WorldWideScience

Sample records for correlation ion chromatography

  1. 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

  2. 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

  3. 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"…

  4. 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.

  5. Correlation ion mobility spectroscopy

    Science.gov (United States)

    Pfeifer, Kent B [Los Lunas, NM; Rohde, Steven B [Corrales, NM

    2008-08-26

    Correlation ion mobility spectrometry (CIMS) uses gating modulation and correlation signal processing to improve IMS instrument performance. Closely spaced ion peaks can be resolved by adding discriminating codes to the gate and matched filtering for the received ion current signal, thereby improving sensitivity and resolution of an ion mobility spectrometer. CIMS can be used to improve the signal-to-noise ratio even for transient chemical samples. CIMS is especially advantageous for small geometry IMS drift tubes that can otherwise have poor resolution due to their small size.

  6. 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 ...

  7. 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

  8. 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

  9. 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

  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. 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)

  12. 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

  13. 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.

  14. Correlated ion stopping in plasmas

    International Nuclear Information System (INIS)

    Zwicknagel, G.; Deutsch, C.

    1997-01-01

    The basic features of correlated ion stopping in plasmas are demonstrated by employing two opposite extremes of cluster structures, a statistical model with a spatial ion distribution of Gaussian shape and the highly regular configuration of N-ion chains and cubic boxes. In the case of the ion chains the resonant character of correlated stopping due to the interference of the excited wake fields is discussed in detail. The general behavior of correlation effects is summarized and its dependence on the ratio of cluster size and interion spacing to the screening length in the plasma, as well as the ratio of the cluster velocity to the mean electron velocity in the target, is stressed out. The validity and applicability of the dielectric response formalism used for describing correlated stopping is critically reviewed. A scheme is presented to extend the linear formalism to weak nonlinear situations that occur, in particular, for small highly charged clusters at moderate or low velocities. For the Gaussian cluster a fit formula is given, which allows a fast and accurate calculation of the enhancement of stopping due to correlation effects and applies for all degrees of degeneracy of the electrons and arbitrary cluster velocities. copyright 1997 The American Physical Society

  15. 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

  16. 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)

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. 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)

  3. ISCO Grab Sample Ion Chromatography Analytical Data

    Data.gov (United States)

    U.S. Environmental Protection Agency — ISCO grab samples were collected from river, wastewater treatment plant discharge, and public drinking water intakes. Samples were analyzed for major ions (ppb)...

  4. 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)

  5. 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)

  6. 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

  7. 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

  8. 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.

  9. 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.

  10. 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

  11. 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...

  12. 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

  13. 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)

  14. 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.

  15. Pion correlations in heavy ion collision

    International Nuclear Information System (INIS)

    Venema, L.

    1991-01-01

    Charged π-correlations are a well established experimental technique to obtain information about π-source sizes. This is, however, not the case for π 0 's, as they decay into photons, resulting in measurements of 4 photon correlations. Here is described what these correlations are, what the problems are to detect and interpret them. These correlations are an additional way to get more information out of the heavy ion collisions. (orig.)

  16. 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.

  17. 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

  18. 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.

  19. 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...

  20. 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

  1. 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)

  2. 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

  3. Observations of strong ion-ion correlations in dense plasmas

    Energy Technology Data Exchange (ETDEWEB)

    Ma, T.; Fletcher, L.; Pak, A.; Chapman, D. A.; Falcone, R. W.; Fortmann, C.; Galtier, E.; Gericke, D. O.; Gregori, G.; Hastings, J.; Landen, O. L.; Le Pape, S.; Lee, H. J.; Nagler, B.; Neumayer, P.; Turnbull, D.; Vorberger, J.; White, T. G.; Wünsch, K.; Zastrau, U.; Glenzer, S. H.; Döppner, T.

    2014-05-01

    Using simultaneous spectrally, angularly, and temporally resolved x-ray scattering, we measure the pronounced ion-ion correlation peak in a strongly coupled plasma. Laser-driven shock-compressed aluminum at ~3× solid density is probed with high-energy photons at 17.9 keV created by molybdenum He-α emission in a laser-driven plasma source. The measured elastic scattering feature shows a well-pronounced correlation peak at a wave vector of k=4k=4Å-1. The magnitude of this correlation peak cannot be described by standard plasma theories employing a linear screened Coulomb potential. Advanced models, including a strong short-range repulsion due to the inner structure of the aluminum ions are however in good agreement with the scattering data. These studies have demonstrated a new highly accurate diagnostic technique to directly measure the state of compression and the ion-ion correlations. We have since applied this new method in single-shot wave-number resolved S(k) measurements to characterize the physical properties of dense plasmas.

  4. 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.

  5. 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.)

  6. 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...

  7. 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.

  8. 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

  9. 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.

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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)

  15. Chromatography.

    Science.gov (United States)

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  16. 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.)

  17. 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)

  18. 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.

  19. Ion-ion correlations across and between electrified graphene layers

    Science.gov (United States)

    Mendez-Morales, Trinidad; Burbano, Mario; Haefele, Matthieu; Rotenberg, Benjamin; Salanne, Mathieu

    2018-05-01

    When an ionic liquid adsorbs onto a porous electrode, its ionic arrangement is deeply modified due to a screening of the Coulombic interactions by the metallic surface and by the confinement imposed upon it by the electrode's morphology. In particular, ions of the same charge can approach at close contact, leading to the formation of a superionic state. The impact of an electrified surface placed between two liquid phases is much less understood. Here we simulate a full supercapacitor made of the 1-butyl-3-methylimidazolium hexafluorophosphate and nanoporous graphene electrodes, with varying distances between the graphene sheets. The electrodes are held at constant potential by allowing the carbon charges to fluctuate. Under strong confinement conditions, we show that ions of the same charge tend to adsorb in front of each other across the graphene plane. These correlations are allowed by the formation of a highly localized image charge on the carbon atoms between the ions. They are suppressed in larger pores, when the liquid adopts a bilayer structure between the graphene sheets. These effects are qualitatively similar to the recent templating effects which have been reported during the growth of nanocrystals on a graphene substrate.

  20. Recovery of monosaccharides from lignocellulosic hydrolysates by ion exclusion chromatography.

    Science.gov (United States)

    Lodi, Gabriele; Pellegrini, Laura Annamaria; Aliverti, Alessandro; Rivas Torres, Beatriz; Bernardi, Marco; Morbidelli, Massimo; Storti, Giuseppe

    2017-05-05

    The production of sugars from lignocellulosic biomass is the key to a sustainable, renewable chemical industry. Glucose, xylose and other monosaccharides can be easily produced by hydrolyzing cellulose and hemicellulose, the primary polysaccharides in biomass. However, the hydrolysis of biomass generates byproducts that, together with the mineral acid normally added in the hydrolysis step, have to be removed before the downstream conversion processes. In this work, the recovery of monosaccharides from lignocellulosic hydrolysates by means of Ion Exclusion Chromatography (IEC) has been studied. The analyzed process relies on new pretreatment and hydrolysis steps, involving the neutralization of the hydrolysate with sodium hydroxide. The adsorption behavior of the main components involved in the separation has been experimentally investigated. Pulse tests at the high loading encountered in preparative conditions have been performed for a selected group of model components found in the hydrolysates. For all the electrolytes, the retention volume fraction was always between the interparticle porosity and the total column porosity, confirming that ion exclusion was the dominant retention mechanism. On the other hand, sugars eluted before the total column porosity, indicating partial steric exclusion from the resin pores. This observation was then confirmed by size-exclusion experiments with polyethylene glycol standards, from which the distribution coefficient of the studied sugars has been determined. The comparison between the elution profiles of the same sugars in pure form and as a mixture present in the hydrolysate showed differences in both peak shape and retention times. Therefore, an investigation of the influence of the main electrolytes contained in the hydrolysates on sugars adsorption has been performed through the pulse on a plateau method. The electrolytes were found to enhance the sugars retention by promoting their adsorption onto the resin. However

  1. 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.

  2. 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...

  3. [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.

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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

  9. Enrichment of 15N by ion exchange chromatography

    International Nuclear Information System (INIS)

    Ohwaki, Masao; Ohtsuka, Haruhisa; Nomura, Masao; Okamoto, Makoto; Fujii, Yasuhiko

    1996-01-01

    15 N isotope separation was studied using cation exchange resins which consist of functional groups: sulfonic acid, carboxylic acid and phenol at various concentration of the eluent LiOH. The isotope separation coefficients for these ion exchange resins were observed to be nearly equal, in spite of the large difference in ion exchange characteristics. The effect of flow rate on 15 N isotope separation was also studied, and the results indicate that the operation at high flow rate would be preferable for the industrial process of 15 N enrichment. Based on the preliminary investigations, a continuous operation using a series of ion exchange columns has been carried out in order to achieve high enrichment of 15 N. (author)

  10. Graphene-coated polymeric anion exchangers for ion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Kai; Cao, Minyi; Lou, Chaoyan [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028 (China); Wu, Shuchao, E-mail: wushch2002@163.com [Zhejiang Institute of Geology and Mineral Resources, Hangzhou 310007 (China); Zhang, Peimin [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028 (China); Zhi, Mingyu [Hangzhou Vocational & Technical College, Hangzhou, 310018 (China); Zhu, Yan, E-mail: zhuyan@zju.edu.cn [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028 (China)

    2017-06-01

    Carbonaceous stationary phases have gained much attention for their peculiar selectivity and robustness. Herein we report the fabrication and application of a graphene-coated polymeric stationary phase for anion exchange chromatography. The graphene-coated particles were fabricated by a facile evaporation-reduction method. These hydrophilic particles were proven appropriate substrates for grafting of hyperbranched condensation polymers (HBCPs) to make pellicular anion exchangers. The new phase was characterized by zeta potentials, Fourier transform infrared spectroscopy, thermogravimetry and scanning electron microscope. Frontal displacement chromatography showed that the capacities of the anion exchangers were tuned by both graphene amount and HBCPs layer count. The chromatographic performance of graphene-coated anion exchangers was demonstrated with separation of inorganic anions, organic acids, carbohydrates and amino acids. Good reproducibility was obtained by consecutive injections, indicating high chemical stability of the coating. - Highlights: • Graphene-coated polymeric particles were fabricated by a facile method. • Hyperbranched condensation polymers (HBCPs) were grafted from graphene-coated particles to make anion exchangers. • Graphene amount and HBCPs layer count had significant effects on the anion exchange capacities. • Separation of diverse anionic analytes on the anion exchangers was demonstrated. • The prepared anion exchangers exhibited high stability.

  11. 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

  12. 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,

  13. 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.

  14. 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.

  15. 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

  16. 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...

  17. 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.

  18. 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%

  19. Electron-ion correlation effects in ion-atom single ionization

    Energy Technology Data Exchange (ETDEWEB)

    Colavecchia, F.D.; Garibotti, C.R. [Centro Atomico Bariloche and Consejo Nacional de Investigaciones Cientificas y Tecnicas, 8400 San Carlos de Bariloche (Argentina); Gasaneo, G. [Departamento de Fisica, Universidad Nacional del Sur, Av. Alem 1253, 8000 Bahia Blanca (Argentina)

    2000-06-28

    We study the effect of electron-ion correlation in single ionization processes of atoms by ion impact. We present a distorted wave model where the final state is represented by a correlated function solution of a non-separable three-body continuum Hamiltonian, that includes electron-ion correlation as coupling terms of the wave equation. A comparison of the electronic differential cross sections computed with this model with other theories and experimental data reveals that the influence of the electron-ion correlation is more significant for low energy emitted electrons. (author). Letter-to-the-editor.

  20. 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.

  1. Chromatography of metal ions with a triazine chelating resin

    International Nuclear Information System (INIS)

    Wang, W.N.

    1979-05-01

    The synthesis, characterization, and some analytical applications of a new triazine resin are described. Separation of group IB, IIB, VIB, and VIIB metal ions from group VIII metal ions is achieved by this PDT-4 resin. Calcium(II) and magnesium(II) are taken up at pH = 6, 0.1 M acetate and are eluted at pH = 6, 0.1 M sodium nitrate. Copper(II) is retained at pH = 6, 0.1 M acetate and pH = 1 hydrochloric acid and is eluted subsequently by 5 M perchloric acid. Molybdenum(VI) is sorbed selectively from 0.1 N sulfuric acid or hydrochloric acid and is eluted in a tight band by 0.1 N sodium hydroxide. Numerous rapid column chromatographic separations are reported using this new resin, including analysis of NBS standard samples

  2. Ra/Ca separation by ion exchange chromatography

    International Nuclear Information System (INIS)

    Flores Mendoza, J.

    1990-01-01

    Ra/Ca separation by ion exchange. The objective of this work was to acquire knowledge of the chromatographic behaviour of the alkaline earth cations calcium, barium and radium and the obtention of well-defined alpha spectra of 226 Ra. Three cationic ion exchange resins (Dower 50 W-X8, AG 50W-XB and Merck I) and three complexing agents (ethylenediaminetetraacetic acid, citric acid and tartaric acid) at various pH values have been investigated. The three types of ions are fixed on the resins at pH 4.8; calcium is eluted at pH between 5 and 6 depending on the resin; barium and radium are eluted at pH values from 8 to 11. Radium is also eluted with a 2 M nitric acid solution, from which it can be electrodeposited on a stainless steel disk potassium fluoride as electrolyte at pH 14. The electrolysis is conducted for 18 hours with a current of mA. Under these conditions high resolution alpha spectra were obtained for 226 Ra, which was practically free from radioactive contaminants (Author)

  3. [Study on the analysis of organogermanium compounds by ion chromatography].

    Science.gov (United States)

    Chen, Q; Mou, S; Hou, X; Ni, Z

    1997-05-01

    A new high performance ion exchange chromatographic method for separation and determination of three organogermanium compounds beta-carboxyethylgermanium sesquioxide (I), beta-(alpha-methyl) carboxyethylgermanium sesquioxide (II) and di-(beta-carboxyethyl) germanium hydroxide (III) has been developed. A Dionex DX-300 Ion Chromatograph equipped with a Dionex PED-II pulsed electrochemical detector (conductivity mode), a Dionex AMMS-1 anion micromembrane suppressor, and a Dionex ACI advanced computer interface coupled with AI-450 chromatographic software was employed. The separation was achieved by using a Dionex IonPac AS4A-SC column as analytical column, sodium tetraborate solution as eluent, and sulfuric acid solution as regenerant. For reducing run time, a gradient program was chosen. The detection limits (S/N = 3, expressed as germanium) for the three compounds were 0.038mg/L (I), 0.035mg/L (II) and 0.025mg/L (III), respectively. The method has been applied to the analysis of two tonic oral drinks, and the average recoveries for the three compounds ranged from 95%-101%. The results obtained were in agreement with those of hydride generation atomic fluorescence spectrometry (HG-AFS).

  4. 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.

  5. 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.

  6. [Determination of 21 fragrance allergens in toys by gas chromatography-ion trap mass spectrometry].

    Science.gov (United States)

    Lü, Qing; Zang, Qing; Bai, Hua; Li, Haiyu; Kang, Suyuan; Wang, Chao

    2012-05-01

    A method of gas chromatography-ion trap mass spectrometry (GC-IT-MS) was developed for the determination of 21 fragrance allergens in sticker toys, plush toys and plastic toys. The experimental conditions, such as sample pretreatment conditions, and the analytical conditions of GC-IT-MS, were optimized. The sticker toy samples and plush toy samples were extracted with acetone by ultrasonic wave, and the extracts were separated on an Agilent HP-1 MS column (50 m x 0.2 mm x 0.5 microm), then determined by IT-MS and quantified by external standard method. The plastic toy samples were extracted by the dissolution-precipitation approach, cleaned up with an Envi-carb solid phase extraction column and concentrated by rotary evaporation and nitrogen blowing, then determined by GC-IT-MS and quantified by external standard method. The calibration curves showed good linearity in the range of 0.002-50 mg/L with the correlation coefficients greater than 0.996 8. The limits of quantification (LOQ, S/N > 10) were 0.02-40 mg/kg. The average recoveries of the target compounds spiked in the sample at three concentration levels were in the range of 82.2%-110.8% with the relative standard deviations (RSDs) of 0.6%-10.5%. These results show that this method is accurate and sensitive for the qualitative and quantitative determination of the 21 fragrance allergens in the 3 types of toys.

  7. Simultaneous Determination of Different Anions in Milk Samples Using Ion Chromatography with Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Gülçin Gümüş Yılmaz

    2016-12-01

    Full Text Available The description of a simple method for simultaneous determination of chloride, nitrate, sulfate, iodide, phosphate, thiocyanate, perchlorate, and orotic acid in milk samples was outlined. The method involves the use of dialysis cassettes for matrix elimination, followed by ion chromatography on a high capacity anion exchange column with suppressed conductivity detection. The novelty of dialysis process was that it did not need any chemical and organic solvent for elimination of macromolecules such as fat, carbohydrates and proteins from milk samples. External standard calibration curves for these analytes were linear with great correlation coefficients. The relative standard deviations of analyte concentrations were acceptable both inter-day and intra-day evaluations. Under optimized conditions, the limit of detection (Signal-to-Noise ratio = 3 for chloride, phosphate, thiocyanate, perchlorate, iodide, nitrate, sulfate, and orotate was found to be 0.012, 0.112, 0.140, 0.280, 0.312, 0.516, 0.520, and 0.840 mg L−1, respectively. Significant results were obtained for various spiked milk samples with % recovery in the range of 93.88 - 109.75 %. The proposed method was successfully applied to milk samples collected from Istanbul markets. The advantages of the method described herein are reagent-free, simple, and reliable.

  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. 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

  10. 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.)

  11. Correlated charge changing ion-atom collisions

    International Nuclear Information System (INIS)

    Bernstein, E.M.; Tanis, J.A.

    1990-02-01

    This report summarizes the progress and accomplishments in accelerator atomic physics research supported by DOE grant FG02-87ER13778 from August 15, 1987 through February 15, 1990. The general scope of this work involves the experimental investigation of fundamental atomic interactions in collisions of highly charged projectiles with neutral targets, with a particular emphasis on two-electron interactions. Inner-shell processes involving excitation, ionization, and charge transfer are investigated using, for the most part, coincidence techniques in which projectile charge-changing events are associated with x-ray emission, target recoil ions, or electron emission. Measurements were conducted using accelerators at the Lawrence Berkeley Laboratory (LBL), Argonne National Laboratory (ANL), Hahn-Meitner-Institut, Berlin (HMI), and Western Michigan University (WMU). The research described here has resulted in 34 published papers, 14 invited presentations at national and international meetings, and 31 contributed presentations. Brief summaries of work completed and work in progress are discussed in this paper

  12. 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.

  13. 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

  14. 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)

  15. 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

  16. 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

  17. 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.

  18. 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

  19. 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.

  20. 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.

  1. Ion Correlation Effects in Salt-Doped Block Copolymers

    Science.gov (United States)

    Brown, Jonathan R.; Seo, Youngmi; Hall, Lisa M.

    2018-03-01

    We apply classical density functional theory to study how salt changes the microphase morphology of diblock copolymers. Polymers are freely jointed and one monomer type favorably interacts with ions, to account for the selective solvation that arises from different dielectric constants of the microphases. By including correlations from liquid state theory of an unbound reference fluid, the theory can treat chain behavior, microphase separation, ion correlations, and preferential solvation, at the same coarse-grained level. We show good agreement with molecular dynamics simulations.

  2. Two-gluon correlations in heavy–light ion collisions

    International Nuclear Information System (INIS)

    Wertepny, Douglas E.

    2014-01-01

    We derive the cross-section for two-gluon production in heavy–light ion collisions in the saturation/Color Glass Condensate framework. This calculation includes saturation effects to all orders in one of the nuclei (heavy ion) along with a single saturation correction in the projectile (light ion). The calculation of the correlation function predicts (qualitatively) two identical ridge-like correlations, near- and away-side. This prediction was later supported by experimental findings in p + A collisions at the LHC. Concentrating on the energy and geometry dependence of the correlation functions we find that the correlation function is nearly center-of-mass energy independent. The geometry dependence of the correlation function leads to an enhancement of near- and away-side correlations for the tip-on-tip U + U collisions when compared with side-on-side U + U collisions, an exactly opposite behavior from the correlations generated by the elliptic flow of the quark–gluon plasma

  3. Simultaneous determination of amino acids and carbohydrates in culture media of Clostridium thermocellum by valve-switching ion chromatography.

    Science.gov (United States)

    Fa, Yun; Yang, Haiyan; Ji, Chengshuai; Cui, He; Zhu, Xinshu; Du, Juan; Gao, Jun

    2013-10-10

    An improved method for the simultaneous determination of 20 amino acids and 7 carbohydrates using one-valve switching after injection, ion chromatography, and integrated pulsed amperometric detection is proposed. The resolution of the amino acids and carbohydrates in the cation trap column was investigated. In addition, parameters including flow liquid type, flow rate, concentration, and valve-switch timing were optimized. The method is time-saving, effective, and accurate for the simultaneous separation of amino acids and carbohydrates, with a mean correlation coefficient of >0.99 and repeatability of 0.5-4.6% for eight replicates. The method was successfully applied in the analysis of amino acids and carbohydrates in aseptic media and in extracellular culture media of three phenotypes of Clostridium thermocellum. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. 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

  5. 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

  6. Analysis of trace inorganic anions in weak acid salts by single pump cycling-column-switching ion chromatography.

    Science.gov (United States)

    Huang, Zhongping; Ni, Chengzhu; Zhu, Zhuyi; Pan, Zaifa; Wang, Lili; Zhu, Yan

    2015-05-01

    The application of ion chromatography with the single pump cycling-column-switching technique was described for the analysis of trace inorganic anions in weak acid salts within a single run. Due to the hydrogen ions provided by an anion suppressor electrolyzing water, weak acid anions could be transformed into weak acids, existing as molecules, after passing through the suppressor. Therefore, an anion suppressor and ion-exclusion column were adopted to achieve on-line matrix elimination of weak acid anions with high concentration for the analysis of trace inorganic anions in weak acid salts. A series of standard solutions consisting of target anions of various concentrations from 0.005 to 10 mg/L were analyzed, with correlation coefficients r ≥ 0.9990. The limits of detection were in the range of 0.67 to 1.51 μg/L, based on the signal-to-noise ratio of 3 and a 25 μL injection volume. Relative standard deviations for retention time, peak area, and peak height were all less than 2.01%. A spiking study was performed with satisfactory recoveries between 90.3 and 104.4% for all anions. The chromatographic system was successfully applied to the analysis of trace inorganic anions in five weak acid salts. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 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)

  8. Determination of vaporization enthalpies of polychlorinated biphenyls by correlation gas chromatography.

    Science.gov (United States)

    Puri, S; Chickos, J S; Welsh, W J

    2001-04-01

    The vaporization enthalpies of 16 polychlorinated biphenyls have been determined by correlation gas chromatography. This study was prompted by the realization that the vaporization enthalpy of the standard compounds used in previous studies, octadecane and eicosane, were values measured at 340 and 362 K, respectively, rather than at 298 K. Adjustment to 298 K amounts to a 7-8 kJ/mol increment in the values. With the inclusion of this adjustment, vaporization enthalpies evaluated by correlation gas chromatography are in good agreement with the values determined previously in the literature. The present results are based on the vaporization enthalpies of several standards whose values are well established in the literature. The standards include a variety of n-alkanes and various chlorinated hydrocarbons. The vaporization enthalpies of PCBs increased with the number of chlorine atoms and were found to be larger for meta- and para-substituted polychlorinated biphenyls.

  9. 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.

  10. 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)

  11. 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...

  12. 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.

  13. 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

  14. The assessment of pellicular anion-exchange resins for the determination of anions by ion chromatography

    International Nuclear Information System (INIS)

    Pohlandt, C.

    1981-01-01

    Because pellicular anion-exchange resins suitable for the determination, by ion chromatography, of anions with alkaline eluents were unavailable in South Africa at the inception of this work, an attempt was made to prepare such resins. In this study it is shown that the pellicular resins produced are more efficient than the surface-aminated resins used previously. The simultaneous separation and determination of five common anions is demonstrated. The method was applied to the analysis of uranium leach liquors, effluent samples, and a solid sample of ferric oxide (goethite)

  15. 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

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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.

  1. Validating a High Performance Liquid Chromatography-Ion Chromatography (HPLC-IC) Method with Conductivity Detection After Chemical Suppression for Water Fluoride Estimation.

    Science.gov (United States)

    Bondu, Joseph Dian; Selvakumar, R; Fleming, Jude Joseph

    2018-01-01

    A variety of methods, including the Ion Selective Electrode (ISE), have been used for estimation of fluoride levels in drinking water. But as these methods suffer many drawbacks, the newer method of IC has replaced many of these methods. The study aimed at (1) validating IC for estimation of fluoride levels in drinking water and (2) to assess drinking water fluoride levels of villages in and around Vellore district using IC. Forty nine paired drinking water samples were measured using ISE and IC method (Metrohm). Water samples from 165 randomly selected villages in and around Vellore district were collected for fluoride estimation over 1 year. Standardization of IC method showed good within run precision, linearity and coefficient of variance with correlation coefficient R 2  = 0.998. The limit of detection was 0.027 ppm and limit of quantification was 0.083 ppm. Among 165 villages, 46.1% of the villages recorded water fluoride levels >1.00 ppm from which 19.4% had levels ranging from 1 to 1.5 ppm, 10.9% had recorded levels 1.5-2 ppm and about 12.7% had levels of 2.0-3.0 ppm. Three percent of villages had more than 3.0 ppm fluoride in the water tested. Most (44.42%) of these villages belonged to Jolarpet taluk with moderate to high (0.86-3.56 ppm) water fluoride levels. Ion Chromatography method has been validated and is therefore a reliable method in assessment of fluoride levels in the drinking water. While the residents of Jolarpet taluk (Vellore distict) are found to be at a high risk of developing dental and skeletal fluorosis.

  2. Complexation ion-exchange chromatography of some metal ions on papers impregnated with Ti(IV)-based inorganic ion exchangers.

    Science.gov (United States)

    Sharma, S D; Gupta, R

    2000-02-01

    The chromatographic behavior of 40 metal ions is studied on titanium (IV) arsenate, titanium (IV) phosphate-, titanium (IV) molybdate-, titanium(IV) tungstate-, and titanium(IV) selenite-impregnated papers in 0.1M oxalic, citric, and tartaric acid as mobile phases. Similar studies are carried out on Whatman No. 1 papers for comparison. The ion-exchange capacity of these papers is determined, and their selectivity for different cations is discussed. The mechanism of migration is explained in terms of ion-exchange, precipitation, and adsorption. The prediction of elution sequence from RF values is also checked. The average Ri is found to be almost linearly dependent on the charge of the metal ions. The effect of the pKa of complexing acids on average RF values of 3d series metal ions is explained. A number of binary and ternary separations are achieved.

  3. 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...

  4. 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)

  5. 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.

  6. 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.

  7. Application of retention modelling to the simulation of separation of organic anions in suppressed ion chromatography.

    Science.gov (United States)

    Zakaria, Philip; Dicinoski, Greg W; Ng, Boon Khing; Shellie, Robert A; Hanna-Brown, Melissa; Haddad, Paul R

    2009-09-18

    The ion-exchange separation of organic anions of varying molecular mass has been demonstrated using ion chromatography with isocratic, gradient and multi-step eluent profiles on commercially available columns with UV detection. A retention model derived previously for inorganic ions and based solely on electrostatic interactions between the analytes and the stationary phase was applied. This model was found to accurately describe the observed elution of all the anions under isocratic, gradient and multi-step eluent conditions. Hydrophobic interactions, although likely to be present to varying degrees, did not limit the applicability of the ion-exchange retention model. Various instrumental configurations were investigated to overcome problems associated with the use of organic modifiers in the eluent which caused compatibility issues with the electrolytically derived, and subsequently suppressed, eluent. The preferred configuration allowed the organic modifier stream to bypass the eluent generator, followed by subsequent mixing before entering the injection valve and column. Accurate elution prediction was achieved even when using 5-step eluent profiles with errors in retention time generally being less than 1% relative standard deviation (RSD) and all being less than 5% RSD. Peak widths for linear gradient separations were also modelled and showed good agreement with experimentally determined values.

  8. Development of complexation ion chromatography for the determination of metal ions

    OpenAIRE

    Bashir, Wasim

    2002-01-01

    A simple ion chromatographic method was developed for the determination of Pb(II) in river and polluted water samples. The method was based upon the use of a colourforming complexing eluent and direct visible detection of the eluting Pb(II) complex. Using the combination of a strong cation exchange column and an eluent consisting of 20 mM sodium acetate-acetic acid buffer and 0.2 mM xylenol orange (XO) (~pH = 4.2), Pb(II) was detected at 572 nm eluting in under 6.5 min. The developed method p...

  9. Angular correlations and fragmentation in intermediate energy heavy ion collisions

    International Nuclear Information System (INIS)

    Kristiansson, Anders.

    1990-05-01

    Intermediate energy heavy-ion collisions have been studied from 35 A MeV up to 94 A MeV at various accelerators. Angular correlations between light particles and detection of projectile- and target-fragments have been used to investigate the reaction mechanisms in this transition region between low- and high energy. An excess of correlations is observed in the particle-particle elastic scattering plane. This excess increases with particle mass and can be understood in terms of momentum conservation. The fragmentation measurements gives an indication that both energy and momentum transfer to the spectator volumes does occur. (author)

  10. Detection of trace fluoride in serum and urine by online membrane-based distillation coupled with ion chromatography.

    Science.gov (United States)

    Lou, Chaoyan; Guo, Dandan; Wang, Nani; Wu, Shuchao; Zhang, Peimin; Zhu, Yan

    2017-06-02

    An online membrane-based distillation (MBD) coupled with ion chromatography (IC) method was proposed for automatic detection of trace fluoride (F - ) in serum and urine samples. The system consisted of a sample vessel, a lab-made membrane module and an ion chromatograph. Hydrophobic polytetrafluoroethylene (PTFE) hollow fiber membrane was used in MBD which was directly performed in serum and urine samples to eliminate the matrix interferences and enrich fluoride, while enabling automation. The determination of fluoride in biological samples was carried out by IC with suppressed conductometric detection. The proposed method feasibly determined trace fluoride in serum and urine matrices with the optimized parameters, such as acid concentration, distillation temperature, and distillation time, etc. Fluoride exhibited satisfactory linearity in the range of 0.01-5.0mg/L with a correlation coefficient of 0.9992. The limit of detection (LOD, S/N=3) and limit of quantification (LOQ, S/N=10) were 0.78μg/L and 2.61μg/L, respectively. The relative standard deviations of peak area and peak height were all less than 5.15%. The developed method was validated for the determination of fluoride in serum and urine with good spiked recoveries ranging between 97.1-101.9%. This method also can be proposed as a suitable alternative for the analysis of fluoride in other complex biological samples. Copyright © 2017. Published by Elsevier B.V.

  11. 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)

  12. Feasibility of correlating separation of ternary mixtures of neutral analytes via thin layer chromatography with supercritical fluid chromatography in support of green flash separations.

    Science.gov (United States)

    Ashraf-Khorassani, M; Yan, Q; Akin, A; Riley, F; Aurigemma, C; Taylor, L T

    2015-10-30

    Method development for normal phase flash liquid chromatography traditionally employs preliminary screening using thin layer chromatography (TLC) with conventional solvents on bare silica. Extension to green flash chromatography via correlation of TLC migration results, with conventional polar/nonpolar liquid mixtures, and packed column supercritical fluid chromatography (SFC) retention times, via gradient elution on bare silica with a suite of carbon dioxide mobile phase modifiers, is reported. Feasibility of TLC/SFC correlation is individually described for eight ternary mixtures for a total of 24 neutral analytes. The experimental criteria for TLC/SFC correlation was assumed to be as follows: SFC/UV/MS retention (tR) increases among each of the three resolved mixture components; while, TLC migration (Rf) decreases among the same resolved mixture components. Successful correlation of TLC to SFC was observed for most of the polar organic solvents tested, with the best results observed via SFC on bare silica with methanol as the CO2 modifier and TLC on bare silica with a methanol/dichloromethane mixture. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. 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.

  14. 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)

  15. Recovery of infective virus particles in ion-exchange and hydrophobic interaction monolith chromatography is influenced by particle charge and total-to-infective particle ratio.

    Science.gov (United States)

    Sviben, Dora; Forcic, Dubravko; Ivancic-Jelecki, Jelena; Halassy, Beata; Brgles, Marija

    2017-06-01

    Viral particles are used in medical applications as vaccines or gene therapy vectors. In order to obtain product of high purity, potency and safety for medical use purification of virus particles is a prerequisite, and chromatography is gaining increased attention to meet this aim. Here, we report on the use of ion-exchange and hydrophobic interaction chromatography on monolithic columns for purification of mumps virus (MuV) and measles virus (MeV). Efficiency of the process was monitored by quantification of infective virus particles (by 50% cell culture infective dose assay) and total virus particles, and monitoring of their size (by Nanoparticle Tracking Analysis). Ion-exchange chromatography was shown to be inefficient for MuV and best results for MeV were obtained on QA column with recovery around 17%. Purification of MuV and MeV by hydrophobic interaction chromatography resulted in recoveries around 60%. Results showed that columns with small channels (d=1.4μm) are not suitable for MuV and MeV, although their size is below 400nm, whereas columns with large channels (6μm) showed to be efficient and recoveries independent on the flow rate up to 10mL/min. Heterogeneity of the virus suspension and its interday variability mostly regarding total-to-infective particle ratio was observed. Interestingly, a trend in recovery depending on the day of the harvest was also observed for both viruses, and it correlated with the total-to-infective particle ratio, indicating influence of the virus sample composition on the chromatography results. Copyright © 2017. Published by Elsevier B.V.

  16. Improved separation of conjugated fatty acid methyl esters by silver ion-high-performance liquid chromatography.

    Science.gov (United States)

    Sehat, N; Rickert, R; Mossoba, M M; Kramer, J K; Yurawecz, M P; Roach, J A; Adlof, R O; Morehouse, K M; Fritsche, J; Eulitz, K D; Steinhart, H; Ku, Y

    1999-04-01

    Operating from one to six silver ion-high-performance liquid chromatography (Ag+-HPLC) columns in series progressively improved the resolution of the methyl esters of conjugated linoleic acid (CLA) isomeric mixtures from natural and commercial products. In natural products, the 8 trans, 10 cis-octadecadienoic (18:2) acid was resolved from the more abundant 7 trans, 9 cis-18:2, and the 10 trans, 12 cis-18:2 was separated from the major 9 cis, 11 trans-18:2 peak. In addition, both 11 trans, 13 cis-18:2 and 11 cis, 13 trans-18:2 isomers were found in natural products and were separated; the presence of the latter, 11 cis, 13 trans-18:2, was established in commercial CLA preparations. Three Ag+-HPLC columns in series appeared to be the best compromise to obtain satisfactory resolution of most CLA isomers found in natural products. A single Ag+-HPLC column in series with one of several normal-phase columns did not improve the resolution of CLA isomers as compared to that of the former alone. The 20:2 conjugated fatty acid isomers 11 cis, 13 trans-20:2 and 12 trans, 14 cis-20:2, which were synthesized by alkali isomerization from 11 cis, 14 cis-20:2, eluted in the same region of the Ag+-HPLC chromatogram just before the corresponding geometric CLA isomers. Therefore, CLA isomers will require isolation based on chain length prior to Ag+-HPLC separation. The positions of conjugated double bonds in 20:2 and 18:2 isomers were established by gas chromatography-electron ionization mass spectrometry as their 4,4-dimethyloxazoline derivatives. The double-bond geometry was determined by gas chromatography-direct deposition-Fourier transform infrared spectroscopy and by the Ag+-HPLC relative elution order.

  17. 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)

  18. Uncovering biologically significant lipid isomers with liquid chromatography, ion mobility spectrometry and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kyle, Jennifer E.; Zhang, Xing; Weitz, Karl K.; Monroe, Matthew E.; Ibrahim, Yehia M.; Moore, Ronald J.; Cha, Jeeyeon; Sun, Xiaofei; Lovelace, Erica S.; Wagoner, Jessica; Polyak, Steve; Metz, Thomas O.; Dey, Sudhansu K.; Smith, Richard D.; Burnum-Johnson, Kristin E.; Baker, Erin Shammel

    2016-01-01

    Understanding how biological molecules are generated, metabolized and eliminated in living systems is important for interpreting processes such as immune response and disease pathology. While genomic and proteomic studies have provided vast amounts of information over the last several decades, interest in lipidomics has also grown due to improved analytical technologies revealing altered lipid metabolism in type 2 diabetes, cancer, and lipid storage disease. Liquid chromatography and mass spectrometry (LC-MS) measurements are currently the dominant approach for characterizing the lipidome by providing detailed information on the spatial and temporal composition of lipids. However, interpreting lipids’ biological roles is challenging due to the existence of numerous structural and stereoisomers (i.e. distinct acyl chain and double-bond positions), which are unresolvable using present LC-MS approaches. Here we show that combining structurally-based ion mobility spectrometry (IMS) with LC-MS measurements distinguishes lipid isomers and allows insight into biological and disease processes.

  19. 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.

  20. 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.

  1. Recovery of 201Tl by ion exchange chromatography from proton bombarded thallium cyclotron targets

    International Nuclear Information System (INIS)

    Walt, T.N. van der; Naidoo, C.

    2000-01-01

    A method based on ion exchange chromatography is presented for the recovery of 201 Tl and its precursor 201 Pb from proton bombarded natural thallium cyclotron targets. After bombardment the target is dissolved in diluted nitric acid. Water, hydrazine and ammonium acetate are added to the solution and the lead radioisotopes separated from the thallium by cation exchange chromatography on a Bio-Rex 70 column. The sorbed lead radioisotopes are eluted with dilute nitric acid and the separation repeated on a second Bio-Rex 70 column. After elution of the remaining thallium the column is left for 32 hours and the 201 Tl formed by decay of 201 Pb is eluted with an ammonium acetate solution. The 201 Tl eluate is acidified with a HNO 3 -HBr-Br 2 mixture and the resulting solution is passed through an AG MP-1 anion exchanger column to remove any remaining lead isotopes. The 201 Tl is eluted with a hydrazine solution, the eluate evaporated to dryness and the 201 Tl finally dissolved in an appropriate solution to produce a 201 TlCl solution suitable for medical use. A high quality 201 Tl product is obtained containing ≤ 0.1 μg of Tl/mCi (37 MBq) 201 Tl. The radionuclidic impurities are less than the maximum values specified by the US Pharmacopoeia and the British Pharmacopoeia. (orig.)

  2. Fractionation of equine antivenom using caprylic acid precipitation in combination with cationic ion-exchange chromatography.

    Science.gov (United States)

    Raweerith, Rutai; Ratanabanangkoon, Kavi

    2003-11-01

    A combined process of caprylic acid (CA) precipitation and ion-exchange chromatography on SP-Sepharose was studied as a means to fractionate pepsin-digested horse antivenom F(ab')(2) antibody. In the CA precipitation, the optimal concentration for fractionation of F(ab')(2) from pepsin-digested horse plasma was 2%, in which 89.61% of F(ab')(2) antibody activity was recovered in the supernatant with 1.5-fold purification. A significant amount of pepsin was not precipitated and remained active under these conditions. An analytical cation exchanger Protein-Pak SP 8HR HPLC column was tested to establish optimal conditions for the effective separation of IgG, albumin, pepsin and CA from the F(ab')(2) product. From these results, the supernatant from CA precipitation of pepsin-digested plasma was subjected to a SP-Sepharose column chromatography using a linear salt gradient. With stepwise elution, a peak containing F(ab')(2) antibody could be obtained by elution with 0.25 M NaCl. The total recovery of antibody was 65.56% with 2.91-fold purification, which was higher than that achieved by ammonium sulfate precipitation. This process simultaneously and effectively removed residual pepsin, high molecular weight aggregates and CA in the final F(ab')(2) product, and should be suitable for large-scale fractionation of therapeutic equine antivenoms.

  3. 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.

  4. Correlated charge-changing ion-atom collisions

    International Nuclear Information System (INIS)

    Tanis, J.A.

    1992-04-01

    This report summarizes the progress and accomplishments in accelerator atomic physics research supported by DOE grant DE-FG02-87ER13778 from March 16, 1991 through March 15, 1992. This work involves the experimental investigation of fundamental atomic processes in collisions of charged projectiles with neutral targets or electrons, with particular emphasis on two-electron interactions and electron correlation effects. Processes involving combinations of excitation, ionization, and charge transfer are investigated utilizing coincidence techniques in which projectiles charge-changing events are associated with x-ray emission, target recoil ions, or electron emission. New results have been obtained for studies involving (1) resonant recombination of atomic ions, (2) double ionization of helium, and (3) continuum electron emission. Experiments were conducted using accelerators at the Lawrence Berkeley Laboratory, Argonne National Laboratory, Michigan State University, Western Michigan University, and the Institute of Nuclear Research, Debrecen, Hungary. Brief summaries of work completed and work in progress are given in this report

  5. 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.

  6. Separation profiles of Sr from irradiated Yttrium matrix using different eluants by ion-exchange chromatography

    International Nuclear Information System (INIS)

    Ashok Kumar, G.V.S.; Vithya, J.; Kumar, R.; VenkataSubramani, C.R.

    2014-01-01

    89 Sr (a pure β - emitter, T 1/2 = 50.5d) is used in palliative care of bone metastases and was produced using the 89 Y(n,p) 89 Sr reaction in Fast Breeder Test Reactor (FBTR), Kalpakkam. The irradiated yttria target was dissolved in nitric acid and bulk separation of yttrium carried out by solvent extraction using TBP-HNO 3 followed by ion exchange chromatography of the aqueous phase with nitric acid as an eluting agent to obtain the pure fraction of 89 Sr. This paper discusses about the feasibility of separation of 89 Sr with other eluting agents in ion exchange chromatography vis-a-vis nitric acid. As this nuclide is injected as the chloride, the purified fraction of Sr in nitric acid medium is finally converted into HCI medium which is the preferred medium of source for its final application. In order to simplify the conversion, HCI medium can be used directly in the purifying stage making the process faster and simpler. Hence the separation profile using HCI was obtained. In addition, the elution pattern using another reagent tri sodium tri meta phosphate (SMP) was also determined. Purification of 89 Sr fraction using the eluants HCI and SMP was established. However, the elution with SMP yielded the 89 Sr fraction in a small volume and shorter period i.e. ∼ 9 h in comparison with 15 h and 22 h in the case of HCI and HNO 3 medium respectively and also generated less liquid waste. This study established that SMP can be a more favoured elution agent for the purification of 89 Sr source during the chemical processing of the bulk irradiated yttria target material. However the direct separation of Sr using the Sr selective crown ether i.e.ditert.butyl dicyclohexano 18 Crown 6, is much preferred over this method which is in progress

  7. Enthalpy of vaporization and vapor pressure of whiskey lactone and menthalactone by correlation gas chromatography

    International Nuclear Information System (INIS)

    Simmons, Daniel; Chickos, James

    2017-01-01

    Highlights: • The vapor pressure and vaporization enthalpies of cis and trans-whiskey lactone have been evaluated. • Enthalpies of vaporization and vapor pressures of (+)-isomintlactone and (−)-mintlactone were also evaluated. • The sublimation enthalpy and corresponding vapor pressure of (+) -isomintlactone at T = 298.15 K is estimated. - Abstract: Enthalpies of vaporization at T = 298.15 K of cis and trans-whiskey lactone have been evaluated by correlation gas chromatography to be (68.4 ± 1.7) kJ·mol −1 and (67.5 ± 1.7) kJ·mol −1 , respectively. The enthalpies of vaporization of isomintlactone and mintlactone also evaluated by correlation gas chromatography have been found to have vaporization enthalpies of (74.2 ± 1.8) kJ·mol −1 and (73.2 ± 1.8) kJ·mol −1 respectively. The vapor pressures for cis and trans-whiskey lactone at T = 298.15 K have been evaluated as (1.5 ± 0.09) Pa and (2.0 ± 0.1) Pa using vapor pressures of a series of lactones as standards. Vapor pressures for isomintlactone and mintlactone were evaluated as (0.26 ± 0.012) Pa and (0.33 ± 0.02) Pa, respectively. Fusion and sublimation enthalpies for (+)-isomintlactone as well as the vapor pressure of the solid have been estimated.

  8. Determination of parabens in serum by liquid chromatography-tandem mass spectrometry: Correlation with lipstick use.

    Science.gov (United States)

    Tahan, Gabriella Padovani; Santos, Nayara de Kássia Souza; Albuquerque, Ana Carolina; Martins, Isarita

    2016-08-01

    Parabens are the most widely used preservative and are considered to be relatively safe compounds. However, studies have demonstrated that they may have estrogenic activity, and there is ongoing debate regarding the safety and potential cancer risk of using products containing these compounds. In the present work, liquid chromatography-tandem mass spectrometry was applied to determine methylparaben and propylparaben concentrations in serum, and the results were correlated with lipstick application. Samples were analyzed using liquid-liquid extraction, followed by liquid chromatography-tandem mass spectrometry. The validation results demonstrated the linearity of the method over a range of 1-20 ng/mL, in addition to the method's precision and accuracy. A statistically significant difference was demonstrated between serum parabens in women who used lipstick containing these substances compared with those not using this cosmetic (p = 0.0005 and 0.0016, respectively), and a strong association was observed between serum parabens and lipstick use (Spearman correlation = 0.7202). Copyright © 2016 Elsevier Inc. All rights reserved.

  9. 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...

  10. 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)

  11. 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

  12. Correlations of neutral pions in ultrarelativistic heavy ion collisions

    International Nuclear Information System (INIS)

    Peitzmann, T.; Beckmann, P.; Berger, F.; Glewing, G.; Dragon, L.; Glasow, R.; Kampert, K.H.; Loehner, H.; Purschke, M.; Santo, R.; Albrecht, R.; Bock, R.; Claesson, G.; Gutbrod, H.H.; Kolb, B.W.; Lund, I.; Schmidt, H.R.; Siemiarczuk, T.; Awes, T.C.; Baktash, C.; Ferguson, R.L.; Lee, I.Y.; Obenshain, F.E.; Plasil, F.; Soerensen, S.P.; Young, G.R.; Eklund, A.; Garpman, S.; Gustafsson, H.A.; Idh, J.; Kristiansson, P.; Oskarsson, A.; Otterlund, I.; Persson, S.; Stenlund, E.; Franz, A.; Poskanzer, A.M.; Ritter, H.G.

    1989-01-01

    Correlations of 4 photons representing neutral pions have been studied in ultrarelativistic heavy ion collisions. Data were taken in the WA80 experiment at the CERN-SPS with a 200 A GeV oxygen beam. The π 0 are detected via their decay photons with a high-granularity lead glass array. Special features of interferometry using neutral pions will be discussed. The extracted preliminary parameters for high p T pions emitted near midrapidity in O+Au collisions lead to rather small effective source sizes. (orig.)

  13. Improved purification process of β- and α-trypsin isoforms by ion-exchange chromatography

    Directory of Open Access Journals (Sweden)

    Alexandre Martins Costa Santos

    2008-08-01

    Full Text Available The purpose of this work was to improve the separation and yield of pure β- and α-trypsin isoforms by ion-exchange chromatography and to characterize some physical-chemical properties of these isoforms. Purification of trypsin isoforms was performed by ion-exchange chromatography in 0.1 mol/L tris-HC buffer, pH 7.10 at 4ºC. The sample loading, salt concentration, flow rate and pH of mobile phase were varied to determine their effects on the resolution of the separation. The resolution was optimized mainly between β- and α-trypsin. Pure isoforms were obtained by chromatographying 100 mg of commercial trypsin during seven days, yielding 51 mg of high purity β-trypsin and 13 mg of α-trypsin partially pure, with small amounts of contaminating of ψ-trypsin. Thus, time and resolution of purification were optimized yielding large amounts of pure active enzymes that are useful for several research areas and biotechnology.O propósito deste trabalho foi melhorar a separação e o rendimento das isoformas puras β- e α-tripsina por meio de cromatografia de troca iônica e caracterizar algumas propriedades físico-químicas dessas isoformas. A purificação de isoformas de tripsina foi realizada em SE Sephadex, com tampão tris-HCl, pH 7,10 a 4ºC. A quantidade de amostra, a concentração salina, o fluxo e o pH da fase móvel foram variados para determinar o efeito sobre a resolução da separação. A resolução foi otimizada principalmente entre β- e α-tripsina, utilizando o pH 7,10 a 4ºC. Isoformas puras foram obtidas a partir de 100 mg de tripsina comercial bovina depois de sete dias de cromatografia, fornecendo 51,0 mg de β-tripsina totalmente pura e 13,0 mg de α-tripsina parcialmente pura, com quantidades pequenas de contaminação por ψ-Tripsina. Assim, tempo e resolução da purificação foram otimizados redendo grandes quantidades de enzimas puras e ativas que são úteis em várias áreas de pesquisa e ciências biotecnológicas.

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

    Science.gov (United States)

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

    2015-07-01

    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 of both chloride and sodium in small volumes of sweat. Precision, linearity and limit of detection of an in-house developed IC/HPLC method were established. Method comparison between the newly developed IC/HPLC method and the traditional Chlorocounter was performed, and trueness was determined using Passing Bablok method comparison with external quality assurance material (Royal College of Pathologists of Australasia). Precision and linearity fulfill criteria as established by UK guidelines are comparable with inductively coupled plasma-mass spectrometry methods. Passing Bablok analysis demonstrated excellent correlation between IC/HPLC measurements and external quality assessment target values, for both chloride and sodium. With a limit of quantitation of 0.95 mmol/L, our method is suitable for the analysis of small amounts of sweat and can thus be used in combination with the Macroduct collection system. Although a chromatographic application results in a somewhat more expensive test compared to a Chlorocounter test, more accurate measurements are achieved. In addition, simultaneous measurements of sodium concentrations will result in better detection of false positives, less test repeating and thus faster and more accurate and effective diagnosis. The described IC/HPLC method, therefore, provides a precise, relatively cheap and easy-to-handle application for the analysis of both chloride and sodium in sweat. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

  15. QCD Jets and particle correlations in heavy-ion collisions

    CERN Document Server

    Nguyen, Matthew

    2017-01-01

    Measurements of jets and particle correlations in nucleus-nucleus collisions are intended to probe QCD interactions in the high temperature phase, where matter is understood to behave as a quark-gluon plasma. Two probes are reviewed: jets which are used to study the energy loss of hard-scattered partons in this medium and particle correlations which are used to understand collective effects of the bulk matter. Whereas collisions of lighter systems, namely proton-ion and proton-proton, initially served primarily as control experiments, certain (but not all) effects first observed in nucleus-nucleus collisions have proven to be pervasive in these systems. Comparative measurements in these three systems have broadened our understanding of many-body QCD phenomena, and raised new questions. This talk reviewed these recent developments.

  16. 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.

  17. 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.

  18. Continuous desalting of refolded protein solution improves capturing in ion exchange chromatography: A seamless process.

    Science.gov (United States)

    Walch, Nicole; Jungbauer, Alois

    2017-06-01

    Truly continuous biomanufacturing processes enable an uninterrupted feed stream throughout the whole production without the need for holding tanks. We have utilized microporous anion and cation exchangers into which only salts, but not proteins, can penetrate into the pores for desalting of protein solutions, while diafiltration or dilution is usually employed for feed adjustments. Anion exchange and cation exchange chromatography columns were connected in series to remove both anions and cations. To increase operation performance, a continuous process was developed comprised of four columns. Continuous mode was achieved by staggered cycle operation, where one set of columns, consisting of one anion exchange and one cation exchange column, was loaded during the regeneration of the second set. Refolding, desalting and subsequent ion exchange capturing with a scFv as the model protein was demonstrated. The refolding solution was successfully desalted resulting in a consistent conductivity below 0.5 mS/cm from initial values of 10 to 11 mS/cm. With continuous operation process time could be reduced by 39% while productivity was increased to 163% compared to batch operation. Desalting of the protein solution resulted in up to 7-fold higher binding capacities in the subsequent ion exchange capture step with conventional protein binding resins. © 2017 The Authors. Biotechnology Journal published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. The use of on-line ion chromatography for high temperature and high pressure reaction studies

    International Nuclear Information System (INIS)

    Lynch, G.J.

    1993-10-01

    This paper describes the use of on-line ion chromatography as a tool for chemistry reaction studies in small volume systems. The technique was used to study chemistry behavior in a high temperature and high pressure autoclave system. A dual analyzer, multi-channel on-line ion chromatograph (IC) was configured to automate the sampling and analysis. Analytical channels were set up for analysis of inorganic anions, monovalent cations, conductivity, and pH. Conductivity and pH were measured using the IC as a flow injection analyzer. Use of the IC system provides significant advantages over conventional sampling and analysis techniques: Reduction in sample volume, a closed sampling system that protects air or light sensitive analytes from breakdown, around-the-clock test performance combined with automatic calibration and quality control checking, and detection and tracking of reaction products or unexpected contaminants. Methods used to correct measured concentrations for the effects of sampling and for calculation of control chemical loss half-lives are presented. A limited evaluation of the flow injection analysis methods for conductivity and pH is provided

  20. 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)

  1. The ion-electron correlation function in liquid metals

    International Nuclear Information System (INIS)

    Takeda, S.; Tamaki, S.; Waseda, Y.

    1985-01-01

    The structure factors of liquid Zn at 723 K, Sn at 523 K and Bi at 573 K have been determined by neutron diffraction with sufficient accuracy and compared with those of X-ray diffraction. A remarkable difference in the structural information between the two methods is clearly found around the first peak region as well as in the slightly varied peak positions, and it is apparently larger than the experimental errors. With these facts in mind, a new method evaluating the ion-electron correlation function in liquid metals has been proposed by using the measured structural data of X-rays and neutrons, with the help of theoretical values of the electron-electron correlation function by he Utsumi-Ichimaru scheme. This method has been applied to liquid Zn, Sn and Bi, and the radial distribution function of valence electrons around an ion has been estimated, from which the ionic radius and the schematic diagram of the electron distribution map are obtained. The ionic radii evaluated in this work have been found to agree well with those proposed by Pauling. (author)

  2. 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.

  3. 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)

  4. Pion correlations in relativistic heavy ion collisions at Heavy Ion Spectrometer Systems (HISS)

    International Nuclear Information System (INIS)

    Christie, W.B. Jr.

    1990-05-01

    This thesis contains the setup, analysis and results of experiment E684H ''Multi-Pion Correlations in Relativistic Heavy Ion Collisions''. The goals of the original proposal were: (1) To initiate the use of the HISS facility in the study of central Relativistic Heavy Ion Collisions (RHIC). (2) To perform a second generation experiment for the detailed study of the pion source in RHIC. The first generation experiments, implied by the second goal above, refer to pion correlation studies which the Riverside group had performed at the LBL streamer chamber. The major advantage offered by moving the pion correlation studies to HISS is that, being an electronic detector system, as opposed to the Streamer Chamber which is a visual detector, one can greatly increase the statistics for a study of this sort. An additional advantage is that once one has written the necessary detector and physics analysis code to do a particular type of study, the study may be extended to investigate the systematics, with much less effort and in a relatively short time. This paper discusses the Physics motivation for this experiment, the experimental setup and detectors used, the pion correlation analysis, the results, and the conclusions possible future directions for pion studies at HISS. If one is not interested in all the details of the experiment, I believe that by reading the sections on intensity interferometry, the section the fitting of the correlation function and the systematic corrections applied, and the results section, one will get a fairly complete synopsis of the experiment

  5. Application of Liquid Chromatography/Ion Trap Mass Spectrometry Technique to Determine Ergot Alkaloids in Grain Products

    Directory of Open Access Journals (Sweden)

    Krystyna Szymczyk

    2015-01-01

    Full Text Available A liquid chromatography/ion trap mass spectrometry-based method to determine six ergot alkaloids and their isomers is presented. The samples were cleaned on neutral alumina-based solid-phase extraction cartridges. The following method parameters were obtained (depending on the analyte and spiking level: method recovery from 63.0 to 104.6 %, relative standard deviation below 18 %, linear range from 1 to 325 μg/kg, linear correlation coefficient not less than 0.98. The developed analytical procedure was applied to determine the levels of ergot alkaloids in 65 samples of selected rye-based food products (flour– 34 samples, bran – 12 samples, rye – 18 samples, flakes – 1 sample. Measurable levels of alkaloids were found in majority of the analysed samples, particularly in rye flour. Additionally, alkaloids were determined in ergot sclerotia isolated from rye grains. Total content was nearly 0.01 % (97.9 mg/kg. However, the alkaloid profi le was dominated by ergocristine at 45.6 % (44.7 mg/kg, an alkaloid not commonly found in the tested food products. Ergocorninine at 0.2 % (0.2 mg/kg was the least abundant alkaloid.

  6. Application of Liquid Chromatography/Ion Trap Mass Spectrometry Technique to Determine Ergot Alkaloids in Grain Products.

    Science.gov (United States)

    Bryła, Marcin; Szymczyk, Krystyna; Jędrzejczak, Renata; Roszko, Marek

    2015-03-01

    A liquid chromatography/ion trap mass spectrometry-based method to determine six ergot alkaloids and their isomers is presented. The samples were cleaned on neutral alumina-based solid-phase extraction cartridges. The following method parameters were obtained (depending on the analyte and spiking level): method recovery from 63.0 to 104.6%, relative standard deviation below 18%, linear range from 1 to 325 µg/kg, linear correlation coefficient not less than 0.98. The developed analytical procedure was applied to determine the levels of ergot alkaloids in 65 samples of selected rye-based food products (flour - 34 samples, bran - 12 samples, rye - 18 samples, flakes - 1 sample). Measurable levels of alkaloids were found in majority of the analysed samples, particularly in rye flour. Additionally, alkaloids were determined in ergot sclerotia isolated from rye grains. Total content was nearly 0.01% (97.9 mg/kg). However, the alkaloid profile was dominated by ergocristine at 45.6% (44.7 mg/kg), an alkaloid not commonly found in the tested food products. Ergocorninine at 0.2% (0.2 mg/kg) was the least abundant alkaloid.

  7. 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.

  8. Adsorption of endotoxins on Ca2+ -iminodiacetic acid by metal ion affinity chromatography.

    Science.gov (United States)

    Lopes, André Moreni; Romeu, Jorge Sánchez; Meireles, Rolando Páez; Perera, Gabriel Marquez; Morales, Rolando Perdomo; Pessoa, Adalberto; Cárdenas, Lourdes Zumalacárregui

    2012-11-01

    Endotoxins (also known as lipopolysaccharides (LPS)) are undesirable by-products of recombinant proteins, purified from Escherichia coli. LPS can be considered stable under a wide range of temperature and pH, making their removal one of the most difficult tasks in downstream processes during protein purification. The inherent toxicity of LPS makes their removal an important step for the application of these proteins in several biological assays and for a safe parenteral administration. Immobilized metal affinity chromatography (IMAC) enables the affinity interactions between the metal ions (immobilized on the support through the chelating compound) and the target molecules, thus enabling high-efficiency separation of the target molecules from other components present in a mixture. Affinity chromatography is applied with Ca2+ -iminodiacetic acid (IDA) to remove most of the LPS contaminants from the end product (more than 90%). In this study, the adsorption of LPS on an IDA-Ca2+ was investigated. The adsorption Freundlich isotherm of LPS-IDA-Ca2+ provides a theoretical basis for LPS removal. It was found that LPS is bound mainly by interactions between the phosphate group in LPS and Ca2+ ligands on the beads. The factors such as pH (4.0 or 5.5) and ionic strength (1.0 mol/L) are essential to obtain effective removal of LPS for contaminant levels between endotoxin' concentration values less than 100 EU/mL and 100 000 EU/mL. This new protocol represents a substantial advantage in time, effort, and production costs.

  9. 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

  10. Partial correlation analysis method in ultrarelativistic heavy-ion collisions

    Science.gov (United States)

    Olszewski, Adam; Broniowski, Wojciech

    2017-11-01

    We argue that statistical data analysis of two-particle longitudinal correlations in ultrarelativistic heavy-ion collisions may be efficiently carried out with the technique of partial covariance. In this method, the spurious event-by-event fluctuations due to imprecise centrality determination are eliminated via projecting out the component of the covariance influenced by the centrality fluctuations. We bring up the relationship of the partial covariance to the conditional covariance. Importantly, in the superposition approach, where hadrons are produced independently from a collection of sources, the framework allows us to impose centrality constraints on the number of sources rather than hadrons, that way unfolding of the trivial fluctuations from statistical hadronization and focusing better on the initial-state physics. We show, using simulated data from hydrodynamics followed with statistical hadronization, that the technique is practical and very simple to use, giving insight into the correlations generated in the initial stage. We also discuss the issues related to separation of the short- and long-range components of the correlation functions and show that in our example the short-range component from the resonance decays is largely reduced by considering pions of the same sign. We demonstrate the method explicitly on the cases where centrality is determined with a single central control bin or with two peripheral control bins.

  11. Two-pion correlations in heavy ion collisions

    International Nuclear Information System (INIS)

    Zajc, W.A.

    1982-08-01

    An application of intensity interferometry to relativistic heavy ion collisions is reported. Specifically, the correlation between two like-charged pions is used to study the reactions Ar+KCl→2π/sup +-/+X and Ne+NaF→2π - +X. Source sizes are obtained that are consistent with a simple geometric interpretation. Lifetimes are less well determined but are indicative of a faster pion production process than predicted by Monte Carlo cascade calculations. There appears to be a substantial coherent component of the pion source, although measurement is complicated by the presence of final state interactions. Additionally, the generation of spectra of uncorrelated events is discussed. In particular, the influence of the correlation function on the background spectrum is analyzed, and a prescription for removal of this influence is given. A formulation to describe the statistical errors in the background is also presented. Finally, drawing from the available literature, a self-contained introduction to Bose-Einstein correlations and the Hanbury-Brown - Twiss effect is provided, with an emphasis on points of contact between classical and quantum mechanical descriptions

  12. Ion specific correlations in bulk and at biointerfaces

    International Nuclear Information System (INIS)

    Kalcher, I; Horinek, D; Netz, R R; Dzubiella, J

    2009-01-01

    Ion specific effects are ubiquitous in any complex colloidal or biological fluid in bulk or at interfaces. The molecular origins of these 'Hofmeister effects' are not well understood and their theoretical description poses a formidable challenge to the modeling and simulation community. On the basis of the combination of atomistically resolved molecular dynamics (MD) computer simulations and statistical mechanics approaches, we present a few selected examples of specific electrolyte effects in bulk, at simple neutral and charged interfaces, and on a short α-helical peptide. The structural complexity in these strongly Coulomb-correlated systems is highlighted and analyzed in the light of available experimental data. While in general the comparison of MD simulations to experiments often lacks quantitative agreement, mostly because molecular force fields and coarse-graining procedures remain to be optimized, the consensus as regards trends provides important insights into microscopic hydration and binding mechanisms.

  13. Ion specific correlations in bulk and at biointerfaces.

    Science.gov (United States)

    Kalcher, I; Horinek, D; Netz, R R; Dzubiella, J

    2009-10-21

    Ion specific effects are ubiquitous in any complex colloidal or biological fluid in bulk or at interfaces. The molecular origins of these 'Hofmeister effects' are not well understood and their theoretical description poses a formidable challenge to the modeling and simulation community. On the basis of the combination of atomistically resolved molecular dynamics (MD) computer simulations and statistical mechanics approaches, we present a few selected examples of specific electrolyte effects in bulk, at simple neutral and charged interfaces, and on a short α-helical peptide. The structural complexity in these strongly Coulomb-correlated systems is highlighted and analyzed in the light of available experimental data. While in general the comparison of MD simulations to experiments often lacks quantitative agreement, mostly because molecular force fields and coarse-graining procedures remain to be optimized, the consensus as regards trends provides important insights into microscopic hydration and binding mechanisms.

  14. Separation of seven arsenic species by ion-pair and ion-exchange high performance liquid chromatography

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Hansen, Sven Hedegaard

    1992-01-01

    Arsenite, arsenate, monomethylarsonate, dimethylarsinate, arsenobetaine, arsenocholine and the tetramethylarsonium ion were subjected to ion-exchange and ion-pair reversed phase HPLC. The ion exchange method was superior in selectivity and time of analysis for the arsenic anions. The ammonium ions...... used for the ion-pair method only resulted in separation of some of the anionic arsenic compounds. Flame atomic absorption spectrometry was used for on-line arsenic-specific detection....

  15. Improvement on simultaneous determination of chromium species in aqueous solution by ion chromatography and chemiluminescence detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Liao, Y.P.; Jons, O.

    1997-01-01

    A sensitive method for the simultaneous determination of chromium(III) and chromium(VI) was chromatography and chemiluminescence detection. Two Dionex ion-exchange guard columns in series, CG5 and AG7, were used to separate chromium(III) from chromium(VI). Chromium(VI) was reduced by potassium......, the stabilities of reductant and luminol solutions were studied. The linear range of the calibration curve for chromium(III) and chromium(VI) was 1-400 mu g l(-1). The detection limit was 0.12 mu g l(-1) for chromium(III) and 0.09 mu g l(-1) for chromium(VI), respectively. The precision at the 20 mu g l(-1) level...... was 1.4% for chromium(III) and 2.5% for chromium(VI), respectively. The accuracy of the chromium(III) determination was determined by analysis of the NIST standard reference material 1643c, Trace elements in water with the result 19.1 +/- 1.0 mu g Cr(III) l(-1) (certified value 19.0 +/- 0.6 mu g Cr...

  16. Short communication: separation and quantification of caseins and casein macropeptide using ion-exchange chromatography.

    Science.gov (United States)

    Holland, B; Rahimi Yazdi, S; Ion Titapiccolo, G; Corredig, M

    2010-03-01

    The aim of this work was to improve an existing method to separate and quantify the 4 major caseins from milk samples (i.e., containing whey proteins) using ion-exchange chromatography. The separation process was carried out using a mini-preparative cation exchange column (1 or 5mL of column volume), using urea acetate as elution buffer at pH 3.5 with a NaCl gradient. All 4 major caseins were separated, and the purity of each peak was assessed using sodium dodecyl sulfate-PAGE. Purified casein fractions were also added to raw milk to confirm their elution volumes. The quantification was carried out using purified caseins in buffer as well as added directly to fresh skim milk. This method can also be employed to determine the decrease in kappa-casein and the release of the casein-macropeptide during enzymatic hydrolysis using rennet. In this case, the main advantage of using this method is the lack of organic solvents compared with the conventional method for separation of macropeptide (using reversed phase HPLC).

  17. Separation of 1,3-Propanediol from Aqueous Solutions by Ion Exchange Chromatography

    Directory of Open Access Journals (Sweden)

    Rukowicz Beata

    2014-06-01

    Full Text Available 1,3-propanediol is a promising monomer with many applications and can be produced by bioconversion of renewable resources. The separation of this product from fermentation broth is a difficult task. In this work, the application of cation exchange resin for the separation of 1,3-propanediol from model aqueous solution was examined. The best effect of separation of 1,3-propanediol from glycerol using sorption method was obtained for H+ resin form, although the observed partition coefficient of 1,3-propanediol was low. On the basis of the results of the sorption of 1,3-propanediol, the ionic forms of the resin were selected and used in the next experiments (H+, Ca2+, Ag+, Na+, Pb2+, Zn2+. The best results in ion exchange chromatography were obtained for cation exchange resin in H+ and Ca2+ form. The use of smaller particle size of resin and a longer length of the column allows to obtain better separation of mixtures.

  18. 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.

  19. Off-line coupling of multidimensional immunoaffinity chromatography and ion mobility spectrometry: A promising partnership.

    Science.gov (United States)

    Armenta, Sergio; de la Guardia, Miguel; Abad-Fuentes, Antonio; Abad-Somovilla, Antonio; Esteve-Turrillas, Francesc A

    2015-12-24

    The extreme specificity of immunoaffinity chromatography (IAC) columns coupled to the high sensitivity of ion mobility spectrometry (IMS) measurements makes this combination really useful for rapid, selective, and sensitive determination of a high variety of analytes in different samples. The capabilities of the IAC-IMS coupling have been highlighted under three different scenarios: (i) multiclass residue analysis using a single IAC column, (ii) multiclass residue analysis using stacked IAC columns, and (iii) isomer analysis. In the first case, the determination of three strobilurin fungicides - azoxystrobin, picoxystrobin, and pyraclostrobin - in water and strawberry juice was considered, obtaining limits of quantification (LOQs) from 11 to 63μgL(-1). Recoveries from 96 to 106% for water, and from 67 to 104% for strawberry juice were obtained. In the second case, anilinopyrimidine compounds, including two analytes with similar drift time, were selectively retained in different IAC columns and analyzed after independent elution in commercial wine samples by IMS. LOQ values of 16, 14 and 12μgL(-1) were obtained for pyrimethanil, mepanipyrim, and cyprodinil, respectively. The obtained recoveries for wine samples spiked with 25 and 100μgL(-1) were from 82 to 123%. Additionally, the stacked IAC columns concept was applied to the separation of Z and E isomers of azoxystrobin that were selectively retained in specific IAC columns and quantified by IMS. Recoveries between 91 and 94% were obtained for both isomers in water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Vapor pressures and vaporization enthalpy of codlemone by correlation gas chromatography

    International Nuclear Information System (INIS)

    Schultz, Shannon M.; Harris, Harold H.; Chickos, James S.

    2015-01-01

    Highlights: • The vaporization enthalpy of codlemone has been evaluated. • The vapor pressure of codlemone has been evaluated from T = (298.15 to T b ) K. • Vapor pressures for the 1-alkanols standards are available from T = (298.15 to 500) K. - Abstract: The vapor pressure and vaporization enthalpy of codlemone (trans, trans 8,10-dodecadien-1-ol), the female sex hormone of the codling moth is evaluated by correlation gas chromatography using a series of saturated primary alcohols as standards. A vaporization enthalpy of (92.3 ± 2.6) kJ · mol −1 and a vapor pressure, p/Pa = (0.083 ± 0.012) were evaluated at T = 298.15 K. An equation for the evaluation of vapor pressure from ambient temperature to boiling has been derived by correlation for codlemone. The calculated boiling temperature of T B = 389 K at p = 267 Pa is within the temperature range reported in the literature. A normal boiling temperature of T B = (549.1 ± 0.1) K is also estimated by extrapolation

  1. Capillary sieving electrophoresis and micellar electrokinetic capillary chromatography produce highly correlated separation of tryptic digests

    Science.gov (United States)

    Dickerson, Jane A.; Dovichi, Norman J.

    2011-01-01

    We perform two-dimensional capillary electrophoresis on fluorescently labeled proteins and peptides. Capillary sieving electrophoresis was performed in the first dimension and micellar electrokinetic capillary chromatography was performed in the second. A cellular homogenate was labeled with the fluorogenic reagent FQ and separated using the system. This homogenate generated a pair of ridges; the first had essentially constant migration time in the CSE dimension, while the second had essentially constant migration time in the MEKC dimension. In addition a few spots were scattered through the electropherogram. The same homogenate was digested using trypsin, and then labeled and subjected to the two dimensional separation. In this case, the two ridges observed from the original two-dimensional separation disappeared, and were replaced by a set of spots that fell along the diagonal. Those spots were identified using a local-maximum algorithm and each was fit using a two-dimensional Gaussian surface by an unsupervised nonlinear least squares regression algorithm. The migration times of the tryptic digest components were highly correlated (r = 0.862). When the slowest migrating components were eliminated from the analysis, the correlation coefficient improved to r = 0.956. PMID:20564272

  2. 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.

  3. Pion correlations in relativistic heavy ion collisions at Heavy Ion Spectrometer Systems (HISS)

    Energy Technology Data Exchange (ETDEWEB)

    Christie, W.B. Jr.

    1990-05-01

    This thesis contains the setup, analysis and results of experiment E684H Multi-Pion Correlations in Relativistic Heavy Ion Collisions''. The goals of the original proposal were: (1) To initiate the use of the HISS facility in the study of central Relativistic Heavy Ion Collisions (RHIC). (2) To perform a second generation experiment for the detailed study of the pion source in RHIC. The first generation experiments, implied by the second goal above, refer to pion correlation studies which the Riverside group had performed at the LBL streamer chamber. The major advantage offered by moving the pion correlation studies to HISS is that, being an electronic detector system, as opposed to the Streamer Chamber which is a visual detector, one can greatly increase the statistics for a study of this sort. An additional advantage is that once one has written the necessary detector and physics analysis code to do a particular type of study, the study may be extended to investigate the systematics, with much less effort and in a relatively short time. This paper discusses the Physics motivation for this experiment, the experimental setup and detectors used, the pion correlation analysis, the results, and the conclusions possible future directions for pion studies at HISS. If one is not interested in all the details of the experiment, I believe that by reading the sections on intensity interferometry, the section the fitting of the correlation function and the systematic corrections applied, and the results section, one will get a fairly complete synopsis of the experiment.

  4. 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)

  5. 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.

  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. A study of trapped ion dynamics by photon-correlation and pulse-probe techniques

    International Nuclear Information System (INIS)

    Rink, J.; Dholakia, K.; Zs, G.; Horvath, K.; Hernandez-Pozos, J. L.; Power, W.; Segal, D. M.; Thompson, R. C.; Walker, T.

    1995-01-01

    We demonstrate non-evasive methods for observing ion and ion cloud oscillation frequencies in a quadrupole ion trap. These trap resonances are measured for small clouds using a photon correlation technique. For large clouds the rotation frequency can be detected with the help of an additional pulsed probe laser. We show applications of the photon correlation method such as estimating the dynamic properties of a combined trap and detecting ion crystals

  8. Determination of anions in pure and commercial phosphoric acid by ion chromatography and manual of 792 basic IC

    International Nuclear Information System (INIS)

    Al-Kabani, F.; Abdulbaki, M. K.

    2007-01-01

    A method for determination of anions in pure and concentrated phosphoric and samples (85%) and commercial phosphoric acid ion chromatography was developed, in order to control the specification of phosphoric acid produced in the pilot plant for phosphoric acid purification. The accuracy of the method was studied and the standard deviation was found to be between 0.09 and 0.10. Operation instructions of 792 Basic IC was described. (author)

  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. 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.

  11. Evaluation and application of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry for complex sample analysis.

    Science.gov (United States)

    Denawaka, Chamila J; Fowlis, Ian A; Dean, John R

    2014-04-18

    An evaluation of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS) has been undertaken to assess its applicability for the determination of 32 volatile compounds (VCs). The key experimental variables of sample incubation time and temperature have been evaluated alongside the MCC-GC variables of column polarity, syringe temperature, injection temperature, injection volume, column temperature and carrier gas flow rate coupled with the IMS variables of temperature and drift gas flow rate. This evaluation resulted in six sets of experimental variables being required to separate the 32 VCs. The optimum experimental variables for SHS-MCC-GC-IMS, the retention time and drift time operating parameters were determined; to normalise the operating parameters, the relative drift time and normalised reduced ion mobility for each VC were determined. In addition, a full theoretical explanation is provided on the formation of the monomer, dimer and trimer of a VC. The optimum operating condition for each VC calibration data was obtained alongside limit of detection (LOD) and limit of quantitation (LOQ) values. Typical detection limits ranged from 0.1ng bis(methylthio)methane, ethylbutanoate and (E)-2-nonenal to 472ng isovaleric acid with correlation coefficient (R(2)) data ranging from 0.9793 (for the dimer of octanal) through to 0.9990 (for isobutyric acid). Finally, the developed protocols were applied to the analysis of malodour in sock samples. Initial work involved spiking an inert matrix and sock samples with appropriate concentrations of eight VCs. The average recovery from the inert matrix was 101±18% (n=8), while recoveries from the sock samples were lower, that is, 54±30% (n=8) for sock type 1 and 78±24% (n=6) for sock type 2. Finally, SHS-MCC-GC-IMS was applied to sock malodour in a field trial based on 11 volunteers (mixed gender) over a 3-week period. By applying the SHS-MCC-GC-IMS database, four VCs were

  12. 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)

  13. Retention behavior of flavonoids on immobilized artificial membrane chromatography and correlation with cell-based permeability.

    Science.gov (United States)

    Tsopelas, Fotios; Tsagkrasouli, Maria; Poursanidis, Pavlos; Pitsaki, Maria; Vasios, George; Danias, Panagiotis; Panderi, Irene; Tsantili-Kakoulidou, Anna; Giaginis, Constantinos

    2018-03-01

    The aim of the study was to investigate the immobilized artificial membrane (IAM) retention mechanism for a set of flavonoids and to evaluate the potential of IAM chromatography to model Caco-2 permeability. For this purpose, the retention behavior of 41 flavonoid analogs on two IAM stationary phases, IAM.PC.MG and IAM.PC.DD2, was investigated. Correlations between retention factors, logk w(IAM) and octanol-water partitioning (logP) were established and the role of hydroxyl groups of flavonoids to the underlying retention mechanism was explored. IAM retention and logP values were used to establish sound linear models with Caco-2 permeability (logP app ) taken from the literature. Both stepwise regression and multivariate analysis confirmed the contribution of hydrogen bond descriptors, as additional parameters in the either logk w(IAM) or logP models. Retention factors on both IAM stationary phases showed comparable performance with n-octanol-water partitioning towards Caco-2 permeability. Copyright © 2017 John Wiley & Sons, Ltd.

  14. Vapor pressure and enthalpy of vaporization of oil of catnip by correlation gas chromatography

    International Nuclear Information System (INIS)

    Simmons, Daniel; Gobble, Chase; Chickos, James

    2016-01-01

    Highlights: • Vaporization enthalpies of the nepetalactones from oil of catnip have been evaluated. • Vapor pressures from T = (298.15 to 350) K have been evaluated. • Oil of catnip has a vapor pressure similar to DEET at T = 298.15 K. - Abstract: The vaporization enthalpy and vapor pressure of the two nepetalactones found in Nepeta cataria have been evaluated by correlation gas chromatography. Vaporization enthalpies at T = 298.15 K of {(68.0 ± 1.9) and (69.4 ± 1.9)} kJ ⋅ mol"−"1 have been derived for the minor diastereomer, (4aS,7S,7aS)-nepetalactone, and major one, (4aS,7S,7aR)-nepetalactone, respectively. Vapor pressures also at T = 298.15 K of p = (1.2 ± 0.04) Pa and (0.91 ± 0.03) Pa have been evaluated for the minor and the major stereoisomer. In addition to being of interest because of the remarkable effect it has on various felids, oil of catnip is also quite effective in repelling mosquitoes, comparable to diethyl-m-toluamide (DEET). The vapor pressures evaluated in this work suggest that the two stereoisomers have similar volatility to DEET at ambient temperatures.

  15. How decays and final-state interactions affect velocity correlations in heavy-ion collisions

    International Nuclear Information System (INIS)

    Wieand, K.L.; Pratt, S.E.; Balantekin, A.B.

    1992-01-01

    We study rapidity correlations by calculating two-particle correlation functions and fractorial moments for a simple thermal model of ultrarelativistic-heavy-ion collisions. In this model correlations arise from decays of unstable hadrons and the final-state interactions of the measured particles. These correlations are shown to be similar but smaller than correlations due to phase separation. (orig.)

  16. 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.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

    Full text: The palladium and platinum are widely used for jewel manufacture because of their beautiful white color. However the most part of these metals are widely adopted in the world as catalysts. Many works on analytical chemistry of platinum group elements published during last years are devoted to determination of platinum and palladium in other materials. There are no articles on analysis technique of the palladium and platinum purity published during last 20 years. Available publications are very old and are published till 70th of the last century, and implement chemical and spectral methods. At the same time, the palladium and platinum are very suitable for NAA. Therefore the purpose of our research was development of high-sensitivity and multielement techniques of radiochemical neutron activation analysis of a high pure palladium and platinum. Research of nuclear characteristics of palladium and platinum has shown that radioactive nuclides with different yields are formed under the reactor neutrons. 109 , 111 , 111m Pd, 109m , 111 Ag, 191 , 197 , 199 Pt, 199 Au are the most important among them. 109Pd separation factor is equal to 1*10 5 at palladium analysis, whereas 197 Pt and 199 Au separation factor is equal to 1*10 4 at the platinum analysis every other day after irradiation. Palladium and platinum can be separated by precipitation, extraction and ion exchange methods. For separation of radioactive nuclide of the matrix elements from the impurity elements we used ion exchange chromatography system Dowex-1x8 - 1 M HNO 3 for palladium and Dowex-1x8 - 0.1 M HNO 3 for platinum. At the HNO 3 acid concentrations variation from 0,1 M to 1 M more then 25 elements have distribution factors less than 1 and 10 elements have distribution factors 5 while matrix elements have distribution factors higher than 100. It allows an effective separation of these elements from palladium and platinum. Optimum sizes of the chromatographic column and the column effluent

  18. Speciation analysis of arsenic compounds in seafood by ion chromatography-atomic fluorescence spectrometry

    Science.gov (United States)

    Han, Tingting; Ji, Hongwei; Li, Huixin; Cui, He; Song, Tian; Duan, Xiaojuan; Zhu, Qianlin; Cai, Feng; Zhang, Li

    2017-06-01

    Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine (AsB), arsenite (As(III)), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), and arsenate (As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L-1 CH3COONH4 and 15 mmol L-1 Na2CO3 with 10 mL CH3CH2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%-109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L-1 for AsB, 0.426 μg L-1 for As(III), 0.216 μg L-1 for DMA, 0.211 μg L-1 for MMA, and 0.709 μg L-1 for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.

  19. Methods for separating boron from borated paraffin wax and its determination by ion chromatography

    International Nuclear Information System (INIS)

    Jeyakumar, S.

    2015-01-01

    Boron compounds are found to be useful in shielding against high-energy neutrons. In radiotherapy treatments, in order to protect occupational workers and patients from the undesirable neutron and gamma doses, paraffin wax containing B 4 C/boric acid is used. Low-level borate wastes generated from the nuclear power plants have been immobilized with paraffin wax using a concentrate waste drying system (CWDS). Borated paraffin waxes are prepared by mixing calculated amounts of either boric acid or boron carbide with the molten wax. This necessitates the determination of boron at different locations in order to check the homogeneous distribution of B over the borated wax. The determination of boron in nuclear materials is inevitable due to its high neutron absorption cross section. For the determination of boron in borated waxes, not many methods have been reported. A method based on the pyrohydrolysis extraction of boron and its quantification with ion chromatography was proposed for paraffin waxes borated with H 3 BO 3 and B 4 C. The B 4 C optimum pyrohydrolysis conditions were identified. Wax samples were mixed with U 3 O 8 , which prevents the sample from flare up, and also accelerates the extraction of boron. Pyrohydrolysis was carried out with moist O 2 at 950℃ for 60 and 90 min for wax with H 3 BO 3 and wax with B 4 C, respectively. Two simple methods of separation based on alkali extraction and melting wax in alkali were also developed exclusively for wax with H 3 BO 3 . In all the separations, the recovery of B was above 98%. During IC separation, B was separated as boron-mannitol anion complex. Linear calibration was obtained between 0.1 and 50 ppm of B, and LOD was calculated as 5 ppb (S/N=3). The reproducibility was better than 5% (RSD)

  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. 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.

  2. 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.

  3. Simultaneous determination of inorganic anions and cations in explosive residues by ion chromatography.

    Science.gov (United States)

    Meng, Hong-Bo; Wang, Tian-Ran; Guo, Bao-Yuan; Hashi, Yuki; Guo, Can-Xiong; Lin, Jin-Ming

    2008-07-15

    A non-suppressed ion chromatographic method by connecting anion-exchange and cation-exchange columns directly was developed for the separation and determination of five inorganic anions (sulfate, nitrate, chloride, nitrite, and chlorate) and three cations (sodium, ammonium, and potassium) simultaneously in explosive residues. The mobile phase was composed of 3.5mM phthalic acid with 2% acetonitrile and water at flow rate of 0.2 mL/min. Under the optimal conditions, the eight inorganic ions were completely separated and detected simultaneously within 16 min. The limits of detection (S/N=3) of the anions and cations were in the range of 50-100 microg/L and 150-320 microg/L, respectively, the linear correlation coefficients were 0.9941-0.9996, and the R.S.D. of retention time and peak area were 0.10-0.29% and 5.65-8.12%, respectively. The method was applied successfully to the analysis of the explosive samples with satisfactory results.

  4. 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.

  5. 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

  6. 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.

  7. Chromatographic retention prediction and octanol-water partition coefficient determination of monobasic weak acidic compounds in ion-suppression reversed-phase liquid chromatography using acids as ion-suppressors.

    Science.gov (United States)

    Ming, Xin; Han, Shu-ying; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

    2009-08-15

    Although simple acids, replacing buffers, have been widely applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography (RPLC), none of the previously reported works focused on the systematic studies about the retention behavior of the acidic solutes in this ion-suppression RPLC mode. The subject of this paper was therefore to investigate the retention behavior of monobasic weak acidic compounds using acetic, perchloric and phosphoric acids as the ion-suppressors. The apparent octanol-water partition coefficient (K" ow) was proposed to calibrate the octanol-water partition coefficient (K(ow)) of these weak acidic compounds, which resulted in a better linear correlation with log k(w), the logarithm of the hypothetical retention factor corresponding to neat aqueous fraction of hydroorganic mobile phase. This log K" ow-log k w linear correlation was successfully validated by the results of monocarboxylic acids and monohydrating phenols, and moreover by the results under diverse experimental conditions for the same solutes. This straightforward relationship not only can be used to effectively predict the retention values of weak acidic solutes combined with Snyder-Soczewinski equation, but also can offer a promising medium for directly measuring K(ow) data of these compounds via Collander equation. In addition, the influence of the different ion-suppressors on the retention of weak acidic compounds was also compared in this RPLC mode.

  8. Seasonal Variations and Correlation Analysis of Water-Soluble Inorganic Ions in PM2.5 in Wuhan, 2013

    Directory of Open Access Journals (Sweden)

    Ting Huang

    2016-03-01

    Full Text Available Daily PM2.5 and water-soluble inorganic ions (NH4+, SO42−, NO3−, Cl−, Ca2+, Na+, K+, Mg2+ were collected at the Hongshan Air Monitoring Station at the China University of Geosciences (Wuhan (30°31′N, 114°23′E, Wuhan, from 1 January to 30 December 2013. A total of 52 effective PM2.5 samples were collected using medium flow membrane filter samplers, and the anionic and cationic ions were determined by ion chromatography and ICP, respectively. The results showed that the average mass concentration of the eight ions was 40.96 µg/m3, which accounted for 62% of the entire mass concentration. In addition, the order of the ion concentrations was SO42− > NO3− > NH4+ > Cl− >K+ > Ca2+ > Na+ > Mg2+. The secondary inorganic species SO42−, NO3− and NH4+ were the major components of water-soluble ions in PM2.5, with a concentration of 92% of the total ions of PM2.5, and the total concentrations of the three ions in the four seasons in descending order as follows: winter, spring, autumn, and summer. NH4+ had a significant correlation with SO42− and NO3−, and the highest correlation coefficients were 0.943 and 0.923 (in winter, while the minimum coefficients were 0.683 and 0.610 (in summer. The main particles were (NH42SO4 and NH4NO3 in PM2.5. The charge of the water-soluble ions was nearly balanced in PM2.5, and the pertinence coefficients of water-soluble anions and cations were more than 0.9. The highest pertinence coefficients were in the spring (0.9887, and the minimum was in summer (0.9459. That is, there were more complicated ions in PM2.5 in the summer. The mean value of NO3−/SO42− was 0.64, indicating that stationary sources of PM2.5 had a greater contribution in Wuhan.

  9. [Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].

    Science.gov (United States)

    Li, Zhaoyong; Wang, Fengmei; Niu, Zengyuan; Luo, Xin; Zhang, Gang; Chen, Junhui

    2014-05-01

    A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) using a gradient elution of acetonitrile/water containing 0.1% (v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3 x 10(-6) (3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N = 3) of the 24 compounds were hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.

  10. 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)

  11. 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

  12. MEASUREMENT OF RADIONUCLIDES USING ION CHROMATOGRAPHY AND FLOW-CELL SCINTILLATION COUNTING WITH PULSE SHAPE DISCRIMINATION

    International Nuclear Information System (INIS)

    Fjeld, R. A.; DeVol, T.A.; Leyba, J.D.

    2000-01-01

    Radiological characterization and monitoring is an important component of environmental management activities throughout the Department of Energy complex. Gamma-ray spectroscopy is the technology most often used for the detection of radionuclides. However, radionuclides which cannot easily be detected by gamma-ray spectroscopy, such as pure beta emitters and transuranics, pose special problems because their quantification generally requires labor intensive radiochemical separations procedures that are time consuming and impractical for field applications. This project focused on a technology for measuring transuranics and pure beta emitters relatively quickly and has the potential of being field deployable. The technology combines ion exchange liquid chromatography and on-line alpha/beta pulse shape discriminating scintillation counting to produce simultaneous alpha and beta chromatograms. The basic instrumentation upon which the project was based was purchased in the early 1990's. In its original commercial form, the instrumentation was capable of separating select activation/fission products in ionic forms from relatively pure aqueous samples. We subsequently developed the capability of separating and detecting actinides (thorium, uranium, neptunium, plutonium, americium, and curium) in less than 30 minutes (Reboul, 1993) and realized that the potential time savings over traditional radiochemical methods for isolating some of these radionuclides was significant. However, at that time, the technique had only been used for radionuclide concentrations that were considerably above environmental levels and for aqueous samples of relatively high chemical purity. For the technique to be useful in environmental applications, development work was needed in lowering detection limits; to be useful in applications involving non-aqueous matrices such as soils and sludges or complex aqueous matrices such as those encountered in waste samples, development work was needed in

  13. Determination of feedstuff amino acids composition by ion-exchange chromatography

    Directory of Open Access Journals (Sweden)

    A. A. Volnin

    2018-01-01

    Full Text Available Determination of animal feeds amino acids composition is the very important part of agricultural sciences and livestock management. This is necessary for normalization and balanced of farm animal’s diets parameters. Advances in husbandry techniques are making in response to the needs for rearing high genetic merit livestock. The nutrition of livestock has a critical role in these developments and is an element which needs to be continually updated as new scientific information becomes available. This article is devoted to the use of ion-exchange chromatography with post-colum derivatization by ninhydrin in the study of the amino acid composition and evaluation of the biological value of livestock feedstuff components. The amino acid composition (except tryptophan of the livestock feed-stuff component is presented for threonine – 3.26 g/100g of protein, leucine – 6.43, isoleucine – 3.24, valine – 4.77, methionine – 2.18, lysine – 2.90, phenylalanine – 3.16, histidine – 2.03, tyrosine – 2.33, sum of asparagine and aspartate – 6.76, serine – 3.97, sum of glutamine and glutamic acid – 12.04, glycine – 6.00, alanine – 6.71, arginine – 6.93, proline – 3.08, sum of cystine and cysteine – 1.38. Biological value of feedstuff component compared with the "ideal" protein (FAO WHO is estimated, limiting amino acids were found. The amino acid score was calculated: for threonine – 81.5%, leucine – 91.9%, isoleucine – 81%, valine – 95.4%, lysine – 52.7%, phenylalanine and tyrosine sum – 91.5%, methionine and cysteine sum – 101.7%. Feedstuff component had a low level of essential amino acids in compare with "ideal" protein (FAO WHO. Feedstuff component can be used for livestock nutrition as a component of essential amino-acid balanced diet.

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

    DEFF Research Database (Denmark)

    Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter

    2010-01-01

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

  15. Separation of transition-metal and 8-hydroxyquinoline-5-sulfonic acid complexes using ion-pair liquid chromatography

    International Nuclear Information System (INIS)

    Basova, E.M.; Demurov, L.M.; Shpigun, O.A.; Van Iyuchun'

    1994-01-01

    The retention of chelates of Fe(3), Cu(2), Co(2), Ni(2), Zn(2), Cd(2), Hg(2), and Pb)(2) with 8-hydroxyquinoline-5-sulfonic acid depending on the concentration of cetyltrimethylammonium bromide, acetonitrile, and pH of the mobile phase was investigated using the ion-pair reversed-phase high-performance liquid chromatography on separon C 18 . Under the optimum conditions, the separation of mixtures of Fe(3), Co(2) and Ni(2) is performed within 8 to 12 min

  16. 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

  17. Separation of boron isotopes by ion exchange chromatography: studies on regeneration of strong base anion exchange resins

    International Nuclear Information System (INIS)

    Sharma, B.K.; Subramanian, R.; Mathur, P.K.

    1994-01-01

    The optimum conditions for the regeneration of strong base anion exchange resins of type-I and type-II were determined for cost-effective separation of isotopes of boron by ion exchange chromatography where the hydroxyl form of an anion exchange resin is equilibrated with boric acid solution containing mannitol as a complexing reagent. The possibility of using unspent alkali content of the effluent was also exploited. Removal of carbonate impurity from Rayon grade caustic lye (used as regenerant after dilution) and recycling of Ba(OH) 2 was studied to avoid waste disposal problems. (author)

  18. 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.

  19. Thin-layer chromatography of 49 metal ions on stannic antimonate in aqueous and mixed solvent systems containing dimethylsulfoxide: quantitative separation of uranium from numerous metal ions

    International Nuclear Information System (INIS)

    Qureshi, M.; Varshney, K.G.; Rajput, R.P.S.

    1976-01-01

    Thin-layer chromatography of 40 metal ions in 31 aqueous and mixed solvent systems has been performed on stannic antimonate ion-exchange material. Dimethylsulfoxide has been utilized to resolve such binary mixtures as La 3+ and Ce 3+ from Pr 3+ , Nd 3+ , and Sm 3+ ; VO 2+ from Ti 4+ , Nb 5+ , and Ta 5+ ; Ga 3+ from In 3+ , Tl + , and Y 3+ ; Fe 3+ from VO 2+ ; and Mg 2+ from Al 3+ . Quantitative separation of 200 to 800 μg U from its binary mixtures and from the synthetic mixtures containing Mg 2+ , Bi 3+ , Fe 3+ , Th 4+ , Ce 4+ , Cr 3+ , Zr 4+ , Hf 4+ , Ti 4+ Mn 2+ , Cu 2+ , Ce 3+ , In 3+ , Y 3+ , Ca 2+ , Co 2+ , Tl + , Nb 5+ , and Ag + has been obtained

  20. 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.

  1. Determination of selenite and selenate in human urine by ion chromatography and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    2000-01-01

    The selenium species selenite, selenate and selenomethionine were separated in aqueous solution by ion chromatography. The separation was performed on an IonPac AG11 in series with an AS11 anion exchange column by elution with 25 mM sodium hydroxide in 2% methanol. The Se-78 and Se-82 isotopes were...... monitored in the inductively coupled plasma mass spectrometry (ICP-MS) detector. When the chromatographic system was applied to analysis of urine samples diluted 1 + 1, the selenomethionine signal appeared in the front together with other unresolved selenium species, while the selenite and selenate signals...... and selenate, respectively, corresponding to absolute amounts of 8 and 16 pg, respectively. Calculations were based on peak height measurements of the Se-82 isotope. In 23 analysed urine samples, the concentration of selenite was in the range selenium...

  2. Determination of methylglyoxal-bis(guanylhydrazone) in body fluids by ion-pair chromatography.

    Science.gov (United States)

    Roboz, J; Wu, K T; Hart, R D

    1980-01-01

    Methylglyoxal-bis(guanylhydrazone), Methyl-G, is a potent antineoplastic agent currently undergoing Phase l clinical trials. Serum, ascitic and pleural fluids, and urine are deproteinized with methanol, supernatant is evaporated, residue is redissolved in the eluent, lipids are removed with carbon tetrachloride, and an aliquot of the aqueous layer injected into the chromatograph. Ethylglyoxal-bis(guanylhydrazone) (Ethyl-G) is the internal standard. The mobile phase is a mixture of an aqueous buffer (containing 0.004 M heptane and pentane sulfonic acid, 90%:10%, buffered to pH 3.5) and methanol (68%:32%). The ion-pair complex is retained on a micro Bondapak C18 column, eluted with a flow of 2.0 mL/min. Absorbance is measured at 280 nm. Detectability: 30 ng/mL (0.11 micro M) in serum, ascitic and pleural fluids, 300 ng/mL (1.1 micro M) in urine. Calibration curves (peak height ratios of Methyl-G/Ethyl-G plotted against known drug concentrations) were linear in the 0.1-30 microg/mL range. Correlation coefficinets were 0.999; coefficients of variation for reproducibility were less than 5%. Residual blood levels of Methyl-G persist for several days. Methyl-G was found to pass into ascitic fluid.

  3. Short range correlations in high energy heavy ion collisions

    International Nuclear Information System (INIS)

    Franco, V.; Nutt, W.T.

    1978-01-01

    We present a technique for including the effects of nucleon-nucleon correlations in the optical phase shift (chi) expansion of the nucleus-nucleus scattering amplitude and present the results for chi to second order. The total and inelastic cross sections are consistently higher than those obtained ignoring correlations, and are in better agreement with the data. Furthermore, the inclusion of correlations leads to second order phase shift functions which do not violate unitarity, in constrast to the case when correlations are ignored in very heavy nuclei (A 1 , A 2 > or approx. = 200). In elastic scattering differential cross sections, the effects of correlations can be quite large

  4. Lithium adduct as precursor ion for sensitive and rapid quantification of 20 (S)-protopanaxadiol in rat plasma by liquid chromatography/quadrupole linear ion trap mass spectrometry and application to rat pharmacokinetic study.

    Science.gov (United States)

    Bao, Yuanwu; Wang, Quanying; Tang, Pingming

    2013-03-01

    A novel, rapid and sensitive liquid chromatography/quadrupole linear ion trap mass spectrometry [LC-ESI-(QqLIT)MS/MS] method was developed and validated for the quantification of protopanaxadiol (PPD) in rat plasma. Oleanolic acid (OA) was used as internal standard (IS). A simple protein precipitation based on acetonitrile (ACN) was employed. Chromatographic separation was performed on a Sepax GP-C18 column (50 × 2.1 mm, 5 μM) with a mobile phase consisting of ACN-water and 1.5 μM formic acid and 25 mM lithium acetate (90 : 10, v/v) at a flow rate of 0.4 ml/min for 3.0 min. Multiple-reaction-monitoring mode was performed using lithium adduct ion as precursor ion of m/z 467.5/449.4 and 455.6/407.4 for the drug and IS, respectively. Calibration curve was recovered over a concentration range of 0.5-100 ng/ml with a correlation coefficient >0.99. The limit of detection was 0.2 ng/ml in rat plasma for PPD. The results of the intraday and interday precision and accuracy studies were well within the acceptable limits. The validated method was successfully applied to investigate the pharmacokinetic study of PPD after intravenous and gavage administration to rat. Copyright © 2013 John Wiley & Sons, Ltd.

  5. Simultaneous determination of borate, chloride and molybdate in pyrohydrolysis distillates of plant and soil samples by ion chromatography.

    Science.gov (United States)

    Mishra, Vivekchandra Guruprasad; Das, Mrinal Kanti; Shah, Dipti Jayesh; Jeyakumar, Subbiah; Tomar, Bhupendra Singh; Ramakumar, Karanam Lakshminarayana

    2018-01-12

    Determination of concentrations of micronutrients in plant samples is important in order to assess the growth and quality of plants. An ion chromatography (IC) method was developed for the simultaneous determination of B, Cl and Mo (micronutrients present in their anionic form in aqueous samples) using a gradient elution with d-mannitol and NaOH. Despite their different chemical nature, these elements could be separated from the matrix by employing pyrohydrolysis. IC was employed for their sequential determination from single aliquot injection into the IC column. It was observed that the optimised procedures developed earlier in our laboratory for the separation of B and halogens using d-Mannitol-NaOH or bicarbonate eluents could not be extended to B-Mo-Cl separation. The concentration levels of d-mannitol in the eluent required for separation of boron impeded the conductivity detection of Mo and the peak sensitivity was seen to be critically dependent on d-mannitol concentration in the eluent. In addition, d-mannitol in NaOH eluent altered the retention times of analytes (B, F - , Cl - , NO 3 - , SO 4 2- and MoO 4 2- ) which were not observed in the case of bicarbonate eluent. The current study deals with the investigation on the influence of d-mannitol on the molybdate as well as its role on the retention time. Formation of Mo-mannitol complex at different pH conditions and de-protonation of mannitol were correlated to the observed effects. Based on the observations, a gradient elution method was proposed for the simultaneous separation and determination of B, Cl and Mo in the pyrohydrolysis distillates of plant samples. The method was calibrated for B (0.05-1 mg/L), Cl (0.1-10 mg/L) and Mo (0.5-10 mg/L) and the linear regression coefficients obtained were 0.9992, 0.9998 and 0.997 respectively. The limit of detection (LOD) for B, Cl and Mo was calculated to be 19, 23 and 96 μg/L, respectively. The developed IC method after pyrohydrolytic separation of B

  6. The application of transition metal ion chromatography to the determination of elemental and radiochemical species in PWR primary coolant

    International Nuclear Information System (INIS)

    Bridle, D.A.; Brown, G.R.; Johnson, P.A.V.

    1992-01-01

    The accurate determination of both elemental and radiochemical transition metal corrosion products, particularly cobalt and nickel, in PWR coolants is necessary if the transport mechanisms and their role in the development of out-of-core radiation fields are to be fully understood. AEA Technology, Winfrith, has collaborated for several years with a number of PWR utilities in Europe, developing advanced sampling and analytical techniques for the determination of both soluble and insoluble corrosion products in primary coolant. The design and installation of continuously flowing isokinetic capillary modifications to the existing sampling systems has been shown to be an effective method of providing a low, but representative, sample flow from high pressure systems for on-line determination of corrosion product species. Transition metal ion chromatography coupled with gamma-spectrometry has been used to determine both insoluble and soluble elemental and radiochemical species in reactor coolant, with particular attention being given to the determination of soluble elemental cobalt at levels as low as 1 ng per kg. Soluble species were determined directly following their concentration from up to 1 litre of coolant. Insoluble species collected on 0.45 micron filter membranes, following filtration of up to 1500 litres of coolant, were solubilised by fusion with potassium hydrogen sulphate before the application of ion chromatography. In each case the eluant from the chromatographic column was collected and the radionuclides determined by gamma-spectrometry

  7. Simultaneous determination of artificial sweeteners, preservatives, caffeine, theobromine and theophylline in food and pharmaceutical preparations by ion chromatography.

    Science.gov (United States)

    Chen, Q C; Wang, J

    2001-12-07

    A novel ion chromatographic method was proposed for the simultaneous determination of artificial sweeteners (sodium saccharin, aspartame, acesulfame-K), preservatives (benzoic acid, sorbic acid), caffeine, theobromine and theophylline. The separation was performed on an anion-exchange analytical column operated at 40 degrees C within 45 min by an isocratic elution with 5 mM aqueous NaH2PO4 (pH 8.20) solution containing 4% (v/v) acetonitrile as eluent, and the determination by wavelength-switching ultraviolet absorbance detection. The detection limits (signal-to-noise ratio 3:1) for all analytes were below the sub-microg/ml level. Under the experimental conditions, several organic acids, including citric acid, malic acid, tartaric acid and ascorbic acid, did not interfere with the determination. The method has been successfully applied to the analysis of various food and pharmaceutical preparations, and the average recoveries for real samples ranged from 85 to 104%. The levels of all analytes determined by this method were in good agreement with those obtained by the high-performance liquid chromatographic procedure. The results also indicated that ion chromatography would be possibly a beneficial alternative to conventional high-performance liquid chromatography for the separation and determination of these compounds.

  8. Validation of ion chromatography for the determination of transition metal ions along with alkali, alkaline earth metal elements for uranium oxide fuel

    International Nuclear Information System (INIS)

    Kelkar, Anoop; Prakash, Amrit; Afzal, Mohd.; Panakkal, J.P.

    2009-02-01

    The present report describes the use of Ion chromatography (IC) methods with spectrophotometric and direct conductivity detection for the determination of transition metal elements and alkali alkaline earth metal ions in UO 2 pellets. Transmet analytical column and Metrosep- cation 1-2 column were used for the separation of transition metal elements and alkali and alkaline earth metal elements respectively. Oxalic acid and mixture of pyridine 2,6-dicarboxylic acid (PDCA), Na 2 SO 4 and NaCl were used as mobile phase for the separation of transition metal ions and monitored after post - column reaction with 4,2-pyridylazo resorcinol (PAR) at 520nm spectrophotometrically. In the determination of alkali and alkaline earth metal ions the interference of transition metals are removed by complexing them with PDCA. Mixture of tartaric acid and PDCA employed in the separation of alkali and alkaline earth metal ions and monitored on direct conductivity detector. Mobile phase composition was optimised for the base line separation. Calibration plots of Fe 3+ , Cu 2+ , Ni 2+ , Co 2+ , Cd 2+ , Mn 2+ , Li + , Na + , K + , Mg 2+ , Ca 2+ and Sr 2+ were linear over a wide dynamic range with regression coefficient better than 0.999. Detection limit of above ions were between 5-30ppb. To prevent the overloading of the cation exchange column, uranium matrix was removed from UO 2 sample by solvent extraction with 30% TBP - TOPO/CCl 4 . Ten sintered UO2 pellets of same lot were analysed and R.S.D. ±10% was obtained. These methods were validated by analysis of ILCE standards of UO 2 . (author)

  9. Structure and electron-ion correlation in liquid Mg

    Energy Technology Data Exchange (ETDEWEB)

    Tahara, Shuta [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu Chuo-ku, Fukuoka 810-8560 (Japan); Fujii, Hiroyuki [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu Chuo-ku, Fukuoka 810-8560 (Japan); Japan Synchrotron Radiation Research Institute, 1-1-1 Kouto Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan); Yokota, Yukinobu [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu Chuo-ku, Fukuoka 810-8560 (Japan); Kawakita, Yukinobu [Department of Physics, Faculty of Sciences, Kyushu University, 4-2-1 Ropponmatsu Chuo-ku, Fukuoka 810-8560 (Japan); Kohara, Shinji [Japan Synchrotron Radiation Research Institute, 1-1-1 Kouto Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan); Takeda, Shin' ichi [Department of Physics, Faculty of Sciences, Kyushu University, 4-2-1 Ropponmatsu Chuo-ku, Fukuoka 810-8560 (Japan)]. E-mail: takeda@rc.kyushu-u.ac.jp

    2006-11-15

    For liquid Mg at 700 deg. C, structure factors were obtained from both neutron and X-ray diffraction measurements. The bond angle and coordination number distributions were derived from the reverse Monte Carlo analysis. By a combination of both structure factors, charge density function and electron-ion partial structure factor were deduced.

  10. 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.

  11. Combined Yamamoto approach for simultaneous estimation of adsorption isotherm and kinetic parameters in ion-exchange chromatography.

    Science.gov (United States)

    Rüdt, Matthias; Gillet, Florian; Heege, Stefanie; Hitzler, Julian; Kalbfuss, Bernd; Guélat, Bertrand

    2015-09-25

    Application of model-based design is appealing to support the development of protein chromatography in the biopharmaceutical industry. However, the required efforts for parameter estimation are frequently perceived as time-consuming and expensive. In order to speed-up this work, a new parameter estimation approach for modelling ion-exchange chromatography in linear conditions was developed. It aims at reducing the time and protein demand for the model calibration. The method combines the estimation of kinetic and thermodynamic parameters based on the simultaneous variation of the gradient slope and the residence time in a set of five linear gradient elutions. The parameters are estimated from a Yamamoto plot and a gradient-adjusted Van Deemter plot. The combined approach increases the information extracted per experiment compared to the individual methods. As a proof of concept, the combined approach was successfully applied for a monoclonal antibody on a cation-exchanger and for a Fc-fusion protein on an anion-exchange resin. The individual parameter estimations for the mAb confirmed that the new approach maintained the accuracy of the usual Yamamoto and Van Deemter plots. In the second case, offline size-exclusion chromatography was performed in order to estimate the thermodynamic parameters of an impurity (high molecular weight species) simultaneously with the main product. Finally, the parameters obtained from the combined approach were used in a lumped kinetic model to simulate the chromatography runs. The simulated chromatograms obtained for a wide range of gradient lengths and residence times showed only small deviations compared to the experimental data. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Probing early-time correlations in heavy ion collisions

    International Nuclear Information System (INIS)

    Gavin, Sean; Moschelli, George

    2013-01-01

    We investigate the common influence of correlations arising from initial state parton density fluctuations on measured multiplicity and momentum fluctuations as well as flow fluctuations. We calculate both a universal correlation scale in an initial stage Glasma flux tube picture and the modification to these correlations from later stage hydrodynamic flow. We find quantitative agreement with measurements over a range of collision systems and energies.

  13. Selenium speciation in pretreated human urine by ion-exchange chromatography and ICP-MS detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.; Bendahl, L.

    2001-01-01

    Urine samples were extracted by benzo-15-crown-5-ether to remove sodium and potassium. More than 90% of the sodium and potassium content of the urine was removed with this extraction. In a cation-exchange system based on oxalic acid at pH 3, chromatography of an untreated urine pool resulted...

  14. Determination of major sodium iodide symporter (NIS) inhibitors in drinking waters using ion chromatography with conductivity detector.

    Science.gov (United States)

    Cengiz, Mehmet Fatih; Bilgin, Ayse Kevser

    2016-02-20

    Goiter is an important health problem all over the world and iodine deficiency is its most common cause. Perchlorate, thiocyanate and nitrate (called as major NIS inhibitors) are known to competitively inhibit iodide uptake by the thyroid gland and thus, human exposure to major NIS inhibitors is a public health concern. In this study, an ion chromatographic method for the determination of most common NIS inhibitor ions in drinking waters was developed and validated. This is the first study where an analytical method is used for the determination of major NIS inhibitors in drinking water by an ion chromatography system in a single run. Chromatographic separations were achieved with an anion-exchange column and separated ions were identified by a conductivity detector. The method was found to be selective, linear, precise accurate and true for all of interested ions. The limits of the detections (LOD) were estimated at 0.003, 0.004 and 0.025mgL(-1) for perchlorate, thiocyanate and nitrate, respectively. Possible interference ions in drinking waters were examined for the best separation of NIS inhibitors. The excellent method validation data and proficiency test result (Z-score for nitrate: -0.1) of the FAPAS(®) suggested that the developed method could be applied for determination of NIS inhibitor residues in drinking waters. To evaluate the usefulness of the method, 75 drinking water samples from Antalya/Turkey were analyzed for NIS inhibitors. Perchlorate concentrations in the samples ranged from not detected (less than LOD) to 0.07±0.02mgL(-1) and the range of nitrate concentrations were found to be 3.60±0.01mgL(-1) and 47.42±0.40mgL(-1). No thiocyanate residues were detected in tested drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. 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.

  16. Anions Analysis in Ground and Tap Waters by Sequential Chemical and CO2-Suppressed Ion Chromatography

    Directory of Open Access Journals (Sweden)

    Glen Andrew D. De Vera

    2011-06-01

    Full Text Available An ion chromatographic method using conductivity detection with sequential chemical and CO2 suppression was optimized for the simultaneous determination of fluoride, chloride, bromide, nitrate,phosphate and sulfate in ground and tap water. The separation was done using an anion exchange column with an eluent of 3.2 mM Na2CO3 and 3.2 mM NaHCO3 mixture. The method was linear in the concentration range of 5 to 300 μg/L with correlation coefficients greater than 0.99 for the six inorganic anions. The method was also shown to be applicable in trace anions analysis as given by the low method detection limits (MDL. The MDL was 1μg/L for both fluoride and chloride. Bromide, nitrate, phosphate and sulfate had MDLs of 7 μg/L, 10 μg/L, 9 μg/L and 2 μg/L, respectively. Good precision was obtained as shown in the relative standard deviation of 0.1 to 12% for peak area and 0.1 to 0.3% for retention time. The sensitivity of the method improved with the addition of CO2 suppressor to chemical suppression as shown in the lower background conductivity and detection limits. The recoveries of the anions spiked in water at 300 μg/L level ranged from 100 to 104%. The method was demonstrated to be sensitive, accurate and precise for trace analysis of the six anions and was applied in the anions analysis in ground and tap waters in Malolos, Bulacan. The water samples were found to contain high concentrations of chloride of up to 476 mg/L followed by sulfate (38 mg/L, bromide (1 mg/L, phosphate (0.4 mg/L, fluoride (0.2 mg/L and nitrate (0.1 mg/L.

  17. Electron correlation in highly-charged-ion collisions

    International Nuclear Information System (INIS)

    Hansen, J.P.; Taulbjerg, K.

    1992-01-01

    We have used the coupled-channel method to study the significance of electron correlation in the reaction mechanism for two-electron capture in C 5+ -He collisions. Two different sets of calculations were performed. While the static correlation energy was generally included in the calculations, further correlation effects were ignored in the first set of calculations. In the second set of calculations the so-called doubly excited symmetry basis (DESB) states were used to model the spatial electron correlation. The difference between the two sets of results is so profound that we can conclude that electron correlation plays an essential role in the reaction mechanism. The results of the DESB-based calculations are in good agreement with experimental data [Holt et al., Phys. Rev. A 43, 607 (1991)

  18. Isolation of nitrosylruthenium nitrato complexes by ion exchange and extraction chromatography

    International Nuclear Information System (INIS)

    Huang, H.; Liu, L.

    TBP Levextrel and cation exchange resins were used to separate RuNO nitrato complexes of different nitric acid concentrations. 7402 quaternary ammonium salt Levextrel was used instead of an anionic exchange resin to separate anionic and neutral complex ions. The results indicated that D 3 and D 4 , which can easily be extracted by TBP, were anionic and neutral complex ions

  19. Angular correlations of coincident electron-positron pairs in heavy ion collisions

    International Nuclear Information System (INIS)

    Graf, O.

    1988-10-01

    In the present thesis angular correlations of coincident electron-positron pairsnin heavy ion collisions are studied. It is meant as a contribution to the answer of fundamental questions in the quantum electrodynamics of strong fields. (orig./HSI) [de

  20. Simple extraction method using syringe filter for detection of ethephon in tomatoes by negative-ion mode liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Cho, Soon-Kil; Cho, Ji-Mi; Abd El-Aty, A M; Rahman, Md Musfiqur; Choi, Jeong-Heui; Seo, Young-Jun; Shin, Ho-Chul; Shim, Jae-Han

    2015-10-01

    In this study, a simple, rapid, and sensitive method was developed for the extraction of ethephon from homogenized tomatoes that does not require a cleanup procedure. In a syringe filter, three distinct layers - aqueous, acetonitrile, and n-hexane - are clearly separated after storage at -80 °C for 5-10 min. A Dionex IonPac column was used to separate the analyte before detection using negative-ion mode liquid chromatography with tandem mass spectrometry (LC/MS/MS). The matrix effect of the tested analyte was negligibly small and the matched calibration showed a good linearity over a concentration range of 0.01-1.0 mg/kg with a correlation coefficient (R(2) ) of 0.9998. The recovery at three fortification levels (0.1, 0.5 and 1.0 mg/kg) was between 82.9 and 108.6% with relative standard deviations (RSDs) <5.0%. The limit of quantification (0.03 mg/kg) was lower than the maximum residue limit (3 mg/kg) set by the Ministry of Food and Drug Safety, Republic of Korea. From a field trial, the method developed herein was applied to calculate the decline pattern and predict the pre-harvest residue limits of ethephon in tomatoes. In conclusion, the proposed sample preparation is feasible for the detection of hydrophilic analytes in tomatoes. Copyright © 2015 John Wiley & Sons, Ltd.

  1. Retention prediction and hydrophobicity estimation of weak acidic compounds by reversed-phase liquid chromatography using acetic and perchloric acids as ion suppressors.

    Science.gov (United States)

    Han, Shu-ying; Ming, Xin; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

    2010-11-01

    Simple acids are usually applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography. The purpose of this study is to investigate the retention behavior of various weak acidic compounds (monoprotic, diprotic, triprotic, and tetraprotic acids) using acetic or perchloric acid as ion suppressor in a binary hydroorganic mobile phase. The apparent n-octanol-water partition coefficient (K(ow)") was proposed to calibrate the n-octanol-water partition coefficient (K(ow)) of weak acidic compound. LogK(ow)" was found to have a better linear correlation with logk(w), the logarithm of the retention factor obtained by extrapolating to neat aqueous fraction of the mobile phase, for all weakly ionizable acidic compounds. This straightforward relationship offers a potential medium for direct measurement of K(ow) data of weak acidic analytes and can be used to predict retention behavior of these compounds in the ion suppression reversed-phase liquid chromatographic mode.

  2. Structure and electron-ion correlation of liquid germanium

    Energy Technology Data Exchange (ETDEWEB)

    Kawakita, Y. [Faculty of Sciences, Kyushu University, 4-2-1 Ropponmatsu, Fukuoka 810-8560 (Japan)]. E-mail: kawakita@rc.kyushu-u.ac.jp; Fujita, S. [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu, Fukuoka 810-8560 (Japan); Kohara, S. [Japan Synchrotron Radiation Research Institute, 1-1-1 Kouto Mikazuki-cho, Hyogo 679-5198 (Japan); Ohshima, K. [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu, Fukuoka 810-8560 (Japan); Fujii, H. [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu, Fukuoka 810-8560 (Japan); Yokota, Y. [Graduate School of Sciences, Kyushu University, 4-2-1 Ropponmatsu, Fukuoka 810-8560 (Japan); Takeda, S. [Faculty of Sciences, Kyushu University, 4-2-1 Ropponmatsu, Fukuoka 810-8560 (Japan)

    2005-08-15

    Structure factor of liquid germanium (Ge) has a shoulder at {theta} = 3.2 A{sup -1} in the high-momentum-transfer region of the first peak. To investigate the origin of such a non-simplicity in the structure, high energy X-ray diffraction measurements have been performed using 113.26 keV incident X-ray, at BL04B2 beamline of SPring-8. By a combination of the obtained structure factor with the reported neutron diffraction data, charge density function and electron-ion partial structure factor have been deduced. The peak position of the charge distribution is located at about 1 A, rather smaller r value than the half value of nearest neighbor distance ({approx}2.7 A), which suggests that valence electrons of liquid Ge play a role of screening electrons around a metallic ion rather than covalently bonding electrons.

  3. Application of perfluorinated acids as ion-pairing reagents for reversed-phase chromatography and retention-hydrophobicity relationships studies of selected beta-blockers.

    Science.gov (United States)

    Flieger, J

    2010-01-22

    The addition of the homologous series of perfluorinated acids-trifluoroacetic acid (TFAA), pentafluoropropionic acid (PFPA), heptafluorobutyric acid (HFBA) to mobile phases for reversed-phase high-performance liquid chromatography (RP-HPLC) of beta-blockers was tested. Acidic modifiers were responsible for acidification of mobile phase (pH 3) ensuring the protonation of the beta-blockers and further ion pairs creation. The effect of the type and concentration of mobile phase additives on retention parameters, the efficiency of the peaks, their symmetry and separation selectivity of the beta-blockers mixture were all studied. It appeared that at increasing acid concentration, the retention factor, for all compounds investigated, increased to varying degrees. It should be stressed that the presence of acids more significantly affected the retention of the most hydrophobic beta-blockers. Differences in hydrophobicity of drugs can be maximized through variation of the hydrophobicity of additives. Thus, the relative increase in the retention depends on either concentration and hydrophobicity of the anionic mobile phase additive or hydrophobicity of analytes. According to QSRR (quantitative structure retention relationship) methodology, chromatographic lipophilicity parameters: isocratic log k and log k(w) values (extrapolated retention to pure water) were correlated with the molecular (log P(o/w)) and apparent (log P(app)) octanol-water partition coefficients obtained experimentally by countercurrent chromatography (CCC) or predicted by Pallas software. The obtained, satisfactory retention-hydrophobicity correlations indicate that, in the case of the basic drugs examined in RP-HPLC systems modified with perfluorinated acids, the retention is mainly governed by their hydrophobicity. Copyright 2009 Elsevier B.V. All rights reserved.

  4. 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

  5. Statistical electron correlation coefficients for the five lowest states of the heliumlike ions

    International Nuclear Information System (INIS)

    Thakkar, A.J.; Smith, V.H. Jr.

    1981-01-01

    Statistical correlation coefficients were introduced by Kutzelnigg, Del Re, and Berthier to provide overall measures of the difference between the electron pair density and the product of one-electron densities in atoms and molecules. Some properties of these coefficients are discussed, and it is shown that an angular correlation coefficient is experimentally accessible. Radial and angular correlation coefficients are computed from highly accurate wave functions for the 1 1 S, 2 3 S, 2 1 S, 2 3 P, and 2 1 P states of the heliumlike ions from He through Mg 10+ . It is found that positive angular correlation coefficients occur in the 2 1 P state of the two-electron positive ions but not in neutral helium. Moreover, the angular correlation coefficients for the 2 1 S and 2 3 S states of the positively charged two-electron ions show that a previously proposed reformulation of Hund's rule is incorrect

  6. Immobilized palladium(II) ion affinity chromatography for recovery of recombinant proteins with peptide tags containing histidine and cysteine.

    Science.gov (United States)

    Kikot, Pamela; Polat, Aise; Achilli, Estefania; Fernandez Lahore, Marcelo; Grasselli, Mariano

    2014-11-01

    Fusion of peptide-based tags to recombinant proteins is currently one of the most used tools for protein production. Also, immobilized metal ion affinity chromatography (IMAC) has a huge application in protein purification, especially in research labs. The combination of expression systems of recombinant tagged proteins with this robust chromatographic system has become an efficient and rapid tool to produce milligram-range amounts of proteins. IMAC-Ni(II) columns have become the natural partners of 6xHis-tagged proteins. The Ni(II) ion is considered as the best compromise of selectivity and affinity for purification of a recombinant His-tagged protein. The palladium(II) ion is also able to bind to side chains of amino acids and form ternary complexes with iminodiacetic acid and free amino acids and other sulfur-containing molecules. In this work, we evaluated two different cysteine- and histidine-containing six amino acid tags linked to the N-terminal group of green fluorescent protein (GFP) and studied the adsorption and elution conditions using novel eluents. Both cysteine-containing tagged GFPs were able to bind to IMAC-Pd(II) matrices and eluted successfully using a low concentration of thiourea solution. The IMAC-Ni(II) system reaches less than 20% recovery of the cysteine-containing tagged GFP from a crude homogenate of recombinant Escherichia coli, meanwhile the IMAC-Pd(II) yields a recovery of 45% with a purification factor of 13. Copyright © 2014 John Wiley & Sons, Ltd.

  7. Pauli correlations in heavy-ion collisions at high energies

    International Nuclear Information System (INIS)

    Franco, V.; Nutt, W.T.

    1977-01-01

    The effects of short-range correlations on the Glauber expansion for nucleus-nucleus collisions are calculated using the Fermi gas model for nuclei. When the Pauli principle is neglected for collisions between heavy nuclei, calculation of the optical phase-shift function leads to non-unitary results and cross sections cannot be obtained. When Pauli correlations are included important cancellations in the optical phase-shift function are found which make possible the calculation of total and differential cross sections for heavy nuclei. (Auth.)

  8. 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

  9. 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.

  10. Fragmentation and momentum correlations in heavy-ion collisions

    Indian Academy of Sciences (India)

    The role of momentum correlations in the production of light and medium mass fragments is studied by imposing momentum cut in the clusterization of the phase space. Our detailed investigation shows that momentum cut has a major role to play in the emission of fragments. A comparison with the experimental data is also ...

  11. Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Sklerov, J H; Kalasinsky, K S; Ehorn, C A

    1999-10-01

    A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

  12. 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)

  13. Analysis of Disperse Dyes Using Liquid Chromatography/Linear Ion Trap Mass Spectrometry (LC/LIT-MSn) and Database Construction.

    Science.gov (United States)

    Kato, Takao; Ikeue, Takahisa; Suzuki, Yasuhiro; Handa, Makoto

    2016-01-01

    Liquid chromatography/linear ion trap mass spectrometry (LC/LIT-MS(n)) was used to construct a database of disperse dyes. Fifty-three standard dyes were subjected to LC/LIT-MS(n) and characterized based on their mass spectra (MS, MS(2), and MS(3)), values of λmax (maximum absorption wavelength in the UV-visible spectrum), and retention times. The results demonstrate that it is possible to reliably identify coexisting dyes that cannot be separated by LC or detected by diode array detection due to their low molecular absorption coefficients. In addition, the by-products included in the standard dyes were found to provide important information for the identification and discrimination of dyestuffs synthesized using different processes. The confirmation of the effectiveness of LC/LIT-MS(n) analysis in detecting small amounts of disperse dyes in this study shows its potential for use in the discrimination of dyed fibers obtained at crime scenes.

  14. Determination of short chain carboxylic acids in vegetable oils and fats using ion exclusion chromatography electrospray ionization mass spectrometry.

    Science.gov (United States)

    Viidanoja, Jyrki

    2015-02-27

    A new method for quantification of short chain C1-C6 carboxylic acids in vegetable oils and fats by employing Liquid Chromatography Mass Spectrometry (LC-MS) has been developed. The method requires minor sample preparation and applies non-conventional Electrospray Ionization (ESI) liquid phase chemistry. Samples are first dissolved in chloroform and then extracted using water that has been spiked with stable isotope labeled internal standards that are used for signal normalization and absolute quantification of selected acids. The analytes are separated using Ion Exclusion Chromatography (IEC) and detected with Electrospray Ionization Mass Spectrometry (ESI-MS) as deprotonated molecules. Prior to ionization the eluent that contains hydrochloric acid is modified post-column to ensure good ionization efficiency of the analytes. The averaged within run precision and between run precision were generally lower than 8%. The accuracy was between 85 and 115% for most of the analytes. The Lower Limit of Quantification (LLOQ) ranged from 0.006 to 7mg/kg. It is shown that this method offers good selectivity in cases where UV detection fails to produce reliable results. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Determination of antimony compounds in waters and juices using ion chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Lin, Ya-An; Jiang, Shiuh-Jen; Sahayam, A C

    2017-09-01

    A method was developed by coupling ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) for the speciation of antimony. In this study, antimony species such as antimonite [Sb(III)], antimonate [Sb(V)] and trimethyl antimony(V) (TMeSb) were separated in less than 8min using anion exchange chromatography with a Hamilton PRP-X100 column as the stationary phase. Mobile phase A was 20mmolL -1 ethylenediaminetetraacetic acid (EDTA), 2mmolL -1 potassium hydrogen phthalate (KHP) in 1% v/v methanol (pH 5.5) and 20mmolL -1 EDTA, 2mmolL -1 KHP, 40mmolL -1 (NH 4 ) 2 CO 3 in 1% v/v methanol (pH 9.0) formed mobile phase B. Detection limits and relative standard deviations (RSD) were 0.012-0.032ngmL -1 and 2.2-2.8% respectively. This method was applied to bottled waters and fruit juices purchased in Kaohsiung, Taiwan. In water samples, Sb(V) was the major species where as in juices organometallic Sb species were also present. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

    Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

    2013-11-15

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

  17. Analysis of perchlorate, thiocyanate, nitrate and iodide in human amniotic fluid using ion chromatography and electrospray tandem mass spectrometry

    International Nuclear Information System (INIS)

    Blount, Benjamin C.; Valentin-Blasini, Liza

    2006-01-01

    Because of health concerns surrounding in utero exposure to perchlorate, we developed a sensitive and selective method for quantifying iodide, as well as perchlorate and other sodium-iodide symporter (NIS) inhibitors in human amniotic fluid using ion chromatography coupled with electrospray ionization tandem mass spectrometry. Iodide and NIS inhibitors were quantified using a stable isotope-labeled internal standards (Cl 18 O 4 - , S 13 CN - and 15 NO 3 - with excellent assay accuracy of 100%, 98%, 99%, 95% for perchlorate, thiocyanate, nitrate and iodide, respectively, in triplicate analysis of spiked amniotic fluid sample). Excellent analytical precision (<5.2% RSD for all analytes) was found when amniotic fluid quality control pools were repetitively analyzed for iodide and NIS-inhibitors. Selective chromatography and tandem mass spectrometry reduced the need for sample cleanup, resulting in a rugged and rapid method capable of routinely analyzing 75 samples/day. Analytical response was linear across the physiologically relevant concentration range for the analytes. Analysis of a set of 48 amniotic fluid samples identified the range and median levels for perchlorate (0.057-0.71, 0.18 μg/L), thiocyanate (<10-5860, 89 μg/L), nitrate (650-8900, 1620 μg/L) and iodide (1.7-170, 8.1 μg/L). This selective, sensitive, and rapid method will help assess exposure of the developing fetus to low levels of NIS-inhibitors and their potential to inhibit thyroid function

  18. 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

  19. DETERMINATION OF A BOUND MUSK XYLENE METABOLITE IN CARP HEMOGLOBIN AS A BIOMARKER OF EXPOSURE BY GAS CHROMATOGRAPHY MASS SPECTROMETRY USING SELECTED ION MONITORING

    Science.gov (United States)

    Musk xylene (MX) is widely used as a fragrance ingredient in commercial toiletries. Identification and quantification of a bound 4-amino-MX (AMX) metabolite was carried out by gas chromatography-mass spectrometry (GC/MS), with selected ion monitoring (SIM). Detection of AMX occur...

  20. Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, Fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques

    NARCIS (Netherlands)

    Nielen, M.W.F.; Engelen, M.C. van; Zuiderent, R.; Ramaker, R.

    2007-01-01

    An emerging trend is recognised in hormone and veterinary drug residue analysis from liquid chromatography tandem mass spectrometry (LC/MS/MS) based screening and confirmation towards accurate mass alternatives such as LC coupled with time-of-flight (TOF), Fourier transform ion cyclotron resonance

  1. 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.

  2. Immobilised metal-ion affinity chromatography purification of histidine-tagged recombinant proteins : a wash step with a low concentration of EDTA

    NARCIS (Netherlands)

    Westra, DF; Welling, GW; Koedijk, DGAM; Scheffer, AJ; The, TH; Welling-Wester, S

    2001-01-01

    Immobilised metal-ion affinity chromatography (IMAC) is widely used for the purification of recombinant proteins in which a poly-histidine tag is introduced. However, other proteins may also bind to IMAC columns. We describe the use of a washing buffer with a low concentration of EDTA (0.5 mM) for

  3. Dispersive solid phase extraction combined with ion-pair ultra high-performance liquid chromatography tandem mass spectrometry for quantification of nucleotides in Lactococcus lactis

    DEFF Research Database (Denmark)

    Magdenoska, Olivera; Martinussen, Jan; Thykær, Jette

    2013-01-01

    solid phase extraction with charcoal and subsequent analysis with ion-pair liquid chromatography coupled with electrospray ionization tandem mass spectrometry was established for quantification of intracellular pools of the 28 most important nucleotides. The method can handle extracts where cells leak...

  4. 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...

  5. Peptide sequencing and characterization of post-translational modifications by enhanced ion-charging and liquid chromatography electron-transfer dissociation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Kjeldsen, Frank; Giessing, Anders; Ingrell, Christian R

    2007-01-01

    We have tested the effect of m-nitrobenzyl alcohol (m-NBA) as a method to increase the average charge state of protonated gas-phase molecular ions generated by ESI from tryptic peptides and phosphopeptides. Various concentrations of m-NBA were added to the mobile phases of a liquid chromatography...

  6. 2-Alkylcyclobutanones as markers for irradiated foodstuffs. III. Improvement of the field of application on the EN 1785 method by using silver ion chromatography

    NARCIS (Netherlands)

    Ndiaye, B; Horvatovich, P; Miesch, M; Hasselmann, C; Marchioni, E

    1999-01-01

    The inclusion of a purification step by silver ion chromatography in the EN 1785 analytical protocol for 2-alkylcyclobutanones (validated by the European Committee for Standardization for the detection of ionizing radiation treatment) has considerably improved the quality of the chromatograms

  7. Regioisomeric analysis of triacylglycerols using silver-ion liquid chromatography-atmospheric pressure chemical ionization mass spectrometry: Comparison of five different mass analyzers

    Czech Academy of Sciences Publication Activity Database

    Holčapek, M.; Dvořáková, H.; Lísa, M.; Girón, A. J.; Sandra, P.; Cvačka, Josef

    2010-01-01

    Roč. 1217, č. 52 (2010), s. 8186-8194 ISSN 0021-9673 R&D Projects: GA ČR GA203/09/0139 Institutional research plan: CEZ:AV0Z40550506 Keywords : triacylglycerols * silver-ion liquid chromatography * regioisomer * HPLC/MS * APCI Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.194, year: 2010

  8. Studies on the determination of trace amounts of nitrogen along with alkali and alkaline earth elements in uranium based samples by ion-chromatography (IC)

    International Nuclear Information System (INIS)

    Verma, Poonam; Rastogi, R.K.; Ramakumar, K.L.

    2006-12-01

    Present report describes an ion chromatography (IC) method with suppressed conductivity detection for the determination of traces of nitrogen along with alkali and alkaline earth elements in uranium based nuclear fuels. Method was developed to determine nitrogen as NH 4 + along with alkali and alkaline earth cations by IC using a cation exchange column. (author)

  9. Sequence-dependent separation of trinucleotides by ion-interaction reversed-phase liquid chromatography A structure-retention study assisted by soft-modelling and molecular dynamics

    Czech Academy of Sciences Publication Activity Database

    Mikulášek, K.; Jaroň, Kamil S.; Kulhánek, P.; Bittová, M.; Havliš, J.

    2016-01-01

    Roč. 1469, October (2016), s. 88-95 ISSN 0021-9673 Institutional support: RVO:68081766 Keywords : Sequence-dependent separation * Ion-interaction reversed-phase liquid chromatography * Trinucleotides * Oligonucleotide sequence isomers * QSRR * Molecular dynamics Subject RIV: CE - Biochemistry Impact factor: 3.981, year: 2016

  10. Comprehensive Analysis of Umami Compounds by Ion-Pair Liquid Chromatography Coupled to Mass Spectrometry

    NARCIS (Netherlands)

    Coulier, L.; Bas, R.; Hekman, M.; Werff, B.J.C. van der; Burgering, M.; Thissen, U.

    2011-01-01

    An ion-pair LC-ESI-MS method was developed capable of analyzing various reported umami or umami-enhancing compounds, including glutamic acid and 5'-ribonucleotides. The method was validated using tomato and potato samples and showed overall good analytical performance with respect to selectivity,

  11. Beta Neutrino Correlation Measurement with Trapped Radioactive Ions

    International Nuclear Information System (INIS)

    Velten, Ph.; Ban, G.; Durand, D.; Flechard, X.; Lienard, E.; Mauger, F.; Naviliat-Cuncic, O.; Mery, A.; Rodriguez, D.; Thomas, J.-C.

    2010-01-01

    The beta-neutrino angular correlation coefficient provides a sensitive observable to search for physics beyond the standard electroweak model in nuclear beta decay. We address here the measurement of this parameter in the pure Gamow-Teller transition of 6 He. A deviation from the standard model prediction would indicate the existence of tensor like couplings, possibly mediated by new bosons like leptoquarks. The aim of the LPCTrap experiment is to measure this coefficient with a statistical uncertainty of 0.5% using a novel transparent Paul trap. The status of the experiment is briefly presented along with the work in progress.

  12. Bose-Einstein correlations between hard photons produced in heavy ions collisions; Correlations Bose-Einstein entre photons durs produits dans les collisions d`ions lourds

    Energy Technology Data Exchange (ETDEWEB)

    Marques Moreno, F M

    1994-06-01

    Heavy-ion collisions offer the unique possibility to create in the laboratory nuclear matter far from equilibrium. The electromagnetic probe constituted by hard photons and the Bose-Einstein correlations were used to study the properties of such a matter (size, density, temperature...). It is shown how the formalism has evolved from Young experiments to heavy-ion collisions experiments. The experiments performed with the photon multidetector TAPS at Ganil are described. The systems studied are: {sup 86}KR + {sup nat}Ni at 60.0 A.MeV, and {sup 181}Ta + {sup 197}Au at 39.5 A.MeV. Results are presented concerning the production of gamma, pi{sup 0}, e{sup +-} and {gamma}{gamma} correlation. The results are interpreted with the help of static and dynamic calculations describing hard photon production in heavy ion collisions. For the first time in Nuclear Physics, the existence of the Bose-Einstein effect for photons in the range of gamma is demonstrated, and the existence of two different photon sources is postulated, reflecting the density oscillations taking place in the nuclear matter created in heavy-ion collisions. (from author) 55 figs., 22 tabs., 76 refs.

  13. Signals of strong electronic correlation in ion scattering processes

    Science.gov (United States)

    Bonetto, F.; Gonzalez, C.; Goldberg, E. C.

    2016-05-01

    Previous measurements of neutral atom fractions for S r+ scattered by gold polycrystalline surfaces show a singular dependence with the target temperature. There is still not a theoretical model that can properly describe the magnitude and the temperature dependence of the neutralization probabilities found. Here, we applied a first-principles quantum-mechanical theoretical formalism to describe the time-dependent scattering process. Three different electronic correlation approaches consistent with the system analyzed are used: (i) the spinless approach, where two charge channels are considered (S r0 and S r+ ) and the spin degeneration is neglected; (ii) the infinite-U approach, with the same charge channels (S r0 and S r+ ) but considering the spin degeneration; and (iii) the finite-U approach, where the first ionization and second ionization energy levels are considered very, but finitely, separated. Neutral fraction magnitudes and temperature dependence are better described by the finite-U approach, indicating that e -correlation plays a significant role in charge-transfer processes. However, none of them is able to explain the nonmonotonous temperature dependence experimentally obtained. Here, we suggest that small changes in the surface work function introduced by the target heating, and possibly not detected by experimental standard methods, could be responsible for that singular behavior. Additionally, we apply the same theoretical model using the infinite-U approximation for the Mg-Au system, obtaining an excellent description of the experimental neutral fractions measured.

  14. Stopping dynamics of ions passing through correlated honeycomb clusters

    Science.gov (United States)

    Balzer, Karsten; Schlünzen, Niclas; Bonitz, Michael

    2016-12-01

    A combined nonequilibrium Green functions-Ehrenfest dynamics approach is developed that allows for a time-dependent study of the energy loss of a charged particle penetrating a strongly correlated system at zero and finite temperatures. Numerical results are presented for finite inhomogeneous two-dimensional Fermi-Hubbard models, where the many-electron dynamics in the target are treated fully quantum mechanically and the motion of the projectile is treated classically. The simulations are based on the solution of the two-time Dyson (Keldysh-Kadanoff-Baym) equations using the second-order Born, third-order, and T -matrix approximations of the self-energy. As application, we consider protons and helium nuclei with a kinetic energy between 1 and 500 keV/u passing through planar fragments of the two-dimensional honeycomb lattice and, in particular, examine the influence of electron-electron correlations on the energy exchange between projectile and electron system. We investigate the time dependence of the projectile's kinetic energy (stopping power), the electron density, the double occupancy, and the photoemission spectrum. Finally, we show that, for a suitable choice of the Hubbard model parameters, the results for the stopping power are in fair agreement with ab initio simulations for particle irradiation of single-layer graphene.

  15. Toxic Cyanobacteria in Svalbard: Chemical Diversity of Microcystins Detected Using a Liquid Chromatography Mass Spectrometry Precursor Ion Screening Method

    Directory of Open Access Journals (Sweden)

    Julia Kleinteich

    2018-04-01

    Full Text Available Cyanobacteria synthesize a large variety of secondary metabolites including toxins. Microcystins (MCs with hepato- and neurotoxic potential are well studied in bloom-forming planktonic species of temperate and tropical regions. Cyanobacterial biofilms thriving in the polar regions have recently emerged as a rich source for cyanobacterial secondary metabolites including previously undescribed congeners of microcystin. However, detection and detailed identification of these compounds is difficult due to unusual sample matrices and structural congeners produced. We here report a time-efficient liquid chromatography-mass spectrometry (LC-MS precursor ion screening method that facilitates microcystin detection and identification. We applied this method to detect six different MC congeners in 8 out of 26 microbial mat samples of the Svalbard Archipelago in the Arctic. The congeners, of which [Asp3, ADMAdda5, Dhb7] MC-LR was most abundant, were similar to those reported in other polar habitats. Microcystins were also determined using an Adda-specific enzyme-linked immunosorbent assay (Adda-ELISA. Nostoc sp. was identified as a putative toxin producer using molecular methods that targeted 16S rRNA genes and genes involved in microcystin production. The mcy genes detected showed highest similarities to other Arctic or Antarctic sequences. The LC-MS precursor ion screening method could be useful for microcystin detection in unusual matrices such as benthic biofilms or lichen.

  16. Separation of polythionates and the gold thiosulfate complex in gold thiosulfate leach solutions by ion-interaction chromatography.

    Science.gov (United States)

    O'Reilly, John W; Shaw, Matthew J; Dicinoski, Greg W; Grosse, Andrew C; Miura, Yasuyuki; Haddad, Paul R

    2002-07-01

    A method for the separation of the polythionates (SxO6(2-), x = 3-5) in gold thiosulfate leach solutions using ion-interaction chromatography with conductivity and ultraviolet (UV) detection is described. Polythionates were eluted within 18 min using an eluent comprising an acetonitrile step gradient at 0.0 min from 15% v/v to 28% v/v, 3 mM TBAOH, and 2.5 mM sodium carbonate, operated using a Dionex NS1-5 micron column with guard. The developed method was capable of separating the gold thiosulfate complex ion in standard solutions, but quantification of this species in realistic leach solutions proved impractical due to a self-elution effect that caused the gold peak to be eluted as a broad band. Detection limits for polythionates using a 10 microL injection volume ranged between 1-6 mg L(-1) (5-23 microM) for conductivity and 0.8-13 mg L(-1) (4-68 microM) for UV detection, based on a signal-to-noise ratio of 2. Calibration was linear over the ranges 5-2000, 10-2000 and 25-2500 mg L(-1) for trithionate, tetrathionate and pentathionate, respectively. The technique was applied successfully to leach liquors containing 0.5 M ammonium thiosulfate, 2 M ammonia, 0.05 M copper sulfate and 20 % m/v gold ore.

  17. The separation of [32P]inositol phosphates by ion-pair chromatography: Optimization of the method and biological applications

    International Nuclear Information System (INIS)

    Sulpice, J.C.; Gascard, P.; Journet, E.; Rendu, F.; Renard, D.; Poggioli, J.; Giraud, F.

    1989-01-01

    We have developed an ion-pair reverse-phase HPLC method to measure inositol phosphates in 32 P-labeled cells. The different chromatographic parameters were analyzed to optimize the resolution of the 32 P-labeled metabolites. Analysis of inositol phosphates in biological samples was improved by a single charcoal pretreatment which eliminated interfering nucleotides without removing inositol phosphates. The kinetics of production of inositol phosphates in calcium-activated erythrocytes, vasopressin-stimulated hepatocytes, and thrombin-activated platelets were analyzed. Original data on the activation of phosphoinositide phospholipase C were obtained in intact erythrocytes by direct measurement of inositol (1,4,5)P3. Data from agonist-stimulated hepatocytes and platelets were consistent with those from previous studies. In conclusion, this technique offers many advantages over the methodologies currently employed involving anion-exchange chromatography and [ 3 H]inositol labeling: (i) 32 P labeling is less expensive and more efficient than 3 H labeling and can be used with all types of cells without permeabilization treatments and (ii) ion-pair HPLC gives good resolution of inositol phosphates from nucleotides with shorter retention times, and long reequilibration periods are not required

  18. Ion chromatography-mass spectrometry: a review of recent technologies and applications in forensic and environmental explosives analysis.

    Science.gov (United States)

    Barron, Leon; Gilchrist, Elizabeth

    2014-01-02

    The development and application of ion chromatography (IC) coupled to mass spectrometry (MS) is discussed herein for the quantitative determination of low-order explosives-related ionic species in environmental and forensic sample types. Issues relating to environmental explosives contamination and the need for more confirmatory IC-MS based applications in forensic science are examined. In particular, the compatibility of a range of IC separation modes with MS detection is summarised along with the analytical challenges that have been overcome to facilitate determinations at the ng-μg L(-1) level. Observed trends in coupling IC to inductively coupled plasma and electrospray ionisation mass spectrometry form a particular focus. This review also includes a discussion of the relative performance of reported IC-MS methods in comparison to orthogonal ion separation-based, spectrometric and spectroscopic approaches to confirmatory detection of low-order explosives. Finally, some promising areas for future research are highlighted and discussed with respect to potential IC-MS applications. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Boron isotope separation by ion exchange chromatography using weakly basic anion exchange resin

    International Nuclear Information System (INIS)

    Sakuma, Yoichi; Aida, Masao; Okamoto, Makoto; Kakihana, Hidetake

    1980-01-01

    Isotopic plateau displacement chromatography, a useful method for isotope separation is presented. The boric acid band formed in a column of weakly basic anion exchange resin Diaion WA21 can be eluted with pure water. In order to obtain good accumulation of the isotope effect, a series of experiments with different migration length were carried out. The boron-10 enriched part of the boric acid absorbed band was always preceded by the isotopic plateau part, in which the atomic fraction of boron-10 was maintained at its original value. The atomic fraction of boron-10 at the end of the chromatogram increased with migration length, and in the case of 256-m migration, boron-10 was enriched from its original atomic fraction of 19.84 to 91.00%, the separation factor S being constant irrespective of migration length: S = 1.0100 +- 0.0005. (author)

  20. Alternative extraction of alkaloid anticarcinogens from Brazilian "vinca rosea" using Ion exchange chromatography

    Directory of Open Access Journals (Sweden)

    Sérgio Freire de Carvalhaes

    Full Text Available Extracts in ethanol and ethanol-ammonia of dried leaves from Catharanthus roseus, gathered at Rio de Janeiro state, were adsorbed in a strongly acidic cation exchange resin with sulfonic acid group, using the finite bath method, resulting in an alkaloid retained fraction and an acidic and neutral unretained fraction. High Performance Liquid Chromatography showed the isolation of the alkaloid fraction to be highly selective and with good performance, with an absence of alkaloids in the unretained fraction, while the retained fraction presented 1,54-6,35 mg/g of vindoline and 0,12-0,91 mg/g of vinblastine, common for an alkaloid-rich concentrate, usually obtained by classic extraction with several steps using solvents.

  1. Ion-Exchange Membrane Chromatography as an Alternative Method of Separation of Potato y Virus

    Directory of Open Access Journals (Sweden)

    Treder Krzysztof

    2015-12-01

    Full Text Available Procedures of separation of virus particles from a plant material are multistage. Furthermore often they are difficult in terms of methodology and require use of expensive, highly specialist equipment and yield of separation is often low. The antigen obtained is often degraded and contains admixtures of other proteins. Therefore, generation of high quality and specificity antibodies based on such antigen is very difficult and quality of the antibodies has impact on reliability, sensitivity and unambiguity of results of immunodiagnostic tests (e.g. ELISA that are currently conventionally used to detect vegetable viruses. In this study three conventionally-performed methods of separation of potato virus Y (PVY were compared and a method of separation based on membrane chromatography, as an alternative separation technique, has been presented. It has been demonstrated that in proper process conditions good quality virus preparation can be obtained.

  2. Relativistic configuration-interaction calculation of the correlation energies of heliumlike ions. Revision 1

    International Nuclear Information System (INIS)

    Cheng, K.T.; Chen, M.H.; Johnson, W.R.

    1994-04-01

    A new relativistic configuration-interaction (CI) method using B-spline basis functions has been developed to study the correlation energies of two-electron heliumlike ions. Based on the relativistic no-pair Hamiltonian, the CI equation leads to a symmetric eigenvalue problem involving large, dense matrices. Davidson's method is used to obtain the lowest few eigenenergies and eigenfunctions. Results on transition energies and finite structure splittings for heliumlike ions are in very good agreement with experiment throughout the periodic table

  3. 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.

  4. Design and performance evaluation of a microfluidic ion-suppression module for anion-exchange chromatography.

    Science.gov (United States)

    Wouters, Sam; Wouters, Bert; Jespers, Sander; Desmet, Gert; Eghbali, Hamed; Bruggink, Cees; Eeltink, Sebastiaan

    2014-08-15

    A microfluidic membrane suppressor has been constructed to suppress ions of alkaline mobile-phases via an acid-base reaction across a sulfonated poly(tetrafluoroethylene)-based membrane and was evaluated for anion-exchange separations using conductivity detection. The membrane was clamped between two chip substrates, accommodating rectangular microchannels for the eluent and regenerant flow, respectively. Additionally, a clamp-on chip holder has been constructed which allows the alignment and stacking of different chip modules. The response and efficacy of the microfluidic chip suppressor was assessed for a wide range of eluent (KOH) concentrations, using 127 and 183μm thick membranes, while optimizing the flow rate and concentration of the regenerant solution (H2SO4). The optimal operating eluent flow rate was determined at 5μL/min, corresponding to the optimal van-Deemter flow velocity of commercially-available column technology, i.e. a 0.4mm i.d.×250mm long column packed with 7.5μm anion-exchange particles. When equilibrated at 10mM KOH, a 99% decrease in conductivity signal could be obtained within 5min when applying 10mM H2SO4 regenerant at 75μL/min. A background signal as low as 1.2μS/cm was obtained, which equals the performance of a commercially-available electrolytic hollow-fiber suppressor. When increasing the temperature of the membrane suppressor from 15 to 20°C, ion suppression was significantly improved allowing the application of 75mM KOH. The applicability of the chip suppressor has been demonstrated with an isocratic baseline separation of a mixture of seven inorganic ions, yielding plate numbers between 5300 and 10,600 and with a gradient separation of a complex ion mixture. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Multiresidue determination of pesticides in malt beverages by capillary gas chromatography with mass spectrometry and selected ion monitoring.

    Science.gov (United States)

    Wong, Jon W; Webster, Michael G; Bezabeh, Dawit Z; Hengel, Mathew J; Ngim, Kenley K; Krynitsky, Alexander J; Ebeler, Susan E

    2004-10-20

    A method was developed to determine pesticides in malt beverages using solid phase extraction on a polymeric cartridge and sample cleanup with a MgSO4-topped aminopropyl cartridge, followed by capillary gas chromatography with electron impact mass spectrometry in the selected ion monitoring mode [GC-MS(SIM)]. Three GC injections were required to analyze and identify organophosphate, organohalogen, and organonitrogen pesticides. The pesticides were identified by the retention times of peaks of the target ion and qualifier-to-target ion ratios. GC detection limits for most of the pesticides were 5-10 ng/mL, and linearity was determined from 50 to 5000 ng/mL. Fortification studies were performed at 10 ng/mL for three malt beverages that differ in properties such as alcohol content, solids, and appearance. The recoveries from the three malt beverages were greater than 70% for 85 of the 142 pesticides (including isomers) studied. The data showed that the different malt beverage matrixes had no significant effect on the recoveries. This method was then applied to the screening and analysis of malt beverages for pesticides, resulting in the detection of the insectide carbaryl and the fungicide dimethomorph in real samples. The study indicates that pesticide levels in malt beverages are significantly lower than the tolerance levels set by the United States Environmental Protection Agency for malt beverage starting ingredients. The use of the extraction/cleanup procedure and analysis by GC-MS(SIM) proved effective in screening malt beverages for a wide variety of pesticides. Copyright 2004 American Chemical Society

  6. Correlated relativistic dynamics and nuclear effects in dielectronic and visible spectra of highly charged ions

    International Nuclear Information System (INIS)

    Harman, Z.; Artemyev, A.N.; Crespo Lopez-Urrutia, J.R.

    2008-01-01

    Dielectronic recombination and visible emission spectra are investigated theoretically and experimentally. Spectra of x-rays emitted from electron beam ion trap plasmas allow the study of correlation and quantum electrodynamic effects in relativistic few-body systems. In the visible range, exploring the forbidden M1 transitions in Be- and B-like argon ions provides one new insights into the relativistic modelling of isotope shift effects and extend the scope of bound-electron g factor measurements to few-electron ions. (author)

  7. Simultaneous determination of arsenic and mercury species in rice by ion-pairing reversed phase chromatography with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Fang, Yong; Pan, Yushi; Li, Peng; Xue, Mei; Pei, Fei; Yang, Wenjian; Ma, Ning; Hu, Qiuhui

    2016-12-15

    An analytical method using reversed phase chromatography-inductively coupled plasma mass spectrometry for arsenic and mercury speciation analysis was described. The effect of ion-pairing reagent on simultaneous separation of four arsenic (arsenite, arsenate, monomethlyarsonate and dimethylarsinate) and three mercury species (inorganic mercury (Hg(II)), methylmecury and ethylmercury) was investigated. Parameters including concentrations and pH of the mobile phase were optimized. The separation and re-equilibration time was attained within 20min. Meanwhile, a sequential extraction method for arsenic and mercury in rice was tested. Subsequently, 1% HNO3 microwave-assisted extraction was chosen. Calibration curves based on peak area measurements were linear with correlation coefficient greater than 0.9958 for each species in the range studied. The detection limits of the species were in the range of 0.84-2.41μg/L for arsenic and 0.01-0.04μg/L for mercury, respectively. The proposed method was then successfully applied for the simultaneous determination of arsenic and mercury species in rice flour standard material and two kinds of rice from local markets. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Physicochemical properties of silica gel coated with a thin layer of polyaniline (PANI) and its application in non-suppressed ion chromatography.

    Science.gov (United States)

    Sowa, Ireneusz; Kocjan, Ryszard; Wójciak-Kosior, Magdalena; Swieboda, Ryszard; Zajdel, Dominika; Hajnos, Mieczysław

    2013-10-15

    Physicochemical properties of a new sorbent and its potential application in non-suppressed ion chromatography (IC) have been investigated. The sorbent was obtained in a process of covering silica gel particles with a film of polyaniline (PANI). The properties of silica modified with polyaniline such as particle size, porosity, average quantity of polyaniline covering carrier and density of sorbent were determined. In our study the following methods were used: microscopic analysis, laser diffraction technique, combustion analysis, mercury porosimetry and helium pycnometry. Column with the newly obtained packing was used for the separation of inorganic anions. Optimized chromatographic system was successfully employed for analysis of iodide and bromide in selected pharmaceutical products (Bochnia salt and Iwonicz salt) applied in chronic respiratory disease. Analysis was carried out using 0.1M solution of HCl in mixture of methanol/water (50:50v/v) as a mobile phase; the flow rate was 0.3 mL min(-1), temperature was 24°C and λ=210 nm. Validation parameters such as correlation coefficient, RSD values, recovery, detection and quantification limits were found to be satisfactory. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Searching for squeezed particle-antiparticle correlations in high-energy heavy-ion collisions

    International Nuclear Information System (INIS)

    Padula, Sandra S.; Socolowski, O. Jr.

    2010-01-01

    Squeezed correlations of particle-antiparticle pairs were predicted to exist if the hadron masses were modified in the hot and dense medium formed in high-energy heavy-ion collisions. Although well-established theoretically, they have not yet been observed experimentally. We suggest here a clear method to search for such a signal by analyzing the squeezed correlation functions in terms of measurable quantities. We illustrate this suggestion for simulated φφ pairs at the Relativistic Heavy Ion Collider (RHIC) energies.

  10. Determination of haloacetic acids in water by ion chromatography--method development.

    Science.gov (United States)

    Lopez-Avila, V; Liu, Y; Charan, C

    1999-01-01

    The microextraction/ion chromatographic (IC) method developed in this study involves extraction of 9 haloacetic acids (HAAs) from aqueous samples (acidified with sulfuric acid to a pH of copper sulfate pentahydrate and sodium sulfate) with methyl tert-butyl ether (MTBE), back extraction into reagent water, and analysis by IC with conductivity detection. The separation column consists of an Ion Pac AG-11 (2 mm id x 50 mm length) guard column and an Ion Pac AS-11 (2 mm id x 250 mm length) analytical column, and the concentration column is a 4 mm id x 35 mm length Dionex TAC-LP column. Use of the 2 mm id Dionex AS-11 column improved detection limits especially for trichloracetic acid (TCAA), bromodichloroacetic acid (BDCAA), dibromochloroacetic acid (DBCAA), and tribromoacetic acid (TBAA). The peak interfering with BCAA elutes at the same retention time as nitrate; however, we have not confirmed the presence of nitrate. Stability studies indicate that HAAs are stable in water for at least 8 days when preserved with ammonium chloride at 100 mg/L and stored at 4 degrees C in the dark. At day 30, recoveries were still high (e.g., 92.1-106%) for dichloroacetic acid (DCAA), BCAA, dibromoacetic acid (DBAA), trichloroacetic acid (TCAA), BDCAA, and DBCAA. However, recoveries of monochloroacetic acid (MCAA), monobromoacetic acid (MBAA), and TBAA were only 54.6, 56.8, and 66.8%, respectively. Stability studies of HAAs in H2SO4-saturated MTBE indicate that all compounds except TBAA are stable for 48 h when stored at 4 degrees C in the dark. TBAA recoveries dropped to 47.1% after 6 h of storage and no TBAA was detected after 48 h of storage. The method described here is only preliminary and was tested in only one laboratory. Additional research is needed to improve method performance.

  11. The vaporization enthalpy and vapor pressure of S (+)-methamphetamine at T = 298.15 K by correlation gas chromatography

    International Nuclear Information System (INIS)

    Thornton, Melissa; Gobble, Chase; Chickos, James

    2014-01-01

    Highlights: • The vaporization enthalpy of (d)-methamphetamine was measured. • The vapor pressure of (d)-methamphetamine as a function of temperature was evaluated. • The vapor pressure of 4-benzylpiperidine as a function of temperature was evaluated. - Abstract: The vaporization enthalpy and vapor pressure of S (+)-methamphetamine is evaluated by correlation-gas chromatography. A vaporization enthalpy of (58.7 ± 4.3) kJ · mol −1 and a vapor pressure, p = (38 ± 9) Pa has been obtained using a variety of secondary aliphatic amines as standards. In addition, equations describing the vapor pressure temperature dependence are provided for standards and S (+)-methamphetamine covering the temperature range from T = 298.15 K to the boiling temperature. Boiling temperatures are reproduced within an interval of 8 K or less

  12. On-Line Ion Exchange Liquid Chromatography as a Process Analytical Technology for Monoclonal Antibody Characterization in Continuous Bioprocessing.

    Science.gov (United States)

    Patel, Bhumit A; Pinto, Nuno D S; Gospodarek, Adrian; Kilgore, Bruce; Goswami, Kudrat; Napoli, William N; Desai, Jayesh; Heo, Jun H; Panzera, Dominick; Pollard, David; Richardson, Daisy; Brower, Mark; Richardson, Douglas D

    2017-11-07

    Combining process analytical technology (PAT) with continuous production provides a powerful tool to observe and control monoclonal antibody (mAb) fermentation and purification processes. This work demonstrates on-line liquid chromatography (on-line LC) as a PAT tool for monitoring a continuous biologics process and forced degradation studies. Specifically, this work focused on ion exchange chromatography (IEX), which is a critical separation technique to detect charge variants. Product-related impurities, including charge variants, that impact function are classified as critical quality attributes (CQAs). First, we confirmed no significant differences were observed in the charge heterogeneity profile of a mAb through both at-line and on-line sampling and that the on-line method has the ability to rapidly detect changes in protein quality over time. The robustness and versatility of the PAT methods were tested by sampling from two purification locations in a continuous mAb process. The PAT IEX methods used with on-line LC were a weak cation exchange (WCX) separation and a newly developed shorter strong cation exchange (SCX) assay. Both methods provided similar results with the distribution of percent acidic, main, and basic species remaining unchanged over a 2 week period. Second, a forced degradation study showed an increase in acidic species and a decrease in basic species when sampled on-line over 7 days. These applications further strengthen the use of on-line LC to monitor CQAs of a mAb continuously with various PAT IEX analytical methods. Implementation of on-line IEX will enable faster decision making during process development and could potentially be applied to control in biomanufacturing.

  13. Critical Evaluation of Acetylcholine Determination in Rat Brain Microdialysates using Ion-Pair Liquid Chromatography with Amperometric Detection

    Directory of Open Access Journals (Sweden)

    Yvette Michotte

    2008-08-01

    Full Text Available Liquid chromatography with amperometric detection remains the most widely used method for acetylcholine quantification in microdialysis samples. Separation of acetylcholine from choline and other matrix components on a microbore chromatographic column (1 mm internal diameter, conversion of acetylcholine in an immobilized enzyme reactor and detection of the produced hydrogen peroxide on a horseradish peroxidase redox polymer coated glassy carbon electrode, achieves sufficient sensitivity for acetylcholine quantification in rat brain microdialysates. However, a thourough validation within the concentration range required for this application has not been carried out before. Furthermore, a rapid degradation of the chromatographic columns and enzyme systems have been reported. In the present study an ion-pair liquid chromatography assay with amperometric detection was validated and its long-term stability evaluated. Working at pH 6.5 dramatically increased chromatographic stability without a loss in sensitivity compared to higher pH values. The lower limit of quantification of the method was 0.3 nM. At this concentration the repeatability was 15.7%, the inter-day precision 8.7% and the accuracy 103.6%. The chromatographic column was stable over 4 months, the immobilized enzyme reactor up to 2-3 months and the enzyme coating of the amperometric detector up to 1-2 months. The concentration of acetylcholine in 30 μl microdialysates obtained under basal conditions from the hippocampus of freely moving rats was 0.40 ± 0.12 nM (mean ± SD, n = 30. The present method is therefore suitable for acetylcholine determination in rat brain microdialysates.

  14. Boron isotope separation by ion exchange chromatography using weakly basic anion exchange resin

    International Nuclear Information System (INIS)

    Itoh, S.; Aida, M.; Okamoto, M.; Nomura, M.; Fujii, Y.

    1985-01-01

    Influences of operating temperatures and concentrations of feed boric acid solutions were examined on the above titled process over the ranges of 25 - 70 0 C and 0.1 - 1.6 mol/dm 3 (M), respectively. The ideal displacement chromatography with a very sharp-cut boundary of the boric acid adsorption band was realized at higher temperatures and lower boric acid concentrations within the experimental conditions. The isotope separation coefficient epsilon was found to decrease with increases in either temperature or the boric acid concentration. The observed values of epsilon at 25 0 C were 0.013, 0.012 and 0.011 corresponding to feed boric acid concentrations of 0.1 M, 0.4 M and 0.8 M, respectively. The epsilon's at 70 0 C were 0.0097 (0.1 M), 0.0086 (0.4 M), 0.0083 (0.8 M) and 0.0073 (1.6 M). A temperature of 40 0 C and 0.4 M of boric acid concentration was considered the optimum operating condition for the production of enriched 10 B. (author)

  15. [Determination of monosaccharides in Sargassum hemiphyllum (Turner) C. Ag. polysaccharides by ion chromatography].

    Science.gov (United States)

    Ou, Yunfu; Yin, Pinghe; Zhao, Ling

    2006-07-01

    Sargassum hemiphyllum polysaccharides (SHP) was extracted from dry Sargassum hemiphyllum (Turner) C. Ag. powder using 60 - 80 degrees C purified water and then hydrolyzed with 4.0 g/L trifluoroacetic acid at 80 degrees C. Without any derivatization reaction, the determination of monosaccharides in SHP was developed by anion-exchange chromatography with pulsed amperometric detection with an Au working electrode and an Ag/AgCl reference electrode. Monosaccharides were separated on a CarboPac PA10 anion-column (2 mm i. d. x 250 mm) by using isocratic elution consisting of 14 mmol/L sodium hydroxide at a flow rate of 0.20 mL/min. Six monosaccharides, xylose, galactose, arabinose, glucose, rhamnose and fructose, contained in SHP were separated and determined. Their contents in SHP were 2 200, 820, 98, 4 560, 358 and 740 mg/kg, respectively. The recoveries of the six monosaccharides were in the range 86.0% - 108.0%. The detection limits for these monosaccharides ranged from 5.6 to 89.6 microg/kg. The experimental results showed that SHP mainly consisted of xylose and glucose with smaller quantities of galactose, arabinose, rhamnose and fructose. This method is suitable for the determination of monosaccharides without any derivatization reaction at the level of microg/kg in dry algae with high sensitivity and good precision.

  16. 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.

  17. Use of ion chromatography for monitoring microbial spoilage in the fruit juice industry.

    Science.gov (United States)

    Trifirò, A; Saccani, G; Gherardi, S; Vicini, E; Spotti, E; Previdi, M P; Ndagijimana, M; Cavalli, S; Reschiotto, C

    1997-05-16

    Fruit juices and purees are defined as fermentable, but unfermented, products obtained by mechanical processing of fresh fruits. The presence of undesired metabolites derived from microbial growth can arise from the use of unsuitable fruit or from defects in the production line or subsequent contamination. This involves a loss in the overall quality that cannot be resolved by thermal treatment following the start of fermentation. With these considerations, together with microbiological control, the analysis of different metabolites, which can be considered as microbial growth markers, such as alcohols (i.e. ethanol, etc.), acids (i.e. acetic, fumaric, lactic, etc.) is fundamental in order to achieve a better evaluation of product quality. Enzymatic determination and other single-component analytical techniques are often used for the determination of these metabolites. When the microbial spoilage is not well known, this results in a long and cumbersome procedure. A versatile technique that is capable of determining many metabolites in one analysis could be helpful in improving routine quality control. For this purpose, an ion chromatographic technique, such as ion exclusion, for separation, and diode array spectrophotometry and conductivity, for detection, were evaluated. Both different industrial samples and inoculated samples were analyzed.

  18. Dissociative electron attachment negative ion mass spectrometry: a chlorine-specific detector for gas chromatography

    Science.gov (United States)

    Curtis, Jonathan M.; Boyd, Robert K.

    1997-11-01

    This work describes the application of negative ion chemical ionization, optimized for dissociative electron attachment (DEA), to location of unknown trace chlorinated compounds in complex gas chromatograms by selected ion recording (SIR) of m / z 35 and 37. The DEA-SIR technique is compared with other GC detectors, including the electron capture detector, electrolytic conductivity detector, the atomic emission detector and the chemical reaction interface mass spectrometry method, with respect to selectivity for chlorine, sensitivity, linear dynamic range, and general robustness and ease of use. When applied to quantitative analysis of target analytes such as polychlorobiphenyls, the DEA-SIR method has potential problems arising from the possibility of suppression effects due to abundant co-eluting components, and possible alleviating measures are discussed. In addition to these practical investigations, literature information on the fundamental physical and chemical phenomena underlying the DEA process is summarized in order to guide future work on extension to other compound types and on general improvements to the technique.

  19. Ion chromatography for determination of nitrite and nitrate in seawater using monolithic ODS columns.

    Science.gov (United States)

    Ito, Kazuaki; Takayama, Yohichi; Makabe, Nobuyuki; Mitsui, Ryo; Hirokawa, Takeshi

    2005-08-12

    A fast and highly sensitive ion chromatographic method using monolithic ODS columns was developed for the determination of nitrite (NO2-) and nitrate (NO3-) in seawater. Two monolithic ODS columns (50 mm x 4.6 mm i.d. + 100 mm x 4.6 mm i.d.) connected in series were coated and equilibrated with 5 mM cetyltrimethylammonium chloride (CTAC) aqueous solution. The column efficiency with 0.5 M NaCl as the mobile phase did not decrease in spite of the increase in flow rate of the mobile phase. Thus, good chromatograms were obtained within 3 minutes for NO2- and NO3 in artificial seawater without interferences by coexisting ions. The detection limit (S/N = 3) with UV detection at 225 nm was 0.8 and 1.6 microg/L for NO2- and NO3-, respectively. The characteristics of the monolithic CTA(+)-coated ODS columns were discussed. The present method was successfully applied to the fast and sensitive determination of NO2- and NO3- in real seawater samples.

  20. Separation of polar betalain pigments from cacti fruits of Hylocereus polyrhizus by ion-pair high-speed countercurrent chromatography.

    Science.gov (United States)

    Wybraniec, Sławomir; Stalica, Paweł; Jerz, Gerold; Klose, Bettina; Gebers, Nadine; Winterhalter, Peter; Spórna, Aneta; Szaleniec, Maciej; Mizrahi, Yosef

    2009-10-09

    Polar betacyanin pigments together with betaxanthins from ripe cactus fruits of Hylocereus polyrhizus (Cactaceae) were fractionated by means of preparative ion-pair high-speed countercurrent chromatography (IP-HSCCC) also using the elution-extrusion (EE) approach for a complete pigment recovery. HSCCC separations were operated in the classical 'head-to-tail' mode with an aqueous mobile phase. Different CCC solvent systems were evaluated in respect of influence and effectiveness of fractionation capabilities to separate the occurring pigment profile of H. polyrhizus. For that reason, the additions of two different volatile ion-pair forming perfluorinated carboxylic acids (PFCA) were investigated. For a direct comparison, five samples of Hylocereus pigment extract were run on preparative scale (900 mg) in 1-butanol-acetonitrile-aqueous TFA 0.7% (5:1:6, v/v/v) and the modified systems tert.-butyl methyl ether-1-butanol-acetonitrile-aqueous PFCA (2:2:1:5, v/v/v/v) using 0.7% and 1.0% trifluoroacetic acid (TFA) or heptafluorobutyric acid (HFBA) in the aqueous phase, respectively. The chemical affinity to the organic stationary CCC solvent phases and in consequence the retention of these highly polar betalain pigments was significantly increased by the use of the more lipophilic fluorinated ion-pair reagent HFBA instead of TFA. The HFBA additions separated more effectively the typical cacti pigments phyllocactin and hylocerenin from betanin as well as their iso-forms. Unfortunately, similar K(D) ratios and selectivity factors alpha around 1.0-1.1 in all tested solvent systems proved that the corresponding diastereomers, 15S-type pigments cannot be resolved from the 15R-epimers (iso-forms). Surprisingly, additions of the stronger ion-pair reagent (HFBA) resulted in a partial separation of hylocerenin from phyllocactin which were not resolved in the other solvent systems. The pigments were detected by means of HPLC-DAD and HPLC-electrospray ionization-MS using also

  1. 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.

  2. A novel method for selective separation of {sup 111}In from impurities by ion exchange chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yavari, R.; Khanachi, A.R.; Ghannad Maragheh, M.; Bagheri, G. [Jaber Ibn-e Hayan Research Laboratories, A.E.O.I., Tehran (Iran)

    2004-07-01

    {sup 111}In is one of the most important cyclotron-produced radionuclides that is prepared from nuclear reactions like Cd (p,xn){sup 111}In and Cd (d,xn) {sup 111}In. It is used in various branches of medicine such as lymphoscintigraphy and cisternography. Several methods have been reported in the literature for the separation of carrier-free {sup 111}In from irradiated cadmium matrix. But there has not been a sufficiently fast method for this purpose until recently. In this work, a new method has been developed for the separation of {sup 111}In from a cadmium target by using Dowex 50W-X8 as an ion exchanger. (orig.)

  3. Optimization of determination of 126Sn by ion exchange chromatography method (presentation)

    International Nuclear Information System (INIS)

    Pasteka, L.; Dulanska, S.

    2013-01-01

    The aim of the work is to optimize the uptake of tin on anion exchange resins and application of this knowledge for the analysis of samples of radioactive waste from the device of Jaslovske Bohunice and Mochovce in determining of 126 Sn. First to be optimized a method for the separation of tin on ion exchange sorbent Anion Exchange Resin (1-X8, Chloride Form) from Eichrom Technologies. Model sample was prepared in 7 mol dm -3 HCl, because in that environment a sorbent effectively captures the tin, which is bounded complexly with chloride anions as SnCl 6 2- . The radiochemical separation yield was monitored by gamma spectrometric measurements on high purity germanium detector HPGe (E = 391 keV) by adding isotope 113 Sn to each model solution. The method of tin separation was optimized on model samples.

  4. Coupling laser desorption with gas chromatography and ion mobility spectrometry for improved olive oil characterisation.

    Science.gov (United States)

    Liedtke, Sascha; Seifert, Luzia; Ahlmann, Norman; Hariharan, Chandrasekhara; Franzke, Joachim; Vautz, Wolfgang

    2018-07-30

    The investigation of volatile compounds in the headspace of liquid samples can often be used for detailed and non-destructive characterisation of the sample. This has great potential for process control or the characterisation of food samples, such as olive oil. We investigated, for the first time, the plume of substances released from olive oil droplets by laser desorption in a feasibility study and applied ion mobility spectrometry coupled to rapid GC pre-separation to enhance selectivity. Our investigation demonstrated that significantly more substances can be detected and quantified via laser desorption than in the usual headspace, enabling a rapid (5-10 min), sensitive (low ng/g range) and comprehensive analysis of the sample, with the potential for quality control and fraud identification. Therefore, laser desorption provides a useful sampling tool for characterising liquids in many applications, requiring only a few µL of sample. Copyright © 2018 Elsevier Ltd. All rights reserved.

  5. Fragmentation of toxicologically relevant drugs in positive-ion liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Niessen, W M A

    2011-01-01

    The identification of drugs and related compounds by LC-MS-MS is an important analytical challenge in several application areas, including clinical and forensic toxicology, doping control analysis, and environmental analysis. Although target-compound based analytical strategies are most frequently applied, at some point the information content of the MS-MS spectra becomes relevant. In this article, the positive-ion MS-MS spectra of a wide variety of drugs and related substances are discussed. Starting point was an MS-MS mass spectral library of toxicologically relevant compounds, available on the internet. The positive-ion MS-MS spectra of ∼570 compounds were interpreted by chemical and therapeutic class, thus involving a wide variety of drug compound classes, such benzodiazepines, beta-blockers, angiotensin-converting enzyme inhibitors, phenothiazines, dihydropyridine calcium channel blockers, diuretics, local anesthetics, vasodilators, as well as various subclasses of anti-diabetic, antidepressant, analgesic, and antihistaminic drugs. In addition, the scientific literature was searched for available MS-MS data of these compound classes and the interpretation thereof. The results of this elaborate study are presented in this article. For each individual compound class, the emphasis is on class-specific fragmentation, as discussing fragmentation of all individual compounds would take far too much space. The recognition of class-specific fragmentation may be quite informative in determining the compound class of a specific unknown, which may further help in the identification. In addition, knowledge on (class-specific) fragmentation may further help in the optimization of the selectivity in targeted analytical approaches of compounds of one particular class. Copyright © 2011 Wiley Periodicals, Inc.

  6. Coherent correlation enhancement of outer shell photoionization cross sections of alkali-like ions

    International Nuclear Information System (INIS)

    Amusia, M.Y.; Avdonina, B.; Pratt, R.H.

    1995-01-01

    An alkali-like ion interaction with inner electrons of an alkali-like ion leads to a significant increase in the photoionization cross section of the outer s electron. This occurs not only for ground-state ions with one s electron in the outer shell, but also when the outer s electron is in an excited state. The reason for this amplification, in addition to coherent enhancement in summing of the correlation amplitudes, is that the zero in the direct amplitude occurs below threshold. This leads to a constructive interference with the correlation amplitude above the photoionization threshold, in contrast to a destructive interference in the case of a neutral atom with the same electronic configuration, for which the zero occurs above threshold. Results of this research were published

  7. Potential of ion chromatography coupled to isotope ratio mass spectrometry via a liquid interface for beverages authentication.

    Science.gov (United States)

    Guyon, Francois; Gaillard, Laetitia; Brault, Audrey; Gaultier, Nicolas; Salagoïty, Marie-Hélène; Médina, Bernard

    2013-12-27

    New tools for the determination of characteristic parameters for food authentication are requested to prevent food adulteration from which health concerns, unfair competition could follow. A new coupling in the area of compound-specific carbon 13 isotope ratio (δ(13)C) analysis was developed to simultaneously quantify δ(13)C values of sugars and organic acids. The coupling of ion chromatography (IC) together with isotope ratio mass spectrometry (IRMS) can be achieved using a liquid interface allowing a chemical oxidation (co) of organic matter. Synthetic solutions containing 1 polyol (glycerol), 3 carbohydrates (sucrose, glucose and fructose) and 12 organic acids (gluconic, lactic, malic, tartaric, oxalic, fumaric, citric and isocitric) were used to optimize chromatographic conditions (concentration gradient and 3 types of column) and the studied isotopic range (-32.28 to -10.65‰) corresponds to the values found in food products. Optimum chromatographic conditions are found using an IonPac AS15, an elution flow rate of 0.3mLmin(-1) and a linear concentration gradient from 2 to 76mM (rate 21mMmin(-1)). Comparison between δ(13)C value individually obtained for each compound with the coupling IRMS and elemental analyzer, EA-IRMS, and the ones measured on the mixture of compounds by IC-co-IRMS does not reveal any isotope fractionation. Thus, under these experimental conditions, IC-co-IRMS results are accurate and reproducible. This new coupling was tested on two food matrices, an orange juice and a sweet wine. Some optimization is necessary as the concentration range between sugars and organic acids is too large: an increase in the filament intensity of the IRMS is necessary to simultaneously detect the two compound families. These first attempts confirm the good results obtained on synthetic solutions and the strong potential of the coupling IC-co-IRMS in food authentication area. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. A Facile, Nonreactive Hydrogen Peroxide (H2O2) Detection Method Enabled by Ion Chromatography with UV Detector.

    Science.gov (United States)

    Song, Mingrui; Wang, Junli; Chen, Baiyang; Wang, Lei

    2017-11-07

    Hydrogen peroxide (H 2 O 2 ) is ubiquitous in the natural environment, and it is now widely used for pollutant control in water and wastewater treatment processes. However, current analytical methods for H 2 O 2 inevitably require reactions between H 2 O 2 and other reactants to yield signals and are thus likely subjective to the interferences of coexisting colored, oxidative, and reductive compounds. In order to overcome these barriers, we herein for the first time propose to analyze H 2 O 2 by ion chromatography (IC) using an ultraviolet (UV) detector. The proposal is based on two principles: first, that H 2 O 2 can deprotonate to hydroperoxyl ion (HO 2 - ) when eluent pH is higher than the acid-dissociation coefficient of H 2 O 2 (pK a = 11.6); and second, that after separation from other compounds via IC column, H 2 O 2 can be quantified by a UV detector. Under favorable operating conditions, this method has successfully achieved acceptable recoveries (>91%) of H 2 O 2 dosed to ultrapure and natural waters, a calibration curve with R 2 > 0.99 for a wide range of H 2 O 2 concentrations from 0.1 to 50 mg/L and a method detection limit of 0.027 mg/L. In addition, this approach was shown to be capable of distinguishing H 2 O 2 from anions (e.g., fluoride and chloride) and organics (e.g., glycolate) and monochloramine, suggesting that it is insensitive to many neighboring compounds as long as they do not react quickly with H 2 O 2 . Hence, this study proves the combination of IC and UV detector a facile and reliable method for H 2 O 2 measurement.

  9. Fragment profiling of low molecular weight heparins using reversed phase ion pair liquid chromatography-electrospray mass spectrometry.

    Science.gov (United States)

    Xu, Xiaohui; Li, Daoyuan; Chi, Lequan; Du, Xuzhao; Bai, Xue; Chi, Lianli

    2015-04-30

    Low molecular weight heparins (LMWHs) are linear and highly charged carbohydrate polymers prepared by chemical or enzymatic depolymerization of heparin. Compared to unfractionated heparin (UFH), LMWHs are prevalently used as clinical anticoagulant drugs due to their lower side effects and better bioavailability. The work presented herein provides a rapid and powerful fragment mapping method for structural characterization of LMWHs. The chain fragments of two types of LMWHs, enoxaparin and nadroparin, were generated by controlled enzymatic digestion with each of heparinase I (Hep I, Enzyme Commission (EC) # 4.2.2.7), heparinase II (Hep II, no EC # assigned) and heparinase III (Hep III, EC # 4.2.2.8). Reversed phase ion pair high performance liquid chromatography (RPIP-HPLC) coupled with electrospray ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) was used to profile the oligosaccharide chains ranging from disaccharides to decasaccharides. A database containing all theoretical structural compositions was established to assist the mass spectra interpretation. The six digests derived by three enzymes from two types of LMWHs exhibited distinguishable fingerprinting patterns. And a total of 94 enoxaparin fragments and 109 nadroparin fragments were detected and identified. Besides the common LMWH oligosaccharides, many components containing characteristic LMWH structures such as saturated L-idopyranosuronic acid, 2,5-anhydro-D-mannitol, 1,6-anhydro-D-aminopyranose, as well as odd number oligosaccharides were also revealed. Quantitative comparison of major components derived from innovator and generic nadroparin products was presented. This approach to profile LMWHs' fragments offers a highly reproducible, high resolution and information-rich tool for evaluating the quality of this category of anticoagulant drugs or comparing structural similarities among samples from various sources. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. Suppression and Two-Particle Correlations of Heavy Mesons in Heavy-Ion Collisions

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Shanshan [Nuclear Science Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Qin, Guang-You [Institute of Particle Physics and Key Laboratory of Quark and Lepton Physics (MOE), Central China Normal University, Wuhan, 430079 (China); Bass, Steffen A. [Department of Physics, Duke University, Durham, NC 27708 (United States)

    2016-12-15

    We study the medium modification of heavy quarks produced in heavy-ion collisions. The evolution of heavy quarks inside the QGP is described using a modified Langevin framework that simultaneously incorporates their collisional and radiative energy loss. Within this framework, we provide good descriptions of the heavy meson suppression and predictions for the two-particle correlation functions of heavy meson pairs.

  11. The effect of correlations on the entropy and hadrochemical composition in heavy ion reactions

    International Nuclear Information System (INIS)

    Barz, H.-W.; Biro, T.S.; Lukacs, B.; Zimanyi, J.

    1987-01-01

    It is shown that spatial correlations between the constituent particles of a gas lead to roughly excluded volume type corrections in the equation of state. These corrections will appreciably change the hadrochemical composition of fireballs formed in heavy ion reactions. (author) 29 refs.; 3 figs

  12. Mean spherical model for hard ions and dipoles: Thermodynamics and correlation functions

    International Nuclear Information System (INIS)

    Vericat, F.; Blum, L.

    1980-01-01

    The solution of the mean spherical model of a mixture of equal-size hard ions and dipoles is reinvestigated. Simple expressions for the coefficients of the Laplace transform of the pair correlation function and the other thermodynamic properties are given

  13. Ion-ion correlation, solvent excluded volume and pH effects on physicochemical properties of spherical oxide nanoparticles.

    Science.gov (United States)

    Ovanesyan, Zaven; Aljzmi, Amal; Almusaynid, Manal; Khan, Asrar; Valderrama, Esteban; Nash, Kelly L; Marucho, Marcelo

    2016-01-15

    One major source of complexity in the implementation of nanoparticles in aqueous electrolytes arises from the strong influence that biological environments has on their physicochemical properties. A key parameter for understanding the molecular mechanisms governing the physicochemical properties of nanoparticles is the formation of the surface charge density. In this article, we present an efficient and accurate approach that combines a recently introduced classical solvation density functional theory for spherical electrical double layers with a surface complexation model to account for ion-ion correlation and excluded volume effects on the surface titration of spherical nanoparticles. We apply the proposed computational approach to account for the charge-regulated mechanisms on the surface chemistry of spherical silica (SiO2) nanoparticles. We analyze the effects of the nanoparticle size, as well as pH level and electrolyte concentration of the aqueous solution on the nanoparticle's surface charge density and Zeta potential. We validate our predictions for 580Å and 200Å nanoparticles immersed in acid, neutral and alkaline mono-valent aqueous electrolyte solutions against experimental data. Our results on mono-valent electrolyte show that the excluded volume and ion-ion correlations contribute significantly to the surface charge density and Zeta potential of the nanoparticle at high electrolyte concentration and pH levels, where the solvent crowding effects and electrostatic screening have shown a profound influence on the protonation/deprotonation reactions at the liquid/solute interface. The success of this approach in describing physicochemical properties of silica nanoparticles supports its broader application to study other spherical metal oxide nanoparticles. Copyright © 2015 Elsevier Inc. All rights reserved.

  14. 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.

  15. Determination of arsenic speciation in sulfidic waters by Ion Chromatography Hydride-Generation Atomic Fluorescence Spectrometry (IC-HG-AFS).

    Science.gov (United States)

    Keller, Nicole S; Stefánsson, Andri; Sigfússon, Bergur

    2014-10-01

    A method for the analysis of arsenic species in aqueous sulfide samples is presented. The method uses an ion chromatography system connected with a Hydride-Generation Atomic Fluorescence Spectrometer (IC-HG-AFS). With this method inorganic As(III) and As(V) species in water samples can be analyzed, including arsenite (HnAs(III)O3(n-3)), thioarsenite (HnAs(III)S3(n-3)), arsenate (HnAs(V)O4(n-3)), monothioarsenate (HnAs(V)SO3(n-3)), dithioarsenate (HnAs(V)S2O2(n-3)), trithioarsenate (HnAs(V)S3O(n-3)) and tetrathioarsenate (HnAs(V)S4(n-3)). The peak identification and retention times were determined based on standard analysis of the various arsenic compounds. The analytical detection limit was ~1-3 µg L(-1) (LOD), depending on the quality of the baseline. This low detection limit makes this method also applicable to discriminate between waters meeting the drinking water standard of max. 10 µg L(-1) As, and waters that do not meet this standard. The new method was successfully applied for on-site determination of arsenic species in natural sulfidic waters, in which seven species were unambiguously identified. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Characterization of Leucaena (Leucaena leucephala) oil by direct analysis in real time (DART) ion source and gas chromatography

    International Nuclear Information System (INIS)

    Alam, M.; Alandis, N.M.; Sharmin, E.; Ahmad, N.; Alrayes, B.F.; Ali, D.

    2017-01-01

    For the first time, we report the characterization of triacylglycerols and fatty acids in Leucaena (Leucaena leucephala) oil [LUCO], an unexplored nontraditional non-medicinal plant belonging to the family Fabaceae. LUCO was converted to fatty acid methyl esters (FAMEs). We analyzed the triacylglycerols (TAGs) of pure LUCO and their FAMEs by time-of-flight mass spectrometry (TOF-MS) followed by multivariate analysis for discrimination among the FAMEs. Our investigations for the analysis of LUCO samples represent noble features of glycerides. A new type of ion source, coupled with high-resolution TOF-MS was applied for the comprehensive analysis of triacylglycerols. The composition of fatty acid based LUCO oil was studied using Gas Chromatography (GC-FID). The major fatty acid components of LUCO oil are linoleic acid (52.08%) oleic acid (21.26%), palmitic acid (7.91%) and stearic acid (6.01%). A metal analysis in LUCO was done by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The structural elucidation and thermal stability of LUCO were studied by FT-IR, 1H NMR, 13C NMR spectroscopic techniques and TGA-DSC, respectively. We also measured the cytotoxicity of LUCO [es

  17. [Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography-negative chemical ion/mass spectrometry].

    Science.gov (United States)

    Xing, Yuanna; Lin, Zhihui; Feng, Anhong; Wang, Xin; Gong, Yemeng; Chen, Zeyong

    2015-02-01

    A novel method was established to determine short chain chlorinated paraffins (SC-CPs) in polyvinyl chloride (PVC) plastics by gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS). Ultrasonic extraction was used to extract SCCPs from PVC plastics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 C and with methane reagent gas at 1. 5 mL/min. This method was not influenced by medium chain chlorinated paraffins (MCCPs) in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0. 3 x 10(2)mg/kg to 3. 5 x 10(4)mg/kg. With respect to European limitation of SC-CPs (1%), four batches of samples did not comply with the European regulation, and they accounted for 33. 3%. Obviously, high SCCPs risk was presented in PVC plastics.

  18. 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

  19. 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.

  20. Simultaneous screening and confirmation of multiple classes of drug residues in fish by liquid chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Smith, Shani; Gieseker, Charles; Reimschuessel, Renate; Decker, Christie-Sue; Carson, Mary C

    2009-11-13

    LC-ion trap mass spectrometry was used to screen and confirm 38 compounds from a variety of drug classes in four species of fish: trout, salmon, catfish, and tilapia. Samples were extracted with acetonitrile and hexane. The acetonitrile phase was evaporated, redissolved in water and acetonitrile, and analyzed by gradient chromatography on a phenyl column. MS(2) or MS(3) spectra were monitored for each compound. Qualitative method performance was evaluated by the analysis over several days of replicate samples of control fish, fish fortified with a drug mixture at 1 ppm, 0.1 ppm and 0.01 ppm, and fish dosed with a representative from each drug class. Half of the 38 drugs were confirmed at 0.01 ppm, the lowest fortification level. This included all of the quinolones and fluoroquinolones, the macrolides, malachite green, and most of the imidazoles. Florfenicol amine, metronidazole, sulfonamides, tetracyclines, and most of the betalactams were confirmed at 0.1 ppm. Ivermectin and penicillin G were only detectable in the 1 ppm fortified samples. With the exception of amoxicillin, emamectin, metronidazole, and tylosin, residue presence was confirmed in all the dosed fish.

  1. Derivatization Ion Chromatography for the Determination of Monoethanolamine in Presence of Hydrazine in PHWR Steam-Water Circuits

    Directory of Open Access Journals (Sweden)

    Ayushi D.

    2011-01-01

    Full Text Available A simple, rapid and accurate method for the determination of monoethanolamine (MEA in PHWR steam-water circuits has been developed. MEA is added in the feed water to provide protection against corrosion while hydrazine is added to scavenge dissolved oxygen. The quantitative determination of MEA in presence of hydrazine was accomplished using derivatization ion chromatography with conductometric detection in nonsuppressed mode. A Metrosep cation 1-2 analytical column and a Metrosep cartridge were used for cation separation. A mixture of 4 mM tartaric acid, 20% acetone and 0.05 mM HNO3 was used as eluent. Acetone in the mobile phase leads to the formation of different derivatives with MEA and hydrazine. The interferences due Na+ and NH4 + were eliminated by adopting a simple pretreatment procedure employing OnGuard-H cartridge. The limit of detection limit of MEA was 0.1 μg mL−1 and the relative standard deviation was 2% for the overall method. The recovery of MEA added was in the range 95%–102%. The method was applied to the determination of MEA in steam generator water samples.

  2. Purification of recombinant aprotinin produced in transgenic corn seed: separation from CTI utilizing ion-exchange chromatography

    Directory of Open Access Journals (Sweden)

    A. R. Azzoni

    2005-09-01

    Full Text Available Protein expression in transgenic plants is considered one of the most promising approaches for producing pharmaceutical proteins. As has happened with other recombinant protein production schemes, the downstream processing (dsp of these proteins produced in plants is key to the technical and economic success of large-scale applications. Since dsp of proteins produced transgenically in plants has not been extensively studied, it is necessary to broaden the investigation in this field in order to more precisely evaluate the commercial feasibility of this route of expression. In this work, we studied the substitution of an IMAC chromatographic step, described in previous work (Azzoni et al., 2002, with ion-exchange chromatography on SP Sepharose Fast Flow resin as the second step in the purification of recombinant aprotinin from transgenic maize seed. The main goal of this second purification step is to separate the recombinant aprotinin from the native corn trypsin inhibitor. Analysis of the adsorption isotherms determined at 25°C under different conditions allowed selection of 0.020 M Tris pH 8.5 as the adsorption buffer. The cation-exchange chromatographic process produced a high-purity aprotinin that was more than ten times more concentrated than that generated using an IMAC step.

  3. Simple column-switching ion chromatography method for determining eight monosaccharides and oligosaccharides in honeydew and nectar.

    Science.gov (United States)

    Ni, Chengzhu; Zhu, Binhe; Wang, Nani; Wang, Muhua; Chen, Suqing; Zhang, Jiajie; Zhu, Yan

    2016-03-01

    Honeydew is excreted by aphids as a sweet waste and nectar is floral honey. Honeydew and nectar are complicated samples which consist of various sugars and amino acids. In this work, a simple ion chromatography with column-switching method was developed for the simultaneous analysis of 8 monosaccharides and oligosaccharides in honeydew and nectar. A reversed-phase column was used as a pretreatment column to eliminate organics on-line and sugars were eluted from a collection loop to analytical column by using column-switching technique. This method showed good linearity (r⩾0.9994) and afforded low limits of detection ranging from 1.55 to 10.17μgL(-1) for all the analytes. Recoveries ranged from 95% to 105% and repeatability results were acceptable with relative standard deviation of less than 3.21% (n=6). This method was successfully applied to quantification of these sugars in honeydew and nectar. These results showed honeydew had much more oligosaccharides than nectar. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. [Determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Lin, Li; Chen, Guang; Chen, Yuhong

    2011-07-01

    A method was established for the determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP/ MS). Alkaline extraction and IC-ICP/MS were applied as the sample pre-treatment method and the detection technique respectively, for iodate and iodide determination. Moreover, high-temperature pyrolysis absorption was adopted as the pre-treatment method for total iodine analysis, which finally converted all the iodine species into iodide and measured the iodide by IC-ICP/MS. The recoveries of iodine for alkaline extraction and high-temperature pyrolysis absorption were 89.6%-97.5% and 95.2%-111.2%, respectively. The results were satisfactory. The detection limit of iodine was 0.010 mg/kg. The iodine and its speciation contents in several kinds of plant samples such as seaweeds, kelp, cabbage, tea leaf and spinach were investigated. It was shown that the iodine in seaweeds mainly existed as organic iodine; while the ones in kelp, cabbage, tea leaf and spinach mainly existed as inorganic iodine.

  5. Mapping of low molecular weight heparins using reversed phase ion pair liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Daoyuan; Chi, Lequan; Jin, Lan; Xu, Xiaohui; Du, Xuzhao; Ji, Shengli; Chi, Lianli

    2014-01-01

    Low molecular weight heparins (LMWHs) are structurally complex, highly sulfated and negatively charged, linear carbohydrate polymers prepared by chemical or enzymatic depolymerization of heparin. They are widely used as anticoagulant drugs possessing better bioavailability, longer half-life, and lower side effects than heparin. Comprehensive structure characterization of LMWHs is important for drug quality assurance, generic drug application, and new drug research and development. However, fully characterization of all oligosaccharide chains in LMWHs is not feasible for current available analytical technologies due to their structure complexity and heterogeneity. Fingerprinting profiling is an efficient way for LMWHs' characterization and comparison. In this work, we present a simple, sensitive, and powerful analytical approach for structural characterization of LMWHs. Two different LMWHs, enoxaparin and nadroparin, were analyzed using reversed phase ion pair electrospray ionization mass spectrometry (RPIP-ESI-MS). More than 200 components were identified, including major structures, minor structures, and process related impurities. This approach is robust for high resolution and complementary fingerprinting analysis of LMWHs. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Dioxin analysis by gas chromatography-Fourier transform ion cyclotron resonance mass spectrometry (GC-FTICRMS).

    Science.gov (United States)

    Taguchi, Vince Y; Nieckarz, Robert J; Clement, Ray E; Krolik, Stefan; Williams, Robert

    2010-11-01

    The feasibility of utilizing a gas chromatograph-tandem quadrupole-Fourier transform ion cyclotron resonance mass spectrometer (GC-MS/MS-FTICRMS) to analyze chlorinated-dioxins/furans (CDDs/CDFs) and mixed halogenated dioxins/furans (HDDs/HDFs) was investigated by operating the system in the GC-FTICRMS mode. CDDs/CDFs and mixed HDDs/HDFs could be analyzed at 50,000 to 100,000 resolving power (RP) on the capillary gas chromatographic time scale. Initial experiments demonstrated that 1 pg of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 5 pg of 2-bromo-3,7,8-trichlorodibenzo-p-dioxin (BTrCDD) could be detected. The feasibility of utilizing an FTICRMS for screening of CDDs/CDFs, HDDs/HDFs and related compounds was also investigated by analyzing an extract from vegetation exposed to fall-out from an industrial fire. CDDs/CDFs, chlorinated pyrenes and chlorinated tetracenes could be detected from a Kendrick plot analysis of the ultrahigh resolution mass spectra. Mass accuracies were of the order of 0.5 ppm on standards with external mass calibration and 1 ppm on a sample with internal mass calibration. Copyright © 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

  7. Profiling the indole alkaloids in yohimbe bark with ultra-performance liquid chromatography coupled with ion mobility quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Sun, Jianghao; Baker, Andrew; Chen, Pei

    2011-09-30

    An ultra-performance liquid chromatography/ion mobility quadrupole time-of-flight mass spectrometry (UPLC/IM-QTOF-MS) method was developed for profiling the indole alkaloids in yohimbe bark. Many indole alkaloids with the yohimbine or ajmalicine core structure, plus methylated, oxidized and reduced species, were characterized. Common fragments and mass differences are described. It was shown that the use of IMS could provide another molecular descriptor, i.e. molecular shape by rotationally averaged collision cross-section; this is of great value for identification of constituents when reference materials are usually not available. Using the combination of high resolution (~40000) accurate mass measurement with time-aligned parallel (TAP) fragmentation, MS(E) (where E represents collision energy), ion mobility mass spectrometry (IMS) and UPLC chromatography, a total 55 indole alkaloids were characterized and a few new indole alkaloids are reported for the first time. Published in 2011 by John Wiley & Sons, Ltd.

  8. An improved method for direct estimation of free cyanide in drinking water by Ion Chromatography-Pulsed Amperometry Detection (IC-PAD) on gold working electrode.

    Science.gov (United States)

    Kumar Meher, Alok; Labhsetwar, Nitin; Bansiwal, Amit

    2018-02-01

    In the present work a fast, reliable and safe Ion Exchange Chromatography-Pulsed Amperometry Detection (IC-PAD) method for direct determination of free cyanide in drinking water has been reported. To the best of our knowledge for the first time we are reporting the application of Gold working electrode for detection of free cyanide in a chromatography system. The system shows a wide linear range up to 8000µg/L. The electrode was found to have improved sensitivity and selectivity in the presence of interfering ions. The detection limit of the system was calculated to be 2µg/L. Long term evaluation of the electrode was found to be stable. Reproducible results were obtained from analysis of drinking water samples with recoveries of 98.3-101.2% and Relative Standard Deviations (RSD) of cyanide in drinking water. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Coordinate transformation based cryo-correlative methods for electron tomography and focused ion beam milling

    International Nuclear Information System (INIS)

    Fukuda, Yoshiyuki; Schrod, Nikolas; Schaffer, Miroslava; Feng, Li Rebekah; Baumeister, Wolfgang; Lucic, Vladan

    2014-01-01

    Correlative microscopy allows imaging of the same feature over multiple length scales, combining light microscopy with high resolution information provided by electron microscopy. We demonstrate two procedures for coordinate transformation based correlative microscopy of vitrified biological samples applicable to different imaging modes. The first procedure aims at navigating cryo-electron tomography to cellular regions identified by fluorescent labels. The second procedure, allowing navigation of focused ion beam milling to fluorescently labeled molecules, is based on the introduction of an intermediate scanning electron microscopy imaging step to overcome the large difference between cryo-light microscopy and focused ion beam imaging modes. These methods make it possible to image fluorescently labeled macromolecular complexes in their natural environments by cryo-electron tomography, while minimizing exposure to the electron beam during the search for features of interest. - Highlights: • Correlative light microscopy and focused ion beam milling of vitrified samples. • Coordinate transformation based cryo-correlative method. • Improved correlative light microscopy and cryo-electron tomography

  10. Minijet thermalization and diffusion of transverse momentum correlation in high-energy heavy-ion collisions

    International Nuclear Information System (INIS)

    Pang Longgang; Wang Qun; Wang Xinnian; Xu Rong

    2010-01-01

    Transverse momentum correlations in the azimuthal angle of hadrons produced owing to minijets are first studied within the HIJING Monte Carlo model in high-energy heavy-ion collisions. Quenching of minijets during thermalization is shown to lead to significant diffusion (broadening) of the correlation. Evolution of the transverse momentum density fluctuation that gives rise to this correlation in azimuthal angle in the later stage of heavy-ion collisions is further investigated within a linearized diffusion-like equation and is shown to be determined by the shear viscosity of the evolving dense matter. This diffusion equation for the transverse momentum fluctuation is solved with initial values given by HIJING and together with the hydrodynamic equation for the bulk medium. The final transverse momentum correlation in azimuthal angle is calculated along the freeze-out hypersurface and is found to be further diffused for higher values of the shear viscosity to entropy density ratio, η/s∼0.2-0.4. Therefore the final transverse momentum correlation in azimuthal angle can be used to study the thermalization of minijets in the early stage of heavy-ion collisions and the viscous effect in the hydrodynamic evolution of strongly coupled quark-gluon plasma.

  11. Application of a simple column-switching ion chromatography technique for removal of matrix interferences and sensitive fluorescence determination of acidic compounds (pharmaceutical drugs) in complex samples.

    Science.gov (United States)

    Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Guo, Dandan; Zhao, Qiming; Wu, Shuchao; Zhu, Yan

    2017-09-15

    This work illustrates the introduction of a simple, rugged and flexible column-switching ion chromatography (IC) technique for an automated on-line QuEChERS extracted samples extracts washing followed by sensitive fluorescence (FLD) determination of five acidic pharmaceutical drugs namely; clofibric acid (CLO), ibuprofen (IBU), aspirin (ASP), naproxen (NAP) and flurobrofen (FLU) in three complex samples (spinach, apple and hospital sewage sludge). An old anion exchange column IonPac ® AS11-HC was utilized as a pre-treatment column for on-line washing of inorganic and organic interferences followed by isocratic separation of five acidic drugs with another anion exchange IonPac ® AS12A analytical column by exploiting the column-switching technique. This novel method exhibited good linearity with correlation coefficients (r 2 ) for all drugs were in the range 0.976-0.996. The limit of detection and quantification of all five acidic drugs were in the range 0.024μg/kg to 8.70μg/kg and 0.082μg/kg to 0.029mg/kg, respectively, and better recoveries in the range 81.17-112.5% with percentage relative standard deviations (RSDs) less than 17.8% were obtained. This on-line sample pre-treatment method showed minimum matrix effect in the range of 0.87-1.25 except for aspirin. This simple rugged and flexible column-switching system required only 28min for maximum elimination of matrices and interferences in three complex samples extracts, isocratic separation of five acidic drugs and for the continuous regeneration of pre-treatment column prior to every subsequent analysis. Finally, this simple automated IC system was appeared so rugged and flexible, which can eliminate and wash out most of interference, impurities and matrices in complex samples, simply by adjusting the NaOH and acetonitrile concentration in washing mobile phase with maximum recoveries of acidic analytes of interest. Copyright © 2017. Published by Elsevier B.V.

  12. Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

    OpenAIRE

    Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

    2017-01-01

    A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R) > 0.992. Low detec...

  13. Determination of soluble bromine in an extra-high-pressure mercury discharge lamp by sodium hydroxide decomposition-suppressed ion chromatography.

    Science.gov (United States)

    Mitsumata, Hiroshi; Mori, Toshio; Maeda, Tatsuo; Kita, Yoshiyuki; Kohatsu, Osamu

    2006-02-01

    We have established a simple method for assaying the quantity of soluble bromine in the discharge tubes of an extra-high-pressure mercury discharge lamp. Each discharge tube is destroyed in 5 ml of 10 mM sodium hydroxide, and the recovered sodium hydroxide solution is analyzed by suppressed-ion chromatography using gradient elution. We have clarified that this method can assay less than 1 microg of soluble bromine in a discharge tube.

  14. 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...

  15. Correlation, Breit and quantum electrodynamics effects on energy level and transition properties of W54+ ion

    International Nuclear Information System (INIS)

    Ding, X.; Sun, R.; Dong, C.; Koike, F.; Kato, D.; Murakami, I.; Sakaue, H.A.

    2017-01-01

    The electron correlation effects and Breit interaction as well as Quantum Electro-Dynamics (QED) effects were expected to have important contribution to the energy level and transition properties of heavy highly charged ions. The study of W 54+ ion provide necessary reference data for the fusion plasma physics as tungsten was chosen to be used as the armour material of the divertor of the ITER project. The ground states [Ne]3s 2 3p 6 3d 2 and first excited states [Ne]3s 2 3p 5 3d 3 of W 54+ ion have been studied by using Multi-Configuration Dirac-Fock method with the implementation of Grasp2K package. A restricted active space method was employed to investigate the correlation contribution from different models. The Breit interaction and QED effects were taken into account in the relativistic configuration interaction calculation with the converged wavefunction. It is found that the correlation contribution from 3s and 3p orbital have important contribution to the energy level, transition wavelength and probability of the ground and the first excited state of W 54+ ion. (authors)

  16. Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

    NARCIS (Netherlands)

    Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

    1998-01-01

    A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC

  17. Quantitation of 11 alkylamines in atmospheric samples: separating structural isomers by ion chromatography

    Science.gov (United States)

    Place, Bryan K.; Quilty, Aleya T.; Di Lorenzo, Robert A.; Ziegler, Susan E.; VandenBoer, Trevor C.

    2017-03-01

    Amines are important drivers in particle formation and growth, which have implications for Earth's climate. In this work, we developed an ion chromatographic (IC) method using sample cation-exchange preconcentration for separating and quantifying the nine most abundant atmospheric alkylamines (monomethylamine (MMAH+), dimethylamine (DMAH+), trimethylamine (TMAH+), monoethylamine (MEAH+), diethylamine (DEAH+), triethylamine (TEAH+), monopropylamine (MPAH+), isomonopropylamine (iMPAH+), and monobutylamine (MBAH+)) and two alkyl diamines (1, 4-diaminobutane (DABH+) and 1, 5-diaminopentane (DAPH+)). Further, the developed method separates the suite of amines from five common atmospheric inorganic cations (Na+, NH4+, K+, Mg2+, Ca2+). All 16 cations are greater than 95 % baseline resolved and elute in a runtime of 35 min. This paper describes the first successful separation of DEAH+ and TMAH+ by IC and achieves separation between three sets of structural isomers, providing specificity not possible by mass spectrometry. The method detection limits for the alkylamines are in the picogram per injection range and the method precision (±1σ) analyzed over 3 months was within 16 % for all the cations. The performance of the IC method for atmospheric application was tested with biomass-burning (BB) particle extracts collected from two forest fire plumes in Canada. In extracts of a size-resolved BB sample from an aged plume, we detected and quantified MMAH+, DMAH+, TMAH+, MEAH+, DEAH+, and TEAH+ in the presence of Na+, NH4+, and K+ at molar ratios of amine to inorganic cation ranging from 1 : 2 to 1 : 1000. Quantities of DEAH+ and DMAH+ of 0.2-200 and 3-1200 ng m-3, respectively, were present in the extracts and an unprecedented amine-to-ammonium molar ratio greater than 1 was observed in particles with diameters spanning 56-180 nm. Extracts of respirable fine-mode particles (PM2. 5) from a summer forest fire in British Columbia in 2015 were found to contain iMPAH+, TMAH+, DEAH

  18. Retention of nucleic acids in ion-pair reversed-phase high-performance liquid chromatography depends not only on base composition but also on base sequence.

    Science.gov (United States)

    Qiao, Jun-Qin; Liang, Chao; Wei, Lan-Chun; Cao, Zhao-Ming; Lian, Hong-Zhen

    2016-12-01

    The study on nucleic acid retention in ion-pair reversed-phase high-performance liquid chromatography mainly focuses on size-dependence, however, other factors influencing retention behaviors have not been comprehensively clarified up to date. In this present work, the retention behaviors of oligonucleotides and double-stranded DNAs were investigated on silica-based C 18 stationary phase by ion-pair reversed-phase high-performance liquid chromatography. It is found that the retention of oligonucleotides was influenced by base composition and base sequence as well as size, and oligonucleotides prone to self-dimerization have weaker retention than those not prone to self-dimerization but with the same base composition. However, homo-oligonucleotides are suitable for the size-dependent separation as a special case of oligonucleotides. For double-stranded DNAs, the retention is also influenced by base composition and base sequence, as well as size. This may be attributed to the interaction of exposed bases in major or minor grooves with the hydrophobic alky chains of stationary phase. In addition, no specific influence of guanine and cytosine content was confirmed on retention of double-stranded DNAs. Notably, the space effect resulted from the stereostructure of nucleic acids also influences the retention behavior in ion-pair reversed-phase high-performance liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Angular correlation of the N+ ions produced in the dissociative double ionization of nitrogen

    International Nuclear Information System (INIS)

    Ezell, R.L.; Edwards, A.K.; Wood, R.M.

    1984-01-01

    The double ionization of N 2 by He + projectiles was studied by measuring the angular correlation between the two N + ions emitted in the dissociation of N 2+ 2 molecular ions. If there were no recoil velocity imposed on the N 2+ 2 ion in the initial ionizing collision, and thermal effects were neglected, the pair of N + ions would have equal and opposite velocity vectors in the laboratory frame of reference. Measuring the coincidence yield of pairs of N + ions as a function of the angle between their velocity vectors permits an estimate to be made of the component of momentum transferred to the N 2+ 2 parent ions in the beam direction. The results presented in this report show the recoil velocity to be considerably less than the mean thermal velocity of N 2 molecules at room temperature. We also report mesurements of the relative cross section for N + production from N 2+ 2 as a function of the orientation of the N 2 target molecules relative to the projectile beam axis

  20. 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.

  1. Comparison of Gas Chromatography-Mass Spectrometry and Gas Chromatography-Tandem Mass Spectrometry with Electron Ionization and Negative-Ion Chemical Ionization for Analyses of Pesticides at Trace Levels in Atmospheric Samples

    Directory of Open Access Journals (Sweden)

    Renata Raina

    2008-01-01

    Full Text Available A comparison of detection limits of gas chromatography-mass spectrometry (GC-MS in selected ion monitoring (SIM with gas chromatography-tandem mass spectrometry (GC-MS/MS in selected reaction monitoring (SRM mode with both electron ionization (EI and negative-ion chemical ionization (NCI are presented for over 50 pesticides ranging from organochlorines (OCs, organophosphorus pesticides (OPs and pre-emergent herbicides used in the Canadian prairies (triallate, trifluralin, ethalfluralin. The developed GC-EI/SIM, GC-NCI/SIM, and GC-NCI/SRM are suitable for the determination of pesticides in air sample extracts at concentrations <100 pg µL -1 (< 100 pg m -3 in air. No one method could be used to analyze the range of pre-emergent herbicides, OPs, and OCs investigated. In general GC-NCI/SIM provided the lowest method detection limits (MDLs commonly 2.5-10 pg µL -1 along with best confirmation (<25% RSD of ion ratio, while GC-NCI/SRM is recommended for use where added selectivity or confirmation is required (such as parathion-ethyl, tokuthion, carbofenothion. GC-EI/SRM at concentration < 100 pg µL -1 was not suitable for most pesticides. GC-EI/SIM was more prone to interference issues than NCI methods, but gave good sensitivity (MDLs 1-10 pg µL -1 for pesticides with poor NCI response (OPs: sulfotep, phorate, aspon, ethion, and OCs: alachlor, aldrin, perthane, and DDE, DDD, DDT.

  2. Forging Fast Ion Conducting Nanochannels with Swift Heavy Ions: The Correlated Role of Local Electronic and Atomic Structure

    Energy Technology Data Exchange (ETDEWEB)

    Sachan, Ritesh [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Material Science and Technology Division; Cooper, Valentino R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Material Science and Technology Division; Liu, Bin [Univ. of Tennessee, Knoxville, TN (United States). Dept. of Materials Science and Engineering; Aidhy, Dilpuneet S. [Univ. of Wyoming, Laramie, WY (United States). Dept. of Mechanical Engineering; Voas, Brian K. [Iowa State Univ., Ames, IA (United States). Dept. of Materials Science and Engineering; Lang, Maik [Univ. of Tennessee, Knoxville, TN (United States). Dept. of Nuclear Engineering; Ou, Xin [Chinese Academy of Sciences (CAS), Shanghai (China). State Key Lab. of Functional Material for Informatics; Trautmann, Christina [GSI Helmholtz Centre for Heavy Ion Research, Darmstadt (Germany); Technical Univ. of Darmstadt (Germany). Dept. of Materials Science; Zhang, Yanwen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Material Science and Technology Division; Univ. of Tennessee, Knoxville, TN (United States). Dept. of Materials Science and Engineering; Chisholm, Matthew F. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Material Science and Technology Division; Weber, William J. [Univ. of Tennessee, Knoxville, TN (United States). Dept. of Materials Science and Engineering; Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Material Science and Technology Division

    2016-12-19

    Atomically disordered oxides have attracted significant attention in recent years due to the possibility of enhanced ionic conductivity. However, the correlation between atomic disorder, corresponding electronic structure, and the resulting oxygen diffusivity is not well understood. The disordered variants of the ordered pyrochlore structure in gadolinium titanate (Gd2Ti2O7) are seen as a particularly interesting prospect due to intrinsic presence of a vacant oxygen site in the unit atomic structure, which could provide a channel for fast oxygen conduction. In this paper, we provide insights into the subangstrom scale on the disordering-induced variations in the local atomic environment and its effect on the electronic structure in high-energy ion irradiation-induced disordered nanochannels, which can be utilized as pathways for fast oxygen ion transport. With the help of an atomic plane-by-plane-resolved analyses, the work shows how the presence of various types of TiOx polyhedral that exist in the amorphous and disordered crystalline phase modify the electronic structures relative to the ordered pyrochlore phase in Gd2Ti2O7. Finally, the correlated molecular dynamics simulations on the disordered structures show a remarkable enhancement in oxygen diffusivity as compared with ordered pyrochlore lattice and make that a suitable candidate for applications requiring fast oxygen conduction.

  3. Electron-electron correlation in two-photon double ionization of He-like ions

    Science.gov (United States)

    Hu, S. X.

    2018-01-01

    Electron correlation plays a crucial role in quantum many-body physics ranging from molecular bonding and strong-field-induced multielectron ionization, to superconducting in materials. Understanding the dynamic electron correlation in the photoionization of relatively simple quantum three-body systems, such as He and He-like ions, is an important step toward manipulating complex systems through photoinduced processes. Here we have performed ab initio investigations of two-photon double ionization (TPDI) of He and He-like ions (L i+,B e2 + , and C4 +) exposed to intense attosecond x-ray pulses. Results from such fully correlated quantum calculations show weaker and weaker electron correlation effects in TPDI spectra as the ionic charge increases, which is opposite to the intuition that the absolute increase of correlation in the ground state should lead to more equal energy sharing in photoionization. These findings indicate that the final-state electron-electron correlation ultimately determines the energy sharing of the two ionized electrons in TPDI.

  4. 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

  5. Femtoscopic analysis of baryon correlations in ultra-relativistic heavy-ion collisions registered by ALICE

    CERN Document Server

    AUTHOR|(INSPIRE)INSPIRE-00361630

    Heavy-ion collisions at ultra-relativistic energies give a unique possibility to create and to analyse the Quark-Gluon Plasma predicted by the theory of Quantum Chromodynamics. The research on the properties of such state of matter is crucial for understanding the features of the strongly interacting system. Experimental results reveal the collective behaviour of matter created in the heavy-ion collisions at ultra-relativistic energies. The existence of this effect can be verified by the measurement of the transverse mass dependence of the source size extracted using different particle species. Such characteristics can be determined using the analysis technique called femtoscopy. This method is based on the correlations of particles with small relative momenta which originate from the effects of Quantum Statistics as well as the strong and Coulomb Final State Interactions. A recent analysis of the particle production at the highest available collision energies of heavy-ion collisions reveals the puzzling res...

  6. Standardization of a fluconazole bioassay and correlation of results with those obtained by high-pressure liquid chromatography.

    Science.gov (United States)

    Rex, J H; Hanson, L H; Amantea, M A; Stevens, D A; Bennett, J E

    1991-01-01

    An improved bioassay for fluconazole was developed. This assay is sensitive in the clinically relevant range (2 to 40 micrograms/ml) and analyzes plasma, serum, and cerebrospinal fluid specimens; bioassay results correlate with results obtained by high-pressure liquid chromatography (HPLC). Bioassay and HPLC analyses of spiked plasma, serum, and cerebrospinal fluid samples (run as unknowns) gave good agreement with expected values. Analysis of specimens from patients gave equivalent results by both HPLC and bioassay. HPLC had a lower within-run coefficient of variation (less than 2.5% for HPLC versus less than 11% for bioassay) and a lower between-run coefficient of variation (less than 5% versus less than 12% for bioassay) and was more sensitive (lower limit of detection, 0.1 micrograms/ml [versus 2 micrograms/ml for bioassay]). The bioassay is, however, sufficiently accurate and sensitive for clinical specimens, and its relative simplicity, low sample volume requirement, and low equipment cost should make it the technique of choice for analysis of routine clinical specimens. PMID:1854166

  7. Vapor pressures and enthalpies of vaporization of a series of γ and δ-lactones by correlation gas chromatography

    International Nuclear Information System (INIS)

    Kozlovskiy, Mikhail; Gobble, Chase; Chickos, James

    2014-01-01

    Highlights: • The vaporization enthalpies of γ-octanolactone, γ- and δ-undecanolactone and γ and δ-dodecanolactone are reported. • Equations for predicting the vapor pressures over the temperature range T = (298.15 to 350) K are provided. • Vaporization enthalpies are compared to predicted values. - Abstract: The vaporization enthalpies of γ-octanolactone, γ- and δ-undecanolactone and γ and δ-dodecanolactone used commercially as flavor ingredients are reported as are their vapor pressures over the temperature range T = (298.15 to 350) K. Vaporization enthalpies at T = 298.15 K of: (66.0 ± 3.9), (79.4 ± 4.4), (80.1 ± 4.5), (83.9 ± 4.6), and (84.61 ± 4.7) kJ · mol −1 and vapor pressures also at T = 298.15 K of: (2.8 ± 0.9), (0.12 ± 0.05), (0.09 ± 0.04), (0.04 ± 0.02), and (0.03 ± 0.02) Pa, respectively, have been evaluated by correlation gas chromatography experiments. The vaporization enthalpies of the lactones studied are reproduced within ±0.5 kJ · mol −1 using a group additivity scheme reported previously for γ- and δ-lactones. The vaporization enthalpies of the γ- and δ-lactones are compared to a similar series of ω-lactones

  8. An examination of the thermodynamics of fusion, vaporization, and sublimation of several parabens by correlation gas chromatography.

    Science.gov (United States)

    Umnahanant, Patamaporn; Chickos, James

    2011-05-01

    The vaporization, fusion, and sublimation enthalpies of methyl, ethyl, propyl, and butyl paraben are reported and compared with literature values. The vaporization enthalpies were measured by correlation gas chromatography and the fusion enthalpies by differential scanning calorimetry. Adjusted to T = 298.15 K, these enthalpies were combined to yield the sublimation enthalpy. The results compare favorably to some of the literature values but do not support the reversal in magnitude of both the vaporization and sublimation enthalpy previously reported for propyl and butyl paraben. The following fusion and vaporization enthalpies were measured for methyl through to butyl paraben, respectively: ΔH(fus) (T(fus) ) 26.3 ± 0.1 (398.6 K), 26.5 ± 0.1 (388.5 K), 27.3 ± 0.1 (368.8), and 25.9 ± 0.3 (340.7 K) kJ·mol(-1); ΔH(vap) (298.15 K) 79.5 ± 0.5, 84.0 ± 0.5, 89.7 ± 0.6, and 95.8 ± 0.6 kJ·mol(-1). The results are believed to be accurate to ± 4 kJ·mol(-1). Copyright © 2011 Wiley-Liss, Inc.

  9. A study of the vaporization enthalpies of some 1-substituted imidazoles and pyrazoles by correlation-gas chromatography.

    Science.gov (United States)

    Lipkind, Dmitry; Plienrasri, Chatchawat; Chickos, James S

    2010-12-23

    The vaporization enthalpies of 1-methyl-, 1-ethyl-, 1-phenyl-, and 1-benzylimidazole, 1-methyl- and 1-phenylpyrazole, and trans-azobenzene are evaluated by correlation-gas chromatography (C-GC) using a variety of azines and diazines as standards. The vaporization enthalpies obtained by C-GC when compared to literature values are approximately 14 kJ·mol(-1) smaller for the imidazoles and 6 kJ·mol(-1) smaller for the pyrazoles. The literature vaporization enthalpies of 1-methylpyrrole and 1-methylindole, two closely related compounds with one less nitrogen, are reproduced by C-GC. These results suggest that the magnitude of the intermolecular interactions present in 1-substituted imidazoles and pyrazoles are significantly larger than the those present in the reference compounds and greater than or equal in magnitude to the enhanced intermolecular interactions observed previously in aromatic 1,2-diazines. The vaporization enthalpy and vapor pressure of a trans-1,2-diazine, trans-azobenzene, measured by C-GC using similar standards reproduced the literature values within experimental error.

  10. On line ion chromatography for the in situ characterization of the Callovo-Oxfordian pore water composition

    International Nuclear Information System (INIS)

    Lundy, M.; Vinsot, A.

    2010-01-01

    , lithium and iodide. Concerning the others species, isolated discrepancies ranging from 8 to 30% were observed. They were mainly explained by analytical uncertainties, which were then reduced with the acquisition of an ultrapure water system for the preparation of eluents and calibration solutions. Although the chromatograph could efficiently be operated by remote control, pre-programmed service interventions were necessary: calibration solutions and eluents had to be replaced every 4 weeks, and some parts (guard columns, in-line filters or peristaltic pump tubing) every 8 weeks. Dust entrance in the housing of the chromatograph provoked several releases of the fire extinguishing system which had been installed for security reasons. Various incidents occurred: high pressure eluent pumps needed to be replaced and problems with the water sampling module connection led to several stops of the measurements. Nevertheless, in spite of these incidents and constraints, the implementation of on line ion chromatography was considered to be successful in regard to the obtained results. (authors)

  11. Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry (IC-ESI-MS/MS)

    Energy Technology Data Exchange (ETDEWEB)

    El Aribi, Houssain [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., L4K 4V8 (Canada)]. E-mail: houssain.aribi@sciex.com; Le Blanc, Yves J.C. [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., L4K 4V8 (Canada); Antonsen, Stephen [Dionex Canada Ltd., 1540 Cornwall Road, Oakville, Ont., L6J 7W5 (Canada); Sakuma, Takeo [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., L4K 4V8 (Canada)

    2006-05-10

    A new IC-ESI-MS/MS method, with simple sample preparation procedure, has been developed for quantification and confirmation of perchlorate (ClO{sub 4} {sup -}) anions in water, fresh and canned food, wine and beer samples at low part-per-trillion (ng l{sup -1}) levels. To the best of our knowledge, this is the first time an analytical method is used for determination of perchlorate in wine and beer samples. The IC-ESI-MS/MS instrumentation consisted of an ICS-2500 ion chromatography (IC) system coupled to either an API 2000{sup TM} or an API 3200{sup TM} mass spectrometer. The IC-ESI-MS/MS system was optimized to monitor two pairs of precursor and fragment ion transitions, i.e., multiple reaction monitoring (MRM). All samples had oxygen-18 isotope labeled perchlorate internal standard (ISTD) added prior to extraction. Chlorine isotope ratio ({sup 35}Cl/{sup 37}Cl) was used as a confirmation tool. The transition of {sup 35}Cl{sup 16}O{sub 4} {sup -} (m/z 98.9) into {sup 35}Cl{sup 16}O{sub 3} {sup -} (m/z 82.9) was monitored for quantifying the main analyte; the transition of {sup 37}Cl{sup 16}O{sub 4} {sup -} (m/z 100.9) into {sup 37}Cl{sup 16}O{sub 3} {sup -} (m/z 84.9) was monitored for examining a proper isotopic abundance ratio of {sup 35}Cl/{sup 37}Cl; and the transition of {sup 35}Cl{sup 18}O{sub 4} {sup -} (m/z 107.0) into {sup 35}Cl{sup 18}O{sub 3} {sup -} (m/z 89.0) was monitored for quantifying the internal standard. The minimum detection limit (MDL) for this method in de-ionized water is 5 ng l{sup -1} (ppt) using the API 2000{sup TM} mass spectrometer and 0.5 ng l{sup -1} using the API 3200{sup TM} mass spectrometer. Over 350 food and beverage samples were analyzed mostly in triplicate. Except for four, all samples were found to contain measurable amounts of perchlorate. The levels found ranged from 5 ng l{sup -1} to 463.5 {+-} 6.36 {mu}g kg{sup -1} using MRM 98.9 {sup {yields}} 82.9 and 100 {mu}l injection.

  12. Determination of adsorbable organic halogens in surface water samples by combustion-microcoulometry versus combustion-ion chromatography titration.

    Science.gov (United States)

    Kinani, Aziz; Sa Lhi, Hacène; Bouchonnet, Stéphane; Kinani, Said

    2018-03-02

    Adsorbable Organic Halogen (AOX) is an analytical parameter of considerable interest since it allows to evaluate the amount of organohalogen disinfection by-products (OXBPs) present in a water sample. Halogen speciation of AOX into adsorbable organic chlorine, bromine and iodine, respectively AOCl, AOBr and AOI, is extremely important since it has been shown that iodinated and brominated organic by-products tend to be more toxic than their chlorinated analogues. Chemical speciation of AOX can be performed by combustion-ion chromatography (C-IC). In the present work, the effectiveness of the nitrate wash according to ISO 9562 standard method protocol to eliminate halide ions interferences was firstly examined. False positive AOX values were observed when chloride concentration exceeded 100 ppm. The improvements made to the washing protocol have eliminated chloride interference for concentrations up to 1000 ppm. A C-IC method for chemical speciation of AOX into AOCl, AOBr, and AOI has been developed and validated. The most important analytical parameters were investigated. The following optimal conditions were established: an aqueous solution containing 2.4 mM sodium bicarbonate/2.0 mM sodium carbonate, and 2% acetone (v/v) as mobile phase, 2 mL of aqueous sodium thiosulfate (500 ppm) as absorption solution, 0.2 mL min -1 as water inlet flow rate for hydropyrolysis, and 10 min as post-combustion time. The method was validated according to NF T90-210 standard method. Calibration curves fitted through a quadratic equation show coefficients of determination (r 2 ) greater than 0.9998, and RSD less than 5%. The LOQs were 0.9, 4.3, and 5.7 μg L -1 Cl for AOCl, AOBr, and AOI, respectively. The accuracy, in terms of relative error, was within a ± 10% interval. The applicability of the validated method was demonstrated by the analysis of twenty four water samples from three rivers in France. The measurements reveals AOX amounts above 10

  13. Fast filtration sampling protocol for mammalian suspension cells tailored for phosphometabolome profiling by capillary ion chromatography - tandem mass spectrometry.

    Science.gov (United States)

    Kvitvang, Hans F N; Bruheim, Per

    2015-08-15

    Capillary ion chromatography (capIC) is the premium separation technology for low molecular phosphometabolites and nucleotides in biological extracts. Removal of excessive amounts of salt during sample preparation stages is a prerequisite to enable high quality capIC separation in combination with reproducible and sensitive MS detection. Existing sampling protocols for mammalian cells used for GC-MS and LC-MS metabolic profiling can therefore not be directly applied to capIC separations. Here, the development of a fast filtration sampling protocol for mammalian suspension cells tailored for quantitative profiling of the phosphometabolome on capIC-MS/MS is presented. The whole procedure from sampling the culture to transfer of filter to quenching and extraction solution takes less than 10s. To prevent leakage it is critical that a low vacuum pressure is applied, and satisfactorily reproducibility was only obtained by usage of a vacuum pressure controlling device. A vacuum of 60mbar was optimal for filtration of multiple myeloma Jjn-3 cell cultures through 5μm polyvinylidene (PVDF) filters. A quick deionized water (DI-water) rinse step prior to extraction was tested, and significantly higher metabolite yields were obtained during capIC-MS/MS analyses in this extract compared to extracts prepared by saline and reduced saline (25%) washing steps only. In addition, chromatographic performance was dramatically improved. Thus, it was verified that a quick DI-water rinse is tolerated by the cells and can be included as the final stage during filtration. Over 30 metabolites were quantitated in JJN-3 cell extracts by using the optimized sampling protocol with subsequent capIC-MS/MS analysis, and up to 2 million cells can be used in a single filtration step for the chosen filter and vacuum pressure. The technical set-up is also highly advantageous for microbial metabolome filtration protocols after optimization of vacuum pressure and washing solutions, and the reduced salt

  14. Ion chromatography separation of lanthanides at trace concentrations from Gd Matrix and quantification by ICP-MS

    International Nuclear Information System (INIS)

    Raut, V.V.; Jeyakumar, S.; Nagar, B.K.; Deb, S.B.; Saxena, M.K.; Tomar, B.S.

    2014-01-01

    Gadolinium compounds are mainly used as burnable poison. The presence of certain impurities is undesirable in the nuclear grade Gd compounds. Gd 2 O 3 , a most common raw material used for the preparation of nuclear grade Gd compounds. Analysis of rare earth impurities in Gd-matrices is one of the important exercises carried out to ensure the purity of Gd 2 O 3 . Determination of lanthanides at trace concentrations in lanthanide (Gd) matrix is complicated and difficult to realize. This is because the selective separation of REE's in one of the lanthanide elements is a challenging task. The present study was carried out to explore the feasibility of separating trace level lanthanides from Gd matrix by ion interaction chromatography (IIC) and to develop an analytical methodology for the determination of lanthanides by inductively coupled plasma mass spectrometry (ICP-MS). In the present investigation, the reversed phase column was dynamically modified into sulphonic acid functionalized surface by using 0.025 M n-Octane sulphonic acid (OSA). With α-HIBA eluent system, the elution order follows as Lu to La. The separations are employed with gradient elution mode. Since the sample has large excess of Gd, elution profiles with concentration gradient of HIBA were attempted. Separated fractions of Light lanthanides (LLn) and Heavy lanthanides (HLn) were collected and analyzed by ICP-MS. During MS analysis, it was observed that due to high concentration of salt (Na salt of OSA) present in the collected fractions caused difficulty in ICP-MS . Hence the experiments were carried out using another ion interacting reagent viz. 0.03 M camphor-10-sulphonic acid (CSA). Initial concentration of HIBA was kept at 0.025 M up to 15 min for the elution of HLns i.e. from Lu to Tb and it was then increased to 0.05 M to 0.3 M in 30 min. After elution of Tb, outlet of the column was switched to drain for 7 min to separate bulk Gd fraction. From 22 to 35 min effluent fraction containing Eu

  15. Identification of phase-II metabolites of flavonoids by liquid chromatography-ion-mobility spectrometry-mass spectrometry.

    Science.gov (United States)

    Chalet, Clément; Hollebrands, Boudewijn; Janssen, Hans-Gerd; Augustijns, Patrick; Duchateau, Guus

    2018-01-01

    Flavonoids are a class of natural compounds with a broad range of potentially beneficial health properties. They are subjected to an extensive intestinal phase-II metabolism, i.e., conjugation to glucuronic acid, sulfate, and methyl groups. Flavonoids and their metabolites can interact with drug transporters and thus interfere with drug absorption, causing food-drug interactions. The site of metabolism plays a key role in the activity, but the identification of the various metabolites remains a challenge. Here, we developed an analytical method to identify the phase-II metabolites of structurally similar flavonoids. We used liquid chromatography-ion-mobility spectrometry-mass spectrometry (LC-IMS-MS) analysis to identify phase-II metabolites of flavonols, flavones, and catechins produced by HT29 cells. We showed that IMS could bring valuable structural information on the different positional isomers of the flavonols and flavones. The position of the glucuronide moiety had a strong influence on the collision cross section (CCS) of the metabolites, with only minor contribution of hydroxyl and methyl moieties. For the catechins, fragmentation data obtained from MS/MS analysis appeared more useful than IMS to determine the structure of the metabolites, mostly due to the high number of metabolites formed. Nevertheless, CCS information as a molecular fingerprint proved to be useful to identify peaks from complex mixtures. LC-IMS-MS thus appears as a valuable tool for the identification of phase-II metabolites of flavonoids. Graphical abstract Structural identification of phase-II metabolites of flavonoids using LC-IMS-MS.

  16. Analysis of haloacetic acids, bromate, and dalapon in natural waters by ion chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wu, Shimin; Anumol, Tarun; Gandhi, Jay; Snyder, Shane A

    2017-03-03

    The addition of oxidants for disinfecting water can lead to the formation of potentially carcinogenic compounds referred to as disinfection byproducts (DBPs). Haloacetic acids (HAAs) are one of the most widely detected DBPs in US water utilities and some of them are regulated by the US Environmental Protection Agency (USEPA). The present study developed a method to analyze all the compounds in the USEPA method 557 (nine HAAs, bromate and dalapon) plus four potentially more toxic iodinated HAAs in water by coupling ion chromatography with tandem mass spectrometry (IC-MS/MS). This aqueous direct injection method has significant advantages over traditional GC methods, which require a derivatization and sample extraction that are laborious, time-consuming, and can negatively impact reproducibility. The method developed in this study requires half the time of the current USEPA method 557 on IC-MS/MS while including more compounds and achieving sub-μg/L level method detection limits (MDLs) for all 15 target analytes. The single laboratory lowest concentration minimum reporting level (LCMRL) has also been determined in reagent water, which ranged from 0.011 to 0.62μg/L for the analytes. The mean recoveries of the analytes during matrix spike recovery tests were 77-125% in finished drinking water and 81-112% in surface water. This method was then applied to untreated, chlorinated, and chloraminated groundwater and surface water samples. Bromate and 9 HAAs were detected at different levels in some of these samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Quantification of trace level of fluoride content in uranium oxide produced by deconversion of HEX gas by ion chromatography

    International Nuclear Information System (INIS)

    Unnikrishnan, E.K.; Padmakumar, P.R.; Shanmugavelu, P.; Sudhakar, T.M.; Bhowmik, A.

    2015-01-01

    Fluoride content in nuclear fuel is detrimental due to its corrosion behavior with cladding material. It is essential to monitor and control the fluoride concentration in nuclear material at various processing stages. Deconversion of upgraded HEX gas is carried out to produce uranium oxide. The performance of the deconversion process of HEX gas is evaluated for which trace level of fluoride concentration accompanying uranium oxide is considered as a marker. An analytical method has been developed for testing the uranium oxide produced from deconversion process of HEX gas. The method involves sample pretreatment followed by analysis using ion chromatography. The test method was validated for its performance using in house synthetic uranyl fluoride (UO 2 F 2 ) standard solutions prepared with different level of fluoride content. The results are in agreement with the expected values with the recovery in the range of 80-95%. This method has been successfully implemented for routine analysis of samples at our lab. Since UO 2 F 2 reference material is not available to validate this method, in house UO 2 F 2 standards were prepared from U 3 O 8 prepared from nuclear grade uranyl nitrate solution. UO 2 F 2 standards were prepared by converting U 3 O 8 to UO 2 F 2 by the addition of HF followed by H 2 O 2 at 200°C on a hot plate. The entire yellow colored UO 2 F 2 was dissolved in nano pure water and recrystallised several times to ensure that all free HF is removed. The crystals dried in air oven at 120° for three hours. Samples containing 1000 mg kg -1 fluoride prepared from this UO 2 F 2 , and subsequently from this sample containing 5 mg kg -1 to 35 mg kg -1 fluoride samples were prepared and analysed against fluoride CRM and the fluoride concentration obtained was analysed

  18. Analysis of a variety of inorganic and organic additives in food products by ion-pairing liquid chromatography coupled to high-resolution mass spectrometry.

    Science.gov (United States)

    Kaufmann, Anton; Widmer, Mirjam; Maden, Kathryn; Butcher, Patrick; Walker, Stephan

    2018-03-05

    A reversed-phase ion-pairing chromatographic method was developed for the detection and quantification of inorganic and organic anionic food additives. A single-stage high-resolution mass spectrometer (orbitrap ion trap, Orbitrap) was used to detect the accurate masses of the unfragmented analyte ions. The developed ion-pairing chromatography method was based on a dibutylamine/hexafluoro-2-propanol buffer. Dibutylamine can be charged to serve as a chromatographic ion-pairing agent. This ensures sufficient retention of inorganic and organic anions. Yet, unlike quaternary amines, it can be de-charged in the electrospray to prevent the formation of neutral analyte ion-pairing agent adducts. This process is significantly facilitated by the added hexafluoro-2-propanol. This approach permits the sensitive detection and quantification of additives like nitrate and mono-, di-, and triphosphate as well as citric acid, a number of artificial sweeteners like cyclamate and aspartame, flavor enhancers like glutamate, and preservatives like sorbic acid. This is a major advantage, since the currently used analytical methods as utilized in food safety laboratories are only capable in monitoring a few compounds or a particular category of food additives. Graphical abstract Deptotonation of ion pair agent in the electrospray interface.

  19. Plan of measurement experiment of correlation between ion beam and plasma

    Energy Technology Data Exchange (ETDEWEB)

    Oguri, Yoshiyuki; Abe, Satoru; Sakumi, Akira; Okazaki, Hisashi; Watanabe, Takeshi [Tokyo Inst. of Tech. (Japan). Research Lab. for Nuclear Reactors

    1996-12-01

    The Research Laboratory, for Nuclear Reactors, Tokyo Institute of Technology has conducted experimental study on accelerating structure and beam behavior of high intensity heavy ion accelerator for a beam driver and its computer simulation study as a circle of fundamental study of the heavy ion inertial nuclear fusion. From last fiscal year, a preliminary study for measuring the correlation between beam and plasma using low speed heavy ion beam from 1.7 MV tandem accelerator was begun. As a result, a possibility of forming a plasma target with above 10 (exp 17)/cu cm in free electron density and about 100 ns in life possible to supply to measurement of the correlation between beam and plasma was obtained by formation of laser plasma target and development of diagnostic measurement system. According to the preliminary calculation, it is expected to be larger charging state of ion passing through plasma than that in normal temperature target, and stoppability is presumed to increase largely and to apply to electron stopper for accelerator. And, a plan of time resolution measurement of energy loss of beam passed through plasma target using magnetic field type spectrometer and high speed plastic scintillator is also preceeding. (G.K.)

  20. Bose-Einstein correlations between hard photons produced in heavy ions collisions

    International Nuclear Information System (INIS)

    Marques Moreno, F.M.

    1994-06-01

    Heavy-ion collisions offer the unique possibility to create in the laboratory nuclear matter far from equilibrium. The electromagnetic probe constituted by hard photons and the Bose-Einstein correlations were used to study the properties of such a matter (size, density, temperature...). It is shown how the formalism has evolved from Young experiments to heavy-ion collisions experiments. The experiments performed with the photon multidetector TAPS at Ganil are described. The systems studied are: 86 KR + nat Ni at 60.0 A.MeV, and 181 Ta + 197 Au at 39.5 A.MeV. Results are presented concerning the production of gamma, pi 0 , e +- and γγ correlation. The results are interpreted with the help of static and dynamic calculations describing hard photon production in heavy ion collisions. For the first time in Nuclear Physics, the existence of the Bose-Einstein effect for photons in the range of gamma is demonstrated, and the existence of two different photon sources is postulated, reflecting the density oscillations taking place in the nuclear matter created in heavy-ion collisions. (from author) 55 figs., 22 tabs., 76 refs

  1. Jets and Jet-like Correlations in Heavy Ion and p+p Collisions at PHENIX

    International Nuclear Information System (INIS)

    2010-01-01

    Jets from heavy ion collisions provide a measurement of the medium-induced parton energy loss and the in-medium fragmentation properties. The medium modification effects are determined by comparing to a p+p baseline measurement, but the high multiplicity background in a heavy ion collision inhibits the direct application of traditional jet reconstruction techniques and novel approaches are needed to deal with this environment. Alternatively, angular correlations between the hadronic fragments of energetic partons can be used to understand the hot dense matter produced in relativistic heavy ion collisions. The yield and shape modifications of the away side peaks as function of transverse momentum compared to p+p has been interpreted as a medium response to parton energy loss. Direct photon-hadron correlations are another excellent channel to study jets from heavy ion collisions. Photons do not interact strongly with the medium and thus the photon approximately balances the momentum of the opposing jet, allowing the measurement of the effective modification to the fragmentation function through jet energy loss in the medium.

  2. Vapor pressures and vaporization enthalpy of (−) α-bisabolol and (dl) menthol by correlation gas chromatography

    International Nuclear Information System (INIS)

    Keating, Leasa; Harris, Harold H.; Chickos, James S.

    2017-01-01

    Highlights: • The vaporization enthalpy and vapor pressure of (−) α-bisabolol and (dl)-menthol have been measured as a function of temperature. • Vapor pressures, vaporization enthalpies and boiling temperatures have been compared to available literature data. • Vapor pressures of (l)-menthol are compared to (dl)-menthol. - Abstract: The vapor pressures and vaporization enthalpies of (−) α-bisabolol and (dl)-menthol, two GRAS chemicals (generally recognized as safe) are evaluated by correlation gas chromatography using a series of saturated primary alcohols as standards. Vaporization enthalpies of (96.6 ± 2.4) and (74.2 ± 2.8) kJ mol −1 and vapor pressures of p/Pa = (0.020 ± 0.003) and (4.5 ± 0.44) were evaluated at T = 298.15 K for (−) α-bisabolol and (dl)-menthol, respectively, and compared to literature values. The vapor pressures of both compounds from T = (298.15 to 500) K have been derived from correlations using vapor pressures of a series of 1-alkanols and corresponding gas chromatographic retention times at 10 K intervals. The results were fit to a second order polynomial. Calculated normal boiling temperatures of T B = (574.8 and 492.7) K are calculated for (−) α-bisabolol and (dl)-menthol, respectively. A normal boiling temperature of T B = (485.2, and 489.7) K has previously been reported for (dl)-menthol. Vapor pressures for both (l)-menthol and (dl)-menthol from a previous study and (dl)-menthol from this study are compared with literature values.

  3. Simultaneous quantification of amino acids and Amadori products in foods through ion-pairing liquid chromatography-high-resolution mass spectrometry.

    Science.gov (United States)

    Troise, Antonio Dario; Fiore, Alberto; Roviello, Giovanni; Monti, Simona Maria; Fogliano, Vincenzo

    2015-01-01

    The formation of the Amadori products (APs) is the first key step of Maillard reaction. Only few papers have dealt with simultaneous quantitation of amino acids and corresponding APs (1-amino-1-deoxy-2-ketose). Chromatographic separation of APs is affected by several drawbacks mainly related to their poor retention in conventional reversed phase separation. In this paper, a method for the simultaneous quantification of amino acids and their respective APs was developed combining high-resolution mass spectrometry with ion-pairing liquid chromatography. The limit of detection was 0.1 ng/mL for tryptophan, valine and arginine, while the limit of quantification ranged from 2 to 5 ng/mL according to the specific sensitivity of each analyte. The relative standard deviation % was lower than 10 % and the coefficient of correlation was higher than 0.99 for each calibration curve. The method was applied to milk, milk-based products, raw and processed tomato. Among the analyzed products, the most abundant amino acid was glutamic acid (16,646.89 ± 1,385.40 µg/g) and the most abundant AP was fructosyl-arginine in tomato puree (774.82 ± 10.01 µg/g). The easiness of sample preparation coupled to the analytical performances of the proposed method introduced the possibility to use the pattern of free amino acids and corresponding APs in the evaluation of the quality of raw food as well as the extent of thermal treatments in different food products.

  4. Simple determination of betaine, l-carnitine and choline in human urine using self-packed column and column-switching ion chromatography with nonsuppressed conductivity detection.

    Science.gov (United States)

    Wei, Dan; Zhu, Yan; Guo, Ming

    2018-02-01

    A sequential online extraction, clean-up and separation system for the determination of betaine, l-carnitine and choline in human urine using column-switching ion chromatography with nonsuppressed conductivity detection was developed in this work. A self-packed pretreatment column (50 × 4.6 mm, i.d.) was used for the extraction and clean-up of betaine, l-carnitine and choline. The separation was achieved using self-packed cationic exchange column (150 × 4.6 mm, i.d.), followed by nonsuppressed conductivity detection. Under optimized experimental conditions, the developed method presented good analytical performance, with excellent linearity in the range of 0.60-100 μg mL -1 for betaine, 0.75-100 μg mL -1 for l-carnitine and 0.50-100 μg mL -1 for choline, with all correlation coefficients (R 2 ) >0.99 in urine. The limits of detection were 0.15 μg mL -1 for betaine, 0.20 μg mL -1 for l-carnitine and 0.09 μg mL -1 for choline. The intra- and inter-day accuracy and precision for all quality controls were within ±10.32 and ±9.05%, respectively. Satisfactory recovery was observed between 92.8 and 102.0%. The validated method was successfully applied to the detection of urinary samples from 10 healthy people. The values detected in human urine using the proposed method showed good agreement with the measurement reported previously. Copyright © 2017 John Wiley & Sons, Ltd.

  5. Separation and determination of carbohydrates in drinks by ion chromatography with a self-regenerating suppressor and an evaporative light-scattering detector.

    Science.gov (United States)

    Li, Jing; Chen, Meilan; Zhu, Yan

    2007-06-29

    Analysis of glucose and other carbohydrates are often performed by use of normal phase HPLC methods with acetonitrile as major eluent coupled with evaporative light-scattering detector (ELSD) or by use of anion-exchange ion chromatography (IC) methods with NaOH as eluent coupled with pulsed amperimetric electrochemical detector. In this work, a novel method for the determination of carbohydrates by IC in conjunction with a self-regenerating suppressor and an ELSD detector was investigated. Three carbohydrates (glucose, fructose, and sucrose) were separated using a KOH eluent generator to avoid the effect of carbon dioxide absorption in the alkaline eluent. Due to the use of the suppressor, non-volatile components were removed and a low salt background (K+ approximately 0.070 microg/mL) can be obtained so the suppressed eluent could directly go into an ELSD detector without obvious interference of inorganic salts. After examining the changes in retention and resolution, an optimized method was established (for IC: using 32 mM KOH as the eluent at a flow rate of 1 mL/min; for ELSD: operated at 95 degrees C, 4.0 bar nitrogen with a gas flow rate of 2.0 L/min) and the linearity, reproducibility, and the limit of detection (LOD) for the three carbohydrates were further evaluated. Regression equations revealed acceptable linearity (correlation coefficients=0.994-0.998) across the working-standard range (100-1000 microg/mL for glucose and sucrose, 150-1000 microg/mL for fructose) and LODs of glucose, fructose, and sucrose were 93, 126, and 90 microg/mL, respectively. This method has successfully been applied to the determination of the three carbohydrates in carbonated cola drinks and fruit juices. The recoveries were between 95 and 113% (n=3) for different carbohydrates.

  6. 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

  7. Positron annihilation and perturbed angular correlation studies of defects in neutron and heavy ion irradiated Si

    International Nuclear Information System (INIS)

    Zhu Shenyun; Li Anli; Li Donghong; Huang Hanchen; Zheng Shengnan; Du Hongshan; Ding Honglin; Gou Zhenhui; Iwata, T.

    1995-01-01

    The positron annihilation and perturbed angular correlation methods have been used to study the radiation damage induced defects in Si irradiated by the fast neutrons of 1.45x10 20 /cm 2 and the 178 W heavy ions of 5x10 11 /cm 2 . The divacancies, quadrivacancies and different types of monovacancy-, divacancy- and quadrivacancy-oxygen complexes were observed. The results obtained by both methods are consistent. (orig.)

  8. Pseudoclassical approach to electron and ion density correlations in simple liquid metals

    International Nuclear Information System (INIS)

    Vericat, F.; Tosi, M.P.; Pastore, G.

    1986-04-01

    Electron-electron and electron-ion structural correlations in simple liquid metals are treated by using effective pair potentials to incorporate quantal effects into a pseudoclassical description of the electron fluid. An effective pair potential between simultaneous electron density fluctuations is first constructed from known properties of the degenerate jellium model, which are the plasmon sum rule, the Kimball-Niklasson relation and Yasuhara's values of the electron pair distribution function at contact. An analytic expression is thereby obtained in the Debye-Hueckel approximation for the electronic structure factor in jellium over a range of density appropriate to metals, with results which compare favourably with those of fully quantal evaluations. A simple pseudoclassical model is then set up for a liquid metal: this involves a model of charged hard spheres for the ion-ion potential and an empty core model for the electron-ion potential, the Coulombic tails being scaled as required by the relation between the long-wavelength partial structure factors and the isothermal compressibility of the metal. The model is solved analytically by a pseudoclassical linear response treatment of the electron-ion coupling and numerical results are reported for partial structure factors in liquid sodium and liquid beryllium. Contact is made for the latter system with data on the electron-electron structure factor in the crystal from inelastic X-ray scattering experiments of Eisenberger, Marra and Brown. (author)

  9. Correlated double electron capture in slow, highly charged ion-atom collisions

    Energy Technology Data Exchange (ETDEWEB)

    Stolterfoht, N.; Havener, C.C.; Phaneuf, R.A.; Swenson, J.K.; Shafroth, S.M.; Meyer, F.W.

    1986-01-01

    Recent measurements of autoionization electrons produced in slow, highly charged ion-atom collisions are reviewed. Mechanisms for double electron capture into equivalent and nonequivalent configurations are analyzed by comparing the probabilities for the creation of L/sub 1/L/sub 23/X Coster Kronig electrons and L-Auger electrons. It is shown that the production of the Coster-Kronig electrons is due to electron correlation effects whose analysis leads beyond the independent-particle model. The importance of correlation effects on different capture mechanisms is discussed. 28 refs., 6 figs.

  10. Correlated double electron capture in slow, highly charged ion-atom collisions

    International Nuclear Information System (INIS)

    Stolterfoht, N.; Havener, C.C.; Phaneuf, R.A.; Swenson, J.K.; Shafroth, S.M.; Meyer, F.W.

    1986-01-01

    Recent measurements of autoionization electrons produced in slow, highly charged ion-atom collisions are reviewed. Mechanisms for double electron capture into equivalent and nonequivalent configurations are analyzed by comparing the probabilities for the creation of L 1 L 23 X Coster Kronig electrons and L-Auger electrons. It is shown that the production of the Coster-Kronig electrons is due to electron correlation effects whose analysis leads beyond the independent-particle model. The importance of correlation effects on different capture mechanisms is discussed. 28 refs., 6 figs

  11. Azimuthal correlations of pions in relativistic heavy ion collisions at 1 GeV/nucl

    International Nuclear Information System (INIS)

    Bass, S.A.; Hartnack, C.; Nantes Univ., 44; Stoecker, H.; Greiner, W.

    1995-01-01

    Triple differential cross sections of pions in heavy ion collisions at 1 GeV/nucl. are studied with the IQMD model. After discussing general properties of Δ resonance and pion production we focus an azimuthal correlations: At projectile- and target-rapidities we observe an anticorrelation in the in-plane transverse momentum between pions and protons. At c.m.-rapidity, however, we find that high p t pions are being preferentially emitted perpendicular to the event-plane. We investigate the causes of those correlations and their sensitivity on the density and momentum dependence of the real and imaginary part of the nucleon and pion optical potential. (orig.)

  12. Identification of mechanisms in heavy ion reactions by measurement of angular correlations

    International Nuclear Information System (INIS)

    Carlin Filho, N.

    1987-01-01

    The identification of reaction mechanisms in light heavy-ion collisions has been performed within the framework of the three body kinematics, by means of angular correlation measurements. The 16 O+ 27 Al, 16 +O+ 28 Si and 10 B+ 27 Al reactions were investigated at Laboratory bombarding energies of 64 MeV, 64 and 48 MeV, respectively. Contributions of transfer-reemission and projectile sequential decay mechanisms were identified by the analysis of the relative kinetic energy of the final state components, excitation energies of the system at the intermediate stages, and also by means of fits to theoretical predictions for the angular correlations. (author) [pt

  13. Backscattering/transmission of 2 MeV He{sup ++} ions quantitative correlation study

    Energy Technology Data Exchange (ETDEWEB)

    Berec, V., E-mail: bervesn@gmail.com [Institute of Nuclear Sciences Vinca, University of Belgrade, P.O. Box 522, 11001 Belgrade (Serbia); Germogli, G.; Mazzolari, A.; Guidi, V. [INFN Sezione di Ferrara and Dipartimento di Fisica e Scienze della Terra, Via Saragat 1, 44100 Ferrara (Italy); De Salvador, D. [Dipartimento di Fisica, Università di Padova, Via Marzolo n.8, 35131 Padova (Italy); INFN Laboratori Nazionali di Legnaro, Viale Università 2, 35020 Legnaro, PD (Italy); Bacci, L. [INFN Laboratori Nazionali di Legnaro, Viale Università 2, 35020 Legnaro, PD (Italy)

    2015-07-15

    In this work we report on detailed findings of planar channeling oscillations of 2 MeV He{sup ++} particles in (1 1 0) silicon crystal. The exact correlation and coherence mechanism between confined particles oscillating trajectories are analyzed theoretically and experimentally in backscattering/transmission geometry. Regular patterns of channeled He{sup ++} ion planar oscillations are shown to be dominated by the crystal harmonic-oscillator potential and multiple scattering effect. For the first time it was shown that under the planar channeling conditions trajectories of positively charged particles exhibit observable correlation dynamics, including the interference effect. Quantitative estimation of channeling efficiency is performed using path integral method.

  14. 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)

  15. Simultaneous quantification of porcine myocardial adenine nucleotides and creatine phosphate by ion-pair reverse-phase high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Cordis, G.A.; Das, D.K.

    1987-01-01

    In order to follow the energy metabolism and the levels of high-energy phosphate compounds in porcine myocardium subjected to ischemic insult, it was necessary to develop a high-performance liquid chromatography (HPLC) method where creatine phosphate (CP) and the adenine nucleotides could be measured simultaneously in a single run. Currently available ion-pair reverse-phase HPLC methods require a separate injection with a change in wavelength and mobile phase in order to measure the creatine phosphate, while baseline separation of AMP is lacking. The ion-exchange HPLC method includes a simultaneous determination, but the baseline drifts due to the gradient and baseline separation of AMP is not achieved. In the following ion-pair reverse-phase HPLC method, simultaneous measurements of porcine myocardial adenine nucleotides and creatine phosphate were achieved along with a stable baseline and homogeneous baseline separation of each measured compound, allowing accurate quantification

  16. Correlation potential of a test ion near a strongly charged plate.

    Science.gov (United States)

    Lu, Bing-Sui; Xing, Xiangjun

    2014-03-01

    We analytically calculate the correlation potential of a test ion near a strongly charged plate inside a dilute m:-n electrolyte. We do this by calculating the electrostatic Green's function in the presence of a nonlinear background potential, the latter having been obtained using the nonlinear Poisson-Boltzmann theory. We consider the general case where the dielectric constants of the plate and the electrolyte are distinct. The following generic results emerge from our analyses: (1) If the distance to the plate Δz is much larger than a Gouy-Chapman length, the plate surface will behave effectively as an infinitely charged surface, and the dielectric constant of the plate effectively plays no role. (2) If Δz is larger than a Gouy-Chapman length but shorter than a Debye length, the correlation potential can be interpreted in terms of an image charge that is three times larger than the source charge. This behavior is independent of the valences of the ions. (3) The Green's function vanishes inside the plate if the surface charge density is infinitely large; hence the electrostatic potential is constant there. In this respect, a strongly charged plate behaves like a conductor plate. (4) If Δz is smaller than a Gouy-Chapman length, the correlation potential is dominated by the conventional image charge due to the dielectric discontinuity at the interface. (5) If Δz is larger than a Debye length, the leading order behavior of the correlation potential will depend on the valences of the ions in the electrolyte. Furthermore, inside an asymmetric electrolyte, the correlation potential is singly screened, i.e., it undergoes exponential decay with a decay width equal to the Debye length.

  17. Simultaneous ionization and analysis of 84 anabolic androgenic steroids in human urine using liquid chromatography-silver ion coordination ionspray/triple-quadrupole mass spectrometry.

    Science.gov (United States)

    Kim, So-Hee; Cha, Eun-Ju; Lee, Kang Mi; Kim, Ho Jun; Kwon, Oh-Seung; Lee, Jaeick

    2014-01-01

    Metal ion coordination ionspray (M(+) CIS) ionization is a powerful technique to enhance ionization efficiency and sensitivity. In this study, we developed and validated an analytical method for simultaneous ionization and analysis of 84 anabolic androgenic steroids (65 exogenous and 19 endogenous) using liquid chromatography-silver ion coordination ionspray/triple-quadrupole mass spectrometry (LC-Ag(+) CIS/MS/MS). The concentrations of silver ions and organic solvents have been optimized to increase the amount of silver ion coordinated complexes. A combination of 25 μM of silver ions and methanol showed the best sensitivity. The validation results showed the intra- (0.8-9.2%) and inter-day (2.5-14.9%) precisions, limits of detection (0.0005-5.0 ng/mL), and matrix effect (71.8-100.3%) for the screening analysis. No significant ion suppression was observed. In addition, this method was successfully applied to analysis of positive samples from suspected abusers and useful for the detection of the trace levels of anabolic steroids in human urine samples. Copyright © 2014 John Wiley & Sons, Ltd.

  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. An examination of the thermodynamics of fusion, vaporization, and sublimation of ibuprofen and naproxen by correlation gas chromatography.

    Science.gov (United States)

    Maxwell, Rachel; Chickos, James

    2012-02-01

    The vaporization enthalpies of (S)-ibuprofen and (S)-naproxen measured by correlation gas chromatography at T = 298.15 K are reported and compared with literature values. Adjustment of the fusion enthalpies of (RS)- and (S)-ibuprofen and (S)-naproxen to T = 298.15 K and combined with the vaporization enthalpy of the (S)-enantiomer of both ibuprofen and naproxen also at T = 298.15 K resulted in the sublimation enthalpies of both (S)-enantiomers. On the assumption that the vaporization enthalpy of the racemic form of ibuprofen is within the experimental uncertainty of the chiral form, the sublimation enthalpy of racemic ibuprofen was also evaluated. The vaporization and sublimation enthalpies compare favorably to the most of the literature values for the racemic form of ibuprofen but differ from the value reported for chiral ibuprofen. The literature values of (S)-naproxen are somewhat smaller than the values measured in this work. The following vaporization enthalpies were measured for (S)-ibuprofen and (S)-naproxen, respectively: ΔH(vap) (298.15 K), 106.0 ± 5.5, 132.2 ± 5.0 kJ·mol(-1) . Sublimation enthalpies of 122.7 ± 5.6 and 155.2 ± 7.1 kJ·mol(-1) were calculated for the (S)-enantiomers of ibuprofen and naproxen and a value of 128.9 ± 5.8 kJ·mol(-1) was estimated for the racemic form of ibuprofen. Copyright © 2011 Wiley Periodicals, Inc.

  20. Isospin and isospin / strangeness correlations in relativistic heavy-ion collisions

    Energy Technology Data Exchange (ETDEWEB)

    Mekjian, A. [Rutgers Univ., Dept. of Physics and Astronomy, NJ (United States); California Institute of Technology, Kellogg Radiation Lab 106-38 - Pasadena, CA (United States)

    2007-10-15

    A fundamental symmetry of nuclear and particle physics is isospin whose third component is the Gell-Mann/Nishijima expression I{sub Z} = Q-(B+S)/2. The role of isospin symmetry in relativistic heavy-ion collisions is studied. An isospin I{sub Z}, strangeness S correlation is shown to be a direct and simple measure of flavor correlations, vanishing in a Q{sub g} phase of uncorrelated flavors in both symmetric N = Z and asymmetric N {ne} Z systems. By contrast, in a hadron phase, a I{sub Z}/S correlation exists as long as the electrostatic charge chemical potential {mu}{sub q} {ne} 0 as in N {ne} Z asymmetric systems. A parallel is drawn with a Zeeman effect which breaks a spin degeneracy. (authors)

  1. Correlative Raman spectroscopy and focused ion beam for targeted phase boundary analysis of titania polymorphs

    Energy Technology Data Exchange (ETDEWEB)

    Mangum, John S.; Chan, Lisa H.; Schmidt, Ute; Garten, Lauren M.; Ginley, David S.; Gorman, Brian P.

    2018-05-01

    Site-specific preparation of specimens using focused ion beam instruments for transmission electron microscopy is at the forefront of targeting regions of interest for nanoscale characterization. Typical methods of pinpointing desired features include electron backscatter diffraction for differentiating crystal structures and energy-dispersive X-Ray spectroscopy for probing compositional variations. Yet there are situations, notably in the titanium dioxide system, where these techniques can fail. Differentiating between the brookite and anatase polymorphs of titania is either excessively laborious or impossible with the aforementioned techniques. However, due to differences in bonding structure, Raman spectroscopy serves as an ideal candidate for polymorph differentiation. In this work, a correlative approach utilizing Raman spectroscopy for targeted focused ion beam specimen preparation was employed. Dark field imaging and diffraction in the transmission electron microscope confirmed the region of interest located via Raman spectroscopy and demonstrated the validity of this new method. Correlative Raman spectroscopy, scanning electron microscopy, and focused ion beam is shown to be a promising new technique for identifying site-specific preparation of nanoscale specimens in cases where conventional approaches do not suffice.

  2. An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

    NARCIS (Netherlands)

    Peters, S.; Kaal, E.; Horsting, I.; Janssen, H.-G.

    2012-01-01

    A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing ‘Micro-extraction in packed sorbent’ (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve

  3. Application of an online ion-chromatography-based instrument for gradient flux measurements of speciated nitrogen and sulfur

    Science.gov (United States)

    Rumsey, Ian C.; Walker, John T.

    2016-06-01

    The dry component of total nitrogen and sulfur atmospheric deposition remains uncertain. The lack of measurements of sufficient chemical speciation and temporal extent make it difficult to develop accurate mass budgets and sufficient process level detail is not available to improve current air-surface exchange models. Over the past decade, significant advances have been made in the development of continuous air sampling measurement techniques, resulting with instruments of sufficient sensitivity and temporal resolution to directly quantify air-surface exchange of nitrogen and sulfur compounds. However, their applicability is generally restricted to only one or a few of the compounds within the deposition budget. Here, the performance of the Monitor for AeRosols and GAses in ambient air (MARGA 2S), a commercially available online ion-chromatography-based analyzer is characterized for the first time as applied for air-surface exchange measurements of HNO3, NH3, NH4+, NO3-, SO2 and SO42-. Analytical accuracy and precision are assessed under field conditions. Chemical concentrations gradient precision are determined at the same sampling site. Flux uncertainty measured by the aerodynamic gradient method is determined for a representative 3-week period in fall 2012 over a grass field. Analytical precision and chemical concentration gradient precision were found to compare favorably in comparison to previous studies. During the 3-week period, percentages of hourly chemical concentration gradients greater than the corresponding chemical concentration gradient detection limit were 86, 42, 82, 73, 74 and 69 % for NH3, NH4+, HNO3, NO3-, SO2 and SO42-, respectively. As expected, percentages were lowest for aerosol species, owing to their relatively low deposition velocities and correspondingly smaller gradients relative to gas phase species. Relative hourly median flux uncertainties were 31, 121, 42, 43, 67 and 56 % for NH3, NH4+, HNO3, NO3-, SO2 and SO42-, respectively. Flux

  4. Hyphenation of capillary high-performance ion-exchange chromatography with mass spectrometry using sheath-flow electrospray ionization.

    Science.gov (United States)

    Kochmann, Sven; Matysik, Frank-Michael

    2014-12-15

    Mass spectrometry (MS) is an attractive method for extending capillary-size ion chromatography (cHPIC) to create a valuable technique for speciation analysis. For hyphenation, the aqueous effluent of cHPIC has to be transformed into a volatile mixture for MS while preserving analytical concentrations as well as peak shapes during transfer from cHPIC to MS. Finally, the approach should technically be flexible and easy-to-use. A combination of cHPIC and sheath-flow electrospray ionization (ESI)-MS offers to solve all these challenges. cHPIC/sheath-flow-ESI-TOFMS was used in this study for the speciation analysis of various arsenic model compounds. These model compounds were analyzed with different hyphenation setups and configurations of cHPIC/MS and their respective assets and drawbacks were examined and discussed. The parameters (flow rate and composition of sheath liquid) of sheath-flow ESI and their influence on the performance of the spray and the sensitivity of the detector were investigated and compared with those of sheathless ESI. Using an injection valve to couple cHPIC and MS was found to be the best method for hyphenation, since it constitutes a flexible and dead-volume-free approach. The investigation of sheath-flow ESI revealed that the flow rate of the sheath liquid has to resemble the flow rate of the IC effluent to ensure a stable spray and that a composition of 2-propanol/water/ammonia at 50:50:0.2 (v/v/v) suits most applications without unilaterally promoting the sensitivity for either organic or inorganic compounds. The optimized setup and conditions were successfully applied to the analysis of a mixture of important arsenic species and used to determine limits of detection of organic and inorganic arsenic species (3.7 µg L(-1) elemental arsenic). A method for cHPIC/sheath-flow-ESI-MS was developed. The method was shown to be a valuable tool for speciation and trace analysis. It features no dead volume, fast transfer from IC to MS, only minimal

  5. Initial state fluctuations and final state correlations in relativistic heavy-ion collisions

    International Nuclear Information System (INIS)

    Luzum, Matthew; Petersen, Hannah

    2014-01-01

    We review the phenomenology and theory of bulk observables in ultra-relativistic heavy-ion collisions, focusing on recent developments involving event-by-event fluctuations in the initial stages of a heavy-ion collision, and how they manifest in observed correlations. We first define the relevant observables and show how each measurement is related to underlying theoretical quantities. Then we review the prevailing picture of the various stages of a collision, including the state-of-the-art modeling of the initial stages of a collision and subsequent hydrodynamic evolution, as well as hadronic scattering and freeze-out in the later stages. We then discuss the recent results that have shaped our current understanding and identify the challenges that remain. Finally, we point out open issues and the potential for progress in the field. (topical review)

  6. The use of isoprene as a novel dopant in negative ion atmospheric pressure photoionization mass spectrometry coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Dousty, Faezeh; O'Brien, Rob

    2015-06-15

    As in the case with positive ion atmospheric pressure photoionization (PI-APPI), the addition of dopants significantly improves the sensitivity of negative ion APPI (NI-APPI). However, the research on dopant-assisted-NI-APPI has been quite limited compared to the studies on dopant-assisted PI-APPI. This work presents the potential of isoprene as a novel dopant for NI-APPI. Thirteen compounds, possessing suitable gas-phase ion energetic properties in order to make stable negative ions, were selected. Dopants were continuously introduced into a tee junction prior to the ion source through a fused-silica capillary, while analytes were directly injected into the same tee. Then both were mixed with the continuous solvent from high-performance liquid chromatography (HPLC), nebulized, and entered the source. The nebulized stream was analyzed by APPI tandem quadrupole mass spectrometry in the negative ion mode. The results obtained using isoprene were compared with those obtained by using toluene as a dopant and dopant-free NI-APPI. Isoprene enhanced the ionization intensities of the studied compounds, which were found to be comparable and, in some cases, more effective than toluene. The mechanisms leading to the observed set of negative analyte ions were also discussed. Because in NI-APPI, thermal electrons, which are produced during the photoionization of a dopant, are considered the main reagent ions, both isoprene and toluene promoted the ionization of analytes through the same mechanisms, as expected. Isoprene was shown to perform well as a novel dopant for NI-APPI. Isoprene has a high photoabsorption cross section in the VUV region; therefore, its photoionization leads to a highly effective production of thermal electrons, which further promotes the ionization of analytes. In addition, isoprene is environmentally benign and less toxic compared to currently used dopants. Copyright © 2015 John Wiley & Sons, Ltd.

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

    DEFF Research Database (Denmark)

    Thomsen, Mohens; Willumsen, Dorthe

    1981-01-01

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

  8. Prediction of collision cross section and retention time for broad scope screening in gradient reversed-phase liquid chromatography-ion mobility-high resolution accurate mass spectrometry

    DEFF Research Database (Denmark)

    Mollerup, Christian Brinch; Mardal, Marie; Dalsgaard, Petur Weihe

    2018-01-01

    artificial neural networks (ANNs). Prediction was based on molecular descriptors, 827 RTs, and 357 CCS values from pharmaceuticals, drugs of abuse, and their metabolites. ANN models for the prediction of RT or CCS separately were examined, and the potential to predict both from a single model......Exact mass, retention time (RT), and collision cross section (CCS) are used as identification parameters in liquid chromatography coupled to ion mobility high resolution accurate mass spectrometry (LC-IM-HRMS). Targeted screening analyses are now more flexible and can be expanded for suspect...

  9. Simultaneous determination of clebopride and a major metabolite N-desbenzylclebopride in plasma by capillary gas chromatography-negative-ion chemical ionization mass spectrometry.

    Science.gov (United States)

    Robinson, P R; Jones, M D; Maddock, J; Rees, L W

    1991-03-08

    A procedure for the simultaneous assay of clebopride and its major metabolite N-desbenzylclebopride in plasma has been developed. The method utilizes capillary gas chromatography-negative-ion chemical ionization mass spectrometry with selected-ion monitoring of characteristic ions. Employing 2-ethoxy analogues as internal standards, the benzamides were extracted from basified plasma using dichloromethane. Subsequent reaction with heptafluorobutyric anhydride produced volatile mono- and diheptafluorobutyryl derivatives of clebopride and N-desbenzylclebopride, respectively. The methane negative-ion mass spectra of these derivatives exhibited intense high-mass ions ideal for specific quantitation of low levels in biological fluids. Using this procedure the recovery of the drug and metabolite from human plasma was found to be 84.4 +/- 1.5% (n = 3) and 77.4 +/- 4.7% (n = 3), respectively, at 0.5 ng/ml. Measurement of both compounds down to 0.10 ng/ml with a coefficient of variation of less than 10.5% is described. Plasma levels are reported in four volunteers up to 24 h following oral administration of 1 mg of clebopride malate salt.

  10. Energy deposition of heavy ions in the regime of strong beam-plasma correlations.

    Science.gov (United States)

    Gericke, D O; Schlanges, M

    2003-03-01

    The energy loss of highly charged ions in dense plasmas is investigated. The applied model includes strong beam-plasma correlation via a quantum T-matrix treatment of the cross sections. Dynamic screening effects are modeled by using a Debye-like potential with a velocity dependent screening length that guarantees the known low and high beam velocity limits. It is shown that this phenomenological model is in good agreement with simulation data up to very high beam-plasma coupling. An analysis of the stopping process shows considerably longer ranges and a less localized energy deposition if strong coupling is treated properly.

  11. 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)

  12. Pion correlations as a function of atomic mass in heavy ion collisions

    International Nuclear Information System (INIS)

    Chacon, A.D.

    1989-01-01

    The method of two pion interferometry was used to obtain source-size and lifetime parameters for the pions produced in heavy ion collisions. The systems used were 1.70 · A GeV 56 Fe + Fe, 1.82 · A GeV 40 Ar + KCl and 1.54 · A GeV 93 Nb + Nb, allowing for a search for dependences on the atomic number. Two acceptances (centered, in the lab., at ∼ 0 degrees and 45 degrees) were used for each system, allowing a search for dependences on the viewing angle. The correlation functions were calculated by comparing the data samples to background (or reference) samples made using the method of event mixing, where pions from different events are combined to produce a data sample in which the Bose-Einstein correlation effect is absent. The effect of the correlation function on the background samples is calculated, and a method for weighting the events to remove the residual correlation effect is presented. The effect of the spectrometer design on the measured correlation functions is discussed, as are methods for correcting for these effects during the data analysis. 58 refs., 39 figs., 18 tabs

  13. Correlated electron-ion collisions in a strong laser field; Korrelierte Elektron-Ion-Stoesse in starken Laserfeldern

    Energy Technology Data Exchange (ETDEWEB)

    Ristow, T.

    2007-12-17

    Electron-ion-collisions in plasmas in the presence of an ultra-short intensive laser pulse can cause high energy transfers to the electrons. During the collision the oscillation energy of the electron in the laser field is changed into drift energy. In this regime, multi-photon processes, known from the ionization of neutral atoms (Above-Threshold Ionization), and successive, so called correlated collisions, are important. The subject of the thesis is a study of binary Coulomb collisions in strong laser fields. The collisions are treated both in the context of classical Newtonian mechanics and in the quantum-mechanical framework by the Schroedinger equation. In the classical case a simplified instantaneous collision model and a complete dynamical treatment are discussed. Collisions can be treated instantaneously, if the ratio of the impact parameter to the quiver amplitude is small. The energy distributions calculated in this approximation show an elastic peak and a broad plateau due to rescattered electrons. At incident velocities smaller than the quiver velocity, correlated collisions are observed in the electron trajectories of the dynamical model. This effect leads to characteristic momentum distributions of the electrons, that are explicitly calculated and compared with the results of the instantaneous model. In addition, the time-dependence of the collisions is discussed in the framework of a singular perturbation theory. The complete description of the Coulomb scattering requires a quantum-mechanical description. A time-dependent method of wave-packet scattering is used and the corresponding time-dependent three-dimensional Schroedinger equation is solved by an implicit ADImethod on a spatial grid. The momentum and the energy distributions of the scattered electrons are calculated by the Fourier transformation of the wavefunction. A comparison of the scattering from a repulsive and an attractive potential is used to distinguish between simple collisions and

  14. Rapid identification and quantitation of compounds with forensic interest using fast liquid chromatography-ion trap mass spectrometry and library searching.

    Science.gov (United States)

    Pihlainen, Katja; Sippola, Erkki; Kostiainen, Risto

    2003-04-25

    A fast liquid chromatography-electrospray tandem mass spectrometric (LC-ESI-MS-MS) method by using a monolithic column, gradient elution and ion trap mass spectrometer was developed for 14 forensically interesting and chemically different compounds. All compounds were eluted within 2.5 min and the total analysis time was 5 min including stabilisation time required for the next injection. All the compounds, basics, neutrals and acids were efficiently ionised by positive ion ESI. A laboratory library including MS-MS spectra and retention times was developed and tested. Results with 476 standard samples and 50 authentic samples showed that the compounds studied can be unambiguously identified with the library. A quantitative method was developed for the compounds using external calibration. The evaluation process showed good linearity of the method and reasonable repeatability. Limits of detection ranged from 10.0 to 50.0 ng/ml.

  15. [Application of reversed-phase ion-pair chromatography for universal estimation of octanol-water partition coefficients of acid, basic and amphoteric drugs].

    Science.gov (United States)

    Zhu, Hui; Yang, Ri-Fang; Yun, Liu-Hong; Jiang, Yu; Li, Jin

    2009-09-01

    This paper is to establish a reversed-phase ion-pair chromatography (RP-IPC) method for universal estimation of the octanol/water partition coefficients (logP) of a wide range of structurally diverse compounds including acidic, basic, neutral and amphoteric species. The retention factors corresponding to 100% water (logk(w)) were derived from the linear part of the logk'/phi relationship, using at least four isocratic logk' values containing different organic compositions. The logk(w) parameters obtained were close to the corresponding logP values obtained with the standard "shake flask" methods. The mean deviation for test drugs is 0.31. RP-IPC with trifluoroacetic acid as non classic ion-pair agents can be applicable to determine the logP values for a variety of drug-like molecules with increased accuracy.

  16. Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

    Directory of Open Access Journals (Sweden)

    Ewa Jaszczak

    2017-01-01

    Full Text Available A simple and accurate ion chromatography (IC method with pulsed amperometric detection (PAD was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R>0.992. Low detection limits (LODs in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n=3 were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

  17. Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection.

    Science.gov (United States)

    Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

    2017-01-01

    A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1-100  μ g/L for urine, 5-100  μ g/L for saliva, and 3-100  μ g/L for sweat samples with determination coefficients ( R ) > 0.992. Low detection limits (LODs) in the range of 1.8  μ g/L, 5.1  μ g/L, and 5.8  μ g/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

  18. Effects of humidity on the quantitative determination of HCl, NOx, H2S, and NH3 using a three-stage filter pack with ion chromatography analysis

    International Nuclear Information System (INIS)

    Borek, T.T.; Wu, C.F.

    1993-01-01

    Low-level transuranic (TRU) waste to be stored underground at the Waste Isolation Pilot Plant (WIPP) has the potential to generate low levels of reactive gases such as HCl, NO x H 2 S, and NH 3 through radiological, biological, and chemical (corrosion) processes. Because of the low levels of gas expected to be produced (< 1 ppM), a method was developed which includes the simultaneous sampling of gases using chemically treated filter papers and analysis of the extracted ions by ion chromatography. To determine the effects of humidification on the collection and determination of reactive gases, a humidification system was added to the trace gas generator system to produce a relative humidity approximately equal to that in the Humid Test Bin. This humidification system consisted of gas washing bottles filled with saturated brine (NaCl) that has been shown to produce a relative humidity of approximately 75% in the temperature range of 68 degree F to 86 degree

  19. Correlation between the structural and optical properties of ion-assisted hafnia thin films

    Science.gov (United States)

    Scaglione, Salvatore; Sarto, Francesca; Alvisi, Marco; Rizzo, Antonella; Perrone, Maria R.; Protopapa, Maria L.

    2000-03-01

    The ion beam assistance during the film growth is one of the most useful method to obtain dense film along with improved optical and structural properties. Afnia material is widely used in optical coating operating in the UV region of the spectrum and its optical properties depend on the production method and the physical parameters of the species involved in the deposition process. In this work afnia thin films were evaporated by an e-gun and assisted during the growth process. The deposition parameters, ion beam energy, density of ions impinging on the growing film and the number of arrival atoms from the crucible, have been related to the optical and structural properties of the film itself. The absorption coefficient and the refractive index were measured by spectrophotometric technique while the microstructure has been studied by means of x-ray diffraction. A strictly correlation between the grain size, the optical properties and the laser damage threshold measurements at 248 nm was found for the samples deposited at different deposition parameters.

  20. Recoil ion momentum spectroscopy in atomic and nuclear physics: applications to low energy ion-atom/molecule collisions and to beta-neutrino angular correlation in beta decay

    International Nuclear Information System (INIS)

    Flechard, X.

    2012-12-01

    Since the early 1990's, Recoil Ion Momentum Spectroscopy is an ideal tool for ion-atom and ion-molecule collisions study. We detail here the development of this experimental technique during the last twenty years, illustrated with some of the most striking results obtained at GANIL (Caen) and J.R. Mac Donald Laboratory (Kansas State University). Recoil Ion Momentum Spectroscopy is also particularly well suited for β-ν angular correlation measurements in nuclear β decay. The LPCTrap experiment, installed at GANIL, is based on this technique, coupled to the use of a Paul trap for the radioactive ions confinement. The precise measurements performed with this setup allow both, to test specific aspects of the Standard Model of elementary particles, and to study the electron shake-off process following β decay. (author)

  1. Steroids in porcine follicular fluid: analysis by HPLC, capillary CG and capillary CG/MS after purification on SEP-PAK C18 and ion exchange chromatography.

    Science.gov (United States)

    Khalil, M W; Lawson, V

    1983-04-01

    Steroids in porcine follicular fluid have been concentrated by reverse phase chromatography in SEP-PAK C18 and purified further on the cation exchanger SP-Sephadex C-25. Fractionation into unconjugated neutral and phenolic steroids, glucuronides and sulfates was carried out on triethylaminohydroxypropyl Sephadex LH-20 (TEAP-LH-20). The unconjugated neutral fraction was analysed by high pressure liquid chromatography (HPLC) on a C18 radial cartridge 5 mm I.D.; 10 mu, or on a C18 5 mu RESOLVE column, and by capillary gas chromatography (GC) on a 12 M OV-1 cross linked fused silica column. Testosterone, progesterone and androstenedione were the major steroids detected by HPLC monitored at 254 nm, although 17- hydroxy-, 20 alpha-dihydro- and 20 beta-dihydroprogesterone were also present. Pregnenolone, pregnanediol, dehydroepiandrosterone, 17-hydroxypregnenolone and androsterone were detected by capillary CG as their 0-methyloxime trimethylsilyether derivatives. Further confirmation of structure was provided by complete mass spectral data or by selective ion monitoring (SIM).

  2. Towards a chromatographic similarity index to establish localised quantitative structure-retention relationships for retention prediction. II Use of Tanimoto similarity index in ion chromatography.

    Science.gov (United States)

    Park, Soo Hyun; Talebi, Mohammad; Amos, Ruth I J; Tyteca, Eva; Haddad, Paul R; Szucs, Roman; Pohl, Christopher A; Dolan, John W

    2017-11-10

    Quantitative Structure-Retention Relationships (QSRR) are used to predict retention times of compounds based only on their chemical structures encoded by molecular descriptors. The main concern in QSRR modelling is to build models with high predictive power, allowing reliable retention prediction for the unknown compounds across the chromatographic space. With the aim of enhancing the prediction power of the models, in this work, our previously proposed QSRR modelling approach called "federation of local models" is extended in ion chromatography to predict retention times of unknown ions, where a local model for each target ion (unknown) is created using only structurally similar ions from the dataset. A Tanimoto similarity (TS) score was utilised as a measure of structural similarity and training sets were developed by including ions that were similar to the target ion, as defined by a threshold value. The prediction of retention parameters (a- and b-values) in the linear solvent strength (LSS) model in ion chromatography, log k=a - blog[eluent], allows the prediction of retention times under all eluent concentrations. The QSRR models for a- and b-values were developed by a genetic algorithm-partial least squares method using the retention data of inorganic and small organic anions and larger organic cations (molecular mass up to 507) on four Thermo Fisher Scientific columns (AS20, AS19, AS11HC and CS17). The corresponding predicted retention times were calculated by fitting the predicted a- and b-values of the models into the LSS model equation. The predicted retention times were also plotted against the experimental values to evaluate the goodness of fit and the predictive power of the models. The application of a TS threshold of 0.6 was found to successfully produce predictive and reliable QSRR models (Q ext(F2) 2 >0.8 and Mean Absolute Error<0.1), and hence accurate retention time predictions with an average Mean Absolute Error of 0.2min. Crown Copyright

  3. Correlation between intrinsic hardness and defect structures of ion irradiated Fe alloys

    International Nuclear Information System (INIS)

    Shin, C.; Jin, H. H.; Kwon, J.

    2008-01-01

    Evolution of micro structures and mechanical properties during an in-service irradiation is one of the key issues to be addressed in nuclear materials. Ion irradiation is an effective method to study these irradiation effects thanks to an ease in handling post-irradiated specimens. But the characteristics of an ion irradiation pose a certain difficulty in evaluating irradiation effects. For example, ion irradiated region extends only a few hundred nano-meters from the surface of a sample and the depth profile of an irradiation damage level is quite heterogeneous. Thus it requires special care to quantify the changes in properties after an ion irradiation. We measured changes in a hardness by using a nano-indentation combined with a continuous stiffness measurement (CSM technique. Although the SM technique allows for a continuous measurement of hardness along penetration depth of an indenter; it is difficult to obtain an intrinsic hardness of an irradiation hardened region because one is measuring hardness of a hard layer located on a soft matrix. Thus we modeled the nano-indentation test by using a finite element method. We can extract the intrinsic hardness and the yield stress of an irradiation hardened region by using a so-called inverse method. We investigated the irradiation effects on Fe-Cr binary alloy by using the methods mentioned above. TEM analysis revealed that an irradiation forms dislocation loops with Burgers vector of and 1/2 . These loops varied in size and density with the Cr content and dose level. We discuss in detail a correlation between the measured irradiation-induced changes in the surface hardness and an irradiation induced defect. (authors)

  4. 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.

  5. Ion chromatography for the analysis of salt splitting capacities of cation and anion resin in premixed resin sample

    International Nuclear Information System (INIS)

    Ghosh, Satinath; Kumar, Rakesh; Tripathy, M.K.; Dhole, K.; Sharma, R.S.; Varde, P.V.

    2017-01-01

    Mixed bed ion exchange resin is commonly used in various plants including nuclear reactors for the purpose of fine polishing. The analysis of ion exchange capacities of cation and anion resin in resin mixture is therefore an agenda in the context of purchasing of premixed resin from the manufacturer. An ion chromatographic method for assaying ion exchange capacities of pure as well as mixed resin has been optimized. The proposed method in contrast to the conventional ASTM method has been found to be quite encouraging to consider it as an alternate method for the analysis of premixed resin. (author)

  6. Automated Gain Control and Internal Calibration With External Ion Accumulation Capillary liquid chromatography-electrospray ionization-fourier transform ion cyclotron resonance.

    Energy Technology Data Exchange (ETDEWEB)

    Belov, Mikhail E.(VISITORS); Zhang, Rui (BATTELLE (PACIFIC NW LAB)); Strittmatter, Eric F.(BATTELLE (PACIFIC NW LAB)); Prior, David C.(BATTELLE (PACIFIC NW LAB)); Tang, Keqi (BATTELLE (PACIFIC NW LAB)); Smith, Richard D.(BATTELLE (PACIFIC NW LAB))

    2003-08-15

    When combined with capillary LC separations, Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (ESI-FTICR MS) has increasingly been applied for advanced characterization of proteolytic digests. Incorporation of external (to the ICR cell) ion accumulation multipoles with FTICR for ion pre selection and accumulation has enhanced the dynamic range, sensitivity and duty cycle of measurements. However, the highly variable ion production rate from an LC separation can result in overfilling of the external trap, resulting in m/z discrimination and fragmentation of peptide ions. An excessive space charge trapped in the ICR cell causes significant shifts in the detected ion cyclotron frequencies, reducing the achievable mass measurement accuracy (MMA) for protein identification. To eliminate m/z discrimination in the external ion trap, further increase the duty cycle and improve MMA, we developed a capability for data-dependent adjustment of ion accumulation times in the course of an LC separation, referred to as Automated Gain Control (AGC), in combination with low kinetic energy gated ion trapping and internal calibration using a dual-channel electrodynamic ion funnel. The system was initially evaluated in the analysis of a 0.5 mg/mL tryptic digest of bovine serum albumin. The implementation of LC/ESI/AGC/FTICR with internal calibration gave rise to a {approx} 10-fold increase in the number of identified tryptic peptides within mass measurement accuracy of 2 ppm as compared to that detected during the conventional LC/FTICR run with a fixed ion accumulation time and external calibration.

  7. Virtual Protein Purification: A Simple Exercise to Introduce pH as A Parameter That Effects Ion Exchange Chromatography

    Science.gov (United States)

    Clark, Daniel D.; Edwards, Daniel J.

    2018-01-01

    This article describes a simple exercise using a free, easy-to-use, established online program. The exercise helps to reinforce protein purification concepts and introduces undergraduates to pH as a parameter that affects anion-exchange chromatography. The exercise was tested with biochemistry majors at California State University-Chico. Given the…

  8. Boehringer immunoinhibition procedure for creatine kinase-MB evaluated and compared with column ion-exchange chromatography

    NARCIS (Netherlands)

    ter Welle, H. F.; Baartscheer, T.; Fiolet, J. W.

    1983-01-01

    In determination of creatine kinase isoenzyme MB (CK-MB), the Boehringer immunoinhibition method gives a high and variable blank activity as compared with column-chromatography. Thus a correction must be applied. Furthermore, a second correction of 1% of total creatine kinase activity is necessary

  9. Determination of nitrite, nitrate, bromide, and iodide in seawater by ion chromatography with UV detection using dilauryldimethylammonium-coated monolithic ODS columns and sodium chloride as an eluent.

    Science.gov (United States)

    Ito, Kazuaki; Nomura, Ryosuke; Fujii, Takuya; Tanaka, Masahito; Tsumura, Tomoaki; Shibata, Hiroyuki; Hirokawa, Takeshi

    2012-11-01

    A method was developed for determination of inorganic anions, including nitrite (NO(2)(-)), nitrate (NO(3)(-)), bromide (Br(-)), and iodide (I(-)), in seawater by ion chromatography (IC). The IC system used two dilauryldimethylammonium bromide (DDAB)-coated monolithic ODS columns (50 × 4.6 mm i.d. and 100 × 4.6 mm i.d.) connected in series for separation of the ions. Aqueous NaCl (0.5 mol/L; flow rate, 3 mL/min) containing 5 mmol/L phosphate buffer (pH 5) was used as the eluent, and detection was with a UV detector at 225 nm. The monolithic ODS columns were coated and equilibrated with a 1-mmol/L DDAB solution (in H(2)O/methanol, 90:10 v/v). The hydrophilic ions (NO(2)(-), NO(3)(-), and Br(-)) were separated within 3 min and the retention time of I(-) was 16 min. No interferences from matrix ions, such as chloride and sulfate ions, were observed in 35 ‰ artificial seawater. The detection limits were 0.6 μg/L for NO(2)(-), 1.1 μg/L for NO(3)(-), 70 μg/L for Br(-), and 1.6 μg/L for I(-) with a 200-μL sample injection. The performance of the coated columns was maintained without addition of DDAB in the eluent. The IC system was successfully applied to real seawater samples with recovery rates of 94-108 % for all ions.

  10. Correlation between dried blood spot thin layer chromatography and plasma high performance liquid chromatography of leucine/isoleucine levels among Filipino patients with maple syrup urine disease (MSUD) seen at the Institute of Human Genetics, National Institutes of Health

    International Nuclear Information System (INIS)

    Yaplito-Lee, Joy; Chiong, Mary Anne D.; Rana, Michelle D.; Rama, Kahlil Izza D.; David-Padilla, Carmencita; Cavan, Barbra Charina; Cordero, Cynthia P.

    2008-01-01

    Management of patients with maple syrup urine disease (MSUD) includes a low protein diet, supplemented with special formulas and constant monitoring of branched chain amino acids (BCAA). The gold standard for monitoring BCAA is plasma amino acid analysis using high performance liquid chromatography (HPLC). In a developing country like the Philippines, however, the cost of this test is prohibitive to the majority of the patients. In our center, dried blood spot leucine/isoleucine (leu/ile) levels analysed by thin layer chromatography (TLC) is often used to diagnose and monitor these patients. This study was done to determine the correlation of leu/ile levels using the two methods (TLC and HPLC). A total of 46 MSUD patients were referred to the Biochemical Genetics Laboratory of the Institute of Human Genetics (IHG) from July 2001 to January 2004. Thirty five samples were obtained from 18 of these patients (some patients were seen at IHG more than once), and paired determinations of plasma amino acid using TLC and HPLC were made. The remaining samples were either hemolyzed or were not analyzed. The correlation coefficient [rho denoted as ρ] was estimated at a 95% confidence level using the Fisher's Z transformation. Of the 18 patients, 12 were males. The youngest was 1 day old and the oldest was 5 years old. The majority had the classical type of MSUD and dietary protein was restricted to between 0.6 gram/kg/day to 1 gram/kg/day of natural protein. Using the first pairs of observation for these 18 patients, the correlation coefficient was 0.76 (95% C1:0.462 to 0.907). This suggest a strong correlation between the two methods. It is recommended that further studies be done to determine the potential of the dried blood spot leu/ile level by TLC as an alternative method that can be used in the diagnosis and monitoring of MSUD patients especially in a developing country. (Author)

  11. Explicit hydration of ammonium ion by correlated methods employing molecular tailoring approach

    Science.gov (United States)

    Singh, Gurmeet; Verma, Rahul; Wagle, Swapnil; Gadre, Shridhar R.

    2017-11-01

    Explicit hydration studies of ions require accurate estimation of interaction energies. This work explores the explicit hydration of the ammonium ion (NH4+) employing Møller-Plesset second order (MP2) perturbation theory, an accurate yet relatively less expensive correlated method. Several initial geometries of NH4+(H2O)n (n = 4 to 13) clusters are subjected to MP2 level geometry optimisation with correlation consistent aug-cc-pVDZ (aVDZ) basis set. For large clusters (viz. n > 8), molecular tailoring approach (MTA) is used for single point energy evaluation at MP2/aVTZ level for the estimation of MP2 level binding energies (BEs) at complete basis set (CBS) limit. The minimal nature of the clusters upto n ≤ 8 is confirmed by performing vibrational frequency calculations at MP2/aVDZ level of theory, whereas for larger clusters (9 ≤ n ≤ 13) such calculations are effected via grafted MTA (GMTA) method. The zero point energy (ZPE) corrections are done for all the isomers lying within 1 kcal/mol of the lowest energy one. The resulting frequencies in N-H region (2900-3500 cm-1) and in O-H stretching region (3300-3900 cm-1) are in found to be in excellent agreement with the available experimental findings for 4 ≤ n ≤ 13. Furthermore, GMTA is also applied for calculating the BEs of these clusters at coupled cluster singles and doubles with perturbative triples (CCSD(T)) level of theory with aVDZ basis set. This work thus represents an art of the possible on contemporary multi-core computers for studying explicit molecular hydration at correlated level theories.

  12. Improving methodological aspects of the analysis of five regulated haloacetic acids in water samples by solid-phase extraction, ion-pair liquid chromatography and electrospray tandem mass spectrometry.

    Science.gov (United States)

    Prieto-Blanco, M C; Alpendurada, M F; López-Mahía, P; Muniategui-Lorenzo, S; Prada-Rodríguez, D; Machado, S; Gonçalves, C

    2012-05-30

    Haloacetic acids (HAAs) are organic pollutants originated from the drinking water disinfection process, which ought to be controlled and minimized. In this work a method for monitoring haloacetic acids (HAAs) in water samples is proposed, which can be used in quality control laboratories using the techniques most frequently available. Among its main advantages we may highlight its automated character, including minimal steps of sample preparation, and above all, its improved selectivity and sensitivity in the analysis of real samples. Five haloacetic acids (HAA5) were analyzed using solid-phase extraction (SPE) combined with ion-pair liquid chromatography and tandem mass spectrometry. For the optimization of the chromatographic separation, two amines (triethylamine, TEA and dibutylamine, DBA) as ion pair reagents were compared, and a better selectivity and sensitivity was obtained using DBA, especially for monohaloacetic acids. SPE conditions were optimized using different polymeric adsorbents. The electrospray source parameters were studied for maximum precursor ion accumulation, while the collision cell energy of the triple quadrupole mass spectrometer was adjusted for optimum fragmentation. Precursor ions detected were deprotonated, dimeric and decarboxylated ions. The major product ions formed were: ionized halogen atom (chloride and bromide) and decarboxylated ions. After enrichment of the HAAs in Lichrolut EN adsorbent, the limits of detection obtained by LC-MS/MS analysis (between 0.04 and 0.3 ng mL(-1)) were comparable to those obtained by GC-MS after derivatization. Linearity with good correlation coefficients was obtained over two orders of magnitude irrespective of the compound. Adequate recoveries were achieved (60-102%), and the repeatability and intermediate precision were in the range of 2.4-6.6% and 3.8-14.8%, respectively. In order to demonstrate the usefulness of the method for routine HAAs monitoring, different types of water samples were

  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. Receptor-based high-throughput screening and identification of estrogens in dietary supplements using bioaffinity liquid-chromatography ion mobility mass spectrometry.

    Science.gov (United States)

    Aqai, Payam; Blesa, Natalia Gómez; Major, Hilary; Pedotti, Mattia; Varani, Luca; Ferrero, Valentina E V; Haasnoot, Willem; Nielen, Michel W F

    2013-11-01

    A high-throughput bioaffinity liquid chromatography-mass spectrometry (BioMS) approach was developed and applied for the screening and identification of recombinant human estrogen receptor α (ERα) ligands in dietary supplements. For screening, a semi-automated mass spectrometric ligand binding assay was developed applying (13)C2, (15) N-tamoxifen as non-radioactive label and fast ultra-high-performance-liquid chromatography-electrospray ionisation-triple-quadrupole-MS (UPLC-QqQ-MS), operated in the single reaction monitoring mode, as a readout system. Binding of the label to ERα-coated paramagnetic microbeads was inhibited by competing estrogens in the sample extract yielding decreased levels of the label in UPLC-QqQ-MS. The label showed high ionisation efficiency in positive electrospray ionisation (ESI) mode, so the developed BioMS approach is able to screen for estrogens in dietary supplements despite their poor ionisation efficiency in both positive and negative ESI modes. The assay was performed in a 96-well plate, and all these wells could be measured within 3 h. Estrogens in suspect extracts were identified by full-scan accurate mass and collision-cross section (CCS) values from a UPLC-ion mobility-Q-time-of-flight-MS (UPLC-IM-Q-ToF-MS) equipped with a novel atmospheric pressure ionisation source. Thanks to the novel ion source, this instrument provided picogram sensitivity for estrogens in the negative ion mode and an additional identification point (experimental CCS values) next to retention time, accurate mass and tandem mass spectrometry data. The developed combination of bioaffinity screening with UPLC-QqQ-MS and identification with UPLC-IM-Q-ToF-MS provides an extremely powerful analytical tool for early warning of ERα bioactive compounds in dietary supplements as demonstrated by analysis of selected dietary supplements in which different estrogens were identified.

  15. Simultaneous identification and quantification of tetrodotoxin in fresh pufferfish and pufferfish-based products using immunoaffinity columns and liquid chromatography/quadrupole-linear ion trap mass spectrometry

    Science.gov (United States)

    Guo, Mengmeng; Wu, Haiyan; Jiang, Tao; Tan, Zhijun; Zhao, Chunxia; Zheng, Guanchao; Li, Zhaoxin; Zhai, Yuxiu

    2017-07-01

    In this study, we established a comprehensive method for simultaneous identification and quantification of tetrodotoxin (TTX) in fresh pufferfish tissues and pufferfish-based products using liquid chromatography/quadrupole-linear ion trap mass spectrometry (LC-QqLIT-MS). TTX was extracted by 1% acetic acid-methanol, and most of the lipids were then removed by freezing lipid precipitation, followed by purification and concentration using immunoaffinity columns (IACs). Matrix effects were substantially reduced due to the high specificity of the IACs, and thus, background interference was avoided. Quantitation analysis was therefore performed using an external calibration curve with standards prepared in mobile phase. The method was evaluated by fortifying samples at 1, 10, and 100 ng/g, respectively, and the recoveries ranged from 75.8%-107%, with a relative standard deviation of less than 15%. The TTX calibration curves were linear over the range of 1-1 000 μg/L, with a detection limit of 0.3 ng/g and a quantification limit of 1 ng/g. Using this method, samples can be further analyzed using an information-dependent acquisition (IDA) experiment, in the positive mode, from a single liquid chromatography-tandem mass spectrometry injection, which can provide an extra level of confirmation by matching the full product ion spectra acquired for a standard sample with those from an enhanced product ion (EPI) library. The scheduled multiple reaction monitoring method enabled TTX to be screened for, and TTX was positively identified using the IDA and EPI spectra. This method was successfully applied to analyze a total of 206 samples of fresh pufferfish tissues and pufferfish-based products. The results from this study show that the proposed method can be used to quantify and identify TTX in a single run with excellent sensitivity and reproducibility, and is suitable for the analysis of complex matrix pufferfish samples.

  16. Separation of aliphatic carboxylic acids and benzenecarboxylic acids by ion-exclusion chromatography with various cation-exchange resin columns and sulfuric acid as eluent.

    Science.gov (United States)

    Ohta, Kazutoku; Ohashi, Masayoshi; Jin, Ji-Ye; Takeuchi, Toyohide; Fujimoto, Chuzo; Choi, Seong-Ho; Ryoo, Jae-Jeong; Lee, Kwang-Pill

    2003-05-16

    The application of various hydrophilic cation-exchange resins for high-performance liquid chromatography (sulfonated silica gel: TSKgel SP-2SW, carboxylated silica gel: TSKgel CM-2SW, sulfonated polymethacrylate resin: TSKgel SP-5PW, carboxylated polymethacrylate resins: TSKgel CM-5PW and TSKgel OA-Pak A) as stationary phases in ion-exclusion chromatography for C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, butyric, isovaleric, valeric, isocaproic, caproic, 2-methylhexanoic and heptanoic acids) and benzenecarboxylic acids (pyromellitic, trimellitic, hemimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic, salicylic acids and phenol) was carried out using diluted sulfuric acid as the eluent. Silica-based cation-exchange resins (TSKgel SP-2SW and TSKgel CM-2SW) were very suitable for the ion-exclusion chromatographic separation of these benzenecarboxylic acids. Excellent simultaneous separation of these benzenecarboxylic acids was achieved on a TSKgel SP-2SW column (150 x 6 mm I.D.) in 17 min using a 2.5 mM sulfuric acid at pH 2.4 as the eluent. Polymethacrylate-based cation-exchange resins (TSKgel SP-5PW, TSKgel CM-5PW and TSKgel OA-Pak A) acted as advanced stationary phases for the ion-exclusion chromatographic separation of these C1-C7 aliphatic carboxylic acids. Excellent simultaneous separation of these C1-C7 acids was achieved on a TSKgel CM-5PW column (150 x 6 mm I.D.) in 32 min using a 0.05 mM sulfuric acid at pH 4.0 as the eluent.

  17. 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.

  18. 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.

  19. 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.

  20. 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...

  1. Correlation of blister diameter and blister skin thickness in helium-ion-irradiated Nb

    International Nuclear Information System (INIS)

    Das, S.K.; Kaminsky, M.; Fenske, G.

    1979-01-01

    A systematic study of the correlation between blister diameter and blister skin thickness has been performed for helium-ion irradiation of monocrystalline and polycrystalline Nb for ion energies ranging from 20 to 500 keV. The results indicate that a relationship Datsub mpatproportionaltatsup 1.50at between the most probable blister diameter, Datsub mpat, and blister skin thickness, t, which has been suggested by other authors, does not exist for the various types of Nb targets studied. For example, for room-temperature irradiation of annealed polycrystalline Nb the experimentally determined relationship is Datsub mpat<10.3tatsup 1.22at. Furthermore, the D-t relationship was found to depend on the irradiation temperature in contrast to theoretical predictions by the lateral stress model of blister formation. These results do not appear to support the lateral stress model which predicts the relationship Dproportionaltatsup 1.5at. However, the experimentally determined relationships can be explained in part by the gas pressure model of blister formation

  2. Cd doping of AlN via ion implantation studied with perturbed angular correlation

    CERN Document Server

    Kessler, Patrick; Miranda, Sérgio MC; Simon, R; Correia, João Guilherme; Johnston, Karl; Vianden, Reiner

    2012-01-01

    AlN with a wide bandgap of 6.2 eV is a promising candidate for ultraviolet light-emitting diodes and laser diodes. However, the production of the required p-type AlN is still challenging. As a possible dopant Cd was suggested among other Group II atoms (Be, Mg, and Zn). In this study the annealing condition of implanted Cd in AlN was investigated with the method of the perturbed angular correlation (PAC). Therefore radioactive $^{117}$Cd or $^{111m}$Cd ions were implanted into thin AlN films on sapphire substrate with an energy of 30 keV and fluences in the range of 10$^{11}$ ions/cm$^{2}$. After thorough annealing with a proximity cap of the same material most of the Cd-probes occupy substitutional lattice sites and almost all implantation damage can be annealed. This results in a distinct frequency in the PAC spectra which increases with temperature. In contrast to the formation of an indium nitrogen-vacancy complex observed with the probe $^{111}$In on substitutional Al-sites no defects are bound to substi...

  3. Ion track etching revisited: I. Correlations between track parameters in aged polymers

    Science.gov (United States)

    Fink, D.; Muñoz H., G.; García A., H.; Vacik, J.; Hnatowicz, V.; Kiv, A.; Alfonta, L.

    2018-04-01

    Some yet poorly understood problems of etching of pristine and swift heavy ion track-irradiated aged polymers were treated, by applying conductometry across the irradiated foils during etching. The onset times of etchant penetration across pristine foils, and the onset times of the different etched track regimes in irradiated foils were determined for polymers of various proveniences, fluences and ages, as well as their corresponding etching speeds. From the results, correlations of the parameters with each other were deduced. The normalization of these parameters enables one to compare irradiated polymer foils of different origin and treatment with one another. In a number of cases, also polymeric gel formation and swelling occur which influence the track etching behaviour. The polymer degradation during aging influences the track etching parameters, which differ from each other on both sides of the foils. With increasing sample age, these differences increase.

  4. Quantitative analysis of volatile organic compounds using ion mobility spectra and cascade correlation neural networks

    Science.gov (United States)

    Harrington, Peter DEB.; Zheng, Peng

    1995-01-01

    Ion Mobility Spectrometry (IMS) is a powerful technique for trace organic analysis in the gas phase. Quantitative measurements are difficult, because IMS has a limited linear range. Factors that may affect the instrument response are pressure, temperature, and humidity. Nonlinear calibration methods, such as neural networks, may be ideally suited for IMS. Neural networks have the capability of modeling complex systems. Many neural networks suffer from long training times and overfitting. Cascade correlation neural networks train at very fast rates. They also build their own topology, that is a number of layers and number of units in each layer. By controlling the decay parameter in training neural networks, reproducible and general models may be obtained.

  5. Correlated electron capture and inner-shell excitation measurements in ion-atom collisions

    International Nuclear Information System (INIS)

    Tanis, J.A.; Bernstein, E.M.; Clark, M.W.

    1985-01-01

    In an ion-atom collision projectile excitation and charge transfer (electron capture) may occur together in a single encounter. If the excitation and capture are correlated, then the process is called resonant transfer and excitation (RTE); if they are uncorrelated, then the process is termed nonresonant transfer and excitation (NTE). Experimental work to date has shown the existence of RTE and provided strong evidence for NTE. Results presented here provide information on the relative magnitudes of RTE and NTE, the charge state dependence of RTE, the effect of the target momentum distribution on RTE, the magnitude of L-shell RTE compared to K-shell RTE, and the target Z dependences of RTE and NTE. 15 refs., 5 figs

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

    Science.gov (United States)

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

    2015-04-01

    Cobalt magnetic nanoparticles surface functionalised with iminodiacetic acid were evaluated as a nano-particulate solid phase extraction absorbent for copper ions (Cu(2+)) from environmental water samples. Using an external magnetic field, the collector nanoparticles could be separated from the aqueous phase, and adsorbed ions simply decomplexed using dilute HNO3. Effects of pH, buffer concentration, sample and sorbent volume, extraction equilibrium time, and interfering ion concentration on extraction efficiency were investigated. Optimal conditions were then applied to the extraction of Cu(2+) ions from natural water samples, prior to their quantitation using high-performance chelation ion chromatography. The limits of detection (LOD) of the combined extraction and chromatographic method were ~0.1 ng ml(-1), based upon a 100-fold preconcentration factor (chromatographic performance; LOD=9.2 ng ml(-1) Cu(2+)), analytical linear range from 20 to 5000 ng mL(-1), and relative standard deviations=4.9% (c=1000 ng ml(-1), n=7). Accuracy and precision of the combined approach was verified using a certified reference standard estuarine water sample (SLEW-2) and comparison of sample determinations with sector field inductively coupled plasma mass spectrometry. Recoveries from the addition of Cu(2+) to impacted estuarine and rain water samples were 103.5% and 108.5%, respectively. Coastal seawater samples, both with and without prior UV irradiation and dissolved organic matter removal were also investigated using the new methodology. The effect of DOM concentration on copper availability was demonstrated. Copyright © 2015. Published by Elsevier B.V.

  7. Chemical speciation analysis for bromine in tap water by ion chromatography/inductively coupled plasma-mass spectrometry and electrospray ionization-mass spectrometry

    International Nuclear Information System (INIS)

    Kurata, Keigo; Suzuki, Yoshinari; Furuta, Naoki

    2010-01-01

    Bromide compounds in tap water were measured by using a hyphenated technique of ion chromatography coupled with inductively coupled plasma - mass spectrometry (IC/ICP-MS) and electrospray ionization mass spectrometry (ESI-MS). We identified bromide ion (Br - ), bromate ion (BrO 3 - ), bromochloroacetic acid (BCAA), dibromoacetic acid (DBAA) and bromodichloroacetic acid (BDCAA) by standard addition methods with IC/ICP-MS. Moreover, we identified BCAA and BDCAA by ESI-MS after separation with IC. Br - , BrO 3 - , BCAA, DBAA and BDCAA in tap water collected from around Tokyo area were quantified by IC/ICP-MS. The maximum concentration of BrO 3 - (1.8 ng mL -1 ) was observed in tap water collected from Bunkyo-ku, although this concentration was lower than 10 ng mL -1 , which is the regulated concentration in Japan. DBAA, which is regulated by United States Environmental Protection Agency, was detected in tap water collected from all sites, except for Ome. However, since BrO 3 - and DBAA are toxic, it is necessary to continue monitoring bromide compounds in tap water. (author)

  8. Mass Spectrometry Parameters Optimization for the 46 Multiclass Pesticides Determination in Strawberries with Gas Chromatography Ion-Trap Tandem Mass Spectrometry

    Science.gov (United States)

    Fernandes, Virgínia C.; Vera, Jose L.; Domingues, Valentina F.; Silva, Luís M. S.; Mateus, Nuno; Delerue-Matos, Cristina

    2012-12-01

    Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or " q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.

  9. Application of high-performance liquid chromatography-tandem mass spectrometry with a quadrupole/linear ion trap instrument for the analysis of pesticide residues in olive oil.

    Science.gov (United States)

    Hernando, M D; Ferrer, C; Ulaszewska, M; García-Reyes, J F; Molina-Díaz, A; Fernández-Alba, A R

    2007-11-01

    This article describes the development of an enhanced liquid chromatography-mass spectrometry (LC-MS) method for the analysis of pesticides in olive oil. One hundred pesticides belonging to different classes and that are currently used in agriculture have been included in this method. The LC-MS method was developed using a hybrid quadrupole/linear ion trap (QqQ(LIT)) analyzer. Key features of this technique are the rapid scan acquisition times, high specificity and high sensitivity it enables when the multiple reaction monitoring (MRM) mode or the linear ion-trap operational mode is employed. The application of 5 ms dwell times using a linearly accelerating (LINAC) high-pressure collision cell enabled the analysis of a high number of pesticides, with enough data points acquired for optimal peak definition in MRM operation mode and for satisfactory quantitative determinations to be made. The method quantifies over a linear dynamic range of LOQs (0.03-10 microg kg(-1)) up to 500 microg kg(-1). Matrix effects were evaluated by comparing the slopes of matrix-matched and solvent-based calibration curves. Weak suppression or enhancement of signals was observed (ion (EPI) and MS3 were developed.

  10. Rapid Quantification of Four Anthocyanins in Red Grape Wine by Hydrophilic Interaction Liquid Chromatography/Triple Quadrupole Linear Ion Trap Mass Spectrometry.

    Science.gov (United States)

    Sun, Yongming; Xia, Biqi; Chen, Xiangzhun; Duanmu, Chuansong; Li, Denghao; Han, Chao

    2015-01-01

    The identification and quantification of four anthocyanins (cyanidin-3-O-glucoside, peonidin-3-O-glucoside, delphinidin-3-O-glucoside, and malvidin-3-O-glucoside) in red grape wine were carried out by hydrophilic interaction liquid chromatography/triple quadrupole linear ion trap MS (HILIC/QTrap-MS/MS). Samples were diluted directly and separated on a Merck ZIC HILIC column with 20 mM ammonium acetate solution-acetonitrile mobile phase. Quantitative data acquisition was carried out in the multiple reaction monitoring mode. Additional identification and confirmation of target compounds were performed using the enhanced product ion mode of the linear ion trap. The LOQs were in the range 0.05-1.0 ng/mL. The average recoveries were in the range 94.6 to 104.5%. The HILIC/QTrap-MS/MS platform offers the best sensitivity and specificity for characterization and quantitative determination of the four anthocyanins in red grape wines and fulfills the quality criteria for routine laboratory application.

  11. First β-ν correlation measurement from the recoil-energy spectrum of Penning trapped Ar35 ions

    Science.gov (United States)

    Van Gorp, S.; Breitenfeldt, M.; Tandecki, M.; Beck, M.; Finlay, P.; Friedag, P.; Glück, F.; Herlert, A.; Kozlov, V.; Porobic, T.; Soti, G.; Traykov, E.; Wauters, F.; Weinheimer, Ch.; Zákoucký, D.; Severijns, N.

    2014-08-01

    We demonstrate a novel method to search for physics beyond the standard model by determining the β-ν angular correlation from the recoil-ion energy distribution after β decay of ions stored in a Penning trap. This recoil-ion energy distribution is measured with a retardation spectrometer. The unique combination of the spectrometer with a Penning trap provides a number of advantages, e.g., a high recoil-ion count rate and low sensitivity to the initial position and velocity distribution of the ions and completely different sources of systematic errors compared to other state-of-the-art experiments. Results of a first measurement with the isotope Ar35 are presented. Although currently at limited precision, we show that a statistical precision of about 0.5% is achievable with this unique method, thereby opening up the possibility of contributing to state-of-the-art searches for exotic currents in weak interactions.

  12. 37Cl/35Cl isotope ratio analysis in perchlorate by ion chromatography/multi collector -ICPMS: Analytical performance and implication for biodegradation studies.

    Science.gov (United States)

    Zakon, Yevgeni; Ronen, Zeev; Halicz, Ludwik; Gelman, Faina

    2017-10-01

    In the present study we propose a new analytical method for 37 Cl/ 35 Cl analysis in perchlorate by Ion Chromatography(IC) coupled to Multicollector Inductively Coupled Plasma Mass Spectrometry (MC-ICPMS). The accuracy of the analytical method was validated by analysis of international perchlorate standard materials USGS-37 and USGS -38; analytical precision better than ±0.4‰ was achieved. 37 Cl/ 35 Cl isotope ratio analysis in perchlorate during laboratory biodegradation experiment with microbial cultures enriched from the contaminated soil in Israel resulted in isotope enrichment factor ε 37 Cl = -13.3 ± 1‰, which falls in the range reported previously for perchlorate biodegradation by pure microbial cultures. The proposed analytical method may significantly simplify the procedure for isotope analysis of perchlorate which is currently applied in environmental studies. Copyright © 2017. Published by Elsevier Ltd.

  13. Measurement of release of endogenous GABA and catabolites of [3H]GABA from synaptosomal preparations using ion-exchange chromatography

    International Nuclear Information System (INIS)

    Grove, J.; Gardner, C.R.; Richards, M.H.

    1982-01-01

    Picomole quantities of endogenous GABA in acidified superfusates of synaptosomal preparations have been measured using micro-bore ion-exchange chromatography and post-column formation of the fluorescent iso-indole derivative. Using this technique superfusates have been analyzed directly, without further manipulations, to investigate the release of endogenous GABA. Spontaneous release of GABA was 2-5 pmol/200 microliters superfusate increasing to 20 pmol/200 microliters with potassium stimulation. When gamma-vinyl GABA (RMI 71754), an inhibitor of GABA-T was injected into rats (750 mg/kg) and synaptosomes prepared the potassium-evoked release of GABA was increased 3-fold compared to controls. Chromatographic separations and measurement of release of endogenous and radiolabeled GABA allowed the real specific activity of released GABA to be calculated. Only when 500 microM amino-oxyacetic acid was added during isolation of synaptosomes was the specific activity of released GABA the same as the initial specific activity

  14. Simultaneous determination of wine sugars, glycerol and organic acids 13C/12C isotopic ratio by ion chromatography-co-IRMS

    Directory of Open Access Journals (Sweden)

    Guyon Francois

    2014-01-01

    Full Text Available Ion chromatography (IC isotope ratio mass spectrometry (IRMS coupling is possible using a liquid interface allowing chemical oxidation (co of organic compounds. Synthetic solutions containing a mixture of glycerol, sugars (sucrose, glucose and fructose and organic acids (gluconic, lactic, malic, tartaric, oxalic, fumaric, citric and isocitric were elaborated to estimate analytical applications of two different IC systems. It appears that the use of carbonated solution in the eluting phase is a perturbation for 13C isotope measurements as it creates a δ13C deviation from the expected values. A sample of authentic sweet wine was analyzed by IC-co-IRMS using KOH gradient. Ratios of isotopic, ratios of organic acids and glycerol was found to be, in average, equal 1.01 ± 0.04 that is in accordance with our previous results.

  15. Simultaneous determination of chloroquine and its three metabolites in human plasma, whole blood and urine by ion-pair high-performance liquid chromatography.

    Science.gov (United States)

    Houzé, P; de Reynies, A; Baud, F J; Benatar, M F; Pays, M

    1992-02-14

    A method was developed for the separation and measurement of chloroquine and three metabolites (desethylchloroquine, bisdesethylchloroquine and 4-amino-7-chloroquinoline) in biological samples by ion-pair high-performance liquid chromatography with UV detection. The method uses 2,3-diaminoaphthalene as an internal standard and provides a limit of detection between 1 and 2 ng/ml for chloroquine and its metabolites. The assay was linear in the range 12.5-250 ng/ml and the analytical recovery and reproducibility were sufficient. The assay was applied to the analysis of biological samples from a patient undergoing chloroquine chemoprophylaxis and a patient who had ingested chloroquine in a suicide attempt.

  16. Rapid Characterization and Identification of Flavonoids in Radix Astragali by Ultra-High-Pressure Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Mass Spectrometry.

    Science.gov (United States)

    Zhang, Jing; Xu, Xiao-Jie; Xu, Wen; Huang, Juan; Zhu, Da-yuan; Qiu, Xiao-Hui

    2015-07-01

    A simple and effective method was established for separation and characterization of flavonoid constituents in Radix Astragali (RA) by combination of ultra-high-pressure liquid chromatography with LTQ-Orbitrap tandem mass spectrometry (u-HPLC-LTQ-Orbitrap-MS(n)). For three major structural types of flavonoids, the proposed fragmentation pathways and major diagnostic fragment ions of isoflavones, pterocarpans and isoflavans were investigated to trace isoflavonoid derivatives in crude plant extracts. Based on the systematic identification strategy, 48 constituents were rapidly detected and characterized or tentatively identified, many of which were first reported in RA. The u-PHLC-LTQ-Orbitrap MS(n) platform was proved as an effective tool for rapid qualitative analysis of secondary metabolite productions from natural resources. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  17. Direct chemical-analysis of uv laser-ablation products of organic polymers by using selective ion monitoring mode in gas-chromatography mass-spectrometry

    Science.gov (United States)

    Cho, Yirang; Lee, H.W.; Fountain, S.T.; Lubman, D.M.

    1994-01-01

    Trace quantities of laser ablated organic polymers were analyzed by using commercial capillary column gas chromatography/mass spectrometry; the instrument was modified so that the laser ablation products could be introduced into the capillary column directly and the constituents of each peak in the chromatogram were identified by using a mass spectrometer. The present study takes advantage of the selective ion monitoring mode for significantly improving the sensitivity of the mass spectrometer as a detector, which is critical in analyzing the trace quantities and confirming the presence or absence of the species of interest in laser ablated polymers. The initial composition of the laser ablated polymers was obtained by using an electron impact reflectron time-of-flight mass spectrometer and the possible structure of the fragments observed in the spectra was proposed based on the structure of the polymers.

  18. A three-scale model for ionic solute transport in swelling clays incorporating ion-ion correlation effects

    Science.gov (United States)

    Le, Tien Dung; Moyne, Christian; Murad, Marcio A.

    2015-01-01

    A new three-scale model is proposed to describe the movement of ionic species of different valences in swelling clays characterized by three separate length scales (nano, micro, and macro) and two levels of porosity (nano- and micropores). At the finest (nano) scale the medium is treated as charged clay particles saturated by aqueous electrolyte solution containing monovalent and divalent ions forming the electrical double layer. A new constitutive law is constructed for the disjoining pressure based on the numerical resolution of non-local problem at the nanoscale which, in contrast to the Poisson-Boltzmann theory for point charge ions, is capable of capturing the short-range interactions between the ions due to their finite size. At the intermediate scale (microscale), the two-phase homogenized particle/electrolyte solution system is represented by swollen clay clusters (or aggregates) with the nanoscale disjoining pressure incorporated in a modified form of Terzaghi's effective principle. At the macroscale, the electro-chemical-mechanical couplings within clay clusters is homogenized with the ion transport in the bulk fluid lying in the micro pores. The resultant macroscopic picture is governed by a three-scale model wherein ion transport takes place in the bulk solution strongly coupled with the mechanics of the clay clusters which play the role of sources/sinks of mass to the bulk fluid associated with ion adsorption/desorption in the electrical double layer at the nanoscale. Within the context of the quasi-steady version of the multiscale model, wherein the electrolyte solution in the nanopores is assumed at instantaneous thermodynamic equilibrium with the bulk fluid in the micropores, we build-up numerically the ion-adsorption isotherms along with the constitutive law of the retardation coefficients of monovalent and divalent ions. In addition, the constitutive law for the macroscopic swelling pressure is reconstructed numerically showing patterns of

  19. Confirmatory analysis method for zeranol, its metabolites and related mycotoxins in urine by liquid chromatography-negative ion electrospray tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bennekom, E.O. van; Brouwer, L.; Laurant, E.H.M.; Hooijerink, H.; Nielen, M.W.F

    2002-11-25

    The determination of the banned anabolic substance zeranol and the metabolites taleranol and zearalanone in bovine urine is complicated by the occurrence of the structurally-related mycotoxin zearalenone and the corresponding {alpha}- and {beta}-zearalenol metabolites which possess similar estrogenic properties. A liquid chromatography-negative ion electrospray tandem mass spectrometric method is presented for the confirmatory analysis of all six resorcylic acid lactones ('zeranols') in urine samples using deuterium-labelled internal standards. The method was validated as a confirmatory method for bovine urine samples according to new draft EU guidelines and showed good precision and linearity, and CC{alpha} and CC{beta} values of 0.02-0.30 and <1.0 ng ml{sup -1}, respectively. The applicability was demonstrated by comparing the results of an incurred sample with previous results on the same sample obtained by gas chromatography high resolution mass spectrometry. Preliminary data show that following a simple matrix solid phase dispersion clean-up, liver samples from poultry will be amenable to this method as well.

  20. Confirmatory analysis method for zeranol, its metabolites and related mycotoxins in urine by liquid chromatography-negative ion electrospray tandem mass spectrometry

    International Nuclear Information System (INIS)

    Bennekom, E.O. van; Brouwer, L.; Laurant, E.H.M.; Hooijerink, H.; Nielen, M.W.F.

    2002-01-01

    The determination of the banned anabolic substance zeranol and the metabolites taleranol and zearalanone in bovine urine is complicated by the occurrence of the structurally-related mycotoxin zearalenone and the corresponding α- and β-zearalenol metabolites which possess similar estrogenic properties. A liquid chromatography-negative ion electrospray tandem mass spectrometric method is presented for the confirmatory analysis of all six resorcylic acid lactones ('zeranols') in urine samples using deuterium-labelled internal standards. The method was validated as a confirmatory method for bovine urine samples according to new draft EU guidelines and showed good precision and linearity, and CCα and CCβ values of 0.02-0.30 and -1 , respectively. The applicability was demonstrated by comparing the results of an incurred sample with previous results on the same sample obtained by gas chromatography high resolution mass spectrometry. Preliminary data show that following a simple matrix solid phase dispersion clean-up, liver samples from poultry will be amenable to this method as well

  1. Study of ion suppression for phenolic compounds in medicinal plant extracts using liquid chromatography-electrospray tandem mass spectrometry.

    Science.gov (United States)

    Faccin, H; Viana, C; do Nascimento, P C; Bohrer, D; de Carvalho, L M

    2016-01-04

    A systematic study on the various sources of ion suppression in UHPLC-MS-MS analysis was carried out for 24 phenolic antioxidants in 6 different extracts of medicinal plants from Amazonia. The contributions of matrix effects, mobile-phase additives, analyte co-elution and electric charge competition during ionization to the global ion suppression were evaluated. Herein, the influence of mobile-phase additives on the ionization efficiency was found to be very pronounced, where ion suppression of approximately 90% and ion enhancement effects greater than 400% could be observed. The negative effect caused by the wrong choice of internal standard (IS) on quantitative studies was also evaluated and discussed from the perspective of ion suppression. This work also shows the importance of performing studies with this approach even for very similar matrices, such as varieties of medicinal plants from the same species, because different effects were observed for the same analyte. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Iminodiacetic acid functionalised organopolymer monoliths: application to the separation of metal cations by capillary high-performance chelation ion chromatography.

    Science.gov (United States)

    Moyna, Áine; Connolly, Damian; Nesterenko, Ekaterina; Nesterenko, Pavel N; Paull, Brett

    2013-03-01

    Lauryl methacrylate-co-ethylene dimethacrylate monoliths were polymerised within fused silica capillaries and subsequently photo-grafted with varying amounts of glycidyl methacrylate (GMA). The grafted monoliths were then further modified with iminodiacetic acid (IDA), resulting in a range of chelating ion-exchange monoliths of increasing capacity. The IDA functional groups were attached via ring opening of the epoxy group on the poly(GMA) structure. Increasing the amount of attached poly(GMA), via photo-grafting with increasing concentrations of GMA, from 15 to 35%, resulted in a proportional and controlled increase in the complexation capacity of the chelating monoliths. Scanning capacitively coupled contactless conductivity detection (sC(4)D) was used to characterise and verify homogenous distribution of the chelating ligand along the length of the capillaries non-invasively. Chelation ion chromatographic separations of selected transition and heavy metals were carried out, with retention factor data proportional to the concentration of grafted poly(GMA). Average peak efficiencies of close to 5,000 N/m were achieved, with the isocratic separation of Na, Mg(II), Mn(II), Co(II), Cd(II) and Zn(II) possible on a 250-mm-long monolith. Multiple monolithic columns produced to the same recipes gave RSD data for retention factors of ions). The monolithic chelating ion-exchanger was applied to the separation of alkaline earth and transition metal ions spiked in natural and potable waters.

  3. Determination of betaine, l-carnitine, and choline in human urine using a self-packed column and column-switching ion chromatography with nonsuppressed conductivity detection.

    Science.gov (United States)

    Wei, Dan; Liu, Junwei; Guo, Ming; Zhu, Yan

    2017-11-01

    A simple method for the determination of betaine, l-carnitine, and choline in human urine was developed based on column-switching ion chromatography coupled with nonsuppressed conductivity detection by using a self-packed column. A pretreatment column (50 mm × 4.6 mm, id) packed with poly(glycidyl methacrylate-divinylbenzene) microspheres was used for the extraction and cleanup of analytes. Chromatographic separation was achieved within 10 min on a cationic exchange column (150 mm × 4.6 mm, id) using maleic anhydride modified poly(glycidyl methacrylate-divinylbenzene) as the particles for packing. The detection was performed by ion chromatography with nonsuppressed conductivity detection. Parameters including column-switching time, eluent type, flow rates of eluent, and interfering effects were optimized. Linearity (r 2 ≥ 0.99) was obtained for the concentration range of 0.50-100, 0.75-100, and 0.25-100 μg/mL for betaine, l-carnitine, and choline, respectively. Detection limits were 0.12, 0.20, and 0.05 μg/mL for betaine, l-carnitine, and choline, respectively. The intra- and interday accuracy and precision for all quality controls were within ±10.11%. Satisfactory recovery was observed between 92.5 and 105.0%. The validated method was successfully applied for the determination of betaine, l-carnitine, and choline in urine samples from healthy people. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Hydrophilic interaction liquid chromatography/positive ion electrospray ionization mass spectrometry method for the quantification of alprazolam and α-hydroxy-alprazolam in human plasma.

    Science.gov (United States)

    Kalogria, Eleni; Pistos, Constantinos; Panderi, Irene

    2013-12-30

    A hydrophilic interaction liquid chromatography/positive ion electrospray-mass spectrometry (HILIC-ESI/MS) has been developed and fully validated for the quantification of alprazolam and its main metabolite, α-hydroxy-alprazolam, in human plasma. The assay is based on 50μL plasma samples, following liquid-liquid extraction. All analytes and the internal standard (tiamulin) were separated by hydrophilic interaction liquid chromatography using an X-Bridge-HILIC analytical column (150.0mm×2.1mm i.d., particle size 3.5μm) under isoscratic elution. The mobile phase was composed of a 7% 10mM ammonium formate water solution in acetonitrile and pumped at a flow rate of 0.20mLmin(-1). Running in positive electrospray ionization and selected ion monitoring (SIM) the mass spectrometer was set to analyze the protonated molecules [M+H](+) at m/z 309, 325 and 494 for alprazolam, α-hydroxy-alprazolam and tiamulin (ISTD) respectively. The assay was linear over the concentration range of 2.5-250ngmL(-1) for alprazolam and 2.5-50ngmL(-1) for α-hydroxy alprazolam. Intermediate precision was less than 4.1% over the tested concentration ranges. The method is the first reported application of HILIC in the analysis benzodiazepines in human plasma. With a small sample size (50μL human plasma) and a run time less than 10.0min for each sample the method can be used to support a wide range of clinical studies concerning alprazolam quantification. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. 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.

  6. Total iodine quantification in fluids and tissues from iodine- or iodide-supplemented rats by ion chromatography following microwave-assisted digestion.

    Science.gov (United States)

    Delgado, Guadalupe; Muñoz-Torres, Carolina; Orozco-Esquivel, Teresa; Anguiano, Brenda; Aceves, Carmen

    2015-03-01

    Iodine is a crucial component of thyroid hormones, and several reports have shown that iodine per se is implicated in the physiopathology of other organs. Innovative ion chromatography detection following a four-step temperature ramp microwave digestion in 25-50 mM nitric acid was developed to measure total iodine in biological fluids and tissue samples from female Sprague-Dawley rats supplemented with 0.05% molecular iodine (I2) or 0.05% potassium iodide (I(-)) in drinking water. The reported method allows the measurement of total iodine with a limit of quantification of 13.7 μg L(-1), recoveries of 96.3-100.3%, and intra- and inter-assay variations, of 3.5% and 7.4% respectively. Analysis of biological fluids showed that after 48 hours, iodine-supplemented animals exhibited significantly higher levels of total iodine in both serum and urine compared with those supplemented with iodide. The half-life of iodine in serum and urine measured over the first 48 h showed similar patterns for both the I2 (7.89 and 7.76 hours) and I(-) (8.27 and 8.90 hours) supplements. Differential uptake patterns were observed in tissues after 6 days of supplements, with I(-) preferentially retained by thyroid, lactating mammary gland, and milk, and a slightly but significantly higher capture of I2 in pituitary, ovary, and virgin mammary gland. We developed a rapid, selective, and accurate digestion method to process fluid and tissue samples that permits reproducible measurements of total iodine by ion chromatography; iodine or iodide supplement show a similar serum and urine half-life, but organ-specific uptake depends on the chemical form of the iodine supplement.

  7. Organic solvent and temperature-enhanced ion chromatography-high resolution mass spectrometry for the determination of low molecular weight organic and inorganic anions

    International Nuclear Information System (INIS)

    Gilchrist, Elizabeth S.; Nesterenko, Pavel N.; Smith, Norman W.; Barron, Leon P.

    2015-01-01

    Highlights: • IC selectivity at high contents of organic solvent in eluent and elevated temperature is studied. • Solvent-enhanced IC coupled to high resolution MS is beneficial for sensitive detection of ions. • The first application of IC-HRMS to the detection of low explosives in fingermarks is shown. - Abstract: There has recently been increased interest in coupling ion chromatography (IC) to high resolution mass spectrometry (HRMS) to enable highly sensitive and selective analysis. Herein, the first comprehensive study focusing on the direct coupling of suppressed IC to HRMS without the need for post-suppressor organic solvent modification is presented. Chromatographic selectivity and added HRMS sensitivity offered by organic solvent-modified IC eluents on a modern hyper-crosslinked polymeric anion-exchange resin (IonPac AS18) are shown using isocratic eluents containing 5–50 mM hydroxide with 0–80% methanol or acetonitrile for a range of low molecular weight anions (<165 Da). Comprehensive experiments on IC thermodynamics over a temperature range between 20–45 °C with the eluent containing up to 60% of acetonitrile or methanol revealed markedly different retention behaviour and selectivity for the selected analytes on the same polymer based ion-exchange resin. Optimised sensitivity with HRMS was achieved with as low as 30–40% organic eluent content. Analytical performance characteristics are presented and compared with other IC-MS based works. This study also presents the first application of IC-HRMS to forensic detection of trace low-order anionic explosive residues in latent human fingermarks

  8. Organic solvent and temperature-enhanced ion chromatography-high resolution mass spectrometry for the determination of low molecular weight organic and inorganic anions

    Energy Technology Data Exchange (ETDEWEB)

    Gilchrist, Elizabeth S. [Analytical & Environmental Science Division, Department of Forensic & Analytical Science, King’s College London, 150 Stamford Street, London, SE1 9NH (United Kingdom); Nesterenko, Pavel N. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart 7001 (Australia); Smith, Norman W. [Analytical & Environmental Science Division, Department of Forensic & Analytical Science, King’s College London, 150 Stamford Street, London, SE1 9NH (United Kingdom); Barron, Leon P., E-mail: leon.barron@kcl.ac.uk [Analytical & Environmental Science Division, Department of Forensic & Analytical Science, King’s College London, 150 Stamford Street, London, SE1 9NH (United Kingdom)

    2015-03-20

    Highlights: • IC selectivity at high contents of organic solvent in eluent and elevated temperature is studied. • Solvent-enhanced IC coupled to high resolution MS is beneficial for sensitive detection of ions. • The first application of IC-HRMS to the detection of low explosives in fingermarks is shown. - Abstract: There has recently been increased interest in coupling ion chromatography (IC) to high resolution mass spectrometry (HRMS) to enable highly sensitive and selective analysis. Herein, the first comprehensive study focusing on the direct coupling of suppressed IC to HRMS without the need for post-suppressor organic solvent modification is presented. Chromatographic selectivity and added HRMS sensitivity offered by organic solvent-modified IC eluents on a modern hyper-crosslinked polymeric anion-exchange resin (IonPac AS18) are shown using isocratic eluents containing 5–50 mM hydroxide with 0–80% methanol or acetonitrile for a range of low molecular weight anions (<165 Da). Comprehensive experiments on IC thermodynamics over a temperature range between 20–45 °C with the eluent containing up to 60% of acetonitrile or methanol revealed markedly different retention behaviour and selectivity for the selected analytes on the same polymer based ion-exchange resin. Optimised sensitivity with HRMS was achieved with as low as 30–40% organic eluent content. Analytical performance characteristics are presented and compared with other IC-MS based works. This study also presents the first application of IC-HRMS to forensic detection of trace low-order anionic explosive residues in latent human fingermarks.

  9. Correlated charge changing ion-atom collisions. Progress report, March 15, 1984-March 15, 1985

    International Nuclear Information System (INIS)

    Bernstein, E.M.; Tanis, J.A.

    1985-04-01

    Correlations between x-ray emission and projectile charge-changing events have been investigated for highly charged ions incident on gas targets under single collision conditions. Measurements were made for 100 to 360 MeV 20 Ca/sup 16,17,18+/ + He, 15 to 200 MeV 16 S 13+ + He, 100 to 370 MeV 20 Ca/sup 12,16,17,18,19+/ + H 2 , and 455 to 705 MeV 57 La 40+ + H 2 . Coincidences between electron capture and K x-ray emission for Ca/sup q+/ + H 2 and He, combined with previous measurements for 180 to 460 MeV 23 V/sup 19,20,21+/ + He, demonstrate the existence and substantiate the theory of resonant transfer and excitation (RTE). Additional K-shell RTE studies include theoretical calculations of the cross sections for Li-like ions with 14 less than or equal to Z less than or equal to 26 incident on He and Ne. The 57 La 40+ + H 2 measurements provide evidence for L-shell RTE. For S 13+ + He new evidence is obtained for nonresonant transfer and excitation, a two-step process in which uncorrelated electron capture and projectile excitation occur in a single encounter. Total electron capture cross sections for S 13+ + He vary by about 10 5 over the energy range investigated and are in reasonable agreement with empirical values. Other studies of electron capture and loss include measurements of the charge-state dependence for V/sup q+/ + He (q = 18 to 23) at 8.55 MeV/amu

  10. Quantification of urinary 0,0'-dityrosine, a biomarker for oxidative damage to proteins, by high performance liquid chromatography with triple quadrupole tandem mas spectrometry. A comparison with ion-trap tandem mass spectrometry.

    NARCIS (Netherlands)

    Orhan, H.; Coolen, S.; Meerman, J.H.N.

    2005-01-01

    We recently described an isotope dilution reversed-phase liquid chromatography-atmospheric pressure chemical ionization-ion-trap-tandem mass spectrometry (HPLC-APCI-MS/MS) method for the quantitative determination of oxidized amino acids in human urine, including o,o′-dityrosine, a specific marker

  11. Bioconversion of red ginseng saponins in the gastro-intestinal tract in vitro model studied by high-performance liquid chromatography-high resolution Fourier transform ion cyclotron resonance mass spectrometry

    NARCIS (Netherlands)

    Kong, H.; Wang, M.; Venema, K.; Maathuis, A.; Heijden, R. van der; Greef, J. van der; Xu, G.; Hankemeier, T.

    2009-01-01

    A high-performance liquid chromatography-high resolution Fourier transform ion cyclotron resonance mass spectrometry (HPLC-FTICR-MS) method was developed to investigate the metabolism of ginsenosides in in vitro models of the gastro-intestinal tract. The metabolites were identified by

  12. EFFECT OF DIFFERENT AMOUNTS OF THE NONIONIC DETERGENTS C-10E(5) AND C-12E(5) PRESENT IN ELUENTS FOR ION-EXCHANGE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY OF INTEGRAL MEMBRANE-PROTEINS OF SENDAI VIRUS

    NARCIS (Netherlands)

    WELLINGWESTER, S; FEIJLBRIEF, M; KOEDIJK, DGAM; BRAAKSMA, MA; DOUMA, BRK; WELLING, GW

    1993-01-01

    Non-ionic detergents (0.03-0.5%) are used as additives to the eluents when integral membrane proteins are subjected to ion-exchange high-performance liquid chromatography (HPIEC). It is not known whether this concentration should bear some relation to the critical micelle concentration (CMC) of a

  13. Application of the bidimensional ion-exchange chromatography for the laboratory preparation of different 15N enrichments and depletions

    International Nuclear Information System (INIS)

    Farjo, K.

    1989-01-01

    The ion-exchange application of the bidimensional solid/liquid technique for the preparation of different 15 N-abundances utilizing the isotope exchange system NH 4 + /NH 3 · aq is reported and the application of the technique for the separation of nitrogen isotopes is briefly discussed. (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. [Separation of p-aminobenzenearsonic acid and its oxide by ion-pair reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Kang, J; Ma, X; Meng, L; Ma, D

    1999-05-01

    To study the separation of p-aminobenzenearsonic acid (PABAA) and its oxide, p-aminophenylarsine oxide (PAPAO), both the absorption spectra were scanned at the wavelengths from 200 nm to 380 nm. PABAA had absorption maximum at 254 nm and PAPAO 258 nm. The effects of salt concentration, column temperature, methanol and ion-pair agent concentrations on the capacity factor were investigated. Compounds of high polarity showed almost no retention on reversed-phase column; as the volume fraction of the methanol decreased from 90% to 10%, the retention time of PABAA gradually increased with broad peak, and partially eluted when methanol volume fraction being below 20%. With temperature rising, the retention time of PABAA was decreased. But PABAA capacity factor can be increased by selecting an appropriate salt concentration for the mobile phase. The cetyltrimethyl and tetrabutyl ammonium ions were separately added as ion-pair agents to the mobile phase containing methanol in phosphate buffer of 10 mmol/L, the changes of retention time were observed. The mechanism of retention based on reversed phase ion-pair model is proposed. Besides, the retention behaviour is also influenced by size exclusion in stationary phase as well as polar interactions with residual silanol group on the silica surface.

  16. Improved sensitivity of ochratoxin A analysis in coffee using high-performance liquid chromatography with hybrid triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS).

    Science.gov (United States)

    Kokina, Aija; Pugajeva, Iveta; Bartkevics, Vadims

    2016-01-01

    A novel and sensitive method utilising high-performance liquid chromatography coupled to triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS) was developed in order to analyse the content of ochratoxin A (OTA) in coffee samples. The introduction of the triple-stage MS scanning mode (MS(3)) has been shown to increase greatly sensitivity and selectivity by eliminating the high chromatographic baseline caused by interference of complex coffee matrices. The analysis included the sample preparation procedure involving extraction of OTA using a methanol-water mixture and clean-up by immunoaffinity columns and detection using the MS(3) scanning mode of LC-QqQLIT-MS/MS. The proposed method offered a good linear correlation (r(2) > 0.998), excellent precision (RSD coffee beans and espresso beverages was 0.010 and 0.003 µg kg(-1), respectively. The developed procedure was compared with traditional methods employing liquid chromatography coupled to fluorescent and tandem quadrupole detectors in conjunction with QuEChERS and solid-phase extraction. The proposed method was successfully applied to the determination of OTA in 15 samples of coffee beans and in 15 samples of espresso coffee beverages obtained from the Latvian market. OTA was found in 10 samples of coffee beans and in two samples of espresso in the ranges of 0.018-1.80 µg kg(-1) and 0.020-0.440 µg l(-1), respectively. No samples exceeded the maximum permitted level of OTA in the European Union (5.0 µg kg(-1)).

  17. A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

    2003-01-01

    A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

  18. Simultaneous Analysis of Monovalent Anions and Cations with a Sub-Microliter Dead-Volume Flow-Through Potentiometric Detector for Ion Chromatography

    Science.gov (United States)

    Dumanli, Rukiye; Attar, Azade; Erci, Vildan; Isildak, Ibrahim

    2016-01-01

    A microliter dead-volume flow-through cell as a potentiometric detector is described in this article for sensitive, selective and simultaneous detection of common monovalent anions and cations in single column ion chromatography for the first time. The detection cell consisted of less selective anion- and cation-selective composite membrane electrodes together with a solid-state composite matrix reference electrode. The simultaneous separation and sensitive detection of sodium (Na+), potassium (K+), ammonium (NH4+), chloride (Cl−) and nitrate (NO3−) in a single run was achieved by using 98% 1.5 mM MgSO4 and 2% acetonitrile eluent with a mixed-bed ion-exchange separation column without suppressor column system. The separation and simultaneous detection of the anions and cations were completed in 6 min at the eluent flow-rate of 0.8 mL/min. Detection limits, at S/N = 3, were ranged from 0.2 to 1.0 µM for the anions and 0.3 to 3.0 µM for the cations, respectively. The developed method was successfully applied to the simultaneous determination of monovalent anions and cations in several environmental and biological samples. PMID:26786906

  19. Monitoring of selected skin- and breath-borne volatile organic compounds emitted from the human body using gas chromatography ion mobility spectrometry (GC-IMS).

    Science.gov (United States)

    Mochalski, Paweł; Wiesenhofer, Helmut; Allers, Maria; Zimmermann, Stefan; Güntner, Andreas T; Pineau, Nicolay J; Lederer, Wolfgang; Agapiou, Agapios; Mayhew, Christopher A; Ruzsanyi, Veronika

    2018-02-15

    Human smuggling and associated cross-border crimes have evolved as a major challenge for the European Union in recent years. Of particular concern is the increasing trend of smuggling migrants hidden inside shipping containers or trucks. Therefore, there is a growing demand for portable security devices for the non-intrusive and rapid monitoring of containers to detect people hiding inside. In this context, chemical analysis of volatiles organic compounds (VOCs) emitted from the human body is proposed as a locating tool. In the present study, an in-house made ion mobility spectrometer coupled with gas chromatography (GC-IMS) was used to monitor the volatile moieties released from the human body under conditions that mimic entrapment. A total of 17 omnipresent volatile compounds were identified and quantified from 35 ion mobility peaks corresponding to human presence. These are 7 aldehydes (acrolein, 2-methylpropanal, 3-methylbutanal, 2-ethacrolein, n-hexanal, n-heptanal, benzaldehyde), 3 ketones (acetone, 2-pentanone, 4-methyl-2-pentanone), 5 esters (ethyl formate, ethyl propionate, vinyl butyrate, butyl acetate, ethyl isovalerate), one alcohol (2-methyl-1-propanol) and one organic acid (acetic acid). The limits of detection (0.05-7.2 ppb) and relative standard deviations (0.6-11%) should be sufficient for detecting these markers of human presence in field conditions. This study shows that GC-IMS can be used as a portable field detector of hidden or entrapped people. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Sensitive measurement of vinorelbine in dog plasma by liquid chromatography-electrospray ionization tandem mass spectrometry utilizing transitions from double-charged precursor ions.

    Science.gov (United States)

    Niwa, Makoto; Kawashiro, Takashi

    2011-04-01

    A sensitive high-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for measuring vinorelbine was developed. A 100 µL aliquot of plasma was spiked with deuterium-labeled internal standard and subjected to solid-phase extraction using an Oasis HLB μ-elution plate. Two microliters of the extracted samples was directly injected into LC/MS/MS. Chromatographic separation was achieved on a Capcell Pak C18 UG column (2 × 75 mm) with a gradient elution of methanol (mobile phase B) against 0.05% formic acid in aqueous 10 mm ammonium formate (mobile phase A). The LC flow rate was set to 0.28 mL/min and the gradient (solvent B concentration) was processed from 40 to 90%. In mass spectrometric detection, observation of the reaction from a double-charged precursor ion [M + 2H](2+) (m/z 390) to product ion m/z 122 provided very high sensitivity. The method was validated with a lower limit of detection of 0.2 ng/mL with 0.1 mL of plasma, and the method was used to determine the plasma pharmacokinetics of vinorelbine in dogs. Copyright © 2010 John Wiley & Sons, Ltd.

  1. The rapid and direct determination of ATPase activity by ion exchange chromatography and the application to the activity of heat shock protein-90.

    Science.gov (United States)

    Bartolini, Manuela; Wainer, Irving W; Bertucci, Carlo; Andrisano, Vincenza

    2013-01-25

    Adenosine nucleotides are involved as substrates or co-factors in several biochemical reactions, catalyzed by enzymes, which modulate energy production, signal transduction and cell proliferation. We here report the development and optimization of an ion exchange liquid chromatography (LC) method for the determination of ATP, ADP and AMP. This method is specifically aimed at the determination of the ATP-ase activity of human heat shock protein 90 (Hsp90), a molecular chaperone that has emerged as target enzyme in cancer therapy. Separation of the three nucleotides was achieved in a 15-min run by using a disk shaped monolithic ethylene diamine stationary phase of small dimensions (2mm×6mm i.d.), under a three-solvent gradient elution mode and UV detection at 256nm. The described direct LC method resulted highly specific as a consequence of the baseline separation of the three adenosine nucleotides and could be applied to the determination of the enzymatic activity of ADP/ATP generating or consuming enzymes (such as kinases). Furthermore, comparison of the LOD and LOQ values of the LC method with those obtained with the malachite green assay, which is one of the most used indirect screening methodologies for ATP-ase activity, showed that the LC method has a similar range of application without presenting the drawbacks related to contamination by inorganic phosphate ions and glycerol, which are present in Hsp90 commercial samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Application of ultra-high pressure liquid chromatography linear ion-trap orbitrap to qualitative and quantitative assessment of pesticide residues.

    Science.gov (United States)

    Farré, M; Picó, Y; Barceló, D

    2014-02-07

    The analysis of pesticides residues using a last generation high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS) was explored. Pesticides were extracted from fruits, fish, bees and sediments by QuEChERS and from water by solid-phase with Oasis HLB cartridges. Ultra-high pressure liquid chromatography (UHPLC)-LTQ-Orbitrap mass spectrometer acquired full scan MS data for quantification, and data dependent (dd) MS(2) and MS(3) product ion spectra for identification and/or confirmation. The regression coefficients (r(2)) for the calibration curves (two order of magnitude up to the lowest calibration level) in the study were ≥0.99. The LODs for 54 validated compounds were ≤2ngmL(-1) (analytical standards). The relative standard deviation (RSD), which was used to estimate precision, was always lower than 22%. The recovery of extraction and matrix effects ranged from 58 to 120% and from -92 to 52%, respectively. Mass accuracy was always ≤4ppm, corresponding to a maximum mass error of 1.6millimass units (mmu). This procedure was then successfully applied to pesticide residues in a set of the above-mentioned food and environmental samples. In addition to target analytes, this method enables the simultaneous detection/identification of non-target pesticides, pharmaceuticals, drugs of abuse, mycotoxins, and their metabolites. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Urinary free cortisol assessment by liquid chromatography tandem mass spectrometry: a case study of ion suppression due to unacquainted administration of piperacillin

    Science.gov (United States)

    Danese, Elisa; Salvagno, Gian Luca; Guzzo, Alessandra; Scurati, Samuele; Fava, Cristiano; Lippi, Giuseppe

    2017-01-01

    Introduction Liquid chromatography coupled to atmospheric pressure ionization tandem mass spectrometry (LC-ESI-MS/MS) is currently considered the reference method for quantitative determination of urinary free cortisol (UFC). One of the major drawbacks of this measurement is a particular form of matrix effect, conventionally known as ion suppression. Materials and methods We describe here the case of a 66-year-old-patient referred to the daily service of general medicine for intravenous antibiotic administration due to a generalized Staphylococcus aureus infection and for routine 24 hours UFC monitoring in the setting of glucocorticoid replacement therapy. Results The observation of 10-fold decrease of internal standard of cortisol signal led us to hypothesize the presence of an ion suppression effect due to a co-eluting endogenous compound. Screening analysis of tandem mass spectrometry (MS/MS) spectra of the interfering molecule, along with in vitro confirmation analyses, were suggestive of the presence of high concentration of piperacillin. The problem was then easily solved with minor modifications of the chromatographic technique. Conclusions According to our findings, antibiotic therapy with piperacillin/tazobactam should be regarded as an important interference in UFC assessment, which may potentially affect detection capability, precision and accuracy of this measurement. This case report emphasizes that accurate anamnesis and standardization of all phases of urine collection are essential aspects for preventing potential interference in laboratory testing. PMID:29180920

  4. Gas chromatography/ion trap mass spectrometry applied for the analysis of triazine herbicides in environmental waters by an isotope dilution technique

    International Nuclear Information System (INIS)

    Cai Zongwei; Wang Dongli; Ma, W.T.

    2004-01-01

    A gas chromatography/ion trap mass spectrometry method was developed for the analysis of simazine, atrazine, cyanazine, as well as the degradation products of atrazine, such as deethylatrazine and deisopropylatrazine in environmental water samples. Isotope dilution technique was applied for the quantitative analysis of atrazine in water at low ng/l levels. One liter of water sample spiked with stable isotope internal standard atrazine-d 5 was extracted with a C 18 solid-phase extraction cartridge. The analysis was performed on an ion trap mass spectrometer operated in MS/MS method. The extraction recoveries were in the range of 83-94% for the triazine herbicides in water at the concentrations of 24, 200, and 1000 ng/l, while poor recoveries were obtained for the degradation products of atrazine. The relative standard deviation (R.S.D.) were within the range of 3.2-16.1%. The detection limits of the method were between 0.75 and 12 ng/l when 1 l of water was analyzed. The method was successfully applied to analyze environmental water samples collected from a reservoir and a river in Hong Kong for atrazine detected at concentrations between 3.4 and 26 ng/l

  5. Supercritical carbon dioxide extraction of electrolyte from spent lithium ion batteries and its characterization by gas chromatography with chemical ionization

    Science.gov (United States)

    Mönnighoff, Xaver; Friesen, Alex; Konersmann, Benedikt; Horsthemke, Fabian; Grützke, Martin; Winter, Martin; Nowak, Sascha

    2017-06-01

    The aging products of the electrolyte from a commercially available state-of-the-art 18650-type cell were investigated. During long term cycling a huge difference in their performance and lifetime at different temperatures was observed. By interpretation of a strong capacity fading of cells cycled at 20 °C compared to cells cycled at 45 °C a temperature depending aging mechanism was determined. To investigate the influence of the electrolyte on this fading, the electrolyte was extracted by supercritical fluid extraction (SFE) and then analyzed by gas chromatography (GC) with electron impact (EI) ionization and mass selective detection. To obtain more information with regard to the identification of unknown decomposition products further analysis with positive chemical ionization (PCI) and negative chemical ionization (NCI) was performed. 17 different volatile organic aging products were detected and identified. So far, seven of them were not yet known in literature and several formation pathways were postulated taking previously published literature into account.

  6. Separation of metals in the form of ion associates by the method of thin-layer chromatography

    International Nuclear Information System (INIS)

    Shapovalova, E.N.; Timerbaev, A.R.; Bol'shova, T.A.; Mel'nik, S.V.; Kordejro, E.

    1990-01-01

    Behaviour of pyridylazo resorcinates of certain metals (Ga, In, Fe, Co) in the form of ionic pairs with tri-n-octylamine (TOA) under conditions of thin-layer chromatography (TLC) has been studied. For all eluents investigated Ga and In complexes possess the highest mobility. Selectivity of ionic associate separation decreases with an increase in mobile phase polarity. Mixtures with 10-15 % content of isopropanol in eluating solution are the optimal ones. Separation of Ga and In from Fe 3+ and Co takes place with separation criterion 3.1 and 4.1 respectively. An attempt to separate ionic associates of In and Ga failed owing to similar stability of their pyridylazoresorcinates. Solution of the problem of In and Ga determination in the presence of iron can contribute to concrete application of the method

  7. Correlation between surface phonon mode and luminescence in nanocrystalline CdS thin films: An effect of ion beam irradiation

    International Nuclear Information System (INIS)

    Kumar, Pragati; Agarwal, Avinash; Saxena, Nupur; Singh, Fouran; Gupta, Vinay

    2014-01-01

    The influence of swift heavy ion irradiation (SHII) on surface phonon mode (SPM) and green emission in nanocrystalline CdS thin films grown by chemical bath deposition is studied. The SHII of nanocrystalline CdS thin films is carried out using 70 MeV Ni ions. The micro Raman analysis shows that asymmetry and broadening in fundamental longitudinal optical (LO) phonon mode increases systematically with increasing ion fluence. To analyze the role of phonon confinement, spatial correlation model (SCM) is fitted to the experimental data. The observed deviation of SCM to the experimental data is further investigated by fitting the micro Raman spectra using two Lorentzian line shapes. It is found that two Lorentzian functions (LFs) provide better fitting than SCM fitting and facilitate to identify the contribution of SPM in the observed distortion of LO mode. The behavior of SPM as a function of ion fluence is studied to correlate the observed asymmetry (Γ a /Γ b ) and full width at half maximum of LO phonon mode and to understand the SHII induced enhancement of SPM. The ion beam induced interstitial and surface state defects in thin films, as observed by photoluminescence (PL) spectroscopy studies, may be the underlying reason for enhancement in SPM. PL studies also show enhancement in green luminescence with increase in ion fluence. PL analysis reveals that the variation in population density of surface state defects after SHII is similar to that of SPM. The correlation between SPM and luminescence and their dependence on ion irradiation fluence is explained with the help of thermal spike model.

  8. Correlation between surface phonon mode and luminescence in nanocrystalline CdS thin films: An effect of ion beam irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Pragati, E-mail: pkumar.phy@gmail.com; Agarwal, Avinash [Department of Physics, Bareilly College, Bareilly 243 005, Uttar Pradesh (India); Saxena, Nupur; Singh, Fouran [Inter University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110 067 (India); Gupta, Vinay [Department of Physics and Astrophysics, University of Delhi, Delhi 110 007 (India)

    2014-07-28

    The influence of swift heavy ion irradiation (SHII) on surface phonon mode (SPM) and green emission in nanocrystalline CdS thin films grown by chemical bath deposition is studied. The SHII of nanocrystalline CdS thin films is carried out using 70 MeV Ni ions. The micro Raman analysis shows that asymmetry and broadening in fundamental longitudinal optical (LO) phonon mode increases systematically with increasing ion fluence. To analyze the role of phonon confinement, spatial correlation model (SCM) is fitted to the experimental data. The observed deviation of SCM to the experimental data is further investigated by fitting the micro Raman spectra using two Lorentzian line shapes. It is found that two Lorentzian functions (LFs) provide better fitting than SCM fitting and facilitate to identify the contribution of SPM in the observed distortion of LO mode. The behavior of SPM as a function of ion fluence is studied to correlate the observed asymmetry (Γ{sub a}/Γ{sub b}) and full width at half maximum of LO phonon mode and to understand the SHII induced enhancement of SPM. The ion beam induced interstitial and surface state defects in thin films, as observed by photoluminescence (PL) spectroscopy studies, may be the underlying reason for enhancement in SPM. PL studies also show enhancement in green luminescence with increase in ion fluence. PL analysis reveals that the variation in population density of surface state defects after SHII is similar to that of SPM. The correlation between SPM and luminescence and their dependence on ion irradiation fluence is explained with the help of thermal spike model.

  9. Baryon Anomaly in Heavy-Ion Collisions and Colour Correlations in QGP

    CERN Document Server

    Levin, Eugene M; Ryskin, Mikhail G; Safarik, Karel

    2013-01-01

    A baryon anomaly – an increased baryon-to-meson production ratio at intermediate pT in heavyion collisions when compared to pp collisions – is observed at RHIC and the LHC. This effect is usually explained by recombination of constituent quarks during QGP hadronization, or as a consequence of a strong radial flow developed during the heavy-ion collision. In this contribution, an additional mechanism to favour baryon over meson production is proposed: when hadrons are formed in the recombination of nearby quarks and antiquarks, only colour-singlet combinations can be chosen. Hadron formation, in particular the probability to create baryons or mesons, depends on the distribution of colour charges among quarks. If the distribution is random – a reasonable assumption for Quark–Gluon Plasma (QGP) – the baryon-to-meson ratio is nearly twice higher than in the situation where quark colours are pre-arranged to obtain a white hadron in the combination of nearest quarks and antiquarks. The correlation of colo...

  10. Fast and sensitive determination of Sr-90 and SR-89 activity in milk by ion-chromatography and liquid scintillation

    International Nuclear Information System (INIS)

    Figueiredo, V.; Herrmann, A.

    1992-01-01

    A method for fast and exact determination of both strontium isotopes in milk and other foodstuffs, combination high performance ion chromatographic separation with by liquid scintillation counting, which enables the desired results to be obtained with very satisfactory precision and reproducibility within 24 hours, has been developed. The lowest detectable activity lies by 3 Bq/liter for Sr-90 and 1 Bq/liter for Sr-89 which is satisfactory for assessing a situation in a time crisis. (author)

  11. Screening of Carotenoids in Tomato Fruits by Using Liquid Chromatography with Diode Array-Linear Ion Trap Mass Spectrometry Detection.

    Science.gov (United States)

    Gentili, Alessandra; Caretti, Fulvia; Ventura, Salvatore; Pérez-Fernández, Virginia; Venditti, Alessandro; Curini, Roberta

    2015-08-26

    This paper presents an analytical strategy for a large-scale screening of carotenoids in tomato fruits by exploiting the potentialities of the triple quadrupole-linear ion trap hybrid mass spectrometer (QqQLIT). The method involves separation on C30 reversed-phase column and identification by means of diode array detection (DAD) and atmospheric pressure chemical ionization-mass spectrometry (APCI-MS). The authentic standards of six model compounds were used to optimize the separative conditions and to predict the chromatographic behavior of untargeted carotenoids. An information dependent acquisition (IDA) was performed with (i) enhanced-mass scan (EMS) as the survey scan, (ii) enhanced-resolution (ER) scan to obtain the exact mass of the precursor ions (16-35 ppm), and (iii) enhanced product ion (EPI) scan as dependent scan to obtain structural information. LC-DAD-multiple reaction monitoring (MRM) chromatograms were also acquired for the identification of targeted carotenoids occurring at low concentrations; for the first time, the relative abundance between the MRM transitions (ion ratio) was used as an extra tool for the MS distinction of structural isomers and the related families of geometrical isomers. The whole analytical strategy was high-throughput, because a great number of experimental data could be acquired with few analytical steps, and cost-effective, because only few standards were used; when applied to characterize some tomato varieties ('Tangerine', 'Pachino', 'Datterino', and 'Camone') and passata of 'San Marzano' tomatoes, our method succeeded in identifying up to 44 carotenoids in the 'Tangerine'" variety.

  12. Determining Double Bond Position in Lipids Using Online Ozonolysis Coupled to Liquid Chromatography and Ion Mobility-Mass Spectrometry.

    Science.gov (United States)

    Harris, Rachel A; May, Jody C; Stinson, Craig A; Xia, Yu; McLean, John A

    2018-02-06

    The increasing focus on lipid metabolism has revealed a need for analytical techniques capable of structurally characterizing lipids with a high degree of specificity. Lipids can exist as any one of a large number of double bond positional isomers, which are indistinguishable by single-stage mass spectrometry alone. Ozonolysis reactions coupled to mass spectrometry have previously been demonstrated as a means for localizing double bonds in unsaturated lipids. Here we describe an online, solution-phase reactor using ozone produced via a low-pressure mercury lamp, which generates aldehyde products diagnostic of cleavage at a particular double bond position. This flow-cell device is utilized in conjunction with structurally selective ion mobility-mass spectrometry. The lamp-mediated reaction was found to be effective for multiple lipid species in both positive and negative ionization modes, and the conversion efficiency from precursor to product ions was tunable across a wide range (20-95%) by varying the flow rate through the ozonolysis device. Ion mobility separation of the ozonolysis products generated additional structural information and revealed the presence of saturated species in a complex mixture. The method presented here is simple, robust, and readily coupled to existing instrument platforms with minimal modifications necessary. For these reasons, application to standard lipidomic workflows is possible and aids in more comprehensive structural characterization of a myriad of lipid species.

  13. Qualitative Metabolome Analysis of Human Cerebrospinal Fluid by 13C-/12C-Isotope Dansylation Labeling Combined with Liquid Chromatography Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    Science.gov (United States)

    Guo, Kevin; Bamforth, Fiona; Li, Liang

    2011-02-01

    Metabolome analysis of human cerebrospinal fluid (CSF) is challenging because of low abundance of metabolites present in a small volume of sample. We describe and apply a sensitive isotope labeling LC-MS technique for qualitative analysis of the CSF metabolome. After a CSF sample is divided into two aliquots, they are labeled by 13C-dansyl and 12C-dansyl chloride, respectively. The differentially labeled aliquots are then mixed and subjected to LC-MS using Fourier-transform ion cyclotron resonance mass spectrometry (FTICR MS). Dansylation offers significant improvement in the performance of chromatography separation and detection sensitivity. Moreover, peaks detected in the mass spectra can be readily analyzed for ion pair recognition and database search based on accurate mass and/or retention time information. It is shown that about 14,000 features can be detected in a 25-min LC-FTICR MS run of a dansyl-labeled CSF sample, from which about 500 metabolites can be profiled. Results from four CSF samples are compared to gauge the detectability of metabolites by this method. About 261 metabolites are commonly detected in replicate runs of four samples. In total, 1132 unique metabolite ion pairs are detected and 347 pairs (31%) matched with at least one metabolite in the Human Metabolome Database. We also report a dansylation library of 220 standard compounds and, using this library, about 85 metabolites can be positively identified. Among them, 21 metabolites have never been reported to be associated with CSF. These results illustrate that the dansylation LC-FTICR MS method can be used to analyze the CSF metabolome in a more comprehensive manner.

  14. High-throughput screening and quantitation of guanidino and ureido compounds using liquid chromatography-drift tube ion mobility spectrometry-mass spectrometry.

    Science.gov (United States)

    Fan, Ruo-Jing; Zhang, Fang; Chen, Xiu-Ping; Qi, Wan-Shu; Guan, Qing; Sun, Tuan-Qi; Guo, Yin-Long

    2017-04-08

    The present work focused on the high-throughput screening and quantitation of guanidino compounds (GCs) and ureido compounds (UCs) in human thyroid tissues. The strategy employed benzylic rearrangement stable isotope labeling (BRSIL) for the sample preparation and then detection using liquid chromatography-drift tube ion mobility spectrometry-quadrupole time of flight mass spectrometry (LC-DTIMS-QTOF MS). A short reversed-phase LC realized an on-line desalting and a measurement cycle of 5.0 min. DTIMS separation enhanced the better specificity and selectivity for the benzil labeled GCs and UCs. The elevated mass resolution of QTOF MS enabled measure of the characteristic ions at accurate mass in MS and tandem MS spectra. Collision cross section (CCS) from DTIMS and accurate mass from QTOF MS were used as two qualifiers for the profiling and identification of GCs and UCs. In addition, an integral abundance arising from 3-D ion features (retention time, drift time, m/z) was applied to quantify the GCs and UCs in human thyroid tissues. The quantitative validation indicated good linearity (coefficient values ≥ 0.9981), good precision (1.0%-12.3% for intra-day and 0.9%-7.8% for inter-day) and good accuracy (91%-109%). The results demonstrated that the developed BRSIL coupled with LC-DTIMS-QTOF MS can be a powerful analysis platform to investigate GCs and UCs in human thyroid tissues. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Determination of hexavalent chromium concentration in industrial waste incinerator stack gas by using a modified ion chromatography with post-column derivatization method.

    Science.gov (United States)

    Miyake, Yuichi; Tokumura, Masahiro; Iwazaki, Yuta; Wang, Qi; Amagai, Takashi; Horii, Yuichi; Otsuka, Hideyuki; Tanikawa, Noboru; Kobayashi, Takeshi; Oguchi, Masahiro

    2017-06-16

    An ion chromatography with post-column derivatization with 1,5-diphenylcarbazide (IC-DPC) analytical method was modified to enable measurement of trace-level hexavalent chromium (Cr(VI)) in air. One of the difficulties in determining trace levels of Cr(VI) in air with conventional IC-DPC methods is co-elution of the solvent and ion peaks due to high concentrations of ionic compounds in the extract. However, by using gradient elution rather than isocratic elution we were able to fully resolve the Cr(VI) ion peak from the solvent peak without the need for diluting the extract, which would have reduced the minimum quantifiable level of the method. With this method, we were able to detect Cr(VI) in air at concentrations of 5.3ng/m 3 (assuming a sampling volume of 1m 3 and a final solution volume of 10mL). Recovery tests at three different concentrations of Cr(VI) (50, 250, 1000ng) were performed with or without fly ash; recovery rates at all the concentrations of Cr(VI), with or without fly ash, ranged from 68% to 110% (mean±relative standard deviation, 96%±11%), and there were no differences in recovery rates with respect to the presence or absence of fly ash. Finally, we used the developed method to determine the concentration of Cr(VI) in stack gases collected from eight industrial waste incinerators located in Japan. The concentration of Cr(VI) in the stack gases ranged from below the method quantification limit to 3100ng/m 3 . The highest concentrations of Cr(VI) detected in the stack gases were two to three orders of magnitude higher than that in ambient air in Japan. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Characterization of a PEGylated protein therapeutic by ion exchange chromatography with on-line detection by native ESI MS and MS/MS.

    Science.gov (United States)

    Muneeruddin, K; Bobst, C E; Frenkel, R; Houde, D; Turyan, I; Sosic, Z; Kaltashov, I A

    2017-01-16

    Detailed profiling of both enzymatic (e.g., glycosylation) and non-enzymatic (e.g., oxidation and deamidation) post-translational modifications (PTMs) is frequently required for the quality assessment of protein-based drugs. Challenging as it is, this task is further complicated for the so-called second-generation biopharmaceuticals, which also contain "designer PTMs" introduced to either enhance their pharmacokinetic profiles (e.g., PEGylated proteins) or endow them with therapeutic activity (e.g., protein-drug conjugates). Such modifications of protein covalent structure can dramatically increase structural heterogeneity, making the very notion of "molecular mass" meaningless, as ions representing different glycoforms of a PEGylated protein may have nearly identical distributions of ionic current as a function of m/z, making their contributions to the mass spectrum impossible to distinguish. In this work we demonstrate that a combination of ion exchange chromatography (IXC) with on-line detection by electrospray ionization mass spectrometry (ESI MS) and methods of ion manipulation in the gas phase (limited charge reduction and collision-induced dissociation) allows meaningful structural information to be obtained on a structurally heterogeneous sample of PEGylated interferon β-1a. IXC profiling of the protein sample gives rise to a convoluted chromatogram with several partially resolved peaks which can represent both deamidation and different glycosylation patterns within the protein, as well as varying extent of PEGylation. Thus, profiling the protein with on-line IXC/ESI/MS/MS allows it to be characterized by providing information on three different types of PTMs (designer, enzymatic and non-enzymatic) within a single protein therapeutic.

  17. Qualitative metabolome analysis of human cerebrospinal fluid by 13C-/12C-isotope dansylation labeling combined with liquid chromatography Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Guo, Kevin; Bamforth, Fiona; Li, Liang

    2011-02-01

    Metabolome analysis of human cerebrospinal fluid (CSF) is challenging because of low abundance of metabolites present in a small volume of sample. We describe and apply a sensitive isotope labeling LC-MS technique for qualitative analysis of the CSF metabolome. After a CSF sample is divided into two aliquots, they are labeled by (13)C-dansyl and (12)C-dansyl chloride, respectively. The differentially labeled aliquots are then mixed and subjected to LC-MS using Fourier-transform ion cyclotron resonance mass spectrometry (FTICR MS). Dansylation offers significant improvement in the performance of chromatography separation and detection sensitivity. Moreover, peaks detected in the mass spectra can be readily analyzed for ion pair recognition and database search based on accurate mass and/or retention time information. It is shown that about 14,000 features can be detected in a 25-min LC-FTICR MS run of a dansyl-labeled CSF sample, from which about 500 metabolites can be profiled. Results from four CSF samples are compared to gauge the detectability of metabolites by this method. About 261 metabolites are commonly detected in replicate runs of four samples. In total, 1132 unique metabolite ion pairs are detected and 347 pairs (31%) matched with at least one metabolite in the Human Metabolome Database. We also report a dansylation library of 220 standard compounds and, using this library, about 85 metabolites can be positively identified. Among them, 21 metabolites have never been reported to be associated with CSF. These results illustrate that the dansylation LC-FTICR MS method can be used to analyze the CSF metabolome in a more comprehensive manner. © American Society for Mass Spectrometry, 2011

  18. Correlation of shear and dielectric ion viscosity of dental resins - Influence of composition, temperature and filler content.

    Science.gov (United States)

    Steinhaus, Johannes; Hausnerova, Berenika; Haenel, Thomas; Selig, Daniela; Duvenbeck, Fabian; Moeginger, Bernhard

    2016-07-01

    Shear viscosity and ion viscosity of uncured visible light-curing (VLC) resins and resin based composites (RBC) are correlated with respect to the resin composition, temperature and filler content to check where Dielectric Analysis (DEA) investigations of VLC RBC generate similar results as viscosity measurements. Mixtures of bisphenol A glycidyl methacrylate (Bis-GMA) and triethylene glycol dimethacrylate (TEGDMA) as well as the pure resins were investigated and compared with two commercial VLC dental resins and RBCs (VOCO, Arabesk Top and Grandio). Shear viscosity data was obtained using a Haake Mars III, Thermo Scientific. Ion viscosity measurements performed by a dielectric cure analyzer (DEA 231/1 Epsilon with Mini IDEX-Sensor, Netzsch-Gerätebau). Shear viscosity depends reciprocally on the mobility of molecules, whereas the ion viscosity also depends on the ion concentration as it is affected by both ion concentration and mixture viscosity. Except of pure TEGDMA, shear and ion viscosities depend on the resin composition qualitatively in a similar manner. Furthermore, shear and ion viscosities of the commercial VLC dental resins and composites exhibited the same temperature dependency regardless of filler content. Application of typical rheological models (Kitano and Quemada) revealed that ion viscosity measurements can be described with respect to filler contents of up to 30vol.%. Rheological behavior of a VLC RBC can be characterized by DEA under the condition that the ion concentration is kept constant. Both methods address the same physical phenomenon - motion of molecules. The proposed relations allows for calculating the viscosity of any Bis-GMA-TEGDMA mixture on the base of the viscosities of the pure components. This study demonstrated the applicability of DEA investigations of VLC RBCs with respect to quality assurance purposes. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  19. Three-pion Hanbury Brown-Twiss correlations in relativistic heavy-ion collisions from the STAR experiment.

    Science.gov (United States)

    Adams, J; Adler, C; Ahammed, Z; Allgower, C; Amonett, J; Anderson, B D; Anderson, M; Arkhipkin, D; Averichev, G S; Balewski, J; Barannikova, O; Barnby, L S; Baudot, J; Bekele, S; Belaga, V V; Bellwied, R; Berger, J; Bichsel, H; Billmeier, A; Bland, L C; Blyth, C O; Bonner, B E; Botje, M; Boucham, A; Brandin, A; Bravar, A; Cadman, R V; Cai, X Z; Caines, H; Calderón de la Barca Sánchez, M; Cardenas, A; Carroll, J; Castillo, J; Castro, M; Cebra, D; Chaloupka, P; Chattopadhyay, S; Chen, Y; Chernenko, S P; Cherney, M; Chikanian, A; Choi, B; Christie, W; Coffin, J P; Cormier, T M; Mora Corral, M; Cramer, J G; Crawford, H J; Derevschikov, A A; Didenko, L; Dietel, T; Draper, J E; Dunin, V B; Dunlop, J C; Eckardt, V; Efimov, L G; Emelianov, V; Engelage, J; Eppley, G; Erazmus, B; Fachini, P; Faine, V; Faivre, J; Fatemi, R; Filimonov, K; Finch, E; Fisyak, Y; Flierl, D; Foley, K J; Fu, J; Gagliardi, C A; Gagunashvili, N; Gans, J; Gaudichet, L; Germain, M; Geurts, F; Ghazikhanian, V; Grachov, O; Guedon, M; Guertin, S M; Gushin, E; Gutierrez, T D; Hallman, T J; Hardtke, D; Harris, J W; Heinz, M; Henry, T W; Heppelmann, S; Herston, T; Hippolyte, B; Hirsch, A; Hjort, E; Hoffmann, G W; Horsley, M; Huang, H Z; Humanic, T J; Igo, G; Ishihara, A; Jacobs, P; Jacobs, W W; Janik, M; Johnson, I; Jones, P G; Judd, E G; Kabana, S; Kaneta, M; Kaplan, M; Keane, D; Kiryluk, J; Kisiel, A; Klay, J; Klein, S R; Klyachko, A; Kollegger, T; Konstantinov, A S; Kopytine, M; Kotchenda, L; Kovalenko, A D; Kramer, M; Kravtsov, P; Krueger, K; Kuhn, C; Kulikov, A I; Kunde, G J; Kunz, C L; Kutuev, R Kh; Kuznetsov, A A; Lamont, M A C; Landgraf, J M; Lange, S; Lansdell, C P; Lasiuk, B; Laue, F; Lauret, J; Lebedev, A; Lednický, R; Leontiev, V M; LeVine, M J; Li, Q; Lindenbaum, S J; Lisa, M A; Liu, F; Liu, L; Liu, Z; Liu, Q J; Ljubicic, T; Llope, W J; Long, H; Longacre, R S; Lopez-Noriega, M; Love, W A; Ludlam, T; Lynn, D; Ma, J; Ma, Y G; Magestro, D; Majka, R; Margetis, S; Markert, C; Martin, L; Marx, J; Matis, H S; Matulenko, Yu A; McShane, T S; Meissner, F; Melnick, Yu; Meschanin, A; Messer, M; Miller, M L; Milosevich, Z; Minaev, N G; Mitchell, J; Molnar, L; Moore, C F; Morozov, V; de Moura, M M; Munhoz, M G; Nelson, J M; Nevski, P; Nikitin, V A; Nogach, L V; Norman, B; Nurushev, S B; Odyniec, G; Ogawa, A; Okorokov, V; Oldenburg, M; Olson, D; Paic, G; Pandey, S U; Panebratsev, Y; Panitkin, S Y; Pavlinov, A I; Pawlak, T; Perevoztchikov, V; Peryt, W; Petrov, V A; Picha, R; Planinic, M; Pluta, J; Porile, N; Porter, J; Poskanzer, A M; Potrebenikova, E; Prindle, D; Pruneau, C; Putschke, J; Rai, G; Rakness, G; Ravel, O; Ray, R L; Razin, S V; Reichhold, D; Reid, J G; Renault, G; Retiere, F; Ridiger, A; Ritter, H G; Roberts, J B; Rogachevski, O V; Romero, J L; Rose, A; Roy, C; Rykov, V; Sakrejda, I; Salur, S; Sandweiss, J; Savin, I; Schambach, J; Scharenberg, R P; Schmitz, N; Schroeder, L S; Schweda, K; Seger, J; Seyboth, P; Shahaliev, E; Shestermanov, K E; Shimanskii, S S; Simon, F; Skoro, G; Smirnov, N; Snellings, R; Sorensen, P; Sowinski, J; Spinka, H M; Srivastava, B; Stephenson, E J; Stock, R; Stolpovsky, A; Strikhanov, M; Stringfellow, B; Struck, C; Suaide, A A P; Sugarbaker, E; Suire, C; Sumbera, M; Surrow, B; Symons, T J M; Szanto de Toledo, A; Szarwas, P; Tai, A; Takahashi, J; Tang, A H; Thein, D; Thomas, J H; Thompson, M; Timoshenko, S; Tokarev, M; Tonjes, M B; Trainor, T A; Trentalange, S; Tribble, R E; Trofimov, V; Tsai, O; Ullrich, T; Underwood, D G; Van Buren, G; Vander Molen, A M; Vasiliev, A N; Vigdor, S E; Voloshin, S A; Vznuzdaev, M; Wang, F; Wang, Y; Ward, H; Watson, J W; Wells, R; Westfall, G D; Whitten, C; Wieman, H; Willson, R; Wissink, S W; Witt, R; Wood, J; Xu, N; Xu, Z; Yakutin, A E; Yamamoto, E; Yang, J; Yepes, P; Yurevich, V I; Zanevski, Y V; Zborovský, I; Zhang, H; Zhang, W M; Zoulkarneev, R; Zoulkarneeva, J; Zubarev, A N

    2003-12-31

    Data from the first physics run at the Relativistic Heavy-Ion Collider at Brookhaven National Laboratory, Au+Au collisions at sqrt[s(NN)]=130 GeV, have been analyzed by the STAR Collaboration using three-pion correlations with charged pions to study whether pions are emitted independently at freeze-out. We have made a high-statistics measurement of the three-pion correlation function and calculated the normalized three-particle correlator to obtain a quantitative measurement of the degree of chaoticity of the pion source. It is found that the degree of chaoticity seems to increase with increasing particle multiplicity.

  20. Analysis of nine food additives in red wine by ion-suppression reversed-phase high-performance liquid chromatography using trifluoroacetic acid and ammonium acetate as ion-suppressors.

    Science.gov (United States)

    Zhao, Yong-Gang; Chen, Xiao-Hong; Yao, Shan-Shan; Pan, Sheng-Dong; Li, Xiao-Ping; Jin, Mi-Cong

    2012-01-01

    A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in red wine. The effects of ion-suppressors, i.e., trifluoroacetic acid (TFA) and ammonium acetate (AmAc) on retention behavior of nine food additives in RP-HPLC separation were discussed in detail. The relationships between retention factors of solutes and volume percent of ion-suppressors in the mobile-phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, respectively. The results showed that the ion suppressors had not only an ion suppression effect, but also an organic modification effect on the acidic analytes. The baseline separation of nine food additives was completed by a gradient elution with acetonitrile-TFA(0.01%, v/v)-AmAc(2.5 mmol L(-1)) aqueous solution as the mobile phase. The recoveries were between 80.2 - 99.5% for all analytes with RSDs in the range of 1.5 - 8.9%. The linearities were in the range of 0.2 - 100.0 mg L(-1) with determination coefficients (r(2)) higher than 0.9991 for all analytes. The limits of quantification (LOQs) were between 0.53 - 0.99 mg L(-1). The applicability of the proposed method to detect and quantify food additives has been demonstrated in the analysis of 30 real samples.

  1. High-performance ion chromatography method for separation and quantification of inositol phosphates in diets and digesta

    DEFF Research Database (Denmark)

    Blaabjerg, Karoline; Hansen-Møller, Jens; Poulsen, Hanne Damgaard

    2010-01-01

    A gradient high-performance ion chromatographic method for separation and quantification of inositol phosphates (InsP2-InsP6) in feedstuffs, diets, gastric and ileal digesta from pigs was developed and validated. The InsP2-InsP6 were separated on a Dionex CarboPacTM PA1 column using a gradient...... with 1.5 mol L-1 methanesulfonic acid and water. The exchange of the commonly used HCl with methanesulfonic acid has two advantages: (i) the obtained baseline during the separation is almost horizontal and (ii) it is not necessary to use an inert HPIC equipment as the methanesulfonic acid...

  2. The vaporization enthalpies and vapor pressures of fatty acid methyl esters C18, C21 to C23, and C25 to C29 by correlation - gas chromatography

    International Nuclear Information System (INIS)

    Chickos, James S.; Zhao Hui; Nichols, Gary

    2004-01-01

    Vapor pressures and vaporization enthalpies for methyl heptadecanoate and methyl heneicosanoate to methyl octacosanoate exclusive of methyl tricosanoate are evaluated as a function of temperature over the temperature range T = 298.15-450 K by correlation gas chromatography. The results are generated by an extrapolative process using literature values for methyl tetradecanoate to methyl eicosanoate as standards. Relationships for calculating vapor pressures of the title compounds from T = 298.15 to 450 K are provided. Experimental fusion enthalpies are also reported for the methyl esters from methyl hexadecanoate to methyl octacosanoate excluding methyl tridecanoate. Vaporization enthalpies and fusion enthalpies adjusted for temperature to T = 298.15 K are combined to provide sublimation enthalpies. The results are compared to available literature values. A rationale for the linear relationship observed between enthalpies of vaporization and enthalpies of transfer from solution to the vapor is also provided

  3. Theory of collective dynamics: flow, fluctuations and correlations in heavy ion collisions

    Energy Technology Data Exchange (ETDEWEB)

    Denicol, Gabriel S. [Physics Department, Brookhaven National Lab, Building 510A, Upton, NY, 11973 (United States); Department of Physics, McGill University, 3600 University Street, Montreal, Quebec, H3A 2T8 (Canada)

    2016-12-15

    I review recent developments in the hydrodynamic modeling of ultra-relativistic heavy ion collisions and the extraction of the properties of bulk QCD matter from heavy ion collision measurements. I briefly summarize the current framework used for the theoretical modeling of heavy ion collisions and report the recent progress on the extraction of the temperature dependence of the shear and bulk viscosity coefficients, the development of statistical tools for data-to-model comparison, and anisotropic hydrodynamics. All these recent developments in our field pave the way for more quantitative determination of the transport properties of bulk QCD matter from the experimental heavy ion collision program.

  4. Incorporating water-release and lateral protein interactions in modeling equilibrium adsorption for ion-exchange chromatography.

    Science.gov (United States)

    Thrash, Marvin E; Pinto, Neville G

    2006-09-08

    The equilibrium adsorption of two albumin proteins on a commercial ion exchanger has been studied using a colloidal model. The model accounts for electrostatic and van der Waals forces between proteins and the ion exchanger surface, the energy of interaction between adsorbed proteins, and the contribution of entropy from water-release accompanying protein adsorption. Protein-surface interactions were calculated using methods previously reported in the literature. Lateral interactions between adsorbed proteins were experimentally measured with microcalorimetry. Water-release was estimated by applying the preferential interaction approach to chromatographic retention data. The adsorption of ovalbumin and bovine serum albumin on an anion exchanger at solution pH>pI of protein was measured. The experimental isotherms have been modeled from the linear region to saturation, and the influence of three modulating alkali chlorides on capacity has been evaluated. The heat of adsorption is endothermic for all cases studied, despite the fact that the net charge on the protein is opposite that of the adsorbing surface. Strong repulsive forces between adsorbed proteins underlie the endothermic heat of adsorption, and these forces intensify with protein loading. It was found that the driving force for adsorption is the entropy increase due to the release of water from the protein and adsorbent surfaces. It is shown that the colloidal model predicts protein adsorption capacity in both the linear and non-linear isotherm regions, and can account for the effects of modulating salt.

  5. Selenium speciation in urine by ion-pairing chromatography with perfluorinated carboxylic acids and ICP-MS detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Bendahl, L.; Sidenius, U.

    2002-01-01

    Five aqueous standards, selenomethionine (SeMet), methylselenomethionine (MeSeMet), methylselenocysteine (MeSeCys), selenogammaaminobutyric acid (SeGaba) and the trimethylselenonium ion (TMSe), were separated in ion-pairing chromatographic systems based on perfluorinated carboxylic acids in metha...... were major compounds in urine samples-even after massive consumption of selenium-containing supplements. The selenium species in the urine samples showed a limited stability, as they changed during storage at +4 degreesC as well as -18 degreesC...... of between 2.3 and 5.1 pg. Urine samples from different individuals before and during supplementation with selenomethionine were analysed. Several species were separated in the different urine samples. A major component eluting at the beginning of the chromatogram was predominant in many samples, especially...... after selenium consumption. This species was not identified and solid phase extraction experiments suggested that it was neutral. When different urine samples were spiked with the available standards, co-elution of species with TMSe, MeSeMet or SeMet was observed in some samples. None of these species...

  6. Chromatography of 49 metal ions on stannic antimonate papers in dimethylsulfoxide: nitric acid systems and aqueous nitric acid systems

    International Nuclear Information System (INIS)

    Qureshi, M.; Varshney, K.G.; Rajput, R.P.S.

    1975-01-01

    Chromatographic separations of 49 metal ions on stannic antimonate papers have been performed using mixed solvent systems containing DMSO. Aqueous HNO 3 systems have also been used. The utility of the papers has been demonstrated by achieving various difficult separations. Some of the important separations (R/sub f/ values given in parentheses) are: Cs + (0.20)-K + (0.30) and Sm 3+ (0.00)-Pr 3+ (0.72) in pure DMSO; Nb 5+ (0.14)-VO 2+ (0.95) in DMSO-6M HNO 3 (1:1); Ti 4+ (0.00)-VO 2 (0.97) in DMSO-0.5M HNO 3 (1:1); and Ba 2+ (0.06)-K + (0.52)-Sr 2+ (0.95), Ba 2+ (0.04)-Cs + (0.41)-Mg 2+ (0.93), and Ca 2+ (0.10)-Sr 2+ (0.94) in DMSO-0.1M HNO 3 (1:1). The time of development in each case is two hours. A discussion is presented on the dependence of Ri, log R/sub f/, and R/sub M/ on pH of the solvent to understand the mechanism of the movement of metal ions on papers impregnated with inorganic materials. (U.S.)

  7. Determination of contaminants in boric acid used as neutron moderator by means of ion chromatography and selective electrodes

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Abrao, A.

    1988-07-01

    The boric acid used as neutron moderator in reactors must observe restrictions about the concentration of some impurities. According to Westinghouse (1) specification, the highest limits for sodium, sulphate, phosphate, fluoride, and chlorine are: Na + - 0,003%; SO 4 -2 - 0,0006%; PO 4 -3 - 0,003%; F - - 0,00002%; Cl - - 0,00004%. This paper describes the determination of ions above mentioned directly in the boric acid solution. The sample is dissolved in water or in an appropriate eluent and is injected in the ion chromatograph. Na + and F - are determined by means of selective electrodes. The determination limits found for F - (0,0002%) and Cl - (0,0002%) are not sufficiently low to attent the specifications. The determination limits found for SO 4 -2 (0,0005%), PO 4 -3 (0,0003%) and Na + (0,0005%) are good enough for nuclear pure boric acid analysis. In some samples nitrate (detection limit 0,0015%) was found as well. Boric acid from different suppliers were analysed. (author) [pt

  8. Correlation of precursor and product ions in single-stage high resolution mass spectrometry. A tool for detecting diagnostic ions and improving the precursor elemental composition elucidation

    Energy Technology Data Exchange (ETDEWEB)

    Borràs, S. [Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1-11, 08028 Barcelona (Spain); Kaufmann, A., E-mail: anton.kaufmann@klzh.ch [Official Food Control Authority, Fehrenstrasse 15, 8032 Zürich (Switzerland); Companyó, R. [Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1-11, 08028 Barcelona (Spain)

    2013-04-15

    Highlights: ► We are describing a technique to spot ions which are derived from each other. ► Single stage high resolution data is used. ► This “in silicon” technique is compared to conventional precursor scan. ► Some applications for this technique are presented. -- Abstract: Monitoring of common diagnostic fragments is essential for recognizing molecules which are members of a particular compound class. Up to now, unit resolving tandem quadrupole mass spectrometers, operating in the precursor ion scan mode, have been typically used to perform such analysis. By means of high-resolution mass spectrometry (HRMS) a much more sensitive and selective detection can be achieved. However, using a single-stage HRMS instrument, there is no unequivocal link to the corresponding precursor ion, since such instrumentation does not permit a previous precursor selection. Thus, to address this limitation, an in silico approach to locate precursor ions, based on diagnostic fragments, was developed. Implemented as an Excel macro, the algorithm rapidly assembles and surveys exact mass data to provide a list of feasible precursor candidates according to the correlation of the chromatographic peak shape profile and other additional filtering criteria (e.g. neutral losses and isotopes). The macro was tested with two families of veterinary drugs, sulfonamides and penicillins, which are known to yield diagnostic product ions when fragmented. Data sets obtained from different food matrices (fish and liver), both at high and low concentration of the target compounds, were investigated in order to evaluate the capabilities and limitations of the reported approach. Finally, other possible applications of this technique, such as the elucidation of elemental compositions based on product ions and corresponding neutral losses, were also presented and discussed.

  9. Correlation of precursor and product ions in single-stage high resolution mass spectrometry. A tool for detecting diagnostic ions and improving the precursor elemental composition elucidation

    International Nuclear Information System (INIS)

    Borràs, S.; Kaufmann, A.; Companyó, R.

    2013-01-01

    Highlights: ► We are describing a technique to spot ions which are derived from each other. ► Single stage high resolution data is used. ► This “in silicon” technique is compared to conventional precursor scan. ► Some applications for this technique are presented. -- Abstract: Monitoring of common diagnostic fragments is essential for recognizing molecules which are members of a particular compound class. Up to now, unit resolving tandem quadrupole mass spectrometers, operating in the precursor ion scan mode, have been typically used to perform such analysis. By means of high-resolution mass spectrometry (HRMS) a much more sensitive and selective detection can be achieved. However, using a single-stage HRMS instrument, there is no unequivocal link to the corresponding precursor ion, since such instrumentation does not permit a previous precursor selection. Thus, to address this limitation, an in silico approach to locate precursor ions, based on diagnostic fragments, was developed. Implemented as an Excel macro, the algorithm rapidly assembles and surveys exact mass data to provide a list of feasible precursor candidates according to the correlation of the chromatographic peak shape profile and other additional filtering criteria (e.g. neutral losses and isotopes). The macro was tested with two families of veterinary drugs, sulfonamides and penicillins, which are known to yield diagnostic product ions when fragmented. Data sets obtained from different food matrices (fish and liver), both at high and low concentration of the target compounds, were investigated in order to evaluate the capabilities and limitations of the reported approach. Finally, other possible applications of this technique, such as the elucidation of elemental compositions based on product ions and corresponding neutral losses, were also presented and discussed

  10. High-throughput screening and quantitation of guanidino and ureido compounds using liquid chromatography-drift tube ion mobility spectrometry-mass spectrometry

    International Nuclear Information System (INIS)

    Fan, Ruo-Jing; Zhang, Fang; Chen, Xiu-Ping; Qi, Wan-Shu; Guan, Qing; Sun, Tuan-Qi; Guo, Yin-Long

    2017-01-01

    The present work focused on the high-throughput screening and quantitation of guanidino compounds (GCs) and ureido compounds (UCs) in human thyroid tissues. The strategy employed benzylic rearrangement stable isotope labeling (BRSIL) for the sample preparation and then detection using liquid chromatography-drift tube ion mobility spectrometry-quadrupole time of flight mass spectrometry (LC-DTIMS-QTOF MS). A short reversed-phase LC realized an on-line desalting and a measurement cycle of 5.0 min. DTIMS separation enhanced the better specificity and selectivity for the benzil labeled GCs and UCs. The elevated mass resolution of QTOF MS enabled measure of the characteristic ions at accurate mass in MS and tandem MS spectra. Collision cross section (CCS) from DTIMS and accurate mass from QTOF MS were used as two qualifiers for the profiling and identification of GCs and UCs. In addition, an integral abundance arising from 3-D ion features (retention time, drift time, m/z) was applied to quantify the GCs and UCs in human thyroid tissues. The quantitative validation indicated good linearity (coefficient values ≥ 0.9981), good precision (1.0%–12.3% for intra-day and 0.9%–7.8% for inter-day) and good accuracy (91%–109%). The results demonstrated that the developed BRSIL coupled with LC-DTIMS-QTOF MS can be a powerful analysis platform to investigate GCs and UCs in human thyroid tissues. - Highlights: • The separation power of DTIMS-MS enhanced peak capacity, spectral clarity, and specificity of benzil labeled GCs and UCs. • Short-column LC for on-line desalting increased the throughput with a measurement cycle of 5.0 min. • CCS and accurate mass as a pair of qualifiers were used for the profiling and identification of GCs and UCs. • An integral abundance arising from 3-D ion features (RT, DT, m/z) was used as a novel quantifier for quantitation. • The developed method was applied to screen and quantify the GCs and UCs in human thyroid tissues.

  11. High-throughput screening and quantitation of guanidino and ureido compounds using liquid chromatography-drift tube ion mobility spectrometry-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Ruo-Jing [National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032 (China); Zhang, Fang, E-mail: fzhang@sioc.ac.cn [National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032 (China); Chen, Xiu-Ping; Qi, Wan-Shu [National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032 (China); Guan, Qing [Department of Head and Neck Surgery, Fudan University Shanghai Cancer Center, Shanghai 200032 (China); Department of Oncology, Shanghai Medical College, Fudan University, Shanghai 200032 (China); Sun, Tuan-Qi, E-mail: tuanqisun@163.com [Department of Head and Neck Surgery, Fudan University Shanghai Cancer Center, Shanghai 200032 (China); Department of Oncology, Shanghai Medical College, Fudan University, Shanghai 200032 (China); Guo, Yin-Long, E-mail: ylguo@sioc.ac.cn [National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032 (China)

    2017-04-08

    The present work focused on the high-throughput screening and quantitation of guanidino compounds (GCs) and ureido compounds (UCs) in human thyroid tissues. The strategy employed benzylic rearrangement stable isotope labeling (BRSIL) for the sample preparation and then detection using liquid chromatography-drift tube ion mobility spectrometry-quadrupole time of flight mass spectrometry (LC-DTIMS-QTOF MS). A short reversed-phase LC realized an on-line desalting and a measurement cycle of 5.0 min. DTIMS separation enhanced the better specificity and selectivity for the benzil labeled GCs and UCs. The elevated mass resolution of QTOF MS enabled measure of the characteristic ions at accurate mass in MS and tandem MS spectra. Collision cross section (CCS) from DTIMS and accurate mass from QTOF MS were used as two qualifiers for the profiling and identification of GCs and UCs. In addition, an integral abundance arising from 3-D ion features (retention time, drift time, m/z) was applied to quantify the GCs and UCs in human thyroid tissues. The quantitative validation indicated good linearity (coefficient values ≥ 0.9981), good precision (1.0%–12.3% for intra-day and 0.9%–7.8% for inter-day) and good accuracy (91%–109%). The results demonstrated that the developed BRSIL coupled with LC-DTIMS-QTOF MS can be a powerful analysis platform to investigate GCs and UCs in human thyroid tissues. - Highlights: • The separation power of DTIMS-MS enhanced peak capacity, spectral clarity, and specificity of benzil labeled GCs and UCs. • Short-column LC for on-line desalting increased the throughput with a measurement cycle of 5.0 min. • CCS and accurate mass as a pair of qualifiers were used for the profiling and identification of GCs and UCs. • An integral abundance arising from 3-D ion features (RT, DT, m/z) was used as a novel quantifier for quantitation. • The developed method was applied to screen and quantify the GCs and UCs in human thyroid tissues.

  12. Method for characterization of low molecular weight organic acids in atmospheric aerosols using ion chromatography mass spectrometry.

    Science.gov (United States)

    Brent, Lacey C; Reiner, Jessica L; Dickerson, Russell R; Sander, Lane C

    2014-08-05

    The structural composition of PM2.5 monitored in the atmosphere is usually divided by the analysis of organic carbon, black (also called elemental) carbon, and inorganic salts. The characterization of the chemical composition of aerosols represents a significant challenge to analysts, and studies are frequently limited to determination of aerosol bulk properties. To better understand the potential health effects and combined interactions of components in aerosols, a variety of measurement techniques for individual analytes in PM2.5 need to be implemented. The method developed here for the measurement of organic acids achieves class separation of aliphatic monoacids, aliphatic diacids, aromatic acids, and polyacids. The selective ion monitoring capability of a triple quadropole mass analyzer was frequently capable of overcoming instances of incomplete separations. Standard Reference Material (SRM) 1649b Urban Dust was characterized; 34 organic acids were qualitatively identified, and 6 organic acids were quantified.

  13. Determination of perfluorobutane in rat blood by automatic headspace capillary gas chromatography and selected ion monitoring mass spectrometry.

    Science.gov (United States)

    Hvattum, E; Normann, P T; Oulie, I; Uran, S; Ringstad, O; Skotland, T

    2001-01-01

    A new contrast agent (Sonazoid; NC100100) for ultrasound imaging has been developed. It is an aqueous suspension of lipid stabilised perfluorobutane (PFB) gas microbubbles. An automatic headspace capillary gas-chromatographic mass spectrometric method using electron impact ionisation was developed for analysis of Sonazoid PFB in rat blood. The calibration standards were gaseous PFB dissolved in ethanol in the range of 0.5-5000 ng PFB. Fluorotrichloromethane (CFC 11) was used as an internal standard of the method and the MS detector was set to single ion monitoring of the base fragment ions of PFB (m/z 69 and 119) and CFC 11 (m/z 101). The calibration graph, made by plotting the peak area ratios of PFB (m/z 69) to CFC 11(m/z 101) against the amount of PFB, was fitted to a second-order polynomial equation with weighting 1/y2 and found to be reproducible. The limit of quantification of the method was set to 0.4 ng PFB. The between-day variation of the method was below 9.2% relative standard deviation (RSD) and the within-day variation of the method was below 7.6% RSD. The accuracy of the method, as compared to Coulter counter, was estimated by determination of PFB in samples where Sonazoid was added to saline and found to range from 91.5% to 105.2%. PFB, added as Sonazoid, was found to be stable for at least 7 months in rat blood samples when stored at -20 degrees C.

  14. Bone metabolic activity measured with positron emission tomography and [18F] fluoride ion in renal osteodystrophy: Correlation with bone histomorphometry

    International Nuclear Information System (INIS)

    Messa, C.; Goodman, W.G.; Hoh, C.K.; Choi, Y.; Nissenson, A.R.; Salusky, I.B.; Phelps, M.E.; Hawkins, R.A.

    1993-01-01

    The authors evaluated the bone metabolic activity in patients with renal osteodystrophy using positron emission tomography and [ 18 F] fluoride ion. Eight patients had secondary hyperparathyroidism (HPT), and three had low-turnover bone disease. Eleven normal subjects were also studied, and three of the eight HPT patients were reevaluated after therapy. A rate constant (K) describing the net transport of [ 18 F] fluoride ion into a bound compartment in bone was calculated using both a three-compartment model and Patlak graphical analysis. Values of K were compared with biochemical data and with histomorphometric indices. The results indicate that K is significantly higher (P 18 F] fluoride ion can differentiate low turnover from high turnover lesions of renal osteodystropy and provide quantitative estimates of bone cell activity that correlate with histomorphometric data

  15. Development of a method for comprehensive and quantitative analysis of plant hormones by highly sensitive nanoflow liquid chromatography-electrospray ionization-ion trap mass spectrometry

    International Nuclear Information System (INIS)

    Izumi, Yoshihiro; Okazawa, Atsushi; Bamba, Takeshi; Kobayashi, Akio; Fukusaki, Eiichiro

    2009-01-01

    In recent plant hormone research, there is an increased demand for a highly sensitive and comprehensive analytical approach to elucidate the hormonal signaling networks, functions, and dynamics. We have demonstrated the high sensitivity of a comprehensive and quantitative analytical method developed with nanoflow liquid chromatography-electrospray ionization-ion trap mass spectrometry (LC-ESI-IT-MS/MS) under multiple-reaction monitoring (MRM) in plant hormone profiling. Unlabeled and deuterium-labeled isotopomers of four classes of plant hormones and their derivatives, auxins, cytokinins (CK), abscisic acid (ABA), and gibberellins (GA), were analyzed by this method. The optimized nanoflow-LC-ESI-IT-MS/MS method showed ca. 5-10-fold greater sensitivity than capillary-LC-ESI-IT-MS/MS, and the detection limits (S/N = 3) of several plant hormones were in the sub-fmol range. The results showed excellent linearity (R 2 values of 0.9937-1.0000) and reproducibility of elution times (relative standard deviations, RSDs, <1.1%) and peak areas (RSDs, <10.7%) for all target compounds. Further, sample purification using Oasis HLB and Oasis MCX cartridges significantly decreased the ion-suppressing effects of biological matrix as compared to the purification using only Oasis HLB cartridge. The optimized nanoflow-LC-ESI-IT-MS/MS method was successfully used to analyze endogenous plant hormones in Arabidopsis and tobacco samples. The samples used in this analysis were extracted from only 17 tobacco dry seeds (1 mg DW), indicating that the efficiency of analysis of endogenous plant hormones strongly depends on the detection sensitivity of the method. Our analytical approach will be useful for in-depth studies on complex plant hormonal metabolism.

  16. Development of a method for comprehensive and quantitative analysis of plant hormones by highly sensitive nanoflow liquid chromatography-electrospray ionization-ion trap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Izumi, Yoshihiro; Okazawa, Atsushi; Bamba, Takeshi; Kobayashi, Akio [Department of Biotechnology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan); Fukusaki, Eiichiro, E-mail: fukusaki@bio.eng.osaka-u.ac.jp [Department of Biotechnology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan)

    2009-08-26

    In recent plant hormone research, there is an increased demand for a highly sensitive and comprehensive analytical approach to elucidate the hormonal signaling networks, functions, and dynamics. We have demonstrated the high sensitivity of a comprehensive and quantitative analytical method developed with nanoflow liquid chromatography-electrospray ionization-ion trap mass spectrometry (LC-ESI-IT-MS/MS) under multiple-reaction monitoring (MRM) in plant hormone profiling. Unlabeled and deuterium-labeled isotopomers of four classes of plant hormones and their derivatives, auxins, cytokinins (CK), abscisic acid (ABA), and gibberellins (GA), were analyzed by this method. The optimized nanoflow-LC-ESI-IT-MS/MS method showed ca. 5-10-fold greater sensitivity than capillary-LC-ESI-IT-MS/MS, and the detection limits (S/N = 3) of several plant hormones were in the sub-fmol range. The results showed excellent linearity (R{sup 2} values of 0.9937-1.0000) and reproducibility of elution times (relative standard deviations, RSDs, <1.1%) and peak areas (RSDs, <10.7%) for all target compounds. Further, sample purification using Oasis HLB and Oasis MCX cartridges significantly decreased the ion-suppressing effects of biological matrix as compared to the purification using only Oasis HLB cartridge. The optimized nanoflow-LC-ESI-IT-MS/MS method was successfully used to analyze endogenous plant hormones in Arabidopsis and tobacco samples. The samples used in this analysis were extracted from only 17 tobacco dry seeds (1 mg DW), indicating that the efficiency of analysis of endogenous plant hormones strongly depends on the detection sensitivity of the method. Our analytical approach will be useful for in-depth studies on complex plant hormonal metabolism.

  17. Determination of melamine in milk-based products and other food and beverage products by ion-pair liquid chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ibanez, Maria; Sancho, Juan V. [Research Institute for Pesticides and Water, University Jaume I, E-12071, Castellon (Spain); Hernandez, Felix, E-mail: felix.hernandez@qfa.uji.es [Research Institute for Pesticides and Water, University Jaume I, E-12071, Castellon (Spain)

    2009-09-01

    This paper describes a fast method for the sensitive and selective determination of melamine in a wide range of food matrices, including several milk-based products. The method involves an extraction with aqueous 1% trichloroacetic acid before the injection of the 10-fold diluted extract into the liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) system, using labelled melamine as the internal standard. As melamine is present in aqueous media in the cationic form, the chromatographic separation in reversed-phase LC requires the use of anionic ion-pair reagents, such as tridecafluoroheptanoic acid (THFA). This allows a satisfactory chromatographic retention and peak shape in all the types of food samples investigated. The method has been validated in six food matrices (biscuit, dry pasta and four milk-based products) by means of recovery experiments in samples spiked at 1 and 5 mg kg{sup -1}. Average recoveries (n = 5) ranged from 77% to 100%, with excellent precision (RSDs lower than 5%) and limits of detection between 0.01 and 0.1 mg kg{sup -1}. In addition, accuracy and robustness of the method was proven in different soya-based matrices by means of quality control (QC) sample analysis. QC recoveries, at 1 and 2.5 mg kg{sup -1}, were satisfactory, ranging from 79% to 110%. The method developed in this work has been applied to the determination of melamine in different types of food samples. All detections were confirmed by acquiring two MS/MS transitions (127 > 85 for quantification; 127 > 68 for confirmation) and comparing their ion intensity ratio with that of reference standards. Accuracy of the method was also assessed by applying it to a milk-based product and a baking mix material as part of an EU proficiency test, in which highly satisfactory results were obtained.

  18. A novel ion-exclusion chromatography-mass spectrometry method to measure concentrations and cycling rates of carbohydrates and amino sugars in freshwaters.

    Science.gov (United States)

    Horňák, Karel; Pernthaler, Jakob

    2014-10-24

    The concentrations of free neutral carbohydrates and amino sugars were determined in freshwater samples of distinct matrix complexity, including meso-, eu- and dystrophic lakes and ponds, using high-performance ion-exclusion chromatography (HPIEC) coupled to mass spectrometry (MS). In contrast to other methods, our approach allowed the quantification of free neutral carbohydrates and amino sugars at low nM concentrations without derivatization, de-salting or pre-concentration. New sample preparation procedures were applied prior to injection employing syringe and hollow fiber filtration. Analytes were separated on a strong cation exchange resin under 100% aqueous conditions using 0.1% formic acid as a mobile phase. To minimize background noise in MS, analytes were detected in a multiple reaction monitoring scan mode with double ion filtering. Detection limits of carbohydrates and amino sugars ranged between 0.2 and 2nM at a signal-to-noise ratio >5. Error ranged between 1 and 12% at 0.5-500nM levels. Using a stable isotope dilution approach, both the utilization and recycling of glucose in Lake Zurich was observed. In contrast, N-acetyl-glucosamine was equally rapidly consumed but there was no visible de novo production. The simple and rapid sample preparation makes our protocol suitable for routine analyses of organic compounds in freshwater samples. Application of stable isotope tracers along with accurate measures of carbohydrate and amino sugar concentrations enables novel insights into the compound in situ dynamics. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Determination of melamine in milk-based products and other food and beverage products by ion-pair liquid chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    Ibanez, Maria; Sancho, Juan V.; Hernandez, Felix

    2009-01-01

    This paper describes a fast method for the sensitive and selective determination of melamine in a wide range of food matrices, including several milk-based products. The method involves an extraction with aqueous 1% trichloroacetic acid before the injection of the 10-fold diluted extract into the liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) system, using labelled melamine as the internal standard. As melamine is present in aqueous media in the cationic form, the chromatographic separation in reversed-phase LC requires the use of anionic ion-pair reagents, such as tridecafluoroheptanoic acid (THFA). This allows a satisfactory chromatographic retention and peak shape in all the types of food samples investigated. The method has been validated in six food matrices (biscuit, dry pasta and four milk-based products) by means of recovery experiments in samples spiked at 1 and 5 mg kg -1 . Average recoveries (n = 5) ranged from 77% to 100%, with excellent precision (RSDs lower than 5%) and limits of detection between 0.01 and 0.1 mg kg -1 . In addition, accuracy and robustness of the method was proven in different soya-based matrices by means of quality control (QC) sample analysis. QC recoveries, at 1 and 2.5 mg kg -1 , were satisfactory, ranging from 79% to 110%. The method developed in this work has been applied to the determination of melamine in different types of food samples. All detections were confirmed by acquiring two MS/MS transitions (127 > 85 for quantification; 127 > 68 for confirmation) and comparing their ion intensity ratio with that of reference standards. Accuracy of the method was also assessed by applying it to a milk-based product and a baking mix material as part of an EU proficiency test, in which highly satisfactory results were obtained.

  20. Liquid chromatography/negative electrospray ionization ion trap MS(2) mass spectrometry application for the determination of microcystins occurrence in Southern Portugal water reservoirs.

    Science.gov (United States)

    Rodrigues, M A; Reis, M P; Mateus, M C

    2013-11-01

    Microcystins (MCs) are toxins produced by cyanobacteria which are common organisms in the phytoplankton of eutrophic lakes, rivers and freshwater reservoirs. In the present work, a novel method of liquid chromatography-electrospray ion trap tandem mass spectrometry (LC/ESI/Ion trap-MS/MS), operated in the negative ionization mode, was developed for the analysis of these cyanotoxins. The method was applied to determine the amounts of total microcystins-LR, -YR and -RR in two water reservoirs in Southern Portugal, namely Alqueva and Beliche. A total of 30 water samples were analysed along 2011. Solid phase extraction (SPE) was used for sample cleaning-up and analyte enrichment. The extracted toxins were separated on a C18 column with a gradient of acetonitrile/water with 0.1% formic acid. Detection of microcystins was carried out using multiple reaction monitoring (MRM) in the negative polarity mode, as this method gave a higher selectivity. The MC-RR, YR and LR quantification limits were 17.9, 31.7 and 15.8 ng/L, respectively; quite below the limits recommended by WHO guidelines for drinking water (1 μg/L). Total MC highest concentrations were found in the warm months of June, July and September in Alqueva sampling sites, with concentrations of MC LR and RR ranging 17-344 and 25-212 ng/L, respectively, showing comparable results for MC-RR and LR and slightly lower concentration of MC-YR. Detected values for Beliche reservoir were below quantification limits. Copyright © 2013 Elsevier Ltd. All rights reserved.