve the resolution and the peak capacity. It is significant for the separation of complex components from Trachelospermum jasminoides .

  4. Probability of failure of the watershed algorithm for peak detection in comprehensive two-dimensional chromatography

    NARCIS (Netherlands)

    Vivó-Truyols, G.; Janssen, H.-G.

    2010-01-01

    The watershed algorithm is the most common method used for peak detection and integration In two-dimensional chromatography However, the retention time variability in the second dimension may render the algorithm to fail A study calculating the probabilities of failure of the watershed algorithm was

  5. Two novel haemoglobin variants that affect haemoglobin A1c measurement by ion-exchange chromatography

    NARCIS (Netherlands)

    Bots, Michael; Stroobants, An K.; Delzenne, Barend; Soeters, Maarten R.; de Vries, Johan E.; Weykamp, Cas W.; Norg, Roelf J. C.; Veldthuis, Martijn; van Zwieten, Rob

    2015-01-01

    Haemoglobin (Hb) variants are well-known factors interfering with accurate HbA1c testing. This report describes two novel Hb variants leading to inappropriate quantification of HbA1c by ion-exchange chromatography. Glycated forms of novel Hb variants were recognised in the blood of two patients with

  6. Study of Separation and Identification of the Active Ingredients in Gardenia jasminoides Ellis Based on a Two-Dimensional Liquid Chromatography by Coupling Reversed Phase Liquid Chromatography and Hydrophilic Interaction Liquid Chromatography.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2017-01-01

    In this paper, by coupling reversed phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), a two-dimensional liquid chromatography system was developed for separation and identification of the active ingredients in Gardenia jasminoides Ellis (GJE). By applying the semi-preparative C18 column as the first dimension and the core-shell column as the second dimension, a total of 896 peaks of GJE were separated. Among the 896 peaks, 16 active ingredients including geniposide, gardenoside, gardoside, etc. were identified by mass spectrometry analysis. The results indicated that the proposed two-dimensional RPLC/HILIC system was an effective method for the analysis of GJE and might hold a high potential to become a useful tool for analysis of other complex mixtures. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  7. Improved determination of flavour compounds in butter by solid-phase (micro)extraction and comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Adahchour, M.; Wiewel, J.; Verdel, R.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2005-01-01

    The practicability and potential of comprehensive two-dimensional gas chromatography (GC × GC) coupled to both conventional flame ionisation (FID) and time-of-flight mass spectrometric (TOF-MS) detection, were compared with those of conventional one-dimensional (1D) GC, with the determination of

  8. Ion Chromatography Applications in Wastewater Analysis

    Directory of Open Access Journals (Sweden)

    Rajmund Michalski

    2018-02-01

    Full Text Available Wastewater analysis is an important area in analytical and environmental chemistry. It can be performed with both the classic wet methods and instrumental techniques. The development of new methods, and modification of the existing ones, constitute a major task for researchers. Ion chromatography plays a predominant role in ion determinations with the instrumental methods. It offers several advantages over the conventional methods, such as simultaneous determinations of alkali and alkaline earth cations and ammonia. Ammonium ions cannot be determined by spectroscopic methods. Ion chromatography has been accepted world-wide as a reference method for analyzing anions and cations in water and wastewater due to the fact that it enables the replacement of several individual wet chemistry methods for common ions with one instrumental technique. The following article describes the principles of ion chromatography, such as stationary phases, eluents, detectors, and sample preparation methods. Moreover, the applications of ion chromatography in wastewater analyses and international standards are presented.

  9. Design and implementation of an array of micro-electrochemical detectors for two-dimensional liquid chromatography--proof of principle.

    Science.gov (United States)

    Abia, Jude A; Putnam, Joel; Mriziq, Khaled; Guiochon, Georges A

    2010-03-05

    Simultaneous two-dimensional liquid chromatography (2D-LC) is an implementation of two-dimensional liquid chromatography which has the potential to provide very fast, yet highly efficient separations. It is based on the use of time x space and space x space separation systems. The basic principle of this instrument has been validated long ago by the success of two-dimensional thin layer chromatography. The construction of a pressurized wide and flat column (100 mm x 100 mm x 1 mm) operated under an inlet pressure of up to 50 bar was described previously. However, to become a modern analytical method, simultaneous 2D-LC requires the development of detectors suitable for the monitoring of the composition of the eluent of this pressurized planar, wide column. An array of five equidistant micro-electrochemical sensors was built for this purpose and tested. Each sensor is a three-electrode system, with the working electrode being a 25 microm polished platinum micro-electrode. The auxiliary electrode is a thin platinum wire and the reference electrode an Ag/AgCl (3M sat. KCl) electrode. In this first implementation, proof of principle is demonstrated, but the final instrument will require a much larger array. 2010 Elsevier B.V. All rights reserved.

  10. Simultaneous Determination of Chelating Agents by Ion-Suppression and Ion-Pair Chromatography in Wastewater

    International Nuclear Information System (INIS)

    Dodi, Alain; Bouscarel, Maelle

    2008-01-01

    This article describes two methods for analysing chelating agents found in nuclear waste. First, ion-suppression chromatography using an anion exchange stationary phase and mobile phase consisting of a nitric acid solution and pure water gradient. UV detection was performed at 330 nm after the reaction with a post-column reagent composed of iron nitrate in perchloric acid. Secondly, ion-pair chromatography with a mobile phase consisting of a mixture of nitric acid, tetra-butyl-ammonium hydrogeno-sulphate, tetra-butyl-ammonium hydroxide and iron chloride. A reversed-phase material was used as a stationary phase and detection was performed by direct measurement of the UV absorption at 260 nm. The quantification limits were lower for ion-pair chromatography than for ion-suppression chromatography. Both methods were easy to implement and allow a multi-element separation in less than 30 min with low detection limits. (authors)

  11. Simultaneous Determination of Chelating Agents by Ion-Suppression and Ion-Pair Chromatography in Wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Dodi, Alain; Bouscarel, Maelle [Commissariat a l' energie atomique - C.E.A, Centre d' Etude de Cadarache, Laboratoire d' Analyses Radiochimiques et Chimiques, St Paul lez Durance (France)

    2008-07-01

    This article describes two methods for analysing chelating agents found in nuclear waste. First, ion-suppression chromatography using an anion exchange stationary phase and mobile phase consisting of a nitric acid solution and pure water gradient. UV detection was performed at 330 nm after the reaction with a post-column reagent composed of iron nitrate in perchloric acid. Secondly, ion-pair chromatography with a mobile phase consisting of a mixture of nitric acid, tetra-butyl-ammonium hydrogeno-sulphate, tetra-butyl-ammonium hydroxide and iron chloride. A reversed-phase material was used as a stationary phase and detection was performed by direct measurement of the UV absorption at 260 nm. The quantification limits were lower for ion-pair chromatography than for ion-suppression chromatography. Both methods were easy to implement and allow a multi-element separation in less than 30 min with low detection limits. (authors)

  12. Optimizing gradient conditions in online comprehensive two-dimensional reversed-phase liquid chromatography by use of the linear solvent strength model

    DEFF Research Database (Denmark)

    Græsbøll, Rune; Janssen, Hans-Gerd; Christensen, Jan H.

    2017-01-01

    The linear solvent strength model was used to predict coverage in online comprehensive two-dimensional reversed-phase liquid chromatography. The prediction model uses a parallelogram to describe the separation space covered with peaks in a system with limited orthogonality. The corners of the par......The linear solvent strength model was used to predict coverage in online comprehensive two-dimensional reversed-phase liquid chromatography. The prediction model uses a parallelogram to describe the separation space covered with peaks in a system with limited orthogonality. The corners...... of the parallelogram are assumed to behave like chromatographic peaks and the position of these pseudo-compounds was predicted. A mix of 25 polycyclic aromatic compounds were used as a test. The precision of the prediction, span 0-25, was tested by varying input parameters, and was found to be acceptable with root...... factors were low, or when gradient conditions affected parameters not included in the model, e.g. second dimension gradient time affects the second dimension equilibration time. The concept shows promise as a tool for gradient optimization in online comprehensive two-dimensional liquid chromatography...

  13. Two-dimensional hydrodynamics of uniform ion plasma in electrostatic field

    International Nuclear Information System (INIS)

    Mahdieh, M. H.; Gavili, A.

    2005-01-01

    Two-dimensional hydrodynamics of ion extraction from uniform quasi-neutral plasma, in electrostatic field has been simulated numerically. Experimentally, tunable pulsed lasers produce non-uniform plasma through stepwise photo-excitation and photo-ionization or multi-photo-ionization processes. Poisson's equation was solved simultaneously with the equations of mass, and momentum, assuming the Maxwell-Boltzmann distribution for electrons. In the calculation, the initial density profile at the boundaries has been assumed to be very steep for the ion plasma. In these calculations dynamics of electric potential and the ions density were assessed. The ion extraction time was also estimated from the calculation. The knowledge of spatial distribution of the ions across the cathode is very important for the practical purposes. In this simulation, the spatial distribution of the ion current density across the cathode as well as its temporal distribution was calculated

  14. Characterisation of Stevia Rebaudiana by comprehensive two-dimensional liquid chromatography time-of-flight mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Pól, Jaroslav; Hohnová, B.; Hyötyläinen, T.

    2007-01-01

    Roč. 1150, 1-2 (2007), s. 85-92 ISSN 0021-9673 R&D Projects: GA AV ČR KJB4031405 Institutional research plan: CEZ:AV0Z40310501 Keywords : comprehensive two-dimensional liquid chromatography * time-of-flight mass spectrometry * Stevia rebaudiana Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.641, year: 2007

  15. [Determination of fatty acids in natural cream and artificial cream by comprehensive two-dimensional gas chromatography-mass spectrometry].

    Science.gov (United States)

    Zhou, Ruize; Zhou, Ya; Mao, Ting; Jiang, Jie

    2018-01-08

    A method for the determination of 37 fatty acids in natural cream and artificial cream was developed by comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS). The samples were extracted with toluene and acetyl chloride-methanol (1:9,v/v) solution was added to the extract for fat esterification. Finally, the fatty acids were analyzed by GC×GC-MS. The GC conditions were as follows:a DB-5 column (30 m×0.25 mm×0.25 μm) was set as the 1st dimensional column and a BPX-50 column (2.5 m×0.1 mm×0.25 μm) was the 2nd dimensional column. The primary oven temperature was programmed from 50℃ (held for 2 min) to 180℃ at a rate of 20℃/min, followed by an increase to 250℃ at 2.5℃/min, then raised up to 300℃ (held for 5 min) at 3℃/min. The ion source temperature was 200℃ with auxiliary temperature of 300℃ in scan mode. All fatty acids were separated effectively and determined accurately while the modulation period was 5s and the scan range of MS was m/z 40-385. This procedure was applied to analyze the fatty acids in commercial natural cream and artificial cream from Chinese markets, among which we found the characteristic components in different kinds of samples. Compared with gas chromatography-flame ionization detector (GC-FID), GC×GC-MS method was more sensitive and more components of fatty acids were detected. Conclusively, this work suggests a new technical approach in analyzing fatty acids in natural cream and artificial cream, which is meaningful to ensure the quality identification and safety of natural cream.

  16. Comprehensive two-dimensional gas chromatography and food sensory properties: potential and challenges.

    Science.gov (United States)

    Cordero, Chiara; Kiefl, Johannes; Schieberle, Peter; Reichenbach, Stephen E; Bicchi, Carlo

    2015-01-01

    Modern omics disciplines dealing with food flavor focus the analytical efforts on the elucidation of sensory-active compounds, including all possible stimuli of multimodal perception (aroma, taste, texture, etc.) by means of a comprehensive, integrated treatment of sample constituents, such as physicochemical properties, concentration in the matrix, and sensory properties (odor/taste quality, perception threshold). Such analyses require detailed profiling of known bioactive components as well as advanced fingerprinting techniques to catalog sample constituents comprehensively, quantitatively, and comparably across samples. Multidimensional analytical platforms support comprehensive investigations required for flavor analysis by combining information on analytes' identities, physicochemical behaviors (volatility, polarity, partition coefficient, and solubility), concentration, and odor quality. Unlike other omics, flavor metabolomics and sensomics include the final output of the biological phenomenon (i.e., sensory perceptions) as an additional analytical dimension, which is specifically and exclusively triggered by the chemicals analyzed. However, advanced omics platforms, which are multidimensional by definition, pose challenging issues not only in terms of coupling with detection systems and sample preparation, but also in terms of data elaboration and processing. The large number of variables collected during each analytical run provides a high level of information, but requires appropriate strategies to exploit fully this potential. This review focuses on advances in comprehensive two-dimensional gas chromatography and analytical platforms combining two-dimensional gas chromatography with olfactometry, chemometrics, and quantitative assays for food sensory analysis to assess the quality of a given product. We review instrumental advances and couplings, automation in sample preparation, data elaboration, and a selection of applications.

  17. Comprehensive two-dimensional gas chromatography for biogas and biomethane analysis.

    Science.gov (United States)

    Hilaire, F; Basset, E; Bayard, R; Gallardo, M; Thiebaut, D; Vial, J

    2017-11-17

    The gas industry is going to be revolutionized by being able to generate bioenergy from biomass. The production of biomethane - a green substitute of natural gas - is growing in Europe and the United-States of America. Biomethane can be injected into the gas grid or used as fuel for vehicles after compression. Due to various biomass inputs (e.g. agricultural wastes, sludges from sewage treatment plants, etc.), production processes (e.g. anaerobic digestion, municipal solid waste (MSW) landfills), seasonal effects and purification processes (e.g. gas scrubbers, pressure swing adsorption, membranes for biogas upgrading), the composition and quality of biogas and biomethane produced is difficult to assess. All previous publications dealing with biogas analysis reported that hundreds of chemicals from ten chemical families do exist in trace amounts in biogas. However, to the best of our knowledge, no study reported a detailed analysis or the implementation of comprehensive two-dimensional gas chromatography (GC×GC) for biogas matrices. This is the reason why the benefit of implementing two-dimensional gas chromatography for the characterization of biogas and biomethane samples was evaluated. In a first step, a standard mixture of 89 compounds belonging to 10 chemical families, representative of those likely to be found, was used to optimize the analytical method. A set consisting of a non-polar and a polar columns, respectively in the first and the second dimension, was used with a modulation period of six seconds. Applied to ten samples of raw biogas, treated biogas and biomethane collected on 4 industrial sites (two MSW landfills, one anaerobic digester on a wastewater treatment plant and one agricultural biogas plant), this analytical method provided a "fingerprint" of the gases composition at the molecular level in all biogas and biomethane samples. Estimated limits of detection (far below the μgNm -3 ) coupled with the resolution of GC×GC allowed the comparison

  18. Maximizing the peak production rate in off-line comprehensive two-dimensional liquid chromatography with mass spectrometry detection

    NARCIS (Netherlands)

    Eeltink, S.; Dolman, S.; Ursem, M.; Swart, R.; McLeod, F.; Schoenmakers, P.J.

    2009-01-01

    This article describes an optimization strategy to obtain the best possible performance in the shortest analysis time—called the peak production rate—for comprehensive off-line two-dimensional liquid chromatography. The demands on column technology (particle size and column length) and LC conditions

  19. Differentiating Fragmentation Pathways of Cholesterol by Two-Dimensional Fourier Transform Ion Cyclotron Resonance Mass Spectrometry.

    Science.gov (United States)

    van Agthoven, Maria A; Barrow, Mark P; Chiron, Lionel; Coutouly, Marie-Aude; Kilgour, David; Wootton, Christopher A; Wei, Juan; Soulby, Andrew; Delsuc, Marc-André; Rolando, Christian; O'Connor, Peter B

    2015-12-01

    Two-dimensional Fourier transform ion cyclotron resonance mass spectrometry is a data-independent analytical method that records the fragmentation patterns of all the compounds in a sample. This study shows the implementation of atmospheric pressure photoionization with two-dimensional (2D) Fourier transform ion cyclotron resonance mass spectrometry. In the resulting 2D mass spectrum, the fragmentation patterns of the radical and protonated species from cholesterol are differentiated. This study shows the use of fragment ion lines, precursor ion lines, and neutral loss lines in the 2D mass spectrum to determine fragmentation mechanisms of known compounds and to gain information on unknown ion species in the spectrum. In concert with high resolution mass spectrometry, 2D Fourier transform ion cyclotron resonance mass spectrometry can be a useful tool for the structural analysis of small molecules. Graphical Abstract ᅟ.

  20. Ion mobility: its role in plasma chromatography

    International Nuclear Information System (INIS)

    Mason, E.A.

    1984-01-01

    This paper is a review of the basic physical theory underlying plasma chromatography. Essentially, plasma chromatography simply measures ion mobility. The new feature of plasma chromatography, as compared to aqueous electrophoresis, is the existence of a highly-developed and accurate body of theory that connects gaseous ion mobility and diffusion to the ion molecule interactions in the drift tube. Attention is restricted to phenomena occurring in the drift tube portion of the apparatus

  1. Characterization of Secondary Organic Aerosol Precursors Using Two-Dimensional Gas-Chromatography

    Science.gov (United States)

    Roskamp, M.; Lou, W.; Pankow, J. F.; Harley, P. C.; Turnipseed, A.; Barsanti, K. C.

    2012-12-01

    The oxidation of volatile organic compounds (VOCs) plays a role in both regional and global air quality. However, field and laboratory research indicate that the body of knowledge around the identities, quantities and oxidation processes of these compounds in the ambient atmosphere is still incomplete (e.g., Goldstein & Galbally, 2007; Robinson et al., 2009). VOCs emitted to the atmosphere largely are of biogenic origin (Guenther et al., 2006), and many studies of ambient secondary organic aerosol (SOA) suggest that SOA is largely of biogenic origin (albeit closely connected to anthropogenic activities, e.g., de Gouw and Jimenez, 2009). Accurate modeling of SOA levels and properties will require a more complete understanding of biogenic VOCs (BOCs) and their atmospheric oxidation products. For example, satellite measurements indicate that biogenic VOC emissions are two to three times greater than levels currently included in models (Heald et al., 2010). Two-dimensional gas chromatography (GC×GC) is a powerful analytical technique that shows much promise in advancing the state-of-knowledge regarding BVOCs and their role in SOA formation. In this work, samples were collected during BEACHON-RoMBAS (Bio-hydro-atmosphere Interactions of Energy, Aerosols, Carbon, H2O, Organics & Nitrogen - Rocky Mountain Biogenic Aerosol Study) in July and August of 2011. The field site was a Ponderosa Pine forest near Woodland, CO, inside the Manitou Experimental Forest, which is operated by the US Forest Service. The area is characteristic of the central Rocky Mountains and trace gas monitoring indicates that little anthropogenic pollution is transported from the nearby urban areas (Kim et al. 2010 and references therein). Ambient and enclosure samples were collected on ATD (adsorption/thermal desorption) cartridges and analyzed for BVOCs using two-dimensional gas chromatography (GC×GC) with time of flight mass spectrometry (TOFMS) and flame ionized detection (FID). Measurements of

  2. Optimizing separations in online comprehensive two‐dimensional liquid chromatography

    OpenAIRE

    Pirok, Bob W.J.; Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2017-01-01

    Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass...

  3. Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

    Science.gov (United States)

    Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

    2016-02-01

    A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Recent developments in comprehensive two-dimensional gas chromatography (GC X GC) I. Introduction and instrumental set-up

    NARCIS (Netherlands)

    Adahchour, M.; Beens, J.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2006-01-01

    We review the literature on comprehensive two-dimensional gas chromatography (GC × GC), emphasizing developments in the period 2003-2005. The review opens with a general introduction, the principles of the technique and the set-up of GC × GC systems. It also discusses theoretical aspects, trends in

  5. Increasing flexibility in two-dimensional liquid chromatography by pulsed elution of the first dimension

    DEFF Research Database (Denmark)

    Jakobsen, Simon S.; Christensen, Jan H.; Verdier, Sylvain

    2017-01-01

    This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension...... online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity...

  6. Ion exchange and liquid column chromatography

    International Nuclear Information System (INIS)

    Walton, H.F.

    1980-01-01

    Major accomplishments in liquid chromatography for the past two years and reported in journals available to December 31, 1979 are reviewed. Emphasis has been placed on principles and methodology with some representative examples of application included. Applications are illustrated in two rather lenghtly tables, one covering inorganic ions and the other covering organic compounds. 544 references, 8 books, and 15 reviews are listed in the bibliography

  7. [Recent advances in analysis of petroleum geological samples by comprehensive two-dimensional gas chromatography].

    Science.gov (United States)

    Gao, Xuanbo; Chang, Zhenyang; Dai, Wei; Tong, Ting; Zhang, Wanfeng; He, Sheng; Zhu, Shukui

    2014-10-01

    Abundant geochemical information can be acquired by analyzing the chemical compositions of petroleum geological samples. The information obtained from the analysis provides scientifical evidences for petroleum exploration. However, these samples are complicated and can be easily influenced by physical (e. g. evaporation, emulsification, natural dispersion, dissolution and sorption), chemical (photodegradation) and biological (mainly microbial degradation) weathering processes. Therefore, it is very difficult to analyze the petroleum geological samples and they cannot be effectively separated by traditional gas chromatography/mass spectrometry. A newly developed separation technique, comprehensive two-dimensional gas chromatography (GC x GC), has unique advantages in complex sample analysis, and recently it has been applied to petroleum geological samples. This article mainly reviews the research progres- ses in the last five years, the main problems and the future research about GC x GC applied in the area of petroleum geology.

  8. Study of ion exchange equilibrium and determination of heat of ion exchange by ion chromatography

    International Nuclear Information System (INIS)

    Liu Kailu; Yang Wenying

    1996-01-01

    Ion chromatography using pellicularia ion exchange resins and dilute solution can be devoted to the study of ion exchange thermodynamics and kinetics. Ion exchange equilibrium equation was obtained, and examined by the experiments. Based on ion exchange equilibrium, the influence of eluent concentration and resin capacity on adjusted retention volumes was examined. The effect of temperature on adjusted retention volumes was investigated and heats of ion exchange of seven anions were determined by ion chromatography. The interaction between anions and skeleton structure of resins were observed

  9. Characterization of lipids in complex samples using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Jover, E.; Adahchour, M.; Bayona, J.M.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2005-01-01

    Most lipids are a complex mixture of classes of compounds such as fatty acids, fatty alcohols, diols, sterols and hydroxy acids. In this study, the suitability of comprehensive two-dimensional gas chromatography coupled to a time-of-light mass spectrometer is studied for lipid characterization in

  10. Two-dimensional particle simulation of negative ion extraction from a volume source

    International Nuclear Information System (INIS)

    Naitou, H.; Fukumasa, O.; Sakachou, K.; Mutou, K.

    1995-01-01

    Two-dimensional electrostatic particle simulation was done to study the extraction of negative ions from a volume plasma source. The simulation model is a rectangular system which consists of an extraction grid, a plasma grid, and a grounded wall. Full dynamics of electrons, ions, and negative ions are followed. Negative ions are extracted from the plasma region to the extraction grid through a slit in the plasma grid. For the lower value of extraction grid potential, the simulation results agree with the Child-Langumuir law, where the extracted negative ion current is proportional to the three-halves power of the potential of the extraction grid. For the higher value of extraction grid potential, the space charge effect of negative ions, which enter into the beamline at the top of the concavity of the positive ion boundary, reduces the negative ion current from the prediction of the Child-Langumuir law. ((orig.))

  11. Supercritical fluid chromatography hyphenated with twin comprehensive two-dimensional gas chromatography for ultimate analysis of middle distillates.

    Science.gov (United States)

    Adam, Frédérick; Thiébaut, Didier; Bertoncini, Fabrice; Courtiade, Marion; Hennion, Marie-Claire

    2010-02-19

    This paper reports the conditions of online hyphenation of supercritical fluid chromatography (SFC) with twin comprehensive two-dimensional gas chromatography (twin-GCxGC) for detailed characterization of middle distillates; this is essential for a better understanding of reactions involved in refining processes. In this configuration, saturated and unsaturated compounds that have been fractionated by SFC are transferred on two different GC x GC columns sets (twin-GCxGC) placed in the same GC oven. Cryogenic focusing is used for transfer of fractions into the first dimension columns before simultaneous GCxGC analysis of both saturated and unsaturated fractions. The benefits of SFC-twin-GC x GC are demonstrated for the extended alkane, iso-alkane, alkene, naphthenes and aromatics analysis (so-called PIONA analysis) of diesel samples which can be achieved in one single injection. For that purpose, saturated and unsaturated compounds have been separated by SFC using a silver loaded silica column prior to GC x GC analysis. Alkenes and naphthenes are quantitatively recovered in the unsaturated and saturated fractions, respectively, allowing their identification in various diesel samples. Thus, resolution between each class of compounds is significantly improved compared to a single GCxGC run, and for the first time, an extended PIONA analysis of diesel samples is presented. Copyright 2009 Elsevier B.V. All rights reserved.

  12. Additional band broadening of peptides in the first size-exclusion chromatographic dimension of an automated stop-flow two-dimensional high performance liquid chromatography.

    Science.gov (United States)

    Xu, Jucai; Sun-Waterhouse, Dongxiao; Qiu, Chaoying; Zhao, Mouming; Sun, Baoguo; Lin, Lianzhu; Su, Guowan

    2017-10-27

    The need to improve the peak capacity of liquid chromatography motivates the development of two-dimensional analysis systems. This paper presented a fully automated stop-flow two-dimensional liquid chromatography system with size exclusion chromatography followed by reversed phase liquid chromatography (SEC×RPLC) to efficiently separate peptides. The effects of different stop-flow operational parameters (stop-flow time, peak parking position, number of stop-flow periods and column temperature) on band broadening in the first dimension (1 st D) SEC column were quantitatively evaluated by using commercial small proteins and peptides. Results showed that the effects of peak parking position and the number of stop-flow periods on band broadening were relatively small. Unlike stop-flow analysis of large molecules with a long running time, additional band broadening was evidently observed for small molecule analytes due to the relatively high effective diffusion coefficient (D eff ). Therefore, shorter analysis time and lower 1 st D column temperature were suggested for analyzing small molecules. The stop-flow two-dimensional liquid chromatography (2D-LC) system was further tested on peanut peptides and an evidently improved resolution was observed for both stop-flow heart-cutting and comprehensive 2D-LC analysis (in spite of additional band broadening in SEC). The stop-flow SEC×RPLC, especially heart-cutting analysis with shorter analysis time and higher 1 st D resolution for selected fractions, offers a promising approach for efficient analysis of complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Application of a trap-free two-dimensional liquid chromatography combined with ion trap/time-of-flight mass spectrometry for separation and characterization of impurities and isomers in cefpiramide.

    Science.gov (United States)

    Wang, Jian; Xu, Yu; Wen, Chunmei; Wang, Zhijian

    2017-11-01

    High-resolution mass spectrometry had been routinely used for structure identification of impurity. However, all LC-MS methods were based on a volatile mobile phase, and a non-volatile system is used in the official analytical method of United States Pharmacopoeia for cefpiramide which limited the use of mass spectrometry for structure characterization of the impurities. Here we presented the utilization of a trap-free two-dimensional liquid chromatography coupled to high resolution ion trap/time-of-flight mass spectrometry (2D LC-IT-TOF MS) with positive and negative modes of electrospray ionization for characterization of eight impurities in cefpiramide. Trap-free two-dimensional liquid chromatography and online desalting technique made it possible to characterize the impurity in cefpiramide in the condition of official standard, and the TIC chromatogram of LC-MS was in conformity with the LC chromatogram of the official analytical method in the peak sequence of impurities, which could further improve the method of official monographs in pharmacopoeias. Each peak separated by the non-volatile mobile phase was trapped by a 20 μL quantitative loop then transferred into a system with a volatile mobile phase connected to a MS detector. In the first dimension, the column was Kromasil C 8 analytical column (250 mm × 4.6 mm, 5 μm) with a non-volatile salt mobile phase at the flow rate of 0.8 mL min -1 . In the second dimension, the column was Shimadzu Shim-pack GISS C 18 (50 mm × 2.1 mm, 1.9 μm) with a volatile salt mobile phase at the flow rate of 0.3 mL min -1 . Through the multiple heart-cutting 2D-LC approach and online desalting technique, the problem of incompatibility between non-volatile salt mobile phase and mass spectrometry was solved completely. The fragmentation behavior of cefpiramide and its eight impurities were studied. The structures of eight impurities in cefpiramide drug substance were deduced based on the HPLC-MS n data, in

  14. Evaluation of the impact of peak description on the quantitative capabilities of comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Place, Benjamin J; Morris, Mallory J; Phillips, Melissa M; Sander, Lane C; Rimmer, Catherine A

    2014-11-14

    Comprehensive, two-dimensional liquid chromatography (LC × LC) is a powerful technique for the separation of complex mixtures. Most studies using LC × LC are focused on qualitative efforts, such as increasing peak capacity. The present study examined the use of LC × LC-UV/vis for the separation and quantitation of polycyclic aromatic hydrocarbons (PAHs). More specifically, this study evaluated the impact of different peak integration approaches on the quantitative performance of the LC × LC method. For well-resolved three-dimensional peaks, parameters such as baseline definition, peak base shape, and peak width determination did not have a significant impact on accuracy and precision. For less-resolved peaks, a dropped baseline and the summation of all slices in the peak improved the accuracy and precision of the integration methods. The computational approaches to three-dimensional peak integration are provided, including fully descriptive, select slice, and summed heights integration methods, each with its own strengths and weaknesses. Overall, the integration methods presented quantify each of the PAHs within acceptable precision and accuracy ranges and have comparable performance to that of single dimension liquid chromatography. Published by Elsevier B.V.

  15. The multi-mode modulator: A versatile fluidic device for two-dimensional gas chromatography.

    Science.gov (United States)

    Seeley, John V; Schimmel, Nicolaas E; Seeley, Stacy K

    2018-02-09

    A fluidic device called the multi-mode modulator (MMM) has been developed for use as a comprehensive two-dimensional gas chromatography (GC x GC) modulator. The MMM can be employed in a wide range of capacities including as a traditional heart-cutting device, a low duty cycle GC x GC modulator, and a full transfer GC x GC modulator. The MMM is capable of producing narrow component pulses (widths <50ms) while operating at flows compatible with high resolution chromatography. The sample path of modulated components is confined to the interior of a joining capillary. The joining capillary dimensions and the position of the columns within the joining capillary can be optimized for the selected modulation mode. Furthermore, the joining capillary can be replaced easily and inexpensively if it becomes fouled due to sample matrix components or column bleed. The principles of operation of the MMM are described and its efficacy is demonstrated as a heart-cutting device and as a GC x GC modulator. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Determination of neurotransmitters and their metabolites using one- and two-dimensional liquid chromatography with acidic potassium permanganate chemiluminescence detection.

    Science.gov (United States)

    Holland, Brendan J; Conlan, Xavier A; Stevenson, Paul G; Tye, Susannah; Reker, Ashlie; Barnett, Neil W; Adcock, Jacqui L; Francis, Paul S

    2014-09-01

    High-performance liquid chromatography with chemiluminescence detection based on the reaction with acidic potassium permanganate and formaldehyde was explored for the determination of neurotransmitters and their metabolites. The neurotransmitters norepinephrine and dopamine were quantified in the left and right hemispheres of rat hippocampus, nucleus accumbens and prefrontal cortex, and the metabolites vanillylmandelic acid, 3,4-dihydrophenylacetic acid, 5-hydroxyindole-3-acetic acid and homovanillic acid were identified in human urine. Under optimised chemiluminescence reagent conditions, the limits of detection for these analytes ranged from 2.5 × 10(-8) to 2.5 × 10(-7) M. For the determination of neurotransmitter metabolites in urine, a two-dimensional high-performance liquid chromatography (2D-HPLC) separation operated in heart-cutting mode was developed to overcome the peak capacity limitations of the one-dimensional separation. This approach provided the greater separation power of 2D-HPLC with analysis times comparable to conventional one-dimensional separations.

  17. Comprehensive two-dimensional PC-3 prostate cancer cell membrane chromatography for screening anti-tumor components from Radix Sophorae flavescentis.

    Science.gov (United States)

    Wang, Qiang; Xu, Junnan; Li, Xiang; Zhang, Dawei; Han, Yong; Zhang, Xu

    2017-07-01

    Radix Sophorae flavescentis is generally used for the treatment of different stages of prostate cancer in China. It has ideal effects when combined with surgical treatment and chemotherapy. However, its active components are still ambiguous. We devised a comprehensive two-dimensional PC-3 prostate cancer cell membrane chromatography system for screening anti-prostate cancer components in Radix Sophorae flavescentis. Gefitinib and dexamethasone were chosen as positive and negative drugs respectively for validation and optimization the selectivity and suitability of the comprehensive two-dimensional chromatographic system. Five compounds, sophocarpine, matrine, oxymatrine, oxysophocarpine, and xanthohumol were found to have significant retention behaviors on the PC-3 cell membrane chromatography and were unambiguously identified by time-of-flight mass spectrometry. Cell proliferation and apoptosis assays confirmed that all five compounds had anti-prostate cancer effects. Matrine and xanthohumol had good inhibitory effects, with half maximal inhibitory concentration values of 0.893 and 0.137 mg/mL, respectively. Our comprehensive two-dimensional PC-3 prostate cancer cell membrane chromatographic system promotes the efficient recognition and rapid analysis of drug candidates, and it will be practical for the discovery of prostate cancer drugs from complex traditional Chinese medicines. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. New on-line separation workflow of microbial metabolites via hyphenation of analytical and preparative comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Yan, Xia; Wang, Li-Juan; Wu, Zhen; Wu, Yun-Long; Liu, Xiu-Xiu; Chang, Fang-Rong; Fang, Mei-Juan; Qiu, Ying-Kun

    2016-10-15

    Microbial metabolites represent an important source of bioactive natural products, but always exhibit diverse of chemical structures or complicated chemical composition with low active ingredients content. Traditional separation methods rely mainly on off-line combination of open-column chromatography and preparative high performance liquid chromatography (HPLC). However, the multi-step and prolonged separation procedure might lead to exposure to oxygen and structural transformation of metabolites. In the present work, a new two-dimensional separation workflow for fast isolation and analysis of microbial metabolites from Chaetomium globosum SNSHI-5, a cytotoxic fungus derived from extreme environment. The advantage of this analytical comprehensive two-dimensional liquid chromatography (2D-LC) lies on its ability to analyze the composition of the metabolites, and to optimize the separation conditions for the preparative 2D-LC. Furthermore, gram scale preparative 2D-LC separation of the crude fungus extract could be performed on a medium-pressure liquid chromatograph×preparative high-performance liquid chromatography system, under the optimized condition. Interestingly, 12 cytochalasan derivatives, including two new compounds named cytoglobosin Ab (3) and isochaetoglobosin Db (8), were successfully obtained with high purity in a short period of time. The structures of the isolated metabolites were comprehensively characterized by HR ESI-MS and NMR. To be highlighted, this is the first report on the combination of analytical and preparative 2D-LC for the separation of microbial metabolites. The new workflow exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Longitudinal On-Column Thermal Modulation for Comprehensive Two-Dimensional Liquid Chromatography.

    Science.gov (United States)

    Creese, Mari E; Creese, Mathew J; Foley, Joe P; Cortes, Hernan J; Hilder, Emily F; Shellie, Robert A; Breadmore, Michael C

    2017-01-17

    Longitudinal on-column thermal modulation for comprehensive two-dimensional liquid chromatography is introduced. Modulation optimization involved a systematic investigation of heat transfer, analyte retention, and migration velocity at a range of temperatures. Longitudinal on-column thermal modulation was realized using a set of alkylphenones and compared to a conventional valve-modulator employing sample loops. The thermal modulator showed a reduced modulation-induced pressure impact than valve modulation, resulting in reduced baseline perturbation by a factor of 6; yielding a 6-14-fold improvement in signal-to-noise. A red wine sample was analyzed to demonstrate the potential of the longitudinal on-column thermal modulator for separation of a complex sample. Discrete peaks in the second dimension using the thermal modulator were 30-55% narrower than with the valve modulator. The results shown herein demonstrate the benefits of an active focusing modulator, such as reduced detection limits and increased total peak capacity.

  20. Blind column selection protocol for two-dimensional high performance liquid chromatography.

    Science.gov (United States)

    Burns, Niki K; Andrighetto, Luke M; Conlan, Xavier A; Purcell, Stuart D; Barnett, Neil W; Denning, Jacquie; Francis, Paul S; Stevenson, Paul G

    2016-07-01

    The selection of two orthogonal columns for two-dimensional high performance liquid chromatography (LC×LC) separation of natural product extracts can be a labour intensive and time consuming process and in many cases is an entirely trial-and-error approach. This paper introduces a blind optimisation method for column selection of a black box of constituent components. A data processing pipeline, created in the open source application OpenMS®, was developed to map the components within the mixture of equal mass across a library of HPLC columns; LC×LC separation space utilisation was compared by measuring the fractional surface coverage, fcoverage. It was found that for a test mixture from an opium poppy (Papaver somniferum) extract, the combination of diphenyl and C18 stationary phases provided a predicted fcoverage of 0.48 and was matched with an actual usage of 0.43. OpenMS®, in conjunction with algorithms designed in house, have allowed for a significantly quicker selection of two orthogonal columns, which have been optimised for a LC×LC separation of crude extractions of plant material. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Characterization of synthetic dyes by comprehensive two-dimensional liquid chromatography combining ion-exchange chromatography and fast ion-pair reversed-phase chromatography

    NARCIS (Netherlands)

    Pirok, B.W.J.; Knip, J.; van Bommel, M.R.; Schoenmakers, P.J.

    2016-01-01

    In the late 19th century, newly invented synthetic dyes rapidly replaced the natural dyes on the market. The characterization of mixtures of these so-called early synthetic dyes is complicated through the occurrence of many impurities and degradation products. Conventional one-dimensional liquid

  2. Optimisation, simulation, and training in ion chromatography - all for free!

    International Nuclear Information System (INIS)

    Dicinoski, G.W.; Shaw, M.J.; Madden, J.E.; Haddad, P.R.

    2001-01-01

    Since its inception in 1975, ion chromatography (IC) has grown to become a powerful separation tool for the analytical chemist. Today, when scientists refer to the term IC, they mean a collection of chromatographic techniques suitable for the separation of inorganic ions and low molecular weight, water-soluble, organic compounds. The range of chromatographic techniques covered by this designation includes: ion-exchange chromatography; reversed-phase ion-interaction chromatography; and ion-exclusion chromatography. The optimization of the IC separation process is extremely time-consuming. A computer simulation software, Virtual Column 2, that accurately mimic retention behaviour in IC, is presented. It is based on large datasets of experimentally measured retention times; an ideal tool for chromatographers

  3. Silver ion chromatography for peak resolution enhancement: Application to the preparative separation of two sesquiterpenes using online heart-cutting LC-LC technique.

    Science.gov (United States)

    Yang, Yang; Zhang, Yongmin; Wei, Chong; Li, Jing; Sun, Wenji

    2018-09-01

    Silver ion chromatography, utilizing columns packed with silver ions bonded to silica gel, has proved to be an invaluable technique for the analysis of some positional isomers. In this work, silver ion chromatography by combination with online heart-cutting LC-LC technique for the preparative separation of two sesquiterpenes positional isomers from a natural product was investigated. On the basis of the evaluation that silver ion content impacts on the separation, the laboratory-made silver ion columns, utilizing silica gel impregnated with 15% silver nitrate as column packing materials, were used for peak resolution improvement of these two isomers and the preparative separation of them in heart-cutting LC-LC. The relationship among the maximal sample load, flow rate and peak resolution in the silver ion column were optimized, and the performance of the silver ion column was compared with conventional C 18 column and silica gel column. Based on the developed chromatographic conditions, online heart-cutting LC-LC chromatographic separation system in combination with a silica gel column and a silver ion column that was applied to preparative separation of these two isomers from a traditional Chinese medicine, Inula racemosa Hook.f., was established. The results showed that the online heart-cutting LC-LC technique by combination of a silica gel column and a silver ion column for the preparative separation of these two positional isomers from this natural plant was superior to the preparative separation performed on a single-column system with C 18 column or silica gel column. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. Comprehensive two-dimensional gas chromatography: A perspective on processes of modulation.

    Science.gov (United States)

    Tranchida, Peter Q

    2018-02-09

    The first comprehensive two-dimensional gas chromatography (GC×GC) experiment was reported about 25 years ago [J. Chromatogr. Sci. 29 (1991) 227-231]; the GC×GC process was made possible by the development of a transfer device, defined as modulator. The process of modulation enables the isolation of effluent segments from the first column, and their re-injection onto the second column, in a continuous and sequential manner throughout the analysis. Over the years, many types of modulation systems have been introduced, each with specific advantages and disadvantages. Cryogenic systems are, at present, the most popular devices and represent the most effective form of modulation. The present contribution is focused on possible future scenarios, with respect to modulation, and as a consequence related to comprehensive GC, in general. The development of new forms of modulation may open the road to a more widespread use of GC×GC technologies. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Two-dimensional Thermal Modeling of Lithium-ion Battery Cell Based on Electrothermal Impedance Spectroscopy

    DEFF Research Database (Denmark)

    Swierczynski, Maciej Jozef; Stroe, Daniel Loan; Knap, Vaclav

    2016-01-01

    Thermal modeling of lithium-ion batteries is gaining its importance together with increasing power density and compact design of the modern battery systems in order to assure battery safety and long lifetime. Thermal models of lithium-ion batteries are usually either expensive to develop...... and accurate or equivalent thermal circuit based with moderate accuracy and without spatial temperature distribution. This work presents initial results that can be used as a fundament for the cost-efficient development of the two-dimensional thermal model of lithium-ion battery based on multipoint...

  6. The versatility of heart-cutting and comprehensive two-dimensional liquid chromatography in monoclonal antibody clone selection.

    Science.gov (United States)

    Sandra, Koen; Steenbeke, Mieke; Vandenheede, Isabel; Vanhoenacker, Gerd; Sandra, Pat

    2017-11-10

    In recent years, two-dimensional liquid chromatography (2D-LC) has seen an enormous evolution and one of the fields where it is being widely adopted is in the analysis of therapeutic monoclonal antibodies (mAbs). We here further add to the many flavours of this powerful technology. Workflows based on heart-cutting (LC-LC) and comprehensive (LC×LC) 2D-LC are described that allow to guide the clone selection process in mAb and biosimilar development. Combining Protein A affinity chromatography in the first dimension with size exclusion (SEC), cation exchange (CEX) or reversed-phase liquid chromatography-mass spectrometry (RPLC-MS) in the second dimension simultaneously allows to assess mAb titer and critical structural aspects such as aggregation, fragmentation, charge heterogeneity, molecular weight (MW), amino acid sequence and glycosylation. Complementing the LC-LC measurements at intact protein level with LC×LC based peptide mapping provides the necessary information to make clear decisions on which clones to take further into development. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Multi-dimensional conversion to the ion-hybrid mode

    International Nuclear Information System (INIS)

    Tracy, E.R.; Kaufman, A.N.; Brizard, A.J.; Morehead, J.J.

    1996-01-01

    We first demonstrate that the dispersion matrix for linear conversion of a magnetosonic wave to an ion-hybrid wave (as in a D-T plasma) can be congruently transformed to Friedland's normal form. As a result, this conversion can be represented as a two-step process of successive linear conversions in phase space. We then proceed to study the multi-dimensional case of tokamak geometry. After fourier transforming the toroidal dependence, we deal with the two-dimensional poloidal xy-plane and the two-dimensional k x k y -plane, forming a four-dimensional phase space. The dispersion manifolds for the magnetosonic wave [D M (x, k) = 0] and the ion-hybrid wave [D H (x, k) = 0] are each three-dimensional. (Their intersection, on which mode conversion occurs, is two-dimensional.) The incident magnetosonic wave (radiated by an antenna) is a two-dimensional set of rays (a lagrangian manifold): k(x) = ∇θ(x), with θ(x) the phase of the magnetosonic wave. When these rays pierce the ion-hybrid dispersion manifold, they convert to a set of ion-hybrid rays. Then, when those rays intersect the magnetosonic dispersion manifold, they convert to a set of open-quotes reflectedclose quotes magnetosonic rays. This set of rays is distinct from the set of incident rays that have been reflected by the inner surface of the tokamak plasma. As a result, the total destructive interference that can occur in the one-dimensional case may become only partial. We explore the implications of this startling phenomenon both analytically and geometrically

  8. New analytical treatment for a kind of two dimensional integrals in ion-atom collisions

    International Nuclear Information System (INIS)

    Yang Qifeng; Kuang Yurang

    1994-01-01

    A kind of two-dimensional integrals, separated from two-center matrix elements in ion-atom collisions, is analytically integrated by introducing the Laplace transform into the integrals and expressed by the modified Bessel functions. The traditional Feynman transform is very complicated for this kind of more general integrals related to the excited state capture

  9. Ion-pair chromatography of nucleic acid derivatives

    International Nuclear Information System (INIS)

    Perrone, P.A.; Brown, P.R.

    1985-01-01

    Little work has been done on the ion-pair chromatography of nucleic acid constituents, although there is a great potential for the use of this technique in the field. Since the classic work in 1949, nucleotides, as well as nucleosides and bases, have been separated by ion-exchange chromatography. However, ion exchange is a difficult mode and most researchers prefer the use of reversed-phase whenever possible. Although reversed-phase is now the method of choice, ionic compounds like nucleotides and some of the more polar bases are not adequately retained by many systems of this type. In addition, it is difficult to analyze simultaneously members of all three classes of nucleic acid compounds (bases, nucleosides, and nucleotides) using a reversed-phase system, even with gradient elution. Ion pairing can be a useful technique because, theoretically, the separation of nonionic bases and nucleosides along with the ionic nucleotides can be achieved. Additionally, each group of compounds may be separated isocratically. In this chapter, they will discuss ion-pair chromatography as applied to nucleic acid constituents. The current theories, advantages and disadvantages, a limited number of applications, and potential for future work are presented

  10. Two-dimensional gas chromatography-online hydrogenation for improved characterization of petrochemical samples.

    Science.gov (United States)

    Potgieter, H; Bekker, R; Govender, A; Rohwer, E

    2016-05-06

    The Fischer-Tropsch (FT) process produces a variety of hydrocarbons over a wide carbon number range and during subsequent product workup a large variety of synthetic fuels and chemicals are produced. The complexity of the product slate obtained from this process is well documented and the high temperature FT (HT-FT) process products are spread over gas, oil and water phases. The characterization of these phases is very challenging even when using comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS). Despite the increase in separation power, peak co-elution still occurs when samples containing isomeric compounds are analysed by comprehensive two dimensional GC. The separation of isomeric compounds with the same double bond equivalents is especially difficult since these compounds elute in a similar position on the GC×GC chromatogram and have identical molecular masses and similar fragmentation patterns in their electron ionization (EI) mass spectra. On-line hydrogenation after GC×GC separation is a possible way to distinguish between these isomeric compounds since the number of rings and alkene double bonds can be determined from the mass spectra of the compounds before and after hydrogenation. This paper describes development of a GC×GC method with post column hydrogenation for the determination of the backbone of cyclic/olefinic structures enabling us to differentiate between classes like dienes and cyclic olefins in complex petrochemical streams. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

    Science.gov (United States)

    Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

    2015-03-27

    A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Chiral separation and chemical profile of Dengzhan Shengmai by integrating comprehensive with multiple heart-cutting two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Sheng, Ning; Zheng, Hao; Xiao, Yao; Wang, Zhe; Li, Menglin; Zhang, Jinlan

    2017-09-29

    Chemical profile for Chinese medicine formulas composed of several herbs is always a challenge due to a big array of small molecules with high chemical diversity so much as isomers. The present paper develops a feasible strategy to characterize and identify complex chemical constituents of a four-herb traditional Chinese medicine formula, Denzhan Shenmai (DZSM) by integrating comprehensive two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC×LC-qTOF-MS) with multiple heart-cutting two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (MHC-qTOF-MS). DZSM was separated by C8×C18 HPLC column system for comprehensive two-dimensional liquid chromatography system and 283 compounds most of which belonged to phenolic acid, flavonoid, saponin and lignan families were characterized and identified within 75min. Some isomers and compounds at low level were analyzed on C8×Chiral HPLC column system for multiple heart-cutting two-dimensional liquid chromatography system with 1D and 2D optimized gradient elution program. These 1D cutting fractions were successively separated on 2D chiral chromatographic column under extended the 2D gradient elution time from 30s to 5.0min. 12 pairs of isomer compounds were separated with good resolution. The combination of LC×LC and MHC system provides a powerful technique for global chemical profiling of DZSM and provided feasible strategy for other complex systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Ion chromatography of anions in the primary and secondary circuit

    International Nuclear Information System (INIS)

    Brandt, F.; Trost, R.

    1984-01-01

    Ion chromatography - though based on the same, well-established basic principles as gas chromatography and high pressure fluid chromatography - has made an actual breakthrough only in recent years. The adaptability of the process permits the measurement of samples of different composition or concentration. Some of the experience which has been accumulated in the laboratory at Goesgen nuclear power station during the last two years, is reported. This relates particularly to the composition of the samples, the need to use extremely pure calibration samples, the choice of special laboratory accessories and the like. (orig.) [de

  14. Smart multi-channel two-dimensional micro-gas chromatography for rapid workplace hazardous volatile organic compounds measurement.

    Science.gov (United States)

    Liu, Jing; Seo, Jung Hwan; Li, Yubo; Chen, Di; Kurabayashi, Katsuo; Fan, Xudong

    2013-03-07

    We developed a novel smart multi-channel two-dimensional (2-D) micro-gas chromatography (μGC) architecture that shows promise to significantly improve 2-D μGC performance. In the smart μGC design, a non-destructive on-column gas detector and a flow routing system are installed between the first dimensional separation column and multiple second dimensional separation columns. The effluent from the first dimensional column is monitored in real-time and decision is then made to route the effluent to one of the second dimensional columns for further separation. As compared to the conventional 2-D μGC, the greatest benefit of the smart multi-channel 2-D μGC architecture is the enhanced separation capability of the second dimensional column and hence the overall 2-D GC performance. All the second dimensional columns are independent of each other, and their coating, length, flow rate and temperature can be customized for best separation results. In particular, there is no more constraint on the upper limit of the second dimensional column length and separation time in our architecture. Such flexibility is critical when long second dimensional separation is needed for optimal gas analysis. In addition, the smart μGC is advantageous in terms of elimination of the power intensive thermal modulator, higher peak amplitude enhancement, simplified 2-D chromatogram re-construction and potential scalability to higher dimensional separation. In this paper, we first constructed a complete smart 1 × 2 channel 2-D μGC system, along with an algorithm for automated control/operation of the system. We then characterized and optimized this μGC system, and finally employed it in two important applications that highlight its uniqueness and advantages, i.e., analysis of 31 workplace hazardous volatile organic compounds, and rapid detection and identification of target gas analytes from interference background.

  15. Using the hydrophobic subtraction model to choose orthogonal columns for online comprehensive two-dimensional liquid chromatography

    DEFF Research Database (Denmark)

    Græsbøll, Rune; Nielsen, Nikoline Juul; Christensen, Jan H.

    2014-01-01

    A method for choosing orthogonal columns for a specific sample set in on-line comprehensive two-dimensional liquid chromatography (LC×LC) was developed on the basis of the hydrophobic subtraction model. The method takes into account the properties of the sample analytes by estimating new F...... neutral and 4 acidic oxygenated polycyclic aromatic compounds (PACs) and 3 nitrogen-containing PAC bases was measured isocratically on 12 columns. The isocratic runs were used to determine the hydrophobic subtraction model analyte parameters, and these were used to estimate new F-weights and predict...

  16. Integrated sampling vs ion chromatography: Mathematical considerations

    International Nuclear Information System (INIS)

    Sundberg, L.L.

    1992-01-01

    This paper presents some general purpose considerations that can be utilized when comparisons are made between the results of integrated sampling over several hours or days, and ion chromatography where sample collection times are measured in minutes. The discussion is geared toward the measurement of soluble transition metal ions in BWR feedwater. Under steady-state conditions, the concentrations reported by both techniques should be in reasonable agreement. Transient operations effect both types of measurements. A simplistic model, applicable to both sampling techniques, is presented that demonstrates the effect of transients which occur during the acquisition of a steady-state sample. For a common set of conditions, the integrated concentration is proportional to the concentration and duration of the transient, and inversely proportional to the sample collection time. The adjustment of the collection period during a known transient allows an estimation of peak transient concentration. Though the probability of sampling a random transient with the integrated sampling technique is very high, the magnitude is severely diluted with long integration times. Transient concentrations are magnified with ion chromatography, but the probability of sampling a transient is significantly lower using normal ion chromatography operations. Various data averaging techniques are discussed for integrated sampling and IC determinations. The use of time-weighted averages appears to offer more advantages over arithmetic and geometric means for integrated sampling when the collection period is variable. For replicate steady-state ion chromatography determinations which bracket a transient sample, it may be advantageous to ignore the calculation of averages, and report the data as trending information only

  17. Ion-pairing reversed-phased chromatography/mass spectrometry of heparin

    DEFF Research Database (Denmark)

    Henriksen, Jens; Roepstorff, Peter; Ringborg, Lene H.

    2006-01-01

    not well characterised. In order to further characterise such mixtures, two on-line ion-pairing reverse-phased chromatography electrospray ionisation (ESI) mass spectrometry methods have been developed. One of the systems allows the determination of more than 200 components in a medium molecular weight...

  18. Two-dimensional particle-in-cell plasma source ion implantation of a prolate spheroid target

    International Nuclear Information System (INIS)

    Cheng-Sen, Liu; Hong-Ying, Han; Xiao-Qing, Peng; Ye, Chang; De-Zhen, Wang

    2010-01-01

    A two-dimensional particle-in-cell simulation is used to study the time-dependent evolution of the sheath surrounding a prolate spheroid target during a high voltage pulse in plasma source ion implantation. Our study shows that the potential contour lines pack more closely in the plasma sheath near the vertex of the major axis, i.e. where a thinner sheath is formed, and a non-uniform total ion dose distribution is incident along the surface of the prolate spheroid target due to the focusing of ions by the potential structure. Ion focusing takes place not only at the vertex of the major axis, where dense potential contour lines exist, but also at the vertex of the minor axis, where sparse contour lines exist. This results in two peaks of the received ion dose, locating at the vertices of the major and minor axes of the prolate spheroid target, and an ion dose valley, staying always between the vertices, rather than at the vertex of the minor axis

  19. Two-dimensional particle-in-cell plasma source ion implantation of a prolate spheroid target

    Science.gov (United States)

    Liu, Cheng-Sen; Han, Hong-Ying; Peng, Xiao-Qing; Chang, Ye; Wang, De-Zhen

    2010-03-01

    A two-dimensional particle-in-cell simulation is used to study the time-dependent evolution of the sheath surrounding a prolate spheroid target during a high voltage pulse in plasma source ion implantation. Our study shows that the potential contour lines pack more closely in the plasma sheath near the vertex of the major axis, i.e. where a thinner sheath is formed, and a non-uniform total ion dose distribution is incident along the surface of the prolate spheroid target due to the focusing of ions by the potential structure. Ion focusing takes place not only at the vertex of the major axis, where dense potential contour lines exist, but also at the vertex of the minor axis, where sparse contour lines exist. This results in two peaks of the received ion dose, locating at the vertices of the major and minor axes of the prolate spheroid target, and an ion dose valley, staying always between the vertices, rather than at the vertex of the minor axis.

  20. New benchmark for basic and neutral nitrogen compounds speciation in middle distillates using comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Adam, Frédérick; Bertoncini, Fabrice; Brodusch, Nicolas; Durand, Emmanuelle; Thiébaut, Didier; Espinat, Didier; Hennion, Marie-Claire

    2007-04-27

    This paper reports an analytical method for the comprehensive two-dimensional gas chromatography (GC x GC) separation and identification of nitrogen compounds (N-compounds) in middle distillates according to their types (basicity). For the evaluation of the best chromatographic conditions, a non-polar x polar approach was chosen. The impact of the second dimension (stationary phase and column length) on the separation of basic and neutral N-compounds was evaluated by mean of two-dimensional resolution. This study revealed that the implementation of polar secondary column having free electron pairs improves drastically the separation of N-compounds. Indeed, the presence of permanent dipole-permanent dipole interactions between neutral N-compounds and the stationary phase was enlightened. The comparison of two different nitrogen chemiluminescence detectors (NCD) was also evaluated for GC x GC selective monitoring of N-compounds. Owing to higher resolution power and enhanced sensitivity achieved using developed chromatographic and detection conditions, it was possible to identify univocally and to quantitate N-compounds (i) by class of compounds and (ii), within a class, by carbon number. Finally, quantitative comparison of GC x GC-NCD with conventional gas chromatography illustrates the benefits of GC x GC leading to an excellent correlation with results obtained by American Society for Testing Materials (ASTM) methods for the determination of basic/neutral nitrogen ratio in diesel samples.

  1. High-capacity cation-exchange column for enhanced resolution of adjacent peaks of cations in ion chromatography.

    Science.gov (United States)

    Rey, M A

    2001-06-22

    One of the advantages of ion chromatography [Anal Chem. 47 (1975) 1801] as compared to other analytical techniques is that several ions may be analyzed simultaneously. One of the most important contributions of cation-exchange chromatography is its sensitivity to ammonium ion, which is difficult to analyze by other techniques [J. Weiss, in: E.L. Johnson (Ed.), Handbook of Ion Chromatography, Dionex, Sunnyvale, CA, USA]. The determination of low concentrations of ammonium ion in the presence of high concentrations of sodium poses a challenge in cation-exchange chromatography [J. Weiss, Ion Chromatography, VCH, 2nd Edition, Weinheim, 1995], as both cations have similar selectivities for the common stationary phases containing either sulfonate or carboxylate functional groups. The task was to develop a new cation-exchange stationary phase (for diverse concentration ratios of adjacent peaks) to overcome limitations experienced in previous trails. Various cation-exchange capacities and column body formats were investigated to optimize this application and others. The advantages and disadvantages of two carboxylic acid columns of different cation-exchange capacities and different column formats will be discussed.

  2. Two-dimensional high-performance thin-layer chromatography of tryptic bovine albumin digest using normal- and reverse-phase systems with silanized silica stationary phase.

    Science.gov (United States)

    Gwarda, Radosław Łukasz; Dzido, Tadeusz Henryk

    2013-10-18

    Among many advantages of planar techniques, two-dimensional (2D) separation seems to be the most important for analysis of complex samples. Here we present quick, simple and efficient two-dimensional high-performance thin-layer chromatography (2D HPTLC) of bovine albumin digest using commercial HPTLC RP-18W plates (silica based stationary phase with chemically bonded octadecyl ligands of coverage density 0.5μmol/m(2) from Merck, Darmstadt). We show, that at low or high concentration of water in the mobile phase comprised methanol and some additives the chromatographic systems with the plates mentioned demonstrate normal- or reversed-phase liquid chromatography properties, respectively, for separation of peptides obtained. These two systems show quite different separation selectivity and their combination into 2D HPTLC process provides excellent separation of peptides of the bovine albumin digest. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Identification and classification of components in flash pyrolysis oil and hydrodeoxygenated oils by two-dimensional gas chromatography and time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Marsman, J. H.; Wildschut, J.; Evers, P.; Heeres, H. J.; Koning de, S.

    2008-01-01

    Hydrodeoxygenated pyrolysis oils (HDO) are considered promising renewable liquid energy carriers. To gain insights in the various reaction pathways taking place during the hydrodeoxygenation reaction of pyrolysis oil, two-dimensional gas chromatography with time-of-flight mass spectrometric analyses

  4. Application of the zeta potential for stationary phase characterization in ion chromatography.

    Science.gov (United States)

    Buszewski, Bogusław; Jaćkowska, Magdalena; Bocian, Szymon; Dziubakiewicz, Ewelina

    2013-01-01

    Two series of homemade stationary bonded phases for ion chromatography were investigated according to their zeta potential. One set of dendrimer anion exchanger was synthesized on the polymer support whereas the second material was prepared on the silica gel. The zeta potential data in water environment as well as buffered water solution were obtained. The influence of the length of anion-exchanger chains, the type of the support of the modified surface, and charge distribution on these data was investigated. Additionally, the zeta potential was correlated with retention factor of inorganic ions to describe their influence on the retention mechanism in ion chromatography. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Comprehensive Two-dimensional Liquid Chromatography coupled to High Resolution Time of Flight Mass Spectrometry for Chemical Characterization of Sewage Treatment Plant Effluents

    NARCIS (Netherlands)

    Ouyang, X.; Leonards, P.E.G.; Legler, J.; van der Oost, R.; de Boer, J.; Lamoree, M.H.

    2015-01-01

    For the first time a comprehensive two-dimensional liquid chromatography (LC. ×. LC) system coupled with a high resolution time-of-flight mass spectrometer (HR-ToF MS) was developed and applied for analysis of emerging toxicants in wastewater effluent. The system was optimized and validated using

  6. Development and validation of a comprehensive two-dimensional gas chromatography-mass spectrometry method for the analysis of phytosterol oxidation products in human plasma

    NARCIS (Netherlands)

    Menéndez-Carreño, M.; Steenbergen, H.; Janssen, H.-G.

    2012-01-01

    Phytosterol oxidation products (POPs) have been suggested to exert adverse biological effects similar to, although less severe than, their cholesterol counterparts. For that reason, their analysis in human plasma is highly relevant. Comprehensive two-dimensional gas chromatography (GC×GC) coupled

  7. Chromatographical analysis of phenolic acids in some species of Polygonum L. genus. Part 1 Qualitative analysis by two-dimensional thin layer chromatography (TLC

    Directory of Open Access Journals (Sweden)

    Helena D. Smolarz

    2014-01-01

    Full Text Available The Two-Dimensional Thin Layer Chromatography method has been used for the separation and identification of phenolic acids from six taxons of Pohygonum L. genus. The following acids were found: caffeic, p-coumaric, ferulic, p-hydroxybenzoic, m-hydroxybenzoic, vanillic, syringic, p-hydroxyphenylacetic, o-hydroxyphenylacetic, synapic, melillotic, salicylic, gentisic, elagic, gallic, chlorogenic, protocatechuic and homoprotocatechuic. Gallic, ferulic, vanillic, p-coumaric and p-hydroxybenzoic acids were isolated from herb Polygonum convolvulus L. using column chromatography.

  8. Isotopic separation by ion chromatography

    International Nuclear Information System (INIS)

    Albert, M.G.; Barre, Y.; Neige, R.

    1994-01-01

    The isotopic exchange reaction and the isotopic separation factor are first recalled; the principles of ion chromatography applied to lithium isotope separation are then reviewed (displacement chromatography) and the process is modelled in the view of dimensioning and optimizing the industrial process; the various dimensioning parameters are the isotopic separation factor, the isotopic exchange kinetics and the material flow rate. Effects of the resin type and structure are presented. Dimensioning is also affected by physico-chemical and hydraulic parameters. Industrial implementation features are also discussed. 1 fig., 1 tab., 5 refs

  9. Design of two-column batch-to-batch recirculation to enhance performance in ion-exchange chromatography.

    Science.gov (United States)

    Persson, Oliver; Andersson, Niklas; Nilsson, Bernt

    2018-01-05

    Preparative liquid chromatography is a separation technique widely used in the manufacturing of fine chemicals and pharmaceuticals. A major drawback of traditional single-column batch chromatography step is the trade-off between product purity and process performance. Recirculation of impure product can be utilized to make the trade-off more favorable. The aim of the present study was to investigate the usage of a two-column batch-to-batch recirculation process step to increase the performance compared to single-column batch chromatography at a high purity requirement. The separation of a ternary protein mixture on ion-exchange chromatography columns was used to evaluate the proposed process. The investigation used modelling and simulation of the process step, experimental validation and optimization of the simulated process. In the presented case the yield increases from 45.4% to 93.6% and the productivity increases 3.4 times compared to the performance of a batch run for a nominal case. A rapid concentration build-up product can be seen during the first cycles, before the process reaches a cyclic steady-state with reoccurring concentration profiles. The optimization of the simulation model predicts that the recirculated salt can be used as a flying start of the elution, which would enhance the process performance. The proposed process is more complex than a batch process, but may improve the separation performance, especially while operating at cyclic steady-state. The recirculation of impure fractions reduces the product losses and ensures separation of product to a high degree of purity. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Peak clustering in two-dimensional gas chromatography with mass spectrometric detection based on theoretical calculation of two-dimensional peak shapes: the 2DAid approach.

    Science.gov (United States)

    van Stee, Leo L P; Brinkman, Udo A Th

    2011-10-28

    A method is presented to facilitate the non-target analysis of data obtained in temperature-programmed comprehensive two-dimensional (2D) gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-ToF-MS). One main difficulty of GC×GC data analysis is that each peak is usually modulated several times and therefore appears as a series of peaks (or peaklets) in the one-dimensionally recorded data. The proposed method, 2DAid, uses basic chromatographic laws to calculate the theoretical shape of a 2D peak (a cluster of peaklets originating from the same analyte) in order to define the area in which the peaklets of each individual compound can be expected to show up. Based on analyte-identity information obtained by means of mass spectral library searching, the individual peaklets are then combined into a single 2D peak. The method is applied, amongst others, to a complex mixture containing 362 analytes. It is demonstrated that the 2D peak shapes can be accurately predicted and that clustering and further processing can reduce the final peak list to a manageable size. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Chemical characterisation of two Australian-grown strawberry varieties by using comprehensive two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Samykanno, Kavitha; Pang, Edwin; Marriott, Philip J

    2013-12-01

    The volatile compositions of two strawberry varieties ('Albion' and 'Juliette') grown in Australia were analysed with comprehensive two-dimensional gas chromatography (GC×GC) combined with time-of-flight mass spectrometry (ToFMS). A suitable data processing method was created that should be sufficiently robust to compare sample chromatograms within a harvest season as well as between seasons with relative ease. Ninety-four compounds were tentatively or positively identified between the two varieties of which 20 have apparently not been previously reported to be components of strawberry volatiles. It was determined that Albion and Juliette have comparable total soluble solids content close to 11°Brix. However, since Juliette exhibited a lower titratable acidity content than Albion, it consequently has a slightly larger sugar/acid ratio. The presence of 2,5-dimethyl-4-hydroxy-(2H)-furan-3-one (furaneol) was detected only in Juliette and this variety also had a higher area percentage of 2,5-dimethyl-4-methoxy-(2H)-furan-3-one (mesifuran), according to the sampling protocol. These experimental results offer possible explanations as to why Juliette is perceived to have a sweeter flavour than Albion. Copyright © 2013 Elsevier Ltd. All rights reserved.

  12. Application of ion chromatography in clinical studies and pharmaceutical industry.

    Science.gov (United States)

    Michalski, Rajmund

    2014-01-01

    Ion chromatography is a well-established regulatory method for analyzing anions and cations in environmental, food and many other samples. It offers an enormous range of possibilities for selecting stationary and mobile phases. Additionally, it usually helps to solve various separation problems, particularly when it is combined with different detection techniques. Ion chromatography can also be used to determine many ions and substances in clinical and pharmaceutical samples. It provides: availability of high capacity stationary phases and sensitive detectors; simple sample preparation; avoidance of hazardous chemicals; decreased sample volumes; flexible reaction options on a changing sample matrix to be analyzed; or the option to operate a fully-automated system. This paper provides a short review of the ion chromatography applications for determining different inorganic and organic substances in clinical and pharmaceutical samples.

  13. Analysis of human plasma lipids by using comprehensive two-dimensional gas chromatography with dual detection and with the support of high-resolution time-of-flight mass spectrometry for structural elucidation.

    Science.gov (United States)

    Salivo, Simona; Beccaria, Marco; Sullini, Giuseppe; Tranchida, Peter Q; Dugo, Paola; Mondello, Luigi

    2015-01-01

    The main focus of the present research is the analysis of the unsaponifiable lipid fraction of human plasma by using data derived from comprehensive two-dimensional gas chromatography with dual quadrupole mass spectrometry and flame ionization detection. This approach enabled us to attain both mass spectral information and analyte percentage data. Furthermore, gas chromatography coupled with high-resolution time-of-flight mass spectrometry was used to increase the reliability of identification of several unsaponifiable lipid constituents. The synergism between both the high-resolution gas chromatography and mass spectrometry processes enabled us to attain a more in-depth knowledge of the unsaponifiable fraction of human plasma. Additionally, information was attained on the fatty acid and triacylglycerol composition of the plasma samples, subjected to investigation by using comprehensive two-dimensional gas chromatography with dual quadrupole mass spectrometry and flame ionization detection and high-performance liquid chromatography with atmospheric pressure chemical ionization quadrupole mass spectrometry, respectively. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Mapping the fundamental niches of two freshwater microalgae, Chlorella vulgaris (Trebouxiophyceae) and Peridinium cinctum (Dinophyceae), in 5-dimensional ion space

    Science.gov (United States)

    A five dimensional experimental design, i.e. a five component ion mixture design for nitrate, phosphate, potassium, sodium and chloride projected across a total ion concentration gradient of 1-30 mM was utilized to map the ion-based, scenopoetic, or ‘Grinnellian’, niche space for two freshwater alga...

  15. Enrichment and Determination of radionuclides by ion chromatography

    International Nuclear Information System (INIS)

    ZAFIMANJATO, J.L.R.

    1996-01-01

    The fundamentals of Ion Chromatography (IC) and Liquid Scintillation Counting (LSC) are reviewed. Ion Chromatography as separation method for cations is coupled with Liquid Scintillation Counting for the determination of Radionuclides in water samples. An experimental arrangement for investigations on the applicability of guard columns for cationic radionuclide enrichment is shown. The saturation behaviour of single and bivalentic cations and their combination is presented. Our results show that radioactive bivalentic cations like strontium-90 and radium-226 are enriched on a Ion Pac CG 12 Dionex guard column from 100 to 300ml natural water in one single step. The procedure is suitable for their determination in concentrations down to 10 -2 Bq.l -1 [fr

  16. Two-dimensional PIC-MCC simulation of ion extraction

    International Nuclear Information System (INIS)

    Xiong Jiagui; Wang Dewu

    2000-01-01

    To explore more simple and efficient ion extraction methods used in atomic vapor laser isotope separation (AVLIS), two-dimensional (2D) PIC-MCC simulation code is used to simulate and compare several methods: parallel electrode method, II type electrode method, improved M type electrode method, and radio frequency (RF) resonance method. The simulations show that, the RF resonance method without magnetic field is the best among others, then the improved M type electrode method. The result of simulation of II type electrode method is quite different from that calculated by 2D electron equilibrium model. The RF resonance method with or without magnetic field has guide different results. Strong resonance occurs in the simulation without magnetic field, whereas no significant resonance occurs under weak magnetic field. And that is quite different from the strong resonance phenomena occurring in the 1D PIC simulation with weak magnetic field. As for practical applications, the RF resonance method without magnetic field has pros and cons, compared with the M type electrode method

  17. Multivariate analytical figures of merit as a metric for evaluation of quantitative measurements using comprehensive two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Eftekhari, Ali; Parastar, Hadi

    2016-09-30

    The present contribution is devoted to develop multivariate analytical figures of merit (AFOMs) as a new metric for evaluation of quantitative measurements using comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS). In this regard, new definition of sensitivity (SEN) is extended to GC×GC-MS data and then, other multivariate AFOMs including analytical SEN (γ), selectivity (SEL) and limit of detection (LOD) are calculated. Also, two frequently used second- and third-order calibration algorithms of multivariate curve resolution-alternating least squares (MCR-ALS) as representative of multi-set methods and parallel factor analysis (PARAFAC) as representative of multi-way methods are discussed to exploit pure component profiles and to calculate multivariate AFOMs. Different GC×GC-MS data sets with different number of components along with various levels of artifacts are simulated and analyzed. Noise, elution time shifts in both chromatographic dimensions, peak overlap and interferences are considered as the main artifacts in this work. Additionally, a new strategy is developed to estimate the noise level using variance-covariance matrix of residuals which is very important to calculate multivariate AFOMs. Finally, determination of polycyclic aromatic hydrocarbons (PAHs) in aromatic fraction of heavy fuel oil (HFO) analyzed by GC×GC-MS is considered as real case to confirm applicability of the proposed metric in real samples. It should be pointed out that the proposed strategy in this work can be used for other types of comprehensive two-dimensional chromatographic (CTDC) techniques like comprehensive two dimensional liquid chromatography (LC×LC). Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Multi-column step-gradient chromatography system for automated ion exchange separations

    International Nuclear Information System (INIS)

    Rucker, T.L.

    1985-01-01

    A multi-column step-gradient chromatography system has been designed to perform automated sequential separations of radionuclides by ion exchange chromatography. The system consists of a digital programmer with automatic stream selection valve, two peristaltic pumps, ten columns, and a fraction collector. The automation allows complicated separations of radionuclides to be made with minimal analyst attention and allows for increased productivity and reduced cost of analyses. Results are reported for test separations on mixtures of radionuclides by the system

  19. Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

    Science.gov (United States)

    Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

    2016-06-01

    In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Characterization of poly(allylamine) as a polymeric ligand for ion-exchange protein chromatography.

    Science.gov (United States)

    Li, Ming; Li, Yanying; Yu, Linling; Sun, Yan

    2017-02-24

    This work reports poly(allylamine) (PAA), as a polymeric ion-exchange ligand for protein chromatography. Sepharose FF was modified with PAA, and six anion exchangers with ionic capacities (ICs) from 165 to 618mmol/L were prepared. Inverse size exclusion chromatography, adsorption equilibrium, uptake kinetics and column elution were performed. It was found that both the adsorption capacity and effective diffusivity maintained low values in the IC range of 165-373mmol/L, but they started to increase beyond 373mmol/L, and increased by 80% and 23 times, respectively, when the IC reached 618mmol/L. Interestingly, a drastic decrease of pore size was observed around the IC of 373mmol/L. The results suggest that the PAA chains played an important role in protein adsorption by altering the inner pore structure of the gels. It is considered that, PAA chains turn from inextensible states with multipoint-grafting on the pore surface at low coupling densities (IC373mmol/L). These characters of the grafted chains at higher IC values benefit in protein adsorption by three-dimensional binding and encouraged the happening of "chain delivery" of bound proteins on the chains. Besides, the ion exchangers showed favorable adsorption and uptake properties in a wide ionic strength range, 0-500mmol/L NaCl, indicating much better salt tolerance feature than the so-far reported ion exchangers. Moreover, a mild condition of pH 5.0 offered effective recovery of bound proteins in elution chromatography. The results indicate that the PAA-based anion exchanger of a high IC value is promising for high-capacity protein chromatography dealing with feedstock of a wide range of ionic strengths. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Investigation of electrostatic ion chromatography for the separation of inorganic ions

    OpenAIRE

    Twohill, Eadaoin

    2002-01-01

    The new technique of ‘electrostatic ion chromatography’ (ion chromatography using a zwittenomc stationary phase) has been applied to the separation of ions using pure water as an eluent, without the addition of any inorganic buffers or organic modifiers. The nature of the separation, le cationic or anionic, is dependent upon the nature of the zwittenomc stationary phase. In the work presented here, the zwittenomc surfactant Zwittergent 3-14 was used to functionalise an octadecylsihca stationa...

  2. Electron-capture process and ion mobility spectra in plasma chromatography

    International Nuclear Information System (INIS)

    Karasek, F.W.; Spangler, G.E.

    1981-01-01

    The basic principles of plasma chromatography are introduced and ion mobility relationships presented. The relationships of plasma chromatography to electron-capture detector mechanisms are discussed, including electron energy considerations and electron-capture reactions. A number of experimental studies by plasma chromatography are described. (C.F.)

  3. Real-time two-dimensional imaging of potassium ion distribution using an ion semiconductor sensor with charged coupled device technology.

    Science.gov (United States)

    Hattori, Toshiaki; Masaki, Yoshitomo; Atsumi, Kazuya; Kato, Ryo; Sawada, Kazuaki

    2010-01-01

    Two-dimensional real-time observation of potassium ion distributions was achieved using an ion imaging device based on charge-coupled device (CCD) and metal-oxide semiconductor technologies, and an ion selective membrane. The CCD potassium ion image sensor was equipped with an array of 32 × 32 pixels (1024 pixels). It could record five frames per second with an area of 4.16 × 4.16 mm(2). Potassium ion images were produced instantly. The leaching of potassium ion from a 3.3 M KCl Ag/AgCl reference electrode was dynamically monitored in aqueous solution. The potassium ion selective membrane on the semiconductor consisted of plasticized poly(vinyl chloride) (PVC) with bis(benzo-15-crown-5). The addition of a polyhedral oligomeric silsesquioxane to the plasticized PVC membrane greatly improved adhesion of the membrane onto Si(3)N(4) of the semiconductor surface, and the potential response was stabilized. The potential response was linear from 10(-2) to 10(-5) M logarithmic concentration of potassium ion. The selectivity coefficients were K(K(+),Li(+))(pot) = 10(-2.85), K(K(+),Na(+))(pot) = 10(-2.30), K(K(+),Rb(+))(pot) =10(-1.16), and K(K(+),Cs(+))(pot) = 10(-2.05).

  4. Analytic solution of the two-dimensional Fokker-Planck equation governing stochastic ion heating by a lower hybrid wave

    International Nuclear Information System (INIS)

    Malescio, G.

    1981-04-01

    The two-dimensional Fokker-Planck equation describing the ion motion in a coherent lower hybrid wave above the stochasticity threshold is analytically solved. An expression is given for the steady state power dissipation

  5. A simplified method for rapid quantification of intracellular nucleoside triphosphates by one-dimensional thin-layer chromatography

    DEFF Research Database (Denmark)

    Jendresen, Christian Bille; Kilstrup, Mogens; Martinussen, Jan

    2011-01-01

    -pyrophosphate (PRPP), and inorganic pyrophosphate (PPi) in cell extracts. The method uses one-dimensional thin-layer chromatography (TLC) and radiolabeled biological samples. Nucleotides are resolved at the level of ionic charge in an optimized acidic ammonium formate and chloride solvent, permitting...... quantification of NTPs. The method is significantly simpler and faster than both current two-dimensional methods and high-performance liquid chromatography (HPLC)-based procedures, allowing a higher throughput while common sources of inaccuracies and technical problems are avoided. For determination of PPi...

  6. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry in the identification of organic compounds in atmospheric aerosols from coniferous forest

    NARCIS (Netherlands)

    Kallio, M.; Jussila, M.; Rissanen, T.; Anttila, P.; Hartonen, K.; Reissell, A.; Vreuls, R.J.J.; Adahchour, M.; Hyotylainen, T.

    2006-01-01

    Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOF-MS) was applied in the identification of organic compounds in atmospheric aerosols from coniferous forest. The samples were collected at Hyytiälä, Finland, as part of the QUEST campaign, in

  7. Separation of five compounds from leaves of Andrographis paniculata (Burm. f.) Nees by off-line two-dimensional high-speed counter-current chromatography combined with gradient and recycling elution.

    Science.gov (United States)

    Zhang, Li; Liu, Qi; Yu, Jingang; Zeng, Hualiang; Jiang, Shujing; Chen, Xiaoqing

    2015-05-01

    An off-line two-dimensional high-speed counter-current chromatography method combined with gradient and recycling elution mode was established to isolate terpenoids and flavones from the leaves of Andrographis paniculata (Burm. f.) Nees. By using the solvent systems composed of n-hexane/ethyl acetate/methanol/water with different volume ratios, five compounds including roseooside, 5,4'-dihydroxyflavonoid-7-O-β-d-pyranglucuronatebutylester, 7,8-dimethoxy-2'-hydroxy-5-O-β-d-glucopyranosyloxyflavon, 14-deoxyandrographiside, and andrographolide were successfully isolated. Purities of these isolated compounds were all over 95% as determined by high-performance liquid chromatography. Their structures were identified by UV, mass spectrometry, and (1) H NMR spectroscopy. It has been demonstrated that the combination of off-line two-dimensional high-speed counter-current chromatography with different elution modes is an efficient technique to isolate compounds from complex natural product extracts. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Comparison of two algorithmic data processing strategies for metabolic fingerprinting by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Almstetter, Martin F; Appel, Inka J; Dettmer, Katja; Gruber, Michael A; Oefner, Peter J

    2011-09-28

    The alignment algorithm Statistical Compare (SC) developed by LECO Corporation for the processing of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) data was validated and compared to the in-house developed retention time correction and data alignment tool INCA (Integrative Normalization and Comparative Analysis) by a spike-in experiment and the comparative metabolic fingerprinting of a wild type versus a double mutant strain of Escherichia coli (E. coli). Starting with the same peak lists generated by LECO's ChromaTOF software, the accuracy of peak alignment and detection of 1.1- to 4-fold changes in metabolite concentration was assessed by spiking 20 standard compounds into an aqueous methanol extract of E. coli. To provide the same quality input signals for both alignment routines, the universal m/z 73 trace of the trimethylsilyl (TMS) group was used as a quantitative measure for all features. The performance of data processing and alignment was evaluated and illustrated by ROC curves. Statistical Compare performed marginally better at the lower fold changes, while INCA did so at the higher fold changes. Using SC, quantitative precision could be improved substantially by exploiting the signal intensities of metabolite-specific unique (U) m/z ion traces rather than the universal m/z 73 trace. A list of 56 features that distinguished the two E. coli strains was obtained by the SC alignment using m/z U with an estimated false discovery rate (FDR) of <0.05. Ultimately, 23 metabolites could be identified, one additional and five less than with INCA due to the failure of SC to extract unitized m/z U's across all fingerprints with suitable spectral intensities for the latter metabolites. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Revealing the Solvation Structure and Dynamics of Carbonate Electrolytes in Lithium-Ion Batteries by Two-Dimensional Infrared Spectrum Modeling.

    Science.gov (United States)

    Liang, Chungwen; Kwak, Kyungwon; Cho, Minhaeng

    2017-12-07

    Carbonate electrolytes in lithium-ion batteries play a crucial role in conducting lithium ions between two electrodes. Mixed solvent electrolytes consisting of linear and cyclic carbonates are commonly used in commercial lithium-ion batteries. To understand how the linear and cyclic carbonates introduce different solvation structures and dynamics, we performed molecular dynamics simulations of two representative electrolyte systems containing either linear or cyclic carbonate solvents. We then modeled their two-dimensional infrared (2DIR) spectra of the carbonyl stretching mode of these carbonate molecules. We found that the chemical exchange process involving formation and dissociation of lithium-ion/carbonate complexes is responsible for the growth of 2DIR cross peaks with increasing waiting time. In addition, we also found that cyclic carbonates introduce faster dynamics of dissociation and formation of lithium-ion/carbonate complexes than linear carbonates. These findings provide new insights into understanding the lithium-ion mobility and its interplay with solvation structure and ultrafast dynamics in carbonate electrolytes used in lithium-ion batteries.

  10. An Empirical Formula From Ion Exchange Chromatography and Colorimetry.

    Science.gov (United States)

    Johnson, Steven D.

    1996-01-01

    Presents a detailed procedure for finding an empirical formula from ion exchange chromatography and colorimetry. Introduces students to more varied techniques including volumetric manipulation, titration, ion-exchange, preparation of a calibration curve, and the use of colorimetry. (JRH)

  11. Application of ion chromatography to batchwise activated sludge process for simultaneous removal of thiosulfate, acetate and ammonium ions.

    OpenAIRE

    田中, 一彦; 黒川, 利一; 中島, 良三

    1988-01-01

    Ion chromatography (IC) with conductivity detection for determining anions and ion-exclusion chromatography (IEC) with conductivity detection for determining cations were investigated. Both techniques were applied to the establishment of the optimal conditions for the simultaneous removal of thiosulfate, acetate, and ammonium ions by a batchwise activated sludge process. The process consists of the combination of aerobic and anaerobic biological treatment processes by a sequential automatic p...

  12. Chromatography Of Metal Ions On Wood Cellulose Impregnated ...

    African Journals Online (AJOL)

    Adsorption chromatography of some heavy metal ions on wood cellulose of saw dust (wood waste dust) modified with hydrochloric acid, urea and thiourea was studied. Atomic absorption spectrophotometry (AAS) was used to determine the initial concentration of solutions of Zn2+, Cu2+, Ni2+, Pb2+, and Fe3+ metal ions.

  13. Partition/Ion-Exclusion Chromatographic Ion Stacking for the Analysis of Trace Anions in Water and Salt Samples by Ion Chromatography.

    Science.gov (United States)

    Akter, Fouzia; Saito, Shingo; Tasaki-Handa, Yuiko; Shibukawa, Masami

    2018-01-01

    A new analytical methodology for a simple and efficient on-line preconcentration of trace inorganic anions in water and salt samples prior to ion chromatographic determination is proposed. The preconcentration method is based on partition/ion-exclusion chromatographic ion stacking (PIEC ion stacking) with a hydrophilic polymer gel column containing a small amount of fixed anionic charges. The developed on-line PIEC ion stacking-ion chromatography method was validated by recovery experiments for the determination of nitrate in tap water in terms of both accuracy and precision, and the results showed the reliability of the method. The method proposed was also successfully applied to the determination of trace impurity nitrite and nitrate in reagent-grade salts of sodium sulfate. A low background level can be achieved since pure water is used as the eluant for the PIEC ion stacking. It is possible to reach sensitive detection at sub-μg L -1 levels by on-line PIEC ion stacking-ion chromatography.

  14. Fractionation of Aspergillus niger cellulases by combined ion exchange affinity chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Boyer, R.F.; Allen, T.L.; Dykema, P.A.

    1987-02-05

    Eight chemically modified cellulose supports were tested for their ability to adsorb components of the Aspergillus niger cellulase system. At least two of the most effective adsorbents, aminoethyl cellulose and carboxymethyl cellulose, were shown to be useful for the fractionation of cellulases. These supports apparently owe their resolving capacity to both ion exchange and biospecific binding effects; however, the relative importance of each effect is unknown. These observations form the basis for a new cellulase fractionation technique, combined ion exchange-affinity chromatography. 22 references.

  15. Determination of Na+ and K+ ions in the high-level liquid waste by ion chromatography (IC)

    International Nuclear Information System (INIS)

    Chen Lianzhong; Ma Guilan

    1992-01-01

    The determination of Na + and k + ions in the high-level liquid waste is investigated using ion chromatography. In order to protect the low capacity ion exchange resin in single column IC and remove the transition metal as well as other heavy metal ions that are contained in liquid waste, the pretreatment column with EDTA chelating resin is used. Those impurity metal ions are strongly absorbed by EDTA chelating resin and 100% of Na + and K + ions in the solution are eluted. The ability of the decontamination of EDTA chelating resin is satisfactory. The sample of the high-level liquid waste is diluted appropriately, then an aliquot of the sample is passed through the pretreatment column with EDTA chelating resin, the eluate is analysed by single column ion chromatography. The precision of this method is better than 5% for the determination of Na + and K + ions (at μg· ml -1 level)

  16. Simultaneous determination of inorganic and organic anions by ion chromatography

    International Nuclear Information System (INIS)

    Park, Yang Soon; Joe, Ki Soo; Han, Sun Ho; Park, Soon Dal; Choi, Kwang Soon

    1999-06-01

    Four methods were investigated for the simultaneous determination of several inorganic and organic anions in aqueous solution by ion chromatography. The first is two columns coupled system. The second is the gradient elution system with an anion exchange column. The third is the system with a mixed-mode stationary phase. The fourth is the system with an anion exchange column and the eluant of low conductivity without ion suppressor. The advantages and disadvantages of individual systems were discussed. The suitable methods were proposed for the application to the samples of the nuclear power industry and the environment. (author)

  17. Normal-Gamma-Bernoulli Peak Detection for Analysis of Comprehensive Two-Dimensional Gas Chromatography Mass Spectrometry Data.

    Science.gov (United States)

    Kim, Seongho; Jang, Hyejeong; Koo, Imhoi; Lee, Joohyoung; Zhang, Xiang

    2017-01-01

    Compared to other analytical platforms, comprehensive two-dimensional gas chromatography coupled with mass spectrometry (GC×GC-MS) has much increased separation power for analysis of complex samples and thus is increasingly used in metabolomics for biomarker discovery. However, accurate peak detection remains a bottleneck for wide applications of GC×GC-MS. Therefore, the normal-exponential-Bernoulli (NEB) model is generalized by gamma distribution and a new peak detection algorithm using the normal-gamma-Bernoulli (NGB) model is developed. Unlike the NEB model, the NGB model has no closed-form analytical solution, hampering its practical use in peak detection. To circumvent this difficulty, three numerical approaches, which are fast Fourier transform (FFT), the first-order and the second-order delta methods (D1 and D2), are introduced. The applications to simulated data and two real GC×GC-MS data sets show that the NGB-D1 method performs the best in terms of both computational expense and peak detection performance.

  18. Proceedings of the DAE-BRNS theme meeting on ion chromatography separations - state of art and perspectives

    International Nuclear Information System (INIS)

    Jeyakumar, S.; Ramakumar, K.L.

    2012-01-01

    Ion Chromatography (IC) plays a vital role in all disciplines of science and technology. In the field of trace separations and speciation studies, use of IC techniques becomes indispensable. In nuclear technology, IC plays a pivotal role in the reactor water chemistry, in the front end of fuel cycle especially in the characterization of nuclear materials including the reactor fuels, post irradiation examination, actinide speciation studies and in understanding the interaction and migration of actinide species in the geo environment. Ion chromatography is also useful in the studies related to waste management particularly for the separation and determination of fission products. The aim of this meeting is to provide a forum to all the researchers in the area of ion chromatography to discuss their recent findings and information, to learn from the mutual experiences and interests, and to promote cooperation both nationally and internationally. Ion chromatography techniques including Ion Chromatography Separations and Nuclear Materials, Speciation Studies by Ion chromatography, Hyphenated -IC Techniques, Reactor Water Chemistry and Ion Chromatography, Solid Phase Extraction and Sample Preparations for IC and Separation of Bio-molecules and Environmental aspects etc are discussed. Papers relevant to INIS are indexed separately

  19. High-throughput determination of vancomycin in human plasma by a cost-effective system of two-dimensional liquid chromatography.

    Science.gov (United States)

    Sheng, Yanghao; Zhou, Boting

    2017-05-26

    Therapeutic drug monitoring (TDM) is one of the most important services of clinical laboratories. Two main techniques are commonly used: the immunoassay and chromatography method. We have developed a cost-effective system of two-dimensional liquid chromatography with ultraviolet detection (2D-LC-UV) for high-throughput determination of vancomycin in human plasma that combines the automation and low start-up costs of the immunoassay with the high selectivity and sensitivity of the liquid chromatography coupled with mass spectrometric detection without incurring their disadvantages, achieving high cost-effectiveness. This 2D-LC system offers a large volume injection to provide sufficient sensitivity and uses simulated gradient peak compression technology to control peak broadening and to improve peak shape. A middle column was added to reduce the analysis cycle time and make it suitable for high-throughput routine clinical assays. The analysis cycle time was 4min and the peak width was 0.8min. Compared with other chromatographic methods that have been developed, the analysis cycle time and peak width for vancomycin was reduced significantly. The lower limit of quantification was 0.20μg/mL for vancomycin, which is the same as certain LC-MS/MS methods that have been recently developed and validated. The method is rapid, automated, and low-cost and has high selectivity and sensitivity for the quantification of vancomycin in human plasma, thus making it well-suited for use in hospital clinical laboratories. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Determination of tropane alkaloids by heart cutting reversed phase - Strong cation exchange two dimensional liquid chromatography.

    Science.gov (United States)

    Long, Zhen; Zhang, Yanhai; Gamache, Paul; Guo, Zhimou; Steiner, Frank; Du, Nana; Liu, Xiaoda; Jin, Yan; Liu, Xingguo; Liu, Lvye

    2018-01-01

    Current Chinese Pharmacopoeia (ChP) standards apply liquid extraction combined with one dimensional liquid chromatography (1DLC) method for determining alkaloids in herbal medicines. The complex pretreatments lead to a low analytical efficiency and possible component loss. In this study, a heart cutting reversed phase - strong cation exchange two dimensional liquid chromatography (RP - SCX 2DLC) approach was optimized for simultaneously quantifying tropane alkaloids (anisodine, scopolamine and hyoscyamine) in herbal medicines and herbal medicine tablets without further treatment of the filtered extract. The chromatographic conditions were systematically optimized in terms of column type, mobile phase composition and flow rate. To improve peak capacity and obtain symmetric peak shape of alkaloids, a polar group embedded C18 column combined with chaotropic salts was used in the first dimension. To remove the disturbance of non-alkaloids, achieve unique selectivity and acquire symmetric peak shape of alkaloids, an SCX column combined with phosphate buffer was used in the second dimension. Method validation was performed in terms of linearity, precision (0.54-0.82%), recovery (94.1-105.2%), limit of detection (LOD) and limit of quantification (LOQ) of the three analytes varied between 0.067-0.115mgL -1 and 0.195-0.268mgL -1 , respectively. The method demonstrated superiority over 1DLC method in respect of resolution (less alkaloid co-eluted), sample preparation (no pretreatment procedure) and transfer rate (minimum component loss). The optimized RP - SCX 2DLC approach was subsequently applied to quantify target alkaloids in five herbal medicines and herbal medicine tablets from three different manufactures. The results demonstrated that the developed heart cutting RP - SCX 2DLC approach represented a new, strategically significant methodology for the quality evaluation of tropane alkaloid in related herbal medicines that involve complex chemical matrix. Copyright

  1. Two-photon polymerization of metal ions doped acrylate monomers and oligomers for three-dimensional structure fabrication

    International Nuclear Information System (INIS)

    Duan Xuanming; Sun Hongbo; Kaneko, Koshiro; Kawata, Satoshi

    2004-01-01

    We have investigated two-photon polymerization of metal ions doped acrylate monomers and oligomers which is applied for three-dimensional (3D) micro/nano-structure fabrication. Titanium (IV) ions doped urethane acrylate photopolymerizable resins were synthesized, and their optical and polymerization properties were investigated. The resolution of two-photon polymerization for micro/nanofabrication was evaluated. Titanium dioxide (TiO 2 ) nanoparticles were generated in the polymer matrix of micron-sized polymer structures. A 3D diamond photonic crystal structure, which consisted of polymer composite materials of TiO 2 nanoparticles, was successfully fabricated by direct laser writing and its photonic bandgap was confirmed. This work would give us a new solution for producing 3D micro/nanodevices of functional polymer composite materials

  2. Effect of background correction on peak detection and quantification in online comprehensive two-dimensional liquid chromatography using diode array detection.

    Science.gov (United States)

    Allen, Robert C; John, Mallory G; Rutan, Sarah C; Filgueira, Marcelo R; Carr, Peter W

    2012-09-07

    A singular value decomposition-based background correction (SVD-BC) technique is proposed for the reduction of background contributions in online comprehensive two-dimensional liquid chromatography (LC×LC) data. The SVD-BC technique was compared to simply subtracting a blank chromatogram from a sample chromatogram and to a previously reported background correction technique for one dimensional chromatography, which uses an asymmetric weighted least squares (AWLS) approach. AWLS was the only background correction technique to completely remove the background artifacts from the samples as evaluated by visual inspection. However, the SVD-BC technique greatly reduced or eliminated the background artifacts as well and preserved the peak intensity better than AWLS. The loss in peak intensity by AWLS resulted in lower peak counts at the detection thresholds established using standards samples. However, the SVD-BC technique was found to introduce noise which led to detection of false peaks at the lower detection thresholds. As a result, the AWLS technique gave more precise peak counts than the SVD-BC technique, particularly at the lower detection thresholds. While the AWLS technique resulted in more consistent percent residual standard deviation values, a statistical improvement in peak quantification after background correction was not found regardless of the background correction technique used. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Fluorine and chlorine determination in oxides and metals by ion chromatography

    International Nuclear Information System (INIS)

    Evseeva, T.I.; Poletaeva, I.L.; Zemlyanukhina, N.A.; Pavlova, I.V.; Rybin, A.M.; Malykh, M.Yu.; Fedorova, L.A.

    1989-01-01

    Method for simultaneous determination of fluorine and chlorine microquantitie in tantalum, uranium and plutonium oxides, based on combined methods of pyrohydrolysis (1000-1100 deg C) and two-column ion chromatography with conductometric detection is suggested. The relative root-mean-square deviation of determination error is 0.2, the fluorine and chlorine content being 5·10 -4 mass%

  4. Comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry peak sorting algorithm.

    Science.gov (United States)

    Oh, Cheolhwan; Huang, Xiaodong; Regnier, Fred E; Buck, Charles; Zhang, Xiang

    2008-02-01

    We report a novel peak sorting method for the two-dimensional gas chromatography/time-of-flight mass spectrometry (GC x GC/TOF-MS) system. The objective of peak sorting is to recognize peaks from the same metabolite occurring in different samples from thousands of peaks detected in the analytical procedure. The developed algorithm is based on the fact that the chromatographic peaks for a given analyte have similar retention times in all of the chromatograms. Raw instrument data are first processed by ChromaTOF (Leco) software to provide the peak tables. Our algorithm achieves peak sorting by utilizing the first- and second-dimension retention times in the peak tables and the mass spectra generated during the process of electron impact ionization. The algorithm searches the peak tables for the peaks generated by the same type of metabolite using several search criteria. Our software also includes options to eliminate non-target peaks from the sorting results, e.g., peaks of contaminants. The developed software package has been tested using a mixture of standard metabolites and another mixture of standard metabolites spiked into human serum. Manual validation demonstrates high accuracy of peak sorting with this algorithm.

  5. Characterisation of middle-distillates by comprehensive two-dimensional gas chromatography (GC x GC): A powerful alternative for performing various standard analysis of middle-distillates.

    Science.gov (United States)

    Vendeuvre, Colombe; Ruiz-Guerrero, Rosario; Bertoncini, Fabrice; Duval, Laurent; Thiébaut, Didier; Hennion, Marie-Claire

    2005-09-09

    The detailed characterisation of middle distillates is essential for a better understanding of reactions involved in refining process. Owing to higher resolution power and enhanced sensitivity, comprehensive two-dimensional gas chromatography (GC x GC) is a powerful tool for improving characterisation of petroleum samples. The aim of this paper is to compare GC x GC and various ASTM methods -- gas chromatography (GC), liquid chromatography (LC) and mass spectrometry (MS) -- for group type separation and detailed hydrocarbon analysis. Best features of GC x GC are demonstrated and compared to these techniques in terms of cost, time consumption and accuracy. In particular, a new approach of simulated distillation (SimDis-GC x GC) is proposed: compared to the standard method ASTM D2887 it gives unequal information for better understanding of conversion process.

  6. [Application of off-line two dimensional reversed-phase liquid chromatography/supercritical fluid chromatography to the separation of the seeds of Trichosanthes kirilowii Maxim].

    Science.gov (United States)

    Yuan, Yun; Xin, Huaxia; Peng, Ziyue; Fu, Qing; Jin, Yu

    2017-07-08

    An off-line two dimensional reversed-phase liquid chromatography/supercritical fluid chromatography (2D RPLC/SFC) method was developed for the separation of the seeds of Trichosanthes kirilowii Maxim . ( T. kirilowii .). In the experiment, RPLC was used in the first dimension to analyze the samples. And 12 fractions (F 1 -F 12 ) were obtained according to the chromatographic peak collection mode, the fractions were re-analyzed in both RPLC and SFC modes. The results clearly showed that this 2D method had good orthogonality. The SFC was used as the second dimension. Ethanol- n -hexane (3:7, v/v) was used as a modifier in SFC. The modifier could provide appropriate elution power. When the sample load increased, it could also ensure the solubility of samples. The 2D RPLC/SFC method had obvious advantages for separating the compounds with similar properties, enriching and purifying the trace components. Finally, 150 peaks could be detected. The off-line 2D RPLC/SFC method will be further enlarged to a preparative level for preparation of compounds. The method can provide a practical reference for the purification of chemical constituents and material basis research of the seeds of T. kirilowii . in the future.

  7. Two-dimensional evaluation of an ion plasma produced by pulsed lasers extracted by non-parallel collectors

    International Nuclear Information System (INIS)

    Mahdieh, M H; Gavili, A

    2003-01-01

    Two-dimensional hydrodynamics of ion extraction from quasi-neutral plasmas has been calculated numerically for non-parallel ion extractors, and the results compared with those for the parallel case. The ions were assumed to be initially uniform with a very steep density profile at the boundaries, and held between two non-parallel metal plates as cathode and anode with fixed potentials. Experimentally, tunable pulsed lasers through stepwise photo-excitation and photo-ionization or multi-photo-ionization processes can produce such plasma. Poisson's equation was solved simultaneously with the equations of mass and momentum, assuming the Maxwell-Boltzmann distribution for electrons. Ordinary Cartesian co-ordinates are not suitable for the rotated extractor geometry; therefore using the 'algebraic method' a transformation from the physical domain into the computational rectangular plane is applied for analysing the irregular boundaries. Such a technique provides adequate resolution for the boundary layer. Using a first-order explicit upwind differencing in an appropriate transformed Cartesian co-ordinate system, the hydrodynamics of the plasma ions between the two non-parallel electrodes was evaluated. In these calculations electric potential, ion density between the two electrodes, and the extraction time were assessed, considering three separate regions for the plasma, i.e. the ion sheath where (n i >>n e ∼0), the transition region (pre-sheath) (n i = n e ), and the quasi-neutral plasma (n i -n e i ). The results were compared with those for parallel electrodes. A significant discrepancy was found between the two results. From the calculation, the non-uniform asymmetric potential contour, and the ion density contour across the plasma, were obtained for the non-parallel electrodes. For comparison with the parallel extractors, we have also obtained almost the same extraction time for the non-parallel extractors

  8. Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

    Science.gov (United States)

    Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

    2017-03-01

    An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Proteomic profiling of human pleural effusion using two-dimensional nano liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Tyan, Yu-Chang; Wu, Hsin-Yi; Lai, Wu-Wei; Su, Wu-Chou; Liao, Pao-Chi

    2005-01-01

    Pleural effusion, an accumulation of pleural fluid, contains proteins originated from plasma filtrate and, especially when tissues are damaged, parenchyma interstitial spaces of lungs and/or other organs. This study details protein profiles in human pleural effusion from 43 lung adenocarcinoma patients by a two-dimensional nano-high performance liquid chromatography electrospray ionization tandem mass spectrometry (2D nano-HPLC-ESI-MS/MS) system. The experimental results revealed the identification of 1415 unique proteins from human pleural effusion. Among these 124 proteins identified with higher confidence levels, some proteins have not been reported in plasma and may represent proteins specifically present in pleural effusion. These proteins are valuable for mass identification of differentially expressed proteins involved in proteomics database and screening biomarker to further study in human lung adenocarcinoma. The significance of the use of proteomics analysis of human pleural fluid for the search of new lung cancer marker proteins, and for their simultaneous display and analysis in patients suffering from lung disorders has been examined.

  10. SnSe2 Two Dimensional Anodes for Advanced Sodium Ion Batteries

    KAUST Repository

    Zhang, Fan

    2017-05-30

    Sodium-ion batteries (SIBs) are considered as a promising alternative to lithium-ion batteries (LIBs) for large-scale renewable energy storage units due to the abundance of sodium resource and its low cost. However, the development of anode materials for SIBs to date has been mainly limited to some traditional anodes for LIBs, such as carbonaceous materials. SnSe2 is a member of two dimensional layered transition metal dichalcogenide (TMD) family, which has been predicted to have high theoretical capacity as anode material for sodium ion batteries (756 mAh g-1), thanks to its layered crystal structure. Yet, there have been no studies on using SnSe2 as Na ion battery anode. In this thesis, we developed a simple synthesis method to prepare pure SnSe2 nanosheets, employing N2 saturated NaHSe solution as a new selenium source. The SnSe2 2D sheets achieve theoretical capacity during the first cycle, and a stable and reversible specific capacity of 515 mAh g-1 at 0.1 A g-1 after 100 cycles, with excellent rate performance. Among all of the reported transition metal selenides, our SnSe2 sample has the highest reversible capacity and the best rate performances. A combination of ex-situ high resolution transmission electron microscopy (HRTEM) and X-ray diffraction was used to study the mechanism of sodiation and desodiation process in this SnSe2, and to understand the reason for the excellent results that we have obtained. The analysis indicate that a combination of conversion and alloying reactions take place with SnSe2 anodes during battery operation, which helps to explain the high capacity of SnSe2 anodes for SIBs compared to other binary selenides. Density functional theory was used to elucidate the volume changes taking place in this important 2D material.

  11. Matrix influences on the determination of common ions by using ion chromatography part 1--determination of inorganic anions.

    Science.gov (United States)

    Michalski, Rajmund; Lyko, Aleksandra; Kurzyca, Iwona

    2012-07-01

    Ion chromatography is the most popular instrumental analytical method used for the determination of anions and cations in water and wastewater. Isocratic ion chromatography with suppressed conductivity detection is frequently used in laboratories carrying out routine analyses of inorganic anions. The paper presents the results of the research into the influence of selected inorganic anions dominant in environmental samples (Cl(-), NO(3)(-), SO(4)(2-)) on the possibility of simultaneous determination of F(-), Cl(-), NO(2)(-), NO(3)(-), PO(4)(3-) and SO(4)(2-) with the application of this most popular ion chromatography type in standard separation conditions. Four Dionex and four Metrohm anion-exchange columns were tested in standard separation conditions recommended by their manufacturers with both standard solutions and environmental samples with complex matrix.

  12. Ion exchange separation of nitrate from uranium compounds and its determination by spectrophotometry and ion chromatography

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Atalla, L.T.; Abrao, A.

    1985-11-01

    A procedure for the separation of nitrate from uranium compounds by retaintion of uranyl ion on a cationic ion exchanger and its determination in the effluent is described. Nitrate is analysed by the spectrometric method with 1-phenol-2,4-dissulphonic acid. This determination covers the 1 to 10 μg NO - 3 /mL range and requires an amount of 10 to 100 μg NO - 3 . The main interference is uranium (VI) due its own intense yellow color. This difficulty is overcome by the complete separation of UO 2 ++ with the cationic resin. Alternatively, the ion chromatography technique is used for the determination of nitrate in the effluent of the cationic resin. The determination was easily made by the comparison of the nitrate peak hights of the analyte and the standard solutions. The ion chromatography method is very sensitive (0,3 μg NO - 3 /mL), reproducible and suitable for routine analysis and permits the determination of fraction of part per million of nitrate in uranium. The results of nitrate determination using both spectrophotometric and ion chromatography techniques are compared. The method is being routinely applied for the quality control of uranium compounds in the fuel cycle, specially uranium oxide, ammonium diuranate, uranium peroxide and ammonium uranyl tricarbonate. (Author) [pt

  13. Characterisation of biodegradation capacities of environmental microflorae for diesel oil by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Penet, Sophie; Vendeuvre, Colombe; Bertoncini, Fabrice; Marchal, Rémy; Monot, Frédéric

    2006-12-01

    In contaminated soils, efficiency of natural attenuation or engineered bioremediation largely depends on biodegradation capacities of the local microflorae. In the present study, the biodegradation capacities of various microflorae towards diesel oil were determined in laboratory conditions. Microflorae were collected from 9 contaminated and 10 uncontaminated soil samples and were compared to urban wastewater activated sludge. The recalcitrance of hydrocarbons in tests was characterised using both gas chromatography (GC) and comprehensive two-dimensional gas chromatography (GCxGC). The microflorae from contaminated soils were found to exhibit higher degradation capacities than those from uncontaminated soil and activated sludge. In cultures inoculated by contaminated-soil microflorae, 80% of diesel oil on an average was consumed over 4-week incubation compared to only 64% in uncontaminated soil and 60% in activated sludge cultures. As shown by GC, n-alkanes of diesel oil were totally utilised by each microflora but differentiated degradation extents were observed for cyclic and branched hydrocarbons. The enhanced degradation capacities of impacted-soil microflorae resulted probably from an adaptation to the hydrocarbon contaminants but a similar adaptation was noted in uncontaminated soils when conifer trees might have released natural hydrocarbons. GCxGC showed that a contaminated-soil microflora removed all aromatics and all branched alkanes containing less than C(15). The most recalcitrant compounds were the branched and cyclic alkanes with 15-23 atoms of carbon.

  14. Using comprehensive two-dimensional gas chromatography to explore the geochemistry of the Santa Barbara oil seeps

    Energy Technology Data Exchange (ETDEWEB)

    Reddy, Christopher; Nelson, Robert

    2013-03-27

    The development of comprehensive two-dimensional gas chromatography (GC x GC) has expanded the analytical window for studying complex mixtures like oil. Compared to traditional gas chromatography, this technology separates and resolves at least an order of magnitude more compounds, has a much larger signal to noise ratio, and sorts compounds based on their chemical class; hence, providing highly refined inventories of petroleum hydrocarbons in geochemical samples that was previously unattainable. In addition to the increased resolution afforded by GC x GC, the resulting chromatograms have been used to estimate the liquid vapor pressures, aqueous solubilities, octanol-water partition coefficients, and vaporization enthalpies of petroleum hydrocarbons. With these relationships, powerful and incisive analyses of phase-transfer processes affecting petroleum hydrocarbon mixtures in the environment are available. For example, GC x GC retention data has been used to quantitatively deconvolve the effects of phase transfer processes such as water washing and evaporation. In short, the positive attributes of GC x GC-analysis have led to a methodology that has revolutionized the analysis of petroleum hydrocarbons. Overall, this research has opened numerous fields of study on the biogeochemical "genetics" (referred to as petroleomics) of petroleum samples in both subsurface and surface environments. Furthermore, these new findings have already been applied to the behavior of oil at other seeps as well, for petroleum exploration and oil spill studies.

  15. Comparison of an Electronic Nose Based on Ultrafast Gas Chromatography, Comprehensive Two-Dimensional Gas Chromatography, and Sensory Evaluation for an Analysis of Type of Whisky

    Directory of Open Access Journals (Sweden)

    Paulina Wiśniewska

    2017-01-01

    Full Text Available Whisky is one of the most popular alcoholic beverages. There are many types of whisky, for example, Scotch, Irish, and American whisky (called bourbon. The whisky market is highly diversified, and, because of this, it is important to have a method which would enable rapid quality evaluation and authentication of the type of whisky. The aim of this work was to compare 3 methods: an electronic nose based on the technology of ultrafast gas chromatography (Fast-GC, comprehensive two-dimensional gas chromatography (GC × GC, and sensory evaluation. The selected whisky brands included 6 blended whiskies from Scotland, 4 blended whiskies from Ireland, and 4 bourbons produced in the USA. For data analysis, peak heights of chromatograms were used. The panelists who took part in sensory evaluations included 4 women and 4 men. The obtained data were analyzed by 2 chemometric methods: partial least squares discriminant analysis (PLS-DA and discrimination function analysis (DFA. E-nose and GC × GC allowed for differentiation between whiskies by type. Sensory analysis did not allow for differentiation between whiskies by type, but it allowed giving consumer preferences.

  16. Evaluation of reversible interconversion in comprehensive two-dimensional gas chromatography using enantioselective columns in first and second dimensions.

    Science.gov (United States)

    Kröger, Sabrina; Wong, Yong Foo; Chin, Sung-Tong; Grant, Jacob; Lupton, David; Marriott, Philip J

    2015-07-24

    The reversible molecular interconversion behaviour of a synthesised oxime (2-phenylpropanaldehyde oxime; (C6H5)CH(CH3)CHN(OH)) was investigated by both, single dimensional gas chromatography (1D GC) and comprehensive two-dimensional gas chromatography (GC×GC). Previous studies on small molecular weight oximes were extended to this larger aromatic oxime (molar mass 149.19gmol(-1)) with interest in the extent of interconversion, enantioselective resolution, and retention time. On a polyethylene glycol (PEG; wax-type) column, a characteristic interconversion zone between two antipodes of E and Z isomers was formed by molecules which have undergone isomerisation on the column (E⇌Z). The extent of interconversion was investigated by varying chromatographic conditions (oven temperature and carrier flow rate) to understand the nature of the behaviour observed. The extent of interconversion was negligible in both enantioselective and methyl-phenylpolysiloxane phase-columns, correlating with the low polarity of the stationary phase. In order to obtain isomerisation along with enantio-resolution, a wax-type and an enantioselective column were coupled in either enantioselective-wax or wax-enantioselective order. The most appropriate column arrangement was selected for study by using a GC×GC experiment with either a wax-phase or phenyl-methylpolysiloxane phase as (2)D column. In addition to evaluation of these fast elution columns, a long narrow-bore enantioselective column (10m) was introduced as (2)D, providing an enantioselective-PEG (coupled-column ensemble: (1)D1+(1)D2)×enantioselective ((2)D) column combination. In this instance, the (1)D1 enantioselective column provides enantiomeric separation of the corresponding enantiomers ((R) and (S)) of (E)- and (Z)-2-phenylpropanaldehyde oxime, followed by E/Z isomerisation in the coupled (1)D2 PEG (reactor) column. The resulting chromatographic interconversion region was modulated and separated into either E/Z isomers

  17. Ion-Exchange Chromatography: Basic Principles and Application.

    Science.gov (United States)

    Cummins, Philip M; Rochfort, Keith D; O'Connor, Brendan F

    2017-01-01

    Ion-Exchange Chromatography (IEC) allows for the separation of ionizable molecules on the basis of differences in charge properties. Its large sample-handling capacity, broad applicability (particularly to proteins and enzymes), moderate cost, powerful resolving ability, and ease of scale-up and automation have led to it becoming one of the most versatile and widely used of all liquid chromatography (LC) techniques. In this chapter, we review the basic principles of IEC, as well as the broader criteria for selecting IEC conditions. By way of further illustration, we outline basic laboratory protocols to partially purify a soluble serine peptidase from bovine whole brain tissue, covering crude tissue extract preparation through to partial purification of the target enzyme using anion-exchange chromatography. Protocols for assaying total protein and enzyme activity in both pre- and post-IEC fractions are also described.

  18. Three-dimensional simulation of the electromagnetic ion/ion beam instability: cross field diffusion

    Directory of Open Access Journals (Sweden)

    H. Kucharek

    2000-01-01

    Full Text Available In a system with at least one ignorable spatial dimension charged particles moving in fluctuating fields are tied to the magnetic field lines. Thus, in one-and two-dimensional simulations cross-field diffusion is inhibited and important physics may be lost. We have investigated cross-field diffusion in self-consistent 3-D magnetic turbulence by fully 3-dimensional hybrid simulation (macro-particle ions, massless electron fluid. The turbulence is generated by the electromagnetic ion/ion beam instability. A cold, low density, ion beam with a high velocity stream relative to the background plasma excites the right-hand resonant instability. Such ion beams may be important in the region of the Earth's foreshock. The field turbulence scatters the beam ions parallel as well as perpendicular to the magnetic field. We have determined the parallel and perpendicular diffusion coefficient for the beam ions in the turbulent wave field. The result compares favourably well (within a factor 2 with hard-sphere scattering theory for the cross-field diffusion coefficient. The cross-field diffusion coefficient is larger than that obtained in a static field with a Kolmogorov type spectrum and similar total fluctuation power. This is attributed to the resonant behaviour of the particles in the fluctuating field.

  19. Fraction transfer process in on-line comprehensive two-dimensional liquid phase separations

    Czech Academy of Sciences Publication Activity Database

    Česla, P.; Křenková, Jana

    2017-01-01

    Roč. 40, č. 1 (2017), s. 109-123 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GA14-06319S Institutional support: RVO:68081715 Keywords : capillary electrophoresis * comprehensive liquid chromatography * fraction transfer * two-dimensional separations * liquid chromatography Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 2.557, year: 2016

  20. Radiogas chromatography mass spectrometry in the selected ion monitoring mode

    International Nuclear Information System (INIS)

    Doerfler, D.L.; Rosenblum, E.R.; Malloy, J.M.; Naworal, J.D.; McManus, I.R.; Campbell, I.M.

    1980-01-01

    The value of selected ion monitoring in analyzing biological radio isotope incorporation experiments by radiogas chromatography mass spectrometry is illustrated with reference to the biosynthesis of the mycotoxin mycophenolic acid in Penicillium brevicompactum and the mode of action of the anticholesterolemic drug 20,25-diazacholesterol. Both examples used 1-[ 14 C]acetate precursors. It is shown that the increased sensitivity and specificity of the selected ion monitoring mode detector permits straightforward detection and identification of the relatively small cellular pools associated with metabolic intermediates. The computer program RADSIM is described. Problems that still exist in using radiogas gas chromatography mass spectrometry technology to analyse isotope incorporation experiments are discussed. (author)

  1. Thermodynamic-based retention time predictions of endogenous steroids in comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Silva, Aline C A; Ebrahimi-Najafadabi, Heshmatollah; McGinitie, Teague M; Casilli, Alessandro; Pereira, Henrique M G; Aquino Neto, Francisco R; Harynuk, James J

    2015-05-01

    This work evaluates the application of a thermodynamic model to comprehensive two-dimensional gas chromatography (GC × GC) coupled with time-of-flight mass spectrometry for anabolic agent investigation. Doping control deals with hundreds of drugs that are prohibited in sports. Drug discovery in biological matrices is a challenging task that requires powerful tools when one is faced with the rapidly changing designer drug landscape. In this work, a thermodynamic model developed for the prediction of both primary and secondary retention times in GC × GC has been applied to trimethylsilylated hydroxyl (O-TMS)- and methoxime-trimethylsilylated carbonyl (MO-TMS)-derivatized endogenous steroids. This model was previously demonstrated on a pneumatically modulated GC × GC system, and is applied for the first time to a thermally modulated GC × GC system. Preliminary one-dimensional experiments allowed the calculation of thermodynamic parameters (ΔH, ΔS, and ΔC p ) which were successfully applied for the prediction of the analytes' interactions with the stationary phases of both the first-dimension column and the second-dimension column. The model was able to predict both first-dimension and second-dimension retention times with high accuracy compared with the GC × GC experimental measurements. Maximum differences of -8.22 s in the first dimension and 0.4 s in the second dimension were encountered for the O-TMS derivatives of 11β-hydroxyandrosterone and 11-ketoetiocholanolone, respectively. For the MO-TMS derivatives, the largest discrepancies were from testosterone (9.65 ) for the first-dimension retention times and 11-keto-etiocholanolone (0.4 s) for the second-dimension retention times.

  2. Second dimension column ensemble pressure tuning in comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Sharif, Khan M; Kulsing, Chadin; Junior, Ademario I da Silva; Marriott, Philip J

    2018-02-09

    A pressure tunable (PT) coupled column ensemble has been implemented for the second dimension ( 2 D) separation in comprehensive two dimensional gas chromatography (GC×PTGC). This process requires two columns to be connected by a pressure junction, as a replacement for a single narrow bore, short column in 2 D. Various 2 D 1 and 2 D 2 columns may be selected to provide complementary selectivity (polarity) compared to the 1 D column. The tunable residence time arising from differential pressure drop in each 2 D column results in a tunable fractional contribution of each column in the 2 D separation. A sample mixture comprising different chemical classes, including alkanes and alcohols, is used to identify the feasibility and extent of selectivity tuning possible in GC×PTGC. The column length is also varied due to the imposed challenge of wraparound in the PT coupled column system as pressures are adjusted in the 2 D separation. Different experimental parameters, stationary phase materials and column lengths have been applied to investigate and understand the separation behaviour of the 2 D PT coupled column GC×GC system. Results are discussed considering analyte retention time, peak width, linear velocity and the contribution of each 2 D column. A specific and unexpected example of GC×GC separation was demonstrated where the peak positions of polar and apolar compounds could almost swap their 2 D retention position by application of PT. Kerosene was analysed as an example of complex sample analysis by GC×PTGC system. This process is shown to be a practical approach for altering different stationary phase selectivities in a single 2 D arrangement in GC×GC. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Two-step ion-exchange chromatographic purification combined with reversed-phase chromatography to isolate C-peptide for mass spectrometric analysis.

    Science.gov (United States)

    Kabytaev, Kuanysh; Durairaj, Anita; Shin, Dmitriy; Rohlfing, Curt L; Connolly, Shawn; Little, Randie R; Stoyanov, Alexander V

    2016-02-01

    A liquid chromatography with mass spectrometry on-line platform that includes the orthogonal techniques of ion exchange and reversed phase chromatography is applied for C-peptide analysis. Additional improvement is achieved by the subsequent application of cation- and anion-exchange purification steps that allow for isolating components that have their isoelectric points in a narrow pH range before final reversed-phase mass spectrometry analysis. The utility of this approach for isolating fractions in the desired "pI window" for profiling complex mixtures is discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Advances in silver ion chromatography for the analysis of fatty acids and triacylglycerols-2001 to 2011.

    Science.gov (United States)

    Momchilova, Svetlana M; Nikolova-Damyanova, Boryana M

    2012-01-01

    An effort is made to critically present the achievements in silver ion chromatography during the last decade. Novelties in columns, mobile-phase compositions and detectors are described. Recent applications of silver ion chromatography in the analysis of fatty acids and triacylglycerols are presented while stressing novel analytical strategies or new objects. The tendencies in the application of the method in complementary ways with reversed-phase chromatography, chiral chromatography and, especially, mass detection are outlined.

  5. Comparative Analysis of Mass Spectral Similarity Measures on Peak Alignment for Comprehensive Two-Dimensional Gas Chromatography Mass Spectrometry

    Science.gov (United States)

    2013-01-01

    Peak alignment is a critical procedure in mass spectrometry-based biomarker discovery in metabolomics. One of peak alignment approaches to comprehensive two-dimensional gas chromatography mass spectrometry (GC×GC-MS) data is peak matching-based alignment. A key to the peak matching-based alignment is the calculation of mass spectral similarity scores. Various mass spectral similarity measures have been developed mainly for compound identification, but the effect of these spectral similarity measures on the performance of peak matching-based alignment still remains unknown. Therefore, we selected five mass spectral similarity measures, cosine correlation, Pearson's correlation, Spearman's correlation, partial correlation, and part correlation, and examined their effects on peak alignment using two sets of experimental GC×GC-MS data. The results show that the spectral similarity measure does not affect the alignment accuracy significantly in analysis of data from less complex samples, while the partial correlation performs much better than other spectral similarity measures when analyzing experimental data acquired from complex biological samples. PMID:24151524

  6. Identification of oxidised proteins in the matrix of rice leaf mitochondria by immunoprecipitation and two-dimensional liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Kristensen, B.K.; Askerlund, P.; Bykova, N.V.

    2004-01-01

    .2 mM CuSO4 for 10 min at room temperature). The oxidised proteins in both samples were tagged with dinitrophenylhydrazine (DNP), which forms a covalent bond with carbonyl groups. The DNP-tagged proteins were immunoprecipitated using anti-DNP antibodies and digested with trypsin. The mixture...... of peptides was analysed by nano-HPLC coupled online to an ESI-Quad-TOF mass spectrometer. The peptides were separated by stepwise ion exchange chromatography followed by reverse phase chromatography (2D-LC), and analysed by MS/MS. Proteins were identified by un-interpreted fragment ion database searches...... blots showed that neither the isolation of mitochondria, nor their subfractionation introduced carbonyl groups. We therefore conclude that a number of proteins are oxidised in the matrix of rice leaf mitochondria in vivo and further identify a group of proteins that are particularly susceptible to mild...

  7. Comparison of one- and two-dimensional liquid chromatography approaches in the label-free quantitative analysis of Methylocella silvestris.

    Science.gov (United States)

    Patel, Nisha A; Crombie, Andrew; Slade, Susan E; Thalassinos, Konstantinos; Hughes, Chris; Connolly, Joanne B; Langridge, James; Murrell, J Colin; Scrivens, James H

    2012-09-07

    The proteome of the bacterium Methylocella silvestris has been characterized using reversed phase ultra high pressure liquid chromatography (UPLC) and two-dimensional reversed phase (high pH)-reversed phase (low pH) UPLC prior to mass spectrometric analysis. Variations in protein expression levels were identified with the aid of label-free quantification in a study of soluble protein extracts from the organism grown using methane, succinate, or propane as a substrate. The number of first dimensional fractionation steps has been varied for 2D analyses, and the impact on data throughput and quality has been demonstrated. Comparisons have been made regarding required experimental considerations including total loading of biological samples required, instrument time, and resulting data file sizes. The data obtained have been evaluated with respect to number of protein identifications, confidence of assignments, sequence coverage, relative levels of proteins, and dynamic range. Good qualitative and quantitative agreement was observed between the different approaches, and the potential benefits and limitations of the reversed phase-reversed phase UPLC technique in label-free analysis are discussed. A preliminary screen of the protein regulation data has also been performed, providing evidence for a possible propane assimilation route.

  8. Identification of snake venom allergens by two-dimensional electrophoresis followed by immunoblotting.

    Science.gov (United States)

    Hu, Yujing; Yang, Liming; Yang, Haiwei; He, Shaoheng; Wei, Ji-Fu

    2017-01-01

    This allergic reaction to snake venom was described to occur in patients after recurrent exposure through bites in amateur and professional snake handlers, which might be underestimated and contribute to fatal snakebites in victim, independently from the toxicity of the venom itself. Few allergens were identified from snake venoms by normal SDS-PAGE, which cannot separate the snake venom completely. In the present study, we identified nine potential allergens by two-dimensional (2D) electrophoresis followed by immunoblotting (named as allergenomics) in Protobothrops mucrosquamatus venom. By multidimensional liquid chromatography-ion trap mass spectrometry (MDLC-ESI-LTQ-MS/MS) analysis, six allergens showed sequence similarity to snake venom serine proteinases. Other allergens showed sequence similarity to snake venom metalloproteinase. These allergic reactions to snake venom allergens might contribute to fatal snakebites in victim, independently. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Ion Chromatography-on-a-chip for Water Quality Analysis

    Science.gov (United States)

    Kidd, R. D.; Noell, A.; Kazarians, G.; Aubrey, A. D.; Scianmarello, N.; Tai, Y.-C.

    2015-01-01

    We report progress towards developing a Micro-Electro-Mechanical Systems (MEMS)- based ion chromatograph (IC) for crewed spacecraft water analysis. This IC-chip is an offshoot of a NASA-funded effort to produce a high performance liquid chromatograph (HPLC)-chip. This HPLC-chip system would require a desalting (i.e. ion chromatography) step. The complete HPLC instrument consists of the Jet Propulsion Labortory's (JPL's) quadrupole ion trap mass spectrometer integrated with a state-of-the-art MEMS liquid chromatograph (LC) system developed by the California Institute of Technology's (Caltech's) Micromachining Laboratory. The IC version of the chip consist of an electrolysis-based injector, a separation column, two electrolysis pumps for gradient generation, mixer, and a built-in conductivity detector. The HPLC version of the chip also includes a nanospray tip. The low instrument mass, coupled with its high analytical capabilities, makes the LC chip ideally suitable for wide range of applications such as trace contaminant, inorganic analytical science and, when coupled to a mass spectrometer, a macromolecular detection system for either crewed space exploration vehicles or robotic planetary missions.

  10. High-Level Heteroatom Doped Two-Dimensional Carbon Architectures for Highly Efficient Lithium-Ion Storage

    Directory of Open Access Journals (Sweden)

    Zhijie Wang

    2018-04-01

    Full Text Available In this work, high-level heteroatom doped two-dimensional hierarchical carbon architectures (H-2D-HCA are developed for highly efficient Li-ion storage applications. The achieved H-2D-HCA possesses a hierarchical 2D morphology consisting of tiny carbon nanosheets vertically grown on carbon nanoplates and containing a hierarchical porosity with multiscale pore size. More importantly, the H-2D-HCA shows abundant heteroatom functionality, with sulfur (S doping of 0.9% and nitrogen (N doping of as high as 15.5%, in which the electrochemically active N accounts for 84% of total N heteroatoms. In addition, the H-2D-HCA also has an expanded interlayer distance of 0.368 nm. When used as lithium-ion battery anodes, it shows excellent Li-ion storage performance. Even at a high current density of 5 A g−1, it still delivers a high discharge capacity of 329 mA h g−1 after 1,000 cycles. First principle calculations verifies that such unique microstructure characteristics and high-level heteroatom doping nature can enhance Li adsorption stability, electronic conductivity and Li diffusion mobility of carbon nanomaterials. Therefore, the H-2D-HCA could be promising candidates for next-generation LIB anodes.

  11. Solid phase extraction in combination with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry for the detailed investigation of volatiles in South African red wines

    NARCIS (Netherlands)

    Weldegergis, B.T.; Crouch, A.M.; Górecki, T.; Villiers, de A.

    2011-01-01

    Comprehensive two-dimensional gas chromatography in combination with time-of-flight mass spectrometry (GC × GC–TOFMS) has been applied for the analysis of volatile compounds in three young South African red wines. In spite of the significant benefits offered by GC × GC–TOFMS for the separation and

  12. Analysis of Polycyclic Aromatic Hydrocarbons in Ambient Aerosols by Using One-Dimensional and Comprehensive Two-Dimensional Gas Chromatography Combined with Mass Spectrometric Method: A Comparative Study

    Directory of Open Access Journals (Sweden)

    Yun Gyong Ahn

    2018-01-01

    Full Text Available Advanced separation technology paired with mass spectrometry is an ideal method for the analysis of atmospheric samples having complex chemical compositions. Due to the huge variety of both natural and anthropogenic sources of organic compounds, simultaneous quantification and identification of organic compounds in aerosol samples represents a demanding analytical challenge. In this regard, comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS has become an effective analytical method. However, verification and validation approaches to quantify these analytes have not been critically evaluated. We compared the performance of gas chromatography with quadrupole mass spectrometry (GC-qMS and GC×GC-TOFMS for quantitative analysis of eighteen target polycyclic aromatic hydrocarbons (PAHs. The quantitative obtained results such as limits of detection (LODs, limits of quantification (LOQs, and recoveries of target PAHs were approximately equivalent based on both analytical methods. Furthermore, a larger number of analytes were consistently identified from the aerosol samples by GC×GC-TOFMS compared to GC-qMS. Our findings suggest that GC×GC-TOFMS would be widely applicable to the atmospheric and related sciences with simultaneous target and nontarget analysis in a single run.

  13. Comprehensive two-dimensional liquid chromatography and hyphenated liquid chromatography to study the degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, T.

    2005-01-01

    Size exclusion chromatography (SEC), gradient polymer elution chromatography (GPEC) and liquid chromatography at critical conditions (LC-CC) have been developed and applied to observe chemical changes in poly(bisphenol A)carbonate (PC) due to hydrolytic degradation. Especially LC-CC appeared to be

  14. Doping of two-dimensional MoS2 by high energy ion implantation

    Science.gov (United States)

    Xu, Kang; Zhao, Yuda; Lin, Ziyuan; Long, Yan; Wang, Yi; Chan, Mansun; Chai, Yang

    2017-12-01

    Two-dimensional (2D) materials have been demonstrated to be promising candidates for next generation electronic circuits. Analogues to conventional Si-based semiconductors, p- and n-doping of 2D materials are essential for building complementary circuits. Controllable and effective doping strategies require large tunability of the doping level and negligible structural damage to ultrathin 2D materials. In this work, we demonstrate a doping method utilizing a conventional high-energy ion-implantation machine. Before the implantation, a Polymethylmethacrylate (PMMA) protective layer is used to decelerate the dopant ions and minimize the structural damage to MoS2, thus aggregating the dopants inside MoS2 flakes. By optimizing the implantation energy and fluence, phosphorus dopants are incorporated into MoS2 flakes. Our Raman and high-resolution transmission electron microscopy (HRTEM) results show that only negligibly structural damage is introduced to the MoS2 lattice during the implantation. P-doping effect by the incorporation of p+ is demonstrated by Photoluminescence (PL) and electrical characterizations. Thin PMMA protection layer leads to large kinetic damage but also a more significant doping effect. Also, MoS2 with large thickness shows less kinetic damage. This doping method makes use of existing infrastructures in the semiconductor industry and can be extended to other 2D materials and dopant species as well.

  15. Comprehensive two-dimensional gas chromatography in combination with rapid scanning quadrupole mass spectrometry in perfume analysis.

    Science.gov (United States)

    Mondello, Luigi; Casillia, Alessandro; Tranchida, Peter Quinto; Dugo, Giovanni; Dugo, Paola

    2005-03-04

    Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI).

  16. Ion exclusion chromatography for the purification of L-glutamine; Ion haijo chromatography ni yoru L-glutamine no seiseiho no kenkyu

    Energy Technology Data Exchange (ETDEWEB)

    Ito, H.; Nishi, A.; Naruse, M. [Ajinomoto Co. Inc., Kawasaki (Japan)

    1998-09-05

    Ion exclusion chromatography for the purification of L-glutamine is studied. L-glutamine is usually produced by fermentation and used in pharmaceuticals. By using a model solution of L-glutamine and L-glutamic acid, the optimum cation exchange resin is examined. As a result of the experiments, it is found that a cation exchange resin which has smaller crosslinkage and smaller diameter is better. Ammonium sulfate, L-glutamic acid and pyrrolidonecarboxylic acid, which are usually contained in fermentation broth as impurities, are effectively separated by this method. Moreover, the experimental data of the chromatography is expressed fairly well by the differential equations which express the mass transfer in the fixed bed. 8 refs., 5 figs., 2 tabs.

  17. Two-ion ICRF heating in Tokamaks

    International Nuclear Information System (INIS)

    Tennfors, E.

    1985-03-01

    The practical consequences for tokamak plasma heating in the ion cyclotron frequency regime of the two-dimensional treatment of the two-ion mode conversion layer are analyzed. The problem of evaluation of the condition for fast wave resonance is analyzed, as well as the limitations imposed by warm plasma effects. Simple ways to find the mode conversion surfaces when they exist are presented. Also for large tokamaks, it is possible to obtain mode conversion conditions for realistic antenna spectra provided species concentration and frequency are chosen such that the surface Epsilon = 0 intersects the plasma midplane just outside of the magnetic axis. (Author)

  18. Intercomparison of the measurements of oxalic acid in aerosols by gas chromatography and ion chromatography

    Science.gov (United States)

    Kawamura, Kimitaka; Barrie, Leonard A.; Toom-Sauntry, Desiree

    2010-12-01

    Oxalate, the anion of oxalic acid, is one of the most abundant measurable organic species in atmospheric aerosols. Traditionally, this bifunctional species has been measured by gas chromatography (GC) after derivatization to butyl ester and by ion chromatography (IC) without derivatization. However, there are few published comparisons of the two techniques. Here, we report the results of an intercomparison study for the measurement of oxalic acid in Arctic aerosols (oxalic acid by GC ranged from 6.5-59.1 ng m -3 (av. 26.0 ng m -3, median 26.2 ng m -3) whereas those by IC ranged from 6.6-52.1 ng m -3 (av. 26.6 ng m -3, median 25.4 ng m -3). They showed a good correlation ( r = 0.84) with a slope of 0.96. Thus, observations of oxalate obtained by GC employing dibutyl esters are almost equal to those by IC. Because the accuracy of oxalic acid by GC method largely depends on the method used, it is important to strictly examine the recovery in each study.

  19. Ion counting method and it's operational characteristics in gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Fujii, Toshihiro

    1976-01-01

    Ion counting method with continuous channel electron multiplier which affords the direct detection of very small ion currents and it's operational characteristics were studied in gas chromatography-mass spectrometry. Then this method was applied to the single ion detection technique of GC-MS. A detection limit was measured, using various standard samples of low level concentration. (auth.)

  20. Single-column ion chromatography with determination of hydrazoic acid produced in spent nuclear fuel reprocessing

    International Nuclear Information System (INIS)

    Ma Guilan; Tan Shuping

    2006-01-01

    The reaction of hydrazine and its derivative with ammonium metavanadate may produce hydrazoic acid (HN 3 ). A single-column ion chromatography is used for the determination of HN 3 after neutralizing the rest acid in the sample with sodium hydroxide. Chromatography separation of HN 3 is carried out on a 25 cm x 0.46 cm (inside diameter) stainless steel column packed with Vydac IC302 ion Chromatography packing. The eluent is 1 mmol/L o-phthalic acid, and the ion is detected by conductivity detector. The detection limit in the presence chromatography is 5 μg/mL, the linear range is from 5 to 201 μg/mL, the linear correlation coefficient is 0.9994, respectively. The analysis accuracy is 2% for standard sample, and the detection limit is 51 μg/mL for HN 3 in the real sample. (authors)

  1. A NEW METHOD OF PEAK DETECTION FOR ANALYSIS OF COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY MASS SPECTROMETRY DATA.

    Science.gov (United States)

    Kim, Seongho; Ouyang, Ming; Jeong, Jaesik; Shen, Changyu; Zhang, Xiang

    2014-06-01

    We develop a novel peak detection algorithm for the analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) data using normal-exponential-Bernoulli (NEB) and mixture probability models. The algorithm first performs baseline correction and denoising simultaneously using the NEB model, which also defines peak regions. Peaks are then picked using a mixture of probability distribution to deal with the co-eluting peaks. Peak merging is further carried out based on the mass spectral similarities among the peaks within the same peak group. The algorithm is evaluated using experimental data to study the effect of different cut-offs of the conditional Bayes factors and the effect of different mixture models including Poisson, truncated Gaussian, Gaussian, Gamma, and exponentially modified Gaussian (EMG) distributions, and the optimal version is introduced using a trial-and-error approach. We then compare the new algorithm with two existing algorithms in terms of compound identification. Data analysis shows that the developed algorithm can detect the peaks with lower false discovery rates than the existing algorithms, and a less complicated peak picking model is a promising alternative to the more complicated and widely used EMG mixture models.

  2. A NEW METHOD OF PEAK DETECTION FOR ANALYSIS OF COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY MASS SPECTROMETRY DATA*

    Science.gov (United States)

    Kim, Seongho; Ouyang, Ming; Jeong, Jaesik; Shen, Changyu; Zhang, Xiang

    2014-01-01

    We develop a novel peak detection algorithm for the analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) data using normal-exponential-Bernoulli (NEB) and mixture probability models. The algorithm first performs baseline correction and denoising simultaneously using the NEB model, which also defines peak regions. Peaks are then picked using a mixture of probability distribution to deal with the co-eluting peaks. Peak merging is further carried out based on the mass spectral similarities among the peaks within the same peak group. The algorithm is evaluated using experimental data to study the effect of different cut-offs of the conditional Bayes factors and the effect of different mixture models including Poisson, truncated Gaussian, Gaussian, Gamma, and exponentially modified Gaussian (EMG) distributions, and the optimal version is introduced using a trial-and-error approach. We then compare the new algorithm with two existing algorithms in terms of compound identification. Data analysis shows that the developed algorithm can detect the peaks with lower false discovery rates than the existing algorithms, and a less complicated peak picking model is a promising alternative to the more complicated and widely used EMG mixture models. PMID:25264474

  3. Two-dimensional mesoporous carbon nanosheets and their derived graphene nanosheets: synthesis and efficient lithium ion storage.

    Science.gov (United States)

    Fang, Yin; Lv, Yingying; Che, Renchao; Wu, Haoyu; Zhang, Xuehua; Gu, Dong; Zheng, Gengfeng; Zhao, Dongyuan

    2013-01-30

    We report a new solution deposition method to synthesize an unprecedented type of two-dimensional ordered mesoporous carbon nanosheets via a controlled low-concentration monomicelle close-packing assembly approach. These obtained carbon nanosheets possess only one layer of ordered mesopores on the surface of a substrate, typically the inner walls of anodic aluminum oxide pore channels, and can be further converted into mesoporous graphene nanosheets by carbonization. The atomically flat graphene layers with mesopores provide high surface area for lithium ion adsorption and intercalation, while the ordered mesopores perpendicular to the graphene layer enable efficient ion transport as well as volume expansion flexibility, thus representing a unique orthogonal architecture for excellent lithium ion storage capacity and cycling performance. Lithium ion battery anodes made of the mesoporous graphene nanosheets have exhibited an excellent reversible capacity of 1040 mAh/g at 100 mA/g, and they can retain at 833 mAh/g even after numerous cycles at varied current densities. Even at a large current density of 5 A/g, the reversible capacity is retained around 255 mAh/g, larger than for most other porous carbon-based anodes previously reported, suggesting a remarkably promising candidate for energy storage.

  4. Determination of clebopride in plasma by capillary gas chromatography-negative-ion chemical ionization mass spectrometry.

    Science.gov (United States)

    Robinson, P R; Jones, M D; Maddock, J

    1988-11-18

    A procedure for the analysis of clebopride in plasma using capillary gas chromatography-negative-ion chemical ionization mass spectrometry has been developed. Employing an ethoxy analogue as internal standard, the two compounds were extracted from basified plasma using dichloromethane. Subsequent reaction with heptafluorobutyryl imidazole produced volatile monoheptafluorobutyryl derivatives whose ammonia negative-ion mass spectra proved ideal for selected-ion monitoring. The recovery of clebopride from plasma at 0.536 nmol/l was found to be 85.5 +/- 0.9% (n = 3) whilst measurement down to 0.268 nmol/l was possible with a coefficient of variation of 7.9%. Plasma levels of the compound are reported in two volunteers following ingestion of 1 mg of clebopride as the malate salt.

  5. Tear proteomic analysis of patients with type 2 diabetes and dry eye syndrome by two-dimensional nano-liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Li, Bing; Sheng, Minjie; Xie, Liqi; Liu, Feng; Yan, Guoquan; Wang, Weifang; Lin, Anjuan; Zhao, Fei; Chen, Yihui

    2014-01-09

    Diabetes mellitus has been shown to be associated with and complicated by dry eye syndrome. We sought to examine and compare the tear film proteome of type 2 diabetic patients with or without dry eye syndrome and normal subjects using two-dimensional nano-liquid chromatography coupled with tandem mass spectrometry (MS)-based proteomics. Tears were collected from eight type 2 diabetes patients with dry eye syndrome, eight type 2 diabetes patients without dry eye syndrome, and eight normal subjects. Tear breakup time (BUT) was determined, and tear proteins were prepared and analyzed using two-dimensional strong cation-exchange/reversed-phase nano-scale liquid chromatography MS. All MS/MS spectra were identified by using SEQUEST against the human International Protein Index (IPI) database and the relative abundance of individual proteins was assessed by spectral counting. Tear BUT was significantly lower in patients with diabetes and dry eye syndrome than in patients with diabetes only and normal subjects. Analysis of spectral counts of tear proteins showed that, compared to healthy controls, patients with diabetes and dry eye syndrome had increased expression of apoptosis-related proteins, like annexin A1, and immunity- and inflammation-related proteins, including neutrophil elastase 2 and clusterin, and glycometabolism-related proteins, like apolipoprotein A-II. Dry eye syndrome in diabetic patients is associated with aberrant expression of tear proteins, and the findings could lead to identification of novel pathways for therapeutic targeting and new diagnostic markers.

  6. Plasma chromatography

    International Nuclear Information System (INIS)

    Anon.

    1984-01-01

    This book examines the fundamental theory and various applications of ion mobility spectroscopy. Plasma chromatography developed from research on the diffusion and mobility of ions. Topics considered include instrument design and description (e.g., performance, spectral interpretation, sample handling, mass spectrometry), the role of ion mobility in plasma chromatography (e.g., kinetic theory of ion transport), atmospheric pressure ionization (e.g., rate equations), the characterization of isomers by plasma chromatography (e.g., molecular ion characteristics, polynuclear aromatics), plasma chromatography as a gas chromatographic detection method (e.g., qualitative analysis, continuous mobility monitoring, quantitative analysis), the analysis of toxic vapors by plasma chromatography (e.g., plasma chromatograph calibration, instrument control and data processing), the analysis of semiconductor devices and microelectronic packages by plasma chromatography/mass spectroscopy (e.g., analysis of organic surface contaminants, analysis of water in sealed electronic packages), and instrument design and automation (hardware, software)

  7. Indirect ultraviolet detection of alkaline earth metal ions using an imidazolium ionic liquid as an ultraviolet absorption reagent in ion chromatography.

    Science.gov (United States)

    Liu, Yong-Qiang; Yu, Hong

    2017-04-01

    A convenient and versatile method was developed for the separation and detection of alkaline earth metal ions by ion chromatography with indirect UV detection. The chromatographic separation of Mg 2+ , Ca 2+ , and Sr 2+ was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid as the mobile phase, in which the imidazolium ionic liquid acted as an UV-absorption reagent. The effects of imidazolium ionic liquids, detection wavelength, acids in the mobile phase, and column temperature on the retention of Mg 2+ , Ca 2+ , and Sr 2+ were investigated. The main factors influencing the separation and detection were the background UV absorption reagent and the concentration of hydrogen ion in ion chromatography with indirect UV detection. The successful separation and detection of Mg 2+ , Ca 2+ , and Sr 2+ within 14 min were achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.06, 0.12, and 0.23 mg/L, respectively. A new separation and detection method of alkaline earth metal ions by ion chromatography with indirect UV detection was developed, and the application range of ionic liquids was expanded. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Two-dimensional chromatographic analysis using three second-dimension columns for continuous comprehensive analysis of intact proteins.

    Science.gov (United States)

    Zhu, Zaifang; Chen, Huang; Ren, Jiangtao; Lu, Juan J; Gu, Congying; Lynch, Kyle B; Wu, Si; Wang, Zhe; Cao, Chengxi; Liu, Shaorong

    2018-03-01

    We develop a new two-dimensional (2D) high performance liquid chromatography (HPLC) approach for intact protein analysis. Development of 2D HPLC has a bottleneck problem - limited second-dimension (second-D) separation speed. We solve this problem by incorporating multiple second-D columns to allow several second-D separations to be proceeded in parallel. To demonstrate the feasibility of using this approach for comprehensive protein analysis, we select ion-exchange chromatography as the first-dimension and reverse-phase chromatography as the second-D. We incorporate three second-D columns in an innovative way so that three reverse-phase separations can be performed simultaneously. We test this system for separating both standard proteins and E. coli lysates and achieve baseline resolutions for eleven standard proteins and obtain more than 500 peaks for E. coli lysates. This is an indication that the sample complexities are greatly reduced. We see less than 10 bands when each fraction of the second-D effluents are analyzed by sodium dodecyl sulfate - polyacrylamide gel electrophoresis (SDS-PAGE), compared to hundreds of SDS-PAGE bands as the original sample is analyzed. This approach could potentially be an excellent and general tool for protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Two-step purification of His-tagged Nef protein in native condition using heparin and immobilized metal ion affinity chromatographies.

    Science.gov (United States)

    Finzi, Andrés; Cloutier, Jonathan; Cohen, Eric A

    2003-07-01

    The Nef protein encoded by human immunodeficiency virus type 1 (HIV-1) has been shown to be an important factor of progression of viral growth and pathogenesis in both in vitro and in vivo. The lack of a simple procedure to purify Nef in its native conformation has limited molecular studies on Nef function. A two-step procedure that includes heparin and immobilized metal ion affinity chromatographies (IMACs) was developed to purify His-tagged Nef (His(6)-Nef) expressed in bacteria in native condition. During the elaboration of this purification procedure, we identified two closely SDS-PAGE-migrating contaminating bacterial proteins, SlyD and GCHI, that co-eluted with His(6)-Nef in IMAC in denaturing condition and developed purification steps to eliminate these contaminants in native condition. Overall, this study describes a protocol that allows rapid purification of His(6)-Nef protein expressed in bacteria in native condition and that removes metal affinity resin-binding bacterial proteins that can contaminate recombinant His-tagged protein preparation.

  10. Purification of 3H-dihydroalprenolol by two dimensional thin layer chromatography

    International Nuclear Information System (INIS)

    Smisterova, J.; Soltes, L.; Kallay, Z.

    1989-01-01

    A two dimensional thin-layer chromatographic method was developed for the purification and analysis of (-)-[ 3 H]dihydroalprenolol by using an acidic mobile phase (butanol/water/acetic acid 25:10:4, v/v) in one direction and a basic eluent (chloroform/acetone/triethylamine 50:40:10, v/v) in another direction. (author)

  11. A rapid method for the separation and estimation of uranium in geological materials using ion chromatography

    International Nuclear Information System (INIS)

    Prakash, Satya; Bangroo, P.N.

    2013-01-01

    Ion Chromatography is an elegant analytical technique which was primarily developed for the analysis of anionic species and over the years it has been used successfully to analyse various elements in different matrices. In this work the potential of Ion Chromatography has been used for the rapid separation and estimation of uranium in hydrogeochemical and other geological materials

  12. Interaction of Ions with Two-Dimensional Transition Metal Carbide (MXene) Films

    Science.gov (United States)

    Ren, Chang

    Nowadays, society is relying more on nanotechnology for solving critical issues, such as the increasing demand for clean energy and freshwater. Among nanotechnologies, two-dimensional (2D) materials with unique properties are investigated with elevated expectations. In 2011, a new family of 2D materials MXenes were discovered, which became an important addition to the 2D word. The general formula of MXene is Mn+1XnTx, where M stands for transition metal atom, X is C and/or N, n = 1, 2 or 3, and Tx represents surface groups. Nanosheets of MXene obtained by delamination can form flexible films. Additionally, ions can intercalate MXene layers, suggesting potential applications in energy storage and water purification. The Ti3C2Tx MXene films of various thicknesses, which have orderly stacked 2D structure, high density and flexibility, and metallic electrical conductivity of 2400 to 5690 S/cm were fabricated by vacuum-assisted filtration. Ti3C2Tx surface was negatively charged and hydrophilic. Additionally, Ti3C 2Tx films showed sufficient mechanical strength for handling, and the tensile strength of a Ti3C2Tx film was comparable to GO membranes. Metal cations intercalated between the MXene layers, and led to intercalation capacitance. Binder-free Ti3C 2Tx films showed volumetric capacitance of 350 to over 1000 F/cm3 in aqueous electrochemical capacitors (ECs), depending on the electrolyte, and the size of Ti3C2Tx nanosheets. Smaller flakes were obtained by increasing time of ultrasonic treatment. They had a lower electrical conductivity, but a higher capacitance. By introducing polymer nanofillers, such as poly(vinyl alcohol) (PVA) between MXene nanosheets, composite films were prepared and showed controllable electrical conductivity, increased interlayer spacing, improved mechanical strength and capacitive performance. By introducing carbon nanomaterials between MXene layers or creating mesopores on MXene, the films were made more accessible to intercalation and

  13. Fast comprehensive two-dimensional gas chromatography method for fatty acid methyl ester separation and quantification using dual ionic liquid columns.

    Science.gov (United States)

    Nosheen, Asia; Mitrevski, Blagoj; Bano, Asghari; Marriott, Philip J

    2013-10-18

    Safflower oil is a complex mixture of C18 saturated and unsaturated fatty acids amongst other fatty acids, and achieving separation between these similar structure components using one dimensional gas chromatography (GC) may be difficult. This investigation aims to obtain improved separation of fatty acid methyl esters in safflower oil, and their quantification using comprehensive two-dimensional GC (GC×GC). Here, GC×GC separation is accomplished by the coupling of two ionic liquid (IL) column phases: the combination of SLB-IL111 with IL59 column phases was finally selected since it provided excellent separation of a FAME standard mixture, as well as fatty acids in safflower and linseed oil, compared to other tested column sets. Safflower oil FAME were well separated in a short run of 16min. FAME validation was demonstrated by method reproducibility, linearity over a range up to 500mgL(-1), and limits of detection which ranged from 1.9mgL(-1) to 5.2mgL(-1) at a split ratio of 20:1. Quantification was carried out using two dilution levels of 200-fold for major components and 20-fold for trace components. The fatty acids C15:0 and C17:0 were not reported previously in safflower oil. The SLB-IL111/IL59 column set proved to be an effective and novel configuration for separation and quantification of vegetable and animal oil fatty acids. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Determination of dibutylphosphate and monobutylphosphate in TBP by ion chromatography

    International Nuclear Information System (INIS)

    Siva Kumar, B.; Vijayalakshmi, S.; Sankaran, K.; Ganesan, V.

    2012-01-01

    Tri-n-butyl phosphate (TBP) is used as solvent in the PUREX (Plutonium Uranium Refining by Extraction) process of nuclear fuel reprocessing. TBP undergoes chemical and radiological degradation to give DBP and MBP which in turn extracts the heavy metal such as U, Pu thereby affecting the performance of the extraction process. Analytical method using ion chromatography (IC) was developed for the determination of dibutyl phosphate (DBP) and monobutyl phosphate (MBP) in TBP. In this method, DBP and MBP were extracted from tri-n-butyl phosphate using carbonate-bicarbonate mixture of eluent composition and the aqueous phase was analyzed using suppressed ion chromatography employing carbonate as eluent. Standardization of extraction was carried out by standard addition studies. The detection limits for both DBP and MBP are found to be in sub ppm level. This method was applied to the analysis of TBP supplied by different suppliers

  15. Analysis of oxidised heavy paraffininc products by high temperature comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Potgieter, H; Bekker, R; Beigley, J; Rohwer, E

    2017-08-04

    Heavy petroleum fractions are produced during crude and synthetic crude oil refining processes and they need to be upgraded to useable products to increase their market value. Usually these fractions are upgraded to fuel products by hydrocracking, hydroisomerization and hydrogenation processes. These fractions are also upgraded to other high value commercial products like lubricant oils and waxes by distillation, hydrogenation, and oxidation and/or blending. Oxidation of hydrogenated heavy paraffinic fractions produces high value products that contain a variety of oxygenates and the characterization of these heavy oxygenates is very important for the control of oxidation processes. Traditionally titrimetric procedures are used to monitor oxygenate formation, however, these titrimetric procedures are tedious and lack selectivity toward specific oxygenate classes in complex matrices. Comprehensive two-dimensional gas chromatography (GC×GC) is a way of increasing peak capacity for the comprehensive analysis of complex samples. Other groups have used HT-GC×GC to extend the carbon number range attainable by GC×GC and have optimised HT-GC×GC parameters for the separation of aromatics, nitrogen-containing compounds as well as sulphur-containing compounds in heavy petroleum fractions. HT-GC×GC column combinations for the separation of oxygenates in oxidised heavy paraffinic fractions are optimised in this study. The advantages of the HT-GC×GC method in the monitoring of the oxidation reactions of heavy paraffinic fraction samples are illustrated. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Intercomparison of ion beam analysis software for the simulation of backscattering spectra from two-dimensional structures

    Energy Technology Data Exchange (ETDEWEB)

    Mayer, M., E-mail: matej.mayer@ipp.mpg.de [Max-Planck-Institut für Plasmaphysik, Boltzmannstr. 2, 85748 Garching (Germany); Malinský, P. [Nuclear Physics Institute of the Czech Academy of Sciences v.v.i., 250 68 Rez (Czech Republic); Department of Physics, Faculty of Science, J.E. Purkinje University, Ceske mladeze 8, 400 96 Usti nad Labem (Czech Republic); Schiettekatte, F. [Regroupement Québécois sur les Matériaux de Pointe (RQMP), Département de Physique, Université de Montréal, Montréal, QC (Canada); Zolnai, Z. [Centre for Energy Research, Institute of Technical Physics and Materials Science (MFA), Konkoly-Thege M. út 29-33, H-1121 Budapest (Hungary)

    2016-10-15

    The codes RBS-MAST, STRUCTNRA, F95-Rough and CORTEO are simulation codes for ion beam analysis spectra from two- or three-dimensional sample structures. The codes were intercompared in a code-code comparison using an idealized grating structure and by comparison to experimental data from a silicon grating on tantalum interlayer. All codes are in excellent agreement at higher incident energies and not too large energy losses. At lower incident energies, grazing angles of incidence and/or larger energy losses plural scattering effects play an increasing role. Simulation codes with plural scattering capabilities offer higher accuracy and better agreement to experimental results in this regime.

  17. Determination of water-soluble forms of oxalic and formic acids in soils by ion chromatography

    Science.gov (United States)

    Karicheva, E.; Guseva, N.; Kambalina, M.

    2016-03-01

    Carboxylic acids (CA) play an important role in the chemical composition origin of soils and migration of elements. The content of these acids and their salts is one of the important characteristics for agrochemical, ecological, ameliorative and hygienic assessment of soils. The aim of the article is to determine water-soluble forms of same carboxylic acids — (oxalic and formic acids) in soils by ion chromatography with gradient elution. For the separation and determination of water-soluble carboxylic acids we used reagent-free gradient elution ion-exchange chromatography ICS-2000 (Dionex, USA), the model solutions of oxalate and formate ions, and leachates from soils of the Kola Peninsula. The optimal gradient program was established for separation and detection of oxalate and formate ions in water solutions by ion chromatography. A stability indicating method was developed for the simultaneous determination of water-soluble organic acids in soils. The method has shown high detection limits such as 0.03 mg/L for oxalate ion and 0.02 mg/L for formate ion. High signal reproducibility was achieved in wide range of intensities which correspond to the following ion concentrations: from 0.04 mg/g to 10 mg/L (formate), from 0.1 mg/g to 25 mg/L (oxalate). The concentration of formate and oxalate ions in soil samples is from 0.04 to 0.9 mg/L and 0.45 to 17 mg/L respectively.

  18. Determination of inorganic ions in natural water by ion chromatography

    International Nuclear Information System (INIS)

    Nazaratul Ashifa Abdullah Salim; Mohd Suhaimi Hamzah; Eewiat Edin Put; Abdul Khalik Wood; Shamsiah Abdul Rahman; Md Suhaimi Elia

    2010-01-01

    Ion chromatography (IC) is a well established methodology for analysis of ionic species. The concentration of ionic species was determined using suppressed IC with conductivity detection. Anion species were determined in a single 15-min run with Na 2 CO 3 and NaHCO 3 eluent. Cation species were analysed by direct injection of 1 ml and isocratic elution with a methanesulfonic acid (MSA) eluent. Natural water were collected from various sources such as rainwater, lake, river and groundwater. Analysis performance of IC system was validated by evaluating the linear regression of calibration curve, recovery of spike sample and quality control sample. (author)

  19. A novel four-dimensional analytical approach for analysis of complex samples.

    Science.gov (United States)

    Stephan, Susanne; Jakob, Cornelia; Hippler, Jörg; Schmitz, Oliver J

    2016-05-01

    A two-dimensional LC (2D-LC) method, based on the work of Erni and Frei in 1978, was developed and coupled to an ion mobility-high-resolution mass spectrometer (IM-MS), which enabled the separation of complex samples in four dimensions (2D-LC, ion mobility spectrometry (IMS), and mass spectrometry (MS)). This approach works as a continuous multiheart-cutting LC system, using a long modulation time of 4 min, which allows the complete transfer of most of the first - dimension peaks to the second - dimension column without fractionation, in comparison to comprehensive two-dimensional liquid chromatography. Hence, each compound delivers only one peak in the second dimension, which simplifies the data handling even when ion mobility spectrometry as a third and mass spectrometry as a fourth dimension are introduced. The analysis of a plant extract from Ginkgo biloba shows the separation power of this four-dimensional separation method with a calculated total peak capacity of more than 8700. Furthermore, the advantage of ion mobility for characterizing unknown compounds by their collision cross section (CCS) and accurate mass in a non-target approach is shown for different matrices like plant extracts and coffee. Graphical abstract Principle of the four-dimensional separation.

  20. Two dimensional hybrid simulation of a curved bow shock

    International Nuclear Information System (INIS)

    Thomas, V.A.; Winske, D.

    1990-01-01

    Results are presented from two dimensional hybrid simulations of curved collisionless supercritical shocks, retaining both quasi-perpendicular and quasi-parallel sections of the shock in order to study the character and origin of the foreshock ion population. The simulations demonstrate that the foreshock ion population is dominated by ions impinging upon the quasi-parallel side of the shock, while nonlocal transport from the quasi-perpendicular side of the shock into the foreshock region is minimal. Further, it is shown that the ions gain energy by drifting significantly in the direction of the convection electric field through multiple shock encounters

  1. Comparison of different transition metal ions for immobilized metal affinity chromatography of selenoprotein P from human plasma

    DEFF Research Database (Denmark)

    Sidenius, U; Farver, O; Jøns, O

    1999-01-01

    Cu2+, Ni2+, Zn2+, Co2+ and Cd2+ were evaluated in metal ion affinity chromatography for enrichment of selenoprotein P, and immobilized Co2+ affinity chromatography was found to be the most selective chromatographic method. The chromatography was performed by fast protein liquid chromatography...

  2. Development of an Advanced Two-Dimensional Thermal Model for Large size Lithium-ion Pouch Cells

    International Nuclear Information System (INIS)

    Samba, Ahmadou; Omar, Noshin; Gualous, Hamid; Firouz, Youssef; Van den Bossche, Peter; Van Mierlo, Joeri; Boubekeur, Tala Ighil

    2014-01-01

    In this work, a LiFePO4/graphite lithium-ion pouch cell with a rated capacity of 45Ah has been used and a two dimensional thermal model is developed to predict the cell temperature distribution over the surface of the battery, this model requires less input parameters and still has high accuracy. The used input parameters are the heat generation and thermal properties. The ANSYS FLUENT software has been used to solve the models. In addition, a new estimation tool has been developed for estimation of the thermal model parameters. Furthermore, the thermal behavior of the proposed battery has been investigated at different environmental conditions as well as during the abuse conditions. Thermal runaway is investigated in depth by the model

  3. Non-polar lipids characterization of Quinoa (Chenopodium quinoa) seed by comprehensive two-dimensional gas chromatography with flame ionization/mass spectrometry detection and non-aqueous reversed-phase liquid chromatography with atmospheric pressure chemical ionization mass spectrometry detection.

    Science.gov (United States)

    Fanali, Chiara; Beccaria, Marco; Salivo, Simona; Tranchida, Peter; Tripodo, Giusy; Farnetti, Sara; Dugo, Laura; Dugo, Paola; Mondello, Luigi

    2015-07-08

    A chemical characterization of major lipid components, namely, triacylglycerols, fatty acids and the unsaponifiable fraction, in a Quinoa seed lipids sample is reported. To tackle such a task, non-aqueous reversed-phase high-performance liquid chromatography with mass spectrometry detection was employed. The latter was interfaced with atmospheric pressure chemical ionization for the analysis of triacylglycerols. The main triacylglycerols (>10%) were represented by OLP, OOL and OLL (P = palmitoyl, O = oleoyl, L = linoleoyl); the latter was present in the oil sample at the highest percentage (18.1%). Furthermore, fatty acid methyl esters were evaluated by gas chromatography with flame ionization detection. 89% of the total fatty acids was represented by unsaturated fatty acid methyl esters with the greatest percentage represented by linoleic and oleic acids accounting for approximately 48 and 28%, respectively. An extensive characterization of the unsaponifiable fraction of Quinoa seed lipids was performed for the first time, by using comprehensive two-dimensional gas chromatography with dual mass spectrometry/flame ionization detection. Overall, 66 compounds of the unsaponifiable fraction were tentatively identified, many constituents of which (particularly sterols) were confirmed by using gas chromatography with high-resolution time-of-flight mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Quantitative analysis of fragrance in selectable one dimensional or two dimensional gas chromatography-mass spectrometry with simultaneous detection of multiple detectors in single injection.

    Science.gov (United States)

    Tan, Hui Peng; Wan, Tow Shi; Min, Christina Liew Shu; Osborne, Murray; Ng, Khim Hui

    2014-03-14

    A selectable one-dimensional ((1)D) or two-dimensional ((2)D) gas chromatography-mass spectrometry (GC-MS) system coupled with flame ionization detector (FID) and olfactory detection port (ODP) was employed in this study to analyze perfume oil and fragrance in shower gel. A split/splitless (SSL) injector and a programmable temperature vaporization (PTV) injector are connected via a 2-way splitter of capillary flow technology (CFT) in this selectable (1)D/(2)D GC-MS/FID/ODP system to facilitate liquid sample injections and thermal desorption (TD) for stir bar sorptive extraction (SBSE) technique, respectively. The dual-linked injectors set-up enable the use of two different injector ports (one at a time) in single sequence run without having to relocate the (1)D capillary column from one inlet to another. Target analytes were separated in (1)D GC-MS/FID/ODP and followed by further separation of co-elution mixture from (1)D in (2)D GC-MS/FID/ODP in single injection without any instrumental reconfiguration. A (1)D/(2)D quantitative analysis method was developed and validated for its repeatability - tR; calculated linear retention indices (LRI); response ratio in both MS and FID signal, limit of detection (LOD), limit of quantitation (LOQ), as well as linearity over a concentration range. The method was successfully applied in quantitative analysis of perfume solution at different concentration level (RSD≤0.01%, n=5) and shower gel spiked with perfume at different dosages (RSD≤0.04%, n=5) with good recovery (96-103% for SSL injection; 94-107% for stir bar sorptive extraction-thermal desorption (SBSE-TD). Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Calcium isotope fractionation in ion-exchange chromatography

    International Nuclear Information System (INIS)

    Russell, W.A.; Papanastassiou, D.A.

    1978-01-01

    Significant fractionation of the isotopes of calcium has been observed during elution through short ion-exchange columns packed with Dowex 50W-X8 resin. A double isotopic tracer was used to provide correction for instrumental fractionation effects. The absolute 40 Ca/ 44 Ca ratio is determined by this method to 0.05% and provides a measure of the fractionation of all Ca isotopes. It is found that the lighter isotopes are preferentially retained by the resin, with variations in 40 Ca/ 44 Ca between the first and last fractions of up to 1.1%. An estimate of the separation factor between batch solute and resin gives epsilon = 2.1 x 10 -4 . Details of the chemical or physical mechanisms causing isotope fractionation of Li, Na, Ca, and other elements during ion-exchange chromatography are not yet clear

  6. Contribution to high-temperature chromatography and high-temperature-gas-chromatography-mass spectrometry of lipids

    International Nuclear Information System (INIS)

    Aichholz, R.

    1998-04-01

    This thesis describes the use of high temperature gas chromatography for the investigation of unusual triacylglycerols, cyanolipids and bees waxes. The used glass capillary columns were pretreated and coated with tailor made synthesized high temperature stable polysiloxane phases. The selective separation properties of the individual columns were tested with a synthetic lipid mixture. Suitable derivatization procedures for the gaschromatographic analyses of neutral lipids, containing multiple bonds as well as hydroxy-, epoxy-, and carboxyl groups, were developed and optimized. Therefore conjugated olefinic-, conjugated olefinic-acetylenic-, hydroxy-, epoxy-, and conjugated olefinic keto triacylglycerols in miscellaneous plant seed oils as well as hydroxy monoesters, diesters and hydroxy diesters in bees waxes could be analysed directly with high temperature gas chromatography for the first time. In order to elucidate the structures of separated lipid compounds, high temperature gas chromatography was coupled to mass spectrometry and tandem mass spectrometry, respectively. Comparable analytical systems are hitherto not commercial available. Therefore instrumental prerequisites for a comprehensive and detailed analysis of seed oils and bees waxes were established. In GC/MS commonly two ionization methods are used, electron impact ionization and chemical ionization. For the analysis of lipids the first is of limited use only. Due to intensive fragmentation only weak molecular ions are observed. In contrast, the chemical ionization yields in better results. Dominant quasi molecular ions enable an unambiguous determination of the molecular weight. Moreover, characteristic fragment ions provide important indications of certain structural features of the examined compounds. Nevertheless, in some cases the chromatographic resolution was insufficient in order to separate all compounds present in natural lipid mixtures. Owing to the selected detection with mass spectrometry

  7. Two-dimensional thermal simulations of aluminum and carbon ion strippers for experiments at SPIRAL2 using the highest beam intensities

    International Nuclear Information System (INIS)

    Tahir, N.A.; Kim, V.; Lamour, E.; Lomonosov, I.V.; Piriz, A.R.; Rozet, J.P.; Stöhlker, Th.; Sultanov, V.; Vernhet, D.

    2012-01-01

    In this paper we report on two-dimensional numerical simulations of heating of a rotating, wheel shaped target impacted by the full intensity of the ion beam that will be delivered by the SPIRAL2 facility at Caen, France. The purpose of this work is to study heating of solid targets that will be used to strip the fast ions of SPIRAL2 to the required high charge state for the FISIC (Fast Ion–Slow Ion Collision) experiments. Strippers of aluminum with different emissivities and of carbon are exposed to high beam current of different ion species as oxygen, neon and argon. These studies show that carbon, due to its much higher sublimation temperature and much higher emissivity, is more favorable compared to aluminum. For the highest beam intensities, an aluminum stripper does not survive. However, problem of the induced thermal stresses and long term material fatigue needs to be investigated before a final conclusion can be drawn.

  8. Rapid and Convenient Separation of Chitooligosaccharides by Ion-Exchange Chromatography

    Science.gov (United States)

    Wu, Yuxiao; Lu, Wei-Peng; Wang, Jianing; Gao, Yunhua; Guo, Yanchuan

    2017-12-01

    Pervious methods for separation of highly purified chitooligosaccharides was time-consuming and labor-intensive, which limited the large-scale production. This study developed a convenient ion-exchange chromatography using the ÄKTA™ avant 150 chromatographic system. Five fractions were automatically collected under detecting the absorption at 210 nm. The fractions were analyzed by high-performance liquid chromatography. It proved that they primarily comprised chitobiose, chitotriose, chitotetraose, chitopentaose, and chitohexaose, respectively, with chromatographic purities over 90%. The separation process was rapid, convenient and could be monitored on-line, which would be benefit for the mass production of chitooligosaccharides.

  9. Comprehensive two-dimensional gas chromatography for fast characterization of oil contamination

    International Nuclear Information System (INIS)

    Van De Weghe, H.; Vanermen, G.; Gemoets, J.; Lookman, R.; Bertels, D.

    2005-01-01

    Most analytical methods for the characterization of oil contamination rely on gas chromatography. Capillary GC offers a high separation power (peak capacity typically 100 - 500), and by using a boiling point column a volatility based distribution is obtained. However, petrochemical mixtures like mineral oil easily contain more then 5000 compounds, and capillary GC does not succeed in separating such mixtures up to the level of individual components. Analytical results are therefore limited to a classification into boiling point (or equivalent-carbon) fractions. Recent methods refined the classification by fractionation in aromatic and aliphatic hydrocarbons prior to GC-analysis (TPH method, Weisman 1998), and by incorporating water solubility (TTE and OK method, for a detailed description we refer to the Consoil 2005 lecture by R. Lookman 'Oil characterization: assessment of composition, degradation and remediation potential of total petroleum hydrocarbons in soil'). However, besides analytical difficulties and time consuming protocols related with these methods, the resulting classification still remains coarse and the various groups are not univocally chemically identified. Recently, comprehensive two-dimensional GC (GCXGC) was introduced. This technique combines two GC-columns with different separation mechanisms. The two columns are connected by a modulator, a device that traps, focuses and re-injects the peaks that elute from the first column into the second column. Each peak from the first column (representing a number of overlapping peaks) is further separated on the second column. The very high separation power of GCXGC (peak capacity 2000 - 10000) is ideal for the analysis of complex mixtures like mineral oil. Another important feature is the generation of structured chromatograms. Isomers appear as distinct groups in the chromatogram as a result of their similar interaction with the 2D-column phase. For chemical identification comprehensive GC can be

  10. Comprehensive two-dimensional gas chromatography for fast characterization of oil contamination

    Energy Technology Data Exchange (ETDEWEB)

    Van De Weghe, H.; Vanermen, G.; Gemoets, J.; Lookman, R.; Bertels, D. [VITO, Mol (Belgium)

    2005-07-01

    Most analytical methods for the characterization of oil contamination rely on gas chromatography. Capillary GC offers a high separation power (peak capacity typically 100 - 500), and by using a boiling point column a volatility based distribution is obtained. However, petrochemical mixtures like mineral oil easily contain more then 5000 compounds, and capillary GC does not succeed in separating such mixtures up to the level of individual components. Analytical results are therefore limited to a classification into boiling point (or equivalent-carbon) fractions. Recent methods refined the classification by fractionation in aromatic and aliphatic hydrocarbons prior to GC-analysis (TPH method, Weisman 1998), and by incorporating water solubility (TTE and OK method, for a detailed description we refer to the Consoil 2005 lecture by R. Lookman 'Oil characterization: assessment of composition, degradation and remediation potential of total petroleum hydrocarbons in soil'). However, besides analytical difficulties and time consuming protocols related with these methods, the resulting classification still remains coarse and the various groups are not univocally chemically identified. Recently, comprehensive two-dimensional GC (GCXGC) was introduced. This technique combines two GC-columns with different separation mechanisms. The two columns are connected by a modulator, a device that traps, focuses and re-injects the peaks that elute from the first column into the second column. Each peak from the first column (representing a number of overlapping peaks) is further separated on the second column. The very high separation power of GCXGC (peak capacity 2000 - 10000) is ideal for the analysis of complex mixtures like mineral oil. Another important feature is the generation of structured chromatograms. Isomers appear as distinct groups in the chromatogram as a result of their similar interaction with the 2D-column phase. For chemical identification comprehensive GC

  11. Solitary wave solutions of two-dimensional nonlinear Kadomtsev ...

    Indian Academy of Sciences (India)

    Aly R Seadawy

    2017-09-13

    Sep 13, 2017 ... We considered the two-dimensional DASWs in colli- sionless, unmagnetized cold plasma consisting of dust fluid, ions and electrons. The dynamics of DASWs is governed by the normalized fluid equations of nonlin- ear continuity (1), nonlinear motion of system (2) and. (3) and linear Poisson equation (4) as.

  12. Two dimensional code for modeling of high ione cyclotron harmonic fast wave heating and current drive

    International Nuclear Information System (INIS)

    Grekov, D.; Kasilov, S.; Kernbichler, W.

    2016-01-01

    A two dimensional numerical code for computation of the electromagnetic field of a fast magnetosonic wave in a tokamak at high harmonics of the ion cyclotron frequency has been developed. The code computes the finite difference solution of Maxwell equations for separate toroidal harmonics making use of the toroidal symmetry of tokamak plasmas. The proper boundary conditions are prescribed at the realistic tokamak vessel. The currents in the RF antenna are specified externally and then used in Ampere law. The main poloidal tokamak magnetic field and the ''kinetic'' part of the dielectric permeability tensor are treated iteratively. The code has been verified against known analytical solutions and first calculations of current drive in the spherical torus are presented.

  13. Determination of anionic concentrations in ground water samples using ion chromatography

    International Nuclear Information System (INIS)

    Prathibha, P.; Saradhi, I.V.; Pandit, G.G.; Puranik, V.D.

    2011-01-01

    Ion chromatography is a powerful separation technique for the quantitative measurement of anions in aqueous samples as well as in soil, sediment and air particulate samples leached in aqueous solutions. Ion chromatographic technique is developed by making use of suppressed ion conductivity detection (Small et.al.,1975) and it is a rapid multi ion analysis technique. The time, processing and effort required for the analysis of anions is much less compared to other techniques available such as ion selective electrode technique. In the present paper ground water samples collected around New BARC campus, Visakhapatnam are analyzed for anions using Ion chromatograph. The data generated will establish the current baseline status of the ionic contaminants in the study area. Groundwater samples are collected at 13 locations around BARC Vizag campus covering 30 km radius in September, 2009, April and July, 2010. The water samples include samples from hand pump and open wells in villages. The water samples are analyzed for fluoride, chloride, nitrate and sulphate using Metrohm make Ion chromatograph. The fluoride concentration in samples varied from 0.22 to 1.26 ppm, chloride from 18.7 to 810.9, nitrate from 1.34 to 378.5 ppm and sulphate from 13.29 to 250.69 ppm. No significant seasonal variations are observed in the samples collected from various locations except chloride at two locations. Ions Chromatograph is found to be a useful tool for simultaneous analysis of environmental samples with good accuracy where the concentrations of anions vary within an order of magnitude among them themselves. (author)

  14. Direct analysis of volatile fatty acids in marine sediment porewater by two-dimensional ion chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Glombitza, Clemens; Pedersen, Jeanette; Røy, Hans

    2014-01-01

    Volatile fatty acids (VFAs) are key intermediates in the microbial food web. However, the analysis of low concentrations of VFAs in marine porewater is hampered by interference from high concentrations of inorganic ions. Published methods often use sample pretreatment, including distillation or d...

  15. Microfabricated thermal modulator for comprehensive two-dimensional micro gas chromatography: design, thermal modeling, and preliminary testing.

    Science.gov (United States)

    Kim, Sung-Jin; Reidy, Shaelah M; Block, Bruce P; Wise, Kensall D; Zellers, Edward T; Kurabayashi, Katsuo

    2010-07-07

    In comprehensive two-dimensional gas chromatography (GC x GC), a modulator is placed at the juncture between two separation columns to focus and re-inject eluting mixture components, thereby enhancing the resolution and the selectivity of analytes. As part of an effort to develop a microGC x microGC prototype, in this report we present the design, fabrication, thermal operation, and initial testing of a two-stage microscale thermal modulator (microTM). The microTM contains two sequential serpentine Pyrex-on-Si microchannels (stages) that cryogenically trap analytes eluting from the first-dimension column and thermally inject them into the second-dimension column in a rapid, programmable manner. For each modulation cycle (typically 5 s for cooling with refrigeration work of 200 J and 100 ms for heating at 10 W), the microTM is kept approximately at -50 degrees C by a solid-state thermoelectric cooling unit placed within a few tens of micrometres of the device, and heated to 250 degrees C at 2800 degrees C s(-1) by integrated resistive microheaters and then cooled back to -50 degrees C at 250 degrees C s(-1). Thermal crosstalk between the two stages is less than 9%. A lumped heat transfer model is used to analyze the device design with respect to the rates of heating and cooling, power dissipation, and inter-stage thermal crosstalk as a function of Pyrex-membrane thickness, air-gap depth, and stage separation distance. Experimental results are in agreement with trends predicted by the model. Preliminary tests using a conventional capillary column interfaced to the microTM demonstrate the capability for enhanced sensitivity and resolution as well as the modulation of a mixture of alkanes.

  16. Three-dimensional structure of porcine pancreatic carboxypeptidase B with an acetate ion and two zinc atoms in the active site

    Energy Technology Data Exchange (ETDEWEB)

    Akparov, V. Kh., E-mail: valery@akparov.ru [State Research Institute for Genetics and Selection of Industrial Microorganisms (Russian Federation); Timofeev, V. I., E-mail: tostars@mail.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography of Federal Scientific Research Centre “Crystallography and Photonics” (Russian Federation); Maghsoudi, N. N., E-mail: maghsudi@yahoo.com [Shahid Beheshti University of Medical Sciences, Neuroscience Research Center (Iran, Islamic Republic of); Kuranova, I. P. [Russian Academy of Sciences, Shubnikov Institute of Crystallography of Federal Scientific Research Centre “Crystallography and Photonics” (Russian Federation)

    2017-03-15

    Crystals of porcine pancreatic carboxypeptidase B (CPB) were grown by the capillary counter-diffusion method in the presence of polyethylene glycol and zinc acetate. The three-dimensional structure of CPB was determined at 1.40 Å resolution using the X-ray diffraction data set collected from the crystals of the enzyme at the SPring 8 synchrotron facility and was refined to R{sub fact} = 17.19%, R{sub free} = 19.78%. The structure contains five zinc atoms, two of which are present in the active site of the enzyme, and an acetate ion. The arrangement of an additional zinc atom in the active site and the acetate ion is different from that reported by Yoshimoto et al.

  17. Determination of trimethylselenonium ion in urine by ion chromatography and inductively coupled plasma mass spectrometry detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jessen, K.D.; Kristensen, F.H.

    2000-01-01

    The selenium species selenite, selenate, selenomethionine (SeMet), and trimethylselenonium iodide (TMSe+) were separated in aqueous solution by ion chromatography. The separation was performed on an Ionpac CS5 cation exchange column by elution with 10 mM oxalic acid and 20 mM potassium sulphate, p...

  18. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    International Nuclear Information System (INIS)

    Mroczek, Tomasz; Ndjoko-Ioset, Karine; Glowniak, Kazimierz; Mietkiewicz-Capala, Agnieszka; Hostettmann, Kurt

    2006-01-01

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C 18 column using a gradient elution. Based on MS n spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide

  19. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mroczek, Tomasz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland)]. E-mail: tmroczek@pharmacognosy.org; Ndjoko-Ioset, Karine [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland); Glowniak, Kazimierz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Mietkiewicz-Capala, Agnieszka [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Hostettmann, Kurt [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland)

    2006-05-04

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C{sub 18} column using a gradient elution. Based on MS {sup n} spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide.

  20. [Simultaneous determination of vitamins A, D3 and E in infant formula and adult nutritions by online two-dimensional liquid chromatography].

    Science.gov (United States)

    Zhang, Yanhai; Qibule, Hasi; Jin, Yan; Wang, Jia; Ma, Wenli

    2015-03-01

    A rapid method for the simultaneous determination of vitamins A, D3 and E in infant formula and adult nutritions has been developed using online two-dimensional liquid chromatography (2D-LC). First of all, C8 and polar embedded C18 columns were chosen as the first and second dimensional column respectively according to hydrophobic-subtraction model, which constituted excellent orthogonal separation system. The detection wavelengths were set at 263 nm for vitamin D3, 296 nm for vitamin E and 325 nm for vitamin A. The purification of vitamin D3 and quantifications of vitamins A and E were completed simultaneously in the first dimensional separation using the left pump of Dual Gradient LC (DGLC) with methanol, acetonitrile and water as mobile phases. The heart-cutting time window of vitamin D3 was confirmed according to the retention time of vitamin D3 in the first dimensional separation. The elute from the first dimensional column (1-D column) which contained vitamin D3 was collected by a 500 µL sample loop and then taken into the second dimensional column (2-D column) by the right pump of DGLC with methanol, acetonitrile and water as mobile phases. The quantification of vitamin D3 was performed in the second dimensional separation with vitamin D2 as internal standard. At last, this method was applied for the analysis of the three vitamins in milk powder, cheese and yogurt. The injected sample solution with no further purification was pre-treated by hot-saponification using 1. 25 kg/L KOH solution and extracted by petroleum ether solvent. The recoveries of vitamin D3 spiked in all samples were 75.50%-85.00%. There was no statistically significant difference for the results between this method and standard method through t-test. The results indicate that vitamins A, D3 and E in infant formula and adult fortified dairy can be determined rapidly and accurately with this method.

  1. The isotope separation by ion exchange chromatography. Application to the lithium isotopes separation; La separation isotopique par chromatographie ionique

    Energy Technology Data Exchange (ETDEWEB)

    Albert, M G; Barre, Y; Neige, R

    1994-12-31

    In this work is described the used study step to demonstrate the industrial feasibility of a lithium isotopes separation process by ion exchange chromatography. After having recalled how is carried out the exchange reaction between the lithium isotopes bound on the cations exchanger resin and those which are in solution and gave the ion exchange chromatography principle, the authors establish a model which takes into account the cascade theory already used for enriched uranium production. The size parameters of this model are: the isotopic separation factor (which depends for lithium of the ligands nature and of the coordination factor), the isotopic exchange kinetics and the mass flow (which depends of the temperature, the lithium concentration, the resins diameter and the front advance). The way they have to be optimized and the implementation of the industrial process are given. (O.M.). 5 refs.

  2. Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Maria Elisabete; Cappelli Fontanive, Fernando; Bastos Caramao, Elina; Alcaraz Zini, Claudia [Universidade Federal do Rio Grande do Sul, Instituto de Quimica, Porto Alegre, RS (Brazil); Oliveira, Jose Vladimir de [URI, Universidade Regional Integrada do Alto Uruguai e das Missoes, Erechim, RS (Brazil)

    2011-11-15

    The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SO{sub x} gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC-qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC x GC-TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC-qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GC x GC-TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC x GC. (orig.)

  3. Mapping the Fundamental Niches of Two Freshwater Microalgae, Chlorella vulgaris (Trebouxiophyceae and Peridinium cinctum (Dinophyceae, in 5-Dimensional Ion Space

    Directory of Open Access Journals (Sweden)

    Terence J. Evens

    2011-01-01

    Full Text Available The fundamental niche defined by five ions, NO3 −, PO4 3−, K+, Na+, and Cl−, was mapped for Chlorella vulgaris (Trebouxiophyceae and Peridinium cinctum (Dinophyceae growth rates and maximum cell densities in batch cultures. A five dimensional ion-mixture experimental design was projected across a total ion concentration gradient of 1 to 30 mM to delineate the ion-based, “potential” niche space, defined as the entire n-dimensional hypervolume demarcated by the feasible ranges of the independent factors under consideration. The growth rate-based, fundamental niche volumes overlapped for ca. 94% of the ion mixtures, although the regions of maximal growth rates and cell densities were different for each alga. Both C. vulgaris and P. cinctum exhibited similar positive responses to cations and negative responses to anions. It was determined that total ion concentration for these five ions, from 1 to 30 mM, did not directly affect either growth rate or maximal cell density for either alga, although it did play an interactive role with several ions. This study is the first that we are aware of to attempt the mapping of a multivariate, ion-based, fundamental niche volume. The implications of the experimental design utilized and the potential utility of this type of approach are discussed.

  4. Ion-streaming induced order transition in three-dimensional dust clusters

    International Nuclear Information System (INIS)

    Ludwig, Patrick; Kählert, Hanno; Bonitz, Michael

    2012-01-01

    Dust dynamics simulations utilizing a dynamical screening approach are performed to study the effect of ion-streaming on the self-organized structures in a three-dimensional spherically confined complex (dusty) plasma. Varying the Mach number M, the ratio of ion drift velocity to the sound velocity, the simulations reproduce the experimentally observed cluster configurations in the two limiting cases: at M = 0 strongly correlated crystalline structures consisting of nested spherical shells (Yukawa balls) and, for M ⩾ 1, flow-aligned dust chains, respectively. In addition, our simulations reveal a discontinuous transition between these two limits. It is found that already a moderate ion drift velocity (M ≈ 0.1 for the plasma conditions considered here) destabilizes the highly ordered Yukawa balls and initiates an abrupt melting transition. The critical value of M is found to be independent of the cluster size. (paper)

  5. Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

    2017-01-27

    A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Application of ion chromatography in pharmaceutical and drug analysis.

    Science.gov (United States)

    Jenke, Dennis

    2011-08-01

    Ion chromatography (IC) has developed and matured into an important analytical methodology in a number of diverse applications and industries, including pharmaceuticals. This manuscript provides a review of IC applications for the determinations of active and inactive ingredients, excipients, degradation products, and impurities relevant to pharmaceutical analyses and thus serves as a resource for investigators looking for insights into the use of the IC methodology in this field of application.

  7. Metabolomics strategy for the mapping of volatile exometabolome from Saccharomyces spp. widely used in the food industry based on comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Martins, Cátia; Brandão, Tiago; Almeida, Adelaide; Rocha, Sílvia M

    2017-05-01

    Saccharomyces spp. are widely used in the food and beverages industries. Their cellular excreted metabolites are important for general quality of products and can contribute to product differentiation. This exploratory study presents a metabolomics strategy for the comprehensive mapping of cellular metabolites of two yeast species, Saccharomyces cerevisiae and S. pastorianus (both collected in an industrial context) through a multidimensional chromatography platform. Solid-phase microextraction was used as a sample preparation method. The yeast viability, a specific technological quality parameter, was also assessed. This untargeted analysis allowed the putative identification of 525 analytes, distributed over 14 chemical families, the origin of which may be explained through the pathways network associated with yeasts metabolism. The expression of the different metabolic pathways was similar for both species, event that seems to be yeast genus dependent. Nevertheless, these species showed different growth rates, which led to statistically different metabolites content. This was the first in-depth approach that characterizes the headspace content of S. cerevisiae and S. pastorianus species cultures. The combination of a sample preparation method capable of providing released volatile metabolites directly from yeast culture headspace with comprehensive two-dimensional gas chromatography was successful in uncovering a specific metabolomic pattern for each species. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Ion-Exclusion Chromatography for Analyzing Organics in Water

    Science.gov (United States)

    Sauer, Richard; Rutz, Jeffrey A.; Schultz, John R.

    2006-01-01

    A liquid-chromatography technique has been developed for use in the quantitative analysis of urea (and of other nonvolatile organic compounds typically found with urea) dissolved in water. The technique involves the use of a column that contains an ion-exclusion resin; heretofore, this column has been sold for use in analyzing monosaccharides and food softeners, but not for analyzing water supplies. The prior technique commonly used to analyze water for urea content has been one of high-performance liquid chromatography (HPLC), with reliance on hydrophobic interactions between analytes in a water sample and long-chain alkyl groups bonded to an HPLC column. The prior technique has proven inadequate because of a strong tendency toward co-elution of urea with other compounds. Co-elution often causes the urea and other compounds to be crowded into a narrow region of the chromatogram (see left part of figure), thereby giving rise to low chromatographic resolution and misidentification of compounds. It is possible to quantitate urea or another analyte via ultraviolet- and visible-light absorbance measurements, but in order to perform such measurements, it is necessary to dilute the sample, causing a significant loss of sensitivity. The ion-exclusion resin used in the improved technique is sulfonated polystyrene in the calcium form. Whereas the alkyl-chain column used in the prior technique separates compounds on the basis of polarity only, the ion-exclusion-resin column used in the improved technique separates compounds on the basis of both molecular size and electric charge. As a result, the degree of separation is increased: instead of being crowded together into a single chromatographic peak only about 1 to 2 minutes wide as in the prior technique, the chromatographic peaks of different compounds are now separated from each other and spread out over a range about 33 minutes wide (see right part of figure), and the urea peak can readily be distinguished from the other

  9. Application of Tandem Two-Dimensional Mass Spectrometry for Top-Down Deep Sequencing of Calmodulin.

    Science.gov (United States)

    Floris, Federico; Chiron, Lionel; Lynch, Alice M; Barrow, Mark P; Delsuc, Marc-André; O'Connor, Peter B

    2018-06-04

    Two-dimensional mass spectrometry (2DMS) involves simultaneous acquisition of the fragmentation patterns of all the analytes in a mixture by correlating their precursor and fragment ions by modulating precursor ions systematically through a fragmentation zone. Tandem two-dimensional mass spectrometry (MS/2DMS) unites the ultra-high accuracy of Fourier transform ion cyclotron resonance (FT-ICR) MS/MS and the simultaneous data-independent fragmentation of 2DMS to achieve extensive inter-residue fragmentation of entire proteins. 2DMS was recently developed for top-down proteomics (TDP), and applied to the analysis of calmodulin (CaM), reporting a cleavage coverage of about ~23% using infrared multiphoton dissociation (IRMPD) as fragmentation technique. The goal of this work is to expand the utility of top-down protein analysis using MS/2DMS in order to extend the cleavage coverage in top-down proteomics further into the interior regions of the protein. In this case, using MS/2DMS, the cleavage coverage of CaM increased from ~23% to ~42%. Graphical Abstract Two-dimensional mass spectrometry, when applied to primary fragment ions from the source, allows deep-sequencing of the protein calmodulin.

  10. Focusing and non-focusing modulation strategies for the improvement of on-line two-dimensional hydrophilic interaction chromatography × reversed phase profiling of complex food samples.

    Science.gov (United States)

    Montero, Lidia; Ibáñez, Elena; Russo, Mariateresa; Rastrelli, Luca; Cifuentes, Alejandro; Herrero, Miguel

    2017-09-08

    Comprehensive two-dimensional liquid chromatography (LC × LC) is ever gaining interest in food analysis, as often, food-related samples are too complex to be analyzed through one-dimensional approaches. The use of hydrophilic interaction chromatography (HILIC) combined with reversed phase (RP) separations has already been demonstrated as a very orthogonal combination, which allows attaining increased resolving power. However, this coupling encompasses different analytical challenges, mainly related to the important solvent strength mismatch between the two dimensions, besides those common to every LC × LC method. In the present contribution, different strategies are proposed and compared to further increase HILIC × RP method performance for the analysis of complex food samples, using licorice as a model sample. The influence of different parameters in non-focusing modulation methods based on sampling loops, as well as under focusing modulation, through the use of trapping columns in the interface and through active modulation procedures are studied in order to produce resolving power and sensitivity gains. Although the use of a dilution strategy using sampling loops as well as the highest possible first dimension sampling rate allowed significant improvements on resolution, focusing modulation produced significant gains also in peak capacity and sensitivity. Overall, the obtained results demonstrate the great applicability and potential that active modulation may have for the analysis of complex food samples, such as licorice, by HILIC × RP. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Lima Gomes, Paulo C F; Barnes, Brian B; Santos-Neto, Álvaro J; Lancas, Fernando M; Snow, Nicholas H

    2013-07-19

    Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.6 to 1200μgL(-1) and limits of detection and quantitation from 0.02 to 100μgL(-1). A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC-ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Application of ion chromatography to the determination of water-soluble inorganic and organic ions in atmospheric aerosols.

    Science.gov (United States)

    Yu, Xue-Chun; He, Ke-Bin; Ma, Yong-Liang; Yang, Fu-Mo; Duan, Feng-Kui; Zheng, Ai-Hua; Zhao, Cheng-Yi

    2004-01-01

    A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F- , Cl- , NO2(-), NO3(-), SO3(2-), SO4(2-) , PO4(3-)), and fifteen water-soluble organic ions(formate, acetate, MSA, oxalate, malonate, succinate, phthalates, etc.) in atmospheric aerosols. The linear concentrations ranged from 0.005 microg/m3 to 500 microg/m3 ( r = 0.999-0.9999). The relative standard deviation (RSD) were 0.43%-2.00% and the detection limits were from 2.7 ng/m3 to 88 ng/m3. The proposed method was successfully applied to the simultaneous determination of those inorganic ions and organic ions in PM2.5 of Beijing.

  13. Calibration of shahid's analytical method for adulterated Zn-edta fertilizers by ion chromatography and atomic absorption spectroscopy

    International Nuclear Information System (INIS)

    Khan, M.S.A.; Akram, M.; Qazi, M.A.

    2010-01-01

    Chelated zinc fertilizers are usually recommended in calcareous alkaline soils to provide Zn nutrition in order to prevent possible Zn precipitation. In Punjab (Pakistan), Zn EDTA products are being manufactured, and marketed to meet the zinc requirement of various crops grown in Zn deficient soils. Under fertilizer control order, 1973 (amended), their quality has to be monitored by the Agriculture Department, Government of the Punjab. None of the traditional method was found suitable which can separate the mineral fraction from that of chelated adulterated fertilizer except for those methods based on ion chromatography. Calibration of ion chromatography method was carried out by determining the mineral Zn fraction leading to estimate remaining Zn EDTA fraction in fertilizer samples of adulterated nature i.e. mixture of chelated and mineral fraction. In order to achieve the objective atomic absorption spectroscopy was coupled with ion chromatography. The method offers a specific, reliable technique for determination of chelated zinc in fertilizers. In the first step chelation was broken down with concentrated sulphuric acid treatment and total zinc contents were determined by atomic absorption spectroscopy. In second step, non-chelated (mineral) portion of zinc was determined by ion chromatography using cation column and conductivity detector. Chelated zinc was calculated by subtracting non-chelated (mineral) fraction from total zinc contents. (author)

  14. High-performance liquid ion-pair chromatography in inorganic analysis

    International Nuclear Information System (INIS)

    Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

    1990-01-01

    In literature review for the recent 15 years theoretical foundations, regularities and mechanisms of ionized compound retention in reverse-phase ion-pair chromatography are considered, possibilities and prospects of its application in inorganic analysis being demonstrated. Analytic characteristics of the methods for the determination of inorganic anions (I - , IO 3 - , MoO 4 2- , etc.), as well as metals (Zr, Hf, V, Nb, Mo, W, Ru, lanthanides, etc.) in the form of chelates, are given

  15. The removal of uranium from acidic media using ion exchange and/or extraction chromatography

    International Nuclear Information System (INIS)

    FitzPatrick, J.R.; Schake, B.S.; Murphy, J.; Holmes, K.; West, M.H.

    1996-06-01

    The separation and purification of uranium from either nitric acid or hydrochloric acid media can be accomplished by using either solvent extraction or ion-exchange. Over the past two years at Los Alamos, emerging programs are focused on recapturing the expertise required to do limited, small-quantity processing of enriched uranium. During this period of time, we have been investigating ion-addition, waste stream polishing is associated with this effort in order to achieve more complete removal of uranium prior to recycle of the acid. Extraction chromatography has been demonstrated to further polish the uranium from both nitric and hydrochloric acid media thus allowing for a more complete recovery of the actinide material and creation of less waste during the processing steps

  16. Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

    NARCIS (Netherlands)

    Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

    1995-01-01

    In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

  17. Capillary ion chromatography with on-column focusing for ultra-trace analysis of methanesulfonate and inorganic anions in limited volume Antarctic ice core samples.

    Science.gov (United States)

    Rodriguez, Estrella Sanz; Poynter, Sam; Curran, Mark; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

    2015-08-28

    Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. High-performance ion-exchange chromatography of alkali metals with conductivity detection

    International Nuclear Information System (INIS)

    Ahmad, M.; Khan, A.R.

    1981-01-01

    High-performance ion-exchange chromatography of alkali metal and ammonium ions was studied using a conductivity meter as detector. Elution with 0.003 N mitric acid gave excellent resolution. Sensitivity levels, for a 200 micro litre injection, vary from 5 ppm for potassium to 0.1 ppm for lithium. A method to decrease retention times by reducing the exchange capacity of the cation exchange column used by loading it with calciumions, without affecting the resolation, has been described. Application of the method to water, soil and uranium dioxide samples has been demonstrated. (author)

  19. Chemically functionalized two-dimensional titanium carbide MXene by in situ grafting-intercalating with diazonium ions to enhance supercapacitive performance

    Science.gov (United States)

    Wang, Hongbing; Zhang, Jianfeng; Wu, Yuping; Huang, Huajie; Jiang, Quanguo

    2018-04-01

    Two-dimensional Ti3C2 MXene nanosheets were functionalized with phenylsulfonic groups derived from in situ generated diazonium ions by the corresponding amine. During the functionalization process, the aryl groups were attached onto the MXene surfaces in the form of strong MXene-aryl (Tisbnd Osbnd C) linkages. Simultaneously, the intercalation of diazonium ions enabled Ti3C2 multi-layers to be delaminated into separate few-layer nanosheets via weak sonication with low energy. As a result of chemical functionalization for MXene Ti3C2, the dispersibility was greatly improved and the specific surface area increased significantly. The grafted functional groups are still stable up to at least 200 °C upon thermogravimetric analysis measurements. With diazonium ions intercalating and electroactive groups grafting between-in MXene layers, the chemically functionalized Ti3C2 electrodes exhibited an enhanced supercapacitive performance, which acquired a specific capacitance more than double that of pristine Ti3C2 samples and excellent cycling stability (91% capacity retention after 10,000 cycles at 3 A g-1). This feasible modification scheme can be also extended to functionalize other types of MXenes materials with this or other aryl diazonium ions as surface modifiers and intercalants, thus offering scope for full potential applications of the new 2D materials.

  20. Establishing the analytical procedure for acetate in water by ion chromatography method

    International Nuclear Information System (INIS)

    Nguyen Thi Hong Thinh; Ha Lan Anh; Vo Thi Anh

    2015-01-01

    In recent studies of contamination sources of arsenic, ammonium, iron, organic carbon in groundwater, acetate is measured a lot because it is the main decomposition product of organic compounds from sediment into groundwater. In order to better support for the study of the origin and mobilization mechanism of the pollutants, acetate was studied analysis method in Isotopes Hydrology Laboratory using ion chromatography technique. Project Researchers used Ion Chromatography system - DX-600 including IonPac ICE-AS1 column for separating acetate and conductivity detector CD 25 to quantify acetate in water samples. The study results showed that project team has successfully developed analytical procedures of acetate in water with acetate’s retention time is 12 minutes, limit of detection (LOD) of the method was 0.01 ppm. The accuracy of the method was established by calculating the precision and bias of 10 analysis times of a standard sample at content levels 1 ppm and 8 ppm. The results of the 10 measurements are satisfiable about precision and bias with repeated standard deviation coefficient CVR were 1.3% and 0.2% and the recoveries R were 99.92% and 101.72%. (author)

  1. Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, Th.

    2006-01-01

    The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical

  2. Comprehensive two-dimensional liquid chromatographic analysis of poloxamers.

    Science.gov (United States)

    Malik, Muhammad Imran; Lee, Sanghoon; Chang, Taihyun

    2016-04-15

    Poloxamers are low molar mass triblock copolymers of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO), having number of applications as non-ionic surfactants. Comprehensive one and two-dimensional liquid chromatographic (LC) analysis of these materials is proposed in this study. The separation of oligomers of both types (PEO and PPO) is demonstrated for several commercial poloxamers. This is accomplished at the critical conditions for one of the block while interaction for the other block. Reversed phase LC at CAP of PEO allowed for oligomeric separation of triblock copolymers with regard to PPO block whereas normal phase LC at CAP of PPO renders oligomeric separation with respect to PEO block. The oligomeric separation with regard to PEO and PPO are coupled online (comprehensive 2D-LC) to reveal two-dimensional contour plots by unconventional 2D IC×IC (interaction chromatography) coupling. The study provides chemical composition mapping of both PEO and PPO, equivalent to combined molar mass and chemical composition mapping for several commercial poloxamers. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. A computationally efficient simulator for three-dimensional Monte Carlo simulation of ion implantation into complex structures

    International Nuclear Information System (INIS)

    Li Di; Wang Geng; Chen Yang; Li Lin; Shrivastav, Gaurav; Oak, Stimit; Tasch, Al; Banerjee, Sanjay; Obradovic, Borna

    2001-01-01

    A physically-based three-dimensional Monte Carlo simulator has been developed within UT-MARLOWE, which is capable of simulating ion implantation into multi-material systems and arbitrary topography. Introducing the third dimension can result in a severe CPU time penalty. In order to minimize this penalty, a three-dimensional trajectory replication algorithm has been developed, implemented and verified. More than two orders of magnitude savings of CPU time have been observed. An unbalanced Octree structure was used to decompose three-dimensional structures. It effectively simplifies the structure, offers a good balance between modeling accuracy and computational efficiency, and allows arbitrary precision of mapping the Octree onto desired structure. Using the well-established and validated physical models in UT-MARLOWE 5.0, this simulator has been extensively verified by comparing the integrated one-dimensional simulation results with secondary ion mass spectroscopy (SIMS). Two options, the typical case and the worst scenario, have been selected to simulate ion implantation into poly-silicon under various scenarios using this simulator: implantation into a random, amorphous network, and implantation into the worst-case channeling condition, into (1 1 0) orientated wafers

  4. Study and application of ion chromatography and activation analysis without chemical separation for the determination of sodium and potassium in muscle tissues

    International Nuclear Information System (INIS)

    Haber, E.P.

    1984-01-01

    The simultaneous determination of Na and K in small amounts of muscular tissue by use of two methods, namely activation analysis and ion chromatography, is presented. For the activation analysis the samples were irradiated for 30 minutes in a 5 X 10 11 n cm sup(-) 2 s sup(-) 1 flux. The induced activities of 24 Na and 42 K were determined, without chemical separation, using a Ge(Li) detector equipped with a 4096 channel analyser on-line with a computer. The gamma ray spectra registered from the samples and standards were analysed and compared by the computer. For the ion chromatography analysis the samples and standards in solution were injected into the apparatus. The ions were separated by an ion-exchange system of columns and the concentrations were measured by conductivity. In addition, the two analytical methods were compared in regard to sensitivity, precision and accuracy as well as simplicity, cost and working time involved in the analysis. From the point of view of the reliability of the results, both techniques proved to be excelent and might be of great value in medical research. (Author) [pt

  5. Nonstationarity of a two-dimensional quasiperpendicular supercritical collisionless shock by self-reformation

    International Nuclear Information System (INIS)

    Lembege, B.; Savoini, P.

    1992-01-01

    Two-dimensional electromagnetic particle simulations evidence a self-reformation of the shock front for a collisionless supercritical magnetosonic shock propagating at angle θ 0 around 90 degree, where θ 0 is the angle between the normal to the shock front and the upstream magnetostatic field. This self-reformation is due to reflected ions which accumulate in front of the shock and is observed (i) in both electric and magnetic components, (ii) for both resistive and nonresistive two-dimensional shocks, and (iii) over a cyclic time period equal to the mean ion gyroperiod measured downstream in the overshoot; resistive effects may be self-consistently included or excluded for θ 0 congruent 90 degree according to a judicious choice of the upstream magnetostatic field orientation. The self-reformation leads to a nonstationary behavior of the shock; however, present results show evidence that the shock becomes stationary for θ less than a critical value θ r , below which the self-reformation disappears. Present results are compared to previous works where one/two-dimensional hybrid and particle codes have been used, and to experimental measurements

  6. Application of Ion Chromatography to the Investigation of Real-World Samples

    Science.gov (United States)

    Whelan, Rebecca J.; Hannon, Theresa E.; Zare, Richard N.

    2004-01-01

    The use of ion chromatography (IC) as a means to teach important analytical concepts while giving the students a valuable opportunity to identify and investigate a real-world system of interest to them is described. A single IC apparatus can be tailored for different classes of analyses by the selection of different column-eluent combinations.

  7. Ion mobility spectrometry after supercritical fluid chromatography

    International Nuclear Information System (INIS)

    Morrissey, M.A.

    1988-01-01

    In this work, a Fourier transform ion mobility spectrometer (FT-IMS) was constructed and evaluated as a detector for supercritical fluid chromatography (SFC). The FT-IMS provides both quantitative and qualitative data of a wide range of compounds, selective and nonselective modes of chromatographic detection, and it is compatible with a wide range of SFC mobile phases. Drift spectra are presented for a number of samples, including polymers, lipids, herbicides, antibiotics, and pharmaceuticals. The unique properties of supercritical fluids made it possible to introduce these compounds into the spectrometer. While the drift spectra presented are generally simple, showing only a quasi-molecular ion, a few are surprising complex. Examples of selective and non-selective detection demonstrate the usefulness of the detector. Examples are presented for fish oil concentrate, bacon grease extract, soil extract, and polymer mixtures. In the case of Triton X-100, a non-ionic surfactant, the FT-IMS was able to selectively detect individual oligomers in the polymer mixture. In the case of a polydimethylsilicone mixture the detector isolated a contaminant in the mixture

  8. Large-scale analysis of in Vivo phosphorylated membrane proteins by immobilized metal ion affinity chromatography and mass spectrometry

    DEFF Research Database (Denmark)

    Nühse, Thomas S; Stensballe, Allan; Jensen, Ole N

    2003-01-01

    specificity. We investigated the potential of IMAC in combination with capillary liquid chromatography coupled to tandem mass spectrometry for the identification of plasma membrane phosphoproteins of Arabidopsis. Without chemical modification of peptides, over 75% pure phosphopeptides were isolated from...... plasma membrane digests and detected and sequenced by mass spectrometry. We present a scheme for two-dimensional peptide separation using strong anion exchange chromatography prior to IMAC that both decreases the complexity of IMAC-purified phosphopeptides and yields a far greater coverage...... of monophosphorylated peptides. Among the identified sequences, six originated from different isoforms of the plasma membrane H(+)-ATPase and defined two previously unknown phosphorylation sites at the regulatory C terminus. The potential for large-scale identification of phosphorylation sites on plasma membrane...

  9. Metal ion-improved complexation countercurrent chromatography for enantioseparation of dihydroflavone enantiomers.

    Science.gov (United States)

    Han, Chao; Wang, Wenli; Xue, Guimin; Xu, Dingqiao; Zhu, Tianyu; Wang, Shanshan; Cai, Pei; Luo, Jianguang; Kong, Lingyi

    2018-01-12

    Cu(II) ion was selected as an additive to improve the enantioseparation efficiency of three dihydroflavone enantiomers in high-speed counter-current chromatography (HSCCC), using hydroxypropyl-β-cyclodextrin (HP-β-CyD) as the chiral selector. The influences of important parameters, including the metal ion, the concentrations of HP-β-CyD and the Cu(II) ion, and the sample size were investigated. Under optimal conditions, three dihydroflavone enantiomers, including (±)-hesperetin, (±)-naringenin, and (±)-farrerol, were successfully enantioseparated. The chiral recognition mechanism was investigated. The enantioseparation was attributed to the different thermodynamic stabilities of the binary complexes of HP-β-CyD and (±)-hesperetin, and Cu(II) ion could enhance this difference by forming ternary complexes with the binary complexes. This Cu(II) ion-improved complexation HSCCC system exhibited improved performance for chiral separation, and therefore it has great application potential in the preparative enantioseparation of other compounds with similar skeletons. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Analysis of catecholamines in urine by unique LC/MS suitable ion-pairing chromatography.

    Science.gov (United States)

    Bergmann, Marianne L; Sadjadi, Seyed; Schmedes, Anne

    2017-07-01

    The catecholamines, epinephrine (E) and norepinephrine (NE) are small polar, hydrophilic molecules, posing significant challenges to liquid chromatography - tandem mass spectrometry (LC-MS/MS) method development. Specifically, these compounds show little retention on conventional reversed-phase liquid chromatography columns. This work presents development and validation of an LC-MS/MS method for determining catecholamines in urine, based on a new approach to ion-pairing chromatography (IPC), in which the ion-pairing reagent (IPR), 1-Heptane Sulfonic Acid (HSA), is added to the extracted samples instead of the mobile phases. A Hamilton STARlet workstation carried out the solid phase extraction of urine samples. The extracted samples were diluted with 60mmol/L HSA and injected on a Kinetex core-shell biphenyl column with conventional LC-MS/MS suitable mobile phases. Chromatographic separation of E and NE was achieved successfully with very stable retention times (RT). In 484 injections, the RTs were steady with a CV of less than ±4%. Furthermore, HSA was separated from E and NE, allowing HSA to be diverted to waste instead of entering the mass spectrometer ion chamber. The method was validated with good analytical performance, and even though the analysis for urinary catecholamines is increasingly being replaced by plasma free metanephrines in diagnosing pheochromocytomas, this work represents the application of a new analytical technique that can be transferred to other small polar molecules, that are difficult to chromatograph on traditional reversed phase columns. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Two-dimensional errors

    International Nuclear Information System (INIS)

    Anon.

    1991-01-01

    This chapter addresses the extension of previous work in one-dimensional (linear) error theory to two-dimensional error analysis. The topics of the chapter include the definition of two-dimensional error, the probability ellipse, the probability circle, elliptical (circular) error evaluation, the application to position accuracy, and the use of control systems (points) in measurements

  12. The isotope separation by ion exchange chromatography. Application to the lithium isotopes separation

    International Nuclear Information System (INIS)

    Albert, M.G.; Barre, Y.; Neige, R.

    1993-01-01

    In this work is described the used study step to demonstrate the industrial feasibility of a lithium isotopes separation process by ion exchange chromatography. After having recalled how is carried out the exchange reaction between the lithium isotopes bound on the cations exchanger resin and those which are in solution and gave the ion exchange chromatography principle, the authors establish a model which takes into account the cascade theory already used for enriched uranium production. The size parameters of this model are: the isotopic separation factor (which depends for lithium of the ligands nature and of the coordination factor), the isotopic exchange kinetics and the mass flow (which depends of the temperature, the lithium concentration, the resins diameter and the front advance). The way they have to be optimized and the implementation of the industrial process are given. (O.M.)

  13. Two-dimensional transport of tokamak plasmas

    International Nuclear Information System (INIS)

    Hirshman, S.P.; Jardin, S.C.

    1979-01-01

    A reduced set of two-fluid transport equations is obtained from the conservation equations describing the time evolution of the differential particle number, entropy, and magnetic fluxes in an axisymmetric toroidal plasma with nested magnetic surfaces. Expanding in the small ratio of perpendicular to parallel mobilities and thermal conductivities yields as solubility constraints one-dimensional equations for the surface-averaged thermodynamic variables and magnetic fluxes. Since Ohm's law E +u x B =R', where R' accounts for any nonideal effects, only determines the particle flow relative to the diffusing magnetic surfaces, it is necessary to solve a single two-dimensional generalized differential equation, (partial/partialt) delpsi. (delp - J x B) =0, to find the absolute velocity of a magnetic surface enclosing a fixed toroidal flux. This equation is linear but nonstandard in that it involves flux surface averages of the unknown velocity. Specification of R' and the cross-field ion and electron heat fluxes provides a closed system of equations. A time-dependent coordinate transformation is used to describe the diffusion of plasma quantities through magnetic surfaces of changing shape

  14. The use of ion chromatography in environmental and process control in the nuclear industry. Vol. 4

    Energy Technology Data Exchange (ETDEWEB)

    Mohamed, M M [Ultra Tech Inc, 28 Teiba St. Dokki-Cairo, (Egypt)

    1996-03-01

    Ion chromatography has become the method choice for determining sub ppb for inorganic anions and cations, such as chloride, sulfide, fluoride, sodium, potassium, and ammonium, in aqueous matrices. Steam generators in pressurized water reactors nuclear power plants occasionally experience tubing degradation by a variety of corrosion related mechanisms which depends on water chemistry. Ion chromatography is also used in other environmental applications such as air pollution, industrial hygiene, drinking water quality, and industrial waste treatment. In this paper, several methods of separation and detection are present and also a number of examples of samples for various types of water are shown. The examples will include sub ppb amounts of chloride, sulfate, sodium, potassium, and ammonium in high purity turbine steam. Testing of chlorinated drinking water for inorganic anions including chlorite, chloride chlorate nitrite, nitrate as other organic anions using chemically suppressed conductivity. The role of chemical suppression is discussed. The analysis of ppb levels of transition moles in high purity water using ion chromatography with post column derivatization and UV detection are reviewed. Testing of disinfected drinking water with ozone for bromate, the detection of cyanide in waste after acid digestion, and the detection of highly toxic hexavalent in the presence of trivalent chromium is discussed. A fast method for the analysis of rain water for anions and cations is described. The presentation will also show new method (chelation ion chromatography) which enables ppb levels of heavy metals to be determined as pollutants in difficult environmental matrices such seawater, and oyster tissue. 4 figs.

  15. The use of ion chromatography in environmental and process control in the nuclear industry. Vol. 4

    International Nuclear Information System (INIS)

    Mohamed, M.M.

    1996-01-01

    Ion chromatography has become the method choice for determining sub ppb for inorganic anions and cations, such as chloride, sulfide, fluoride, sodium, potassium, and ammonium, in aqueous matrices. Steam generators in pressurized water reactors nuclear power plants occasionally experience tubing degradation by a variety of corrosion related mechanisms which depends on water chemistry. Ion chromatography is also used in other environmental applications such as air pollution, industrial hygiene, drinking water quality, and industrial waste treatment. In this paper, several methods of separation and detection are present and also a number of examples of samples for various types of water are shown. The examples will include sub ppb amounts of chloride, sulfate, sodium, potassium, and ammonium in high purity turbine steam. Testing of chlorinated drinking water for inorganic anions including chlorite, chloride chlorate nitrite, nitrate as other organic anions using chemically suppressed conductivity. The role of chemical suppression is discussed. The analysis of ppb levels of transition moles in high purity water using ion chromatography with post column derivatization and UV detection are reviewed. Testing of disinfected drinking water with ozone for bromate, the detection of cyanide in waste after acid digestion, and the detection of highly toxic hexavalent in the presence of trivalent chromium is discussed. A fast method for the analysis of rain water for anions and cations is described. The presentation will also show new method (chelation ion chromatography) which enables ppb levels of heavy metals to be determined as pollutants in difficult environmental matrices such seawater, and oyster tissue. 4 figs

  16. High-resolution mapping of two-dimensional lattice distortions in ion-implanted crystals from X-ray diffractometry data

    International Nuclear Information System (INIS)

    Nikulin, A.Y.; Gureyev, T.E.; Stevenson, A.W.; Wilkins, S.W.; Hashizume, H.; Cookson, D.

    1996-01-01

    The triple-crystal synchrotron X-ray diffractometry data described in Nikulin, Stevenson, Hashizume, Wilkins, Foran, Cookson and Garrett (J. Appl. Cryst. 28, 57-60 (1995)) has been analyzed to map out two-dimensional (2D) lattice distortions in silicon (111) crystals implanted with B + ions of 100 keV energy through a periodic SiO 2 strip pattern. The lateral periodic structure produced a series of satellite reflections associated with the 111 Bragg peak. The 2D reconstruction incorporates the use of the Petrashen-Chukhovskii method, which retrieves the phases of the Bragg waves for these satellite reflections, together with that for the fundamental. The finite Fourier series is then synthesized with the relative phases determined. Localized distortions perpendicular to the surface arising from deposited B + ions in near-surface layers of the crystal are clearly displayed with spatial resolutions of 0.016 and 0.265 μm in the depth and lateral directions respectively. For a sample with the oxide layer removed from the surface, two equally plausible strain maps have been obtained by assigning relative phases to eleven satellites using a sequential trial method and a minimum-energy method. Failed map reconstructions for the oxide-covered sample are discussed in terms of the non-unique solutions of the Petrashen-Chukhovskii phase-recovery algorithm and the ambiguous phases determined for the satellites. 16 refs., 8 figs

  17. Two-dimensional quantum repeaters

    Science.gov (United States)

    Wallnöfer, J.; Zwerger, M.; Muschik, C.; Sangouard, N.; Dür, W.

    2016-11-01

    The endeavor to develop quantum networks gave rise to a rapidly developing field with far-reaching applications such as secure communication and the realization of distributed computing tasks. This ultimately calls for the creation of flexible multiuser structures that allow for quantum communication between arbitrary pairs of parties in the network and facilitate also multiuser applications. To address this challenge, we propose a two-dimensional quantum repeater architecture to establish long-distance entanglement shared between multiple communication partners in the presence of channel noise and imperfect local control operations. The scheme is based on the creation of self-similar multiqubit entanglement structures at growing scale, where variants of entanglement swapping and multiparty entanglement purification are combined to create high-fidelity entangled states. We show how such networks can be implemented using trapped ions in cavities.

  18. Determination of chloride and sulphur in sodium by ion chromatography and its application to PFBR sodium samples

    International Nuclear Information System (INIS)

    Vijayalakshmi, S.; Ushalakshmi, K.

    2011-01-01

    Analytical method using ion chromatography was developed for the determination of chloride and sulphur in sodium. In this method, sodium was dissolved in water and various sulphur species present in the sample was oxidized to sulphate using hydrogen peroxide. Carbon dioxide gas was passed through the solution to convert sodium hydroxide to carbonate solution. The resulting sample solution was analysed using suppressed Ion chromatography employing carbonate eluent. This method was applied to the analysis of sodium samples procured for prototype fast breeder reactor. (author)

  19. Ion-exchange chromatography for the characterization of biopharmaceuticals.

    Science.gov (United States)

    Fekete, Szabolcs; Beck, Alain; Veuthey, Jean-Luc; Guillarme, Davy

    2015-09-10

    Ion-exchange chromatography (IEX) is a historical technique widely used for the detailed characterization of therapeutic proteins and can be considered as a reference and powerful technique for the qualitative and quantitative evaluation of charge heterogeneity. The goal of this review is to provide an overview of theoretical and practical aspects of modern IEX applied for the characterization of therapeutic proteins including monoclonal antibodies (Mabs) and antibody drug conjugates (ADCs). The section on method development describes how to select a suitable stationary phase chemistry and dimensions, the mobile phase conditions (pH, nature and concentration of salt), as well as the temperature and flow rate, considering proteins isoelectric point (pI). In addition, both salt-gradient and pH-gradient approaches were critically reviewed and benefits as well as limitations of these two strategies were provided. Finally, several applications, mostly from pharmaceutical industries, illustrate the potential of IEX for the characterization of charge variants of various types of biopharmaceutical products. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Discriminating Brazilian crude oils using comprehensive two-dimensional gas chromatography-mass spectrometry and multiway principal component analysis.

    Science.gov (United States)

    Prata, Paloma S; Alexandrino, Guilherme L; Mogollón, Noroska Gabriela S; Augusto, Fabio

    2016-11-11

    The geochemical characterization of petroleum is an essential task to develop new strategies and technologies when analyzing the commercial potential of crude oils for exploitation. Due to the chemical complexity of these samples, the use of modern analytical techniques along with multivariate exploratory data analysis approaches is an interesting strategy to extract relevant geochemical characteristics about the oils. In this work, important geochemical information obtained from crude oils from different production basins were obtained analyzing the maltene fraction of the oils by comprehensive two-dimensional gas chromatography coupled to quadrupole mass spectrometry (GC×GC-QMS), and performing multiway principal component analysis (MPCA) of the chromatographic data. The results showed that four MPC explained 93.57% of the data variance, expressing mainly the differences on the profiles of the saturated hydrocarbon fraction of the oils (C 13 -C 18 and C 19 -C 30 n-alkanes and the pristane/phytane ratio). The MPC1 grouped the samples severely biodegraded oils, while the type of the depositional paleoenvironments of the oils and its oxidation conditions (as well as their thermal maturity) could be inferred analysing others relevant MPC. Additionally, considerations about the source of the oil samples was also possible based on the overall distribution of relevant biomarkers such as the phenanthrene derivatives, tri-, tetra- and pentacyclic terpanes. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products

    Energy Technology Data Exchange (ETDEWEB)

    Qiu, Ying-Kun, E-mail: qyk@xmu.edu.cn; Chen, Fang-Fang; Zhang, Ling-Ling; Yan, Xia; Chen, Lin; Fang, Mei-Juan; Wu, Zhen, E-mail: wuzhen@xmu.edu.cn

    2014-04-01

    Highlights: • Preparative MDLC system was developed for separation of complicated natural products. • Medium-pressure LC and preparative HPLC were connected by interface of SPE. • Automated multi-step preparative separation of 25 compounds was achieved by using this system. - Abstract: An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm × 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC × preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, {sup 1}H NMR and even by less-sensitive {sup 13}C NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods.

  2. Role of ion chromatography in the chemical characterization of PFBR MOX fuel

    International Nuclear Information System (INIS)

    Kelkar, Anoop; Das, D.K.; Prakash, Amrit; Behere, P.G.; Afzal, Mohd

    2012-01-01

    Ion chromatography (IC) is multi-element technique with the feasibility of determination of metallic as well as non metallic impurities on a single instrument. IC has been used for various analytical purposes in nuclear industry. lt has advantages of low capital investment, small sample size, less radioactive waste generation, comparable precision to spectroscopic techniques and ease of fume hood/glove box adaptation. Present paper describes the determination of trace metallic (alkali, alkaline earth, transition and lanthanide metal ions) and non metallic impurities in PFBR MOX fuel

  3. Utilization of Ion-Exclusion Chromatography for Water Quality Monitoring in a Suburban River in Jakarta, Indonesia

    Directory of Open Access Journals (Sweden)

    Daisuke Kozaki

    2014-07-01

    Full Text Available We evaluated the use of ion-exclusion chromatographic systems for analyzing the behavior of inorganic ions (e.g., bicarbonate, sulfate, chloride, nitrate, phosphate, dissolved silicate, sodium, ammonium, potassium, magnesium, and calcium ions in a suburban river located in Jakarta, Indonesia. Carbonate, phosphate, and silicate ion concentrations were determined using ion-exclusion chromatography (IEC on a weakly acidic cation-exchange resin column (WCX in the H+-form with water eluent. Other ions were identified by ion-exclusion/cation-exchange chromatography (IEC/CEC on a WCX column with tartaric acid eluent. The use of IEC systems for water quality monitoring was advantageous for the following reasons: (1 the concentrations of analyte ions, except NO3− and silicate ions, increased from upstream to downstream; and (2 the speciation of inorganic nitrogen ions could be analyzed by single injection into the IEC/CEC. The IEC approach provided beneficial information for the construction of sewage treatment facilities in our study area. Results showed that (1 the analyte concentrations for samples obtained in the downstream area were higher than those in the upstream area owing to contamination by domestic sewage; (2 the concentrations of NO3− and NH4+ correlated with the concentration of dissolved oxygen; and (3 bicarbonate concentrations increased downstream, likely due to respiration of bacteria and dissolution of concrete under low-oxygen conditions.

  4. Quality evaluation of Hypericum ascyron extract by two-dimensional high-performance liquid chromatography coupled with the colorimetric 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide method.

    Science.gov (United States)

    Li, Xiu-Mei; Luo, Xue-Gang; Zhang, Chao-Zheng; Wang, Nan; Zhang, Tong-Cun

    2015-02-01

    In this paper, a heart-cutting two-dimensional high-performance liquid chromatography coupled with the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) method was established for controlling the quality of different batches of Hypericum ascyron extract for the first time. In comparison with the common one-dimensional fingerprint, the second-dimensional fingerprint compiled additional spectral data and was hence more informative. The quality of H. ascyron extract was further evaluated by similarity measures and the same results were achieved, the correlation coefficients of the similarity of ten batches of H. ascyron extract were >0.99. Furthermore, we also evaluated the quality of the ten batches of H. ascyron extract by antibacterial activity. The result demonstrated that the quality of the ten batches of H. ascyron extract was not significantly different by MTT. Finally, we demonstrated that the second-dimensional fingerprint coupled with the MTT method was a more powerful tool to characterize the quality of samples of batch to batch. Therefore the proposed method could be used to comprehensively conduct the quality control of traditional Chinese medicines. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Towards chemical profiling of ignitable liquids with comprehensive two-dimensional gas chromatography: Exploring forensic application to neat white spirits.

    Science.gov (United States)

    Sampat, Andjoe A S; Lopatka, Martin; Vivó-Truyols, Gabriel; Schoenmakers, Peter J; van Asten, Arian C

    2016-10-01

    The application of GC×GC-FID and GC×GC-MS for the chemical analysis and profiling of neat white spirit is explored and the benefit of the enhanced peak capacity offered by comprehensive two-dimensional gas chromatography is demonstrated. An extensive sampling exercise was conducted throughout The Netherlands and the production and logistics in terms of bottling and distribution of white spirits were studied. An exploratory approach based on target-peak tables and principal component analysis was employed to study the brand-to-brand differences and production variations over time. Despite the complex chemical composition of white spirit samples this study shows that chemical variation during productions is actually quite limited. Hence care has to be taken with the chemical comparison for forensic purposes. Although some clustering was noticed on brand level, the large scale production process leads to a very consistent composition across stores and brands. However, because of the broad specifications of this commodity product, substantial chemical variation was found over time. This temporal discrimination could be of forensic value when considering white spirits supplies in individual households. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  6. A two-dimensional kinetic model of the scrape-off layer

    International Nuclear Information System (INIS)

    Catto, P.J.; Hazeltine, R.D.

    1993-09-01

    A two-dimensional (radius and poloidal angle), analytically tractable kinetic model of the ion (or energetic electron) behavior in the scrape-off layer of a limiter or divertor plasma in a tokamak is presented. The model determines the boundary conditions on the core ion density and ion temperature gradients, the power load on the limiter or divertor plates, the energy carried per particle to the walls, and the effective flux limit. The self-consistent electrostatic potential in the quasi-neutral scrape-off layer is determined by using the ion kinetic model of the layer along with a Maxwell-Boltzmann electron response that occurs because most electrons are reflected by the Debye sheaths (assumed to be infinitely thin) at the limiter or divertor plates

  7. Use of extraction chromatography, ion chromatography and liquid scintillation spectrometry for rapid determination of strontium-89 and strontium-90 in food in cases of increased release of radionuclides

    International Nuclear Information System (INIS)

    Heilgeist, M.

    2000-01-01

    For rapid determination of 89 Sr and 90 Sr in food, isocratic ion chromatography used for Sr isolation and purification is integrated in a complete analytical system comprising sample preparation, incineration, dissolution, phosphate precipitation for alkali/alkaline earth separation, and Sr specific extraction chromatography on crown ether basis for Ca/Sr separation. Strontium-89 and 90 Sr are determined by liquid scintillation spectrometry after carbonate precipitation. The components of the mixed spectra obtained are calculated by the computerized spectra subtraction method. Two days plus measuring time are required for single, three for double analysis. The limit of detection for 89 Sr and 90 Sr is ca. 0.1 Bq x kg -1 , related to the fresh produce. (author)

  8. ONE-DIMENSIONAL AND TWO-DIMENSIONAL LEADERSHIP STYLES

    Directory of Open Access Journals (Sweden)

    Nikola Stefanović

    2007-06-01

    Full Text Available In order to motivate their group members to perform certain tasks, leaders use different leadership styles. These styles are based on leaders' backgrounds, knowledge, values, experiences, and expectations. The one-dimensional styles, used by many world leaders, are autocratic and democratic styles. These styles lie on the two opposite sides of the leadership spectrum. In order to precisely define the leadership styles on the spectrum between the autocratic leadership style and the democratic leadership style, leadership theory researchers use two dimensional matrices. The two-dimensional matrices define leadership styles on the basis of different parameters. By using these parameters, one can identify two-dimensional styles.

  9. Photo-switchable two-dimensional nanofluidic ionic diodes.

    Science.gov (United States)

    Wang, Lili; Feng, Yaping; Zhou, Yi; Jia, Meijuan; Wang, Guojie; Guo, Wei; Jiang, Lei

    2017-06-01

    The bottom-up assembly of ion-channel-mimetic nanofluidic devices and materials with two-dimensional (2D) nano-building blocks paves a straightforward way towards the real-world applications of the novel transport phenomena on a nano- or sub-nanoscale. One immediate challenge is to provide the 2D nanofluidic systems with adaptive responsibilities and asymmetric ion transport characteristics. Herein, we introduce a facile and general strategy to provide a graphene-oxide-based 2D nanofluidic system with photo-switchable ionic current rectification (ICR). The degree of ICR can be prominently enhanced upon UV irradiation and it can be perfectly retrieved under irradiation with visible light. A maximum ICR ratio of about 48 was achieved. The smart and functional nanofluidic devices have applications in energy conversion, chemical sensing, water treatment, etc .

  10. Determination of chlorine in graphite by combustion-ion chromatography

    International Nuclear Information System (INIS)

    Chen Lianzhong; Watanabe, Kazuo; Itoh, Mitsuo.

    1995-09-01

    A combustion/ion chromatographic method has been studied for the sensitive determination of chlorine in graphite. A graphite sample was burnt at 900degC in a silica reaction tube at an oxygen flow rate of 200 ml/min. Chlorine evolved was absorbed in 20 ml of a 0.1 mM sodium carbonate solution. The solution was evaporated to dryness. The residue was dissolved with a small volume of water. Chlorine in the solution was determined using ion chromatography. The method was applied to JAERI graphite certified reference materials and practical graphite materials. The detection limit was about 0.8 μgCl/g for a 2.0 g sample. The precision was about 2.5% (relative standard deviation) for samples with chlorine content of 70 μg/g level. The method is also usable for coal samples. (author)

  11. Use of a two-dimensional ionization chamber array for proton therapy beam quality assurance

    International Nuclear Information System (INIS)

    Arjomandy, Bijan; Sahoo, Narayan; Ding Xiaoning; Gillin, Michael

    2008-01-01

    Two-dimensional ion chamber arrays are primarily used for conventional and intensity modulated radiotherapy quality assurance. There is no commercial device of such type available on the market that is offered for proton therapy quality assurance. We have investigated suitability of the MatriXX, a commercial two-dimensional ion chamber array detector for proton therapy QA. This device is designed to be used for photon and electron therapy QA. The device is equipped with 32x32 parallel plate ion chambers, each with 4.5 mm diam and 7.62 mm center-to-center separation. A 250 MeV proton beam was used to calibrate the dose measured by this device. The water equivalent thickness of the buildup material was determined to be 3.9 mm using a 160 MeV proton beam. Proton beams of different energies were used to measure the reproducibility of dose output and to evaluate the consistency in the beam flatness and symmetry measured by MatriXX. The output measurement results were compared with the clinical commissioning beam data that were obtained using a 0.6 cc Farmer chamber. The agreement was consistently found to be within 1%. The profiles were compared with film dosimetry and also with ion chamber data in water with an excellent agreement. The device is found to be well suited for quality assurance of proton therapy beams. It provides fast two-dimensional dose distribution information in real time with the accuracy comparable to that of ion chamber measurements and film dosimetry

  12. POLAR ORGANIC CHEMICAL INTEGRATIVE SAMPLING AND LIQUID CHROMATOGRAPHY-ELECTROSPRAY/ION-TRAP MASS SPECTROMETRY FOR ASSESSING SELECTED PRESCRIPTION AND ILLICIT DRUGS IN TREATED SEWAGE EFFLUENTS

    Science.gov (United States)

    The purpose of the research presented in this paper is two-fold: (1) to demonstrate the 4 coupling of two state-of-the-art techniques: a time-weighted polar organic integrative sampler (POCIS) and micro-liquid chromatography-electrospray/ion trap mass spectrometry (u-LC-6 ES/ITMS...

  13. Protein composition of wheat gluten polymer fractions determined by quantitative two-dimensional gel electrophoresis and tandem mass spectrometry

    Science.gov (United States)

    Flour proteins from the US bread wheat Butte 86 were extracted in 0.5% SDS using a two-step procedure with and without sonication and further separated by size exclusion chromatography into monomeric and polymeric fractions. Proteins in each fraction were analyzed by quantitative two-dimensional gel...

  14. Active Solvent Modulation: A Valve-Based Approach To Improve Separation Compatibility in Two-Dimensional Liquid Chromatography.

    Science.gov (United States)

    Stoll, Dwight R; Shoykhet, Konstantin; Petersson, Patrik; Buckenmaier, Stephan

    2017-09-05

    Two-dimensional liquid chromatography (2D-LC) is increasingly being viewed as a viable tool for solving difficult separation problems, ranging from targeted separations of structurally similar molecules to untargeted separations of highly complex mixtures. In spite of this performance potential, though, many users find method development challenging and most frequently cite the "incompatibility" between the solvent systems used in the first and second dimensions as a major obstacle. This solvent strength related incompatibility can lead to severe peak distortion and loss of resolution and sensitivity in the second dimension. In this paper, we describe a novel approach to address the incompatibility problem, which we refer to as Active Solvent Modulation (ASM). This valve-based approach enables dilution of 1 D effluent with weak solvent prior to transfer to the 2 D column but without the need for additional instrument hardware. ASM is related to the concept we refer to as Fixed Solvent Modulation (FSM), with the important difference being that ASM allows toggling of the diluent stream during each 2 D separation cycle. In this work, we show that ASM eliminates the major drawbacks of FSM including complex elution solvent profiles, baseline disturbances, and slow 2 D re-equilibration and demonstrate improvements in 2 D separation quality using both simple small molecule probes and degradants of heat-treated bovine insulin as case studies. We believe that ASM will significantly ease method development for 2D-LC, providing a path to practical methods that involve both highly complementary 1 D and 2 D separations and sensitive detection.

  15. Organophosphorus pesticide and ester analysis by using comprehensive two-dimensional gas chromatography with flame photometric detection.

    Science.gov (United States)

    Liu, Xiangping; Li, Dengkun; Li, Jiequan; Rose, Gavin; Marriott, Philip J

    2013-12-15

    Thirty-seven phosphorus (P)-containing compounds comprising organophosphorus pesticides and organophosphate esters were analyzed by using comprehensive two-dimensional gas chromatography with flame photometric detection in P mode (GC × GC-FPD(P)), with a non-polar/moderately polar column set. A suitable modulation temperature and period was chosen based on experimental observation. A number of co-eluting peak pairs on the (1)D column were well separated in 2D space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC × GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021-0.048 μmol L(-1), and linear calibration correlation coefficients (R(2)) for all 37 P-compounds were at least 0.998. The P-compounds were spiked in 2% diesel and good reproducibility for their response areas and retention times was obtained. Spiked recoveries were 88%-157% for 5 μg L(-1) and 80%-138% for 10 μg L(-1) spiked levels. Both (1)tR and (2)tR shifts were noted when the content of diesel was in excess of 5% in the matrix. Soil samples were analyzed by using the developed method; some P-compounds were positively detected. In general, this study shows that GC × GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Multiple heart-cutting two dimensional liquid chromatography quadrupole time-of-flight mass spectrometry of pyrrolizidine alkaloids.

    Science.gov (United States)

    van de Schans, Milou G M; Blokland, Marco H; Zoontjes, Paul W; Mulder, Patrick P J; Nielen, Michel W F

    2017-06-23

    Pyrrolizidine alkaloids (PAs) and their and the corresponding N-oxides (PAs-ox) are genotoxic plant metabolites which can be present as unwanted contaminants in food products of herbal origin like tea and food supplements. PAs and PAs-ox come in a wide variety of molecular structures including many structural isomers. For toxicity assessment it is important to determine the composition of a sample and to resolve all isomeric PAs and PAs-ox, which is currently not possible in one liquid or gas chromatographic (LC or GC) run. In this study an online two dimensional liquid chromatography quadrupole time-of-flight mass spectrometry (2D-LC QToF-MS) method was developed to resolve isomeric PAs and PAs-ox. After comprehensive column and mobile phase selection a polar endcapped C 18 column was used at pH 3 in the first dimension, and a cross-linked C 18 column at pH 10 in the second dimension. Injection solvents, column IDs, flow rates and temperatures were carefully optimized. The method with column selection valve switching described in this study was able to resolve and visualize 20 individual PAs/PAs-ox (6 sets of isomers) in one 2D-LC QToF-MS run. Moreover, it was shown that all isomeric PAs/PAs-ox could be unambiguously annotated. The method was shown to be applicable for the determination and quantification of isomeric PAs/PAs-ox in plant extracts and could be easily extended to include other PAs and PAs-ox. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Comprehensive two-dimensional liquid chromatography–time-of-flight mass spectrometry in the analysis of acidic compounds in atmospheric aerosols

    Czech Academy of Sciences Publication Activity Database

    Pól, Jaroslav; Hohnová, B.; Jussila, M.; Hyötyläinen, T.

    2006-01-01

    Roč. 1130, č. 1 (2006), s. 64-71 ISSN 0021-9673. [International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers /9./. York, 08.02.2006-10.02.2006] Institutional research plan: CEZ:AV0Z40310501 Keywords : comprehensive two-dimensional liquid chromatography * time-of-flight mass spectrometry * atmospheric aerosol analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.554, year: 2006

  18. Two-Dimensional Spectroscopy Is Being Used to Address Core Scientific Questions in Biology and Materials Science.

    Science.gov (United States)

    Petti, Megan K; Lomont, Justin P; Maj, Michał; Zanni, Martin T

    2018-02-15

    Two-dimensional spectroscopy is a powerful tool for extracting structural and dynamic information from a wide range of chemical systems. We provide a brief overview of the ways in which two-dimensional visible and infrared spectroscopies are being applied to elucidate fundamental details of important processes in biological and materials science. The topics covered include amyloid proteins, photosynthetic complexes, ion channels, photovoltaics, batteries, as well as a variety of promising new methods in two-dimensional spectroscopy.

  19. [Determination of acetanilide herbicide residues in tea by gas chromatography-mass spectrometry with two different ionization techniques].

    Science.gov (United States)

    Shen, Weijian; Xu, Jinzhong; Yang, Wenquan; Shen, Chongyu; Zhao, Zengyun; Ding, Tao; Wu, Bin

    2007-09-01

    An analytical method of solid phase extraction-gas chromatography-mass spectrometry with two different ionization techniques was established for simultaneous determination of 12 acetanilide herbicide residues in tea-leaves. Herbicides were extracted from tea-leaf samples with ethyl acetate. The extract was cleaned-up on an active carbon SPE column connected to a Florisil SPE column. Analytical screening was determined by the technique of gas chromatography (GC)-mass spectrometry (MS) in the selected ion monitoring (SIM) mode with either electron impact ionization (EI) or negative chemical ionization (NCI). It is reliable and stable that the recoveries of all herbicides were in the range from 50% to 110% at three spiked levels, 10 microg/kg, 20 microg/kg and 40 microg/kg, and the relative standard deviations (RSDs) were no more than 10.9%. The two different ionization techniques are complementary as more ion fragmentation information can be obtained from the EI mode while more molecular ion information from the NCI mode. By comparison of the two techniques, the selectivity of NCI-SIM was much better than that of EI-SIM method. The sensitivities of the both techniques were high, the limit of quantitative (LOQ) for each herbicide was no more than 2.0 microg/kg, and the limit of detection (LOD) with NCI-SIM technique was much lower than that of EI-SIM when analyzing herbicides with several halogen atoms in the molecule.

  20. Two-dimensional heterostructures for energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Gogotsi, Yury G. [Drexel Univ., Philadelphia, PA (United States); Pomerantseva, Ekaterina [Drexel Univ., Philadelphia, PA (United States)

    2017-06-12

    Two-dimensional (2D) materials provide slit-shaped ion diffusion channels that enable fast movement of lithium and other ions. However, electronic conductivity, the number of intercalation sites, and stability during extended cycling are also crucial for building high-performance energy storage devices. While individual 2D materials, such as graphene, show some of the required properties, none of them can offer all properties needed to maximize energy density, power density, and cycle life. Here we argue that stacking different 2D materials into heterostructured architectures opens an opportunity to construct electrodes that would combine the advantages of the individual building blocks while eliminating the associated shortcomings. We discuss characteristics of common 2D materials and provide examples of 2D heterostructured electrodes that showed new phenomena leading to superior electrochemical performance. As a result, we also consider electrode fabrication approaches and finally outline future steps to create 2D heterostructured electrodes that could greatly expand current energy storage technologies.

  1. Two-dimensional NMR spectrometry

    International Nuclear Information System (INIS)

    Farrar, T.C.

    1987-01-01

    This article is the second in a two-part series. In part one (ANALYTICAL CHEMISTRY, May 15) the authors discussed one-dimensional nuclear magnetic resonance (NMR) spectra and some relatively advanced nuclear spin gymnastics experiments that provide a capability for selective sensitivity enhancements. In this article and overview and some applications of two-dimensional NMR experiments are presented. These powerful experiments are important complements to the one-dimensional experiments. As in the more sophisticated one-dimensional experiments, the two-dimensional experiments involve three distinct time periods: a preparation period, t 0 ; an evolution period, t 1 ; and a detection period, t 2

  2. Ion chromatography for the precise analysis of chloride and sodium in sweat for the diagnosis of cystic fibrosis

    NARCIS (Netherlands)

    Doorn, J.; Storteboom, T. T. R.; Mulder, A. M.; de Jong, W. H. A.; Rottier, B. L.; Kema, I. P.

    BACKGROUND: Measurement of chloride in sweat is an essential part of the diagnostic algorithm for cystic fibrosis. The lack in sensitivity and reproducibility of current methods led us to develop an ion chromatography/high-performance liquid chromatography (IC/HPLC) method, suitable for the analysis

  3. The determination of cyanide in hydrometallurgical process solutions and effluents by ion chromatography

    International Nuclear Information System (INIS)

    Pohlandt, C.

    1984-01-01

    Three methods are described for the determination of cyanide species in hydrometallurgical process solutions and in effluents. The determination of excess cyanide in the presence of weak metal cyanide complexes was achieved by the use of a flow-injection system with 0,05mM sodium chloride as the carrier stream. The procedure was found to be fast, precise (S(sub r)0,0142), and reasonably accurate. Free cyanide and cyanide derived from weak metal cyanide complexes were determined by ion chromatography. This method is free from interferences and precise (s(sub r)0,0112), and has a limit of determination of 10μg0l. The 'total' cyanide content of solutions was determined by ion chromatography after the strong metal cyanide complexes had been dissociated in hypophosphorous acid by ultraviolet irradiation. The procedure (of 10 minutes duration) is faster than conventional distillation methods, and is accurate and precise (S(sub r)0,027)

  4. Determination of sulphite in wines using suppressed ion chromatography.

    Science.gov (United States)

    Yoshikawa, Kenji; Uekusa, Yuki; Sakuragawa, Akio

    2015-05-01

    Suppressed ion chromatography with the use of a conductivity detector was developed for the determination of sulphite ions in wine samples. When a mixed solution of sodium carbonate, sodium bicarbonate, and acetone was used as the mobile phase, simultaneous determination of eight inorganic anions (i.e., fluoride, chloride, nitrite, nitrate, sulphite, phosphate, sulphate, and thiosulphate) was completed in approximately 25 min. Linearity, reproducibility, and detection limits were determined for the proposed method. In the case of sulphite detection, a linear calibration curve with a good correlation coefficient of 0.9992 was obtained from the peak height of sulphite with a relative standard deviation (n = 6) 1.48%. In addition, the detection limit of sulphite was 0.27 mg/L at a signal-to-noise ratio of 3. Further, the developed method was applied for the determination of sulphite contained in several wine samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  5. Two dimensional simulation of ion beam-plasm interaction | Echi ...

    African Journals Online (AJOL)

    Hybrid plasma simulation is a model in which different components of the plasma are treated differently. In this work the ions are treated as particles while the electrons are treated as a neutralizing background fluid through which electric signals may propagate. Deuterium ion beams incident on the tritium plasma interact ...

  6. Buneman and ion two-stream instabilities in the foot of collisionless shocks

    International Nuclear Information System (INIS)

    Fumio Takahara

    2008-01-01

    Two-dimensional electrostatic PIC simulations as well as linear analysis have been made for double periodic boundary conditions mimicking the shock foot region of supernova remnants. We found that modes propagating obliquely to the beam direction grow fast enough so that no surfing acceleration occurs. We also found that a new type of instability called ion two-stream instability is excited after the Buneman instability saturated instead of the ion acoustic instability. Implications for electron heating are shortly discussed. (author)

  7. Simultaneous quantitative analysis of metabolites using ion-pair liquid chromatography-electrospray ionization mass spectrometry

    NARCIS (Netherlands)

    Coulier, L.; Bas, R.; Jespersen, S.; Verheij, E.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    We have developed an analytical method, consisting of ion-pair liquid chromatography coupled to electrospray ionization mass spectrometry (IP-LC-ESI-MS), for the simultaneous quantitative analysis of several key classes of polar metabolites, like nucleotides, coenzyme A esters, sugar nucleotides,

  8. Web Server for Peak Detection, Baseline Correction, and Alignment in Two-Dimensional Gas Chromatography Mass Spectrometry-Based Metabolomics Data.

    Science.gov (United States)

    Tian, Tze-Feng; Wang, San-Yuan; Kuo, Tien-Chueh; Tan, Cheng-En; Chen, Guan-Yuan; Kuo, Ching-Hua; Chen, Chi-Hsin Sally; Chan, Chang-Chuan; Lin, Olivia A; Tseng, Y Jane

    2016-11-01

    Two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC/TOF-MS) is superior for chromatographic separation and provides great sensitivity for complex biological fluid analysis in metabolomics. However, GC×GC/TOF-MS data processing is currently limited to vendor software and typically requires several preprocessing steps. In this work, we implement a web-based platform, which we call GC 2 MS, to facilitate the application of recent advances in GC×GC/TOF-MS, especially for metabolomics studies. The core processing workflow of GC 2 MS consists of blob/peak detection, baseline correction, and blob alignment. GC 2 MS treats GC×GC/TOF-MS data as pictures and clusters the pixels as blobs according to the brightness of each pixel to generate a blob table. GC 2 MS then aligns the blobs of two GC×GC/TOF-MS data sets according to their distance and similarity. The blob distance and similarity are the Euclidean distance of the first and second retention times of two blobs and the Pearson's correlation coefficient of the two mass spectra, respectively. GC 2 MS also directly corrects the raw data baseline. The analytical performance of GC 2 MS was evaluated using GC×GC/TOF-MS data sets of Angelica sinensis compounds acquired under different experimental conditions and of human plasma samples. The results show that GC 2 MS is an easy-to-use tool for detecting peaks and correcting baselines, and GC 2 MS is able to align GC×GC/TOF-MS data sets acquired under different experimental conditions. GC 2 MS is freely accessible at http://gc2ms.web.cmdm.tw .

  9. Tile-based Fisher-ratio software for improved feature selection analysis of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry data.

    Science.gov (United States)

    Marney, Luke C; Siegler, W Christopher; Parsons, Brendon A; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

    2013-10-15

    Comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a highly capable instrumental platform that produces complex and information-rich multi-dimensional chemical data. The data can be initially overwhelming, especially when many samples (of various sample classes) are analyzed with multiple injections for each sample. Thus, the data must be analyzed in such a way as to extract the most meaningful information. The pixel-based and peak table-based Fisher ratio algorithmic approaches have been used successfully in the past to reduce the multi-dimensional data down to those chemical compounds that are changing between the sample classes relative to those that are not changing (i.e., chemical feature selection). We report on the initial development of a computationally fast novel tile-based Fisher-ratio software that addresses the challenges due to 2D retention time misalignment without explicitly aligning the data, which is often a shortcoming for both pixel-based and peak table-based algorithmic approaches. Concurrently, the tile-based Fisher-ratio algorithm significantly improves the sensitivity contrast of true positives against a background of potential false positives and noise. In this study, eight compounds, plus one internal standard, were spiked into diesel at various concentrations. The tile-based F-ratio algorithmic approach was able to "discover" all spiked analytes, within the complex diesel sample matrix with thousands of potential false positives, in each possible concentration comparison, even at the lowest absolute spiked analyte concentration ratio of 1.06, the ratio between the concentrations in the spiked diesel sample to the native concentration in diesel. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Screening of oil sources by using comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry and multivariate statistical analysis.

    Science.gov (United States)

    Zhang, Wanfeng; Zhu, Shukui; He, Sheng; Wang, Yanxin

    2015-02-06

    Using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/TOFMS), volatile and semi-volatile organic compounds in crude oil samples from different reservoirs or regions were analyzed for the development of a molecular fingerprint database. Based on the GC×GC/TOFMS fingerprints of crude oils, principal component analysis (PCA) and cluster analysis were used to distinguish the oil sources and find biomarkers. As a supervised technique, the geological characteristics of crude oils, including thermal maturity, sedimentary environment etc., are assigned to the principal components. The results show that tri-aromatic steroid (TAS) series are the suitable marker compounds in crude oils for the oil screening, and the relative abundances of individual TAS compounds have excellent correlation with oil sources. In order to correct the effects of some other external factors except oil sources, the variables were defined as the content ratio of some target compounds and 13 parameters were proposed for the screening of oil sources. With the developed model, the crude oils were easily discriminated, and the result is in good agreement with the practical geological setting. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Proton transfer through hydrogen bonds in two-dimensional water layers: A theoretical study based on ab initio and quantum-classical simulations

    International Nuclear Information System (INIS)

    Bankura, Arindam; Chandra, Amalendu

    2015-01-01

    The dynamics of proton transfer (PT) through hydrogen bonds in a two-dimensional water layer confined between two graphene sheets at room temperature are investigated through ab initio and quantum-classical simulations. The excess proton is found to be mostly solvated as an Eigen cation where the hydronium ion donates three hydrogen bonds to the neighboring water molecules. In the solvation shell of the hydronium ion, the three coordinated water molecules with two donor hydrogen bonds are found to be properly presolvated to accept a proton. Although no hydrogen bond needs to be broken for transfer of a proton to such presolvated water molecules from the hydronium ion, the PT rate is still found to be not as fast as it is for one-dimensional chains. Here, the PT is slowed down as the probability of finding a water with two donor hydrogen bonds in the solvation shell of the hydronium ion is found to be only 25%-30%. The hydroxide ion is found to be solvated mainly as a complex anion where it accepts four H-bonds through its oxygen atom and the hydrogen atom of the hydroxide ion remains free all the time. Here, the presolvation of the hydroxide ion to accept a proton requires that one of its hydrogen bonds is broken and the proton comes from a neighboring water molecule with two acceptor and one donor hydrogen bonds. The coordination number reduction by breaking of a hydrogen bond is a slow process, and also the population of water molecules with two acceptor and one donor hydrogen bonds is only 20%-25% of the total number of water molecules. All these factors together tend to slow down the hydroxide ion migration rate in two-dimensional water layers compared to that in three-dimensional bulk water

  12. The use of ion chromatography for the determination of impurities in crude phosphoric acid

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Atalla, L.T.; Abrao, A.

    1988-07-01

    The determination of fluoride, nitrate, sulphate and phosphate ions in crude phosphoric acid by means of ion chromatography is described. A previous separation of interferent cations was made by using a cationic resin or EDTA complexation. The last alternative allowed more reproductible results. The technique described is very quick and is being applied for the simultaneous determination of impurities in phosphoric acid and its own phosphospate concentration. The method is quick and has good reprodutibility. (author) [pt

  13. Simulation study of two-ion hybrid resonance heating

    International Nuclear Information System (INIS)

    Riyopoulos, S.; Tajima, T.

    1986-02-01

    A one-dimensional low-noise, low-frequency electromagnetic particle simulation code that is appropriate for investigation of ion cyclotron resonance heating (ICRH) is developed. Retaining the hyperbolicity of the electromagnetic waves and exploiting nearly one-dimensional characteristics (perpendicular to the external magnetic field) of the ICRH, we use the guiding center electron approximation for the transverse electronic current calculation. We observe mode conversion of the incoming magnetosonic wave into the electrostatic ion-ion hybrid mode accompanied by strong ion-heating. The dependence of this heating on the different plasma parameters is examined through a series of simulations, focusing mainly on wave incidence from the high field side. Because K/sub parallel/ = 0 in our runs, the conventional Landau damping cannot explain the ion heating. Non-linear mechanisms for energy transfer are discussed. Our numerical results demonstrate the importance of the non-linear wave particle interaction for energy transfer are discussed. Our numerical results demonstrate the importance of the non-linear wave particle interaction for energy absorption during radio frequency heating in the ion cyclotron regime. 32 refs., 17 figs

  14. Two-dimensional model of a freely expanding plasma

    International Nuclear Information System (INIS)

    Khalid, Q.

    1975-01-01

    The free expansion of an initially confined plasma is studied by the computer experiment technique. The research is an extension to two dimensions of earlier work on the free expansion of a collisionless plasma in one dimension. In the two-dimensional rod model, developed in this research, the plasma particles, electrons and ions are modeled as infinitely long line charges or rods. The line charges move freely in two dimensions normal to their parallel axes, subject only to a self-consistent electric field. Two approximations, the grid approximation and the periodic boundary condition are made in order to reduce the computation time. In the grid approximation, the space occupied by the plasma at a given time is divided into boxes. The particles are subject to an average electric field calculated for that box assuming that the total charge within each box is located at the center of the box. However, the motion of each particle is exactly followed. The periodic boundary condition allows us to consider only one-fourth of the total number of particles of the plasma, representing the remaining three-fourths of the particles as symmetrically placed images of those whose positions are calculated. This approximation follows from the expected azimuthal symmetry of the plasma. The dynamics of the expansion are analyzed in terms of average ion and electron positions, average velocities, oscillation frequencies and relative distribution of energy between thermal, flow and electric field energies. Comparison is made with previous calculations of one-dimensional models which employed plane, spherical or cylindrical sheets as charged particles. In order to analyze the effect of the grid approximation, the model is solved for two different grid sizes and for each grid size the plasma dynamics is determined. For the initial phase of expansion, the agreement for the two grid sizes is found to be good

  15. A new computationally-efficient two-dimensional model for boron implantation into single-crystal silicon

    International Nuclear Information System (INIS)

    Klein, K.M.; Park, C.; Yang, S.; Morris, S.; Do, V.; Tasch, F.

    1992-01-01

    We have developed a new computationally-efficient two-dimensional model for boron implantation into single-crystal silicon. This paper reports that this new model is based on the dual Pearson semi-empirical implant depth profile model and the UT-MARLOWE Monte Carlo boron ion implantation model. This new model can predict with very high computational efficiency two-dimensional as-implanted boron profiles as a function of energy, dose, tilt angle, rotation angle, masking edge orientation, and masking edge thickness

  16. Hyphenated techniques in multidimensional gas chromatography for analysis of wine aroma and related odorants

    OpenAIRE

    Chin, Sung Tong

    2017-01-01

    The advent of analytical multidimensional gas chromatography (MDGC) techniques, with recent development in comprehensive two-dimensional gas chromatography (GC×GC) as well as microfluidic technology in conventional heart-cut MDGC, has achieved excellent separation efficiency for advanced characterization of complex volatile and semi-volatile samples, which is unlikely to be accomplished by single dimensional chromatography. This dissertation work has highlighted the potential opportunities fo...

  17. Application of linear pH gradients for the modeling of ion exchange chromatography: Separation of monoclonal antibody monomer from aggregates.

    Science.gov (United States)

    Kluters, Simon; Wittkopp, Felix; Jöhnck, Matthias; Frech, Christian

    2016-02-01

    The mobile phase pH is a key parameter of every ion exchange chromatography process. However, mechanistic insights into the pH influence on the ion exchange chromatography equilibrium are rare. This work describes a mechanistic model capturing salt and pH influence in ion exchange chromatography. The pH dependence of the characteristic protein charge and the equilibrium constant is introduced to the steric mass action model based on a protein net charge model considering the number of amino acids interacting with the stationary phase. This allows the description of the adsorption equilibrium of the chromatographed proteins as a function of pH. The model parameters were determined for a monoclonal antibody monomer, dimer, and a higher aggregated species based on a manageable set of pH gradient experiments. Without further modification of the model parameters the transfer to salt gradient elution at fixed pH is demonstrated. A lumped rate model was used to predict the separation of the monoclonal antibody monomer/aggregate mixture in pH gradient elution and for a pH step elution procedure-also at increased protein loadings up to 48 g/L packed resin. The presented model combines both salt and pH influence and may be useful for the development and deeper understanding of an ion exchange chromatography separation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Bovine plasma protein fractionation by ion exchange chromatography.

    Science.gov (United States)

    Moure, F; Rendueles, M; Díaz, M

    2004-12-01

    An ion exchange chromatography process was developed to separate the main protein fractions of bovine blood plasma using a composite material, Q-HyperD resin, and a gel material, DEAE-Sepharose. The experiments were carried out at semipreparative scale. It was necessary to establish analytical methods of electrophoresis and HPLC to identify the fractionated proteins. Results show that these materials are able to adequately fractionate different protein groups from the raw blood plasma. This method may be used to avoid chemical fractionation using agents such as ethanol or PEG and, thus, decrease protein denaturation of the different fractions to be used for research or pharmaceutical purposes. The Q-HyperD resin presents a better retention capacity for plasma protein than DEAE-Sepharose under the experimental conditions employed.

  19. Evolution of potent odorants within the volatile metabolome of high-quality hazelnuts (Corylus avellana L.): evaluation by comprehensive two-dimensional gas chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Rosso, Marta Cialiè; Liberto, Erica; Spigolon, Nicola; Fontana, Mauro; Somenzi, Marco; Bicchi, Carlo; Cordero, Chiara

    2018-01-09

    Within the pattern of volatiles released by food products (volatilome), potent odorants are bio-active compounds that trigger aroma perception by activating a complex array of odor receptors (ORs) in the regio olfactoria. Their informative role is fundamental to select optimal post-harvest and storage conditions and preserve food sensory quality. This study addresses the volatile metabolome from high-quality hazelnuts (Corylus avellana L.) from the Ordu region (Turkey) and Tonda Romana from Italy, and investigates its evolution throughout the production chain (post-harvest, industrial storage, roasting) to find functional correlations between technological strategies and product quality. The volatile metabolome is analyzed by headspace solid-phase microextration combined with comprehensive two-dimensional gas chromatography and mass spectrometry. Dedicated pattern recognition, based on 2D data (targeted fingerprinting), is used to mine analytical outputs, while principal component analysis (PCA), Fisher ratio, hierarchical clustering, and analysis of variance are used to find decision makers among the most informative chemicals. Low-temperature drying (18-20 °C) has a decisive effect on quality; it correlates negatively with bacteria and mold metabolic activity, nut viability, and lipid oxidation products (2-methyl-1-propanol, 3-methyl-1-butanol, 2-ethyl-1-hexanol, 2-octanol, 1-octen-3-ol, hexanal, octanal and (E)-2-heptanal). Protective atmosphere storage (99% N 2 -1% O 2 ) effectively limits lipid oxidation for 9-12 months after nut harvest. The combination of optimal drying and storage preserves the aroma potential; after roasting at different shelf-lives, key odorants responsible for malty and buttery (2- and 3-methylbutanal, 2,3-butanedione and 2,3-pentanedione), earthy (methylpyrazine, 2-ethyl-5-methyl pyrazine and 3-ethyl-2,5-dimethyl pyrazine) and caramel-like and musty notes (2,5-dimethyl-4-hydroxy-3(2H)-furanone - furaneol and acetyl pyrrole) show no

  20. Chromatography of phosphorus oxoacids

    International Nuclear Information System (INIS)

    Ohashi, S.

    1975-01-01

    The present state of studies on the chromatographic separation of phosphorus oxoacids is surveyed. In this paper, chromatographic techniques are divided into four groups, i.e. paper and thin-layer chromatography, paper electrophoresis, ion-exchange chromatography, and gel chromatography. The separation mechanisms and characteristics for these chromatographic methods are discussed and some examples for the separation of phosphorus oxoacids are described. As examples of the application of ion-exchange and gel chromatography, studies on the hot atom chemistry of 32 P in solid inorganic phosphates and those on the substitution reactions between diphosphonate (diphosphite) and polyphosphates are reported. (author)

  1. Application of ion chromatography in the analysis of metals

    International Nuclear Information System (INIS)

    Doepke, T.; Braun, N.; Wuensch, G.

    1992-01-01

    Methods for the determination of chloride in molybdenum, tungsten, niobium and tantalum and of phosphorus in molybdenum and tungsten are presented. After oxidative digestion the analytes are separated from the matrix and accumulated in a small volume of liquid. Unsuppressed ion chromatography serves as the final determination method. The trace-matrix-separation and enrichment of chloride is largely independent of the kind of matrix. The procedure is therefore also applicable to concentrated solutions of various salts. A closed system ensures chloride blanks around 0.2 ppm and detection limits in the higher ppb range. A modification allows an enrichment of bromide and the simultaneous determination of chloride and bromide. (orig.) [de

  2. Illicit Drug Analysis Using Two-Dimension Liquid Chromatography/Tandem Mass Spectrometry.

    Science.gov (United States)

    Mallet, Claude; Botch-Jones, Sabra

    2016-10-01

    For the identification of illicit drugs in forensic toxicological casework, analysis can be delayed and potentially compromised due to lengthy sample preparation techniques. For a complete forensic identification, a robust methodology is required and the current trend in forensic laboratories is the use of liquid chromatography coupled to mass spectrometry (LC/MS or LC/MS-MS). However, to achieve satisfactory results, extensive and time-consuming sample preparation protocols are required to reach sub-ng/mL levels. The concept of sequential 2D extraction was designed to capture the retention behavior of a target analyte in response to various extraction parameters. Therefore, optimized conditions can be selected to excise a region of interest during extraction. The utilization of multi-dimensional chromatography combined with a micro-extraction technique was evaluated to decrease sample preparation time while enhancing the separation integrity observed with current single-dimensional chromatography techniques. A wide range of illicit drugs were spiked in human urine and extracted using three extraction protocols for performance evaluation. The extraction process was performed using a reversed-phase solid phase extraction (SPE) in 1D, 2D-optimized, 2D-sequential and cumulative elution modes. The chosen 2D chromatography conditions that were used in this application were identified using a 6 × 6 automated methods development protocol (144 methods total). The extraction of urine samples containing target analytes was completed in less than 20 min. The analysis was performed using 200 µL of the final organic solvent (MeOH) extracts. The limit of detection for all drugs was measured at 100 pg/mL (ppt) from a 1 mL sample volume. Several analytes showed excellent signal at 10 pg/mL (ppt). © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  3. Highly ordered three-dimensional macroporous carbon spheres for determination of heavy metal ions

    International Nuclear Information System (INIS)

    Zhang, Yuxiao; Zhang, Jianming; Liu, Yang; Huang, Hui; Kang, Zhenhui

    2012-01-01

    Highlights: ► Highly ordered three dimensional macroporous carbon spheres (MPCSs) were prepared. ► MPCS was covalently modified by cysteine (MPCS–CO–Cys). ► MPCS–CO–Cys was first time used in electrochemical detection of heavy metal ions. ► Heavy metal ions such as Pb 2+ and Cd 2+ can be simultaneously determined. -- Abstract: An effective voltammetric method for detection of trace heavy metal ions using chemically modified highly ordered three dimensional macroporous carbon spheres electrode surfaces is described. The highly ordered three dimensional macroporous carbon spheres were prepared by carbonization of glucose in silica crystal bead template, followed by removal of the template. The highly ordered three dimensional macroporous carbon spheres were covalently modified by cysteine, an amino acid with high affinities towards some heavy metals. The materials were characterized by physical adsorption of nitrogen, scanning electron microscopy, and transmission electron microscopy techniques. While the Fourier-transform infrared spectroscopy was used to characterize the functional groups on the surface of carbon spheres. High sensitivity was exhibited when this material was used in electrochemical detection (square wave anodic stripping voltammetry) of heavy metal ions due to the porous structure. And the potential application for simultaneous detection of heavy metal ions was also investigated.

  4. A one-dimensional collisional model for plasma-immersion ion implantation

    International Nuclear Information System (INIS)

    Vahedi, V.; Lieberman, M.A.; Alves, M.V.; Verboncoeur, J.P.; Birdsall, C.K.

    1991-01-01

    Plasma-immersion ion implantation (also known as plasma-source ion implantation) is a process in which a target is immersed in a plasma and a series of large negative-voltage pulses are applied to it to extract ions from the plasma and implant them into the target. A general one-dimensional model is developed to study this process in different coordinate systems for the case in which the pressure of the neutral gas is large enough that the ion motion in the sheath can be assumed to be highly collisional

  5. Enhanced Characterization of the Smell of Death by Comprehensive Two-Dimensional Gas Chromatography-Time-of-Flight Mass Spectrometry (GCxGC-TOFMS)

    Science.gov (United States)

    Dekeirsschieter, Jessica; Stefanuto, Pierre-Hugues; Brasseur, Catherine; Haubruge, Eric; Focant, Jean-François

    2012-01-01

    Soon after death, the decay process of mammalian soft tissues begins and leads to the release of cadaveric volatile compounds in the surrounding environment. The study of postmortem decomposition products is an emerging field of study in forensic science. However, a better knowledge of the smell of death and its volatile constituents may have many applications in forensic sciences. Domestic pigs are the most widely used human body analogues in forensic experiments, mainly due to ethical restrictions. Indeed, decomposition trials on human corpses are restricted in many countries worldwide. This article reports on the use of comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOFMS) for thanatochemistry applications. A total of 832 VOCs released by a decaying pig carcass in terrestrial ecosystem, i.e. a forest biotope, were identified by GCxGC-TOFMS. These postmortem compounds belong to many kinds of chemical class, mainly oxygen compounds (alcohols, acids, ketones, aldehydes, esters), sulfur and nitrogen compounds, aromatic compounds such as phenolic molecules and hydrocarbons. The use of GCxGC-TOFMS in study of postmortem volatile compounds instead of conventional GC-MS was successful. PMID:22723918

  6. Enhanced characterization of the smell of death by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GCxGC-TOFMS.

    Directory of Open Access Journals (Sweden)

    Jessica Dekeirsschieter

    Full Text Available Soon after death, the decay process of mammalian soft tissues begins and leads to the release of cadaveric volatile compounds in the surrounding environment. The study of postmortem decomposition products is an emerging field of study in forensic science. However, a better knowledge of the smell of death and its volatile constituents may have many applications in forensic sciences. Domestic pigs are the most widely used human body analogues in forensic experiments, mainly due to ethical restrictions. Indeed, decomposition trials on human corpses are restricted in many countries worldwide. This article reports on the use of comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOFMS for thanatochemistry applications. A total of 832 VOCs released by a decaying pig carcass in terrestrial ecosystem, i.e. a forest biotope, were identified by GCxGC-TOFMS. These postmortem compounds belong to many kinds of chemical class, mainly oxygen compounds (alcohols, acids, ketones, aldehydes, esters, sulfur and nitrogen compounds, aromatic compounds such as phenolic molecules and hydrocarbons. The use of GCxGC-TOFMS in study of postmortem volatile compounds instead of conventional GC-MS was successful.

  7. Evaluation of a novel helium ionization detector within the context of (low-)flow modulation comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Franchina, Flavio A; Maimone, Mariarosa; Sciarrone, Danilo; Purcaro, Giorgia; Tranchida, Peter Q; Mondello, Luigi

    2015-07-10

    The present research is focused on the use and evaluation of a novel helium ionization detector, defined as barrier discharge ionization detector (BID), within the context of (low-)flow modulation comprehensive two-dimensional gas chromatography (FM GC×GC). The performance of the BID device was compared to that of a flame ionization detector (FID), under similar FM GC×GC conditions. Following development and optimization of the FM GC×GC method, the BID was subjected to fine tuning in relation to acquisition frequency and discharge flow. Moreover, the BID performance was measured and compared to that of the FID, in terms of extra-column band broadening, sensitivity and dynamic range. The comparative study was carried out by using standard compounds belonging to different chemical classes, along with a sample of diesel fuel. Advantages and disadvantages of the BID system, also within the context of FM GC×GC, are critically discussed. In general, the BID system was characterized by a more limited dynamic range and increased sensitivity, compared to the FID. Additionally, BID and FID contribution to band broadening was found to be similar under the operational conditions applied. Particular attention was devoted to the behaviour of the FM GC×GC-BID system toward saturated and aromatic hydrocarbons, for a possible future use in the field of mineral-oil food contamination research. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Analysis of honeybush tea (Cyclopia spp.) volatiles by comprehensive two-dimensional gas chromatography using a single-stage thermal modulator.

    Science.gov (United States)

    Ntlhokwe, Gaalebalwe; Tredoux, Andreas G J; Górecki, Tadeusz; Edwards, Matthew; Vestner, Jochen; Muller, Magdalena; Erasmus, Lené; Joubert, Elizabeth; Christel Cronje, J; de Villiers, André

    2017-07-01

    The applicability of comprehensive two-dimensional gas chromatography (GC×GC) using a single-stage thermal modulator was explored for the analysis of honeybush tea (Cyclopia spp.) volatile compounds. Headspace solid phase micro-extraction (HS-SPME) was used in combination with GC×GC separation on a non-polar × polar column set with flame ionisation (FID) detection for the analysis of fermented Cyclopia maculata, Cyclopia subternata and Cyclopia genistoides tea infusions of a single harvest season. Method optimisation entailed evaluation of the effects of several experimental parameters on the performance of the modulator, the choice of columns in both dimensions, as well as the HS-SPME extraction fibre. Eighty-four volatile compounds were identified by co-injection of reference standards. Principal component analysis (PCA) showed clear differentiation between the species based on their volatile profiles. Due to the highly reproducible separations obtained using the single-stage thermal modulator, multivariate data analysis was simplified. The results demonstrate both the complexity of honeybush volatile profiles and the potential of GC×GC separation in combination with suitable data analysis techniques for the investigation of the relationship between sensory properties and volatile composition of these products. The developed method therefore offers a fast and inexpensive methodology for the profiling of honeybush tea volatiles. Graphical abstract Surface plot obtained for the GC×GC-FID analysis of honeybush tea volatiles.

  9. What can in situ ion chromatography offer for Mars exploration?

    Science.gov (United States)

    Shelor, C Phillip; Dasgupta, Purnendu K; Aubrey, Andrew; Davila, Alfonso F; Lee, Michael C; McKay, Christopher P; Liu, Yan; Noell, Aaron C

    2014-07-01

    The successes of the Mars exploration program have led to our unprecedented knowledge of the geological, mineralogical, and elemental composition of the martian surface. To date, however, only one mission, the Phoenix lander, has specifically set out to determine the soluble chemistry of the martian surface. The surprising results, including the detection of perchlorate, demonstrated both the importance of performing soluble ion measurements and the need for improved instrumentation to unambiguously identify all the species present. Ion chromatography (IC) is the state-of-the-art technique for soluble ion analysis on Earth and would therefore be the ideal instrument to send to Mars. A flight IC system must necessarily be small, lightweight, low-power, and have low eluent consumption. We demonstrate here a breadboard system that addresses these issues by using capillary IC at low flow rates with an optimized eluent generator and suppressor. A mix of 12 ions known or plausible for the martian soil, including 4 (oxy)chlorine species, has been separated at flow rates ranging from 1 to 10 μL/min, requiring as little as 200 psi at 1.0 μL/min. This allowed the use of pneumatic displacement pumping from a pressurized aluminum eluent reservoir and the elimination of the high-pressure pump entirely (the single heaviest and most energy-intensive component). All ions could be separated and detected effectively from 0.5 to 100 μM, even when millimolar concentrations of perchlorate were present in the same mixtures.

  10. On intermittency in heavy ion collisions and the importance of γ-conversion in a multi-dimensional intermittency analysis

    International Nuclear Information System (INIS)

    Adamovich, M.I.; Alexandrov, Y.A.; Aggarwal, M.M.

    1992-03-01

    Non-statistical fluctuations are used to probe the dynamical behaviour of multiparticle production in heavy ion interactions at ultra-relativistic energies. In a one-dimensional analysis a 1/ρ-scaling is established and it is furthermore found that effects from higher order particle correlations are small. In a two-dimensional analysis it is shown that a small background of particle-pairs with a narrow opening angle can distort the observed signal. As an example we estimate of the influence of γ-conversion and find that in our experiment γ-conversion alone gives results consistent with the experimental observations from a two-dimensional analysis. Whereas a two-dimensional analysis filters events where two particles are extremely close in phase space, the one-dimensional analysis picks out events with particles clustered in pseudorapidity, which are at the same time diluted in the azimuthal plane. (au)

  11. Radiation effects on two-dimensional materials

    Energy Technology Data Exchange (ETDEWEB)

    Walker, R.C. II; Robinson, J.A. [Department of Materials Science, Penn State, University Park, PA (United States); Center for Two-Dimensional Layered Materials, Penn State, University Park, PA (United States); Shi, T. [Department of Mechanical and Nuclear Engineering, Penn State, University Park, PA (United States); Department of Nuclear Engineering and Radiological Sciences, University of Michigan, Ann Arbor, MI (United States); Silva, E.C. [GlobalFoundries, Malta, NY (United States); Jovanovic, I. [Department of Nuclear Engineering and Radiological Sciences, University of Michigan, Ann Arbor, MI (United States)

    2016-12-15

    The effects of electromagnetic and particle irradiation on two-dimensional materials (2DMs) are discussed in this review. Radiation creates defects that impact the structure and electronic performance of materials. Determining the impact of these defects is important for developing 2DM-based devices for use in high-radiation environments, such as space or nuclear reactors. As such, most experimental studies have been focused on determining total ionizing dose damage to 2DMs and devices. Total dose experiments using X-rays, gamma rays, electrons, protons, and heavy ions are summarized in this review. We briefly discuss the possibility of investigating single event effects in 2DMs based on initial ion beam irradiation experiments and the development of 2DM-based integrated circuits. Additionally, beneficial uses of irradiation such as ion implantation to dope materials or electron-beam and helium-beam etching to shape materials have begun to be used on 2DMs and are reviewed as well. For non-ionizing radiation, such as low-energy photons, we review the literature on 2DM-based photo-detection from terahertz to UV. The majority of photo-detecting devices operate in the visible and UV range, and for this reason they are the focus of this review. However, we review the progress in developing 2DMs for detecting infrared and terahertz radiation. (copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  12. Identification of chemical components in Baidianling Capsule based on gas chromatography-mass spectrometry and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Wu, Wenying; Chen, Yu; Wang, Binjie; Sun, Xiaoyang; Guo, Ping; Chen, Xiaohui

    2017-08-01

    Baidianling Capsule, which is made from 16 Chinese herbs, has been widely used for treating vitiligo clinically. In this study, the sensitive and rapid method has been developed for the analysis of chemical components in Baidianling Capsule by gas chromatography-mass spectrometry in combination with retention indices and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Firstly, a total of 110 potential volatile compounds obtained from different extraction procedures including alkanes, alkenes, alkynes, ketones, ethers, aldehydes, alcohols, phenols, organic acids, esters, furans, pyrrole, acid amides, heterocycles, and oxides were detected from Baidianling Capsule by gas chromatography-mass spectrometry, of which 75 were identified by mass spectrometry in combination with the retention index. Then, a total of 124 components were tentatively identified by high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Fifteen constituents from Baidianling Capsule were accurately identified by comparing the retention times with those of reference compounds, others were identified by comparing the retention times and mass spectrometry data, as well as retrieving the reference literature. This study provides a practical strategy for rapidly screening and identifying the multiple constituents of a complex traditional Chinese medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. 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. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Three-dimensional velocity map imaging: Setup and resolution improvement compared to three-dimensional ion imaging

    International Nuclear Information System (INIS)

    Kauczok, S.; Goedecke, N.; Veckenstedt, M.; Maul, C.; Gericke, K.-H.; Chichinin, A. I.

    2009-01-01

    For many years the three-dimensional (3D) ion imaging technique has not benefited from the introduction of ion optics into the field of imaging in molecular dynamics. Thus, a lower resolution of kinetic energy as in comparable techniques making use of inhomogeneous electric fields was inevitable. This was basically due to the fact that a homogeneous electric field was needed in order to obtain the velocity component in the direction of the time of flight spectrometer axis. In our approach we superimpose an Einzel lens field with the homogeneous field. We use a simulation based technique to account for the distortion of the ion cloud caused by the inhomogeneous field. In order to demonstrate the gain in kinetic energy resolution compared to conventional 3D Ion Imaging, we use the spatial distribution of H + ions emerging from the photodissociation of HCl following the two photon excitation to the V 1 Σ + state. So far a figure of merit of approximately four has been achieved, which means in absolute numbers Δv/v=0.022 compared to 0.086 at v≅17 000 m/s. However, this is not a theoretical limit of the technique, but due to our rather short TOF spectrometer (15 cm). The photodissociation of HBr near 243 nm has been used to recognize and eliminate systematic deviations between the simulation and the experimentally observed distribution. The technique has also proven to be essential for the precise measurement of translationally cold distributions.

  15. Comprehensive analysis of pharmaceutical products using simultaneous mixed-mode (ion-exchange/reversed-phase) and hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Kazarian, Artaches A; Nesterenko, Pavel N; Soisungnoen, Phimpha; Burakham, Rodjana; Srijaranai, Supalax; Paull, Brett

    2014-08-01

    Liquid chromatographic assays were developed using a mixed-mode column coupled in sequence with a hydrophilic interaction liquid chromatography column to allow the simultaneous comprehensive analysis of inorganic/organic anions and cations, active pharmaceutical ingredients, and excipients (carbohydrates). The approach utilized dual sample injection and valve-mediated column switching and was based upon a single high-performance liquid chromatography gradient pump. The separation consisted of three distinct sequential separation mechanisms, namely, (i) ion-exchange, (ii) mixed-mode interactions under an applied dual gradient (reversed-phase/ion-exchange), and (iii) hydrophilic interaction chromatography. Upon first injection, the Scherzo SS C18 column (Imtakt) provided resolution of inorganic anions and cations under isocratic conditions, followed by a dual organic/salt gradient to elute active pharmaceutical ingredients and their respective organic counterions and potential degradants. At the top of the mixed-mode gradient (high acetonitrile content), the mobile phase flow was switched to a preconditioned hydrophilic interaction liquid chromatography column, and the standard/sample was reinjected for the separation of hydrophilic carbohydrates, some of which are commonly known excipients in drug formulations. The approach afforded reproducible separation and resolution of up to 23 chemically diverse solutes in a single run. The method was applied to investigate the composition of commercial cough syrups (Robitussin®), allowing resolution and determination of inorganic ions, active pharmaceutical ingredients, excipients, and numerous well-resolved unknown peaks. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Qualitative and quantitative analysis of pyrolysis oil by gas chromatography with flame ionization detection and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry.

    Science.gov (United States)

    Sfetsas, Themistoklis; Michailof, Chrysa; Lappas, Angelos; Li, Qiangyi; Kneale, Brian

    2011-05-27

    Pyrolysis oils have attracted a lot of interest, as they are liquid energy carriers and general sources of chemicals. In this work, gas chromatography with flame ionization detector (GC-FID) and two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) techniques were used to provide both qualitative and quantitative results of the analysis of three different pyrolysis oils. The chromatographic methods and parameters were optimized and solvent choice and separation restrictions are discussed. Pyrolysis oil samples were diluted in suitable organic solvent and were analyzed by GC×GC-TOFMS. An average of 300 compounds were detected and identified in all three samples using the ChromaToF (Leco) software. The deconvoluted spectra were compared with the NIST software library for correct matching. Group type classification was performed by use of the ChromaToF software. The quantification of 11 selected compounds was performed by means of a multiple-point external calibration curve. Afterwards, the pyrolysis oils were extracted with water, and the aqueous phase was analyzed both by GC-FID and, after proper change of solvent, by GC×GC-TOFMS. As previously, the selected compounds were quantified by both techniques, by means of multiple point external calibration curves. The parameters of the calibration curves were calculated by weighted linear regression analysis. The limit of detection, limit of quantitation and linearity range for each standard compound with each method are presented. The potency of GC×GC-TOFMS for an efficient mapping of the pyrolysis oil is undisputable, and the possibility of using it for quantification as well has been demonstrated. On the other hand, the GC-FID analysis provides reliable results that allow for a rapid screening of the pyrolysis oil. To the best of our knowledge, very few papers have been reported with quantification attempts on pyrolysis oil samples using GC×GC-TOFMS most of which make use of the

  17. Resolution of co-eluting compounds of Cannabis Sativa in comprehensive two-dimensional gas chromatography/mass spectrometry detection with Multivariate Curve Resolution-Alternating Least Squares.

    Science.gov (United States)

    Omar, Jone; Olivares, Maitane; Amigo, José Manuel; Etxebarria, Nestor

    2014-04-01

    Comprehensive Two Dimensional Gas Chromatography - Mass Spectrometry (GC × GC/qMS) analysis of Cannabis sativa extracts shows a high complexity due to the large variety of terpenes and cannabinoids and to the fact that the complete resolution of the peaks is not straightforwardly achieved. In order to support the resolution of the co-eluted peaks in the sesquiterpene and the cannabinoid chromatographic region the combination of Multivariate Curve Resolution and Alternating Least Squares algorithms was satisfactorily applied. As a result, four co-eluting areas were totally resolved in the sesquiterpene region and one in the cannabinoid region in different samples of Cannabis sativa. The comparison of the mass spectral profiles obtained for each resolved peak with theoretical mass spectra allowed the identification of some of the co-eluted peaks. Finally, the classification of the studied samples was achieved based on the relative concentrations of the resolved peaks. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. The role of helium ion microscopy in the characterisation of complex three-dimensional nanostructures

    International Nuclear Information System (INIS)

    Rodenburg, C.; Liu, X.; Jepson, M.A.E.; Zhou, Z.; Rainforth, W.M.; Rodenburg, J.M.

    2010-01-01

    This work addresses two major issues relating to Helium Ion Microscopy (HeIM). First we show that HeIM is capable of solving the interpretation difficulties that arise when complex three-dimensional structures are imaged using traditional high lateral resolution techniques which are transmission based, such as scanning transmission electron microscopy (STEM). Secondly we use a nano-composite coating consisting of amorphous carbon embedded in chromium rich matrix to estimate the mean escape depth for amorphous carbon for secondary electrons generated by helium ion impact as a measure of HeIM depth resolution.

  19. Nitrate and nitrite content in bottled beverages by ion-pair high-performance liquid chromatography.

    Science.gov (United States)

    Song, Yang; Deng, Gui-Fang; Xu, Xiang-Rong; Chen, Yong-Hong; Chen, Feng; Li, Hua-Bin

    2013-01-01

    Nitrate and nitrite levels in six types of beverages--total of 292 individual samples from 73 brands (four bottles each)--from Guangzhou city in China were evaluated by ion-pair high-performance liquid chromatography. All samples contained nitrate. Nitrate and nitrite ranges were 0.43-46.08 and safety of Chinese bottled beverages.

  20. Analysis of wax esters by silver-ion high-performance liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vrkoslav, Vladimír; Urbanová, Klára; Háková, Martina; Cvačka, Josef

    2013-01-01

    Roč. 1302, Aug 9 (2013), s. 105-110 ISSN 0021-9673 R&D Projects: GA ČR GA203/09/0139 Institutional support: RVO:61388963 Keywords : jojoba * human hair * wax esters * mass spectrometry * silver-ion liquid chromatography * long-chain esters Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.258, year: 2013

  1. Consequences of transition from liquid chromatography to supercritical fluid chromatography on the overall performance of a chiral zwitterionic ion-exchanger.

    Science.gov (United States)

    Wolrab, Denise; Frühauf, Peter; Gerner, Christopher; Kohout, Michal; Lindner, Wolfgang

    2017-09-29

    Major differences in the chromatographic performance of a zwitterion ion-exchange type (ZWIX) chiral stationary phase (CSP) in supercritical fluid chromatography (SFC) and high-performance liquid chromatography (HPLC) have been observed. To explain these differences, transition from HPLC to SFC conditions has been performed. The amount of a protic organic modifier in supercritical carbon dioxide (scCO 2 ) was stepwise increased and the effect of this change studied using acidic, basic and ampholytic analytes. At the same time, the effect of various basic additives to the mobile phase and transient acidic buffer species, formed by the reaction of scCO 2 with the organic modifier and additives, was assessed. Evidence is provided that a transient acid together with the intrinsic counter-ions present in the ZWIX selector structure drive the elution of analytes even when no buffer is employed. We show that the tested analytes can be enantioseparated under both SFC and HPLC conditions; the best conditions for the resolution of ampholytes are in the so-called enhanced-fluidity mobile phase region. As a consequence, subcritical fluid and enhanced-fluidity mobile phase regions seem to be chromatographic modes with a high potential for operating ZWIX CSPs. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Highly ordered three-dimensional macroporous carbon spheres for determination of heavy metal ions

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yuxiao; Zhang, Jianming [Institute of Functional Nano and Soft Materials (FUNSOM) and Jiangsu Key Laboratory for Carbon-Based Functional Materials and Devices, Soochow University, Suzhou 215123 (China); Liu, Yang, E-mail: yangl@suda.edu.cn [Institute of Functional Nano and Soft Materials (FUNSOM) and Jiangsu Key Laboratory for Carbon-Based Functional Materials and Devices, Soochow University, Suzhou 215123 (China); Huang, Hui [Institute of Functional Nano and Soft Materials (FUNSOM) and Jiangsu Key Laboratory for Carbon-Based Functional Materials and Devices, Soochow University, Suzhou 215123 (China); Kang, Zhenhui, E-mail: zhkang@suda.edu.cn [Institute of Functional Nano and Soft Materials (FUNSOM) and Jiangsu Key Laboratory for Carbon-Based Functional Materials and Devices, Soochow University, Suzhou 215123 (China)

    2012-04-15

    Highlights: Black-Right-Pointing-Pointer Highly ordered three dimensional macroporous carbon spheres (MPCSs) were prepared. Black-Right-Pointing-Pointer MPCS was covalently modified by cysteine (MPCS-CO-Cys). Black-Right-Pointing-Pointer MPCS-CO-Cys was first time used in electrochemical detection of heavy metal ions. Black-Right-Pointing-Pointer Heavy metal ions such as Pb{sup 2+} and Cd{sup 2+} can be simultaneously determined. -- Abstract: An effective voltammetric method for detection of trace heavy metal ions using chemically modified highly ordered three dimensional macroporous carbon spheres electrode surfaces is described. The highly ordered three dimensional macroporous carbon spheres were prepared by carbonization of glucose in silica crystal bead template, followed by removal of the template. The highly ordered three dimensional macroporous carbon spheres were covalently modified by cysteine, an amino acid with high affinities towards some heavy metals. The materials were characterized by physical adsorption of nitrogen, scanning electron microscopy, and transmission electron microscopy techniques. While the Fourier-transform infrared spectroscopy was used to characterize the functional groups on the surface of carbon spheres. High sensitivity was exhibited when this material was used in electrochemical detection (square wave anodic stripping voltammetry) of heavy metal ions due to the porous structure. And the potential application for simultaneous detection of heavy metal ions was also investigated.

  3. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo

    2016-07-13

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Comparison of originator and biosimilar therapeutic monoclonal antibodies using comprehensive two-dimensional liquid chromatography coupled with time-of-flight mass spectrometry.

    Science.gov (United States)

    Sorensen, Matthew; Harmes, David C; Stoll, Dwight R; Staples, Gregory O; Fekete, Szabolcs; Guillarme, Davy; Beck, Alain

    2016-10-01

    As research, development, and manufacturing of biosimilar protein therapeutics proliferates, there is great interest in the continued development of a portfolio of complementary analytical methods that can be used to efficiently and effectively characterize biosimilar candidate materials relative to the respective reference (i.e., originator) molecule. Liquid phase separation techniques such as liquid chromatography and capillary electrophoresis are powerful tools that can provide both qualitative and quantitative information about similarities and differences between reference and biosimilar materials, especially when coupled with mass spectrometry. However, the inherent complexity of these protein materials challenges even the most modern one-dimensional (1D) separation methods. Two-dimensional (2D) separations present a number of potential advantages over 1D methods, including increased peak capacity, 2D peak patterns that can facilitate unknown identification, and improvement in the compatibility of some separation methods with mass spectrometry. In this study, we demonstrate the use of comprehensive 2D-LC separations involving cation-exchange (CEX) and reversed-phase (RP) separations in the first and second dimensions to compare 3 reference/biosimilar pairs of monoclonal antibodies (cetuximab, trastuzumab and infliximab) that cover a range of similarity/disimilarity in a middle-up approach. The second dimension RP separations are coupled to time-of-flight mass spectrometry, which enables direct identification of features in the chromatograms obtained from mAbs digested with the IdeS enzyme, or digestion with IdeS followed by reduction with dithiothreitol. As many as 23 chemically unique mAb fragments were detected in a single sample. Our results demonstrate that these rich datasets enable facile assesment of the degree of similarity between reference and biosimilar materials.

  5. Optimization of a two-dimensional liquid chromatography-supercritical fluid chromatography-mass spectrometry (2D-LC-SFS-MS) system to assess "in-vivo" inter-conversion of chiral drug molecules.

    Science.gov (United States)

    Goel, Meenakshi; Larson, Eli; Venkatramani, C J; Al-Sayah, Mohammad A

    2018-05-01

    Enantioselective analysis is an essential requirement during the pharmaceutical development of chiral drug molecules. In pre-clinical and clinical studies, the Food and Drug Administration (FDA) mandates the assessment of "in vivo" inter-conversion of chiral drugs to determine their physiological effects. In-vivo analysis of the active pharmaceutical ingredient (API) and its potential metabolites could be quite challenging due to their low abundance (ng/mL levels) and matrix interferences. Therefore, highly selective and sensitive analytical techniques are required to separate the API and its metabolites from the matrix components and one another. Additionally, for chiral APIs, further analytical separation is required to resolve the API and its potential metabolites from their corresponding enantiomers. In this work, we demonstrate the optimization of our previously designed two-dimensional liquid chromatography-supercritical fluid chromatography-mass spectrometry (2D-LC-SFC -MS) system to achieve 10 ng/mL detection limit [1]. The first LC dimension, used as a desalting step, could efficiently separate the API from its potential metabolites and matrix components. The API and its metabolites were then trapped/focused on small trapping columns and transferred onto the second SFC dimension for chiral separation. Detection can be achieved by ultra-violet (UV) or MS detection. Different system parameters such as column dimensions, transfer volumes, trapping column stationary phase, system tubing internal diameter (i.d.), and detection techniques, were optimized to enhance the sensitivity of the 2D-LC-SFC-MS system. The limit of detection was determined to be 10 ng/mL. An application is described where a mouse hepatocyte treated sample was analyzed using the optimized 2D-LC-SFC-MS system with successful assessment of the ratio of API to its metabolite (1D-LC), as well as the corresponding enantiomeric excess values (% e.e.) of each (2D-SFC). Copyright © 2018

  6. Ion trace detection algorithm to extract pure ion chromatograms to improve untargeted peak detection quality for liquid chromatography/time-of-flight mass spectrometry-based metabolomics data.

    Science.gov (United States)

    Wang, San-Yuan; Kuo, Ching-Hua; Tseng, Yufeng J

    2015-03-03

    Able to detect known and unknown metabolites, untargeted metabolomics has shown great potential in identifying novel biomarkers. However, elucidating all possible liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS) ion signals in a complex biological sample remains challenging since many ions are not the products of metabolites. Methods of reducing ions not related to metabolites or simply directly detecting metabolite related (pure) ions are important. In this work, we describe PITracer, a novel algorithm that accurately detects the pure ions of a LC/TOF-MS profile to extract pure ion chromatograms and detect chromatographic peaks. PITracer estimates the relative mass difference tolerance of ions and calibrates the mass over charge (m/z) values for peak detection algorithms with an additional option to further mass correction with respect to a user-specified metabolite. PITracer was evaluated using two data sets containing 373 human metabolite standards, including 5 saturated standards considered to be split peaks resultant from huge m/z fluctuation, and 12 urine samples spiked with 50 forensic drugs of varying concentrations. Analysis of these data sets show that PITracer correctly outperformed existing state-of-art algorithm and extracted the pure ion chromatograms of the 5 saturated standards without generating split peaks and detected the forensic drugs with high recall, precision, and F-score and small mass error.

  7. LC-IMS-MS Feature Finder: detecting multidimensional liquid chromatography, ion mobility and mass spectrometry features in complex datasets.

    Science.gov (United States)

    Crowell, Kevin L; Slysz, Gordon W; Baker, Erin S; LaMarche, Brian L; Monroe, Matthew E; Ibrahim, Yehia M; Payne, Samuel H; Anderson, Gordon A; Smith, Richard D

    2013-11-01

    The addition of ion mobility spectrometry to liquid chromatography-mass spectrometry experiments requires new, or updated, software tools to facilitate data processing. We introduce a command line software application LC-IMS-MS Feature Finder that searches for molecular ion signatures in multidimensional liquid chromatography-ion mobility spectrometry-mass spectrometry (LC-IMS-MS) data by clustering deisotoped peaks with similar monoisotopic mass, charge state, LC elution time and ion mobility drift time values. The software application includes an algorithm for detecting and quantifying co-eluting chemical species, including species that exist in multiple conformations that may have been separated in the IMS dimension. LC-IMS-MS Feature Finder is available as a command-line tool for download at http://omics.pnl.gov/software/LC-IMS-MS_Feature_Finder.php. The Microsoft.NET Framework 4.0 is required to run the software. All other dependencies are included with the software package. Usage of this software is limited to non-profit research to use (see README). rds@pnnl.gov. Supplementary data are available at Bioinformatics online.

  8. Numerical analysis of ion temperature effects to the plasma wall transition using a one-dimensional two-fluid model. I. Finite Debye to ionization length ratio

    Science.gov (United States)

    Gyergyek, T.; Kovačič, J.

    2017-06-01

    A one-dimensional, two-fluid, steady state model is used for the analysis of ion temperature effects to the plasma-wall transition. In this paper, the model is solved for a finite ratio ɛ between the Debye and the ionization length, while in Part II [T. Gyergyek and J. Kovačič, Phys Plasmas 24, 063506 (2017)], the solutions for ɛ = 0 are presented. Ion temperature is treated as a given, independent parameter and it is included in the model as a boundary condition. It is shown that when the ion temperature larger than zero is selected, the ion flow velocity and the electric field at the boundary must be consistent with the selected ion temperature. A numerical procedure, how to determine such "consistent boundary conditions," is proposed, and a simple relation between the ion temperature and ion velocity at the boundary of the system is found. The effects of the ion temperature to the pre-sheath length, potential, ion temperature, and ion density drops in the pre-sheath and in the sheath are investigated. It is concluded that larger ion temperature results in a better shielding of the plasma from the wall. An attempt is made to include the ion heat flux qi into the model in its simplest form q i = - K ' /d T i d x , where K ' is a constant heat conduction coefficient. It is shown that inclusion of such a term into the energy transfer equation introduces an additional ion heating mechanism into the system and the ion flow then becomes isothermal instead of adiabatic even in the sheath.

  9. Experimental investigation of two-dimensional critical surface structure, stimulated Raman scattering, and two-plasmon decay instability. Annual report, January 1, 1981-April 30, 1982

    International Nuclear Information System (INIS)

    Wong, A.Y.; Eggleston, D.L.; Tanikawa, T.; Qian, S.J.

    1982-11-01

    Experimental observations of the space and time evolution of resonantly enhanced electrostatic electric fields and plasma density in cylindrical geometry demonstrate the development of two-dimensional caviton structure when an initial density perturbation is imposed on the plasma in the direction perpendicular to the driver field. This two-dimensional structure is observed after the development of profile modification and grows on the ion time scale. The existence of a large azimuthal electric field component is an observational signature of two-dimensional structure. Enhanced electric field maxima are found to be azimuthally correlated with the density minima. Both the density cavities and electric field peaks exhibit increased azimuthal location with the growth of two-dimensional structure. The two-dimensional development exhibits a strong dependence on both perturbation wavenumber and driver power. The related theoretical literature is reviewed and numerical, analytical, and qualitative hybrid models for a driven, two-dimensional, inhomogeneous plasma are presented. Preliminary work is presented in the following additional areas: weak magnetic field effects on critical surface physics, optical measurements of fast electron production, two-dimensional effects in microwave-plasma interactions, Langmuir wave trapping, stimulated Raman scattering and two-plasmon decay instability

  10. Ion chromatography with the indirect ultraviolet detection of alkali metal ions and ammonium using imidazolium ionic liquid as ultraviolet absorption reagent and eluent.

    Science.gov (United States)

    Liu, Yong-Qiang; Yu, Hong

    2016-08-01

    Indirect ultraviolet detection was conducted in ultraviolet-absorption-agent-added mobile phase to complete the detection of the absence of ultraviolet absorption functional group in analytes. Compared with precolumn derivatization or postcolumn derivatization, this method can be widely used, has the advantages of simple operation and good linear relationship. Chromatographic separation of Li(+) , Na(+) , K(+) , and NH4 (+) was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid/organic solvent as the mobile phase, in which imidazolium ionic liquids acted as ultraviolet absorption reagent and eluting agent. The retention behaviors of four kinds of cations are discussed, and the mechanism of separation and detection are described. The main factors influencing the separation and detection were the background ultraviolet absorption reagent and the concentration of hydrogen ion in the ion chromatography-indirect ultraviolet detection. The successful separation and detection of Li(+) , Na(+) , K(+) , and NH4 (+) within 13 min was achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.02, 0.11, 0.30, and 0.06 mg/L, respectively. A new separation and analysis method of alkali metal ions and ammonium by ion chromatography with indirect ultraviolet detection method was developed, and the application range of ionic liquid was expanded. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Three-dimensional thin film for lithium-ion batteries and supercapacitors.

    Science.gov (United States)

    Yang, Yang; Peng, Zhiwei; Wang, Gunuk; Ruan, Gedeng; Fan, Xiujun; Li, Lei; Fei, Huilong; Hauge, Robert H; Tour, James M

    2014-07-22

    Three-dimensional heterogeneously nanostructured thin-film electrodes were fabricated by using Ta2O5 nanotubes as a framework to support carbon-onion-coated Fe2O3 nanoparticles along the surface of the nanotubes. Carbon onion layers function as microelectrodes to separate the two different metal oxides and form a nanoscale 3-D sandwich structure. In this way, space-charge layers were formed at the phase boundaries, and it provides additional energy storage by charge separation. These 3-D nanostructured thin films deliver both excellent Li-ion battery properties (stabilized at 800 mAh cm(–3)) and supercapacitor (up to 18.2 mF cm(–2)) performance owing to the synergistic effects of the heterogeneous structure. Thus, Li-ion batteries and supercapacitors are successfully assembled into the same electrode, which is promising for next generation hybrid energy storage and delivery devices.

  12. Full evaporation dynamic headspace in combination with selectable one-dimensional/two-dimensional gas chromatography-mass spectrometry for the determination of suspected fragrance allergens in cosmetic products.

    Science.gov (United States)

    Devos, Christophe; Ochiai, Nobuo; Sasamoto, Kikuo; Sandra, Pat; David, Frank

    2012-09-14

    Suspected fragrance allergens were determined in cosmetic products using a combination of full evaporation-dynamic headspace (FEDHS) with selectable one-dimensional/two-dimensional GC-MS. The full evaporation dynamic headspace approach allows the non-discriminating extraction and injection of both apolar and polar fragrance compounds, without contamination of the analytical system by high molecular weight non-volatile matrix compounds. The method can be applied to all classes of cosmetic samples, including water containing matrices such as shower gels or body creams. In combination with selectable (1)D/(2)D GC-MS, consisting of a dedicated heart-cutting GC-MS configuration using capillary flow technology (CFT) and low thermal mass GC (LTM-GC), a highly flexible and easy-to-use analytical solution is offered. Depending on the complexity of the perfume fraction, analyses can be performed in one-dimensional GC-MS mode or in heart-cutting two-dimensional GC-MS mode, without the need of hardware reconfiguration. The two-dimensional mode with independent temperature control of the first and second dimension column is especially useful to confirm the presence of detected allergen compounds when mass spectral deconvolution is not possible. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Two-chamber configuration of Bio-Nano electron cyclotron resonance ion source for fullerene modification

    Energy Technology Data Exchange (ETDEWEB)

    Uchida, T., E-mail: uchida-t@toyo.jp [Bio-Nano Electronics Research Centre, Toyo University, Kawagoe 350-8585 (Japan); Graduate School of Interdisciplinary New Science, Toyo University, Kawagoe 350-8585 (Japan); Rácz, R.; Biri, S. [Institute for Nuclear Research (Atomki), Hungarian Academy of Sciences, Bem tér 18/C, H-4026 Debrecen (Hungary); Muramatsu, M.; Kitagawa, A. [National Institute of Radiological Sciences (NIRS), Chiba 263-8555 (Japan); Kato, Y. [Graduate School of Engineering, Osaka University, Suita 565-0871 (Japan); Yoshida, Y. [Bio-Nano Electronics Research Centre, Toyo University, Kawagoe 350-8585 (Japan); Faculty of Science and Engineering, Toyo University, Kawagoe 350-8585 (Japan)

    2016-02-15

    We report on the modification of fullerenes with iron and chlorine using two individually controllable plasmas in the Bio-Nano electron cyclotron resonance ion source (ECRIS). One of the plasmas is composed of fullerene and the other one is composed of iron and chlorine. The online ion beam analysis allows one to investigate the rate of the vapor-phase collisional modification process in the ECRIS, while the offline analyses (e.g., liquid chromatography-mass spectrometry) of the materials deposited on the plasma chamber can give information on the surface-type process. Both analytical methods show the presence of modified fullerenes such as fullerene-chlorine, fullerene-iron, and fullerene-chlorine-iron.

  14. Novel two-dimensional uranyl-organic assemblages in the citrate and D(-)-citramalate families

    International Nuclear Information System (INIS)

    Thuery, P.

    2008-01-01

    Uranyl nitrate reacts with D(-)-citramalic acid (H(3)citml) under mild hydrothermal conditions to give the two-dimensional polymer [UO 2 (Hcitml)] 1, in which each ligand chelates one metal atom through its hydroxyl and alpha- carboxylate groups and binds to three others in monodentate fashion. The resulting neutral layers display isolated uranyl pentagonal bipyramidal polyhedra. Whereas citric acid (H(4)cit) has been shown previously to give various three- and mono-dimensional uranyl organic assemblages, complexation under hydrothermal conditions in the presence of either NaOH/NEt 4 Cl or pyridine yields the complexes [NEt 4 ] 2 [(UO 2 ) 3 (cit) 2 (H 2 O) 2 ]· 2H 2 O 2 and [Hpy] 2 )[(UO 2 ) 3 (cit)(Hcit)(OH)] 3, respectively, which both crystallize as two- dimensional frameworks. The layers are either planar and separated by the counter ions in 2 or corrugated and hydrogen bonded to one another in 3. In both 2 and 3, [UO 2 (cit)] 2 4- dimeric subunits with edge-sharing pentagonal bipyramidal uranium coordination polyhedra are present but, in both cases and in contrast with previous structures containing [UO 2 (Hcit)] 2 2- dimers, the carboxylate group not involved in the dimer formation is coordinated to another uranyl unit, which is part of either a centrosymmetric hexagonal bipyramidal bis-aquated group or a different, [(UO 2 ) 2 (Hcit)(OH)] dimer. These examples of two- dimensional assemblages further illustrate the variety of architectures which can be obtained with citric and related acids and the important structure-directing effects of the counter ions. (author)

  15. Fabrication of electrolytic cell for online post-column electrochemical derivatization in ion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Wu Shuchao [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, Zhejiang (China); Xu Wei [State Key Laboratory for Diagnosis and Treatment of Infectious Diseases, The First Affiliated Hospital, College of Medicine, Zhejiang University, Hangzhou 310028, Zhejiang (China); Yang Bingcheng [School of Pharmacy, East China University of Science and Technology, Shanghai 200237 (China); Ye Mingli [Thermofisher scientific (China), Shanghai 201203 (China); Zhang Peimin [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, Zhejiang (China); Shentu Chao [College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015 (China); Zhu Yan, E-mail: zhuyan@zju.edu.cn [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, Zhejiang (China)

    2012-07-20

    Highlight: Black-Right-Pointing-Pointer An electrolytic cell including ruthenium modified titanium electrode was fabricated. Black-Right-Pointing-Pointer Ion chromatography/electrochemical derivatization/fluorescence detection was developed. Black-Right-Pointing-Pointer Strong oxidation capacity of this EC was obtained by using the Ru/Ti electrode with large surface area. - Abstract: An electrolytic cell (EC), composed of two ruthenium-plated titanium electrodes separated by cation-exchange membranes, was fabricated and evaluated for online postcolumn derivatization in ion chromatography (IC). Folic acid (FA) and methotrexate (MTX) were preliminarily used as prototype analytes to test the performance of EC. After separation by an anion exchange column, FA and MTX, which emit very weak fluorescence when excited, were electrochemically oxidized online in the anode chamber of the EC. The compounds with strong fluorescence, which are oxidation products, were detected by the fluorescence detector. The phosphate buffer solution (100 mM KH{sub 2}PO{sub 4}) served as an optimal eluent for anion exchange chromatographic separation and a suitable supporting electrolyte for electro-oxidation, leading to ideal compatibility between IC separation and the postcolumn electrochemical derivatization. For the presently proposed method, the linear ranges were from 0.01 mg L{sup -1} to 5 mg L{sup -1} for both FA and MTX. The detection limits of FA and MTX were 1.8 and 2.1 {mu}g L{sup -1}, and the relative standard deviations (RSD, n = 7) were 2.9% and 3.6%, respectively. The method was applied for the simultaneous determination of FA and MTX in the plasma of patients being treated for rheumatoid arthritis. The determination of MTX in the urine of the patients of diffuse large B cell lymphoma was also demonstrated.

  16. Quantitative analysis of valsartan by two-dimensional liquid chromatography (2D-HPLC) and its application in a bioequivalence study in Chinese volunteers
.

    Science.gov (United States)

    Zhang, Min; Deng, Yang; Cai, Hua-Lin; Fang, Ping-Fei; Yan, Miao; Zhang, Bi-Kui; Wu, Yan-Qin

    2017-04-01

    To develop a sensitive, two-dimensional liquid chromatography (2D-LC) method for determination of valsartan, applied to investigate bioequivalence of two valsartan tablets in Chinese volunteers under fasting condition. A full automatic 2D-HPLC system was used to quantify valsartan in human plasma. The analytes were extracted by protein precipitation, using telmisartan as internal standard. The analytical method was applied in a randomized, crossover bioequivalence study of valsartan tablets; the study enrolled 18 Chinese volunteers (12 were men and 6 were women). The subjects received a single 160-mg dose of test or reference preparation with 7-days of washout under fasting state. Plasma samples were collected, pharmacokinetic parameters were obtained and the bioequivalence was evaluated. The calibration range was 9.2 - 4213.8 ng×mL-1. Inter- and intraprecision was less than 7.0%, and accuracies ranged from 99.5 to 103.8%. The extraction recovery for valsartan varied between 89.3 and 97.8%, and the stability in all conditions was excellent. The 90% CI of AUC0→36h and Cmax were 96.5 - 109.4% and 94.2 - 108.6%, respectively. The relative bioavailability was 103.9 ± 15.7%. No gender difference was observed in pharmacokinetic parameters. A sensitive 2D-HPLC method was established for the estimation of valsartan in human plasma and successfully applied in a bioequivalence study of valsartan, which suggests that these two formulations can be assumed to be bioequivalent.
.

  17. Analysis of Poly-β-Hydroxybutyrate in Rhizobium japonicum Bacteroids by Ion-Exclusion High-Pressure Liquid Chromatography and UV Detection †

    Science.gov (United States)

    Karr, Dale B.; Waters, James K.; Emerich, David W.

    1983-01-01

    Ion-exclusion high-pressure liquid chromatography (HPLC) was used to measure poly-β-hydroxybutyrate (PHB) in Rhizobium japonicum bacteroids. The products in the acid digest of PHB-containing material were fractionated by HPLC on Aminex HPX-87H ion-exclusion resin for organic acid analysis. Crotonic acid formed from PHB during acid digestion was detected by its intense absorbance at 210 nm. The Aminex-HPLC method provides a rapid and simple chromatographic technique for routine analysis of organic acids. Results of PHB analysis by Aminex-HPLC were confirmed by gas chromatography and spectrophotometric analysis. PMID:16346443

  18. Application of ion mobility-mass spectrometry to microRNA analysis.

    Science.gov (United States)

    Takebayashi, Kosuke; Hirose, Kenji; Izumi, Yoshihiro; Bamba, Takeshi; Fukusaki, Eiichiro

    2013-03-01

    Liquid chromatography/mass spectrometry is widely used for studying sequence determination and modification analysis of small RNAs. However, the efficiency of liquid chromatography-based separation of intact small RNA species is insufficient, since the physiochemical properties among small RNAs are very similar. In this study, we focused on ion mobility-mass spectrometry (IM-MS), which is a gas-phase separation technique coupled with mass spectrometry; we have evaluated the utility of IM-MS for microRNA (miRNA) analysis. A multiply charged deprotonated ion derived from an 18-24-nt-long miRNA was formed by electrospray ionization, and then the time, called the "drift time", taken by each ion to migrate through a buffer gas was measured. Each multivalent ion was temporally separated on the basis of the charge state and structural formation; 3 types of unique mass-mobility correlation patterns (i.e., chainlike-form, hairpin-form, and dimer-form) were present on the two-dimensional mobility-mass spectrum. Moreover, we found that the ion size (sequence length) and the secondary structures of the small RNAs strongly contributed to the IM-MS-based separation, although solvent conditions such as pH had no effect. Therefore, sequence isomers could also be discerned by the selection of each specific charged ion, i.e., the 6(-) charged ion reflected a majority among chainlike-, hairpin-, and other structures. We concluded that the IM-MS provides additional capability for separation; thus, this analytical method will be a powerful tool for comprehensive small RNA analysis. Copyright © 2012. Published by Elsevier B.V.

  19. Application of ion chromatography to the control of materials of nuclear interest

    International Nuclear Information System (INIS)

    Pires, M.A.F.

    1989-01-01

    The present work concerns ion chromatrography (IC) with conductometric detection as analytical technique for controling several materials of nuclear interest by determining the chemical elements present in them. Priority has been given to the individual determination of the lanthanide elements and yttrium. Complexing agents were used as eluents for the elements studied. Several experiments were performed in which the eluent composition as well as its pH were varied, so obtaining the eluent's iso-pH and iso-concentration values for each of the lanthanide and yttrium. The importance of the presence of the ethylenediamine ion on the separation and elution of the rare-earths was investigated. The determination of the alkaline metals and ammonium ion, alkaline-earth elements, fluoride, chloride, nitrate and phosphate anions in several solutions and in different materials that are involved in the chemical processes belonging to the fuel cycle was carried out. Single column ion chromatography technique was applied for determining all the lanthanide elements as well as yttrium, magnesium, calcium, strontium and barium and the sensibility of the measurements determined. A rapid chromatographic method for determining gadolinium in urania-gadolinia matrix is also proposed. Quantitative data on the separation of the lanthanide elements and yttrium from large amounts or other ions, rare earths for example, are presented. (author) [pt

  20. Supramolecular nano-architectures and two-dimensional/three-dimensional aggregation of a bolaamphiphilic diacid at the air/water interface

    International Nuclear Information System (INIS)

    Jiao Tifeng; Liu Minghua

    2005-01-01

    The spreading behavior and nano-architectures of a bolaamphiphilic diacid, 1, 13-tridecandicarboxylic acid (TDA) on water surface and the subphase containing Eu(III) ion were investigated. It was found that although TDA itself could not spread on water surface, it could form an ultrathin film on the aqueous subphase containing Eu(III) ion. In addition, interesting nano-architectures were observed for the transferred film on mica surface. It was found that the formation and change of the nano-architectures were depended on the surface pressure and concentration of Eu(III) ion in the subphase. A rectangular slide morphology was observed for the film spread on an aqueous subphase containing lower concentration of Eu(III), while a walnut-like nano-architectures were observed for the film spread on a higher concentration of Eu(III) ion. Flower structure was observed at a higher surface pressure. The nano-architecture can be further regulated through mixing TDA with octadecylamine (OA) in which linear fiber nanostructure was obtained. It was revealed that while the nano-architectures were formed mainly through a three dimensional aggregation in the case of TDA/Eu(III) films, a two-dimensional aggregation occurred when TDA was mixed with OA. A series of methods such as atomic force microscope, field emission scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction were used to characterize the supramolecular structures. A possible mechanism for the formation of these nano-architectures was discussed

  1. Separation of boron isotopes by ion exchange chromatography: studies with Duolite-162, a type-II resin

    International Nuclear Information System (INIS)

    Sharma, B.K.; Subramanian, R.; Balasubramanian, R.; Mathur, P.K.

    1994-01-01

    The selection of resin plays an important role in the process of separation of boron isotopes by ion exchange chromatography. The determination of (i) ion exchange capacity of Duolite-162 resin for hydroxyl - chloride exchange, (ii) hydroxyl - borate exchange, (iii) isotopic exchange separation factor by batch method and (iv) effect of concentration of boric acid on isotopic exchange separation factor to test the suitability of the above resin for this process are discussed in this report. (author)

  2. Application of ion chromatography for the determination of inorganic ions, especially thiocyanates, in human semen samples as biomarkers of environmental tobacco smoke exposure.

    Science.gov (United States)

    Demkowska, Ilona; Polkowska, Żaneta; Kiełbratowska, Bogumiła; Namieśnik, Jacek

    2010-11-01

    Tobacco smoking constitutes a significant source of indoor air pollution. Various chemical compounds that are emitted during tobacco smoking can have a direct cytotoxic effect on spermatozoa by damaging DNA. There is some evidence that tobacco smoking in men could affect male fertility. The goals of this study were to find relationships between thiocyanates (as biomarkers of environmental tobacco smoke exposure) and other inorganic ions in human semen samples and present the effectiveness of the proposed sample preparation procedure combined with ion chromatography technique for the determination of inorganic ions, especially thiocyanates, in human semen samples collected from heavy, moderate, and passive smokers, as well as nonsmoking individuals.

  3. The two-dimensional thiophosphate CsCrP2S7

    Directory of Open Access Journals (Sweden)

    Kyounghee Kim

    2010-09-01

    Full Text Available The quaternary title compound, caesium chromium(III heptathiodiphosphate(V, CsCrP2S7, has been synthesized using the reactive halide flux method. It is isotypic with other AMP2S7 (A = alkali metal; M = Cr, V or In structures and consists of two-dimensional ∞2[CrP2S7]− layers extending parallel to (001 which are separated from each other by Cs+ ions (symmetry 2. The layer is built up from slightly distorted octahedral [CrS6] units (symmetry 2 and bent [P2S7] units consisting of two corner-sharing [PS4] tetrahedra. The [CrS6] octahedra share two edges and two corners with the [PS4] tetrahedra. There are only van der Waals interactions present between the layers. The Cs+ ions are located in this van der Waals gap and stabilize the structure through weak ionic interactions. The classical charge balance of the title compound can be expressed as [Cs+][Cr3+][P5+]2[S2−]7.

  4. Oxygen speciation in upgraded fast pyrolysis bio-oils by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Omais, Badaoui; Crepier, Julien; Charon, Nadège; Courtiade, Marion; Quignard, Alain; Thiébaut, Didier

    2013-04-21

    Biomass fast pyrolysis is considered as a promising route to produce liquid for the transportation field from a renewable resource. However, the derived bio-oils are mainly oxygenated (45-50%w/w O on a wet basis) and contain almost no hydrocarbons. Therefore, upgrading is necessary to obtain a liquid with lower oxygen content and characterization of oxygenated compounds in these products is essential to assist conversion reactions. For this purpose, comprehensive two-dimensional gas chromatography (GC × GC) can be investigated. Oxygen speciation in such matrices is hampered by the large diversity of oxygenated families and the complexity of the hydrocarbon matrix. Moreover, response factors must be taken into account for oxygenate quantification as the Flame Ionisation Detector (FID) response varies when a molecule contains heteroatoms. To conclude, no distillation cuts were accessible and the analysis had to cover a large range of boiling points (30-630 °C). To take up this analytical challenge, a thorough optimization approach was developed. In fact, four GC × GC column sets were investigated to separate oxygenated compounds from the hydrocarbon matrix. Both model mixtures and the upgraded biomass flash pyrolysis oil were injected using GC × GC-FID to reach a suitable chromatographic separation. The advantages and drawbacks of each column combination for oxygen speciation in upgraded bio-oils are highlighted in this study. Among the four sets, an original polar × semi-polar column combination was selected and enabled the identification by GC × GC-ToF/MS of more than 40 compounds belonging to eight chemical families: ketones, furans, alcohols, phenols, carboxylic acids, guaiacols, anisols, and esters. For quantification purpose, the GC × GC-FID chromatogram was divided into more than 60 blobs corresponding to the previously identified analyte and hydrocarbon zones. A database associating each blob to a molecule and its specific response factor (determined

  5. Comparative proteomics analysis of sheep sperm under two doses of heavy ion to irradiation

    International Nuclear Information System (INIS)

    Li Hongyan; Zhao Xingxu; He Yuxuan; Zhang Yong; Zhang Hong; Wang Yanling; Li Fadi; Ma Youji

    2011-01-01

    The object of this study was to investigate differential proteomic expressions in sheep sperm protein under two doses (0.5 and 0.3 kGy) heavy ion radiation. The current research presented the protein changes using two-dimensional gel electrophoresis (2-DE) after staining with silver nitrate, differential expression proteins were detected by PDQuest 8.0 software and subjected to ion trap mass spectrometer equipped with a Surveyor HPLC system, and differential spots of protein were identified. Results showed that eight common different expressed protein spots in two doses 2D gels were identified to be three up-regulated proteins (glutaredoxin -1, transcription factor AP -2-alpha and enolase). It was concluded that there was significant difference at protein level in sheep sperm after heavy ion radiation and differential proteome expression analysis may be useful to clarify the physiology state of sheep sperm in heavy ion radiation, which laid a foundation for the further studies on heavy ion radiation of sheep sperm proteomics. (authors)

  6. Equivalence of two-dimensional gravities

    International Nuclear Information System (INIS)

    Mohammedi, N.

    1990-01-01

    The authors find the relationship between the Jackiw-Teitelboim model of two-dimensional gravity and the SL(2,R) induced gravity. These are shown to be related to a two-dimensional gauge theory obtained by dimensionally reducing the Chern-Simons action of the 2 + 1 dimensional gravity. The authors present an explicit solution to the equations of motion of the auxiliary field of the Jackiw-Teitelboim model in the light-cone gauge. A renormalization of the cosmological constant is also given

  7. Relationship of Ambient Atmosphere and Biological Aerosol Responses from a Fielded Pyrolysis-Gas Chromatography-Ion Mobility Spectrometry Bioanalytical Detector

    National Research Council Canada - National Science Library

    Snyder, A

    2003-01-01

    .... A pyrolysis-gas chromatography-ion mobility spectrometry stand-alone bioaerosol system was interfaced to an aerosol concentrator to collect ambient background aerosols and produce bioanalytical...

  8. Selective One-Dimensional Total Correlation Spectroscopy Nuclear Magnetic Resonance Experiments for a Rapid Identification of Minor Components in the Lipid Fraction of Milk and Dairy Products: Toward Spin Chromatography?

    Science.gov (United States)

    Papaemmanouil, Christina; Tsiafoulis, Constantinos G; Alivertis, Dimitrios; Tzamaloukas, Ouranios; Miltiadou, Despoina; Tzakos, Andreas G; Gerothanassis, Ioannis P

    2015-06-10

    We report a rapid, direct, and unequivocal spin-chromatographic separation and identification of minor components in the lipid fraction of milk and common dairy products with the use of selective one-dimensional (1D) total correlation spectroscopy (TOCSY) nuclear magnetic resonance (NMR) experiments. The method allows for the complete backbone spin-coupling network to be elucidated even in strongly overlapped regions and in the presence of major components from 4 × 10(2) to 3 × 10(3) stronger NMR signal intensities. The proposed spin-chromatography method does not require any derivatization steps for the lipid fraction, is selective with excellent resolution, is sensitive with quantitation capability, and compares favorably to two-dimensional (2D) TOCSY and gas chromatography-mass spectrometry (GC-MS) methods of analysis. The results of the present study demonstrated that the 1D TOCSY NMR spin-chromatography method can become a procedure of primary interest in food analysis and generally in complex mixture analysis.

  9. An Automated High Performance Capillary Liquid Chromatography Fourier Transform Ion Cyclotron Resonance Mass Spectrometer for High-Throughput Proteomics

    International Nuclear Information System (INIS)

    Belov, Mikhail E.; Anderson, Gordon A.; Wingerd, Mark A.; Udseth, Harold R.; Tang, Keqi; Prior, David C.; Swanson, Kenneth R.; Buschbach, Michael A.; Strittmatter, Eric F.; Moore, Ronald J.; Smith, Richard D.

    2004-01-01

    We report on a fully automated 9.4 tesla Fourier transform ion resonance cyclotron (FTICR) mass spectrometer coupled to reverse-phase chromatography for high-throughput proteomic studies. Modifications made to the front-end of a commercial FTICR instrument--a dual-ESI-emitter ion source; dual-channel electrodynamic ion funnel; and collisional-cooling, selection and accumulation quadrupoles--significantly improved the sensitivity, dynamic range and mass measurement accuracy of the mass spectrometer. A high-pressure capillary liquid chromatography (LC) system was incorporated with an autosampler that enabled 24 h/day operation. A novel method for accumulating ions in the ICR cell was also developed. Unattended operation of the instrument revealed the exceptional reproducibility (1-5% deviation in elution times for peptides from a bacterial proteome), repeatability (10-20% deviation in detected abundances for peptides from the same aliquot analyzed a few weeks apart) and robustness (high-throughput operation for 5 months without downtime) of the LC/FTICR system. When combined with modulated-ion-energy gated trapping, the internal calibration of FTICR mass spectra decreased dispersion of mass measurement errors for peptide identifications in conjunction with high resolution capillary LC separations to < 5 ppm over a dynamic range for each spectrum of 10 3

  10. The quantitation of 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) in human urine specimens, a metabolite of LSD: comparative analysis using liquid chromatography-selected ion monitoring mass spectrometry and liquid chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Poch, G K; Klette, K L; Anderson, C

    2000-04-01

    This paper compares the potential forensic application of two sensitive and rapid procedures (liquid chromatography-mass spectrometry and liquid chromatography-ion trap mass spectrometry) for the detection and quantitation of 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) a major LSD metabolite. O-H-LSD calibration curves for both procedures were linear over the concentration range 0-8,000 pg/mL with correlation coefficients (r2) greater than 0.99. The observed limit of detection (LOD) and limit of quantitation (LOQ) for O-H-LSD in both procedures was 400 pg/mL. Sixty-eight human urine specimens that had previously been found to contain LSD by gas chromatography-mass spectrometry were reanalyzed by both procedures for LSD and O-H-LSD. These specimens contained a mean concentration of O-H-LSD approximately 16 times higher than the LSD concentration. Because both LC methods produce similar results, either procedure can be readily adapted to O-H-LSD analysis for use in high-volume drug-testing laboratories. In addition, the possibility of significantly increasing the LSD detection time window by targeting this major LSD metabolite for analysis may influence other drug-free workplace programs to test for LSD.

  11. Qualitative characteristics and comparison of volatile fraction of vodkas made from different botanical materials by comprehensive two-dimensional gas chromatography and the electronic nose based on the technology of ultra-fast gas chromatography.

    Science.gov (United States)

    Wiśniewska, Paulina; Śliwińska, Magdalena; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek

    2017-03-01

    Vodka is a spirit-based beverage made from ethyl alcohol of agricultural origin. At present, increasingly more vodka brands have labels that specify the botanical origin of the product. Until now, the techniques for distinguishing between vodkas of different botanical origin have been costly, time-consuming and insufficient for making a distinction between vodka produced from similar raw materials. Therefore, it is of utmost importance to find a fast and relatively inexpensive technique for conducting such tests. In the present study, we employed comprehensive two-dimensional gas chromatography (GC×GC) and an electronic nose based on the technology of ultra-fast GC with chemometric methods such as partial least square discriminant analysis, discriminant function analysis and soft independent modeling of class analogy. Both techniques allow a distinction between the vodkas produced from different raw materials. In the case of GC×GC, the differences between vodkas were more noticeable than in the analysis by electronic nose; however, the electronic nose allowed the significantly faster analysis of vodkas. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  12. Two-dimensional metamaterial optics

    International Nuclear Information System (INIS)

    Smolyaninov, I I

    2010-01-01

    While three-dimensional photonic metamaterials are difficult to fabricate, many new concepts and ideas in the metamaterial optics can be realized in two spatial dimensions using planar optics of surface plasmon polaritons. In this paper we review recent progress in this direction. Two-dimensional photonic crystals, hyperbolic metamaterials, and plasmonic focusing devices are demonstrated and used in novel microscopy and waveguiding schemes

  13. Application of High-Performance Liquid Chromatography Coupled with Linear Ion Trap Quadrupole Orbitrap Mass Spectrometry for Qualitative and Quantitative Assessment of Shejin-Liyan Granule Supplements

    OpenAIRE

    Jifeng Gu; Weijun Wu; Mengwei Huang; Fen Long; Xinhua Liu; Yizhun Zhu

    2018-01-01

    A method for high-performance liquid chromatography coupled with linear ion trap quadrupole Orbitrap high-resolution mass spectrometry (HPLC-LTQ-Orbitrap MS) was developed and validated for the qualitative and quantitative assessment of Shejin-liyan Granule. According to the fragmentation mechanism and high-resolution MS data, 54 compounds, including fourteen isoflavones, eleven ligands, eight flavonoids, six physalins, six organic acids, four triterpenoid saponins, two xanthones, two alkaloi...

  14. [Determination a variety of acidic gas in air of workplace by Ion Chromatography].

    Science.gov (United States)

    Li, Shiyong

    2014-10-01

    To establish a method for determination of a variety of acid gas in the workplace air by Ion Chromatography. (hydrofluoric acid, hydrogen chloride or hydrochloric acid, sulfur anhydride or sulfuric acid, phosphoric acid, oxalic acid). The sample in workplace air was collected by the porous glass plate absorption tube containing 5 ml leacheate. (Sulfuric acid fog, phosphoric acid aerosol microporous membrane after collection, eluted with 5 ml of eluent.) To separated by AS14+AG14 chromatography column, by carbonate (2.0+1.0) mmol/L (Na(2)CO(3)-NaHCO(3)) as eluent, flow rate of 1 ml/min, then analyzed by electrical conductivity detector. The retain time was used for qualitative and the peak area was used for quantitation. The each ion of a variety of acid gas in the air of workplace were excellent in carbonate eluent separation. The linear range of working curve of 0∼20 mg/L. The correlation coefficient r>0.999; lower detection limit of 3.6∼115 µg/L; quantitative limit of 0.012∼0.53 mg/L; acquisition of 15L air were measured, the minimum detection concentration is 0.004 0∼0.13 mg/m(3). The recovery rate is 99.7%∼101.1%. In the sample without mutual interference ions. Samples stored at room temperature for 7 days. The same analysis method, the detection of various acidic gases in the air of workplace, simple operation, good separation effect, high sensitivity, high detection efficiency, easy popularization and application.

  15. Organophosphorus pesticide and ester analysis by using comprehensive two-dimensional gas chromatography with flame photometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiangping; Li, Dengkun; Li, Jiequan [Nanjing Centre for Disease Control and Prevention, Zizhulin Street, Gulou 210003, Nanjing (China); Rose, Gavin [Department of Environment and Primary Industries, Macleod Centre, Ernest Jones Drive, Macleod, Vic 3085 (Australia); Marriott, Philip J., E-mail: philip.marriott@monash.edu [Australian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton 3800 (Australia)

    2013-12-15

    Highlights: • GC × GC-FPD(P-mode) was applied to detection of 37 phosphorus (P)-containing compounds. • The method improves resolution of P-compounds that coelute in the first dimension. • P-compounds are analyzed with excellent sensitivity supported by cryogenic modulation. • The FPD(P-mode) selectivity allows analysis in high hydrocarbon (H/C) matrix. • Soil samples and spiked chemical weapon compounds in H/C matrix are readily screened. -- Abstract: Thirty-seven phosphorus (P)-containing compounds comprising organophosphorus pesticides and organophosphate esters were analyzed by using comprehensive two-dimensional gas chromatography with flame photometric detection in P mode (GC × GC-FPD(P)), with a non-polar/moderately polar column set. A suitable modulation temperature and period was chosen based on experimental observation. A number of co-eluting peak pairs on the {sup 1}D column were well separated in 2D space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC × GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021–0.048 μmol L{sup −1}, and linear calibration correlation coefficients (R{sup 2}) for all 37 P-compounds were at least 0.998. The P-compounds were spiked in 2% diesel and good reproducibility for their response areas and retention times was obtained. Spiked recoveries were 88%–157% for 5 μg L{sup −1} and 80%–138% for 10 μg L{sup −1} spiked levels. Both {sup 1}t{sub R} and {sup 2}t{sub R} shifts were noted when the content of diesel was in excess of 5% in the matrix. Soil samples were analyzed by using the developed method; some P-compounds were positively detected. In general, this study shows that GC × GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples.

  16. Separation and screening of short-chain chlorinated paraffins in environmental samples using comprehensive two-dimensional gas chromatography with micro electron capture detection.

    Science.gov (United States)

    Xia, Dan; Gao, Lirong; Zhu, Shuai; Zheng, Minghui

    2014-11-01

    Short-chain chlorinated paraffins (SCCPs) are highly complex technical mixtures with thousands of isomers and numerous homologs. They are classified as priority candidate persistent organic pollutants under the Stockholm Convention for their persistence, bioaccumulation, and toxicity. Analyzing SCCPs is challenging because of the complexity of the mixtures. Chromatograms of SCCPs acquired using one-dimensional (1D) gas chromatography (GC) contain a large characteristic "peak" with a broad and unresolved profile. Comprehensive two-dimensional GC (GC×GC) shows excellent potential for separating complex mixtures. In this study, GC×GC coupled with micro electron capture detection (μECD) was used to separate and screen SCCPs. The chromatographic parameters, including the GC column types, oven temperature program, and modulation period, were systematically optimized. The SCCP congeners were separated into groups using a DM-1 column connected to a BPX-50 column. The SCCP congeners in technical mixtures were separated according to the number of chlorine substituents for a given carbon chain length and according to the number of carbon atoms plus chlorine atoms for different carbon chain lengths. A fish tissue sample was analyzed to illustrate the feasibility of the GC×GC-μECD method in analyzing biological samples. Over 1,500 compounds were identified in the fish extract, significantly more than were identified using 1D GC. The detection limits for five selected SCCP congeners were between 1 and 5 pg/L using the GC×GC method, and these were significantly lower than those achieved using 1D GC. This method is a good choice for analysis of SCCPs in environmental samples, exhibiting good separation and good sensitivity.

  17. Two-dimensional spatial structure of the dissipative trapped-electron mode

    International Nuclear Information System (INIS)

    Rewoldt, G.; Tang, W.M.; Frieman, E.A.

    1976-09-01

    This paper deals with the complete two-dimensional structure of the dissipative trapped-electron mode over its full width, which may extend over several mode-rational surfaces. The complete integro-differential equation is studied in the limit k/sub r/rho/sub i/ less than 1, where rho/sub i/ is the ion gyroradius, and k/sub r/, the radial wavenumber, is regarded as a differential operator. This is converted into a matrix equation which is then solved by standard numerical methods

  18. An algorithm to calculate secondary sputtering by the reflection of ions in two dimensions

    International Nuclear Information System (INIS)

    Smith, R.; Tagg, M.A.

    1986-01-01

    A method for computing the secondary sputtering of ions reflected from two-dimensional surfaces is described. The surface contour is first approximated by a set of line segments and the displacement of these line segments under ion erosion is determined computationally, by summing the contributions of the primary and reflected fluxes. This method can be used as an alternative to the method of characteristics which is normally used to determine primary ion beam effects. Some simple examples are evaluated. These examples illustrate that primary surface erosion theory is not in itself sufficient to explain the topography which can exist on an ion-eroded surface, particularly close to steep-sided structures. (author)

  19. Two-Dimensional MoS2-Based Zwitterionic Hydrophilic Interaction Liquid Chromatography Material for the Specific Enrichment of Glycopeptides.

    Science.gov (United States)

    Xia, Chaoshuang; Jiao, Fenglong; Gao, Fangyuan; Wang, Heping; Lv, Yayao; Shen, Yehua; Zhang, Yangjun; Qian, Xiaohong

    2018-06-05

    Mass spectrometry (MS)-based glycoproteomics research requires highly efficient sample preparation to eliminate interference from non-glycopeptides and to improve the efficiency of glycopeptide detection. In this work, a novel MoS 2 /Au-NP (gold nanoparticle)-L-cysteine nanocomposite was prepared for glycopeptide enrichment. The two-dimensional (2D) structured MoS 2 nanosheets served as a matrix that could provide a large surface area for immobilizing hydrophilic groups (such as L-cysteine) with low steric hindrance between the materials and the glycopeptides. As a result, the novel nanomaterial possessed an excellent ability to capture glycopeptides. Compared to commercial zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC) materials, the novel nanomaterials exhibited excellent enrichment performance with ultrahigh selectivity and sensitivity (approximately 10 fmol), high binding capacity (120 mg g -1 ), high enrichment recovery (more than 93%), satisfying batch-to-batch reproducibility, and good universality for glycopeptide enrichment. In addition, its outstanding specificity and efficiency for glycopeptide enrichment was confirmed by the detection of glycopeptides from an human serum immunoglobulin G (IgG) tryptic digest in quantities as low as a 1:1250 molar ratio of IgG tryptic digest to bovine serum albumin tryptic digest. The novel nanocomposites were further used for the analysis of complex samples, and 1920 glycopeptide backbones from 775 glycoproteins were identified in three replicate analyses of 50 μg of proteins extracted from HeLa cell exosomes. The resulting highly informative mass spectra indicated that this multifunctional nanomaterial-based enrichment method could be used as a promising tool for the in-depth and comprehensive characterization of glycoproteomes in MS-based glycoproteomics.

  20. Comparison of comprehensive two-dimensional gas chromatography coupled with sulfur-chemiluminescence detector to standard methods for speciation of sulfur-containing compounds in middle distillates.

    Science.gov (United States)

    Ruiz-Guerrero, Rosario; Vendeuvre, Colombe; Thiébaut, Didier; Bertoncini, Fabrice; Espinat, Didier

    2006-10-01

    The monitoring of total sulfur content and speciation of individual sulfur-containing compounds in middle distillates is required for efficient catalyst selection and for a better understanding of the kinetics of the reactions involved in hydrotreament processes. Owing to higher resolution power and enhanced sensitivity, comprehensive two-dimensional gas chromatography (GCxGC) hyphenated to sulfur chemiluminescence detection (SCD) has recently evolved as a powerful tool for improving characterization and identification of sulfur compounds. The aim of this paper is to compare quantitatively GCxGC-SCD and various other methods commonly employed in the petroleum industry, such as X-ray fluorescence, conventional GC-SCD, and high-resolution mass spectrometry, for total sulfur content determination and speciation analysis. Different samples of middle distillates have been analyzed to demonstrate the high potential and important advantages of GCxGC-SCD for innovative and quantitative analysis of sulfur-containing compounds. More accurate and detailed results for benzothiophenes and dibenzothiophenes are presented, showing that GCxGC-SCD should become, in the future, an essential tool for sulfur speciation analysis.

  1. One- and two-dimensional chemical exchange nuclear magnetic resonance studies of the creatine kinase catalyzed reaction

    International Nuclear Information System (INIS)

    Gober, J.R.

    1988-01-01

    The equilibrium chemical exchange dynamics of the creatine kinase enzyme system were studied by one- and two-dimensional 31 P NMR techniques. Pseudo-first-order reaction rate constants were measured by the saturation transfer method under an array of experimental conditions of pH and temperature. Quantitative one-dimensional spectra were collected under the same conditions in order to calculate the forward and reverse reaction rates, the K eq , the hydrogen ion stoichiometry, and the standard thermodynamic functions. The pure absorption mode in four quadrant two-dimensional chemical exchange experiment was employed so that the complete kinetic matrix showing all of the chemical exchange process could be realized

  2. Systematic generation of buffer systems for pH gradient ion exchange chromatography and their application.

    Science.gov (United States)

    Kröner, Frieder; Hubbuch, Jürgen

    2013-04-12

    pH gradient protein separations are widely used techniques in the field of protein analytics, of which isoelectric focusing is the most well known application. The chromatographic variant, based on the formation of pH gradients in ion exchange columns is only rarely applied due to the difficulties to form controllable, linear pH gradients over a broad pH range. This work describes a method for the systematic generation of buffer compositions with linear titration curves, resulting in well controllable pH gradients. To generate buffer compositions with linear titration curves an in silico method was successfully developed. With this tool, buffer compositions for pH gradient ion exchange chromatography with pH ranges spanning up to 7.5 pH units were established and successfully validated. Subsequently, the buffer systems were used to characterize the elution behavior of 22 different model proteins in cation and anion exchange pH gradient chromatography. The results of both chromatographic modes as well as isoelectric focusing were compared to describe differences in between the methods. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Negative refraction at infrared wavelengths in a two-dimensional photonic crystal

    International Nuclear Information System (INIS)

    Berrier, A.; Mulot, M.; Swillo, M.; Qiu, M.; Thylen, L.; Anand, S.; Talneau, A.

    2004-01-01

    We report on the first experimental evidence of negative refraction at telecommunication wavelengths by a two-dimensional photonic crystal field. Samples were fabricated by chemically assisted ion beam etching in the InP-based low-index constrast system. Experiments of beam imaging and light collection show light focusing by the photonic crystal field. Finite-difference time-domain simulations confirm that the observed focusing is due to negative refraction in the photonic crystal area

  4. SnSe2 Two Dimensional Anodes for Advanced Sodium Ion Batteries

    KAUST Repository

    Zhang, Fan

    2017-01-01

    Sodium-ion batteries (SIBs) are considered as a promising alternative to lithium-ion batteries (LIBs) for large-scale renewable energy storage units due to the abundance of sodium resource and its low cost. However, the development of anode

  5. Application of ion chromatography for the determination of inorganic ions, especially thiocyanates in human saliva samples as biomarkers of environmental tobacco smoke exposure.

    Science.gov (United States)

    Demkowska, Ilona; Polkowska, Zaneta; Namieśnik, Jacek

    2008-11-15

    Environmental tobacco smoke is a major factor influencing the indoor air quality. Various toxic compounds emitted during tobacco smoking into the environment have a significant influence on the chemical composition of human biological fluids. The thiocyanate concentration in saliva is a biochemical measure, frequently used as an objective indicator of tobacco consumption. The goal of this study was to find significant relationships between salivary thiocyanates and other inorganic ions, which are constituents of natural saliva (Na(+), K(+), Mg(2+), Ca(2+), Cl(-), PO(4)(3-)) and to present the effectiveness of the proposed sample preparation procedure combined with ion chromatography technique for the determination of inorganic ions in human saliva samples collected from passive, moderate and heavy smokers.

  6. On-line separation of Pu(III) and Am(III) using extraction and ion chromatography

    International Nuclear Information System (INIS)

    Jernstroem, J.; Lehto, J.; Betti, M.

    2007-01-01

    An on-line method developed for separating plutonium and americium was developed. The method is based on the use of HPLC pump with three analytical chromatographic columns. Plutonium is reduced throughout the procedure to trivalent oxidation state, and is recovered in the various separation steps together with americium. Light lanthanides and trivalent actinides are separated with TEVA resin in thiocyanate/formic acid media. Trivalent plutonium and americium are pre-concentrated in a TCC-II cation-exchange column, after which the separation is performed in CS5A ion chromatography column by using two different eluents. Pu(III) is eluted with a dipicolinic acid eluent, and Am(III) with oxalic acid eluent. Radiochemical and chemical purity of the eluted plutonium and americium fractions were ensured with alpha-spectrometry. (author)

  7. Power of Ultra Performance Liquid Chromatography/Electrospray Ionization-MS Reconstructed Ion Chromatograms in the Characterization of Small Differences in Polymer Microstructure.

    Science.gov (United States)

    Epping, Ruben; Panne, Ulrich; Falkenhagen, Jana

    2018-03-06

    From simple homopolymers to functionalized, 3-dimensional structured copolymers, the complexity of polymeric materials has become more and more sophisticated. With new applications, for instance, in the semiconductor or pharmaceutical industry, the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isomeric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector but affect the properties of materials significantly. For a drug delivery system, for example, the degree of branching and branching distribution is crucial for the formation of micelles. Instead of a complicated, time-consuming, and/or expensive 2D-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, in this work, a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization (ESI) mass spectrometry is proposed. The online coupling allows the analysis of reconstructed ion chromatograms (RICs) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities. Although some microstructural heterogeneities like short chain branching can for large polymers be characterized with methods such as light scattering, for oligomers where the heterogeneities just start to form and their influence is at the maximum, they are inaccessible with these methods. It is also shown that with a proper calibration even quantitative information can be obtained. This method is suitable to detect small differences in, e.g., branching, 3D-structure, monomer sequence, or tacticity and could potentially be used in routine analysis to quickly determine deviations.

  8. Verification of frequency scaling laws for capacitive radio-frequency discharges using two-dimensional simulations

    International Nuclear Information System (INIS)

    Vahedi, V.; Birdsall, C.K.; Lieberman, M.A.; DiPeso, G.; Rognlien, T.D.

    1993-01-01

    Weakly ionized processing plasmas are studied in two dimensions using a bounded particle-in-cell (PIC) simulation code with a Monte Carlo collision (MCC) package. The MCC package models the collisions between charged and neutral particles, which are needed to obtain a self-sustained plasma and the proper electron and ion energy loss mechanisms. A two-dimensional capacitive radio-frequency (rf) discharge is investigated in detail. Simple frequency scaling laws for predicting the behavior of some plasma parameters are derived and then compared with simulation results, finding good agreements. It is found that as the drive frequency increases, the sheath width decreases, and the bulk plasma becomes more uniform, leading to a reduction of the ion angular spread at the target and an improvement of ion dose uniformity at the driven electrode

  9. Detection of structurally similar adulterants in botanical dietary supplements by thin-layer chromatography and surface enhanced Raman spectroscopy combined with two-dimensional correlation spectroscopy.

    Science.gov (United States)

    Li, Hao; Zhu, Qing xia; Chwee, Tsz sian; Wu, Lin; Chai, Yi feng; Lu, Feng; Yuan, Yong fang

    2015-07-09

    Thin-layer chromatography (TLC) coupled with surface enhanced Raman spectroscopy (SERS) has been widely used for the study of various complex systems, especially for the detection of adulterants in botanical dietary supplements (BDS). However, this method is not sufficient to distinguish structurally similar adulterants in BDS since the analogs have highly similar chromatographic and/or spectroscopic behaviors. Taking into account the fact that higher cost and more time will be required for comprehensive chromatographic separation, more efforts with respect to spectroscopy are now focused on analyzing the overlapped SERS peaks. In this paper, the combination of a TLC-SERS method with two-dimensional correlation spectroscopy (2DCOS), with duration of exposure to laser as the perturbation, is applied to solve this problem. Besides the usual advantages of the TLC-SERS method, such as its simplicity, rapidness, and sensitivity, more advantages are presented here, such as enhanced selectivity and good reproducibility, which are obtained by 2DCOS. Two chemicals with similar structures are successfully differentiated from the complex BDS matrices. The study provides a more accurate qualitative screening method for detection of BDS with adulterants, and offers a new universal approach for the analysis of highly overlapped SERS peaks. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Automating data analysis for two-dimensional gas chromatography/time-of-flight mass spectrometry non-targeted analysis of comparative samples.

    Science.gov (United States)

    Titaley, Ivan A; Ogba, O Maduka; Chibwe, Leah; Hoh, Eunha; Cheong, Paul H-Y; Simonich, Staci L Massey

    2018-03-16

    Non-targeted analysis of environmental samples, using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC/ToF-MS), poses significant data analysis challenges due to the large number of possible analytes. Non-targeted data analysis of complex mixtures is prone to human bias and is laborious, particularly for comparative environmental samples such as contaminated soil pre- and post-bioremediation. To address this research bottleneck, we developed OCTpy, a Python™ script that acts as a data reduction filter to automate GC × GC/ToF-MS data analysis from LECO ® ChromaTOF ® software and facilitates selection of analytes of interest based on peak area comparison between comparative samples. We used data from polycyclic aromatic hydrocarbon (PAH) contaminated soil, pre- and post-bioremediation, to assess the effectiveness of OCTpy in facilitating the selection of analytes that have formed or degraded following treatment. Using datasets from the soil extracts pre- and post-bioremediation, OCTpy selected, on average, 18% of the initial suggested analytes generated by the LECO ® ChromaTOF ® software Statistical Compare feature. Based on this list, 63-100% of the candidate analytes identified by a highly trained individual were also selected by OCTpy. This process was accomplished in several minutes per sample, whereas manual data analysis took several hours per sample. OCTpy automates the analysis of complex mixtures of comparative samples, reduces the potential for human error during heavy data handling and decreases data analysis time by at least tenfold. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Thermal structure of the ionosphere of Mars - simulations with one- and two-dimensional models

    International Nuclear Information System (INIS)

    Singhal, R.P.; Whitten, R.C.

    1988-01-01

    Heat flux saturation effects are included in the present one- and two-dimensional models of the Martian upper ionosphere's thermal structure. The inclusion of small upper boundary and volume heat sources is found to yield satisfactory simulations of the dayside ion temperature observation results obtained by Viking 1's retarding potential analyzers. It is noted that the plasma flow-transport of heat from the dayside to the nightside makes no contribution to the ion and electron temperatures that have been calculated for the nightside. 22 references

  12. Fractional calculus phenomenology in two-dimensional plasma models

    Science.gov (United States)

    Gustafson, Kyle; Del Castillo Negrete, Diego; Dorland, Bill

    2006-10-01

    Transport processes in confined plasmas for fusion experiments, such as ITER, are not well-understood at the basic level of fully nonlinear, three-dimensional kinetic physics. Turbulent transport is invoked to describe the observed levels in tokamaks, which are orders of magnitude greater than the theoretical predictions. Recent results show the ability of a non-diffusive transport model to describe numerical observations of turbulent transport. For example, resistive MHD modeling of tracer particle transport in pressure-gradient driven turbulence for a three-dimensional plasma reveals that the superdiffusive (2̂˜t^α where α> 1) radial transport in this system is described quantitatively by a fractional diffusion equation Fractional calculus is a generalization involving integro-differential operators, which naturally describe non-local behaviors. Our previous work showed the quantitative agreement of special fractional diffusion equation solutions with numerical tracer particle flows in time-dependent linearized dynamics of the Hasegawa-Mima equation (for poloidal transport in a two-dimensional cold-ion plasma). In pursuit of a fractional diffusion model for transport in a gyrokinetic plasma, we now present numerical results from tracer particle transport in the nonlinear Hasegawa-Mima equation and a planar gyrokinetic model. Finite Larmor radius effects will be discussed. D. del Castillo Negrete, et al, Phys. Rev. Lett. 94, 065003 (2005).

  13. The quantification of short-chain chlorinated paraffins in sediment samples using comprehensive two-dimensional gas chromatography with μECD detection.

    Science.gov (United States)

    Muscalu, Alina M; Morse, Dave; Reiner, Eric J; Górecki, Tadeusz

    2017-03-01

    The analysis of persistent organic pollutants in environmental samples is a challenge due to the very large number of compounds with varying chemical and physical properties. Chlorinated paraffins (CPs) are complex mixtures of chlorinated n-alkanes with varying chain lengths (C 10 to C 30 ) and degree of chlorination (30 to 70% by weight). Their physical-chemical properties make these compounds persistent in the environment and able to bioaccumulate in living organisms. Comprehensive two-dimensional gas chromatography (GC × GC) coupled with micro-electron capture detection (μECD) was used to separate and quantify short-chain chlorinated paraffins (SCCP) in sediment samples. Distinct ordered bands were observed in the GC × GC chromatograms pointing to group separation. Using the Classification function of the ChromaTOF software, summary tables were generated to determine total area counts to set up multilevel-calibration curves for different technical mixes. Fortified sediment samples were analyzed by GC × GC-μECD with minimal extraction and cleanup. Recoveries ranged from 120 to 130%. To further validate the proposed method for the analysis of SCCPs, the laboratory participated in interlaboratory studies for the analysis of standards and sediment samples. The results showed recoveries between 75 and 95% and z-score values <2, demonstrating that the method is suitable for the analysis of SCCPs in soil/sediment samples. Graphical abstract Quantification of SCCPs by 2D-GC-μECD.

  14. A novel multidimensional protein identification technology approach combining protein size exclusion prefractionation, peptide zwitterion-ion hydrophilic interaction chromatography, and nano-ultraperformance RP chromatography/nESI-MS2 for the in-depth analysis of the serum proteome and phosphoproteome: application to clinical sera derived from humans with benign prostate hyperplasia.

    Science.gov (United States)

    Garbis, Spiros D; Roumeliotis, Theodoros I; Tyritzis, Stavros I; Zorpas, Kostas M; Pavlakis, Kitty; Constantinides, Constantinos A

    2011-02-01

    The current proof-of-principle study was aimed toward development of a novel multidimensional protein identification technology (MudPIT) approach for the in-depth proteome analysis of human serum derived from patients with benign prostate hyperplasia (BPH) using rational chromatographic design principles. This study constituted an extension of our published work relating to the identification and relative quantification of potential clinical biomarkers in BPH and prostate cancer (PCa) tissue specimens. The proposed MudPIT approach encompassed the use of three distinct yet complementary liquid chromatographic chemistries. High-pressure size-exclusion chromatography (SEC) was used for the prefractionation of serum proteins followed by their dialysis exchange and solution phase trypsin proteolysis. The tryptic peptides were then subjected to offline zwitterion-ion hydrophilic interaction chromatography (ZIC-HILIC) fractionation followed by their online analysis with reversed-phase nano-ultraperformance chromatography (RP-nUPLC) hyphenated to nanoelectrospray ionization-tandem mass spectrometry using an ion trap mass analyzer. For the spectral processing, the sequential use of the SpectrumMill, Scaffold, and InsPecT software tools was applied for the tryptic peptide product ion MS(2) spectral processing, false discovery rate (FDR) assessment, validation, and protein identification. This milestone serum analysis study allowed the confident identification of over 1955 proteins (p ≤ 0.05; FDR ≤ 5%) with a broad spectrum of biological and physicochemical properties including secreted, tissue-specific proteins spanning approximately 12 orders of magnitude as they occur in their native abundance levels in the serum matrix. Also encompassed in this proteome was the confident identification of 375 phosphoproteins (p ≤ 0.05; FDR ≤ 5%) with potential importance to cancer biology. To demonstrate the performance characteristics of this novel MudPIT approach, a comparison

  15. Algorithm for statistical noise reduction in three-dimensional ion implant simulations

    International Nuclear Information System (INIS)

    Hernandez-Mangas, J.M.; Arias, J.; Jaraiz, M.; Bailon, L.; Barbolla, J.

    2001-01-01

    As integrated circuit devices scale into the deep sub-micron regime, ion implantation will continue to be the primary means of introducing dopant atoms into silicon. Different types of impurity profiles such as ultra-shallow profiles and retrograde profiles are necessary for deep submicron devices in order to realize the desired device performance. A new algorithm to reduce the statistical noise in three-dimensional ion implant simulations both in the lateral and shallow/deep regions of the profile is presented. The computational effort in BCA Monte Carlo ion implant simulation is also reduced

  16. Detailed analysis and group-type separation of natural fats and oils using comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Mondello, Luigi; Casilli, Alessandro; Tranchida, Peter Quinto; Dugo, Paola; Dugo, Giovanni

    2003-11-26

    Comprehensive gas chromatography (GC x GC) is an adequate methodology for the separation and identification of very complex samples. It is based on the coupling of two capillary columns that each give a different but substantial contribution to the unprecedented resolving power of this technique. The 2D space chromatograms that derive from GC x GC analysis have great potential for identification. This is due to the fact that the contour plot positions, pinpointed by two retention time coordinates, give characteristic patterns for specific families of compounds that can be mathematically translated. This investigation concerned the application of this principle to fatty acid methyl esters that were grouped on an equal double bond number basis. The ester samples were derived from various lipids and all underwent bidimensional analysis on two sets of columns. Peak attribution was supported by mass spectra, linear retention indices and information reported in the literature.

  17. Two-dimensional structure of poly[[[μ2-1,4-bis(pyridin-4-ylbutane]bis(μ4-pentanedioatodicopper(II] acetonitrile disolvate

    Directory of Open Access Journals (Sweden)

    Do Nam Lee

    2017-10-01

    Full Text Available In the title compound, {[Cu2(μ4-C5H6O42(μ2-C14H16N2]·2CH3CN}n, the Cu2 dinuclear units are connected by glutartate ligands, forming one-dimensional double chains. These chains, are in turn bridged by 1,4-bis(pyridin-4-ylbutane ligands to form a two-dimensional layer structure parallel to (112. The carboxylate groups of the glutarate ligand bridge two copper(II ions, forming a paddle-wheel-type Cu2(CO24 dinuclear secondary building unit. A crystallographic inversion centre is located midway between two CuII ions, with a Cu...Cu distance of 2.639 (3 Å. The coordination geometry of the unique CuII ion is slightly disorted square pyramidal, formed by four equatorial carboxylate O atoms and an axial pyridyl N atom.

  18. Ion acoustic waves in one- and two-negative ion species plasmas

    International Nuclear Information System (INIS)

    Ichiki, Ryuta; Shindo, Masako; Yoshimura, Shinji; Watanabe, Tsuguhiro; Kawai, Yoshinobu

    2001-01-01

    Ion acoustic waves in multi-ion plasmas including two negative ion species are investigated both numerically and experimentally. Numerically, the kinetic dispersion relation in two-negative ion plasmas is investigated. There are three modes of the ion acoustic waves in two-negative ion plasmas. In an Ar + -F - -SF 6 - plasma, only one of the three modes is dominant, regardless of the values of the electron and the ion temperatures. In a Xe + -F - -SF 6 - plasma, on the other hand, two modes can be important for a certain range of the electron-ion temperature ratio. The results also imply the possibility of the coexistence of the fast mode and the slow mode in one-negative ion plasmas. Experimentally, ion acoustic waves are observed in an Ar + -F - -SF 6 - plasma and are found to show a mode transition that agrees with the theoretical prediction for one of the three ion acoustic modes

  19. Multi-dimensional microanalysis of masklessly implanted atoms using focused heavy ion beam

    International Nuclear Information System (INIS)

    Mokuno, Yoshiaki; Iiorino, Yuji; Chayahara, Akiyoshi; Kiuchi, Masato; Fujii, Kanenaga; Satou, Mamoru

    1992-01-01

    Multi-dimensional structure fabricated by maskless MeV gold implantation in silicon wafer was analyzed by 3 MeV carbon ion microprobe using a microbeam line developed at GIRIO. The minimum line width of the implanted region was estimated to be about 5 μm. The advantages of heavy ions for microanalysis were demonstrated. (author)

  20. A size exclusion-reversed phase two dimensional-liquid chromatography methodology for stability and small molecule related species in antibody drug conjugates.

    Science.gov (United States)

    Li, Yi; Gu, Christine; Gruenhagen, Jason; Zhang, Kelly; Yehl, Peter; Chetwyn, Nik P; Medley, Colin D

    2015-05-08

    Antibody drug conjugates (ADCs) are complex therapeutic agents combining the specific targeting properties of antibodies and highly potent cytotoxic small molecule drugs to selectively eliminate tumor cells while limiting the toxicity to normal healthy tissues. One unique critical quality attribute of ADCs is the content of unconjugated small molecule drug present from either incomplete conjugation or degradation of the ADC. In this work, size exclusion chromatography (SEC) was coupled with reversed-phase (RP) HPLC in an online 2-dimensional chromatography format for identification and quantitation of unconjugated small molecule drugs and related small molecule impurities in ADC samples directly without sample preparation. The SEC method in the 1st dimension not only separated the small molecule impurities from the intact ADC, but also provided information about the size variants (monomer, dimer, aggregates, etc.) of the ADC. The small molecule peak from the SEC was trapped and sent to a RP-HPLC in the 2nd dimension to further separate and quantify the different small molecule impurities present in the ADC sample. This SEC-RP 2D-LC method demonstrated excellent precision (%RSDmolecule degradation products and aggregation of the conjugate were observed in the stability samples and the degradation pathways of the ADC were investigated. This 2D-LC method offers a powerful tool for ADC characterization and provides valuable information for conjugation and formulation development. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    International Nuclear Information System (INIS)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

    2014-01-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag + ) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg −1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm

  2. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A., E-mail: joseph.caruso@uc.edu; Landero-Figueroa, Julio

    2014-10-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag{sup +}) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg{sup −1} detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

  3. A large area two-dimensional position sensitive multiwire proportional detector

    CERN Document Server

    Moura, M M D; Souza, F A; Alonso, E E; Fujii, R J; Meyknecht, A B; Added, N; Aissaoui, N; Cardenas, W H Z; Ferraretto, M D; Schnitter, U; Szanto, E M; Szanto de Toledo, A; Yamamura, M S; Carlin, N

    1999-01-01

    Large area two-dimensional position sensitive multiwire proportional detectors were developed to be used in the study of light heavy-ion nuclear reactions at the University of Sao Paulo Pelletron Laboratory. Each detector has a 20x20 cm sup 2 active area and consists of three grids (X-position, anode and Y-position) made of 25 mu m diameter gold plated tungsten wires. The position is determined through resistive divider chains. Results for position resolution, linearity and efficiency as a function of energy and position for different elements are reported.

  4. On the two-dimensional Saigo-Maeda fractional calculus asociated with two-dimensional Aleph TRANSFORM

    Directory of Open Access Journals (Sweden)

    Dinesh Kumar

    2013-11-01

    Full Text Available This paper deals with the study of two-dimensional Saigo-Maeda operators of Weyl type associated with Aleph function defined in this paper. Two theorems on these defined operators are established. Some interesting results associated with the H-functions and generalized Mittag-Leffler functions are deduced from the derived results. One dimensional analog of the derived results is also obtained.

  5. Quantitative analysis of essential oils in perfume using multivariate curve resolution combined with comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    de Godoy, Luiz Antonio Fonseca; Hantao, Leandro Wang; Pedroso, Marcio Pozzobon; Poppi, Ronei Jesus; Augusto, Fabio

    2011-08-05

    The use of multivariate curve resolution (MCR) to build multivariate quantitative models using data obtained from comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC-FID) is presented and evaluated. The MCR algorithm presents some important features, such as second order advantage and the recovery of the instrumental response for each pure component after optimization by an alternating least squares (ALS) procedure. A model to quantify the essential oil of rosemary was built using a calibration set containing only known concentrations of the essential oil and cereal alcohol as solvent. A calibration curve correlating the concentration of the essential oil of rosemary and the instrumental response obtained from the MCR-ALS algorithm was obtained, and this calibration model was applied to predict the concentration of the oil in complex samples (mixtures of the essential oil, pineapple essence and commercial perfume). The values of the root mean square error of prediction (RMSEP) and of the root mean square error of the percentage deviation (RMSPD) obtained were 0.4% (v/v) and 7.2%, respectively. Additionally, a second model was built and used to evaluate the accuracy of the method. A model to quantify the essential oil of lemon grass was built and its concentration was predicted in the validation set and real perfume samples. The RMSEP and RMSPD obtained were 0.5% (v/v) and 6.9%, respectively, and the concentration of the essential oil of lemon grass in perfume agreed to the value informed by the manufacturer. The result indicates that the MCR algorithm is adequate to resolve the target chromatogram from the complex sample and to build multivariate models of GC×GC-FID data. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. A novel one-dimensional chain built of vanadyl ions and pyrazine-2,5-dicarboxylate

    NARCIS (Netherlands)

    Lankelma, M.; de Boer, J.; Ferbinteanu, M.; Dantas Ramos, A.L.; Tanasa, R.; Rothenberg, G.; Tanase, S.

    2015-01-01

    We present a new coordination polymer, {[VO(pzdc)(H2O)(2)] H2O}(n), built from vanadyl and pyrazine-2,5-dicarboxylate (pzdc) ions. It consists of a one-dimensional chain of vanadyl ions linked by pzdc ions. The carboxylate groups show monodentate coordination, while the pyrazine ring is present both

  7. Analysis of N-nitrosodiethylamine by ion chromatography coupled with UV photolysis pretreatment

    Directory of Open Access Journals (Sweden)

    Xueli Li

    2016-04-01

    Full Text Available Nitrosamines such as N-nitrosodiethylamine (NDEA are commonly detected by spectrophotometry after photolysis and Griess reaction (PG in food industries for lower cost. Results of this research indicate that NDEA decays rapidly under UV irradiation, and concentrations of the generated NO2− and NO3− ions vary with photolysis conditions. Thus, the measurement of the PG method may be inconsistent because it is based on the amount of photoproduced NO2−. In addition, more errors may be present in the PG method since NO3− cannot be measured colorimetrically using Griess reagent. In this work, the sum of the concentrations of photoproduced NO2− and NO3− was found to be equivalent to the initial NDEA before photolysis, and a photolysis–ion chromatography method was validated, which may serve as a feasible and accurate method to determine nitrosamines.

  8. An Advanced Analytical Chemistry Experiment Using Gas Chromatography-Mass Spectrometry, MATLAB, and Chemometrics to Predict Biodiesel Blend Percent Composition

    Science.gov (United States)

    Pierce, Karisa M.; Schale, Stephen P.; Le, Trang M.; Larson, Joel C.

    2011-01-01

    We present a laboratory experiment for an advanced analytical chemistry course where we first focus on the chemometric technique partial least-squares (PLS) analysis applied to one-dimensional (1D) total-ion-current gas chromatography-mass spectrometry (GC-TIC) separations of biodiesel blends. Then, we focus on n-way PLS (n-PLS) applied to…

  9. 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.

  10. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo, E-mail: jbwan@umac.mo

    2016-07-13

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. - Highlights: • An UHPLC/Q-TOF tsMIM MS-based pseudotargeted metabolomics was proposed. • Compared to full scan, the improved method exhibits better repeatability and a wider linear range. • The proposed method could achieve pseudotargeted analysis on one UHPLC/Q-TOF/MS instrument. • The developed method was successfully used to discover biomarkers for alcohol-induced liver injury.

  11. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo

    2016-01-01

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. - Highlights: • An UHPLC/Q-TOF tsMIM MS-based pseudotargeted metabolomics was proposed. • Compared to full scan, the improved method exhibits better repeatability and a wider linear range. • The proposed method could achieve pseudotargeted analysis on one UHPLC/Q-TOF/MS instrument. • The developed method was successfully used to discover biomarkers for alcohol-induced liver injury.

  12. Two-dimensional nuclear magnetic resonance spectroscopy

    International Nuclear Information System (INIS)

    Bax, A.; Lerner, L.

    1986-01-01

    Great spectral simplification can be obtained by spreading the conventional one-dimensional nuclear magnetic resonance (NMR) spectrum in two independent frequency dimensions. This so-called two-dimensional NMR spectroscopy removes spectral overlap, facilitates spectral assignment, and provides a wealth of additional information. For example, conformational information related to interproton distances is available from resonance intensities in certain types of two-dimensional experiments. Another method generates 1 H NMR spectra of a preselected fragment of the molecule, suppressing resonances from other regions and greatly simplifying spectral appearance. Two-dimensional NMR spectroscopy can also be applied to the study of 13 C and 15 N, not only providing valuable connectivity information but also improving sensitivity of 13 C and 15 N detection by up to two orders of magnitude. 45 references, 10 figures

  13. Separation techniques: Chromatography

    Science.gov (United States)

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  14. Ion chromatography of transition metals: specific alteration of retention by complexation reactions in the mobile and on the stationary phase

    International Nuclear Information System (INIS)

    Baumgartner, S.

    1992-05-01

    Ion chromatography of mono- and bivalent cations was performed on a conventional cation exchanger. The pH influence of an ethylene-diamine/citrate eluent was significant for the retention of alkaline earth and transition metals, but negligible for alkali ions. This was dealt with from a mechanistic point of view. Mobile phase optimization allowed fast isocratic analysis of mono- and bivalent cations and the separation of the radionuclides Cs-137 and Sr-90. A newly synthesized stationary phase containing iminodiacetate (IDA) function was investigated for cation chromatography using ethylenediamine/citrate eluents, polyhydroxy acid and dipicolinic acid. The column's high selectivity for transition metal ions in comparison to alkali and alkaline earth metals may be governed by the choice of complexing ability and pH of the eluent. Applications verified by atomic absorption spectroscopy include alkaline earth metals in beverages and the determination of Co, Cd and Zn in solutions containing more than 10 14 -fold excess of Na and Mg, such as sea water

  15. IDENTIFICATION OF MICROCYSTIN TOXINS FROM A STRAIN OF MICROCYSTIS AERUGINOSA BY LIQUID CHROMATOGRAPHY INTRODUCTION INTO A HYBRID LINEAR ION TRAP-FOURIER TRANSFORM ION CYCLOTRON RESONANCE MASS SPECTROMETER

    Science.gov (United States)

    The cyclic heptapeptide microcystin toxins produced by a strain of Microcystis aeruginosa that has not been investigated previously were separated by liquid chromatography and identified by high-accuracy m/z measurements of their [M + H]+ ions and the fragment i...

  16. Measurement of radionuclides using ion chromatography and flow-cell scintillation counting with pulse shape discrimination

    International Nuclear Information System (INIS)

    DeVol, T.A.; Fjeld, R.A.

    1995-01-01

    The use of ion chromatography (IC) for radiochemical separations is a well established technique. IC is commonly used in routine environmental monitoring applications as well as in specialized research applications. Typical usage involves the separation of a single radionuclide from the non-radioactive constituents. During the past decade, a limited amount of research has been conducted using automated IC systems in actinide separation applications (e.g.). More recently, separation procedures for common non-gamma emitting activation and fission products were developed utilizing a high performance liquid chromatography (HPLC) system. In addition, a separation procedure for six common actinides has been developed using a HPLC system. These latter systems used on-line flow-cell detectors for quantification of the radioactive constituents of the effluent stream

  17. Liquid Chromatography in 1982.

    Science.gov (United States)

    Freeman, David H.

    1982-01-01

    Reviews trends in liquid chromatography including apparatus, factors affecting efficient separation of a mixture (peak sharpness and speed), simplified problem-solving, adsorption, bonded phase chromatography, ion selectivity, and size exclusion. The current trend is to control chemical selectivity by the liquid phase. (Author/JN)

  18. On some classes of two-dimensional local models in discrete two-dimensional monatomic FPU lattice with cubic and quartic potential

    International Nuclear Information System (INIS)

    Quan, Xu; Qiang, Tian

    2009-01-01

    This paper discusses the two-dimensional discrete monatomic Fermi–Pasta–Ulam lattice, by using the method of multiple-scale and the quasi-discreteness approach. By taking into account the interaction between the atoms in the lattice and their nearest neighbours, it obtains some classes of two-dimensional local models as follows: two-dimensional bright and dark discrete soliton trains, two-dimensional bright and dark line discrete breathers, and two-dimensional bright and dark discrete breather. (condensed matter: structure, thermal and mechanical properties)

  19. Characterization of Chemical Composition of Pericarpium Citri Reticulatae Volatile Oil by Comprehensive Two-Dimensional Gas Chromatography with High-Resolution Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Kunming Qin

    2013-01-01

    Full Text Available Pericarpium Citri Reticulatae (Chenpi in Chinese has been widely used as an herbal medicine in Korea, China, and Japan. Chenpi extracts are used to treat indigestion and inflammatory syndromes of the respiratory tract such as bronchitis and asthma. This thesis will analyze chemical compositions of Chenpi volatile oil, which was performed by comprehensive two-dimensional gas chromatography with high-resolution time-of-flight mass spectrometry (GC × GC-HR-TOFMS. One hundred and sixty-seven components were tentatively identified, and terpene compounds are the main components of Chenpi volatile oil, a significant larger number than in previous studies. The majority of the eluted compounds, which were identified, were well separated as a result of high-resolution capability of the GC × GC method, which significantly reduces, the coelution. β-Elemene is tentatively qualified by means of GC × GC in tandem with high-resolution TOFMS detection, which plays an important role in enhancing the effects of many anticancer drugs and in reducing the side effects of chemotherapy. This study suggests that GC × GC-HR-TOFMS is suitable for routine characterization of chemical composition of volatile oil in herbal medicines.

  20. Two-dimensional models

    International Nuclear Information System (INIS)

    Schroer, Bert; Freie Universitaet, Berlin

    2005-02-01

    It is not possible to compactly review the overwhelming literature on two-dimensional models in a meaningful way without a specific viewpoint; I have therefore tacitly added to the above title the words 'as theoretical laboratories for general quantum field theory'. I dedicate this contribution to the memory of J. A. Swieca with whom I have shared the passion of exploring 2-dimensional models for almost one decade. A shortened version of this article is intended as a contribution to the project 'Encyclopedia of mathematical physics' and comments, suggestions and critical remarks are welcome. (author)

  1. Biomarker discovery in low-grade breast cancer using isobaric stable isotope tags and two-dimensional liquid chromatography-tandem mass spectrometry (iTRAQ-2DLC-MS/MS) based quantitative proteomic analysis.

    Science.gov (United States)

    Bouchal, Pavel; Roumeliotis, Theodoros; Hrstka, Roman; Nenutil, Rudolf; Vojtesek, Borivoj; Garbis, Spiros D

    2009-01-01

    The present pilot study constitutes a proof-of-principle in the use of a quantitative LC-MS/MS based proteomic method for the comparative analysis of representative low-grade breast primary tumor tissues with and without metastases and metastasis in lymph node relative to the nonmetastatic tumor type. The study method incorporated iTRAQ stable isotope labeling, two-dimensional liquid chromatography, nanoelectrospray ionization and high resolution tandem mass spectrometry using the hybrid QqTOF platform (iTRAQ-2DLC-MS/MS). The principal aims of this study were (1) to define the protein spectrum obtainable using this approach, and (2) to highlight potential candidates for verification and validation studies focused on biomarkers involved in metastatic processes in breast cancer. The study resulted in the reproducible identification of 605 nonredundant proteins (p biomarker discovery program.

  2. Infinite-Dimensional Boundary Observer for Lithium-Ion Battery State Estimation

    DEFF Research Database (Denmark)

    Hasan, Agus; Jouffroy, Jerome

    2017-01-01

    This paper presents boundary observer design for state-of-charge (SOC) estimation of lithium-ion batteries. The lithium-ion battery dynamics are governed by thermal-electrochemical principles, which mathematically modeled by partial differential equations (PDEs). In general, the model is a reaction......-diffusion equation with time-dependent coefficients. A Luenberger observer is developed using infinite-dimensional backstepping method and uses only a single measurement at the boundary of the battery. The observer gains are computed by solving the observer kernel equation. A numerical example is performed to show...

  3. Three-dimensional stability of solitary kinetic Alfven waves and ion-acoustic waves

    International Nuclear Information System (INIS)

    Ghosh, G.; Das, K.P.

    1994-01-01

    Starting from a set of equations that lead to a linear dispersion relation coupling kinetic Alfven waves and ion-acoustic waves, three-dimensional KdV equations are derived for these waves. These equations are then used to investigate the three-dimensional stability of solitary kinetic Alfven waves and ion-acoustic waves by the small-k perturbation expansion method of Rowlands and Infeld. For kinetic Alfven waves it is found that there is instability if the direction of the plane-wave perturbation lies inside a cone, and the growth rate of the instability attains a maximum when the direction of the perturbation lies in the plane containing the external magnetic field and the direction of propagation of the solitary wave. For ion-acoustic waves the growth rate of instability attains a maximum when the direction of the perturbation lies in a plane perpendicular to the direction of propagation of the solitary wave. (Author)

  4. Improving quantitative gas chromatography-electron ionization mass spectrometry results using a modified ion source: demonstration for a pharmaceutical application.

    Science.gov (United States)

    D'Autry, Ward; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Van Schepdael, Ann

    2011-07-01

    Gas chromatography-mass spectrometry is a well established analytical technique. However, mass spectrometers with electron ionization sources may suffer from signal drifts, hereby negatively influencing quantitative performance. To demonstrate this phenomenon for a real application, a static headspace-gas chromatography method in combination with electron ionization-quadrupole mass spectrometry was optimized for the determination of residual dichloromethane in coronary stent coatings. Validating the method, the quantitative performance of an original stainless steel ion source was compared to that of a modified ion source. Ion source modification included the application of a gold coating on the repeller and exit plate. Several validation aspects such as limit of detection, limit of quantification, linearity and precision were evaluated using both ion sources. It was found that, as expected, the stainless steel ion source suffered from signal drift. As a consequence, non-linearity and high RSD values for repeated analyses were obtained. An additional experiment was performed to check whether an internal standard compound would lead to better results. It was found that the signal drift patterns of the analyte and internal standard were different, consequently leading to high RSD values for the response factor. With the modified ion source however, a more stable signal was observed resulting in acceptable linearity and precision. Moreover, it was also found that sensitivity improved compared to the stainless steel ion source. Finally, the optimized method with the modified ion source was applied to determine residual dichloromethane in the coating of coronary stents. The solvent was detected but found to be below the limit of quantification. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. 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.

  6. Identification of volatiles from pineapple (Ananas comosus L.) pulp by comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Pedroso, Marcio P; Ferreira, Ernesto C; Hantao, Leandro W; Bogusz, Stanislau; Augusto, Fabio

    2011-07-01

    Combining qualitative data from the chromatographic structure of 2-D gas chromatography with flame ionization detection (GC×GC-FID) and that from gas chromatography-mass spectrometry (GC/MS) should result in a more accurate assignment of the peak identities than the simple analysis by GC/MS, where coelution of analytes is unavoidable in highly complex samples (rendering spectra unsuitable for qualitative purposes) or for compounds in very low concentrations. Using data from GC×GC-FID combined with GC/MS can reveal coelutions that were not detected by mass spectra deconvolution software. In addition, some compounds can be identified according to the structure of the GC×GC-FID chromatogram. In this article, the volatile fractions of fresh and dehydrated pineapple pulp were evaluated. The extraction of the volatiles was performed by dynamic headspace extraction coupled to solid-phase microextraction (DHS-SPME), a technique appropriate for slurries or solid matrices. Extracted analytes were then analyzed by GC×GC-FID and GC/MS. The results obtained using both techniques were combined to improve compound identifications. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Separation of halogens from uranium compounds by means of pyrohydrolysis and their determination by ion chromatography

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Brandao Filho, D.; Abrao, A.

    1987-07-01

    This paper describs the determination of fluorine in nuclear grade uranium compounds by means of phyrohydrolysis. A stream of wet oxygem at a temperature of 900 to 1000 0 C is passed through a quartz tube where the powdered samples is put. The halogens are volatilized as their respective acids that are absorbed in a buffer solution or water. The measurements are made with ion-seletive eletrodes or by ion chromatography. The sensitivity is of 1μg F - /g and 5μg Cl - /g. The separation of fluorine from uranium compounds by diferent methods is discussed. (Author) [pt

  8. Two-dimensional PIC simulations of ion beam instabilities in Supernova-driven plasma flows

    Energy Technology Data Exchange (ETDEWEB)

    Dieckmann, M E; Shukla, P K [Institut fuer Theoretische Physik IV, Ruhr-Universitaet Bochum, D-44780 Bochum (Germany); Meli, A; Mastichiadis, A [Department of Physics, National University of Athens, Panepistimiopolis, Zografos 15783 (Greece); Drury, L O C [Dublin Institute for Advanced Studies, Dublin 2 (Ireland)], E-mail: markd@tp4.rub.de

    2008-06-15

    Supernova remnant blast shells can reach the flow speed v{sub s} = 0.1c and shocks form at its front. Instabilities driven by shock-reflected ion beams heat the plasma in the foreshock, which may inject particles into diffusive acceleration. The ion beams can have the speed v{sub b} {approx} v{sub s}. For v{sub b} << v{sub s} the Buneman or upper-hybrid instabilities dominate, while for v{sub b} >> v{sub s} the filamentation and mixed modes grow faster. Here the relevant waves for v{sub b} {approx} v{sub s} are examined and how they interact nonlinearly with the particles. The collision of two plasma clouds at the speed v{sub s} is modelled with particle-in-cell simulations, which convect with them magnetic fields oriented perpendicular to their flow velocity vector. One simulation models equally dense clouds and the other one uses a density ratio of 2. Both simulations show upper-hybrid waves that are planar over large spatial intervals and that accelerate electrons to {approx}10 keV. The symmetric collision yields only short oscillatory wave pulses, while the asymmetric collision also produces large-scale electric fields, probably through a magnetic pressure gradient. The large-scale fields destroy the electron phase space holes and they accelerate the ions, which facilitates the formation of a precursor shock.

  9. Purification of dirucotide, a synthetic 17-aminoacid peptide, by ion exchange centrifugal partition chromatography.

    Science.gov (United States)

    Boudesocque, Leslie; Forni, Luciano; Martinez, Agathe; Nuzillard, Jean-Marc; Giraud, Matthieu; Renault, Jean-Hugues

    2017-09-01

    Dirucotide is a synthetic drug candidate for the treatment of multiple sclerosis. This 17-aminoacid peptide was successfully purified by ion exchange centrifugal partition chromatography. The optimized conditions involved the biphasic methyl tert-butyl ether/acetonitrile/n-butanol/water (2:1:2:5, v/v) solvent system in the descending mode, the di(2-ethylhexyl)phosphoric acid cation-exchanger with an exchanger (di(2-ethylhexyl)phosphoric acid)/dirucotide mole ratio of 100 and Ca 2+ ions in aqueous solution as displacer. Critical impurities were efficiently eliminated and dirucotide was recovered in high yield and purity (69% and 98%, respectively) and with a productivity of 2.29g per liter of stationary phase per hour. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-12-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  11. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-02-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  12. Accurate determination of trace amounts of lanthanum, yttrium and all stable lanthanides in biological materials by Ion Chromatography

    International Nuclear Information System (INIS)

    Dybczynski, R.S.; Kulisa, K.; Danko, B.; Samczynski, Z.

    2007-01-01

    The analytical procedure for the isolation and preconcentration of La, Y and the lanthanides from biological materials and their determination by ion chromatography (IC) with the use of Dionex Ion Pac CS3 + CG3 column (sulfonic acid type), α-hydroxyisobutyric acid (α-HIBA) as an eluent, and PAR or Arsenazo III as color forming reagents, was elaborated. The scheme originally devised for NAA, involving microwave assisted digestion and multi step separation employing ion exchange and extraction chromatography columns was used to selectively recover REE fraction (without scandium) with 100% yield. The REE fraction was analyzed by IC at 25 and 70 o C. The run at 70 o C enabled resolution of Y and Dy peaks and as a result made possible quantitative determination of La, Y, and all lanthanides. Investigation on the mechanism of band spreading revealed that longitudinal diffusion in the stationary phase considerably contributed to the total plate height. Surprisingly, the plate height (H) calculated from Y peak was distinctly lower than H values of the adjacent lanthanides. The method was validated by analyzing several certified reference materials (CRMs). (authors)

  13. Two-dimensional multifractal cross-correlation analysis

    International Nuclear Information System (INIS)

    Xi, Caiping; Zhang, Shuning; Xiong, Gang; Zhao, Huichang; Yang, Yonghong

    2017-01-01

    Highlights: • We study the mathematical models of 2D-MFXPF, 2D-MFXDFA and 2D-MFXDMA. • Present the definition of the two-dimensional N 2 -partitioned multiplicative cascading process. • Do the comparative analysis of 2D-MC by 2D-MFXPF, 2D-MFXDFA and 2D-MFXDMA. • Provide a reference on the choice and parameter settings of these methods in practice. - Abstract: There are a number of situations in which several signals are simultaneously recorded in complex systems, which exhibit long-term power-law cross-correlations. This paper presents two-dimensional multifractal cross-correlation analysis based on the partition function (2D-MFXPF), two-dimensional multifractal cross-correlation analysis based on the detrended fluctuation analysis (2D-MFXDFA) and two-dimensional multifractal cross-correlation analysis based on the detrended moving average analysis (2D-MFXDMA). We apply these methods to pairs of two-dimensional multiplicative cascades (2D-MC) to do a comparative study. Then, we apply the two-dimensional multifractal cross-correlation analysis based on the detrended fluctuation analysis (2D-MFXDFA) to real images and unveil intriguing multifractality in the cross correlations of the material structures. At last, we give the main conclusions and provide a valuable reference on how to choose the multifractal algorithms in the potential applications in the field of SAR image classification and detection.

  14. Determination of glufosinate ammonium and its metabolite (AE F064619 and AE F061517) residues in water by gas chromatography with tandem mass spectrometry after ion exchange cleanup and derivatization.

    Science.gov (United States)

    Royer, A; Beguin, S; Sochor, H; Communal, P Y

    2000-11-01

    An analytical method for the determination of glufosinate ammonium and its principal metabolites, AE F064619 and AE F061517, in water of two different hardnesses (5 and 30 DH, French hardness) has been developed and validated. Samples were spiked at different levels (0. 05 and 0.5 microgram/L) and were purified by column chromatography on ion-exchange resins. After derivatization with glacial acetic acid and trimethylarthoacetate mixture, the derivatives were quantified by using capillary gas chromatography with an ion-trap tandem mass spectrometric detector. Analytical conditions for MS/MS detection were optimized, and the quantification was carried out on the areas of the most representative ions. The limit of quantification was validated at 0.05 microgram/L for each compound. The mean recovery value and the relative standard deviation (n = 20) were 92.0% and 17. 8% for glufosinate ammonium, 90.2% and 15.8% for AE F064619, and 89. 7% and 12.7% for AE F061517.

  15. Two-dimensional beam profiles and one-dimensional projections

    Science.gov (United States)

    Findlay, D. J. S.; Jones, B.; Adams, D. J.

    2018-05-01

    One-dimensional projections of improved two-dimensional representations of transverse profiles of particle beams are proposed for fitting to data from harp-type monitors measuring beam profiles on particle accelerators. Composite distributions, with tails smoothly matched on to a central (inverted) parabola, are shown to give noticeably better fits than single gaussian and single parabolic distributions to data from harp-type beam profile monitors all along the proton beam transport lines to the two target stations on the ISIS Spallation Neutron Source. Some implications for inferring beam current densities on the beam axis are noted.

  16. Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

    International Nuclear Information System (INIS)

    Kim, Jeong Soo; Kim, Keon; Kim, Do Hwan

    2012-01-01

    A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL

  17. Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jeong Soo; Kim, Keon [Korea Univ., Seoul (Korea, Republic of); Kim, Do Hwan [Daegu Univ., Gyeongsan (Korea, Republic of)

    2012-12-15

    A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

  18. A two-dimensional layered Cd(II) coordination polymer with a three-dimensional supramolecular architecture incorporating mixed multidentate N- and O-donor ligands.

    Science.gov (United States)

    Huang, Qiu-Ying; Su, Ming-Yang; Meng, Xiang-Ru

    2015-06-01

    The combination of N-heterocyclic and multicarboxylate ligands is a good choice for the construction of metal-organic frameworks. In the title coordination polymer, poly[bis{μ2-1-[(1H-benzimidazol-2-yl)methyl]-1H-tetrazole-κ(2)N(3):N(4)}(μ4-butanedioato-κ(4)O(1):O(1'):O(4):O(4'))(μ2-butanedioato-κ(2)O(1):O(4))dicadmium], [Cd(C4H4O4)(C9H8N6)]n, each Cd(II) ion exhibits an irregular octahedral CdO4N2 coordination geometry and is coordinated by four O atoms from three carboxylate groups of three succinate (butanedioate) ligands and two N atoms from two 1-[(1H-benzimidazol-2-yl)methyl]-1H-tetrazole (bimt) ligands. Cd(II) ions are connected by two kinds of crystallographically independent succinate ligands to generate a two-dimensional layered structure with bimt ligands located on each side of the layer. Adjacent layers are further connected by hydrogen bonding, leading to a three-dimensional supramolecular architecture in the solid state. Thermogravimetric analysis of the title polymer shows that it is stable up to 529 K and then loses weight from 529 to 918 K, corresponding to the decomposition of the bimt ligands and succinate groups. The polymer exhibits a strong fluorescence emission in the solid state at room temperature.

  19. FPGA Implementation of one-dimensional and two-dimensional cellular automata

    International Nuclear Information System (INIS)

    D'Antone, I.

    1999-01-01

    This report describes the hardware implementation of one-dimensional and two-dimensional cellular automata (CAs). After a general introduction to the cellular automata, we consider a one-dimensional CA used to implement pseudo-random techniques in built-in self test for VLSI. Due to the increase in digital ASIC complexity, testing is becoming one of the major costs in the VLSI production. The high electronics complexity, used in particle physics experiments, demands higher reliability than in the past time. General criterions are given to evaluate the feasibility of the circuit used for testing and some quantitative parameters are underlined to optimize the architecture of the cellular automaton. Furthermore, we propose a two-dimensional CA that performs a peak finding algorithm in a matrix of cells mapping a sub-region of a calorimeter. As in a two-dimensional filtering process, the peaks of the energy clusters are found in one evolution step. This CA belongs to Wolfram class II cellular automata. Some quantitative parameters are given to optimize the architecture of the cellular automaton implemented in a commercial field programmable gate array (FPGA)

  20. Three-Dimensional Carbon Nanostructures for Advanced Lithium-Ion Batteries

    Directory of Open Access Journals (Sweden)

    Chiwon Kang

    2016-10-01

    Full Text Available Carbon nanostructural materials have gained the spotlight as promising anode materials for energy storage; they exhibit unique physico-chemical properties such as large surface area, short Li+ ion diffusion length, and high electrical conductivity, in addition to their long-term stability. However, carbon-nanostructured materials have issues with low areal and volumetric densities for the practical applications in electric vehicles, portable electronics, and power grid systems, which demand higher energy and power densities. One approach to overcoming these issues is to design and apply a three-dimensional (3D electrode accommodating a larger loading amount of active anode materials while facilitating Li+ ion diffusion. Furthermore, 3D nanocarbon frameworks can impart a conducting pathway and structural buffer to high-capacity non-carbon nanomaterials, which results in enhanced Li+ ion storage capacity. In this paper, we review our recent progress on the design and fabrication of 3D carbon nanostructures, their performance in Li-ion batteries (LIBs, and their implementation into large-scale, lightweight, and flexible LIBs.

  1. Lie algebra contractions on two-dimensional hyperboloid

    International Nuclear Information System (INIS)

    Pogosyan, G. S.; Yakhno, A.

    2010-01-01

    The Inoenue-Wigner contraction from the SO(2, 1) group to the Euclidean E(2) and E(1, 1) group is used to relate the separation of variables in Laplace-Beltrami (Helmholtz) equations for the four corresponding two-dimensional homogeneous spaces: two-dimensional hyperboloids and two-dimensional Euclidean and pseudo-Euclidean spaces. We show how the nine systems of coordinates on the two-dimensional hyperboloids contracted to the four systems of coordinates on E 2 and eight on E 1,1 . The text was submitted by the authors in English.

  2. Quasi-two-dimensional holography

    International Nuclear Information System (INIS)

    Kutzner, J.; Erhard, A.; Wuestenberg, H.; Zimpfer, J.

    1980-01-01

    The acoustical holography with numerical reconstruction by area scanning is memory- and time-intensive. With the experiences by the linear holography we tried to derive a scanning for the evaluating of the two-dimensional flaw-sizes. In most practical cases it is sufficient to determine the exact depth extension of a flaw, whereas the accuracy of the length extension is less critical. For this reason the applicability of the so-called quasi-two-dimensional holography is appropriate. The used sound field given by special probes is divergent in the inclined plane and light focussed in the perpendicular plane using cylindrical lenses. (orig.) [de

  3. Correlation of rocket propulsion fuel properties with chemical composition using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry followed by partial least squares regression analysis.

    Science.gov (United States)

    Kehimkar, Benjamin; Hoggard, Jamin C; Marney, Luke C; Billingsley, Matthew C; Fraga, Carlos G; Bruno, Thomas J; Synovec, Robert E

    2014-01-31

    There is an increased need to more fully assess and control the composition of kerosene-based rocket propulsion fuels such as RP-1. In particular, it is critical to make better quantitative connections among the following three attributes: fuel performance (thermal stability, sooting propensity, engine specific impulse, etc.), fuel properties (such as flash point, density, kinematic viscosity, net heat of combustion, and hydrogen content), and the chemical composition of a given fuel, i.e., amounts of specific chemical compounds and compound classes present in a fuel as a result of feedstock blending and/or processing. Recent efforts in predicting fuel chemical and physical behavior through modeling put greater emphasis on attaining detailed and accurate fuel properties and fuel composition information. Often, one-dimensional gas chromatography (GC) combined with mass spectrometry (MS) is employed to provide chemical composition information. Building on approaches that used GC-MS, but to glean substantially more chemical information from these complex fuels, we recently studied the use of comprehensive two dimensional (2D) gas chromatography combined with time-of-flight mass spectrometry (GC×GC-TOFMS) using a "reversed column" format: RTX-wax column for the first dimension, and a RTX-1 column for the second dimension. In this report, by applying chemometric data analysis, specifically partial least-squares (PLS) regression analysis, we are able to readily model (and correlate) the chemical compositional information provided by use of GC×GC-TOFMS to RP-1 fuel property information such as density, kinematic viscosity, net heat of combustion, and so on. Furthermore, we readily identified compounds that contribute significantly to measured differences in fuel properties based on results from the PLS models. We anticipate this new chemical analysis strategy will have broad implications for the development of high fidelity composition-property models, leading to an

  4. METHOD 332.0: DETERMINATION OF PERCHLORATE IN DRINKING WATER BY ION CHROMATOGRAPHY WITH SUPPRESSED CONDUCTIVITY AND ELECTROSPRAY IONIZATION MASS SPECTROMETRY

    Science.gov (United States)

    This method is applicable to the identification and quantitation of perchlorate in raw and finished drinking waters. The approach used is ion chromatography with suppressed conductivity and electrospray ionization mass spectrometry (IC-ESI/MS)

  5. Topology optimization of two-dimensional waveguides

    DEFF Research Database (Denmark)

    Jensen, Jakob Søndergaard; Sigmund, Ole

    2003-01-01

    In this work we use the method of topology optimization to design two-dimensional waveguides with low transmission loss.......In this work we use the method of topology optimization to design two-dimensional waveguides with low transmission loss....

  6. Traditional Semiconductors in the Two-Dimensional Limit.

    Science.gov (United States)

    Lucking, Michael C; Xie, Weiyu; Choe, Duk-Hyun; West, Damien; Lu, Toh-Ming; Zhang, S B

    2018-02-23

    Interest in two-dimensional materials has exploded in recent years. Not only are they studied due to their novel electronic properties, such as the emergent Dirac fermion in graphene, but also as a new paradigm in which stacking layers of distinct two-dimensional materials may enable different functionality or devices. Here, through first-principles theory, we reveal a large new class of two-dimensional materials which are derived from traditional III-V, II-VI, and I-VII semiconductors. It is found that in the ultrathin limit the great majority of traditional binary semiconductors studied (a series of 28 semiconductors) are not only kinetically stable in a two-dimensional double layer honeycomb structure, but more energetically stable than the truncated wurtzite or zinc-blende structures associated with three dimensional bulk. These findings both greatly increase the landscape of two-dimensional materials and also demonstrate that in the double layer honeycomb form, even ordinary semiconductors, such as GaAs, can exhibit exotic topological properties.

  7. Sufficient Controllability Condition for Affine Systems with Two-Dimensional Control and Two-Dimensional Zero Dynamics

    Directory of Open Access Journals (Sweden)

    D. A. Fetisov

    2015-01-01

    Full Text Available The controllability conditions are well known if we speak about linear stationary systems: a linear stationary system is controllable if and only if the dimension of the state vector is equal to the rank of the controllability matrix. The concept of the controllability matrix is extended to affine systems, but relations between affine systems controllability and properties of this matrix are more complicated. Various controllability conditions are set for affine systems, but they deal as usual either with systems of some special form or with controllability in some small neighborhood of the concerned point. An affine system is known to be controllable if the system is equivalent to a system of a canonical form, which is defined and regular in the whole space of states. In this case, the system is said to be feedback linearizable in the space of states. However there are examples, which illustrate that a system can be controllable even if it is not feedback linearizable in any open subset in the space of states. In this article we deal with such systems.Affine systems with two-dimensional control are considered. The system in question is assumed to be equivalent to a system of a quasicanonical form with two-dimensional zero dynamics which is defined and regular in the whole space of states. Therefore the controllability of the original system is equivalent to the controllability of the received system of a quasicanonical form. In this article the sufficient condition for an available solution of the terminal problem is proven for systems of a quasicanonical form with two-dimensional control and two-dimensional zero dynamics. The condition is valid in the case of an arbitrary time interval and arbitrary initial and finite states of the system. Therefore the controllability condition is set for systems of a quasicanonical form with two-dimensional control and two-dimensional zero dynamics. An example is given which illustrates how the proved

  8. Enhanced Lithium Ion Transport by Superionic Pathways Formed on the Surface of Two-dimensional Structured Li0.85Na0.15V3O8 for High-Performance Lithium Ion Batteries

    International Nuclear Information System (INIS)

    Lu, Xuena; Shang, Yu; Zhang, Sen; Deng, Chao

    2015-01-01

    Highlights: • Li 0.85 Na 0.15 V 3 O 8 nanosheet with superionic conductive layer was constructed. • Li x V 2 O 5 surface layer provides facile pathways for lithium migration. • Li x V 2 O 5 -Li 0.85 Na 0.15 V 3 O 8 composite displays good high rate capability. - Abstract: Poor ion transport and rate capability are the main challenges for LiV 3 O 8 as cathode material for lithium ion batteries. Here we report a novel strategy for enhancing lithium ion transport by building superionic pathways on the surface of Li 0.85 Na 0.15 V 3 O 8 nanosheet. The two-dimensional Li 0.85 Na 0.15 V 3 O 8 nanoparticle with an ion conductive layer of Li x V 2 O 5 on its surface is constructed by a modified sol–gel strategy with carefully controlled sodium incorporation and elements stoichiometry. Ultrathin Li x V 2 O 5 surface layer not only provides facile pathways for lithium migration, but also increases the structure stability during cycling. The Li x V 2 O 5 -Li 0.85 Na 0.15 V 3 O 8 composite displays good high rate capability of 172.3 mAh g −1 at 5C and excellent cycling stability of 98.9% over fifty cycles. This superior electrochemical property is attributed to the occupation of lithium site by Na + in LiV 3 O 8 host crystals and the surface superionic pathways of Li x V 2 O 5 phase. Therefore, the advantages of both high ion transport and the structure stabilization in present study put forward a new strategy for achieving high-performance LiV 3 O 8 electrode material with tailored nanoarchitecture

  9. Ripening-dependent metabolic changes in the volatiles of pineapple (Ananas comosus (L.) Merr.) fruit: I. Characterization of pineapple aroma compounds by comprehensive two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Steingass, Christof Björn; Carle, Reinhold; Schmarr, Hans-Georg

    2015-03-01

    Qualitative ripening-dependent changes of pineapple volatiles were studied via headspace solid-phase microextraction and analyzed by comprehensive two-dimensional gas chromatography quadrupole mass spectrometry (HS-SPME-GC×GC-qMS). Early green-ripe stage, post-harvest ripened, and green-ripe fruits at the end of their commercial shelf-life were compared to air-freighted pineapples harvested at full maturity. In total, more than 290 volatiles could be identified by mass spectrometry and their linear retention indices. The majority of compounds comprise esters (methyl and ethyl esters of saturated and unsaturated fatty acids, acetates), terpenes, alcohols, aldehydes, 2-ketones, free fatty acids, and miscellaneous γ- and δ-lactones. The structured separation space obtained by GC×GC allowed revealing various homologous series of compound classes as well as clustering of sesquiterpenes. Post-harvest ripening increased the diversity of the volatile profile compared to both early green-ripe maturity stages and on-plant ripened fruits.

  10. Determination of sulfur anions in spent oil shale leachates by ion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Niss, N.D.

    1989-07-01

    The leaching and transport of chemical constituents from spent oil shale disposal areas is an area of environmental concern at the present time. Sulfur-containing compounds are prevalent in spent oil shales and have the potential to leach into aqueous systems surrounding disposal sites. Computer modeling has been used in recent years to predict the transport of species in an aqueous environment. The quality of model predictions, however, depends on the validation steps taken in comparing model predictions with laboratory data on ion speciation. Further, the quality of the validation step depends on the reliability of laboratory methods in generating ion speciation data. The purpose of this study was to develop methods to separate and quantify sulfur-containing anions in spent oil shale leachates by suppressed ion chromatography. The anions studied were S{sup 2{minus}} (sulfide), SO{sup 2{minus}}{sub 3} (sulfite), SO{sup 2{minus}}{sub 4} (sulfate), SCN{sup {minus}} (thiocyanate), S{sub 2}O{sup 2{minus}}{sub 3} (thiosulfate), and S{sub 4}O{sup 2{minus}}{sub 6} (tetrathionate). After the separations were developed, a series of method-challenging experiments were performed to test the reliability of the methods and assure the development of an analytically sound product. 24 refs., 7 figs., 5 tabs.

  11. Fingerprinting of traditional Chinese medicines on the C18-Diol mixed-mode column in online or offline two-dimensional liquid chromatography on the single column modes.

    Science.gov (United States)

    Wang, Qing; Tong, Ling; Yao, Lin; Zhang, Peng; Xu, Li

    2016-06-05

    In the present study, a mixed-mode stationary phase, C18-Diol, was applied for fingerprint analysis of traditional Chinese medicines. Hydrophobic, hydrogen bonding and electrostatic interactions were demonstrated to contribute the retention separately or jointly, which endowed the C18-Diol stationary phase with distinct selectivity compared to the bare C18 one. The separation of total alkaloids extracted from Fritillaria hupehensis was compared on the C18-Diol and conventional C18 column with the greater resolving power and better symmetry responses on the former one. Besides, a novel two-dimensional liquid chromatography on the single column (2D-LC-1C) was realized on C18-Diol with the offline mode for the alcohol extract of Fritillaria hupehensis and online mode for Ligusticum chuanxiong Hort. The early co-eluted extracted components with great polarity on the first dimension were reinjected on the same column and well separated on the second dimension. The results exhibited that the two complementary RPLC and HILIC modes on C18-Diol stationary phase enhanced the separation capacity and revealed more abundant chemical information of the sample, which was a powerful tool in analyzing complex herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Two-dimensional flexible nanoelectronics

    Science.gov (United States)

    Akinwande, Deji; Petrone, Nicholas; Hone, James

    2014-12-01

    2014/2015 represents the tenth anniversary of modern graphene research. Over this decade, graphene has proven to be attractive for thin-film transistors owing to its remarkable electronic, optical, mechanical and thermal properties. Even its major drawback--zero bandgap--has resulted in something positive: a resurgence of interest in two-dimensional semiconductors, such as dichalcogenides and buckled nanomaterials with sizeable bandgaps. With the discovery of hexagonal boron nitride as an ideal dielectric, the materials are now in place to advance integrated flexible nanoelectronics, which uniquely take advantage of the unmatched portfolio of properties of two-dimensional crystals, beyond the capability of conventional thin films for ubiquitous flexible systems.

  13. A one-dimensional ion beam figuring system for x-ray mirror fabrication

    International Nuclear Information System (INIS)

    Idir, Mourad; Huang, Lei; Bouet, Nathalie; Kaznatcheev, Konstantine; Vescovi, Matthew; Lauer, Ken; Conley, Ray; Rennie, Kent; Kahn, Jim; Nethery, Richard; Zhou, Lin

    2015-01-01

    We report on the development of a one-dimensional Ion Beam Figuring (IBF) system for x-ray mirror polishing. Ion beam figuring provides a highly deterministic method for the final precision figuring of optical components with advantages over conventional methods. The system is based on a state of the art sputtering deposition system outfitted with a gridded radio frequency inductive coupled plasma ion beam source equipped with ion optics and dedicated slit developed specifically for this application. The production of an IBF system able to produce an elongated removal function rather than circular is presented in this paper, where we describe in detail the technical aspect and present the first obtained results

  14. A one-dimensional ion beam figuring system for x-ray mirror fabrication

    Energy Technology Data Exchange (ETDEWEB)

    Idir, Mourad, E-mail: midir@bnl.gov; Huang, Lei; Bouet, Nathalie; Kaznatcheev, Konstantine; Vescovi, Matthew; Lauer, Ken [NSLS-II, Brookhaven National Laboratory, P.O. Box 5000, Upton, New York 11973 (United States); Conley, Ray [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Rennie, Kent; Kahn, Jim; Nethery, Richard [Kaufman & Robinson, Inc., 1330 Blue Spruce Drive, Fort Collins, Colorado 80524 (United States); Zhou, Lin [College of Mechatronics and Automation, National University of Defense Technology, 109 Deya Road, Changsha, Hunan 410073 (China); Hu’nan Key Laboratory of Ultra-precision Machining Technology, Changsha, Hunan 410073 (China)

    2015-10-15

    We report on the development of a one-dimensional Ion Beam Figuring (IBF) system for x-ray mirror polishing. Ion beam figuring provides a highly deterministic method for the final precision figuring of optical components with advantages over conventional methods. The system is based on a state of the art sputtering deposition system outfitted with a gridded radio frequency inductive coupled plasma ion beam source equipped with ion optics and dedicated slit developed specifically for this application. The production of an IBF system able to produce an elongated removal function rather than circular is presented in this paper, where we describe in detail the technical aspect and present the first obtained results.

  15. Ultrasensitive and simultaneous detection of heavy metal ions based on three-dimensional graphene-carbon nanotubes hybrid electrode materials

    International Nuclear Information System (INIS)

    Huang, Hui; Chen, Ting; Liu, Xiuyu; Ma, Houyi

    2014-01-01

    Highlights: • Three-dimensional graphene-MWCNTs nanocomposites were prepared. • Graphene-MWCNTs based electrochemical sensor was used to detect heavy metal ions for the first time. • The proposed sensor was certified capable for real sample with satisfactory results. - Abstract: A green and facile method was developed to prepare a novel hybrid nanocomposite that consisted of one-dimensional multi-walled carbon nanotubes (MWCNTs) and two-dimensional graphene oxide (GO) sheets. The as-prepared three-dimensional GO–MWCNTs hybrid nanocomposites exhibit excellent water-solubility owing to the high hydrophilicity of GO components; meanwhile, a certain amount of MWCNTs loaded on the surface of GO sheets through π–π interaction seem to be “dissolved” in water. Moreover, the graphene(G)-MWCNTs nanocomposites with excellent conductivity were obtained conveniently by the direct electrochemical reduction of GO–MWCNTs nanocomposites. Seeing that there is a good synergistic effect between MWCNTs and graphene components in enhancing preconcentration efficiency of metal ions and accelerating electron transfer rate at G-MWCNTs/electrolyte interface, the G-MWCNTs nanocomposites possess fast, simultaneous and sensitive detection performance for trace amounts of heavy metal ions. The electrochemical results demonstrate that the G-MWCNTs nanocomposites can act as a kind of practical sensing material to simultaneously determine Pb 2+ and Cd 2+ ions in terms of anodic stripping voltammetry (ASV). The linear calibration plots for Pb 2+ and Cd 2+ ranged from 0.5 μg L −1 to 30 μg L −1 . The detection limits were determined to be 0.2 μg L −1 (S/N = 3) for Pb 2+ and 0.1 μg L −1 (S/N = 3) for Cd 2+ in the case of a deposition time of 180 s. It is worth mentioning that the G-MWCNTs modified electrodes were successfully applied to the simultaneous detection of Cd 2+ and Pb 2+ ions in real electroplating effluent samples containing lots of surface active impurities

  16. Qualitative and quantitative characterization of plasma proteins when incorporating traveling wave ion mobility into a liquid chromatography-mass spectrometry workflow for biomarker discovery: use of product ion quantitation as an alternative data analysis tool for label free quantitation.

    Science.gov (United States)

    Daly, Charlotte E; Ng, Leong L; Hakimi, Amirmansoor; Willingale, Richard; Jones, Donald J L

    2014-02-18

    Discovery of protein biomarkers in clinical samples necessitates significant prefractionation prior to liquid chromatography-mass spectrometry (LC-MS) analysis. Integrating traveling wave ion mobility spectrometry (TWIMS) enables in-line gas phase separation which when coupled with nanoflow liquid chromatography and data independent acquisition tandem mass spectrometry, confers significant advantages to the discovery of protein biomarkers by improving separation and inherent sensitivity. Incorporation of TWIMS leads to a packet of concentrated ions which ultimately provides a significant improvement in sensitivity. As a consequence of ion packeting, when present at high concentrations, accurate quantitation of proteins can be affected due to detector saturation effects. Human plasma was analyzed in triplicate using liquid-chromatography data independent acquisition mass spectrometry (LC-DIA-MS) and using liquid-chromatography ion-mobility data independent acquisition mass spectrometry (LC-IM-DIA-MS). The inclusion of TWIMS was assessed for the effect on sample throughput, data integrity, confidence of protein and peptide identification, and dynamic range. The number of identified proteins is significantly increased by an average of 84% while both the precursor and product mass accuracies are maintained between the modalities. Sample dynamic range is also maintained while quantitation is achieved for all but the most abundant proteins by incorporating a novel data interpretation method that allows accurate quantitation to occur. This additional separation is all achieved within a workflow with no discernible deleterious effect on throughput. Consequently, TWIMS greatly enhances proteome coverage and can be reliably used for quantification when using an alternative product ion quantification strategy. Using TWIMS in biomarker discovery in human plasma is thus recommended.

  17. Separation and characterization of chemical constituents in Ginkgo biloba extract by off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography coupled with quadrupole-time of flight mass spectrometry.

    Science.gov (United States)

    Ji, Shuai; He, Dan-Dan; Wang, Tian-Yun; Han, Jie; Li, Zheng; Du, Yan; Zou, Jia-Hui; Guo, Meng-Zhe; Tang, Dao-Quan

    2017-11-30

    Ginkgo biloba extract (GBE), derived from the leaves of Ginkgo biloba L., is one of the most widely used traditional Chinese medicines worldwide. Due to high structural diversity and low abundance of chemical constituents in GBE, conventional reversed-phase liquid chromatography has limited power to meet the needs of its quality control. In this study, an off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography (HILIC×RP 2D-LC) system coupled with diode array detection (DAD) and quadrupole time-of-flight mass spectrometry (qTOF-MS) was established to comprehensively analyze the chemical constituents of GBE. After optimizing the chromatographic columns and mobile phase of 2D-LC, a Waters XBridge Amide column using acetonitrile/water/formic acid as the mobile phase was selected as the first dimension to fractionate GBE, and the obtained fractions were further separated on an Agilent Zorbax XDB-C18 column with methanol/water/formic acid as the mobile phase. As a result, a total of 125 compounds were detected in GBE. The orthogonality of the 2D-LC system was 69.5%, and the practical peak capacity was 3864 and 2994, respectively, calculated by two different methods. The structures of 104 compounds were tentatively characterized by qTOF-MS analysis, and 21 of them were further confirmed by comparing with reference standards. This established HILIC×RP 2D-LC-qTOF/MS system can greatly improve the separation and characterization of natural products in GBE or other complicated herbal extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Two-Dimensional Metal Oxide Nanomaterials for Next-Generation Rechargeable Batteries.

    Science.gov (United States)

    Mei, Jun; Liao, Ting; Kou, Liangzhi; Sun, Ziqi

    2017-12-01

    The exponential increase in research focused on two-dimensional (2D) metal oxides has offered an unprecedented opportunity for their use in energy conversion and storage devices, especially for promising next-generation rechargeable batteries, such as lithium-ion batteries (LIBs) and sodium-ion batteries (NIBs), as well as some post-lithium batteries, including lithium-sulfur batteries, lithium-air batteries, etc. The introduction of well-designed 2D metal oxide nanomaterials into next-generation rechargeable batteries has significantly enhanced the performance of these energy-storage devices by providing higher chemically active interfaces, shortened ion-diffusion lengths, and improved in-plane carrier-/charge-transport kinetics, which have greatly promoted the development of nanotechnology and the practical application of rechargeable batteries. Here, the recent progress in the application of 2D metal oxide nanomaterials in a series of rechargeable LIBs, NIBs, and other post lithium-ion batteries is reviewed relatively comprehensively. Current opportunities and future challenges for the application of 2D nanomaterials in energy-storage devices to achieve high energy density, high power density, stable cyclability, etc. are summarized and outlined. It is believed that the integration of 2D metal oxide nanomaterials in these clean energy devices offers great opportunities to address challenges driven by increasing global energy demands. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Combined untargeted and targeted fingerprinting by comprehensive two-dimensional gas chromatography: revealing fructose-induced changes in mice urinary metabolic signatures.

    Science.gov (United States)

    Bressanello, Davide; Liberto, Erica; Collino, Massimo; Chiazza, Fausto; Mastrocola, Raffaella; Reichenbach, Stephen E; Bicchi, Carlo; Cordero, Chiara

    2018-04-01

    This study exploits the information potential of comprehensive two-dimensional gas chromatography configured with a parallel dual secondary column-dual detection by mass spectrometry and flame ionization (GC×2GC-MS/FID) to study changes in urinary metabolic signatures of mice subjected to high-fructose diets. Samples are taken from mice fed with normal or fructose-enriched diets provided either in aqueous solution or in solid form and analyzed at three stages of the dietary intervention (1, 6, and 12 weeks). Automated Untargeted and Targeted fingerprinting for 2D data elaboration is adopted for the most inclusive data mining of GC×GC patterns. The UT fingerprinting strategy performs a fully automated peak-region features fingerprinting and combines results from pre-targeted compounds and unknowns across the sample-set. The most informative metabolites, with statistically relevant differences between sample groups, are obtained by unsupervised multivariate analysis (MVA) and cross-validated by multi-factor analysis (MFA) with external standard quantitation by GC-MS. Results indicate coherent clustering of mice urine signatures according to dietary manipulation. Notably, the metabolite fingerprints of mice fed with liquid fructose exhibited greater derangement in fructose, glucose, citric, pyruvic, malic, malonic, gluconic, cis-aconitic, succinic and 2-keto glutaric acids, glycine acyl derivatives (N-carboxy glycine, N-butyrylglycine, N-isovaleroylglycine, N-phenylacetylglycine), and hippuric acid. Untargeted fingerprinting indicates some analytes which were not a priori pre-targeted which provide additional insights: N-acetyl glucosamine, N-acetyl glutamine, malonyl glycine, methyl malonyl glycine, and glutaric acid. Visual features fingerprinting is used to track individual variations during experiments, thereby extending the panorama of possible data elaboration tools. Graphical abstract ᅟ.

  20. Determination of vanillin, ethyl vanillin, and coumarin in infant formula by liquid chromatography-quadrupole linear ion trap mass spectrometry.

    Science.gov (United States)

    Shen, Yan; Han, Chao; Liu, Bin; Lin, Zhengfeng; Zhou, Xiujin; Wang, Chengjun; Zhu, Zhenou

    2014-02-01

    A simple, precise, accurate, and validated liquid chromatography-quadrupole linear ion trap mass spectrometry method was developed for the determination of vanillin, ethyl vanillin, and coumarin in infant formula samples. Following ultrasonic extraction with methanol/water (1:1, vol/vol), and clean-up on an HLB solid-phase extraction cartridge (Waters Corp., Milford, MA), samples were separated on a Waters XSelect HSS T3 column (150 × 2.1-mm i.d., 5-μm film thickness; Waters Corp.), with 0.1% formic acid solution-acetonitrile as mobile phase at a flow rate of 0.25 mL/min. Quantification of the target was performed by the internal standard approach, using isotopically labeled compounds for each chemical group, to correct matrix effects. Data acquisition was carried out in multiple reaction monitoring transitions mode, monitoring 2 multiple reaction monitoring 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 of the linear ion trap. The novel liquid chromatography-quadrupole linear ion trap mass spectrometry platform offers the best sensitivity and specificity for characterization and quantitative determination of vanillin, ethyl vanillin, and coumarin in infant formula and fulfills the quality criteria for routine laboratory application. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  1. Radioanalytical determination of plutonium and americium using ion exchange and extraction chromatography technique in urine

    International Nuclear Information System (INIS)

    Santhanakrishnan, V.; Sreedevi, K.R.; Rajaram, S.; Ravi, P.M.

    2011-01-01

    The use of anion exchange chromatography for the separation of Pu and extraction chromatography technique for the separation of Am from urine samples was studied. In the earlier method, Pu separation was carried out by anion exchange chromatography followed by Am separation by cation exchange chromatography. The chemical recovery of Am obtained by cation exchange separation method was inconsistent and low in the range 30-70%. In this study, the average Pu recovery obtained using anion exchange chromatography was 89.2 with standard deviation of 10.4 and the average Am recovery obtained using extraction chromatography with TRU resin was 77.4 with standard deviation of 14.8. Moreover, Am separation could be completed within three hours using the TRU column compared to two days that were required for the cation exchange chromatography. (author)

  2. Approximate solutions for the two-dimensional integral transport equation. Solution of complex two-dimensional transport problems

    International Nuclear Information System (INIS)

    Sanchez, Richard.

    1980-11-01

    This work is divided into two parts: the first part deals with the solution of complex two-dimensional transport problems, the second one (note CEA-N-2166) treats the critically mixed methods of resolution. A set of approximate solutions for the isotropic two-dimensional neutron transport problem has been developed using the interface current formalism. The method has been applied to regular lattices of rectangular cells containing a fuel pin, cladding, and water, or homogenized structural material. The cells are divided into zones that are homogeneous. A zone-wise flux expansion is used to formulate a direct collision probability problem within a cell. The coupling of the cells is effected by making extra assumptions on the currents entering and leaving the interfaces. Two codes have been written: CALLIOPE uses a cylindrical cell model and one or three terms for the flux expansion, and NAUSICAA uses a two-dimensional flux representation and does a truly two-dimensional calculation inside each cell. In both codes, one or three terms can be used to make a space-independent expansion of the angular fluxes entering and leaving each side of the cell. The accuracies and computing times achieved with the different approximations are illustrated by numerical studies on two benchmark problems and by calculations performed in the APOLLO multigroup code [fr

  3. Two-dimensional topological field theories coupled to four-dimensional BF theory

    International Nuclear Information System (INIS)

    Montesinos, Merced; Perez, Alejandro

    2008-01-01

    Four-dimensional BF theory admits a natural coupling to extended sources supported on two-dimensional surfaces or string world sheets. Solutions of the theory are in one to one correspondence with solutions of Einstein equations with distributional matter (cosmic strings). We study new (topological field) theories that can be constructed by adding extra degrees of freedom to the two-dimensional world sheet. We show how two-dimensional Yang-Mills degrees of freedom can be added on the world sheet, producing in this way, an interactive (topological) theory of Yang-Mills fields with BF fields in four dimensions. We also show how a world sheet tetrad can be naturally added. As in the previous case the set of solutions of these theories are contained in the set of solutions of Einstein's equations if one allows distributional matter supported on two-dimensional surfaces. These theories are argued to be exactly quantizable. In the context of quantum gravity, one important motivation to study these models is to explore the possibility of constructing a background-independent quantum field theory where local degrees of freedom at low energies arise from global topological (world sheet) degrees of freedom at the fundamental level

  4. Electroforming free resistive switching memory in two-dimensional VOx nanosheets

    KAUST Repository

    Hota, Mrinal Kanti

    2015-10-21

    We report two-dimensional VOx nanosheets containing multi-oxidation states (V5+, V4+, and V3+), prepared by a hydrothermal process for potential applications in resistive switching devices. The experimental results demonstrate a highly reproducible, electroforming-free, low SET bias bipolar resistive switching memory performance with endurance for more than 100 cycles maintaining OFF/ON ratio of ∼60 times. These devices show better memory performance as compared to previously reported VOx thin film based devices. The memory mechanism in VOx is proposed to be originated from the migration of oxygen vacancies/ions, an influence of the bottom electrode and existence of multi-oxidation states.

  5. Impurity profiling of a chemical weapon precursor for possible forensic signatures by comprehensive two-dimensional gas chromatography/mass spectrometry and chemometrics.

    Science.gov (United States)

    Hoggard, Jamin C; Wahl, Jon H; Synovec, Robert E; Mong, Gary M; Fraga, Carlos G

    2010-01-15

    In this report we present the feasibility of using analytical and chemometric methodologies to reveal and exploit the chemical impurity profiles from commercial dimethyl methylphosphonate (DMMP) samples to illustrate the type of forensic information that may be obtained from chemical-attack evidence. Using DMMP as a model compound of a toxicant that may be used in a chemical attack, we used comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GC x GC/TOF-MS) to detect and identify trace organic impurities in six samples of commercially acquired DMMP. The GC x GC/TOF-MS data was analyzed to produce impurity profiles for all six DMMP samples using 29 analyte impurities. The use of PARAFAC for the mathematical resolution of overlapped GC x GC peaks ensured clean spectra for the identification of many of the detected analytes by spectral library matching. The use of statistical pairwise comparison revealed that there were trace impurities that were quantitatively similar and different among five of the six DMMP samples. Two of the DMMP samples were revealed to have identical impurity profiles by this approach. The use of nonnegative matrix factorization indicated that there were five distinct DMMP sample types as illustrated by the clustering of the multiple DMMP analyses into five distinct clusters in the scores plots. The two indistinguishable DMMP samples were confirmed by their chemical supplier to be from the same bulk source. Sample information from the other chemical suppliers supported the idea that the other four DMMP samples were likely from different bulk sources. These results demonstrate that the matching of synthesized products from the same source is possible using impurity profiling. In addition, the identified impurities common to all six DMMP samples provide strong evidence that basic route information can be obtained from impurity profiles. Finally, impurities that may be unique to the sole bulk manufacturer of DMMP were

  6. Interfacial nondegenerate doping of MoS2 and other two-dimensional semiconductors.

    Science.gov (United States)

    Behura, Sanjay; Berry, Vikas

    2015-03-24

    Controlled nondegenerate doping of two-dimensional semiconductors (2DSs) with their ultraconfined carriers, high quantum capacitance, and surface-sensitive electronics can enable tuning their Fermi levels for rational device design. However, doping techniques for three-dimensional semiconductors, such as ion implantation, cannot be directly applied to 2DSs because they inflict high defect density. In this issue of ACS Nano, Park et al. demonstrate that interfacing 2DSs with substrates having dopants can controllably inject carriers to achieve nondegenerate doping, thus significantly broadening 2DSs' functionality and applications. Futuristically, this can enable complex spatial patterning/contouring of energy levels in 2DSs to form p-n junctions, integrated logic, and opto/electronic devices. The process is also extendable to biocellular-interfaced devices, band-continuum structures, and intricate 2D circuitry.

  7. Influence of column type and chromatographic conditions on the ion-exchange chromatography of immunoglobulins.

    Science.gov (United States)

    Yang, Y B; Harrison, K

    1996-08-30

    Immunoglobulins are often purified by affinity chromatography. However, this technique is costly, can result in poor resolution for subclasses (or is only group specific), and leads to possible leaching of contaminants into the purified products. Ion-exchange chromatography has shown great potential and has found an increased usage in the purification of immunoglobulins. The aim of this study is to further understand the separation mechanism with emphasis on the influence of column type and chromatographic conditions on the peak shape, selectivity and changes in the elution patterns. Included are strong cation-exchange, strong anion-exchange and weak anion-exchange columns. Five immunoglobulin G antibodies were used as test probes. Some sera and ascites were also used in the study. Among the chromatographic conditions examined were mobile phase pH, buffer type, buffer concentration, gradient rate, and column temperature. Significant differences in the chromatographic behavior (elution pattern, peak shape and selectivity) of the test samples are discussed in regard to the column type and the chromatographic conditions.

  8. Separation of amaranthine-type betacyanins by ion-pair high-speed countercurrent chromatography.

    Science.gov (United States)

    Jerz, Gerold; Gebers, Nadine; Szot, Dominika; Szaleniec, Maciej; Winterhalter, Peter; Wybraniec, Slawomir

    2014-05-30

    Betacyanins, red-violet plant pigments, were fractionated by ion-pair high-speed countercurrent chromatography (IP-HSCCC) from leaves extract of Iresine lindenii Van Houtte, an ornamental plant of the family Amaranthaceae. An HSCCC solvent system consisting of TBME-1-BuOH-ACN-H2O (1:3:1:5, v/v/v/v) was applied using ion-pair forming heptafluorobutyric acid (HFBA). Significantly different elution profiles of betacyanin diastereomeric pairs (derivatives based on betanidin and isobetanidin) observed in the HSCCC in comparison to HPLC systems indicate a complementarity of both techniques' fractionation capabilities. The numerous diastereomeric pairs can be selectively separated from each other using the HSCCC system simplifying the pigment purification process. Apart from the three well known highly abundant pigments (amaranthine, betanin and iresinin I) together with their isoforms, three new acylated (feruloylated and sinapoylated) betacyanins as well as known pigment hylocerenin (previously isolated from cacti fruits) were characterized in the plant for the first time and they are new for the whole Amaranthaceae family. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. New EDTA determination method based on ion chromatography with suppressed conductimetric detection

    International Nuclear Information System (INIS)

    Gyoergy Patzay; Yahya Ramadan; Csilla Tonko

    2014-01-01

    A novel direct method for the determination of EDTA in alkaline radioactive evaporator residue solution was developed and validated based on ion chromatography with suppressed conductimetric detection and anion exchange columns (A Supp 4, 4 mm × 250 mm and A Supp 5, 4 mm × 150 mm). The yttrium-EDTA complex resulted one single chromatographic peak in the eluent and allowed the correct determination of EDTA in an alkaline, high concentration radioactive waste water. Depending on coexisting substances, suitable eluent is 10.0 mM carbonate buffer/pH 10.6 or 10.75 (t R ,Y-EDTA = 7.01 and 6.4 min, respectively). For 10.0 mM carbonate buffer/pH 10.6 and isocratic flow rate of 1.0 cm 3 /min, a linear calibration curve was obtained from 5 to 40 mg/dm 3 (r > 0.999) EDTA. Good resolution was achieved from commonly coexisting anions (chloride, nitrite, nitrate, sulphate, phosphate, bromide and citrate). The developed simple ion chromatographic method was applied for the assay of EDTA in various radioactive alkaline solutions. (author)

  10. Beginning Introductory Physics with Two-Dimensional Motion

    Science.gov (United States)

    Huggins, Elisha

    2009-01-01

    During the session on "Introductory College Physics Textbooks" at the 2007 Summer Meeting of the AAPT, there was a brief discussion about whether introductory physics should begin with one-dimensional motion or two-dimensional motion. Here we present the case that by starting with two-dimensional motion, we are able to introduce a considerable…

  11. Two-dimensional thermofield bosonization

    International Nuclear Information System (INIS)

    Amaral, R.L.P.G.; Belvedere, L.V.; Rothe, K.D.

    2005-01-01

    The main objective of this paper was to obtain an operator realization for the bosonization of fermions in 1 + 1 dimensions, at finite, non-zero temperature T. This is achieved in the framework of the real-time formalism of Thermofield Dynamics. Formally, the results parallel those of the T = 0 case. The well-known two-dimensional Fermion-Boson correspondences at zero temperature are shown to hold also at finite temperature. To emphasize the usefulness of the operator realization for handling a large class of two-dimensional quantum field-theoretic problems, we contrast this global approach with the cumbersome calculation of the fermion-current two-point function in the imaginary-time formalism and real-time formalisms. The calculations also illustrate the very different ways in which the transmutation from Fermi-Dirac to Bose-Einstein statistics is realized

  12. Collisional plasma transport: two-dimensional scalar formulation of the initial boundary value problem and quasi one-dimensional models

    International Nuclear Information System (INIS)

    Mugge, J.W.

    1979-10-01

    The collisional plasma transport problem is formulated as an initial boundary value problem for general characteristic boundary conditions. Starting from the full set of hydrodynamic and electrodynamic equations an expansion in the electron-ion mass ratio together with a multiple timescale method yields simplified equations on each timescale. On timescales where many collisions have taken place for the simplified equations the initial boundary value problem is formulated. Through the introduction of potentials a two-dimensional scalar formulation in terms of quasi-linear integro-differential equations of second order for a domain consisting of plasma and vacuum sub-domains is obtained. (Auth.)

  13. Two-dimensional x-ray diffraction

    CERN Document Server

    He, Bob B

    2009-01-01

    Written by one of the pioneers of 2D X-Ray Diffraction, this useful guide covers the fundamentals, experimental methods and applications of two-dimensional x-ray diffraction, including geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis and combinatorial screening. Experimental examples in materials research, pharmaceuticals, and forensics are also given. This presents a key resource to resea

  14. A new method of analysis of peroxydisulfate using ion chromatography and its application to the simultaneous determination of peroxydisulfate and other common inorganic ions in a peroxydisulfate matrix.

    Science.gov (United States)

    Khan, Nymul E; Adewuyi, Yusuf G

    2011-01-21

    A new method for the determination of peroxydisulfate using ion chromatography has been developed. Elution of peroxydisulfate was effected by isocratic elution using 200 mM NaOH at 40°C. A modification of the method using gradient elution was able to simultaneously determine other common inorganic ions (nitrate, nitrite, sulfate and chloride) down to significantly low concentrations in a peroxydisulfate matrix. The relative standard deviations (RSD) were in the range of 0.5-5%, for peak areas and ion was 0.2 ppm and for the other ions were ≤2×10(-2) ppm. The calibration curves were linear with slope and intercepts close to 1 and 0, respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

  15. Three-dimensional structure of recombinant carboxypeptidase T from Thermoactinomyces vulgaris without calcium ions

    Science.gov (United States)

    Akparov, V. Kh.; Timofeev, V. I.; Kuranova, I. P.

    2011-07-01

    Crystals of recombinant carboxypeptidase T (CPT) from Thermoactinomyces vulgaris were grown in a capillary by the counterdiffusion method in the absence of calcium ions. The three-dimensional structure of CPT was solved at 1.69-Å resolution using the X-ray diffraction data collected from the crystals of the enzyme on the SPring-8 synchrotron radiation facility and was then refined to Rfact = 16.903% and Rfree = 18.165%. The coordinates of the refined model were deposited in the Protein Data Bank (PDB ID: 3QNV). A comparison of this structure with the structure of wild-type CPT containing bound calcium ions, which was determined earlier, revealed a number of conformational changes both in the calcium-binding sites and the enzyme active site. Based on the results of this comparison, the possible factors responsible for the difference in the catalytic activity of the two forms of the enzyme are considered.

  16. Electrochemical Detectors in HPLC and Ion Chromatography.

    Science.gov (United States)

    Horvai, George; Pungor, ErnÕ

    1989-01-01

    Back in 1952, the renowned Polish electrochemist Wiktor Kemula introduced chromato-polarography, 1 i.e., polaro-graphic detection for liquid chromatography. This technique continued to develop slowly until the early 1970s (for a review see Reference 2) when modem high-performance liquid chromatography (HPLC) emerged. This new, highly efficient chromatographc method could only be. used with detectors ensuring low dispersion. It was not easy to modify the dropping mercury electrode cells to satisfy this requirement. However, at the same time, electroanalytical chemists, who already had much experience in using carbon-based electrodes for oxidative detection in flow analysis, put forward the idea of oxidative amperometric detection in liquid chromatography. 3,4 In this technique, solid or quasi-solid (paste) electrodes were used and this made possible the construction of miniaturized cells with just a few microliter volume.

  17. Piezoelectricity in Two-Dimensional Materials

    KAUST Repository

    Wu, Tao

    2015-02-25

    Powering up 2D materials: Recent experimental studies confirmed the existence of piezoelectricity - the conversion of mechanical stress into electricity - in two-dimensional single-layer MoS2 nanosheets. The results represent a milestone towards embedding low-dimensional materials into future disruptive technologies. © 2015 Wiley-VCH Verlag GmbH & Co. KGaA.

  18. Application of silver ion in the separation of macrolide antibiotic components by high-speed counter-current chromatography.

    Science.gov (United States)

    Wen, Yaoming; Wang, Jiaoyan; Chen, Xiuming; Le, Zhanxian; Chen, Yuxiang; Zheng, Wei

    2009-05-29

    Three macrolide antibiotic components - ascomycin, tacrolimus and dihydrotacrolimus - were separated and purified by silver ion high-speed counter-current chromatography (HSCCC). The solvent system consisted of n-hexane-tert-butyl methyl ether-methanol-water (1:3:6:5, v/v) and silver nitrate (0.10mol/l). The silver ion acted as a pi-complexing agent with tacrolimus because of its extra side double bond compared with ascomycin and dihydrotacrolimus. This complexation modified the partition coefficient values and the separation factors of the three components. As a result, ascomycin, tacrolimus and dihydrotacrolimus were purified from 150mg extracted crude sample with purities of 97.6%, 98.7% and 96.5%, respectively, and yields over 80% (including their tautomers). These results cannot be achieved with the same solvent system but without the addition of silver ion.

  19. Consistent calculation of the stopping power for slow ions in two-dimensional electron gases

    International Nuclear Information System (INIS)

    Wang, You-Nian; Ma, Teng-Gai

    1997-01-01

    Within the framework of quantum scattering theory, we present a consistent calculation of the stopping power for slow protons and antiprotons moving in two-dimensional electron gases. The Friedel sum rule is used to determine the screening constant in the scattering potential. For the stopping power our results are compared with that of the random-phase approximation dielectric theory and that predicted by the linear Thomas-Fermi potential. copyright 1997 The American Physical Society

  20. Evaluation of complexing agents and column temperature in ion chromatographic separation of alkali metals, alkaline earth metals and transition metals ion

    International Nuclear Information System (INIS)

    Kelkar, Anoop; Pandey, Ashish; Name, Anil B.; Das, D.K.; Behere, P.G.; Mohd Afzal

    2015-01-01

    The aim of ion chromatography method development is the resolution of all metal ions of interests. Resolution can be improved by changing the selectivity. Selectivity in chromatography can be altered by changes in mobile phase (eg eluent type, eluent strength) or through changes in stationary phase. Temperature has been used in altering the selectivity of particularly in reversed phase liquid chromatography and ion exchange chromatography. Present paper describe the retention behaviour of alkali metals, alkaline earth metals and transition metal ions on a silica based carboxylate function group containing analyte column. Alkali metals, alkaline earth metals and transition metal ions were detected by ion conductivity and UV-VIS detectors respectively

  1. The principle of pooled calibrations and outlier retainment elucidates optimum performance of ion chromatography

    DEFF Research Database (Denmark)

    Andersen, Jens; Mikolajczak, Maria; Wojtachnio-Zawada, Katarzyna Olga

    2012-01-01

    A principle with quality assurance of ion chromatography (IC) is presented. Since the majority of scientists and costumers are interested in the determination of the true amount of analyte in real samples, the focus of attention should be directed towards the concept of accuracy rather than...... investigations of method validations where it was found that the principle of pooled calibrations provides a more realistic picture of the analytical performance with the drawback, however, that generally higher levels of uncertainties should be accepted, as compared to contemporary literature values...

  2. Strong Cation Exchange Chromatography in Analysis of Posttranslational Modifications: Innovations and Perspectives

    Science.gov (United States)

    Edelmann, Mariola J.

    2011-01-01

    Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide. PMID:22174558

  3. Two-dimensional confinement of heavy fermions

    International Nuclear Information System (INIS)

    Shishido, Hiroaki; Shibauchi, Takasada; Matsuda, Yuji; Terashima, Takahito

    2010-01-01

    Metallic systems with the strongest electron correlations are realized in certain rare-earth and actinide compounds whose physics are dominated by f-electrons. These materials are known as heavy fermions, so called because the effective mass of the conduction electrons is enhanced via correlation effects up to as much as several hundreds times the free electron mass. To date the electronic structure of all heavy-fermion compounds is essentially three-dimensional. Here we report on the first realization of a two-dimensional heavy-fermion system, where the dimensionality is adjusted in a controllable fashion by fabricating heterostructures using molecular beam epitaxy. The two-dimensional heavy fermion system displays striking deviations from the standard Fermi liquid low-temperature electronic properties. (author)

  4. Numerical simulation and experimental validation of the three-dimensional flow field and relative analyte concentration distribution in an atmospheric pressure ion source.

    Science.gov (United States)

    Poehler, Thorsten; Kunte, Robert; Hoenen, Herwart; Jeschke, Peter; Wissdorf, Walter; Brockmann, Klaus J; Benter, Thorsten

    2011-11-01

    In this study, the validation and analysis of steady state numerical simulations of the gas flows within a multi-purpose ion source (MPIS) are presented. The experimental results were obtained with particle image velocimetry (PIV) measurements in a non-scaled MPIS. Two-dimensional time-averaged velocity and turbulent kinetic energy distributions are presented for two dry gas volume flow rates. The numerical results of the validation simulations are in very good agreement with the experimental data. All significant flow features have been correctly predicted within the accuracy of the experiments. For technical reasons, the experiments were conducted at room temperature. Thus, numerical simulations of ionization conditions at two operating points of the MPIS are also presented. It is clearly shown that the dry gas volume flow rate has the most significant impact on the overall flow pattern within the APLI source; far less critical is the (larger) nebulization gas flow. In addition to the approximate solution of Reynolds-Averaged Navier-Stokes equations, a transport equation for the relative analyte concentration has been solved. The results yield information on the three-dimensional analyte distribution within the source. It becomes evident that for ion transport into the MS ion transfer capillary, electromagnetic forces are at least as important as fluid dynamic forces. However, only the fluid dynamics determines the three-dimensional distribution of analyte gas. Thus, local flow phenomena in close proximity to the spray shield are strongly impacting on the ionization efficiency.

  5. Two-dimensional topological photonics

    Science.gov (United States)

    Khanikaev, Alexander B.; Shvets, Gennady

    2017-12-01

    Originating from the studies of two-dimensional condensed-matter states, the concept of topological order has recently been expanded to other fields of physics and engineering, particularly optics and photonics. Topological photonic structures have already overturned some of the traditional views on wave propagation and manipulation. The application of topological concepts to guided wave propagation has enabled novel photonic devices, such as reflection-free sharply bent waveguides, robust delay lines, spin-polarized switches and non-reciprocal devices. Discrete degrees of freedom, widely used in condensed-matter physics, such as spin and valley, are now entering the realm of photonics. In this Review, we summarize the latest advances in this highly dynamic field, with special emphasis on the experimental work on two-dimensional photonic topological structures.

  6. Ion chromatography characterization of polysaccharides in ancient wall paintings.

    Science.gov (United States)

    Colombin, Maria Perla; Ceccarini, Alessio; Carmignani, Alessia

    2002-08-30

    An analytical procedure for the characterisation of polysaccharides and the identification of plant gums in old polychrome samples is described. The procedure is based on hydrolysis with 2 M trifluoroacetic acid assisted by microwaves (20 min, 120 degrees C, 500 W), clean-up of the hydrolysate by an ion-exchange resin, and analysis by high-performance anion-exchange chromatography with pulsed amperometric detection. Using this method the hydrolysis time was reduced to 20 min and the chromatographic separation of seven monosaccharides (fucose, rhamnose, arabinose, galactose, glucose, mannose, xylose) and two uronic acids (galacturonic and glucuronic) was achieved in 40 min. The whole analytical procedure allows sugar determination in plant gums at picomole levels, with an average recovery of 72% with an RSD of 8% as tested on arabic gum. The analytical procedure was tested with several raw gums, watercolour samples and reference painting specimens prepared according to old recipes at the Opificio delle Pietre Dure of Florence (Italian Ministry of Cultural Heritage, Italy). All the data collected expressed in relative sugar percentage contents were submitted to principal components analysis for gum identification: five groups were spatially separated and this enabled the identification of arabic, tragacanth, karaya, cherry+ghatty, and guar+locust bean gum. Wall painting samples from Macedonian tombs (Greece) of the 4th-3rd Centuries B.C., processed by the suggested method, showed the presence of a complex paint media mainly consisting of tragacanth and fruit tree gums. Moreover, starch had probably been added to plaster as highlighted by the presence of a huge amount of glucose.

  7. Structures of two-dimensional three-body systems

    International Nuclear Information System (INIS)

    Ruan, W.Y.; Liu, Y.Y.; Bao, C.G.

    1996-01-01

    Features of the structure of L = 0 states of a two-dimensional three-body model system have been investigated. Three types of permutation symmetry of the spatial part, namely symmetric, antisymmetric, and mixed, have been considered. A comparison has been made between the two-dimensional system and the corresponding three-dimensional one. The effect of symmetry on microscopic structures is emphasized. (author)

  8. Dual cascade time-of-flight mass spectrometer basing on electrostatic mirrors with two dimensional fields

    International Nuclear Information System (INIS)

    Glikman, L. G.; Goloskokov, Yu. V.; Karetskaya, S.P.; Mit', A.G.

    1999-01-01

    In the report [1] we have suggested the scheme of time-of-flight spectrometer containing two electrostatic mirrors with two dimensional field that doesn't depend on one of the Cartesian coordinates). In the articles [2,3] there have been found conditions for obtaining high quality of time-of-flight and spatial focusing. One of basic advantages of this scheme - is availability of intermediate stigmatic image. In the plane where this image is it's possible to place controlled diaphragm that limits ion scatter along the energy if the scatter is too large. With the help of this diaphragm at the spectrometer you can register mass spectrum with the selected energy. Good focusing quality allows reducing of initial ion energy by this increasing the time of their flight and thus analyzers resolving ability. Ion source and receiver are spaced at rather a long distances. This can be useful to solve some practical tasks

  9. New separation and detection methods in capillary electrophoresis and ion chromatography for the analysis of ionic compounds

    International Nuclear Information System (INIS)

    Mayrhofer, K.

    1999-10-01

    The first part of the thesis deals with the simultaneous analysis of inorganic anions and organic acids in electrodeposition coatings with the co-electroosmotic capillary electrophoresis. The coating of workpieces, e.g. car bodies, by means of an electrodeposition process is an important methodology especially in the automotiv industries. It is usually performed by introducing the object into a basin filled with a water-based electro-dipcoat, applying a voltage of 200-400 Volts (direct current) and using the bodywork as cathode. Because the workpiece has to pass a number of preliminary treatments before the coating procedure, ionic compound may be carried into the basin. If the concentrations of these ionic impurities is too high, the electro-deposition of the binding agent fails or the thickness of the coating is not reproducible. The organic acids are used as neutralization agents in order to control and to keep the pH of the basin constant. The common method of analysing ionic impurities is ion chromatography. The organic acids have to be separated in an ion exclusion chromatography column because organic acids may coelute with the inorganic anions or elute with the dead volume. Therefore a separation method for capillary electrophoresis was developed which enables the simultaneouse analysis of inorganic anions and organic acids in less then 5 minutes. Chloride, nitrate, sulfate, fuoride, phosphate, carbonate, formic acid, acetic acid, lactic acid and butyric acid were detected with indirect UV-detection at 254 nm. For removal of the the binding agent and the pigments the lacquer was mixed with a 0.01 M sodium hydroxide solution and then filtered through a 0.45 μm filter cartridge. 5 mM trimellitic acid, titrated with sodium hydroxid to pH 10, 0.001 % hexadimethrinbromide and 20 % acetonitrile served as buffer. The analytes were separated with a satisfactory resolution. Between every analysis the fused silica capillary was purged for two minutes with buffer. So

  10. Traceability and Quality Control in Traditional Chinese Medicine: From Chemical Fingerprint to Two-Dimensional Barcode

    Directory of Open Access Journals (Sweden)

    Yong Cai

    2015-01-01

    Full Text Available Chemical fingerprinting is currently a widely used tool that enables rapid and accurate quality evaluation of Traditional Chinese Medicine (TCM. However, chemical fingerprints are not amenable to information storage, recognition, and retrieval, which limit their use in Chinese medicine traceability. In this study, samples of three kinds of Chinese medicines were randomly selected and chemical fingerprints were then constructed by using high performance liquid chromatography. Based on chemical data, the process of converting the TCM chemical fingerprint into two-dimensional code is presented; preprocess and filtering algorithm are also proposed aiming at standardizing the large amount of original raw data. In order to know which type of two-dimensional code (2D is suitable for storing data of chemical fingerprints, current popular types of 2D codes are analyzed and compared. Results show that QR Code is suitable for recording the TCM chemical fingerprint. The fingerprint information of TCM can be converted into data format that can be stored as 2D code for traceability and quality control.

  11. Electrostatic and electromagnetic instabilities associated with electrostatic shocks: Two-dimensional particle-in-cell simulation

    International Nuclear Information System (INIS)

    Kato, Tsunehiko N.; Takabe, Hideaki

    2010-01-01

    A two-dimensional electromagnetic particle-in-cell simulation with the realistic ion-to-electron mass ratio of 1836 is carried out to investigate the electrostatic collisionless shocks in relatively high-speed (∼3000 km s -1 ) plasma flows and also the influence of both electrostatic and electromagnetic instabilities, which can develop around the shocks, on the shock dynamics. It is shown that the electrostatic ion-ion instability can develop in front of the shocks, where the plasma is under counterstreaming condition, with highly oblique wave vectors as was shown previously. The electrostatic potential generated by the electrostatic ion-ion instability propagating obliquely to the shock surface becomes comparable with the shock potential and finally the shock structure is destroyed. It is also shown that in front of the shock the beam-Weibel instability gradually grows as well, consequently suggesting that the magnetic field generated by the beam-Weibel instability becomes important in long-term evolution of the shock and the Weibel-mediated shock forms long after the electrostatic shock vanished. It is also observed that the secondary electrostatic shock forms in the reflected ions in front of the primary electrostatic shock.

  12. Multi-dimensional TOF-SIMS analysis for effective profiling of disease-related ions from the tissue surface.

    Science.gov (United States)

    Park, Ji-Won; Jeong, Hyobin; Kang, Byeongsoo; Kim, Su Jin; Park, Sang Yoon; Kang, Sokbom; Kim, Hark Kyun; Choi, Joon Sig; Hwang, Daehee; Lee, Tae Geol

    2015-06-05

    Time-of-flight secondary ion mass spectrometry (TOF-SIMS) emerges as a promising tool to identify the ions (small molecules) indicative of disease states from the surface of patient tissues. In TOF-SIMS analysis, an enhanced ionization of surface molecules is critical to increase the number of detected ions. Several methods have been developed to enhance ionization capability. However, how these methods improve identification of disease-related ions has not been systematically explored. Here, we present a multi-dimensional SIMS (MD-SIMS) that combines conventional TOF-SIMS and metal-assisted SIMS (MetA-SIMS). Using this approach, we analyzed cancer and adjacent normal tissues first by TOF-SIMS and subsequently by MetA-SIMS. In total, TOF- and MetA-SIMS detected 632 and 959 ions, respectively. Among them, 426 were commonly detected by both methods, while 206 and 533 were detected uniquely by TOF- and MetA-SIMS, respectively. Of the 426 commonly detected ions, 250 increased in their intensities by MetA-SIMS, whereas 176 decreased. The integrated analysis of the ions detected by the two methods resulted in an increased number of discriminatory ions leading to an enhanced separation between cancer and normal tissues. Therefore, the results show that MD-SIMS can be a useful approach to provide a comprehensive list of discriminatory ions indicative of disease states.

  13. Microstructure in two- and three-dimensional hybrid simulations of perpendicular collisionless shocks

    Czech Academy of Sciences Publication Activity Database

    Burgess, D.; Hellinger, Petr; Gingell, I.; Trávníček, Pavel M.

    2016-01-01

    Roč. 82, č. 4 (2016), 905820401/1-905820401/23 ISSN 0022-3778 Institutional support: RVO:68378289 Keywords : ion-acceleration * numerical simulations * bow shock * electron acceleration * cluster observations * self-reformation * magnetic-field * whistler waves * injection * nonstationarity Subject RIV: BL - Plasma and Gas Discharge Physics Impact factor: 1.160, year: 2016 https://www.cambridge.org/core/ journals /journal-of-plasma-physics/article/microstructure-in-two-and-three-dimensional-hybrid-simulations-of-perpendicular-collisionless-shocks/F964EF89FB14A6504A49CFAD54970E2B

  14. Modeling of the financial market using the two-dimensional anisotropic Ising model

    Science.gov (United States)

    Lima, L. S.

    2017-09-01

    We have used the two-dimensional classical anisotropic Ising model in an external field and with an ion single anisotropy term as a mathematical model for the price dynamics of the financial market. The model presented allows us to test within the same framework the comparative explanatory power of rational agents versus irrational agents with respect to the facts of financial markets. We have obtained the mean price in terms of the strong of the site anisotropy term Δ which reinforces the sensitivity of the agent's sentiment to external news.

  15. Determination of oxidation products in radiolysis of halophenols with pulse radiolysis, hplc, and ion chromatography

    International Nuclear Information System (INIS)

    Ye, M.; Schuler, R.H.

    1990-01-01

    This paper reports on hydroxyl radicals that react with halogen substituted phenols by several different ways. One is addition of OH radicals to the aromatic ring, which is followed by elimination of hydrogen halide, H 2 O or H - . The positions of OH radicals attack are dependent on the nature of the halogen which affects the electronic distribution in the ring. The oxidation of fluorophenols, chlorophenols and bromophenols with hydroxyl radicals in N 2 O saturated solution has been investigated with pulse radiolysis and γ-irradiation experiments. The intermediates of the reactions were studied by pulse radiolysis. The products created in the γ-irradiation of aqueous solutions of halophenols were analyzed by ion chromatography and high performance liquid chromatography (HPLC). With the combination of time-resolved and steady-state experiments a complete and detailed description of radiolytic oxidation of halophenols by hydroxyl radicals was obtained

  16. Coupling Front-End Separations, Ion Mobility Spectrometry, and Mass Spectrometry For Enhanced Multidimensional Biological and Environmental Analyses

    Science.gov (United States)

    Zheng, Xueyun; Wojcik, Roza; Zhang, Xing; Ibrahim, Yehia M.; Burnum-Johnson, Kristin E.; Orton, Daniel J.; Monroe, Matthew E.; Moore, Ronald J.; Smith, Richard D.; Baker, Erin S.

    2017-01-01

    Ion mobility spectrometry (IMS) is a widely used analytical technique for rapid molecular separations in the gas phase. Though IMS alone is useful, its coupling with mass spectrometry (MS) and front-end separations is extremely beneficial for increasing measurement sensitivity, peak capacity of complex mixtures, and the scope of molecular information available from biological and environmental sample analyses. In fact, multiple disease screening and environmental evaluations have illustrated that the IMS-based multidimensional separations extract information that cannot be acquired with each technique individually. This review highlights three-dimensional separations using IMS-MS in conjunction with a range of front-end techniques, such as gas chromatography, supercritical fluid chromatography, liquid chromatography, solid-phase extractions, capillary electrophoresis, field asymmetric ion mobility spectrometry, and microfluidic devices. The origination, current state, various applications, and future capabilities of these multidimensional approaches are described in detail to provide insight into their uses and benefits. PMID:28301728

  17. X-ray imaging device for one-dimensional and two-dimensional radioscopy

    International Nuclear Information System (INIS)

    1978-01-01

    The X-ray imaging device for the selectable one-dimensional or two-dimensional pictures of objects illuminated by X-rays, comprising an X-ray source, an X-ray screen, and an opto-electrical picture development device placed behind the screen, is characterized by an anamorphotic optical system, which is positioned with a one-dimensional illumination between the X-ray screen and the opto-electrical device and that a two-dimensional illumination will be developed, and that in view of the lens system which forms part of the opto-electrical device, there is placed an X-ray screen in a specified beam direction so that a magnified image may be formed by equalisation of the distance between the X-ray screen and the lens system. (G.C.)

  18. Two-dimensional magnetism in the triangular antiferromagnet NiGa2S4

    International Nuclear Information System (INIS)

    Nambu, Yusuke

    2013-01-01

    At sufficiently low temperatures, electron spins in normal magnets generally order into some fashion, for instance, ferromagnetic and antiferromagnetic. Geometrical frustration and/or reduced dimensionality can suppress such conventional orders, and occasionally induce unknown states of matter. This is the case for the two-dimensional (2D) triangular antiferromagnet Ni(Ga 2 S 4 , in which S=1 nickel spins do not order, instead show an exotic magnetism. We found (1) a resonant critical slowing down toward T*=8.5 K followed by a viscous spin liquid behavior, and (2) a spin-size dependent ground state. To elucidate (1), spin dynamics ranging from 10 -13 to 10 0 seconds were quantitatively explored through the experimental techniques such as inelastic neutron scattering, backscattering, neutron spin echo, ac and nonlinear susceptibilities. The finding of (2) is evidenced by impurity effects. Integer spins substituted systems such as zinc and iron ions retain a quadratic temperature dependence of the magnetic specific heat as for the parent compound. However, substitutions of half-odd integer spins, cobalt and manganese ions, eventually induce a distinct behavior, indicating an importance of integer size of spins to stabilize the 2D magnetism realized in NiGa 2 S 4 . The article gives our experimental findings and as well as some relevant theoretical scenarios. (author)

  19. Hamiltonian formalism of two-dimensional Vlasov kinetic equation.

    Science.gov (United States)

    Pavlov, Maxim V

    2014-12-08

    In this paper, the two-dimensional Benney system describing long wave propagation of a finite depth fluid motion and the multi-dimensional Russo-Smereka kinetic equation describing a bubbly flow are considered. The Hamiltonian approach established by J. Gibbons for the one-dimensional Vlasov kinetic equation is extended to a multi-dimensional case. A local Hamiltonian structure associated with the hydrodynamic lattice of moments derived by D. J. Benney is constructed. A relationship between this hydrodynamic lattice of moments and the two-dimensional Vlasov kinetic equation is found. In the two-dimensional case, a Hamiltonian hydrodynamic lattice for the Russo-Smereka kinetic model is constructed. Simple hydrodynamic reductions are presented.

  20. Novel target design algorithm for two-dimensional optical storage (TwoDOS)

    NARCIS (Netherlands)

    Huang, Li; Chong, T.C.; Vijaya Kumar, B.V.K.; Kobori, H.

    2004-01-01

    In this paper we introduce the Hankel transform based channel model of Two-Dimensional Optical Storage (TwoDOS) system. Based on this model, the two-dimensional (2D) minimum mean-square error (MMSE) equalizer has been derived and applied to some simple but common cases. The performance of the 2D

  1. Two-dimensional ferroelectrics

    Energy Technology Data Exchange (ETDEWEB)

    Blinov, L M; Fridkin, Vladimir M; Palto, Sergei P [A.V. Shubnikov Institute of Crystallography, Russian Academy of Sciences, Moscow, Russian Federaion (Russian Federation); Bune, A V; Dowben, P A; Ducharme, Stephen [Department of Physics and Astronomy, Behlen Laboratory of Physics, Center for Materials Research and Analysis, University of Nebraska-Linkoln, Linkoln, NE (United States)

    2000-03-31

    The investigation of the finite-size effect in ferroelectric crystals and films has been limited by the experimental conditions. The smallest demonstrated ferroelectric crystals had a diameter of {approx}200 A and the thinnest ferroelectric films were {approx}200 A thick, macroscopic sizes on an atomic scale. Langmuir-Blodgett deposition of films one monolayer at a time has produced high quality ferroelectric films as thin as 10 A, made from polyvinylidene fluoride and its copolymers. These ultrathin films permitted the ultimate investigation of finite-size effects on the atomic thickness scale. Langmuir-Blodgett films also revealed the fundamental two-dimensional character of ferroelectricity in these materials by demonstrating that there is no so-called critical thickness; films as thin as two monolayers (1 nm) are ferroelectric, with a transition temperature near that of the bulk material. The films exhibit all the main properties of ferroelectricity with a first-order ferroelectric-paraelectric phase transition: polarization hysteresis (switching); the jump in spontaneous polarization at the phase transition temperature; thermal hysteresis in the polarization; the increase in the transition temperature with applied field; double hysteresis above the phase transition temperature; and the existence of the ferroelectric critical point. The films also exhibit a new phase transition associated with the two-dimensional layers. (reviews of topical problems)

  2. Three Dimensional Explicit Model for Cometary Tail Ions Interactions with Solar Wind

    Science.gov (United States)

    Al Bermani, M. J. F.; Alhamed, S. A.; Khalaf, S. Z.; Ali, H. Sh.; Selman, A. A.

    2009-06-01

    The different interactions between cometary tail and solar wind ions are studied in the present paper based on three-dimensional Lax explicit method. The model used in this research is based on the continuity equations describing the cometary tail-solar wind interactions. Three dimensional system was considered in this paper. Simulation of the physical system was achieved using computer code written using Matlab 7.0. The parameters studied here assumed Halley comet type and include the particle density rho, the particles velocity v, the magnetic field strength B, dynamic pressure p and internal energy E. The results of the present research showed that the interaction near the cometary nucleus is mainly affected by the new ions added to the plasma of the solar wind, which increases the average molecular weight and result in many unique characteristics of the cometary tail. These characteristics were explained in the presence of the IMF.

  3. Anion analysis in uranium more concentrates by ion chromatography

    International Nuclear Information System (INIS)

    Badaut, V.

    2009-01-01

    In the present exploratory study, the applicability of anionic impurities or attributing nuclear material to a certain chemical process or origin has been investigated. Anions (e.g., nitrate, sulphate, fluoride, chloride) originate from acids or salt solutions that are used for processing of solutions containing uranium or plutonium. The study focuses on uranium ore concentrates ('yellow cakes') originating from different mines. Uranium is mined from different types of ore body and depending on the type of rock, different chemical processes for leaching, dissolving and precipitating the uranium need to be applied. Consequently, the anionic patterns observed in he products of these processes (the 'ore concentrates') are different. The concentrations of different anionic species were measured by ion chromatography using conductivity detection. The results show clear differences of anion concentrations and patterns between samples from different uranium mines. Besides this, differences between sampling campaigns n a same mine were also observed indicating that the uranium ore is not homogeneous in a mine. These within-mine variations, however, were smaller than the between-mine variations. (author)

  4. Proteomic analysis of Bacillus thuringiensis at different growth phases by using an automated online two-dimensional liquid chromatography-tandem mass spectrometry strategy.

    Science.gov (United States)

    Huang, Shaoya; Ding, Xuezhi; Sun, Yunjun; Yang, Qi; Xiao, Xiuqing; Cao, Zhenping; Xia, Liqiu

    2012-08-01

    The proteome of a new Bacillus thuringiensis subsp. kurstaki strain, 4.0718, from the middle vegetative (T(1)), early sporulation (T(2)), and late sporulation (T(3)) phases was analyzed using an integrated liquid chromatography (LC)-based protein identification system. The system comprised two-dimensional (2D) LC coupled with nanoscale electrospray ionization (ESI) tandem mass spectrometry (MS/MS) on a high-resolution hybrid mass spectrometer with an automated data analysis system. After deletion of redundant proteins from the different batches and B. thuringiensis subspecies, 918, 703, and 778 proteins were identified in the respective three phases. Their molecular masses ranged from 4.6 Da to 477.4 Da, and their isoelectric points ranged from 4.01 to 11.84. Function clustering revealed that most of the proteins in the three phases were functional metabolic proteins, followed by proteins participating in cell processes. Small molecular and macromolecular metabolic proteins were further classified according to the Kyoto Encyclopedia of Genes and Genome and BioCyc metabolic pathway database. Three protoxins (Cry2Aa, Cry1Aa, and Cry1Ac) as well as a series of potential intracellular active factors were detected. Many significant proteins related to spore and crystal formation, including sporulation proteins, help proteins, chaperones, and so on, were identified. The expression patterns of two identified proteins, CotJc and glutamine synthetase, were validated by Western blot analysis, which further confirmed the MS results. This study is the first to use shotgun technology to research the proteome of B. thuringiensis. Valuable experimental data are provided regarding the methodology of analyzing the B. thuringiensis proteome (which can be used to produce insecticidal crystal proteins) and have been added to the related protein database.

  5. Two-Dimensional Materials for Sensing: Graphene and Beyond

    Directory of Open Access Journals (Sweden)

    Seba Sara Varghese

    2015-09-01

    Full Text Available Two-dimensional materials have attracted great scientific attention due to their unusual and fascinating properties for use in electronics, spintronics, photovoltaics, medicine, composites, etc. Graphene, transition metal dichalcogenides such as MoS2, phosphorene, etc., which belong to the family of two-dimensional materials, have shown great promise for gas sensing applications due to their high surface-to-volume ratio, low noise and sensitivity of electronic properties to the changes in the surroundings. Two-dimensional nanostructured semiconducting metal oxide based gas sensors have also been recognized as successful gas detection devices. This review aims to provide the latest advancements in the field of gas sensors based on various two-dimensional materials with the main focus on sensor performance metrics such as sensitivity, specificity, detection limit, response time, and reversibility. Both experimental and theoretical studies on the gas sensing properties of graphene and other two-dimensional materials beyond graphene are also discussed. The article concludes with the current challenges and future prospects for two-dimensional materials in gas sensor applications.

  6. Determination of calcium and magnesium in nuclear grade alumina by ion chromatography technique

    International Nuclear Information System (INIS)

    Hespanhol, E.C.B.; Pires, M.A.F.; Atalla, L.T.

    1987-07-01

    A simple method for solubilization of alumina and separation of magnesium and calcium from alumina matrix was developed by initial coprecipitation of those elements with iron(III) hydroxide. Calcium and magnesium were later separated from iron chloride anionic complex in a Dowex 1-X 10 anionic exchange resin. The ion chromatography tecnnique was employed for the analysis of calcium and magnesium. One hundred percent recovery for calcium and magnesium was obtained in their separation from alumina. A precision of 6% and 10% for magnesium and calcium, respectively, was obtained in alumina samples analysis which contain less than 0,02% of magnesium and less than 0,08% of calcium. (Author) [pt

  7. Two-dimensional calculus

    CERN Document Server

    Osserman, Robert

    2011-01-01

    The basic component of several-variable calculus, two-dimensional calculus is vital to mastery of the broader field. This extensive treatment of the subject offers the advantage of a thorough integration of linear algebra and materials, which aids readers in the development of geometric intuition. An introductory chapter presents background information on vectors in the plane, plane curves, and functions of two variables. Subsequent chapters address differentiation, transformations, and integration. Each chapter concludes with problem sets, and answers to selected exercises appear at the end o

  8. Magnetic structure of the quasi-two-dimensional compound CoTa{sub 2}O{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Kinast, E.J. [Universidade Estadual do Rio Grande do Sul, Rua 7 de Setembro, 1156, 90010-191 Porto Alegre (Brazil); Santos, C.A. dos [Instituto de Fisica, Universidade Federal do Rio Grande do Sul, C.P. 15051, 91501-970 Porto Alegre (Brazil); Schmitt, D. [Laboratoire de Geophysique Interne et Tectonophysique, Universite Joseph Fourier, B. P. 53, 38041 Grenoble Cedex 9 (France); Isnard, O., E-mail: olivier.isnard@grenoble.cnrs.f [Institut Neel, CNRS/Universite Jospeh Fourier, avenue des martyrs B. P. 166, 38042 Grenoble Cedex 9 (France); Gusmao, M.A.; Cunha, J.B.M. da [Instituto de Fisica, Universidade Federal do Rio Grande do Sul, C.P. 15051, 91501-970 Porto Alegre (Brazil)

    2010-02-18

    We report on a detailed investigation of magnetic properties of CoTa{sub 2}O{sub 6} using several techniques: neutron and X-ray diffraction, specific-heat, magnetic susceptibility, and magnetization measurements. The compound shows quasi-two-dimensional behavior due to its layered structure of alternating Co-O and Ta-O planes. We find that all magnetic moments lie entirely in the Co-O planes, along easy axes determined by the orientations of oxygen octahedra that surround the Co ions. The easy axes in successive magnetic planes have relative orientations that differ by 90{sup o}. Antiferromagnetic ordering is observed below 6.6 K, with propagation vectors ({+-}1/4,1/4,1/4) associated to the two non-equivalent sets of Co{sup 2+} ions, whose magnetic moments are perpendicularly oriented.

  9. Phase transitions in two-dimensional systems

    International Nuclear Information System (INIS)

    Salinas, S.R.A.

    1983-01-01

    Some experiences are related using synchrotron radiation beams, to characterize solid-liquid (fusion) and commensurate solid-uncommensurate solid transitions in two-dimensional systems. Some ideas involved in the modern theories of two-dimensional fusion are shortly exposed. The systems treated consist of noble gases (Kr,Ar,Xe) adsorbed in the basal plane of graphite and thin films formed by some liquid crystal shells. (L.C.) [pt

  10. Ultrasensitive and simultaneous detection of heavy metal ions based on three-dimensional graphene-carbon nanotubes hybrid electrode materials

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Hui; Chen, Ting [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Liu, Xiuyu [Shandong Academy of Sciences, Jinan 250114 (China); Ma, Houyi, E-mail: hyma@sdu.edu.cn [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2014-12-10

    Highlights: • Three-dimensional graphene-MWCNTs nanocomposites were prepared. • Graphene-MWCNTs based electrochemical sensor was used to detect heavy metal ions for the first time. • The proposed sensor was certified capable for real sample with satisfactory results. - Abstract: A green and facile method was developed to prepare a novel hybrid nanocomposite that consisted of one-dimensional multi-walled carbon nanotubes (MWCNTs) and two-dimensional graphene oxide (GO) sheets. The as-prepared three-dimensional GO–MWCNTs hybrid nanocomposites exhibit excellent water-solubility owing to the high hydrophilicity of GO components; meanwhile, a certain amount of MWCNTs loaded on the surface of GO sheets through π–π interaction seem to be “dissolved” in water. Moreover, the graphene(G)-MWCNTs nanocomposites with excellent conductivity were obtained conveniently by the direct electrochemical reduction of GO–MWCNTs nanocomposites. Seeing that there is a good synergistic effect between MWCNTs and graphene components in enhancing preconcentration efficiency of metal ions and accelerating electron transfer rate at G-MWCNTs/electrolyte interface, the G-MWCNTs nanocomposites possess fast, simultaneous and sensitive detection performance for trace amounts of heavy metal ions. The electrochemical results demonstrate that the G-MWCNTs nanocomposites can act as a kind of practical sensing material to simultaneously determine Pb{sup 2+} and Cd{sup 2+} ions in terms of anodic stripping voltammetry (ASV). The linear calibration plots for Pb{sup 2+} and Cd{sup 2+} ranged from 0.5 μg L{sup −1} to 30 μg L{sup −1}. The detection limits were determined to be 0.2 μg L{sup −1} (S/N = 3) for Pb{sup 2+} and 0.1 μg L{sup −1} (S/N = 3) for Cd{sup 2+} in the case of a deposition time of 180 s. It is worth mentioning that the G-MWCNTs modified electrodes were successfully applied to the simultaneous detection of Cd{sup 2+} and Pb{sup 2+} ions in real electroplating

  11. Determination of anionic surfactants during wastewater recycling process by ion pair chromatography with suppressed conductivity detection

    Science.gov (United States)

    Levine, L. H.; Judkins, J. E.; Garland, J. L.; Sager, J. C. (Principal Investigator)

    2000-01-01

    A direct approach utilizing ion pairing reversed-phase chromatography coupled with suppressed conductivity detection was developed to monitor biodegradation of anionic surfactants during wastewater recycling through hydroponic plant growth systems and fixed-film bioreactors. Samples of hydroponic nutrient solution and bioreactor effluent with high concentrations (up to 120 mS electrical conductance) of inorganic ions can be analyzed without pretreatment or interference. The presence of non-ionic surfactants did not significantly affect the analysis. Dynamic linear ranges for tested surfactants [Igepon TC-42, ammonium lauryl sulfate, sodium laureth sulfate and sodium alkyl (C10-C16) ether sulfate] were 2 to approximately 500, 1 to approximately 500, 2.5 to approximately 550 and 3.0 to approximately 630 microg/ml, respectively.

  12. The theory of critical phenomena in two-dimensional systems

    International Nuclear Information System (INIS)

    Olvera de la C, M.

    1981-01-01

    An exposition of the theory of critical phenomena in two-dimensional physical systems is presented. The first six chapters deal with the mean field theory of critical phenomena, scale invariance of the thermodynamic functions, Kadanoff's spin block construction, Wilson's renormalization group treatment of critical phenomena in configuration space, and the two-dimensional Ising model on a triangular lattice. The second part of this work is made of four chapters devoted to the application of the ideas expounded in the first part to the discussion of critical phenomena in superfluid films, two-dimensional crystals and the two-dimensional XY model of magnetic systems. Chapters seven to ten are devoted to the following subjects: analysis of long range order in one, two, and three-dimensional physical systems. Topological defects in the XY model, in superfluid films and in two-dimensional crystals. The Thouless-Kosterlitz iterated mean field theory of the dipole gas. The renormalization group treatment of the XY model, superfluid films and two-dimensional crystal. (author)

  13. Separation of deuteriated isotopomers of dopamine by ion-pair reversed-phase high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Masters, C.F.; Markey, S.P.; Mefford, I.N.; Duncan, M.W.

    1988-01-01

    The ion-pair reversed-phase separation of dopamine and deuterium-substituted dopamine isotopomers is described. Chromatographic parameters and deuterium isotope effects governing the resolution are examined and compared to the factors regulating the resolution are examined and compared to the factors regulating the resolution of the chemically distinct entities dopamine, norepinephrine, and epinephrine. The potential utility of the [ 2 H 7 ]dopamine, isotopomer as an internal standard for the high-performance liquid chromatography analysis of dopamine is demonstrated by using aluminum oxide extraction prior to chromatographic separation

  14. Hydrothermal carbon nanosphere-based agglomerated anion exchanger for ion chromatography.

    Science.gov (United States)

    Zhao, Qiming; Wu, Shuchao; Zhang, Kai; Lou, Chaoyan; Zhang, Peiming; Zhu, Yan

    2016-10-14

    This work reports the application of hydrothermal carbon nanospheres (HCNSs) as stationary phases in ion chromatography. HCNSs were facilely quaternized through polycondensation of methylamine and 1,4-butanediol diglycidyl ether. The quaternization was confirmed by Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. Owing to the electrostatic interaction, quaternized HCNSs were equably attached onto the surface of sulfonated polystyrene-divinylbenzene (PS-DVB) beads to construct the anion exchangers. The aggregation was verified by scanning electron microscopy and elemental analysis. Common anions, aliphatic monocarboxylic acids, polarizable anions, and aromatic acids were well separated on the stationary phases with good stability and symmetry. The prepared column was further applied to detect phosphate content in Cola drink samples. The limit of detection (S/N=3) was 0.09mg/L, and the relative standard deviation (n=10) of retention time was 0.31%. The average recovery was 99.58%. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Transition-metal-doped group-IV monochalcogenides: a combination of two-dimensional triferroics and diluted magnetic semiconductors

    Science.gov (United States)

    Yang, Liu; Wu, Menghao; Yao, Kailun

    2018-05-01

    We report the first-principles evidence of a series of two-dimensional triferroics (ferromagnetic + ferroelectric + ferroelastic), which can be obtained by doping transition-metal ions in group-IV monochalcogenide (SnS, SnSe, GeS, GeSe) monolayers, noting that a ferromagnetic Fe-doped SnS2 monolayer has recently been realized (Li B et al 2017 Nat. Commun. 8 1958). The ferroelectricity, ferroelasticity and ferromagnetism can be coupled and the magnetization direction may be switched upon ferroelectric/ferroelastic switching, rendering electrical writing + magnetic reading possible. They can be also two-dimensional half-metals or diluted magnetic semiconductors, where p/n channels or even multiferroic tunneling junctions can be designed by variation in doping and incorporated into a monolayer wafer.

  16. Dimethylamine and ammonia measurements with ion chromatography during the CLOUD4 campaign

    CERN Document Server

    Praplan, A P; Dommen, J; Baltensperger, U

    2012-01-01

    The CLOUD project investigates the influence of galactic cosmic rays on the nucleation of new particles in an environmental chamber at CERN. Dimethylamine (DMA) was injected intentionally into the CLOUD chamber to reach atmospherically relevant levels away from sources (up to 100 pptv) in order to study its effect on nucleation with sulphuric acid and water at 278 K. Quantification of DMA and also background ammonia (NH 3 ) was performed with ion chromatography (IC). The IC method used together with the sampling line developed for CLOUD in order to measure NH 3 and DMA at low pptv levels is described; the overall sampling efficiency of the method is discussed; and, finally, mixing ratios of NH 3 and DMA measured during CLOUD4 are reported.

  17. Mass spectrometer with two ion sources

    International Nuclear Information System (INIS)

    Glickman, L.G.; Mit', A.G.

    2002-01-01

    Static mass spectrometer with mid-plane near which ions are moving is considered in this article. Two ion sources are used, their exit slits are perpendicular to the mid-plane. The simple method of the replacement of source is offered. Two concave two-electrode transaxial mirrors with two-plate electrodes are used for this aim. The mid-plane of these mirrors coincides with the mid-plane of the device. The exit slit of each source is located in the principal plane of the object space. The principal planes of the image space of the both mirrors coincide. The images of the exit slits of the sources are in these planes and coincide too. We used the mirrors making stigmatic images with the magnification one to one, in which the dispersion on energy and spherical aberrations of the second order are equal to zero. These images are the objects on which the ion-optical system of the mass spectrometer is tuned. When you choose one from two ion sources it is enough to switch the corresponding mirror

  18. Using contemporary liquid chromatography theory and technology to improve capillary gradient ion-exchange separations.

    Science.gov (United States)

    Wouters, Bert; Broeckhoven, Ken; Wouters, Sam; Bruggink, Cees; Agroskin, Yury; Pohl, Christopher A; Eeltink, Sebastiaan

    2014-11-28

    The gradient-performance limits of capillary ion chromatography have been assessed at maximum system pressure (34.5 MPa) using capillary columns packed with 4.1 μm macroporous anion-exchange particles coated with 65 nm positively-charged nanobeads. In analogy to the van-Deemter curve, the gradient performance was assessed applying different flow rates, while decreasing the gradient time inversely proportional to the increase in flow rate in order to maintain the same retention properties. The gradient kinetic-performance limits were determined at maximum system pressure, applying tG/t0=5, 10, and 20. In addition, the effect of retention on peak width was assessed in gradient mode for mono-, di-, and trivalent inorganic anions. The peak width of late-eluting ions can be significantly reduced by using concave gradient, resulting in better detection sensitivity. A signal enhancement factor of 8 was measured for a late-eluting ion when applying a concave instead of a linear gradient. For the analysis of a complex anion mixture, a coupled column with a total length of 1.05 m was operated at the kinetic-performance limit applying a linear 250 min gradient (tG/t0=10). The peak capacity varied between 200 and 380 depending on analyte retention, and hence on charge and size of the ion. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Three-dimensional ultrastructure of osteocytes assessed by focused ion beam-scanning electron microscopy (FIB-SEM).

    Science.gov (United States)

    Hasegawa, Tomoka; Yamamoto, Tomomaya; Hongo, Hiromi; Qiu, Zixuan; Abe, Miki; Kanesaki, Takuma; Tanaka, Kawori; Endo, Takashi; de Freitas, Paulo Henrique Luiz; Li, Minqi; Amizuka, Norio

    2018-04-01

    The aim of this study is to demonstrate the application of focused ion beam-scanning electron microscopy, FIB-SEM for revealing the three-dimensional features of osteocytic cytoplasmic processes in metaphyseal (immature) and diaphyseal (mature) trabeculae. Tibiae of eight-week-old male mice were fixed with aldehyde solution, and treated with block staining prior to FIB-SEM observation. While two-dimensional backscattered SEM images showed osteocytes' cytoplasmic processes in a fragmented fashion, three-dimensional reconstructions of FIB-SEM images demonstrated that osteocytes in primary metaphyseal trabeculae extended their cytoplasmic processes randomly, thus maintaining contact with neighboring osteocytes and osteoblasts. In contrast, diaphyseal osteocytes extended thin cytoplasmic processes from their cell bodies, which ran perpendicular to the bone surface. In addition, these osteocytes featured thick processes that branched into thinner, transverse cytoplasmic processes; at some point, however, these transverse processes bend at a right angle to run perpendicular to the bone surface. Osteoblasts also possessed thicker cytoplasmic processes that branched off as thinner processes, which then connected with cytoplasmic processes of neighboring osteocytes. Thus, FIB-SEM is a useful technology for visualizing the three-dimensional structures of osteocytes and their cytoplasmic processes.

  20. Three-dimensional, two-species magnetohydrodynamic studies of the early time behaviors of the Combined Release and Radiation Effects Satellite G2 barium release

    International Nuclear Information System (INIS)

    Xie, Lianghai; Li, Lei; Wang, Jingdong; Zhang, Yiteng

    2014-01-01

    We present a three-dimensional, two-species (Ba + and H + ) MHD model to study the early time behaviors of a barium release at about 1 R E like Combined Release and Radiation Effects Satellite G2, with emphasis placed on the three-dimensional evolution of the barium cloud and its effects on the ambient plasma environment. We find that the perturbations caused by the cloud are the combined results of the initial injection, the radial expansion, and the diamagnetic effect and propagate as fast MHD waves in the magnetosphere. In return, the transverse expansion and the cross-B motion of barium ions are constrained by the magnetic force, which lead to a field-aligned striation of ions and the decoupling of these ions from the neutrals. Our simulation shows the formation and collapse of the diamagnetic cavity in the barium cloud. The estimated time scale for the cavity evolution might be much shorter if photoionization time scale and field aligned expansion of barium ions are considered. In addition, our two species MHD simulation also finds the snowplow effect resulting from the momentum coupling between barium ions and background H + , which creates density hole and bumps in the background H + when barium ions expanding along the magnetic field lines