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Sample records for exchange chromatography techniques

  1. Radioanalytical determination of plutonium and americium using ion exchange and extraction chromatography technique in urine

    International Nuclear Information System (INIS)

    Santhanakrishnan, V.; Sreedevi, K.R.; Rajaram, S.; Ravi, P.M.

    2011-01-01

    The use of anion exchange chromatography for the separation of Pu and extraction chromatography technique for the separation of Am from urine samples was studied. In the earlier method, Pu separation was carried out by anion exchange chromatography followed by Am separation by cation exchange chromatography. The chemical recovery of Am obtained by cation exchange separation method was inconsistent and low in the range 30-70%. In this study, the average Pu recovery obtained using anion exchange chromatography was 89.2 with standard deviation of 10.4 and the average Am recovery obtained using extraction chromatography with TRU resin was 77.4 with standard deviation of 14.8. Moreover, Am separation could be completed within three hours using the TRU column compared to two days that were required for the cation exchange chromatography. (author)

  2. 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

  3. 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)

  4. 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"…

  5. 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.

  6. Semi-automated technique for the separation and determination of barium and strontium in surface waters by ion exchange chromatography and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Pierce, F.D.; Brown, H.R.

    1977-01-01

    A semi-automated method for the separation and the analysis of barium and strontium in surface waters by atomic emission spectrometry is described. The method employs a semi-automated separation technique using ion exchange and an automated aspiration-analysis procedure. Forty specimens can be prepared in approximately 90 min and can be analyzed for barium and strontium content in 20 min. The detection limits and sensitivities provided by the described technique are 0.003 mg/l and 0.01 mg/l respectively for barium and 0.00045 mg/l and 0.003 mg/l respectively for strontium

  7. A high-throughput 2D-analytical technique to obtain single protein parameters from complex cell lysates for in silico process development of ion exchange chromatography.

    Science.gov (United States)

    Kröner, Frieder; Elsäßer, Dennis; Hubbuch, Jürgen

    2013-11-29

    The accelerating growth of the market for biopharmaceutical proteins, the market entry of biosimilars and the growing interest in new, more complex molecules constantly pose new challenges for bioseparation process development. In the presented work we demonstrate the application of a multidimensional, analytical separation approach to obtain the relevant physicochemical parameters of single proteins in a complex mixture for in silico chromatographic process development. A complete cell lysate containing a low titre target protein was first fractionated by multiple linear salt gradient anion exchange chromatography (AEC) with varying gradient length. The collected fractions were subsequently analysed by high-throughput capillary gel electrophoresis (HT-CGE) after being desalted and concentrated. From the obtained data of the 2D-separation the retention-volumes and the concentration of the single proteins were determined. The retention-volumes of the single proteins were used to calculate the related steric-mass action model parameters. In a final evaluation experiment the received parameters were successfully applied to predict the retention behaviour of the single proteins in salt gradient AEC. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Applications of pressurized cation exchange chromatography for fission yield determination

    International Nuclear Information System (INIS)

    Yan Shuheng; Lin Fa; Zhang Hongdi; Li Xueliang; Zhang Shulan

    1988-01-01

    In order to determine the fission yields of lanthanides precisely, lanthanides with carriers of 1-2 mg per element are separated from each other by means of pressurized cation exchange chromatography - αHIBA concentration gradient elution. The effect of initial loading technique, concentration gradient, flow rate, and temperature on separation were investigated in detail. Under the optimum conditions adapted according to the results given in this work, all the lanthanides can be completely separated within about 90 minutes with a recovery of more than 95% and purity higher than 99%. (author) 3 refs.; 6 figs

  9. Sm isotope composition and Sm/Eu ratio determination in an irradiated 153Eu sample by ion exchange chromatography-quadrupole inductively coupled plasma mass spectrometry combined with double spike isotope dilution technique

    International Nuclear Information System (INIS)

    Bourgeois, M.; Isnard, H.; Gourgiotis, A.; Stadelmann, G.; Gautier, C.; Mialle, S.; Nonell, A.; Chartier, F.

    2011-01-01

    Within the framework of the research undertaken by the French Atomic Energy Commission on transmutation of long-lived radionuclides, targets of highly enriched actinides and fission products were irradiated in the fast neutron reactor Phenix. Precise and accurate measurements of the isotopic and elemental composition of the enriched elements are therefore required. In order to obtain the uncertainties of several per mil and to reduce handling time and exposure to analyst on radioactive material, the on-line coupling of ion exchange chromatography with quadrupole inductively coupled plasma mass spectrometry has been associated with the technique of the double spike isotope dilution. We present in this paper the results obtained on an irradiated sample of Europium oxide powder (enriched at 99.13% in 153 Eu). After irradiation of around 5 mg of Eu 2 O 3 powder the theoretical calculations predict the formation of several micrograms of gadolinium and samarium isotopes. In relation to the very high activity of the sample after irradiation and the very low quantity of Sm formed, the on-line ion exchange chromatography separation of Gd, Sm and Eu before Sm isotope ratio measurements has been developed for the quantification of the 152 Sm/ 153 Eu ratio. These on-line measurements were associated with the double spike isotope dilution technique after calibration of a 147 Sm/ 151 Eu spike solution. The external reproducibility of Sm isotopic ratios was determined to be around 0.5% (2 σ) resulting in a final uncertainty on the 152 Sm/ 153 Eu ratio of around 1% (2 σ). These on-line measurements present therefore a robust and high-throughput alternative to the thermal-ionisation mass spectrometry technique used so far in combination with off-line chromatographic separation, particularly in nuclear applications where characterisation of high activity sample solutions is required. (authors)

  10. Test procedure for cation exchange chromatography

    International Nuclear Information System (INIS)

    Cooper, T.D.

    1994-01-01

    The purpose of this test plan is to demonstrate the synthesis of inorganic antimonate ion exchangers and compare their performance against the standard organic cation exchangers. Of particular interest is the degradation rate of both inorganic and organic cation exchangers. This degradation rate will be tracked by determining the ion exchange capacity and thermal stability as a function of time, radiation dose, and chemical reaction

  11. Test procedure for anion exchange chromatography

    International Nuclear Information System (INIS)

    Cooper, T.D.

    1994-01-01

    Plutonium from stored nitrate solutions will be sorbed onto anion exchange resins and converted to storable plutonium dioxide. Useful information will be simultaneously gained on the thermal stability and ion exchange capacity of four commercially available anion exchange resins over several years and under severe degradative conditions. This information will prove useful in predicting the safe and efficient lifetimes of these resins

  12. 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

  13. 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

  14. Exploration of overloaded cation exchange chromatography for monoclonal antibody purification.

    Science.gov (United States)

    Liu, Hui F; McCooey, Beth; Duarte, Tiago; Myers, Deanna E; Hudson, Terry; Amanullah, Ashraf; van Reis, Robert; Kelley, Brian D

    2011-09-28

    Cation exchange chromatography using conventional resins, having either diffusive or perfusive flow paths, operated in bind-elute mode has been commonly employed in monoclonal antibody (MAb) purification processes. In this study, the performance of diffusive and perfusive cation exchange resins (SP-Sepharose FF (SPSFF) and Poros 50HS) and a convective cation exchange membrane (Mustang S) and monolith (SO(3) Monolith) were compared. All matrices were utilized in an isocratic state under typical binding conditions with an antibody load of up to 1000 g/L of chromatographic matrix. The dynamic binding capacity of the cation exchange resins is typically below 100 g/L resin, so they were loaded beyond the point of anticipated MAb break through. All of the matrices performed similarly in that they effectively retained host cell protein and DNA during the loading and wash steps, while antibody flowed through each matrix after its dynamic binding capacity was reached. The matrices differed, though, in that conventional diffusive and perfusive chromatographic resins (SPSFF and Poros 50HS) demonstrated a higher binding capacity for high molecular weight species (HMW) than convective flow matrices (membrane and monolith); Poros 50HS displayed the highest HMW binding capacity. Further exploration of the conventional chromatographic resins in an isocratic overloaded mode demonstrated that the impurity binding capacity was well maintained on Poros 50HS, but not on SPSFF, when the operating flow rate was as high as 36 column volumes per hour. Host cell protein and HMW removal by Poros 50HS was affected by altering the loading conductivity. A higher percentage of host cell protein removal was achieved at a low conductivity of 3 mS/cm. HMW binding capacity was optimized at 5 mS/cm. Our data from runs on Poros 50HS resin also showed that leached protein A and cell culture additive such as gentamicin were able to be removed under the isocratic overloaded condition. Lastly, a MAb

  15. 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.

  16. Methods of uranium isotpic separation by chemical exchange chromatography

    International Nuclear Information System (INIS)

    Pena V, L.A.; Valle M, L.

    1985-01-01

    Chemical exchange chromatography as applied to isotope separation has undergone a constant development during the last few years. The results so far indicate that this method could eventually become commercially useful. This work presents a critical review of the experimental methods presently under study by principal research groups, and which have not get been compared. (Author)

  17. 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.

  18. Fractionation of lithium isotopes in cation-exchange chromatography

    International Nuclear Information System (INIS)

    Oi, Takao; Kawada, Kazuhiko; Kakihana, Hidetake; Hosoe, Morikazu

    1991-01-01

    Various methods for lithium isotope separation have been developed, and their applicability to large-scale enriched lithium isotope production has been assessed. Ion-exchange chromatography is one such method. Cation-exchange chromatography of lithium was carried out to investigate the lithium isotope effect in aqueous ion-exchange systems. The heavier isotope. 7 Li, was preferentially fractionated into the resin phase in every experiment conducted, and this result is consistent with the results of previous work. The value of the separation factor was 1.00089-1.00171 at 25C. A comparison of lithium isotope effect with those of potassium and rubidium indicated that the isotope effect originating from hydration is larger than the effect due to phase change for lithium, while the opposite is the case with potassium and rubidium

  19. 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.

  20. Isotopic enrichment of 15N by ionic exchange chromatography

    International Nuclear Information System (INIS)

    Trivelin, P.C.O.

    1979-01-01

    The present paper presents some studies on production of 15 N-enriched ammonium sulphate with 5% atoms by ionic exchange chromatography method. Two systems are described of columns of resin, where experiments were conducted by eluition of NH 4 + bands with sodium hydroxide solution. Analyses were made of the cost of production of 15 N-enriched ammonium sulphate 5% atoms and, based on the experiments developed, a cost was obtained which was compatible with the international price of the product. The isotopic analyses of nitrogen were made by mass spectrometry. (Author) [pt

  1. Magnesium isotope fractionation in cation-exchange chromatography

    International Nuclear Information System (INIS)

    Oi, T.; Yanase, S.; Kakihana, H.

    1987-01-01

    Band displacement chromatography of magnesium has been carried out successfully for the purpose of magnesium isotope separation by using a strongly acidic cation-exchange resin and the strontium ion as the replacement ion. A small but definite accumulation of the heavier isotopes ( 25 Mg, 26 Mg) has been observed at the front parts of the magnesium chromatograms. The heavier isotopes have been fractionated preferentially into the solution phase. The single-stage separation factors have been calculated for the 25 Mg/ 24 Mg and 26 Mg/ 24 isotopic pairs at 25 0 C. The reduced partition function ratios of magnesium species involved in the present study have been estimated

  2. 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

  3. Strong Cation Exchange Chromatography in Analysis of Posttranslational Modifications: Innovations and Perspectives

    Science.gov (United States)

    Edelmann, Mariola J.

    2011-01-01

    Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide. PMID:22174558

  4. 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.

  5. Determination of Pb-210 and actinides by extraction chromatography and anion exchange chromatography

    International Nuclear Information System (INIS)

    Kalmykov, St.N.; Sapozhnikov, Yu.A.

    1997-01-01

    This work is devoted to the determination of Pb-210 and actinides (Pu-238, Pu-239, Am-241, U-235, U-238, Th-232) by means of highly selective chromatographic resins and anion exchangers. The special interest was paid to the analysis of large quantities of samples with high concentration of competitive ions like ocean sediments, bone ash and others.The commercially available TRU-Spec chromatographic resins was used for separation of actinides from the matrix. Then U, Th, Am, and Pu were separated from other using anion exchange chromatography with AG-1X4 anionite in Cl - form, electro-deposed and α-counted.Pb-21- and Bi-210 were determined by liquid scintillation counting. The developed procedure is rather express, effective and could be adopted for the determination of radionuclides like Ba-133, Ra, Np-239

  6. 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.

  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. Purification of bacteriophage M13 by anion exchange chromatography.

    Science.gov (United States)

    Monjezi, Razieh; Tey, Beng Ti; Sieo, Chin Chin; Tan, Wen Siang

    2010-07-01

    M13 is a non-lytic filamentous bacteriophage (phage). It has been used widely in phage display technology for displaying foreign peptides, and also for studying macromolecule structures and interactions. Traditionally, this phage has been purified by cesium chloride (CsCl) density gradient ultracentrifugation which is highly laborious and time consuming. In the present study, a simple, rapid and efficient method for the purification of M13 based on anion exchange chromatography was established. A pre-packed SepFast Super Q column connected to a fast protein liquid chromatography (FPLC) system was employed to capture released phages in clarified Escherichia coli fermented broth. An average yield of 74% was obtained from a packed bed mode elution using citrate buffer (pH 4), containing 1.5 M NaCl at 1 ml/min flow rate. The purification process was shortened substantially to less than 2 h from 18 h in the conventional ultracentrifugation method. SDS-PAGE revealed that the purity of particles was comparable to that of CsCl gradient density ultracentrifugation method. Plaque forming assay showed that the purified phages were still infectious. Copyright 2010 Elsevier B.V. All rights reserved.

  9. 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.

  10. 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.

  11. 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.

  12. Cation exchange separation of 16 rare earth metals by microscale high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Ishii, D.; Hirose, A.; Iwasaki, Y.

    1978-01-01

    The separation of rare earth metals has been studied with a microcolumn of 0.5 mm i.d. and 75 mm length, packed with TSK LS-212 high-performance cation exchange resin. A micro-feeder (Model MF-2, from Azumadenki Kogyo) was used to drive carrier and sample solutions through the ion exchange column and detection cell. By combining a 250 μl syringe and a 0.5 mm i.d. sampling tube the micro-feeder, 0.1-1.0 μl rare earth metals were separated within 38 min, using only 304 μl of 0.4M α-hydroxy-isobutyric acid solution adjusted to pH 3.1-6.0 with ammonia solution as gradient carrier solution. The gradient elution was successfully performed by applying a new technique developed for microscale liquid chromatography. (author)

  13. 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

  14. 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)

  15. Characterization of Low-Molecular-Weight Heparins by Strong Anion-Exchange Chromatography.

    Science.gov (United States)

    Sadowski, Radosław; Gadzała-Kopciuch, Renata; Kowalkowski, Tomasz; Widomski, Paweł; Jujeczka, Ludwik; Buszewski, Bogusław

    2017-11-01

    Currently, detailed structural characterization of low-molecular-weight heparin (LMWH) products is an analytical subject of great interest. In this work, we carried out a comprehensive structural analysis of LMWHs and applied a modified pharmacopeial method, as well as methods developed by other researchers, to the analysis of novel biosimilar LMWH products; and, for the first time, compared the qualitative and quantitative composition of commercially available drugs (enoxaparin, nadroparin, and dalteparin). For this purpose, we used strong anion-exchange (SAX) chromatography with spectrophotometric detection because this method is more helpful, easier, and faster than other separation techniques for the detailed disaccharide analysis of new LMWH drugs. In addition, we subjected the obtained results to statistical analysis (factor analysis, t-test, and Newman-Keuls post hoc test).

  16. 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)

  17. 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.)

  18. 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)

  19. 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

  20. Ligand exchange chromatography of free amino acids and proteins on porous microparticulate zirconium oxide

    International Nuclear Information System (INIS)

    Blackwell, J.A.; Carr, P.W.

    1992-01-01

    The Lewis acid sites present on the underlying zirconium oxide particles are responsible for the unusual elution sequence for amino acids on copper loaded, phosphated zirconium oxide supports reported in an earlier study. To more thoroughly examine the effect of these strong Lewis acid sites in this paper. The authors have studied ligand exchange chromatography on copper loaded zirconium oxide particles. It is shown here that carboxylate functional groups on amino acid solutes strongly interact with surface Lewis acid sites. Addition of competing hard Lewis bases to the eluent attenuates these specific interactions. The result is a chromatographic system with high selectivity which is also suitable for ligand exchange chromatography of proteins

  1. Computer simulation of displacement cation exchange chromatography: separation of trivalent actinides and lanthanides

    International Nuclear Information System (INIS)

    Forsberg, C.W.

    1980-05-01

    A first-generation mathematical model of displacement cation exchange chromatography (CES) was constructed. The model incorporated the following phenomena: diffusion of cations up and down the column, diffusion of cations from the bulk liquid to the resin surface, and equilibrium of cations between liquid and solid resin beads. A limited number of experiments with rare earths using DTPA as the separation agent were undertaken to increase the current understanding of the processes involved in cation exchange chromatography. The numerical computer program based on the mathematical model was written in FORTRAN IV for use on the IBM 360 series of computers

  2. 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.

  3. Affinity chromatography: A versatile technique for antibody purification.

    Science.gov (United States)

    Arora, Sushrut; Saxena, Vikas; Ayyar, B Vijayalakshmi

    2017-03-01

    Antibodies continue to be extremely utilized entities in myriad applications including basic research, imaging, targeted delivery, chromatography, diagnostics, and therapeutics. At production stage, antibodies are generally present in complex matrices and most of their intended applications necessitate purification. Antibody purification has always been a major bottleneck in downstream processing of antibodies, due to the need of high quality products and associated high costs. Over the years, extensive research has focused on finding better purification methodologies to overcome this holdup. Among a plethora of different techniques, affinity chromatography is one of the most selective, rapid and easy method for antibody purification. This review aims to provide a detailed overview on affinity chromatography and the components involved in purification. An array of support matrices along with various classes of affinity ligands detailing their underlying working principles, together with the advantages and limitations of each system in purifying different types of antibodies, accompanying recent developments and important practical methodological considerations to optimize purification procedure are discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  4. 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)

  5. 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...

  6. 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

  7. Evaluation of the separation and purification of 227Th from its decay progeny by anion exchange and extraction chromatography

    International Nuclear Information System (INIS)

    Ivanov, P.I.; Collins, S.M.; Es, E.M. van; García-Miranda, M.; Jerome, S.M.; Russell, B.C.

    2017-01-01

    Thorium-227 is currently undergoing evaluation as a potential radionuclide for targeted cancer therapy, and as such a high chemical purity of the material is required. To establish a reliable procedure for radiochemical isolation of 227 Th from the parent 227 Ac and decay progeny, which includes the radiotherapeutic 223 Ra, the performance of three different separation schemes based on ion-exchange and extraction chromatography have been evaluated. The results suggest that both ion exchange and extraction chromatographic techniques can be successfully used for the separation of 227 Th from its decay progeny, however extraction chromatographic resins demonstrate favourable performance in terms of Th recovery and purification from radionuclide impurities. - Highlights: • Development of a radiochemical separation of 227 Th from residual 227Ac as well as from decay progeny. • Evaluation of ion-exchange and extraction chromatography techniques. • TEVA resin demonstrates favourable performance in terms of Th recovery and purification. • Developed method is applicable to both nuclear medicine and environmental analysis.

  8. 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)

  9. 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)

  10. 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)

  11. EXCHANGE-RATES FORECASTING: EXPONENTIAL SMOOTHING TECHNIQUES AND ARIMA MODELS

    Directory of Open Access Journals (Sweden)

    Dezsi Eva

    2011-07-01

    Full Text Available Exchange rates forecasting is, and has been a challenging task in finance. Statistical and econometrical models are widely used in analysis and forecasting of foreign exchange rates. This paper investigates the behavior of daily exchange rates of the Romanian Leu against the Euro, United States Dollar, British Pound, Japanese Yen, Chinese Renminbi and the Russian Ruble. Smoothing techniques are generated and compared with each other. These models include the Simple Exponential Smoothing technique, as the Double Exponential Smoothing technique, the Simple Holt-Winters, the Additive Holt-Winters, namely the Autoregressive Integrated Moving Average model.

  12. 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.

  13. Effects of arginine on multimodal anion exchange chromatography.

    Science.gov (United States)

    Hirano, Atsushi; Arakawa, Tsutomu; Kameda, Tomoshi

    2015-12-01

    The effects of arginine on binding and elution properties of a multimodal anion exchanger, Capto adhere, were examined using bovine serum albumin (BSA) and a monoclonal antibody against interleukin-8 (mAb-IL8). Negatively charged BSA was bound to the positively charged Capto adhere and was readily eluted from the column with a stepwise or gradient elution using 1M NaCl at pH 7.0. For heat-treated BSA, small oligomers and remaining monomers were also eluted using a NaCl gradient, whereas larger oligomers required arginine for effective elution. The positively charged mAb-IL8 was bound to Capto adhere at pH 7.0. Arginine was also more effective for elution of the bound mAb-IL8 than was NaCl. The results imply that arginine interacts with the positively charged Capto adhere. The mechanism underlying the interactions of arginine with Capto adhere was examined by calculating the binding free energy between an arginine molecule and a Capto adhere ligand in water through molecular dynamics simulations. The overall affinity of arginine for Capto adhere is attributed to the hydrophobic and π-π interactions between an arginine side chain and the aromatic moiety of the ligand as well as hydrogen bonding between arginine and the ligand hydroxyl group, which may account for the characteristics of protein elution using arginine. Copyright © 2015 Elsevier Inc. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

    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

  15. 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.

  16. Techniques for the improvement of heat exchange

    International Nuclear Information System (INIS)

    Huyghe, J.

    1983-01-01

    The target of the described techniques is either to improve the performances of the equipements or to reduce their cost price. These techniques were developed at the laboratory scale and some of them were tested in pilot units. Neither of them has yet been applied in commercial plants. Different type of corrogated tubes, thin film evaporation, dropwise condensation, plastic tube or plates, tube configuration and heat pipes are examined [fr

  17. Ligand exchange chromatography for analysis and preparative separation of tritium-labelled amino acids

    International Nuclear Information System (INIS)

    Zolotarev, Yu.A.; Zaitsev, D.A.; Penkina, V.I.; Dostavalov, I.N.; Myasoedov, N.F.

    1988-01-01

    Racemic tritium-labelled amino acids were separated into optical isomers by chromatography on a chiral polyacrylamide sorbent filled with copper ions. The polyacrylamide sorbent is synthesized by Mannich's reaction through the action of formaldehyde and L-phenylalanine upon polyacrylamide Biogel P-4 in an alkali phosphate buffer. Tritium-labelled amino acids are eluted by a weak alkali solution of ammonium carbonate. Data are presented on the ligand exchange chromatography of amino acids depending on the degree to which the sorbent is filled with copper ions and on the eluent concentration. Amino acids are isolated from the eluent on short columns filled with sulfonated cation exchanger in the H + form. HPLC on modified silica gel sorbents is also used for the analysis of tritium-labelled optically active amino acids. Amino acids are eluted by a weakly acidic water-methanol solution containing ammonium acetate. UV and scintillation flow type detectors are used. (author) 7 refs.; 8 figs

  18. Advanced techniques for energy-efficient industrial-scale continuous chromatography

    Energy Technology Data Exchange (ETDEWEB)

    DeCarli, J.P. II (Dow Chemical Co., Midland, MI (USA)); Carta, G. (Virginia Univ., Charlottesville, VA (USA). Dept. of Chemical Engineering); Byers, C.H. (Oak Ridge National Lab., TN (USA))

    1989-11-01

    Continuous annular chromatography (CAC) is a developing technology that allows truly continuous chromatographic separations. Previous work has demonstrated the utility of this technology for the separation of various materials by isocratic elution on a bench scale. Novel applications and improved operation of the process were studied in this work, demonstrating that CAC is a versatile apparatus which is capable of separations at high throughput. Three specific separation systems were investigated. Pilot-scale separations at high loadings were performed using an industrial sugar mixture as an example of scale-up for isocratic separations. Bench-scale experiments of a low concentration metal ion mixture were performed to demonstrate stepwise elution, a chromatographic technique which decreases dilution and increases sorbent capacity. Finally, the separation of mixtures of amino acids by ion exchange was investigated to demonstrate the use of displacement development on the CAC. This technique, which perhaps has the most potential, when applied to the CAC allowed simultaneous separation and concentration of multicomponent mixtures on a continuous basis. Mathematical models were developed to describe the CAC performance and optimize the operating conditions. For all the systems investigated, the continuous separation performance of the CAC was found to be very nearly the same as the batchwise performance of conventional chromatography. the technology appears, thus, to be very promising for industrial applications. 43 figs., 9 tabs.

  19. 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.

  20. Enhancing recovery of recombinant hepatitis B surface antigen in lab-scale and large-scale anion-exchange chromatography by optimizing the conductivity of buffers.

    Science.gov (United States)

    Mojarrad Moghanloo, Gol Mohammad; Khatami, Maryam; Javidanbardan, Amin; Hosseini, Seyed Nezamedin

    2018-01-01

    In biopharmaceutical science, ion-exchange chromatography (IEC) is a well-known purification technique to separate the impurities such as host cell proteins from recombinant proteins. However, IEC is one of the limiting steps in the purification process of recombinant hepatitis B surface antigen (rHBsAg), due to its low recovery rate (rate of 82% in both lab-scale and large-scale weak anion-exchange chromatography without any harsh effect on the purity percentage of rHBsAg. The recovery enhancement via increasing the conductivity of Eq. and Wash. buffers can be explained by their roles in reducing the binding strength and aggregation of retained particles in the column. Moreover, further increase in the salt concentration of Elut. Buffer could substantially promote the ion exchange process and the elution of retained rHBsAg. Copyright © 2017 Elsevier Inc. All rights reserved.

  1. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    Science.gov (United States)

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

  2. 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.

  3. 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.)

  4. 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.

  5. Online Simultaneous Hydrogen/Deuterium Exchange of Multitarget Gas-Phase Molecules by Electrospray Ionization Mass Spectrometry Coupled with Gas Chromatography.

    Science.gov (United States)

    Jeong, Eun Sook; Cha, Eunju; Cha, Sangwon; Kim, Sunghwan; Oh, Han Bin; Kwon, Oh-Seung; Lee, Jaeick

    2017-11-21

    In this study, a hydrogen/deuterium (H/D) exchange method using gas chromatography-electrospray ionization/mass spectrometry (GC-ESI/MS) was first investigated as a novel tool for online H/D exchange of multitarget analytes. The GC and ESI source were combined with a homemade heated column transfer line. GC-ESI/MS-based H/D exchange occurs in an atmospheric pressure ion source as a result of reacting the gas-phase analyte eluted from GC with charged droplets of deuterium oxide infused as the ESI spray solvent. The consumption of the deuterated solvent at a flow rate of 2 μL min -1 was more economical than that in online H/D exchange methods reported to date. In-ESI-source H/D exchange by GC-ESI/MS was applied to 11 stimulants with secondary amino or hydroxyl groups. After H/D exchange, the spectra of the stimulants showed unexchanged, partially exchanged, and fully exchanged ions showing various degrees of exchange. The relative abundances corrected for naturally occurring isotopes of the fully exchanged ions of stimulants, except for etamivan, were in the range 24.3-85.5%. Methylephedrine and cyclazodone showed low H/D exchange efficiency under acidic, neutral, and basic spray solvent conditions and nonexchange for etamivan with an acidic phenolic OH group. The in-ESI-source H/D exchange efficiency by GC-ESI/MS was sufficient to determine the number of hydrogen by elucidation of fragmentation from the spectrum. Therefore, this online H/D exchange technique using GC-ESI/MS has potential as an alternative method for simultaneous H/D exchange of multitarget analytes.

  6. Purification of adenoviral vectors by combined anion exchange and gel filtration chromatography.

    Science.gov (United States)

    Eglon, Marc N; Duffy, Aoife M; O'Brien, Timothy; Strappe, Padraig M

    2009-11-01

    Adenoviral vectors are used extensively in human gene therapy trials and in vaccine development. Large-scale GMP production requires a downstream purification process, and liquid chromatography is emerging as the most powerful mode of purification, enabling the production of vectors at a clinically relevant scale and quality. The present study describes the development of a two-step high-performance liquid chromatography (HPLC) process combining anion exchange (AIEX) and gel filtration (GF) in comparison with the caesium chloride density gradient method. HEK-293 cells were cultured in ten-layer CellStacks() and infected with 10 pfu/cell of adenoviral vector expressing green fluorescent protein (Ad5-GFP). Cell-bound virus was harvested and benzonase added to digest DNA, crude lysate was clarified by centrifugation and filtration prior to HPLC. Chromatography fractions were added to HEK-293 cells and GFP expression measured using a fluorescent plate reader. Using AIEX then GF resulted in an adenoviral vector with purity comparable to Ad5-GFP purified by CsCl, whereas the reverse process (GF-AIEX) showed a reduced purity by electrophoresis and required further buffer exchange of the product. The optimal process (AIEX-GF) resulted in a vector yield of 2.3 x 10(7) pfu/cm(2) of cell culture harvested compared to 3.3 x 10(7) pfu/cm(2) for CsCl. The process recovery for the HPLC process was 36% compared to 27.5% for CsCl and total virion to infectious particle ratios of 18 and 11, respectively, were measured. We present a simple two-step chromatography process that is capable of producing high-quality adenovirus at a titre suitable for scale-up and clinical translation.

  7. 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)

  8. 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.

  9. 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)

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

    OpenAIRE

    Chin, Sung Tong

    2017-01-01

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

  11. 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)

  12. 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.

  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. 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.

  15. Separation and determination of alditols and sugars by high-pH anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Andersen, Rikke; Sørensen, A.

    2000-01-01

    Carbohydrates such as alditols (polyols or sugar alcohols), monosaccharides and disaccharides are separated as anions by anion-exchange chromatography with a sodium hydroxide eluent, MA1 CarboPac column and pulsed amperometric detection. We report a high-pH anion-exchange chromatographic-pulsed a......Carbohydrates such as alditols (polyols or sugar alcohols), monosaccharides and disaccharides are separated as anions by anion-exchange chromatography with a sodium hydroxide eluent, MA1 CarboPac column and pulsed amperometric detection. We report a high-pH anion-exchange chromatographic......-pulsed amperometric detection (HPAEC-PAD) method that determines all the polyols used as food additives in food products and the most commonly found mono- and disaccharides on a routine basis. The linearity, repeatability, internal reproducibility and accuracy are described. The applicability of the method has been...

  16. 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

  17. 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.

  18. 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

  19. Mixed retention mechanism of proteins in weak anion-exchange chromatography.

    Science.gov (United States)

    Liu, Peng; Yang, Haiya; Geng, Xindu

    2009-10-30

    Using four commercial weak anion-exchange chromatography (WAX) columns and 11 kinds of different proteins, we experimentally examined the involvement of hydrophobic interaction chromatography (HIC) mechanism in protein retention on the WAX columns. The HIC mechanism was found to operate in all four WAX columns, and each of these columns had a better resolution in the HIC mode than in the corresponding WAX mode. Detailed analysis of the molecular interactions in a chromatographic system indicated that it is impossible to completely eliminate hydrophobic interactions from a WAX column. Based on these results, it may be possible to employ a single WAX column for protein separation by exploiting mixed modes (WAX and HIC) of retention. The stoichiometric displacement theory and two linear plots were used to show that mechanism of the mixed modes of retention in the system was a combination of two kinds of interactions, i.e., nonselective interactions in the HIC mode and selective interactions in the IEC mode. The obtained U-shaped elution curve of proteins could be distinguished into four different ranges of salt concentration, which also represent four retention regions.

  20. 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.

  1. 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…

  2. 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).

  3. Volume reduction of ion exchange resin by a pyrolysis technique

    International Nuclear Information System (INIS)

    Matsuda, M.; Funabashi, K.; Uchida, S.; Kikuchi, M.

    1985-01-01

    Volume reduction techniques, such as incineration and acid digestion, of spent ion exchange resins from nuclear power plants are being developed with a view toward reducing radioactive waste volume and also making the final waste form more stable. The authors chose pyrolysis as a technique that can be done at low operating temperatures and low gas flow rates in a reactor vessel. Fundamental experiments were performed to clarify the resin pyrolysis characteristics, and the optimum pyrolysis temperature was determined. Consequently, a pilot plant with a treatment capacity of approx. 50 kg/batch was constructed based on the results. Using the pilot plant, the authors are now performing pyrolysis of the resins and solidification of their residues. This report will give the results of fundamental experiments and pilot plant tests

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

    Science.gov (United States)

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

    2018-01-01

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

  5. [Blood levels of homocysteine by high pressure liquid chromatography and comparison with two other techniques].

    Science.gov (United States)

    Ceppa, F; Drouillard, I; Chianea, D; Burnat, P; Perrier, F; Vaillant, C; El Jahiri, Y

    1999-01-01

    Cardio-vascular diseases are the most common cause of death in industrialized countries. A new marker has emerged among offending risk factors in the past few years: homocysteine. This sulphured amino-acid is an important intermediate in transsulphuration and remethylation reactions of methionine's metabolism. We proposed to evaluate a home made method of determination for this parameter by high performance liquid chromatography (HPLC) and to compare it to fluorescence polarization immunoassay technique (FPIA) and to gaz phase chromatography (CG-SM). This method associated with good sensibility and precision remain much less expensive than FPIA technique.

  6. 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)

  7. An on-line monitor for cation exchange elution chromatography using lithium silicate glass beads as solid scintillator

    International Nuclear Information System (INIS)

    Zhu Rongbao; Yang Liucheng; Wei Liansheng; Ji Liqiang; Zhang Zengrui

    1988-03-01

    A new type of on-line monitoring system used to monitor radioactive nuclides with α or soft β radiation in the effluent from a high pressure ion exchange column is described. The beads made of cerium-impregnated lithium silicate glass are used as scientillation material. They are filled into a quartz glass tube to form a flow cell. By reducing the diameter of glass beads to more closly approximate the average range of α or soft β radiation in solution, the absolute counting efficiency for 241 Am, 242 Cm α radiation have reached and 85.8% and 92.8% respectively, for 14 C, 90 Sr- 90 Y β radiation, 62.1% and 88.6% respectively. These values can be comparable to those achieved with on-line liquid scientillation technique. When the total amount of 241 Am added into column is decreased to 7.4 Bq it is still possible to obtain a clear chromatography peak (half peak width = 0.22 mL)

  8. 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.

  9. Characterisation of brewpub beer carbohydrates using high performance anion exchange chromatography coupled with pulsed amperometric detection.

    Science.gov (United States)

    Arfelli, Giuseppe; Sartini, Elisa

    2014-01-01

    High performance anion exchange chromatography (HPAEC) coupled with pulsed amperometric detection (PAD) was optimised in order to quantify mannose, maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose and maltoheptaose content of beer. The method allows the determination of above mentioned oligosaccharides, in a single chromatographic run, without any pre-treatment. Limit of detection and limit of quantification were suitable for beer. Accuracy and repeatability were good for the entire amount considered. Once optimised HPAEC PAD for the specific matrix, the second goal of this research was to verify the possibility to discriminate beers, depending on their style. The carbohydrates content of brewpub commercial beers was very variable, ranging from 19.3 to 1469mg/L (mannose), 34.5 to 2882mg/L (maltose), 141.9 to 20731mg/L (maltotriose), 168.5 to 7650mg/L (maltotetraose), 20.1 to 2537mg/L (maltopentaose), 22.9 to 3295mg/L (maltohexaose), 8.5 to 2492mg/L (maltoeptaose), even in the same style of beer. However, the carbohydrates content was useful, jointed with other compounds amount, to discriminate different styles of beer. As a matter of fact, principal component analysis put in evidence beer differences considering some fermentation conditions and colour. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. 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.

  11. 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.

  12. 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

  13. 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.

  14. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    Science.gov (United States)

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Chiral ligand exchange high-speed countercurrent chromatography: mechanism, application and comparison with conventional liquid chromatography in enantioseparation of aromatic α-hydroxyl acids

    Science.gov (United States)

    Tong, Shengqiang; Shen, Mangmang; Cheng, Dongping; Ito, Yoichiro; Yan, Jizhong

    2014-01-01

    This work concentrates on the separation mechanism and application of chiral ligand exchange high-speed countercurrent chromatography (HSCCC) in enantioseparations, and comparison with traditional chiral ligand exchange high performance liquid chromatography (HPLC). The enantioseparation of ten aromatic α-hydroxyl acids were performed by these two chromatographic methods. Results showed that five of the racemates were successfully enantioseparated by HSCCC while only three of the racemates could be enantioseparated by HPLC using a suitable chiral ligand mobile phase additive. For HSCCC, the two-phase solvent system was composed of butanol-water (1:1, v/v), to which N-n-dodecyl-L-proline was added in the organic phase as chiral ligand and cupric acetate was added in the aqueous phase as a transition metal ion. Various operation parameters in HSCCC were optimized by enantioselective liquid-liquid extraction. Based on the results of the present studies the separation mechanism for HSCCC was proposed. For HPLC, the optimized mobile phase composed of aqueous solution containing 6 mmol L−1 L-phenylalanine and 3 mmol L−1 cupric sulfate and methanol was used for enantioseparation. Among three ligands tested on a conventional reverse stationary phase column, only one was found to be effective. In the present studies HSCCC presented unique advantages due to its high versatility of two-phase solvent systems and it could be used as an alternative method for enantioseparations. PMID:25087742

  16. Sequence-Specific Model for Peptide Retention Time Prediction in Strong Cation Exchange Chromatography.

    Science.gov (United States)

    Gussakovsky, Daniel; Neustaeter, Haley; Spicer, Victor; Krokhin, Oleg V

    2017-11-07

    The development of a peptide retention prediction model for strong cation exchange (SCX) separation on a Polysulfoethyl A column is reported. Off-line 2D LC-MS/MS analysis (SCX-RPLC) of S. cerevisiae whole cell lysate was used to generate a retention dataset of ∼30 000 peptides, sufficient for identifying the major sequence-specific features of peptide retention mechanisms in SCX. In contrast to RPLC/hydrophilic interaction liquid chromatography (HILIC) separation modes, where retention is driven by hydrophobic/hydrophilic contributions of all individual residues, SCX interactions depend mainly on peptide charge (number of basic residues at acidic pH) and size. An additive model (incorporating the contributions of all 20 residues into the peptide retention) combined with a peptide length correction produces a 0.976 R 2 value prediction accuracy, significantly higher than the additive models for either HILIC or RPLC. Position-dependent effects on peptide retention for different residues were driven by the spatial orientation of tryptic peptides upon interaction with the negatively charged surface functional groups. The positively charged N-termini serve as a primary point of interaction. For example, basic residues (Arg, His, Lys) increase peptide retention when located closer to the N-terminus. We also found that hydrophobic interactions, which could lead to a mixed-mode separation mechanism, are largely suppressed at 20-30% of acetonitrile in the eluent. The accuracy of the final Sequence-Specific Retention Calculator (SSRCalc) SCX model (∼0.99 R 2 value) exceeds all previously reported predictors for peptide LC separations. This also provides a solid platform for method development in 2D LC-MS protocols in proteomics and peptide retention prediction filtering of false positive identifications.

  17. 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

  18. 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.

  19. Preparation and evaluation of a hydrophilic interaction and cation-exchange chromatography stationary phase modified with 2-methacryloyloxyethyl phosphorylcholine.

    Science.gov (United States)

    Xiong, Caifeng; Yuan, Jie; Wang, Zhiying; Wang, Siyao; Yuan, Chenchen; Wang, Lili

    2018-04-20

    In this work, 2-methacryloyloxyethyl phosphorylcholine (MPC) was used as a ligand to prepare a novel mixed-mode chromatography (MMC) stationary phase by the thiol-ene click reaction onto silica (MPC-silica). It was found that this MPC-silica showed the retention characteristics of hydrophilic interaction chromatography (HILIC) and weak cation exchange chromatography (WCX) under suitable mobile phase conditions. In detail, acidic and basic hydrophilic compounds and puerarin from pueraria were separated quickly with HILIC mode. Meanwhile, six standard proteins were allowed to reach baseline separation in WCX mode, and protein separation from egg white was also achieved with this mode. In addition, reduced/denatured lysozyme could be refolded with the MPC-silica column. In the meantime, the MPC-silica has been applied for refolding with simultaneous purification of recombinant human Delta-like1-RGD (rhDll1-RGD) expressed in Escherichia coli. The results show that the mass recovery and purity of rhDll1-RGD could reach 63.4% and 97% by one step, respectively. Furthermore, the reporter assay results demonstrated that refolded with simultaneously purified rhDll1-RGD could efficiently activate the signalling pathway in a dose-dependent manner. In general, this MPC-silica has good resolution and selectivity in the separation of polar compounds and protein samples in different high-performance liquid chromatography (HPLC) modes, and it successfully achieved refolding with simultaneous purification of denatured protein. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Separation of Poly(styrene-block-t-butyl methacrylate) Copolymers by Various Liquid Chromatography Techniques

    Science.gov (United States)

    Šmigovec Ljubič, Tina; Pahovnik, David; Žigon, Majda; Žagar, Ema

    2012-01-01

    The separation of a mixture of three poly(styrene-block-t-butyl methacrylate) copolymers (PS-b-PtBMA), consisting of polystyrene (PS) blocks of similar length and t-butyl methacrylate (PtBMA) blocks of different lengths, was performed using various chromatographic techniques, that is, a gradient liquid chromatography on reversed-phase (C18 and C8) and normal-phase columns, a liquid chromatography under critical conditions for polystyrene as well as a fully automated two-dimensional liquid chromatography that separates block copolymers by chemical composition in the first dimension and by molar mass in the second dimension. The results show that a partial separation of the mixture of PS-b-PtBMA copolymers can be achieved only by gradient liquid chromatography on reversed-phase columns. The coelution of the two block copolymers is ascribed to a much shorter PtBMA block length, compared to the PS block, as well as a small difference in the length of the PtBMA block in two of these copolymers, which was confirmed by SEC-MALS and NMR spectroscopy. PMID:22489207

  1. Peak broadening in paper chromatography and related techniques : III. Peak broadening in thin-layer chromatography on cellulose powder

    NARCIS (Netherlands)

    Ligny, C.L. de; Remijnse, A.G.

    1968-01-01

    The mechanism of peak broadening in thin-layer chromatography on cellulose powder was investigated by comparing the peak widths obtained in chromatography with those caused only by diffusion in the cellulose powder, for a set of amino acids of widely differing RF values and six kinds of cellulose

  2. Quantification of the Pyrrolizidine Alkaloid Jacobine in Crassocephalum crepidioides by Cation Exchange High-Performance Liquid Chromatography.

    Science.gov (United States)

    Rozhon, Wilfried; Kammermeier, Lukas; Schramm, Sebastian; Towfique, Nayeem; Adebimpe Adedeji, N; Adesola Ajayi, S; Poppenberger, Brigitte

    2018-01-01

    Pyrrolizidine alkaloids (PAs) are secondary plant metabolites with considerable hepatoxic, tumorigenic and genotoxic potential. For separation, reversed phase chromatography is commonly used because of its excellent compatibility with detection by mass spectrometry. However, reversed phase chromatography has a low selectivity for PAs. The objective of this work was to investigate the suitability of cation exchange chromatography for separation of PAs and to develop a rapid method for quantification of jacobine in Crassocephalum crepidioides that is suitable for analysis of huge sample numbers as required for mutant screening procedures. We demonstrate that cation exchange chromatography offers excellent selectivity for PAs allowing their separation from most other plant metabolites. Due to the high selectivity, plant extracts can be directly analysed after simple sample preparation. Detection with UV at 200 nm instead of mass spectrometry can be applied, which makes the method very simple and cost-effective. The recovery rate of the method exceeded 95%, the intra-day and inter-day standard deviations were below 7% and the limit of detection and quantification were 1 mg/kg and 3 mg/kg, respectively. The developed method is sufficiently sensitive for reproducible detection of jacobine in C. crepidioides. Simple sample preparation and rapid separation allows for quantification of jacobine in plant material in a high-throughput manner. Thus, the method is suitable for genetic screenings and may be applicable for other plant species, for instance Jacobaea maritima. In addition, our results show that C. crepidioides cannot be considered safe for human consumption. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  3. 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.

  4. Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

    NARCIS (Netherlands)

    Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

    2003-01-01

    Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry

  5. Indirect fluorometric detection techniques on thin layer chromatography and effect of ultrasound on gel electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Yinfa, Ma.

    1990-12-10

    Thin-layer chromatography (TLC) is a broadly applicable separation technique. It offers many advantages over high performance liquid chromatography (HPLC), such as easily adapted for two-dimensional separation, for whole-column'' detection and for handling multiple samples, etc. However, due to its draggy development of detection techniques comparing with HPLC, TLC has not received the attention it deserves. Therefore, exploring new detection techniques is very important to the development of TLC. It is the principal of this dissertation to present a new detection method for TLC -- indirect fluorometric detection method. This detection technique is universal sensitive, nondestructive, and simple. This will be described in detail from Sections 1 through Section 5. Section 1 and 3 describe the indirect fluorometric detection of anions and nonelectrolytes in TLC. In Section 2, a detection method for cations based on fluorescence quenching of ethidium bromide is presented. In Section 4, a simple and interesting TLC experiment is designed, three different fluorescence detection principles are used for the determination of caffeine, saccharin and sodium benzoate in beverages. A laser-based indirect fluorometric detection technique in TLC is developed in Section 5. Section 6 is totally different from Sections 1 through 5. An ultrasonic effect on the separation of DNA fragments in agarose gel electrophoresis is investigated. 262 refs.

  6. Analysis of human milk oligosaccharides using high-performance anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    ) and lacto-N-neotetraose (Galβ1-4GlcNAcβ1-3Galβ1-4Glc), among others. High-performance anion-exchange chromatography (HPAE) with pulsed amperometric detection (PAD) is an analysis method highly suited for carbohydrates. HPAE with alkaline eluents results in retention of neutral carbohydrates depending...... on the number of charged group in the molecule, pH and concentration of competing anions, while the PAD has sensitivity for carbohydrates in the pmol-range (Lee 1990). As a basis for the development and optimisation of HPAE elution methods, the parameter space was investigated in terms of eluent concentrations...

  7. Separation of human milk oligosaccharides using high-performance anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    individual mothers is considerable, ranging from as few as 23 and up to 130 different oligosaccharides. HMOs are known as beneficial for infant health and development, and have received increasing attention in recent years (Bode & Jantscher-Krenn 2012). High-performance anion-exchange chromatography (HPAE......) with pulsed amperometric detection (PAD) is an analysis method highly suited for carbohydrates. HPAE with alkaline eluents results in retention of neutral carbohydrates depending on the number of charged groups in the molecule, pH and concentration of competing anions, while PAD has sensitivity...

  8. Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

    Science.gov (United States)

    Baghdady, Yehia Z; Schug, Kevin A

    2016-01-01

    Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. 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

  10. Analysis of polymeric phenolics in red wines using different techniques combined with gel permeation chromatography fractionation.

    Science.gov (United States)

    Guadalupe, Zenaida; Soldevilla, Alberto; Sáenz-Navajas, María-Pilar; Ayestarán, Belén

    2006-04-21

    A multiple-step analytical method was developed to improve the analysis of polymeric phenolics in red wines. With a common initial step based on the fractionation of wine phenolics by gel permeation chromatography (GPC), different analytical techniques were used: high-performance liquid chromatography-diode array detection (HPLC-DAD), HPLC-mass spectrometry (MS), capillary zone electrophoresis (CZE) and spectrophotometry. This method proved to be valid for analyzing different families of phenolic compounds, such as monomeric phenolics and their derivatives, polymeric pigments and proanthocyanidins. The analytical characteristics of fractionation by GPC were studied and the method was fully validated, yielding satisfactory statistical results. GPC fractionation substantially improved the analysis of polymeric pigments by CZE, in terms of response, repeatability and reproducibility. It also represented an improvement in the traditional vanillin assay used for proanthocyanidin (PA) quantification. Astringent proanthocyanidins were also analyzed using a simple combined method that allowed these compounds, for which only general indexes were available, to be quantified.

  11. 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.

  12. 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

  13. Supercritical fluid chromatography coupled with in-source atmospheric pressure ionization hydrogen/deuterium exchange mass spectrometry for compound speciation.

    Science.gov (United States)

    Cho, Yunju; Choi, Man-Ho; Kim, Byungjoo; Kim, Sunghwan

    2016-04-29

    An experimental setup for the speciation of compounds by hydrogen/deuterium exchange (HDX) with atmospheric pressure ionization while performing chromatographic separation is presented. The proposed experimental setup combines the high performance supercritical fluid chromatography (SFC) system that can be readily used as an inlet for mass spectrometry (MS) and atmospheric pressure photo ionization (APPI) or atmospheric pressure chemical ionization (APCI) HDX. This combination overcomes the limitation of an approach using conventional liquid chromatography (LC) by minimizing the amount of deuterium solvents used for separation. In the SFC separation, supercritical CO2 was used as a major component of the mobile phase, and methanol was used as a minor co-solvent. By using deuterated methanol (CH3OD), AP HDX was achieved during SFC separation. To prove the concept, thirty one nitrogen- and/or oxygen-containing standard compounds were analyzed by SFC-AP HDX MS. The compounds were successfully speciated from the obtained SFC-MS spectra. The exchange ions were observed with as low as 1% of CH3OD in the mobile phase, and separation could be performed within approximately 20min using approximately 0.24 mL of CH3OD. The results showed that SFC separation and APPI/APCI HDX could be successfully performed using the suggested method. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Large scale chromatographic separations using continuous displacement chromatography (CDC)

    International Nuclear Information System (INIS)

    Taniguchi, V.T.; Doty, A.W.; Byers, C.H.

    1988-01-01

    A process for large scale chromatographic separations using a continuous chromatography technique is described. The process combines the advantages of large scale batch fixed column displacement chromatography with conventional analytical or elution continuous annular chromatography (CAC) to enable large scale displacement chromatography to be performed on a continuous basis (CDC). Such large scale, continuous displacement chromatography separations have not been reported in the literature. The process is demonstrated with the ion exchange separation of a binary lanthanide (Nd/Pr) mixture. The process is, however, applicable to any displacement chromatography separation that can be performed using conventional batch, fixed column chromatography

  15. Novel Method for Exchange of Impella Circulatory Assist Catheter: The "Trojan Horse" Technique.

    Science.gov (United States)

    Phillips, Colin T; Tamez, Hector; Tu, Thomas M; Yeh, Robert W; Pinto, Duane S

    2017-07-01

    Patients with an indwelling Impella may require escalation of hemodynamic support or exchange to another circulatory assistance platform. As such, preservation of vascular access is preferable in cases where anticoagulation cannot be discontinued or to facilitate exchange to an alternative catheter or closure device. Challenges exist in avoiding bleeding and loss of wire access in these situations. We describe a single-access "Trojan Horse" technique that minimizes bleeding while maintaining arterial access for rapid exchange of this percutaneous ventricular assist device.

  16. Probing the Complementarity of FAIMS and Strong Cation Exchange Chromatography in Shotgun Proteomics

    OpenAIRE

    Creese, Andrew J.; Shimwell, Neil J.; Larkins, Katherine P. B.; Heath, John K.; Cooper, Helen J.

    2013-01-01

    High field asymmetric waveform ion mobility spectrometry (FAIMS), also known as differential ion mobility spectrometry, coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) offers benefits for the analysis of complex proteomics samples. Advantages include increased dynamic range, increased signal-to-noise, and reduced interference from ions of similar m/z. FAIMS also separates isomers and positional variants. An alternative, and more established, method of reducing sample co...

  17. An iterative homogenization technique that preserves assembly core exchanges

    International Nuclear Information System (INIS)

    Mondot, Ph.; Sanchez, R.

    2003-01-01

    A new interactive homogenization procedure for reactor core calculations is proposed that requires iterative transport assembly and diffusion core calculations. At each iteration the transport solution of every assembly type is used to produce homogenized cross sections for the core calculation. The converged solution gives assembly fine multigroup transport fluxes that preserve macro-group assembly exchanges in the core. This homogenization avoids the periodic lattice-leakage model approximation and gives detailed assembly transport fluxes without need of an approximated flux reconstruction. Preliminary results are given for a one-dimensional core model. (authors)

  18. 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.

  19. Bicarbonate adsorption band of the chromatography for carbon isotope separation using anion exchangers

    International Nuclear Information System (INIS)

    Takeda, Kunihiko; Obanawa, Heiichiro; Hata, Masahisa; Sato, Katsuya

    1985-01-01

    The equilibria of bicarbonate ion between two phases were studied for the carbon isotope separation using anion exchangers. The condition of the formation of a bicarbonate adsorption band was quantitatively discussed. The formation of the adsorption band depends on the difference of S-potential which is the sum of the standard redection chemical potentials and L-potential which is the sum of the reduction chemical potential. The isotopic separation factor observed was about 1.012, independent of the concentrations of acid and alkali in the solutions. The isotopic separation factor was considered to be determined by the reaction of bicarbonate ion on anion exchangers and carbon dioxide dissolved in solutions. The enriched carbon isotope whose isotopic abundance ratio ( 13 C/ 12 C) was 1.258 was obtained with the column packed with anion exchangers. (author)

  20. Review of online coupling of sample preparation techniques with liquid chromatography.

    Science.gov (United States)

    Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-03-07

    Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Behavior of copper (II )and uranium ( VI) in precipitation chromatography in the system anion exchange resin - hexacyanoferrate (II )

    International Nuclear Information System (INIS)

    Seneda, Jose Antonio

    1997-01-01

    In this work it is shown the efficiency of precipitation chromatography for separation and concentration of metallic elements by using a strong anionic-exchange resin saturated with hexacyanoferrate (II). Metallic cations, like Cu (II) and U (VI), are retained from highly diluted solutions and enriched into the resin, in the form of the correspondent insoluble hexacyanoferrate (II), precipitated inside the resin, which permitted the visual observation of a chromatographic zone on the top of the column. It will be discussed the conditions of sorption and elution of the cations uptake by the resin. This system permits the enrichment of the above mentioned cations onto the resin and offers the possibility of interesting separations as well. (author)

  2. N-Decyl-S-trityl-(R)-cysteine, a new chiral selector for "green" ligand-exchange chromatography applications.

    Science.gov (United States)

    Carotti, Andrea; Ianni, Federica; Camaioni, Emidio; Pucciarini, Lucia; Marinozzi, Maura; Sardella, Roccaldo; Natalini, Benedetto

    2017-09-10

    In search for new enantioselectivity profiles, the N-decyl-S-trityl-(R)-cysteine [C 10 -(R)-STC] was synthesized through a one-step procedure and then hydrophobically adsorbed onto an octadecylsilica surface to generate a stable chiral stationary phase for ligand-exchange chromatography (CLEC-CSP) applications. The CLEC analysis was carried out on underivatized amino acids, by using a Cu(II) sulphate (1.0mM) containing aqueous eluent system. Most of the analysed compounds (34 out of 45) were enantiodiscriminated by the C 10 -(R)-STC-based CSP, with resolution factor (R S ) values up to 8.86. Conformationally rigid and hydrophobic ligands often experienced the largest enantioselectivity effects. A high loadability emerged from the analysis of rac-NorVal (selected as prototype test compound): up to 20mg/mL were efficiently enantioseparated with the CLEC-CSP. Two in-line hand-made cartridges filled with a strong cation-exchange resin allowed the effective catching of Cu(II) ions after the semi-preparative enantioseparation. The quantitative recovery of the rac-NorVal enantiomers was made possible by flowing through the cartridge a 5% (v) ammonia solution. The CLEC phase proved successful in the enantioselective analysis of a commercially available (S)-Leu containing tablet. Furthermore, in order to understand the molecular basis for a successful use of the C 10 -(R)-STC-based CLEC system, a descriptive structure-separation relationship study was performed. As a result, all compounds with a MEAN-QPlogS (a hydrophilicity descriptor) value lower than 0.373 can be most likely enantioseparated with the CLEC system under investigation. In the work, the numerous aspects complying with the principles of green chromatography are highlighted and discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  4. Systematic comparison of static and dynamic headspace sampling techniques for gas chromatography.

    Science.gov (United States)

    Kremser, Andreas; Jochmann, Maik A; Schmidt, Torsten C

    2016-09-01

    Six automated, headspace-based sample preparation techniques were used to extract volatile analytes from water with the goal of establishing a systematic comparison between commonly available instrumental alternatives. To that end, these six techniques were used in conjunction with the same gas chromatography instrument for analysis of a common set of volatile organic carbon (VOC) analytes. The methods were thereby divided into three classes: static sampling (by syringe or loop), static enrichment (SPME and PAL SPME Arrow), and dynamic enrichment (ITEX and trap sampling). For PAL SPME Arrow, different sorption phase materials were also included in the evaluation. To enable an effective comparison, method detection limits (MDLs), relative standard deviations (RSDs), and extraction yields were determined and are discussed for all techniques. While static sampling techniques exhibited sufficient extraction yields (approx. 10-20 %) to be reliably used down to approx. 100 ng L(-1), enrichment techniques displayed extraction yields of up to 80 %, resulting in MDLs down to the picogram per liter range. RSDs for all techniques were below 27 %. The choice on one of the different instrumental modes of operation (aforementioned classes) was thereby the most influential parameter in terms of extraction yields and MDLs. Individual methods inside each class showed smaller deviations, and the least influences were observed when evaluating different sorption phase materials for the individual enrichment techniques. The option of selecting specialized sorption phase materials may, however, be more important when analyzing analytes with different properties such as high polarity or the capability of specific molecular interactions. Graphical Abstract PAL SPME Arrow during the extraction of volatile analytes from the headspace of an aqueous sample.

  5. The influence of retention on the plate height in ion-exchange chromatography

    DEFF Research Database (Denmark)

    Hansen, Ernst; Mollerup, Jørgen

    2004-01-01

    The plate heights for the amino acid tyrosine (anion exchange) and the polypeptide aprotinin (cation exchange) were determined on a porous media (Resource 15) and a get filled media (HyperD 20) at salt concentrations ranging from weak to strong retention. At a constant velocity, measurements showed....... In this article, the rate of mass transfer in the particles is described by three different rate mechanisms, pore diffusion, solid diffusion, and parallel diffusion. The van Deemter equation was used to model the data to determine the mass-transfer properties. The development of the plate height with increasing...... retention revealed a characteristic behavior for each rate mechanism. In the pore diffusion model, the plate height increased toward a constant value at strong retention, while the plate height in the solid diffusion model decreased, approaching a constant value at strong retention. In the parallel...

  6. Multiple inert gas elimination technique by micropore membrane inlet mass spectrometry--a comparison with reference gas chromatography.

    Science.gov (United States)

    Kretzschmar, Moritz; Schilling, Thomas; Vogt, Andreas; Rothen, Hans Ulrich; Borges, João Batista; Hachenberg, Thomas; Larsson, Anders; Baumgardner, James E; Hedenstierna, Göran

    2013-10-15

    The mismatching of alveolar ventilation and perfusion (VA/Q) is the major determinant of impaired gas exchange. The gold standard for measuring VA/Q distributions is based on measurements of the elimination and retention of infused inert gases. Conventional multiple inert gas elimination technique (MIGET) uses gas chromatography (GC) to measure the inert gas partial pressures, which requires tonometry of blood samples with a gas that can then be injected into the chromatograph. The method is laborious and requires meticulous care. A new technique based on micropore membrane inlet mass spectrometry (MMIMS) facilitates the handling of blood and gas samples and provides nearly real-time analysis. In this study we compared MIGET by GC and MMIMS in 10 piglets: 1) 3 with healthy lungs; 2) 4 with oleic acid injury; and 3) 3 with isolated left lower lobe ventilation. The different protocols ensured a large range of normal and abnormal VA/Q distributions. Eight inert gases (SF6, krypton, ethane, cyclopropane, desflurane, enflurane, diethyl ether, and acetone) were infused; six of these gases were measured with MMIMS, and six were measured with GC. We found close agreement of retention and excretion of the gases and the constructed VA/Q distributions between GC and MMIMS, and predicted PaO2 from both methods compared well with measured PaO2. VA/Q by GC produced more widely dispersed modes than MMIMS, explained in part by differences in the algorithms used to calculate VA/Q distributions. In conclusion, MMIMS enables faster measurement of VA/Q, is less demanding than GC, and produces comparable results.

  7. 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.

  8. Ergot alkaloids in rye flour determined by solid-phase cation-exchange and high-pressure liquid chromatography with fluorescence detection

    DEFF Research Database (Denmark)

    Storm, Ida Marie Lindhardt Drejer; Rasmussen, Peter Have; Strobel, B.W.

    2008-01-01

    Ergot alkaloids are mycotoxins that are undesirable contaminants of cereal products, particularly rye. A method was developed employing clean-up by cation-exchange solid-phase extraction, separation by high-performance liquid chromatography under alkaline conditions and fluorescence detection...

  9. 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.

  10. Cation-exchange high-performance liquid chromatography for variant hemoglobins and HbF/A2: What must hematopathologists know about methodology?

    Science.gov (United States)

    Sharma, Prashant; Das, Reena

    2016-03-26

    Cation-exchange high-performance liquid chromatography (CE-HPLC) is a widely used laboratory test to detect variant hemoglobins as well as quantify hemoglobins F and A2 for the diagnosis of thalassemia syndromes. It's versatility, speed, reproducibility and convenience have made CE-HPLC the method of choice to initially screen for hemoglobin disorders. Despite its popularity, several methodological aspects of the technology remain obscure to pathologists and this may have consequences in specific situations. This paper discusses the basic principles of the technique, the initial quality control steps and the interpretation of various controls and variables that are available on the instrument output. Subsequent sections are devoted to methodological considerations that arise during reporting of cases. For instance, common problems of misidentified peaks, totals crossing 100%, causes of total area being above or below acceptable limits and the importance of pre-integration region peaks are dealt with. Ultimately, CE-HPLC remains an investigation, the reporting of which combines in-depth knowledge of the biological basics with more than a working knowledge of the technological aspects of the technique.

  11. Validation of Extraction Paper Chromatography as a Quality Control Technique for Analysis of Sr-90 in Y-90 Product

    International Nuclear Information System (INIS)

    Nipavan, Poramatikul; Jatupol, Sangsuriyan; Wiranee, Sriweing

    2009-07-01

    Full text: Yttrium-90 (Y-90) is a daughter product of strontium-90 (Sr-90). It is specified that there should be less than 2 micro-curie of Sr-90 in Y-90 radiopharmaceuticals. Since both nuclides are beta emitting and there is always a contamination of Y-90 in Sr-90 sample, validation of the analytical method is necessary. In this study, commercial Y-90 and Sr-85 (a gamma emitting isotope of strontium) were used as daughter and mother nuclides, respectively. Extraction paper chromatography technique and its efficient validation method were investigated. Bis-(2-ethylhexyl) diphosphonate was dropped at the origin of chromatography paper and air dried prior to sample drops. Validation of the separation was done by radio-chromatography scanning of the chromatography paper. Their energy spectra were identified in the spectra mode of Packard Cobra II automatic gamma counter, which can differentiate a pure gamma, a pure beta and a mixture of beta and gamma nuclides. Results showed that yttrium acetate remained fixed at the origin of the chromatography paper while strontium acetate moved to the solvent front when developed in saline. In conclusion, the extraction paper chromatography technique can effectively separate Sr-90 from Y-90

  12. Simultaneous determination of 13 carbohydrates using high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry.

    Science.gov (United States)

    Zhao, Dan; Feng, Feng; Yuan, Fei; Su, Jin; Cheng, Yan; Wu, Hanqiu; Song, Kun; Nie, Bo; Yu, Lian; Zhang, Feng

    2017-04-01

    A simple, accurate, and highly sensitive method was developed for the determination of 13 carbohydrates in polysaccharide of Spirulina platensis based on high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry. Samples were extracted with deionized water using ultrasonic-assisted extraction, and the ultrasound-assisted extraction conditions were optimized by Box-Behnken design. Then the extracted polysaccharide was hydrolyzed by adding 1 mol/L trifluoroacetic acid before determination by high-performance anion-exchange chromatography coupled with pulsed amperometric detection and confirmed by high-performance anion-exchange chromatography coupled with mass spectrometry. The high-performance anion-exchange chromatography coupled with pulsed amperometric detection method was performed on a CarboPac PA20 column by gradient elution using deionized water, 0.1 mol/L sodium hydroxide solution, and 0.4 mol/L sodium acetate solution. Excellent linearity was observed in the range of 0.05-10 mg/L. The average recoveries ranged from 80.7 to 121.7%. The limits of detection and limits of quantification for 13 carbohydrates were 0.02-0.10 and 0.2-1.2  μg/kg, respectively. The developed method has been successfully applied to ambient samples, and the results indicated that high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry could provide a rapid and accurate method for the simultaneous determination of carbohydrates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Sulfur isotope separation by anion exchange chromatography: 34 S isotope enrichment

    International Nuclear Information System (INIS)

    Bendassolli, Jose Albertino; Trivelin, Paulo Cesar O.; Carneiro Junior, Francisco

    1995-01-01

    The 34 S isotope separation was carried out by isotopic exchange reactions between sulphurous acid in solution and bisulphite anions adsorbed on an ammonium quaternary (Dowex 1 x 8 and Dowex 2 x 8, 100-200 mesh) anion exchange resin packed in columns. Each resin column had 130 cm length and 2.2 cm diameter. The columns were connected in series during displacement of bisulphite bands. For the experiments, a band of bisulphite was fixed to the anion resin, initially in the hydroxyl ion form, and subsequently eluted with 0.2 0.3, 0.4 and 0.6 mol L -1 HCL solution. The hydrochloric acid solution was kept under a nitrogen atmosphere at 245 KPa of pressure, in order to prevent the evolution of gases and also the oxidation of the bisulphite. The experiments showed that the best results were obtained with the elution of bisulphite with 0.2 mol.L -1 HCL, with the Dowex 1 x 8 resin. Enrichments in 34 S of 17.33 atoms% were obtained using Dowex 1 x 8 resin, 0.2 mol.L -1 HCL solution and band displacement of 50 m. Replacing the depleted portion of the band with natural bisulphite, for each 10 m of band displacement, produced 6.79 mmol of sulphurous acid enriched with approximately 17% of 34 S, after 14 m of band dislocation. (author). 7 refs., 1 fig., 2 tabs

  14. 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.)

  15. Radiochemical separation from111In from Cd and Cu by Ion exchange chromatography

    International Nuclear Information System (INIS)

    Yavari, R.; Khanchi, A. R.; Rafii, H.; Maragheh, M. G.; Farajzadeh, M. A.

    2005-01-01

    In this work, during the nuclear reaction of nat Cd (p, xn) 111 In, the irradiated cadmium target was dissolved in 3 M nitric acid. It was passed through a cation exchange column, containing 4 g. of AG 5OW-X8, and then was separated from cadmium and copper impurities by using a simple two stage procedure. At the first stage, cadmium was eluted with acetone-water-hydrobromic acid solution. At the second stage, indium was eluted with acetone-water-hydrochloric acid solution. The effluent was evaporated to dry and the residue was dissolved in 0.01M hydrochloric acid. The overall yield of the procedure was 95 ± 1 percent and the amount of cadmium and copper contamination were 0.3 and 0.1 ppm, respectively

  16. Quantitative chromatography in the analysis of labelled compounds 1. Quantitative paper chromotography of amino acids by A spot comparison technique

    International Nuclear Information System (INIS)

    Barakat, M.F.; Farag, A.N.; El-Gharbawy, A.A.

    1974-01-01

    For the determination of the specific activity of labelled compounds separated by paper sheet chromatography, it was found essential to perfect the quantitative aspect of the paper chromatographic technique. Actually, so far paper chromatography has been used as a separation tool mainly and its use in quantification of the separated materials is by far less studied. In the present work, the quantitative analysis of amino acids by paper sheet chromatography has been carried out by methods, depending on the use of the relative spot area values for correcting the experimental data obtained. The results obtained were good and reproducible. The main advantage of the proposed technique is its extreme simplicity. No complicated equipment of procedures are necessary

  17. 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.

  18. Size exclusion and anion exchange high performance liquid chromatography for characterizing metals bound to marine dissolved organic matter

    International Nuclear Information System (INIS)

    García-Otero, Natalia; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2013-01-01

    Highlights: ► Fractionation methods for assessing metals bound to marine DOM were developed. ► SEC and AEC with UV detection and hyphenated with inductively coupled plasma-mass spectrometry were used. ► SEC-UV showed marine DOM of molecular weights from 16 to 1 kDa. ► Cobalt, manganese, strontium and zinc are bound to marine DOM. - Abstract: Size exclusion chromatography (SEC) followed by anion exchange chromatography (AEC) hyphenated with inductively coupled plasma-mass spectrometry (ICP-MS) was applied for fractionating metals bound to marine dissolved organic matter (DOM). Surface seawater samples (100 L) were subjected to tangential flow ultrafiltration (10,000 Da cut off) for isolating and pre-concentrating dissolved large molecules. The isolated fraction (retentate) consisted of 1 L, which was further freeze-dried and re-dissolved to 250 mL with ultrapure water. After HI Trap desalting of the re-dissolved retentate, SEC with UV detection showed marine DOM ranging from 6.5 kDa (lower than the permeable volume of the SEC column) to 16 kDa. A further characterization of this fraction by AEC with UV detection revealed the existence of four groups of macromolecules exhibiting retention times of 2.3, 2.8, 4.5 and 14.0 min. AEC hyphenated with ICP-MS showed the presence of strontium and zinc in the first AE fraction isolated from the SEC fraction; while manganese was found to be bound to the second AE fraction. Cobalt was found to be bound to molecules comprising the third AE fraction.

  19. Impact of Detoxification Techniques on Pulmonary Gas Exchange Function in Patients with Generalized Peritonitis

    Directory of Open Access Journals (Sweden)

    R. A. Mlinnik

    2012-01-01

    Full Text Available Objective: to analyze the impact of different detoxification techniques on pulmonary gas exchange function in patients with generalized peritonitis complicated by multiple organ failure. Subjects and methods. One hundred and thirty patients with generalized peritonitis were examined. According to the used detoxification techniques, the patients were divided into 5 groups. All the patients underwent a comprehensive examination, the key element of which was the evaluation of gas exchange parameters. Results. Membrane plasmapheresis and plasmapheresis with sodium hypochlorite infusion to the plasma filter in patients with peritonitis are shown to improve pulmonary blood oxygenation.

  20. Simplified production and concentration of HIV-1-based lentiviral vectors using HYPERFlask vessels and anion exchange membrane chromatography

    Science.gov (United States)

    Kutner, Robert H; Puthli, Sharon; Marino, Michael P; Reiser, Jakob

    2009-01-01

    Background During the past twelve years, lentiviral (LV) vectors have emerged as valuable tools for transgene delivery because of their ability to transduce nondividing cells and their capacity to sustain long-term transgene expression in target cells in vitro and in vivo. However, despite significant progress, the production and concentration of high-titer, high-quality LV vector stocks is still cumbersome and costly. Methods Here we present a simplified protocol for LV vector production on a laboratory scale using HYPERFlask vessels. HYPERFlask vessels are high-yield, high-performance flasks that utilize a multilayered gas permeable growth surface for efficient gas exchange, allowing convenient production of high-titer LV vectors. For subsequent concentration of LV vector stocks produced in this way, we describe a facile protocol involving Mustang Q anion exchange membrane chromatography. Results Our results show that unconcentrated LV vector stocks with titers in excess of 108 transduction units (TU) per ml were obtained using HYPERFlasks and that these titers were higher than those produced in parallel using regular 150-cm2 tissue culture dishes. We also show that up to 500 ml of an unconcentrated LV vector stock prepared using a HYPERFlask vessel could be concentrated using a single Mustang Q Acrodisc with a membrane volume of 0.18 ml. Up to 5.3 × 1010 TU were recovered from a single HYPERFlask vessel. Conclusion The protocol described here is easy to implement and should facilitate high-titer LV vector production for preclinical studies in animal models without the need for multiple tissue culture dishes and ultracentrifugation-based concentration protocols. PMID:19220915

  1. Strong cation exchange-type chiral stationary phase for enantioseparation of chiral amines in subcritical fluid chromatography.

    Science.gov (United States)

    Wolrab, Denise; Kohout, Michal; Boras, Mario; Lindner, Wolfgang

    2013-05-10

    A new strong cation exchange type chiral stationary phase (SCX CSP) based on a syringic acid amide derivative of trans-(R, R)-2-aminocyclohexanesulfonic acid was applied to subcritical fluid chromatography (SFC) for separation of various chiral basic drugs and their analogues. Mobile phase systems consisting of aliphatic alcohols as polar modifiers and a broad range of amines with different substitution patterns and lipophilicity were employed to evaluate the impact on the SFC retention and selectivity characteristics. The observed results point to the existence of carbonic and carbamic acid salts formed as a consequence of reactions occurring between carbon dioxide, the alcoholic modifiers and the amine species present in the sub/supercritical fluid medium, respectively. Evidence is provided that these species are essential for affecting ion exchange between the strongly acidic chiral selector units and the basic analytes, following the well-established stoichiometric displacement mechanisms. Specific trends were observed when different types of amines were used as basic additives. While ammonia gave rise to the formation of the most strongly eluting carbonic and carbamic salt species, simple tertiary amines consistently provided superior levels of enantioselectivity. Furthermore, trends in the chiral SFC separation characteristics were investigated by the systematic variation of the modifier content and temperature. Different effects of additives are interpreted in terms of changes in the relative concentration of the transient ionic species contributing to analyte elution, with ammonia-derived carbamic salts being depleted at elevated temperatures by decomposition. Additionally, in an effort to optimize SFC enantiomer separation conditions for selected analytes, the impact of the type of the organic modifier, temperature, flow rate and active back pressure were also investigated. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Impact of airway gas exchange on the multiple inert gas elimination technique: theory.

    Science.gov (United States)

    Anderson, Joseph C; Hlastala, Michael P

    2010-03-01

    The multiple inert gas elimination technique (MIGET) provides a method for estimating alveolar gas exchange efficiency. Six soluble inert gases are infused into a peripheral vein. Measurements of these gases in breath, arterial blood, and venous blood are interpreted using a mathematical model of alveolar gas exchange (MIGET model) that neglects airway gas exchange. A mathematical model describing airway and alveolar gas exchange predicts that two of these gases, ether and acetone, exchange primarily within the airways. To determine the effect of airway gas exchange on the MIGET, we selected two additional gases, toluene and m-dichlorobenzene, that have the same blood solubility as ether and acetone and minimize airway gas exchange via their low water solubility. The airway-alveolar gas exchange model simulated the exchange of toluene, m-dichlorobenzene, and the six MIGET gases under multiple conditions of alveolar ventilation-to-perfusion, VA/Q, heterogeneity. We increased the importance of airway gas exchange by changing bronchial blood flow, Qbr. From these simulations, we calculated the excretion and retention of the eight inert gases and divided the results into two groups: (1) the standard MIGET gases which included acetone and ether and (2) the modified MIGET gases which included toluene and m-dichlorobenzene. The MIGET mathematical model predicted distributions of ventilation and perfusion for each grouping of gases and multiple perturbations of VA/Q and Qbr. Using the modified MIGET gases, MIGET predicted a smaller dead space fraction, greater mean VA, greater log(SDVA), and more closely matched the imposed VA distribution than that using the standard MIGET gases. Perfusion distributions were relatively unaffected.

  3. Measurement of denitrification on grassland using gas chromatography and 15N tracer technique

    International Nuclear Information System (INIS)

    Lippold, H.; Foerster, I.; Hagemann, O.; Matzel, W.

    1981-01-01

    Alternative covering of grassland micro-plots fertilized with 15 NH 4 15 NO 3 allowed on the basis on N 2 and N 2 O quantities released within several weeks to measure denitrification and to calculate it by means of methane as gas tracer. Thus the gas exchange was rendered visible and the N quantities measured could be corrected. In some variants, the acetylene blocking technique was successfully applied by adding acetylene to the soil air. The losses measured at 6 dates are discussed together with the 15 N balance and atmospherical conditions. The method is suited for recording the high losses occurring mainly in the second quarter of the year immediately after fertilization. Under the conditions mentioned soil N losses were small (3 kg N/ha). The immobilized fertilizer N quantities reached 20 to 30 kg/ha (fertilizer rate 100 kg N/ha) and were comparably independent of the date of fertilization. (author)

  4. Quantification of genetically modified soya using strong anion exchange chromatography and time-of-flight mass spectrometry.

    Science.gov (United States)

    Chang, Po-Chih; Reddy, P Muralidhar; Ho, Yen-Peng

    2014-09-01

    Stable-isotope dimethyl labeling was applied to the quantification of genetically modified (GM) soya. The herbicide-resistant gene-related protein 5-enolpyruvylshikimate-3-phosphate synthase (CP4 EPSPS) was labeled using a dimethyl labeling reagent, formaldehyde-H2 or -D2. The identification and quantification of CP4 EPSPS was performed using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). The CP4 EPSPS protein was separated from high abundance proteins using strong anion exchange chromatography and sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Then, the tryptic peptides from the samples and reference were labeled with formaldehyde-H2 and formaldehyde-D2, respectively. The two labeled pools were mixed and analyzed using MALDI-MS. The data showed a good correlation between the peak ratio of the H- and D-labeled peptides and the GM soya percentages at 0.5, 1, 3, and 5 %, with R (2) of 0.99. The labeling reagents are readily available. The labeling experiments and the detection procedures are simple. The approach is useful for the quantification of GM soya at a level as low as 0.5 %.

  5. Simplified in vitro refolding and purification of recombinant human granulocyte colony stimulating factor using protein folding cation exchange chromatography.

    Science.gov (United States)

    Vemula, Sandeep; Dedaniya, Akshay; Thunuguntla, Rahul; Mallu, Maheswara Reddy; Parupudi, Pavani; Ronda, Srinivasa Reddy

    2015-01-30

    Protein folding-strong cation exchange chromatography (PF-SCX) has been employed for efficient refolding with simultaneous purification of recombinant human granulocyte colony stimulating factor (rhG-CSF). To acquire a soluble form of renatured and purified rhG-CSF, various chromatographic conditions, including the mobile phase composition and pH was evaluated. Additionally, the effects of additives such as urea, amino acids, polyols, sugars, oxidizing agents and their amalgamations were also investigated. Under the optimal conditions, rhG-CSF was efficaciously solubilized, refolded and simultaneously purified by SCX in a single step. The experimental results using ribose (2.0M) and arginine (0.6M) combination were found to be satisfactory with mass yield, purity and specific activity of 71%, ≥99% and 2.6×10(8)IU/mg respectively. Through this investigation, we concluded that the SCX refolding method was more efficient than conventional methods which has immense potential for the large-scale production of purified rhG-CSF. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Method for the direct determination of available carbohydrates in low-carbohydrate products using high-performance anion exchange chromatography.

    Science.gov (United States)

    Ellingson, David; Potts, Brian; Anderson, Phillip; Burkhardt, Greg; Ellefson, Wayne; Sullivan, Darryl; Jacobs, Wesley; Ragan, Robert

    2010-01-01

    An improved method for direct determination of available carbohydrates in low-level products has been developed and validated for a low-carbohydrate soy infant formula. The method involves modification of an existing direct determination method to improve specificity, accuracy, detection levels, and run times through a more extensive enzymatic digestion to capture all available (or potentially available) carbohydrates. The digestion hydrolyzes all common sugars, starch, and starch derivatives down to their monosaccharide components, glucose, fructose, and galactose, which are then quantitated by high-performance anion-exchange chromatography with photodiode array detection. Method validation consisted of specificity testing and 10 days of analyzing various spike levels of mixed sugars, maltodextrin, and corn starch. The overall RSD was 4.0% across all sample types, which contained within-day and day-to-day components of 3.6 and 3.4%, respectively. Overall average recovery was 99.4% (n = 10). Average recovery for individual spiked samples ranged from 94.1 to 106% (n = 10). It is expected that the method could be applied to a variety of low-carbohydrate foods and beverages.

  7. Process optimisation for anion exchange monolithic chromatography of 4.2kbp plasmid vaccine (pcDNA3F).

    Science.gov (United States)

    Ongkudon, Clarence M; Danquah, Michael K

    2010-10-15

    Anion exchange monolithic chromatography is increasingly becoming a prominent tool for plasmid DNA purification but no generic protocol is available to purify all types of plasmid DNA. In this work, we established a simple framework and used it to specifically purify a plasmid DNA model from a clarified alkaline-lysed plasmid-containing cell lysate. The framework involved optimising ligand functionalisation temperature (30-80°C), mobile phase flow rate (0.1-1.8mL/min), monolith pore size (done by changing the porogen content in the polymerisation reaction by 50-80%), buffer pH (6-10), ionic strength of binding buffer (0.3-0.7M) and buffer gradient elution slope (1-10% buffer B/min). We concluded that preferential pcDNA3F adsorption and optimum resolution could be achieved within the tested conditions by loading the clarified cell lysate into 400nm pore size of monolith in 0.7M NaCl (pH 6) of binding buffer followed by increasing the NaCl concentration to 1.0M at 3%B/min. Copyright © 2010 Elsevier B.V. All rights reserved.

  8. Application of the Guided Wave Technique to the Heat Exchanger Tube in NPP

    International Nuclear Information System (INIS)

    Yang, Dong Soon; Kim, Hyung Nam; Yoo, Hyun Joo

    2005-01-01

    The heat exchanger tube is examined by the method of eddy current test(ECT) to identify the integrity of the nuclear power plant. Because ECT probe is moved through the tube inside to identify flaws, the ECT probe should be exchanged periodically due to the wear of probe surface in order to remove the noise form the ECT signal. Moreover, it is impossible to examine the tube by ECT method because the ECT probe can not move through the inside due to the deformation such as dent. Recently, the theory of guided wave was established and the equipment applying the theory has been actively developed so as to overcome the limitation of ECT method for the tube inspection of heater exchanger in nuclear power plant. The object of this study is to know the application of the guided wave technique to heat exchanger tube in NPP

  9. Comparison of derivatization/ionization techniques for liquid chromatography tandem mass spectrometry analysis of oxylipins.

    Science.gov (United States)

    Meckelmann, Sven W; Hellhake, Stefan; Steuck, Maryvonne; Krohn, Michael; Schebb, Nils Helge

    2017-05-01

    The performance of two derivatization and ionization techniques for the quantitative reversed phase liquid chromatography (LC)- mass spectrometry (MS) analysis of hydroxy fatty acids (OH-PUFA) in plasma was evaluated: One used AMPP (N-(4-aminomethylphenyl)pyridinium chloride) leading to a positive charged amid-derivate which can be detected by electrospray ionization (ESI)-MS. Second yielded penta fluorobenzyl bromide (PFB) ester derivates allowing detection in electron capture atmospheric pressure chemical ionization (ecAPCI)-MS. The sensitivity of detection of a comprehensive set of hydroxy fatty acids of n6- and n3- poly unsaturated fatty acids was investigated. On the SCIEX3200 MS the applied PFB derivatization led to poor limits of detection (LOD) of 10-100nM (0.1-1pmol/0.03-0.3ng on column). By contrast, AMPP derivatization led to a similar sensitivity compared to the standard ESI(-) of non derivatized analytes (LOD about 1nM (10fmol/3pg on column)). For several analytes, including 9-HETE, 11-HETE and 17-HDHA the AMPP derivatization improved sensitivity enabling their detection in human plasma. However, precision was reduced by AMPP derivatization and variation in IS recovery indicated a strong matrix influence on the MS-signal. In sum, with the instrumentation used, neither of these derivatization methods improves in our hands the LC-MS based quantification of oxylipins. Copyright © 2017 Elsevier Inc. All rights reserved.

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

    Science.gov (United States)

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

    2011-09-23

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

  11. Cation-exchange high-performance liquid chromatography for variant hemoglobins and HbF/A2: What must hematopathologists know about methodology?

    OpenAIRE

    Sharma, Prashant; Das, Reena

    2016-01-01

    Cation-exchange high-performance liquid chromatography (CE-HPLC) is a widely used laboratory test to detect variant hemoglobins as well as quantify hemoglobins F and A2 for the diagnosis of thalassemia syndromes. It’s versatility, speed, reproducibility and convenience have made CE-HPLC the method of choice to initially screen for hemoglobin disorders. Despite its popularity, several methodological aspects of the technology remain obscure to pathologists and this may have consequences in spec...

  12. Preparation of a novel dual-function strong cation exchange/hydrophobic interaction chromatography stationary phase for protein separation.

    Science.gov (United States)

    Zhao, Kailou; Yang, Li; Wang, Xuejiao; Bai, Quan; Yang, Fan; Wang, Fei

    2012-08-30

    We have explored a novel dual-function stationary phase which combines both strong cation exchange (SCX) and hydrophobic interaction chromatography (HIC) characteristics. The novel dual-function stationary phase is based on porous and spherical silica gel functionalized with ligand containing sulfonic and benzyl groups capable of electrostatic and hydrophobic interaction functionalities, which displays HIC character in a high salt concentration, and IEC character in a low salt concentration in mobile phase employed. As a result, it can be employed to separate proteins with SCX and HIC modes, respectively. The resolution and selectivity of the dual-function stationary phase were evaluated under both HIC and SCX modes with standard proteins and can be comparable to that of conventional IEC and HIC columns. More than 96% of mass and bioactivity recoveries of proteins can be achieved in both HIC and SCX modes, respectively. The results indicated that the novel dual-function column could replace two individual SCX and HIC columns for protein separation. Mixed retention mechanism of proteins on this dual-function column based on stoichiometric displacement theory (SDT) in LC was investigated to find the optimal balance of the magnitude of electrostatic and hydrophobic interactions between protein and the ligand on the silica surface in order to obtain high resolution and selectivity for protein separation. In addition, the effects of the hydrophobicity of the ligand of the dual-function packings and pH of the mobile phase used on protein separation were also investigated in detail. The results show that the ligand with suitable hydrophobicity to match the electrostatic interaction is very important to prepare the dual-function stationary phase, and a better resolution and selectivity can be obtained at pH 6.5 in SCX mode. Therefore, the dual-function column can replace two individual SCX and HIC columns for protein separation and be used to set up two-dimensional liquid

  13. Anion exchange chromatography of 99mTc(Sn)-EHDP complexes: determination of the charge of the components and influence of pH and ligand concentration

    International Nuclear Information System (INIS)

    Huigen, Y.M.; Diender, M.; Gelsema, W.J.; De Ligny, C.L.

    1991-01-01

    The components of a 99m Tc(Sn)-EHDP complex mixture were separated by means of normal pressure and high-pressure anion exchange chromatography. Precautions were taken to prevent the dissociation of the complexes during chromatography. The charges of the components were determined according to the methods of Wilson and Pinkerton (1985) and Russell and Bischoff (1985). The values of the charges obtained with the two methods are not in agreement. Russell and Bischoff's method, in which a reference ion is used, must be preferred. However, even with this method the accuracy of the data obtained is probably limited, due to the difficulty of making corrections for activity coefficients of highly-charge ions at the rather high electrolyte concentrations that must be used in the ion exchange method. So, we think that it is only warranted to conclude that the mean charge of the components of 99m Tc(Sn)-EHDP is about -6 at pH 7, and that the charges of the individual components are in the range of -4 to -9. The influence of pH and ligand concentration in the reaction mixture was determined with high pressure anion exchange chromatography. It was found that a decrease in the pH of the reaction mixture favours the production of complexes with a long retention time, which leads to a slightly higher mean charge. The ligand concentration of the reaction mixture scarcely influenced the relative concentrations of the components. (author)

  14. The Binding of Biotin to Sepharose-Avidin Column: Demonstration of the Affinity Chromatography Technique

    Science.gov (United States)

    Landman, A. D.; Landman, N. N.

    1976-01-01

    Describes a biochemistry experiment that illustrates the methodology of affinity chromatography by attaching avidin, a glycoprotein in egg white, to a Sepharose matrix in order to bind biotin-containing proteins. (MLH)

  15. Composition of atmospheric precipitation. I. Sampling technique. Use of ion exchange resins

    Energy Technology Data Exchange (ETDEWEB)

    Egner, H; Eriksson, E; Emanuelsson, A

    1947-01-01

    In order to investigate the composition of atmospheric precipitations in Sweden, a technique using ion exchange resins has been developed. The possibilities of nitrate reduction, and ammonia losses, when the precipitation is collected in zinc gauges is stressed. Glass funnels are used, and they are effectively protected from bird droppings. The ion exchange resins so far available are quite serviceable but show some deficiencies as to stability, and activity in alkaline solutions. New resins, which are not yet available, seem to offer definite advantages.

  16. Chemometric profile of root extracts of Rhodiola imbricata Edgew. with hyphenated gas chromatography mass spectrometric technique.

    Directory of Open Access Journals (Sweden)

    Amol B Tayade

    Full Text Available Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo, belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S; 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl; α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful

  17. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    International Nuclear Information System (INIS)

    Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega

    2007-01-01

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  18. Reducing elution in anion exchange chromatography as a pretreatment of colorimetry of chromium(VI) and vanadium(V)

    International Nuclear Information System (INIS)

    Shigetomi, Yasumasa; Hatamoto, Takeji; Nagoshi, Kimie; Yamashige, Takashi.

    1976-01-01

    In order to increase the selectivity of the colorimetry of chromium and vanadium, the separation by means of anion exchange chromatography was tested. The column, phi 0.8x5.0 cm packing (50--100 mesh) Dowex 1x4 anion exchange resin was used for the separation of chromium. The solution containing chromium (VI), zinc(II), cadmium(II), iron(III) and reducing organic substances contained in industrial waste water was introduced into the column and then the substances other than chromium(VI) were removed by washing the column with distilled water. Finally chromium(VI) was reduced to chromium(III) by hydroxylamine in the eluent and eluted. The concentration of sulfuric acid and hydroxylamine in the eluent were 0.1 mol/l and 0.001 mol/l respectively. For analyzing chromium(III) in the mixture of chromium(VI) and chromium(III), after removal of chromium(VI) it should be oxidized to chromium(VI) anion with the oxidant, e.g., sodium peroxide or hydrogen peroxide, before introducing it into the column. In terms of the pretreatment by using the acetate form resin column, chromium (VI) and chromium(III) can be determined separately in the solution whose concentration ranges from 0.05 ppm to 0.5 ppm despite the presence of contaminants, which interfere with the colorimetric determination of chromium(VI) using diphenylcarbonohydrazide, in the original solution. The separation of vanadium(V) in the solution containing copper(II), cobalt(II) and etc. was made using the mixed solution of hydrochloric acid (2 mol/l) and hydroxylamine (0.2 mol/l) similarly to chromium(VI). In terms of the similar pretreatment vanadium could be determined precisely as far as 0.1 ppm by the colorimetry using 4-(2-pyridylazo) resorcinol despite the presence of copper(II), cobalt(II), nickel(II) and etc in the original solution. (auth.)

  19. 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.

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

    Science.gov (United States)

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

    2007-09-01

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

  1. Application of ion exchange and extraction chromatography to the separation of actinium from proton-irradiated thorium metal for analytical purposes.

    Science.gov (United States)

    Radchenko, V; Engle, J W; Wilson, J J; Maassen, J R; Nortier, F M; Taylor, W A; Birnbaum, E R; Hudston, L A; John, K D; Fassbender, M E

    2015-02-06

    Actinium-225 (t1/2=9.92d) is an α-emitting radionuclide with nuclear properties well-suited for use in targeted alpha therapy (TAT), a powerful treatment method for malignant tumors. Actinium-225 can also be utilized as a generator for (213)Bi (t1/2 45.6 min), which is another valuable candidate for TAT. Actinium-225 can be produced via proton irradiation of thorium metal; however, long-lived (227)Ac (t1/2=21.8a, 99% β(-), 1% α) is co-produced during this process and will impact the quality of the final product. Thus, accurate assays are needed to determine the (225)Ac/(227)Ac ratio, which is dependent on beam energy, irradiation time and target design. Accurate actinium assays, in turn, require efficient separation of actinium isotopes from both the Th matrix and highly radioactive activation by-products, especially radiolanthanides formed from proton-induced fission. In this study, we introduce a novel, selective chromatographic technique for the recovery and purification of actinium isotopes from irradiated Th matrices. A two-step sequence of cation exchange and extraction chromatography was implemented. Radiolanthanides were quantitatively removed from Ac, and no non-Ac radionuclidic impurities were detected in the final Ac fraction. An (225)Ac spike added prior to separation was recovered at ≥ 98%, and Ac decontamination from Th was found to be ≥ 10(6). The purified actinium fraction allowed for highly accurate (227)Ac determination at analytical scales, i.e., at (227)Ac activities of 1-100 kBq (27 nCi to 2.7 μCi). Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Analysis of [U-13C6]glucose in human plasma using liquid chromatography/isotope ratio mass spectrometry compared with two other mass spectrometry techniques

    NARCIS (Netherlands)

    Schierbeek, H.; Moerdijk-Poortvliet, T.C.W.; van den Akker, C.H.P.; te Braake, F.W.J.; Boschker, H.T.S.; van Goudoever, J.B.

    2009-01-01

    The use of stable isotope labelled glucose provides insight into glucose metabolism. The 13C-isotopic enrichment of glucose is usually measured by gas chromatography/mass spectrometry (GC/MS) or gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). However, in both techniques

  3. Heat Exchanger Tube Inspection of Nuclear Power Plants using IRIS Technique

    International Nuclear Information System (INIS)

    Yoon, Byung Sik; Yang, Seung Han; Song, Seok Yoon; Kim, Yong Sik; Lee, Hee Jong

    2005-01-01

    Inspection of heat exchange tubing include steam generator of nuclear power plant mostly performed with eddy current method. Recently, various inspection technique is available such as remote field eddy current, flux leakage and ultrasonic methods. Each of these techniques has its merits and limitations. Electromagnetic techniques are very useful to locate areas of concern but sizing is hard because of the difficult interpretation of an electric signature. On the other hand, ultrasonic methods are very accurate in measuring wall loss damage, and are reliable for detecting cracks. Additionally ultrasound methods is not affected by support plates or tube sheets and variation of electrical conductivity or permeability. Ultrasound data is also easier to analyze since the data displayed is generally the remaining wall thickness. It should be emphasized that ultrasound is an important tool for sizing defects in tubing. In addition, it can be used in situations where eddy current or remote field eddy current is not reliable, or as a flaw assessment tool to supplement the electromagnetic data. The need to develop specialized ultrasonic tools for tubing inspection was necessary considering the limitations of electromagnetic techniques to some common inspection problems. These problems the sizing of wall loss in carbon steel tubes near the tube sheet or support plate, sizing internal erosion damage, and crack detection. This paper will present an IRIS(Internal Rotating Inspection System) ultrasonic tube inspection technique for heat exchanger tubing in nuclear power plant and verify inspection reliability for artificial flaw embedded to condenser tube

  4. Use of the neutron diffraction - H/D exchange technique to determine the conformational dynamics of trypsin

    International Nuclear Information System (INIS)

    Kossiakoff, A.A.

    1982-01-01

    Reported here are studies analyzing the extent and nature of the inherent conformational fluctuations in trypsin by neutron diffraction - hydrogen exchange techniques. The pattern of exchange investigates systematic relationships between exchangeable sites and the structural and chemical properties of the molecule. Our findings that pH 7, 20 0 and 1 year of soaking all sites of trypsin are fully exchanged except those which are especially well protected by the structure. Essentially all the sites in which the peptide hydrogens are bonded directly to water molecules - either in the bulk solvent regions or in interior clusters - are fully exchanged. 41 references, 10 figures

  5. Alternative sample-introduction technique to avoid breakthrough in gradient-elution liquid chromatography of polymers

    NARCIS (Netherlands)

    Reingruber, E.; Bedani, F.; Buchberger, W.; Schoenmakers, P.

    2010-01-01

    Gradient-elution liquid chromatography (GELC) is a powerful tool for the characterization of synthetic polymers. However, gradient-elution chromatograms often suffer from breakthrough phenomena. Breakthrough can be averted by using a sample solvent as weak as the mobile phase. However, this approach

  6. Column liquid chromatography- mass spectrometry: selected techniques in environmental applications for polar pesticides and related compounds.

    NARCIS (Netherlands)

    Slobodnik, J.; van Baar, B.L.M.; Brinkman, U.A.T.

    1995-01-01

    A review covering the field of environmental applications of liquid chromatography-mass spectrometry (LC-MS) is presented. Recent developments and advances are discussed with emphasis on the presently popular thermospray, particle beam and atmospheric pressure ionisation interfaces. Each interface

  7. Chlorococcalean microalgae Ankistrodesmus convolutes biodiesel characterization with Fourier transform-infrared spectroscopy and gas chromatography mass spectroscopy techniques

    Directory of Open Access Journals (Sweden)

    Swati SONAWANE

    2015-12-01

    Full Text Available The Chlorococcalean microalgae Ankistrodesmus convolutes was found in fresh water Godawari reservoir, Ahmednagar district of Maharashtra State, India. Microalgae are modern biomass for the production of liquid biofuel due to its high solar cultivation efficiency. The collection, harvesting and drying processes were play vital role in converting algal biomass into energy liquid fuel. The oil extraction was the important step for the biodiesel synthesis. The fatty acid methyl ester (FAME synthesis was carried through base catalyzed transesterification method. The product was analyzed by using the hyphened techniques like Fourier Transform-Infrared spectroscopy (FT-IR and Gas Chromatography Mass Spectroscopy (GCMS. FT-IR Spectroscopy was results the ester as functional group of obtained product while the Gas Chromatography Mass Spectroscopy was results the six type of fatty acid methyl ester with different concentration. Ankistrodesmus convolutes biodiesel consist of 46.5% saturated and 49.14% unsaturated FAME.

  8. Development of isotope dilution-liquid chromatography/mass spectrometry combined with standard addition techniques for the accurate determination of tocopherols in infant formula

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Joonhee; Jang, Eun-Sil; Kim, Byungjoo, E-mail: byungjoo@kriss.re.kr

    2013-07-17

    Graphical abstract: -- Highlights: •ID-LC/MS method showed biased results for tocopherols analysis in infant formula. •H/D exchange of deuterated tocopherols in sample preparation was the source of bias. •Standard addition (SA)-ID-LC/MS was developed as an alternative to ID-LC/MS. •Details of calculation and uncertainty evaluation of the SA-IDMS were described. •SA-ID-LC/MS showed a higher-order metrological quality as a reference method. -- Abstract: During the development of isotope dilution-liquid chromatography/mass spectrometry (ID-LC/MS) for tocopherol analysis in infant formula, biased measurement results were observed when deuterium-labeled tocopherols were used as internal standards. It turned out that the biases came from intermolecular H/D exchange and intramolecular H/D scrambling of internal standards in sample preparation processes. Degrees of H/D exchange and scrambling showed considerable dependence on sample matrix. Standard addition-isotope dilution mass spectrometry (SA-IDMS) based on LC/MS was developed in this study to overcome the shortcomings of using deuterium-labeled internal standards while the inherent advantage of isotope dilution techniques is utilized for the accurate recovery correction in sample preparation processes. Details of experimental scheme, calculation equation, and uncertainty evaluation scheme are described in this article. The proposed SA-IDMS method was applied to several infant formula samples to test its validity. The method was proven to have a higher-order metrological quality with providing very accurate and precise measurement results.

  9. Meningococcal X polysaccharide quantification by high-performance anion-exchange chromatography using synthetic N-acetylglucosamine-4-phosphate as standard.

    Science.gov (United States)

    Micoli, F; Adamo, R; Proietti, D; Gavini, M; Romano, M R; MacLennan, C A; Costantino, P; Berti, F

    2013-11-15

    A method for meningococcal X (MenX) polysaccharide quantification by high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD) is described. The polysaccharide is hydrolyzed by strong acidic treatment, and the peak of glucosamine-4-phosphate (4P-GlcN) is detected and measured after chromatography. In the selected conditions of hydrolysis, 4P-GlcN is the prevalent species formed, with GlcN detected for less than 5% in moles. As standard for the analysis, the monomeric unit of MenX polysaccharide, N-acetylglucosamine-4-phosphate (4P-GlcNAc), was used. This method for MenX quantification is highly selective and sensitive, and it constitutes an important analytical tool for the development of a conjugate vaccine against MenX. Copyright © 2013 Elsevier Inc. All rights reserved.

  10. Review of disposal techniques for radioactively contaminated organic ion-exchange resins

    International Nuclear Information System (INIS)

    Inman, J.R.; Mack, J.

    1993-03-01

    Organic ion-exchange resins are used in the UK nuclear industry to remove radioactive nuclides from dilute aqueous solution. Resins represent a significant proportion of the organic content of ILW and LLW, particularly ILW. Spent resins are destined to be disposed of in the UK deep repository. There are concerns regarding the potential effects of organic materials on long-term repository performance, and these effects have been the subject of much recent research work. The object of this study has been to conduct a worldwide review of treatment and conditioning techniques available for spent organic ion-exchange resins with the intention of recommending the best option for dealing with the waste in the UK. Data on available techniques have been gathered together, and are presented in tabular form at the back of the report. The techniques have been reviewed and compared considering safety, practicality and cost, and a best option selected on the basis of current knowledge. On balance it would appear that wet oxidation using hydrogen peroxide with residue encapsulation in BFS/OPC is the most appropriate technique, probably implemented using a mobile plant. This conclusion and recommendation is not however clear cut and further advice regarding the acceptability of organic material in the repository is necessary before a definite recommendation can be made. (Author)

  11. Therapeutic drug monitoring of nevirapine in saliva in Uganda using high performance liquid chromatography and a low cost thin-layer chromatography technique.

    Science.gov (United States)

    Lamorde, Mohammed; Fillekes, Quirine; Sigaloff, Kim; Kityo, Cissy; Buzibye, Allan; Kayiwa, Joshua; Merry, Concepta; Nakatudde-Katumba, Lillian; Burger, David; de Wit, Tobias F Rinke

    2014-09-01

    In resource limited settings access to laboratory monitoring of HIV treatment is limited and therapeutic drug monitoring is generally unavailable. This study aimed to evaluate nevirapine concentrations in saliva using low-cost thin-layer chromatography (TLC) and nevirapine concentrations in plasma and saliva using high performance liquid chromatography (HPLC) methods; and to correlate nevirapine plasma concentrations to HIV treatment outcomes in Ugandan patients. Paired plasma and stimulated saliva samples were obtained from Ugandan, HIV-infected adults on nevirapine-based ART. Nevirapine concentrations were measured using a validated HPLC method and a novel TLC method. Plasma nevirapine concentrations HPLC were considered subtherapeutic. Negative/positive predictive values of different thresholds for subtherapeutic nevirapine concentrations in saliva were determined. Virologic testing and, if applicable, HIV drug resistance testing was performed. Median (interquartile range, IQR) age of 297 patients was 39.1 (32.8-45.2) years. Three hundred saliva and 287 plasma samples were available for analysis. Attempts failed to determine nevirapine saliva concentrations by TLC. Using HPLC, median (IQR) nevirapine concentrations in saliva and plasma were 3.40 (2.59-4.47) mg/L and 6.17 (4.79-7.96) mg/L, respectively. The mean (coefficient of variation,%) nevirapine saliva/plasma ratio was 0.58 (62%). A cut-off value of 1.60 mg/L nevirapine in saliva was associated with a negative/positive predictive value of 0.99/0.72 and a sensitivity/specificity of 87%/98% for predicting subtherapeutic nevirapine plasma concentrations, respectively. Only 5% (15/287) of patients had subtherapeutic nevirapine plasma concentrations, of which 3 patients had viral load results > 400 copies/mL. Patients with nevirapine concentrations in plasma 400 copies/mL). The low-cost TLC technique for monitoring nevirapine in saliva was unsuccessful but monitoring nevirapine saliva and plasma

  12. Qualitative and quantitative analysis of branches in dextran using high-performance anion exchange chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Yi, Lin; Ouyang, Yilan; Sun, Xue; Xu, Naiyu; Linhardt, Robert J; Zhang, Zhenqing

    2015-12-04

    Dextran, a family of natural polysaccharides, consists of an α (1→6) linked-glucose main (backbone) chain having a number of branches. The determination of the types and the quantities of branches in dextran is important in understanding its various biological roles. In this study, a hyphenated method using high-performance anion exchange chromatography (HPAEC) in parallel with pulsed amperometric detection (PAD) and mass spectrometry (MS) was applied to qualitative and quantitative analysis of dextran branches. A rotary cation-exchange cartridge array desalter was used for removal of salt from the HPAEC eluent making it MS compatible. MS and MS/MS were used to provide structural information on the enzymatically prepared dextran oligosaccharides. PAD provides quantitative data on the ratio of enzyme-resistant, branched dextran oligosaccharides. Both the types and degree of branching found in a variety of dextrans could be simultaneously determined online using this method. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Lithium isotope effects in cation exchange chromatography of lithium lactate in water-dimethyl sulfoxide and water-acetone mixed solvent media

    International Nuclear Information System (INIS)

    Oi, Takao; Kondoh, Akiko; Ohno, Etsuko; Hosoe, Morikazu

    1993-01-01

    Lithium isotope separation by ion exchange displacement chromatography of lithium lactate in water-dimethyl sulfoxide (DMSO) and water-acetone mixed solvent media at 25 C was explored. In both the water-DMSO and water-acetone system, the single stage isotope separation factor (S) was a convex function of the mixing ratio of the solvents in the external solution phase; S had its maximum value of 1.00254 at water: DMSO=25:75 v/v and 1.00182 at water: acetone=75:25 v/v. Strong correlations of S with solvent partitions between the solution and the exchanger phases were found in both systems, which was qualitatively explainable by considering the lithium isotope distributions between the two phases based on the fundamental lithium isotope effects and the relative affinities of water, DMSO and acetone towards the lithium ion. (orig.)

  14. Ultrafiltration technique in conjunction with competing ligand exchange method for Ni–humics speciation in aquatic environment

    Digital Repository Service at National Institute of Oceanography (India)

    Chakraborty, P.; Boissel, M.; Reuillon, A.; Babu, P.V.R.; Parthiban, G.

    The combination of ultrafiltration technique with competing ligand exchange method provides a better understanding of interactions between Ni and different molecular weight fractions of humic acid (HA) at varying pH in aquatic environment...

  15. 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

  16. 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).

  17. Validation of a technique by high-performance liquid chromatography for the determination of total isoflavones

    Directory of Open Access Journals (Sweden)

    Pilar A. Soledispa Cañarte

    2017-04-01

    Full Text Available Context: Isoflavones may act as selective regulators in the prevention of various diseases. The most important source of isoflavones is the soy, from which different phytotherapeutics are elaborated of use in Ecuadorian population. However, its concentration varies depending on several factors, therefore quality assessment need to be carried out through out several analytical methods. Aims: To validate an analytical method by high precision liquid chromatography (HPLC to quantify total isoflavones in herbal medicine. Methods: To quantify isoflavones, it was used a brand liquid chromatography with UV/VIS detector at 260 nm, C-18 column using isocratic method. The mobile phase was composed of 2% acetic acid: acetonitrile (75:25. The quantification was performed against reference standard. The parameters for the validation followed the established in the USP 33. Results: The chromatogram presented six peaks with elution between 1.557 and 18.913 min. The linearity of the system and the method got r2 equal to 0.98 and 0.99 respectively. The coefficients of variation 1.5% in the study of repetitiveness and 2% in intermediate precision. The accuracy of the adjusted lineal model exhibited r=0.95 and intercept reliable interval (-0.921; 1.743. Conclusions: The validated method was specific, accurate, precise and linear. It can be used for quality control and stability studies of isoflavones present in herbal medicine.

  18. Cromatografia unificada Unified chromatography

    Directory of Open Access Journals (Sweden)

    Carin von Mühlen

    2004-10-01

    Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

  19. Separation of individual lanthanides through the combined techniques of urea fractionated homogeneous precipitation and ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Umeda, K; Abrao, A

    1975-06-01

    The separation of individual lanthanides, especially Ce, Nd, Pr, Sm and La, from a rare earth chlorides concentrate by the industrial processing of monazite sand is made. To reach this goal the homogeneous fractional precipitation and ion exchange techniques were combined. Using the rare earths concentrate depleted in Cerium, fractions enriched in Nd, Pr and Sm, and one final filtrate enriched in La were obtained, by the hydrolysis of urea. The separation of individual lanthanides (Nd, Pr, Sm and La) was accomplished using two strong cationic ion exchanger columns, the second with Cu(II) as retaining ion, and EDTA-NH/sub 4/ solution buffered with acetic acid as eluant. The annoying problem of precipitation into the column during the RE elution was solved. The difficult EDTA and Cu(II) recovery was the precipitation of Cu/sub 2/S and disruption of Cu-EDTA complex by hydrolysis of thiourea. The combination of both techniques allowed the preparation of individual lanthanides as Nd, Pr and La with 99% and Sm with 90% purity.

  20. Separation of individual lanthanides through the combined techniques of urea fractionated homogeneous precipitation and ion exchange

    International Nuclear Information System (INIS)

    Umeda, K.; Abrao, A.

    1975-01-01

    The separation of individual lanthanides, especially Ce, Nd, Pr, Sm and La, from a rare earth chlorides concentrate by the industrial processing of monazite sand is made. To reach this goal the homogeneous fractional precipitation and ion exchange techniques were combined. Using the rare earths concentrate depleted in Cerium, fractions enriched in Nd, Pr and Sm, and one final filtrate enriched in La were obtained, by the hydrolysis of urea. The separation of individual lanthanides (Ns, Pr, Sm and La) was accomplished using two strong cationic ion exchanger columns, the second with Cu(II) as retaining ion, and EDTA-NH 4 solution buffered with acetic acid as eluant. The annoy problem of precipitation into the column during the RE elution was solved. The difficult EDTA and Cu(II) recovery was the precipitation of Cu 2 S and disruption of CU-EDTA complex by hydrolysis of thiourea. The combination of both techniques allowed the preparation of individual lanthanides as Nd, Pr and La with 99% and Sm with 90% purity

  1. 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

  2. Oral to nasal tube exchange under fibroscopic view: a new technique for nasal intubation in a predicted difficult airway.

    Science.gov (United States)

    Monclus, Enric; Garcés, Antonio; Artés, David; Mabrock, Maged

    2008-07-01

    For a predicted difficult airway, oral intubation techniques are well established in pediatric anesthesia, but nasotracheal intubation remains a problem. There are many reports concerning this, but the risk of bleeding, added to the lack of cooperation make this procedure difficult and hazardous. We describe a modification of the nasal intubation technique in two stages. First an oral intubation and then exchanging the oral for a nasal tube, in the case of a 13-year-old boy affected by an advanced stage of cherubism. Oral intubation using a laryngeal mask technique has already been reported, but problems appear during the exchange procedure and even more when direct laryngoscopy is impossible. Fiberscopic control of the exchange, and the introduction of a Cook Exchange Catheter into the trachea through the oral tube before withdrawal, permits oxygenation of the patient and acts as a guide for oral tube reintroduction if required.

  3. The Application of Resonance-Enhanced Multiphoton Ionization Technique in Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Adan Li

    2014-01-01

    Full Text Available Gas chromatography resonance-enhanced multiphoton ionization time-of-flight mass spectrometry (GC/REMPI-TOFMS using a nanosecond laser has been applied to analyze the 16 polycyclic aromatic hydrocarbons (PAHs. The excited-state lifetime, absorption characters, and energy of electronic states of the 16 PAHs were investigated to optimize the ionization yield. A river water sample pretreated by means of solid phase extraction was analyzed to evaluate the performance of the analytical instrument. The results suggested that REMPI is superior to electron impact ionization method for soft ionization and suppresses the background signal due to aliphatic hydrocarbons. Thus, GC/REMPI-TOFMS is a more reliable method for the determination of PAHs present in the environment.

  4. Fuel spill identification by gas chromatography -- genetic algorithms/pattern recognition techniques

    International Nuclear Information System (INIS)

    Lavine, B.K.; Moores, A.J.; Faruque, A.

    1998-01-01

    Gas chromatography and pattern recognition methods were used to develop a potential method for typing jet fuels so a spill sample in the environment can be traced to its source. The test data consisted of 256 gas chromatograms of neat jet fuels. 31 fuels that have undergone weathering in a subsurface environment were correctly identified by type using discriminants developed from the gas chromatograms of the neat jet fuels. Coalescing poorly resolved peaks, which occurred during preprocessing, diminished the resolution and hence information content of the GC profiles. Nevertheless a genetic algorithm was able to extract enough information from these profiles to correctly classify the chromatograms of weathered fuels. This suggests that cheaper and simpler GC instruments ca be used to type jet fuels

  5. Discrimination of honeys using colorimetric sensor arrays, sensory analysis and gas chromatography techniques.

    Science.gov (United States)

    Tahir, Haroon Elrasheid; Xiaobo, Zou; Xiaowei, Huang; Jiyong, Shi; Mariod, Abdalbasit Adam

    2016-09-01

    Aroma profiles of six honey varieties of different botanical origins were investigated using colorimetric sensor array, gas chromatography-mass spectrometry (GC-MS) and descriptive sensory analysis. Fifty-eight aroma compounds were identified, including 2 norisoprenoids, 5 hydrocarbons, 4 terpenes, 6 phenols, 7 ketones, 9 acids, 12 aldehydes and 13 alcohols. Twenty abundant or active compounds were chosen as key compounds to characterize honey aroma. Discrimination of the honeys was subsequently implemented using multivariate analysis, including hierarchical clustering analysis (HCA) and principal component analysis (PCA). Honeys of the same botanical origin were grouped together in the PCA score plot and HCA dendrogram. SPME-GC/MS and colorimetric sensor array were able to discriminate the honeys effectively with the advantages of being rapid, simple and low-cost. Moreover, partial least squares regression (PLSR) was applied to indicate the relationship between sensory descriptors and aroma compounds. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Modeling and simulation of anion-exchange membrane chromatography for purification of Sf9 insect cell-derived virus-like particles.

    Science.gov (United States)

    Ladd Effio, Christopher; Hahn, Tobias; Seiler, Julia; Oelmeier, Stefan A; Asen, Iris; Silberer, Christine; Villain, Louis; Hubbuch, Jürgen

    2016-01-15

    Recombinant protein-based virus-like particles (VLPs) are steadily gaining in importance as innovative vaccines against cancer and infectious diseases. Multiple VLPs are currently evaluated in clinical phases requiring a straightforward and rational process design. To date, there is no generic platform process available for the purification of VLPs. In order to accelerate and simplify VLP downstream processing, there is a demand for novel development approaches, technologies, and purification tools. Membrane adsorbers have been identified as promising stationary phases for the processing of bionanoparticles due to their large pore sizes. In this work, we present the potential of two strategies for designing VLP processes following the basic tenet of 'quality by design': High-throughput experimentation and process modeling of an anion-exchange membrane capture step. Automated membrane screenings allowed the identification of optimal VLP binding conditions yielding a dynamic binding capacity of 5.7 mg/mL for human B19 parvovirus-like particles derived from Spodoptera frugiperda Sf9 insect cells. A mechanistic approach was implemented for radial ion-exchange membrane chromatography using the lumped-rate model and stoichiometric displacement model for the in silico optimization of a VLP capture step. For the first time, process modeling enabled the in silico design of a selective, robust and scalable process with minimal experimental effort for a complex VLP feedstock. The optimized anion-exchange membrane chromatography process resulted in a protein purity of 81.5%, a DNA clearance of 99.2%, and a VLP recovery of 59%. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. 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.

  8. 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....

  9. Performance evaluation of anion exchange resins Purolite NRW-5050 and Duolite A-611 by application of radioisotopic techniques

    International Nuclear Information System (INIS)

    Singare, P.U.

    2014-01-01

    Radioanalytical techniques using 131 I and 82 Br as tracer isotopes were applied to study the kinetics of iodide and bromide ion-isotopic exchange reactions taking place between the external labeled ionic solution and the resin surface. The results indicate low values of specific reaction rate (min -1 ), amount of ion exchanged (mmol) and initial rate of ion exchange (mmol/min) for bromide ion-isotopic exchange reaction as compared to that obtained for iodide ion-isotopic exchange reaction. It was observed that for iodide ion-isotopic exchange reaction performed at 35.0 C, 1 000 g of ion exchange resins and 0.002 mol/L labeled iodide ion solution, the values of specific reaction rate (min -1 ), amount of iodide ion exchanged (mmol), initial rate of iodide ion exchange (mmol/min) and log K d were 0.340, 0.394, 0.134 and 20.2 respectively for Purolite NRW-5050 resin, which was higher than the respective values of 0.216, 0.290, 0.063 and 18.2 as that obtained by using Duolite A-611. The results of present investigation indicate that during the two ion-isotopic exchange reactions, for both the resins, there exists a strong positive linear correlation between amount of ions exchanged and concentration of ionic solution; and strong negative correlation between amount of ions exchanged and temperature of exchanging medium. From the results it appears that as compared to Duolite A-611 resins, Purolite NRW-5050 resins shows superior performance under identical experimental conditions.

  10. Retrospective Study of Rapid-Exchange Monorail Versus Over-the-Wire Technique for Femoropopliteal Angioplasty

    International Nuclear Information System (INIS)

    Jahnke, Thomas; Schaefer, Jost Philipp; Bolte, Hendrik; Schaefer, Fritz; Michalek, Jens; Charalambous, Nicholas; Sapoval, Marc; Mueller-Huelsbeck, Stefan

    2008-01-01

    PurposeThe purpose of this study was to compare procedural outcome of rapid-exchange (RX) monorail versus conventional over-the-wire (OTW) technique for femoropopliteal angioplasty.Materials and MethodsDemographic data, procedure details, angioplasty success, and complications of 328 consecutive percutaneous transluminal angioplasties (PTAs) were collected from a prospective database and retrospectively analyzed. Procedure details included duration of fluoroscopy, area-dose product, amount of contrast agent, sheath sizes, access route, length of stenosis, presence of total occlusion, technical and anatomical success (residual stenosis <30% in the absence of complications), need for bail-out stenting, and periprocedural complications. The RX technique alone was used in 102 of 328 cases (31%); the OTW technique, in 226 of 328 of cases (68%).ResultsTechnical success was 98% for the RX versus 95.4% for the OTW technique (p = 0.2). A significantly greater number of stents had to be implanted due to angioplasty failure when the OTW technique was used (RX, 5.9%; OTW, 13.7%; p = 0.04). There were no significant differences in fluorocopy time, dose-area product, or amount of contrast medium used. The RX system facilitated the use of smaller sheath sizes (5 Fr = 38% and 6 Fr = 59% for RX versus 5 Fr = 16.8% and ≥6 Fr = 82.5% for OTW) but showed only a tendency toward lower overall complication rates (16.6% [17/102] in the RX group versus 19.9% [45/226] in the OTW group; p = 0.09). There was no effect on length of hospitalization. RX monorail systems were not associated with higher procedural costs when compared to conventional OTW technique.ConclusionWe conclude that RX monorail systems seem to enhance the technical success of femoropopliteal angioplasty. Although smaller sheath sizes can be used due to the lower profile of the RX systems, there is only a tendency toward lower complication rates.

  11. Ion-Exchange Sample Displacement Chromatography as a Method for Fast and Simple Isolation of Low- and High-Abundance Proteins from Complex Biological Mixtures

    Directory of Open Access Journals (Sweden)

    Martina Srajer Gajdosik

    2014-01-01

    Full Text Available Sample displacement chromatography (SDC in reversed phase and ion-exchange modes was introduced at the end of 1980s. This chromatographic method was first used for preparative purification of synthetic peptides, and subsequently adapted for protein fractionation, mainly in anion-exchange mode. In the past few years, SDC has been successfully used for enrichment of low- and medium-abundance proteins from complex biological fluids on both monolithic and bulk chromatographic supports. If aqueous mobile phase is used with the application of mild chromatographic conditions, isolated proteins are not denatured and can also keep their biological activity. In this paper, the use of SDC in anion-exchange mode on a high-capacity chromatographic resin for separation of proteins from complex biological mixtures such as human plasma is demonstrated. By use of three and more columns coupled in series during sample application, and subsequent parallel elution of detached columns, additional separation of bound proteins was achieved. Highly enriched human serum albumin fraction and a number of physiologically active medium- and low-abundance proteins could be fractionated and detected by electrospray ionization tandem mass spectrometry (ESI-MS/MS and matrix assisted laser desorption/ionization time-of-flight tandem mass spectrometry (MALDI-TOF/TOF-MS. The use of the aforementioned columns that can be sanitized with 1 M sodium hydroxide for further application of SDC in biotechnology and food technology was discussed.

  12. Expanded separation technique for chlorophyll metabolites in Oriental tobacco leaf using non aqueous reversed phase chromatography.

    Science.gov (United States)

    Ishida, Naoyuki

    2011-08-26

    An improved separation method for chlorophyll metabolites in Oriental tobacco leaf was developed. While Oriental leaf still gives the green color even after the curing process, little attention has been paid to the detailed composition of the remaining green pigments. This study aimed to identify the green pigments using non aqueous reversed phase chromatography (NARPC). To this end, liquid chromatograph (LC) equipped with a photo diode array detector (DAD) and an atmospheric pressure chemical ionization/mass spectrometer (APCI/MSD) was selected, because it is useful for detecting low polar non-volatile compounds giving green color such as pheophytin a. Identification was based on the wavelength spectrum, mass spectrum and retention time, comparing the analytes in Oriental leaf with the commercially available and synthesized components. Consequently, several chlorophyll metabolites such as hydroxypheophytin a, solanesyl pheophorbide a and solanesyl hydroxypheophorbide a were newly identified, in addition to typical green pigments such as chlorophyll a and pheophytin a. Chlorophyll metabolites bound to solanesol were considered the tobacco specific components. NARPC expanded the number of detectable low polar chlorophyll metabolites in Oriental tobacco leaf. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Gas exchange at the air-sea interface: a technique for radon measurements in seawater

    International Nuclear Information System (INIS)

    Queirazza, G.; Roveri, M.

    1991-01-01

    The rate of exchange of various gas species, such as O 2 , CO 2 etc. across the air-water interface can be evaluated from the 222 Rn vertical profiles in the water column. Radon profiles were measured in 4 stations in the NW Adriatic Sea, in September 1990, using solvent extraction and liquid scintillation counting techniques, directly on board the ship. The radiochemical procedure is described in detail. The lower limit of detection is approximately 0.4 mBq 1 -1 . The radon deficiency in the profiles gives estimates of the gas transfer rate across the air-sea interface ranging from 0.9 to 7.0 m d -1 . The suitability of the radon deficiency method in shallow water, enclosed seas is briefly discussed. (Author)

  14. Analysis and optimization of a proton exchange membrane fuel cell using modeling techniques

    International Nuclear Information System (INIS)

    Torre Valdés, Ing. Raciel de la; García Parra, MSc. Lázaro Roger; González Rodríguez, MSc. Daniel

    2015-01-01

    This paper proposes a three-dimensional, non-isothermal and steady-state model of Proton Exchange Membrane Fuel Cell using Computational Fluid Dynamic techniques, specifically ANSYS FLUENT 14.5. It's considered multicomponent diffusion and two-phasic flow. The model was compared with experimental published data and with another model. The operation parameters: reactants pressure and temperature, gases flow direction, gas diffusion layer and catalyst layer porosity, reactants humidification and oxygen concentration are analyzed. The model allows the fuel cell design optimization taking in consideration the channels dimensions, the channels length and the membrane thickness. Furthermore, fuel cell performance is analyzed working with SPEEK membrane, an alternative electrolyte to Nafion. In order to carry on membrane material study, it's necessary to modify the expression that describes the electrolyte ionic conductivity. It's found that the device performance has got a great sensibility to pressure, temperature, reactant humidification and oxygen concentration variations. (author)

  15. Comparative study on ion-isotopic exchange reaction kinetics by application of tracer technique

    International Nuclear Information System (INIS)

    Lokhande, R.S.; Singare, P.U.

    2007-01-01

    The radioactive isotopes 131 I and 82 Br were used to trace the ion-isotopic exchange reactions using industrial grade ion exchange resins Amberlite IRA-400. The experiments were performed to understand the effect of temperature and concentration of ionic solution on kinetics of exchange reactions. Both the exchange reactions were greatly influenced by rise in temperature, which result in higher percentage of ions exchanged. For bromide ion-isotopic exchange reactions, the calculated values of specific reaction rate/min -1 , and amount of ions exchanged/mmol were obtained higher than that for iodide ion-isotopic exchange reactions under identical experimental conditions. The observed variation in the results for two ion-isotopic exchange reactions was due to the difference in the ionic size of bromide and iodide ions. (orig.)

  16. Application of resin in pulp technique for ion exchange separation of uranium from alkaline leachate

    International Nuclear Information System (INIS)

    Sreenivas, T.; Rajan, K.; Chakravorty, J.

    2014-01-01

    The hydrometallurgical process for the recovery of uranium from different ores uses ion exchange (IX) technique for the separation of dissolved uranium values. Conventionally, the IX process is carried out on leach solution obtained after the filtration or counter-current decantation of the leach slurries. Amongst the two types of leach pulps generated in uranium ore processing, viz acidic and alkaline, the latter one consists of predominantly fine-size pulps of higher viscosity, thus making the solid-liquid separation an arduous task. Sustained research for improvising the efficiency of various unit operations in the uranium process flowsheet have resulted in advent of new generation resins which are mechanically re-silent, posses higher exchange capacity thereby enabling separation of dissolved uranium ions from the leach pulps directly. Some of the prominent low-grade uranium ore deposits in India are hosted in acid consuming gangue matrix. These ore deposits necessitate fine grinding as well as application of alkaline leaching for the dissolution of uranium values. The leach pulps analyse 500 – 600 mg/l of U3O8 and contain total dissolved solutes (TDS) to the extent of about 50 g/l. Analysis of the characteristics of the leach pulp indicated suitability of resin-in-pulp technique for the separation of uranyl carbonate anions from the leachate. This paper describes the results of the RIP test work on alkaline leach slurry using various commercially available strong base anionic exchange resins. Parametric variation studies were conducted to establish the adsorption isotherm and sorption kinetics followed by elution of loaded uranium. Based on these results semi-continuous experiments on “carousel” mode were carried out. The results indicate superiority of gel type polystyrene based resins grafted with quaternary ammonium ion in comparison to the macro-porous resins. Semi-continuous counter-current extraction and elution tests indicated that about 98% of

  17. Rapid fluorescence detection of pathogenic bacteria using magnetic enrichment technique combined with magnetophoretic chromatography.

    Science.gov (United States)

    Che, Yulan; Xu, Yi; Wang, Renjie; Chen, Li

    2017-08-01

    A rapid and sensitive analytical method was developed to detect pathogenic bacteria which combined magnetic enrichment, fluorescence labeling with polyethylene glycol (PEG) magnetophoretic chromatography. As pathogenic bacteria usually exist in complex matrixes at low concentration, an efficient enrichment is essential for diagnosis. In order to capture series types of pathogenic bacteria in samples, amino-modified magnetic nanoparticles (Fe 3 O 4 @SiO 2 -NH 2 ) were prepared for efficient enrichment by the electrostatic interaction with pathogenic bacteria. It was shown that the capture efficiency reached up to 95.4% for Escherichia coli (E. coli). Furthermore, quantitative analysis of the bacteria was achieved by using acridine orange (AO) as a fluorescence probe for the captured E. coli due to its ability of staining series types of bacteria and rapid labeling. In order to remove the free magnetic nanoparticles and redundant fluorescent reagent, the labeled suspension was poured into a PEG separation column and was separated by applying an external magnetic field. The presence of 100 cfu mL -1 E. coli could be detected for semi-quantitative analysis by observing the separation column with the naked eye, and the concentration could be further evaluated by fluorescence detection. All the above processes were finished within 80 min. It was demonstrated that a good linear relationship existed between the fluorescence intensity and the concentration of E. coli ranging from 10 2 to 10 6  cfu mL -1 , with a detection limit of 100 cfu mL -1 when E. coli acted as target bacteria. The recovery rate of E. coli was 93.6∼102.0% in tap water and cooked meat samples, and the RSD was lower than 7% (n = 6); the result coincided with the conventional plate count method. Graphical abstract ᅟ.

  18. 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.

  19. Determination of total ribonucleotide pool in plant materials by high-pH anion-exchange high-performance liquid chromatography following extraction with potassium hydroxide.

    Science.gov (United States)

    Riondet, Christophe; Morel, Sylvain; Alcaraz, Gérard

    2005-06-10

    A new, improved method that only requires a potassium hydroxide extraction procedure is presented for the analysis of a full nucleotide pool in plant materials. Quantification was performed by high-pH anion-exchange chromatography (HPAEC) with UV detection after a potassium hydroxide extraction, and allowed the quantification of 13 linear ribonucleotides in a single run. The method has been validated by comparison of six extraction methods and also by measurement of the intracellular nucleotide levels of three plant species (cell cultures and leaves). The evolution of the nucleotide pool of Nicotiana tabacum cell culture during growth has also been measured, and showed an increase in the pool until the fifth day, where the growth rate reaches a maximum, after which a decrease was observed.

  20. Carbohydrate and alditol analysis by high-performance anion-exchange chromatography coupled with electrochemical detection at a cobalt-modified electrode.

    Science.gov (United States)

    Casella, Innocenzo G; Contursi, Michela

    2003-07-01

    A cobalt oxyhydroxide film dispersed on a carbon electrode surface was characterized and proposed as an amperometric sensor for determination of alditols and carbohydrates in flowing streams. Complex mixtures of carbohydrates were separated by anion-exchange chromatography using a moderately alkaline solution as mobile phase. The cobalt modified electrode (GC-Co) was employed under a constant applied potential of 0.5 V (vs Ag/AgCl). Under these experimental conditions the detection limits (S/N=3) for all analyzed electroactive molecules ranged between 0.3 micromol L(-1) and 1.5 micromol L(-1) and the dynamic linear ranges spanned generally three orders of magnitude above the relevant detection limits. Analytical determinations of carbohydrates and alditols in red and white wines, are reported.

  1. Partially hydrolyzed guar gum characterization and sensitive quantification in food matrices by high performance anion exchange chromatography with pulsed amperometric detection--validation using accuracy profile.

    Science.gov (United States)

    Mercier, G; Campargue, C

    2012-11-02

    Interest concerning functional ingredients and especially dietary fibres has been growing in recent years. At the same time, the variety of ingredient accepted as dietary fibres and their mixing at low level in complex matrices have considerably complicated their quantitative analysis by approved AOAC methods. These reasons have led to the specific development of an innovative analytical method performed by high-performance anion-exchange chromatography (HPAEC) with pulsed amperometric detection (PAD) to detect and quantify partially hydrolyzed guar gum (PHGG) in fruit preparation and dairy matrices. The analytical methodology was divided in two steps which could be deployed separately or in conjunction. The first, consists in a complete characterization of PHGG by size exclusion chromatography (SEC) with multi-angle light scattering and refractive index detection and HPAEC-PAD to determine its physico-chemical properties and galactomannans content, and the second step is the development of a new HPAEC-PAD method for PHGG direct quantification in complex matrices (dairy product). Validation in terms of detection and quantification limits, linearity of the analytical range, average accuracy (recovery, trueness) and average uncertainty were statistically carried out with accuracy profile. Overall, this new chromatographic method has considerably improved the possibility to quantify without fractionation treatment, low level of dietary fibres emerging from specific galactomannans, in complex matrices and many foodstuffs. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. 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.

  3. Retrospective study of rapid-exchange monorail versus over-the-wire technique for femoropopliteal angioplasty.

    Science.gov (United States)

    Jahnke, Thomas; Schäfer, Jost Philipp; Bolte, Hendrik; Schäfer, Fritz; Michalek, Jens; Charalambous, Nicholas; Sapoval, Marc; Müller-Hülsbeck, Stefan

    2008-01-01

    The purpose of this study was to compare procedural outcome of rapid-exchange (RX) monorail versus conventional over-the-wire (OTW) technique for femoropopliteal angioplasty. Demographic data, procedure details, angioplasty success, and complications of 328 consecutive percutaneous transluminal angioplasties (PTAs) were collected from a prospective database and retrospectively analyzed. Procedure details included duration of fluoroscopy, area-dose product, amount of contrast agent, sheath sizes, access route, length of stenosis, presence of total occlusion, technical and anatomical success (residual stenosis or = 6 Fr = 82.5% for OTW) but showed only a tendency toward lower overall complication rates (16.6% [17/102] in the RX group versus 19.9% [45/226] in the OTW group; p = 0.09). There was no effect on length of hospitalization. RX monorail systems were not associated with higher procedural costs when compared to conventional OTW technique. We conclude that RX monorail systems seem to enhance the technical success of femoropopliteal angioplasty. Although smaller sheath sizes can be used due to the lower profile of the RX systems, there is only a tendency toward lower complication rates.

  4. Therapeutic drug monitoring of nevirapine in saliva in Uganda using high performance liquid chromatography and a low cost thin-layer chromatography technique

    NARCIS (Netherlands)

    Lamorde, M.; Fillekes, Q.; Sigaloff, K.; Kityo, C.; Buzibye, A.; Kayiwa, J.; Merry, C.; Nakatudde-Katumba, L.; Burger, D.M.; Wit, T.F. de

    2014-01-01

    BACKGROUND: In resource limited settings access to laboratory monitoring of HIV treatment is limited and therapeutic drug monitoring is generally unavailable. This study aimed to evaluate nevirapine concentrations in saliva using low-cost thin-layer chromatography (TLC) and nevirapine concentrations

  5. Therapeutic drug monitoring of nevirapine in saliva in Uganda using high performance liquid chromatography and a low cost thin-layer chromatography technique

    NARCIS (Netherlands)

    Lamorde, Mohammed; Fillekes, Quirine; Sigaloff, Kim; Kityo, Cissy; Buzibye, Allan; Kayiwa, Joshua; Merry, Concepta; Nakatudde-Katumba, Lillian; Burger, David; Rinke de Wit, Tobias F.

    2014-01-01

    In resource limited settings access to laboratory monitoring of HIV treatment is limited and therapeutic drug monitoring is generally unavailable. This study aimed to evaluate nevirapine concentrations in saliva using low-cost thin-layer chromatography (TLC) and nevirapine concentrations in plasma

  6. The influence of salt type on the retention of bovine serum albumin in ion-exchange chromatography

    DEFF Research Database (Denmark)

    Al-Jibbouri, Sattar

    2007-01-01

    In this paper, an analysis of the influence of the salt types, NaCl, NaCH"3COO, Na"2SO"4 and Na"3C"6H"5O"7, on the isocratic retention behaviour of bovine serum albumin (BSA) on two anion-exchangers media (Source 30Q and TSK Gel Super Q 5 PW) has been presented. The retention data demonstrated...

  7. 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.

  8. 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

  9. Determination of ethephon residues in water by gas chromatography with cubic mass spectrometry after ion-exchange purification and derivatisation with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide.

    Science.gov (United States)

    Royer, A; Laporte, F; Bouchonnet, S; Communal, P-Y

    2006-03-03

    An analytical method has been developed for the determination of residues of ethephon (2-chloroethyl phosphonic acid) in drinking and surface water. The procedure is based on de-ionisation with an anion/cation-exchange resin, solid phase extraction by means of anion-exchange polystyrene-divinylbenzene extraction disks, elution with a mixture of methanol and 10 M hydrochloric acid (98/2, v/v), redisolution into acetonitrile after evaporation and silylation with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Quantification is performed by gas chromatography with ion-trap cubic mass spectrometric detection in the electron impact mode (GC-EI-MS3). Method validation was conducted using samples of mineral, tap, and river water that were fortified with ethephon at concentration levels ranging from 0.1 to 1.0 microg/L. The mean recovery from all the fortified samples (n = 36) amounted to 88% with a relative standard deviation of 17%. The method, therefore, was shown to allow accurate determination of ethephon residues in drinking and surface water with a limit of quantification of 0.1 microg/L.

  10. Offline coupling of low-pressure anion-exchange chromatography with MALDI-MS to determine the elution order of human milk oligosaccharides.

    Science.gov (United States)

    Finke, B; Mank, M; Daniel, H; Stahl, B

    2000-09-10

    Pooled human milk oligosaccharides were separated into neutral and several acidic oligosaccharide fractions by preparative anion-exchange chromatography (AEC) using AG 1-X2. The oligosaccharides were eluted stepwise using deionized water and three different concentrations of ammonium acetate buffer, pH 6.8. The elution order of the compounds was determined directly by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) analysis of the AEC effluent without any cleanup or concentration steps. Up to a concentration of 500 mM ammonium acetate, the masses of acidic oligosaccharides could be detected by screening the fractions in an automated mode. The combination of the improved chromatographic procedure, the applied MALDI matrices, and operating parameters is suitable for the detection of neutral oligosaccharides as well as acidic oligosaccharides. The method provides high sensitivity and mass accuracy, including for the high-molecular-weight monosialylated oligosaccharides up to 2751.5 Da. The applied ionic strength of the anion-exchange eluents enables a rapid and an unambiguous composition assignment by MALDI-MS for neutral, monosialylated, and disialylated oligosaccharides from human milk. The acidic fractions have to be desalted by electrodialysis and were finally analyzed by HPAEC-PAD to get a high-resolution "fingerprint" of structures present in each fraction. From these analyses, it can be concluded that the isomeric variety of monosialylated oligosaccharides occurring in human milk is higher than estimated before. Copyright 2000 Academic Press.

  11. Application of liquid chromatography techniques to the measurement of soluble transition metals in PWR primary coolant

    International Nuclear Information System (INIS)

    Amey, M.D.H.; Brown, G.R.

    1987-01-01

    Two chromatographic techniques have been developed, and evaluated for the on-line analysis of soluble transition metals, particularly cobalt, in PWR primary coolant. Automatic operation and control, together with data processing and storage has been achieved by interfacing a Dionex ion chromatograph to a microprocessor control system. An absolute detection limit of 0.1 ng cobalt has been obtained which, with on-line sample preconcentration (100 ml), has enabled measurements to be made down to part-per-trillion levels (0.001 ppb). Application of the techniques to PWR coolant analysis was demonstrated by a programme of work on the Half Megawatt Loop at Winfrith. During this work some aspects of the behaviour of soluble metal species have been studied in both de-oxygenated and hydrogenated conditions. The effects of changes in coolant chemistry, operating temperature, and sample line flowrates on circulating impurity levels are reported, together with the dramatic effects observed when part of the circuit pipework was replaced with new stainless steel tubing. (author)

  12. Development and Application of a Fast Chromatography Technique for Analysis of Biogenic Volatile Organic Compounds in Plant Emissions

    Science.gov (United States)

    Jones, C. E.; Kato, S.; Nakashima, Y.; Yamazakii, S.; Kajii, Y. J.

    2011-12-01

    Biogenic volatile organic compounds (BVOCs) emitted from vegetation constitute the largest fraction (>90 %) of total global non-methane VOC supplied to the atmosphere, yet the chemical complexity of these emissions means that achieving comprehensive measurements of BVOCs, and in particular the less volatile terpenes, is not straightforward. As such, there is still significant uncertainty associated with the contribution of BVOCs to the tropospheric oxidation budget, and to atmospheric secondary organic aerosol (SOA) formation. The rate of BVOC emission from vegetation is regulated by environmental conditions such as light intensity and temperature, and thus can be highly variable, necessitating high time-resolution BVOC measurements. In addition, the numerous monoterpene and sesquiterpene isomers, which are indistinguishable by some analytical techniques, have greatly varying lifetimes with respect to atmospheric oxidants, and as such quantification of each individual isomer is fundamental to achieving a comprehensive characterisation of the impact of BVOCs upon the atmospheric oxidation capacity. However, established measurement techniques for these trace gases typically offer a trade-off between sample frequency and the level of speciation; detailed information regarding chemical composition may be obtained, but with reduced time resolution, or vice versa. We have developed a Fast-GC-FID technique for quantification of a range of monoterpene, sesquiterpene and oxygenated C10 BVOC isomers, which retains the separation capability of conventional gas chromatography, yet offers considerably improved sample frequency. Development of this system is ongoing, but currently a 20 m x 0.18 mm i.d resistively heated metal column is employed to achieve chromatographic separation of thirteen C10-C15 BVOCs, within a total cycle time of ~15 minutes. We present the instrument specifications and analytical capability, together with the first application of this Fast-GC technique

  13. Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

    Directory of Open Access Journals (Sweden)

    Mª Esther Torres Padrón

    2014-07-01

    Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

  14. Characterisation of lipid fraction of marine macroalgae by means of chromatography techniques coupled to mass spectrometry.

    Science.gov (United States)

    Ragonese, Carla; Tedone, Laura; Beccaria, Marco; Torre, Germana; Cichello, Filomena; Cacciola, Francesco; Dugo, Paola; Mondello, Luigi

    2014-02-15

    In this work the characterisation of the lipid fraction of several species of marine macro algae gathered along the eastern coast of Sicily is reported. Two species of green marine algae (Chloropyceae), two species of red marine algae (Rhodophyceae) and four species of brown marine algae (Pheophyceae) were evaluated in terms of fatty acids, triacylglycerols, pigments and phospholipids profile. Advanced analytical techniques were employed to fully characterise the lipid profile of these Mediterranean seaweeds, such as GC-MS coupled to a novel mass spectra database supported by the simultaneous use of linear retention index (LRI) for the identification of fatty acid profile; LC-MS was employed for the identification of triacylglycerols (TAGs), carotenoids and phospholipids; the determination of accurate mass was carried out on carotenoids and phospholipids. Quantitative data are reported on fatty acids and triacylglycerols as relative percentage of total fraction. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Analysis of human bone alkaline phosphatase isoforms: comparison of isoelectric focusing and ion-exchange high-performance liquid chromatography.

    Science.gov (United States)

    Sharp, Christopher A; Linder, Cecilia; Magnusson, Per

    2007-04-01

    Several isoforms of alkaline phosphatase (ALP) can be identified in human tissues and serum after separation by anion-exchange HPLC and isoelectric focusing (IEF). We purified four soluble bone ALP (BALP) isoforms (B/I, B1x, B1 and B2) from human SaOS-2 cells, determined their specific pI values by broad range IEF (pH 3.5-9.5), compared these with commercial preparations of bone, intestinal and liver ALPs and established the effects of neuraminidase and wheat germ lectin (WGA) on enzyme activity. Whilst the isoforms B1x (pI=4.48), B1 (pI=4.32) and B2 (pI=4.12) resolved as well-defined bands, B/I resolved as a complex (pI=4.85-6.84). Neuraminidase altered the migration of all BALP isoforms to pI=6.84 and abolished their binding to the anion-exchange matrix, but increased their enzymatic activities by 11-20%. WGA precipitated the BALP isoforms in IEF gels and the HPLC column and attenuated their enzymatic activities by 54-73%. IEF resolved the commercial BALP into 2 major bands (pI=4.41 and 4.55). Migration of BALP isoforms is similar in IEF and anion-exchange HPLC and dependent on sialic acid content. HPLC is preferable in smaller scale research applications where samples containing mixtures of BALP isoforms are analysed. Circulating liver ALP (pI=3.85) can be resolved from BALP by either method. IEF represents a simpler approach for routine purposes even though some overlapping of the isoforms may occur.

  16. Development of a broad toxicological screening technique for urine using ultra-performance liquid chromatography and time-of-flight mass spectrometry

    DEFF Research Database (Denmark)

    Lee, Hon Kit; Ho, Chung Shun; Iu, Yan Ping Heidi

    2009-01-01

    Withdrawal of the support for the REMEDi HS drug profiling system has necessitated its replacement within our laboratories with an alternative broad toxicological screening technique. To this end, a novel method, based on ultra-performance liquid chromatography (UPLC) and time-of-flight (TOF) mass...

  17. Laser Stimulated Genomic Exchange in Stem Cells. Laser Non-cloning Techniques

    Science.gov (United States)

    Stefan, V. Alexander

    2012-02-01

    I propose a novel technique for a pluripotent stem cell generation. Genomic exchange is stimulated by the beat-wave free electron laser, (B-W FEL), frequency matching with the frequencies of the DNAootnotetextJ.D. Watson and F. H. C. Crick, Nature, 171, 737-738 (1953). eigen-oscillations. B-W FEL-1ootnotetextV. Stefan, B.I.Cohen, C. Joshi Science, 243,4890, (Jan 27,1989); Stefan, et al., Bull. APS. 32, No. 9, 1713 (1987); Stefan, APS March-2011, #S1.143; APS- March-2009, #K1.276. scans entire stem cell; B-W FEL-2 probes the chromosomes. The scanning and probing lasers: 300-500nm and 100-300nm, respectively; irradiances: the order-of-10s mW/cm^2 (above the threshold value for a particular gene structure); repetition rate of few-100s Hz. A variety of genetic-matching conditions can be arranged. Genomic glitches, (the cell nucleus transferootnotetextScott Noggle et al. Nature, 478, 70-75 (06 October 2011).), can be hedged by the use of lasers.

  18. Alternative solidification techniques for radioactive ion exchange resins and liquid concentrates

    International Nuclear Information System (INIS)

    Thegerstroem, C.

    1980-01-01

    Methods, that are used or are under development for solidification of radioactive ion exchange resins or liquid concentrates, utilize normally cement, bitumen or some polymere as matrix material. This report contains a review and a description of these solidification processes and their products, especially of relatively new techniques that are under development in different countries. It is possible that solidification in thermosetting resins will be more used in the future, especially when product quality requirements are high (for instance when solidifying medium level resins) or when special waste categories has to be solidified. However it is not probable that thermosetting resins will be extensively used in a broad application as matrix material. In that case the methods are to complicated and expensive compared to, for instance, solidification in concrete. Systems for incorporation in polyesteremulsions (Dow-process) have a potential as they are quite simple and can accept a large variation of liquid wastes. Some methods in an early stage of development (for instance Inert Carrier Radwaste Process) will have to be tested in active application before they can be further evaluated. (author)

  19. Application of Resin in Pulp Technique for Ion Exchange Separation of Uranium from Alkaline Leachate

    International Nuclear Information System (INIS)

    Sreenivas, T.; Rajan, K.C.; Chakravartty, J.K.

    2014-01-01

    Conclusions: • Resin-in-pulp technique was applied for purification and enrichment of uranium values from a finely ground uranium ore leach slurry of alkaline nature using strong base anion exchange resin (size 500 - 675μm). • The chemical composition of the solution phase of the alkaline leach slurry (pH 9.5) was consisting of about 40 g/L of total dissolved solutes (TDS) predominantly with Na_2CO_3 and NaHCO_3 and minor levels of Na_2SO_4. The uranium content was only 730 mg/L and d50 of solids was 34μm. • Amongst the various commercially available resins studied PFA 4740 and 4783 having quaternary ammonium ion on polystyrene crosslink with divibyl benzez (DVB) gave best performance. The maximum loading capacity achieved in the RIP studies was about 60-65 g of U_3O_8/L of wet settled resin amounting to 98% of loading. This has necessitated 4 stages of counter-current extraction with overall contact time of 100 minutes at a resin to leach slurry volume ratio of about 1:50. Practically the entire uranium values loaded on the resin were eluted using NaCl. • The RIP process was found quite efficient for uranium bearing alkaline leach slurries.

  20. A novel Fast Gas Chromatography based technique for higher time resolution measurements of speciated monoterpenes in air

    Science.gov (United States)

    Jones, C. E.; Kato, S.; Nakashima, Y.; Kajii, Y.

    2013-12-01

    Biogenic emissions supply the largest fraction of non-methane volatile organic compounds (VOC) from the biosphere to the atmospheric boundary layer, and typically comprise a complex mixture of reactive terpenes. Due to this chemical complexity, achieving comprehensive measurements of biogenic VOC (BVOC) in air within a satisfactory time resolution is analytically challenging. To address this, we have developed a novel, fully automated Fast Gas Chromatography (Fast-GC) based technique to provide higher time resolution monitoring of monoterpenes (and selected other C9-C15 terpenes) during plant emission studies and in ambient air. To our knowledge, this is the first study to apply a Fast-GC based separation technique to achieve quantification of terpenes in air. Three chromatography methods have been developed for atmospheric terpene analysis under different sampling scenarios. Each method facilitates chromatographic separation of selected BVOC within a significantly reduced analysis time compared to conventional GC methods, whilst maintaining the ability to quantify individual monoterpene structural isomers. Using this approach, the C10-C15 BVOC composition of single plant emissions may be characterised within a ~ 14 min analysis time. Moreover, in situ quantification of 12 monoterpenes in unpolluted ambient air may be achieved within an ~ 11 min chromatographic separation time (increasing to ~ 19 min when simultaneous quantification of multiple oxygenated C9-C10 terpenoids is required, and/or when concentrations of anthropogenic VOC are significant). This corresponds to a two- to fivefold increase in measurement frequency compared to conventional GC methods. Here we outline the technical details and analytical capability of this chromatographic approach, and present the first in situ Fast-GC observations of 6 monoterpenes and the oxygenated BVOC linalool in ambient air. During this field deployment within a suburban forest ~ 30 km west of central Tokyo, Japan, the

  1. Leak detection in a high-pressure heat exchanger system in a refinery using radiotracer technique

    International Nuclear Information System (INIS)

    Samantray, J.S.; Sunil Goswami; Sharma, V.K.; Jayashree Biswal; Pant, H.J.

    2014-01-01

    A radiotracer investigation was carried out in a diesel hydrotreater (DHDT) unit in a refinery for leak detection in a breech-lock heat exchanger system. The main objectives of the study were to identify the leaking heat exchanger in a system with six heat exchangers and estimate the leak rate. Bromine-82 as dibromobiphenyl was selected and used as radiotracer for the investigation. The radiotracer was instantaneously injected into the suction end of the feed pump line to the heat exchanger of the DHDT unit. The movement of the tracer was measured at strategically selected locations using NaI(Tl) scintillation detectors. Based upon the results of the radiotracer investigation, it was found that out of six heat exchangers, exchanger E-1F was leaking. (author)

  2. Optimization of elution salt concentration in stepwise elution of protein chromatography using linear gradient elution data. Reducing residual protein A by cation-exchange chromatography in monoclonal antibody purification.

    Science.gov (United States)

    Ishihara, Takashi; Kadoya, Toshihiko; Endo, Naomi; Yamamoto, Shuichi

    2006-05-05

    Our simple method for optimization of the elution salt concentration in stepwise elution was applied to the actual protein separation system, which involves several difficulties such as detection of the target. As a model separation system, reducing residual protein A by cation-exchange chromatography in human monoclonal antibody (hMab) purification was chosen. We carried out linear gradient elution experiments and obtained the data for the peak salt concentration of hMab and residual protein A, respectively. An enzyme-linked immunosorbent assay was applied to the measurement of the residual protein A. From these data, we calculated the distribution coefficient of the hMab and the residual protein A as a function of salt concentration. The optimal salt concentration of stepwise elution to reduce the residual protein A from the hMab was determined based on the relationship between the distribution coefficient and the salt concentration. Using the optimized condition, we successfully performed the separation, resulting in high recovery of hMab and the elimination of residual protein A.

  3. Dependence of chlorine isotope separation in ion exchange chromatography on the nature and concentration of the eluent

    International Nuclear Information System (INIS)

    Heumann, K.G.; Baier, K.

    1980-01-01

    In a heterogeneous electrolyte system of a strongly basic anion exchanger and solutions of NaBF 4 or NaClO 4 we established the influence of the nature and concentration of the eluent in chromatographic experiments on chlorine isotope separation. Results show that when the elctrolyte concentration is increased the degree of isotope separation decreases. With NaBF 4 the separation factor is greater than with NaClO 4 under conditions which are otherwise the same. For electrolyte solutions containing ClO 4 -, NO 3 - and BF 4 - there is a linear relation between the separation factor of the chlorine isotopes and the logarithm of the heat of anion hydration of the elution electrolyte. (orig.)

  4. Solvent Front Position Extraction procedure with thin-layer chromatography as a mode of multicomponent sample preparation for quantitative analysis by instrumental technique.

    Science.gov (United States)

    Klimek-Turek, A; Sikora, E; Dzido, T H

    2017-12-29

    A concept of using thin-layer chromatography to multicomponent sample preparation for quantitative determination of solutes followed by instrumental technique is presented. Thin-layer chromatography (TLC) is used to separate chosen substances and their internal standard from other components (matrix) and to form a single spot/zone containing them at the solvent front position. The location of the analytes and internal standard in the solvent front zone allows their easy extraction followed by quantitation by HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Inter-comparison of laser photoacoustic spectroscopy and gas chromatography techniques for measurements of ethene in the atmosphere.

    Science.gov (United States)

    Kuster, William C; Harren, Frans J M; de Gouw, Joost A

    2005-06-15

    Laser photoacoustic spectroscopy (LPAS) is highly suitable for the detection of ethene in air due to the overlap between its strongest absorption lines and the wavelengths accessible by high-powered CO2 lasers. Here, we test the ability of LPAS to measure ethene in ambient air by comparing the measurements in urban air with those from a gas chromatography flame-ionization detection (GC-FID) instrument. Over the course of several days, we obtained quantitative agreement between the two measurements. Over this period, the LPAS instrument had a positive offset of 330 +/- 140 pptv (parts-per-trillion by volume) relative to the GC-FID instrument, possibly caused by interference from other species. The detection limit of the LPAS instrument is currently estimated around 1 ppbv and is limited by this offset and the statistical noise in the data. We conclude that LPAS has the potential to provide fast-response measurements of ethene in the atmosphere, with significant advantages over existing techniques when measuring from moving platforms and in the vicinity of emission sources.

  6. Forensic Analysis of Blue Ball point Pen Inks on Questioned Documents by High Performance Thin Layer Chromatography Technique (HPTLC)

    International Nuclear Information System (INIS)

    Lee, L.C.; Siti Mariam Nunurung; Abdul Aziz Ishak

    2014-01-01

    Nowadays, crimes related to forged documents are increasing. Any erasure, addition or modification in the document content always involves the use of writing instrument such as ball point pens. Hence, there is an evident need to develop a fast and accurate ink analysis protocol to solve this problem. This study is aimed to determine the discrimination power of high performance thin layer chromatography (HPTLC) technique for analyzing a set of blue ball point pen inks. Ink samples deposited on paper were extracted using methanol and separated via a solvent mixture of ethyl acetate, methanol and distilled water (70: 35: 30, v/ v/ v). In this method, the discrimination power of 89.40 % was achieved, which confirm that the proposed method was able to differentiate a significant number of pen-pair samples. In addition, composition of blue pen inks was found to be homogeneous (RSD < 2.5 %) and the proposed method showed good repeatability and reproducibility (RSD < 3. 0%). As a conclusion, HPTLC is an effective tool to separate blue ball point pen inks. (author)

  7. Comparison of gas chromatography/mass spectrometry and immunoassay techniques on concentrations of atrazine in storm runoff

    Science.gov (United States)

    Lydy, Michael J.; Carter, D.S.; Crawford, Charles G.

    1996-01-01

    Gas chromatography/mass spectrometry (GC/MS) and enzyme-linked immunosorbent assay (ELISA) techniques were used to measure concentrations of dissolved atrazine in 149 surface-water samples. Samples were collected during May 1992–September 1993 near the mouth of the White River (Indiana) and in two small tributaries of the river. GC/MS was performed on a Hewlett-Packard 5971 A, with electron impact ionization and selected ion monitoring of filtered water samples extracted by C-18 solid phase extraction; ELISA was performed with a magnetic-particle-based assay with photometric analysis. ELISA results compared reasonably well to GC/MS measurements at concentrations below the Maximum Contaminant Level for drinking water set by the U.S. Environmental Protection Agency (3.0 μg/L), but a systematic negative bias was observed at higher concentrations. When higher concentration samples were diluted into the linear range of calibration, the relation improved. A slight positive bias was seen in all of the ELISA data compared to the GC/MS results, and the bias could be partially explained by correcting the ELISA data for cross reactivity with other triazine herbicides. The highest concentrations of atrazine were found during the first major runoff event after the atrazine was applied. Concentrations decreased throughout the rest of the sampling period even though large runoff events occurred during this time, indicating that most atrazine loading to surface waters in the study area occurs within a few weeks after application.

  8. Characterisation and discrimination of various types of lac resin using gas chromatography mass spectrometry techniques with quaternary ammonium reagents.

    Science.gov (United States)

    Sutherland, K; del Río, J C

    2014-04-18

    A variety of lac resin samples obtained from artists' suppliers, industrial manufacturers, and museum collections were analysed using gas chromatography mass spectrometry (GCMS) and reactive pyrolysis GCMS with quaternary ammonium reagents. These techniques allowed a detailed chemical characterisation of microgram-sized samples, based on the detection and identification of derivatives of the hydroxy aliphatic and cyclic (sesquiterpene) acids that compose the resin. Differences in composition could be related to the nature of the resin, e.g. wax-containing (unrefined), bleached, or aged samples. Furthermore, differences in the relative abundances of aliphatic hydroxyacids appear to be associated with the biological source of the resin. The diagnostic value of newly characterised lac components, including 8-hydroxyacids, is discussed here for the first time. Identification of derivatised components was aided by AMDIS deconvolution software, and discrimination of samples was enhanced by statistical evaluation of data using principal component analysis. The robustness of the analyses, together with the minimal sample size required, make these very powerful approaches for the characterisation of lac resin in museum objects. The value of such analyses for enhancing the understanding of museum collections is illustrated by two case studies of objects in the collection of the Philadelphia Museum of Art: a restorer's varnish on a painting by Luca Signorelli, and a pictorial inlay in an early nineteenth-century High Chest by George Dyer. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Separation of bismuth from gram amounts of thallium and silver by cation-exchange chromatography in nitric acid.

    Science.gov (United States)

    Meintjies, E; Strelow, F W; Victor, A H

    1987-04-01

    Traces and small amounts of bismuth can be separated from gram amounts of thallium and silver by successively eluting these elements with 0.3M and 0.6M nitric acid from a column containing 13 ml (3 g) of AG50W-X4, a cation-exchanger (100-200 mesh particle size) with low cross-linking. Bismuth is retained and can be eluted with 0.2M hydrobromic acid containing 20% v/v acetone, leaving many other trace elements absorbed. Elution of thallium is quite sharp, but silver shows a small amount of tailing (less than 1 gmg/ml silver in the eluate) when gram amounts are present, between 20 and 80 mug of silver appearing in the bismuth fraction. Relevant elution curves and results for the analysis of synthetic mixtures containing between 50 mug and 10 mg of bismuth and up to more than 1 g of thallium and silver are presented, as well as results for bismuth in a sample of thallium metal and in Merck thallium(I) carbonate. As little as 0.01 ppm of bismuth can be determined when the separation is combined with electrothermal atomic-absorption spectrometry.

  10. Determination of sugar compounds in olive plant extracts by anion-exchange chromatography with pulsed amperometric detection.

    Science.gov (United States)

    Cataldi, T R; Margiotta, G; Iasi, L; Di Chio, B; Xiloyannis, C; Bufo, S A

    2000-08-15

    We describe a chromatographic method that uses isocratic elution and pulsed amperometric detection to determine soluble carbohydrates in plant tissues. Such a method provides a rapid and convenient means to obtain a complete profile of the sugar components of leaves and roots from olive (Olea europaea L. cv. Coratina) plants. A simple purification of plant extracts using pure water was developed, which is far less time-consuming and retains a high level of accuracy. Excellent separation of myo-inositol, galactinol, mannitol, galactose, glucose, fructose, sucrose, raffinose, and stachyose was achieved with an anion-exchange column and 12 mM NaOH spiked with 1 mM barium acetate as an eluent. At a flow rate of 1.0 mL/min, the time of analysis was less than 25 min, and repeatability of the method on the order of 2.2% as RSD or better for retention times and lower than 5.2% for peak areas. Recoveries approximated 100% (range 97.2-104.5%), and the method provided good precision with a coefficient of variation which ranged between 0.9 and 3.3%. Among identified carbohydrates extracted from leaves and roots of olive plants, glucose and mannitol were major compounds. Their molar ratio was estimated to be 1.2+/-0.1 and 2.2+/-0.3 for olive leaves and roots, respectively. The occurrence of soluble galactinol in plant tissues was also validated.

  11. Rapid analysis of charge variants of monoclonal antibodies using non-linear salt gradient in cation-exchange high performance liquid chromatography.

    Science.gov (United States)

    Joshi, Varsha; Kumar, Vijesh; Rathore, Anurag S

    2015-08-07

    A method is proposed for rapid development of a short, analytical cation exchange high performance liquid chromatography method for analysis of charge heterogeneity in monoclonal antibody products. The parameters investigated and optimized include pH, shape of elution gradient and length of the column. It is found that the most important parameter for development of a shorter method is the choice of the shape of elution gradient. In this paper, we propose a step by step approach to develop a non-linear sigmoidal shape gradient for analysis of charge heterogeneity for two different monoclonal antibody products. The use of this gradient not only decreases the run time of the method to 4min against the conventional method that takes more than 40min but also the resolution is retained. Superiority of the phosphate gradient over sodium chloride gradient for elution of mAbs is also observed. The method has been successfully evaluated for specificity, sensitivity, linearity, limit of detection, and limit of quantification. Application of this method as a potential at-line process analytical technology tool has been suggested. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Chiral ligand-exchange high-performance liquid chromatography with copper (II)-L-phenylalanine complexes for separation of 3,4-dimethoxy-α-methylphenylalanine racemes.

    Science.gov (United States)

    Jia, Dong-Xu; Ai, Zheng-Gui; Xue, Ya-Ping; Zheng, Yu-Guo

    2014-11-01

    L-3, 4-dimethoxy-α-methylphenylalanine (L-DMMD) is an important intermediate for the synthesis of 3-hydroxy-α-methyl-L-tyrosine (L-methyldopa). This paper describes an efficient, accurate, and low-priced method of high-performance liquid chromatography (HPLC) using chiral mobile phase and conventional C18 column to separate L-DMMD from its enantiomers. The effects of ligands, copper salts, organic modifiers, pHs of mobile phase, and temperatures on the retention factors (k') and selectivity (α) were evaluated to achieve optimal separation performance. Then, thermal analysis of the optimal separation conditions was investigated as well. It was confirmed that the optimal mobile phase was composed of 20 % (v/v) methanol, 8 mM L-phenylalanine (L-Phe), and 4 mM cupric sulfate in water of pH 3.2, and the column temperature was set at 20 °C. Baseline separation of two enantiomers could be obtained through the conventional C18 column with a resolution (R) of 3.18 in less than 18 min. Thermodynamic data (∆∆H and ∆∆S) obtained by Van't Hoff plots revealed the chiral separation was an enthalpy-controlled process. To the best of our knowledge, this is the first report regarding the enantioseparation of DMMD by chiral ligand-exchange HPLC.

  13. Fast analysis of quaternary ammonium pesticides in food and beverages using cation-exchange chromatography coupled with isotope-dilution high-resolution mass spectrometry.

    Science.gov (United States)

    Nardin, Tiziana; Barnaba, Chiara; Abballe, Franco; Trenti, Gianmaria; Malacarne, Mario; Larcher, Roberto

    2017-10-01

    A fast separation based on cation-exchange liquid chromatography coupled with high-resolution mass spectrometry is proposed for simultaneous determination of chlormequat, difenzoquat, diquat, mepiquat and paraquat in several food and beverage commodities. Solid samples were extracted using a mixture of water/methanol/formic acid (69.6:30:0.4, v/v/v), while liquid samples were ten times diluted with the same solution. Separation was carried out on an experimental length-modified IonPac CS17 column (2 × 15 mm 2 ) that allowed the use of formic acid and acetonitrile as mobile phase. Detection limits for food and beverage matrices were established at 1.5 μg/L for chlormequat, difenzoquat and mepiquat, and 3 μg/L for diquat and paraquat, while for drinking water a pre-analytical sample concentration allowed detection limits of 9 and 20 ng/L, respectively. Precision, as repeatability (RSD%), ranged from 0.2 to 24%, with a median value of 6%, and trueness, as recovery, ranged from 64 to 118%, with a median value of 96%. The method developed was successfully applied to investigate the presence of herbicide residues in commercial commodities (mineral water, orange juice, beer, tea, green coffee bean, toasted coffee powder, cocoa bean, white corn flour, rice and sugar samples). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. 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.

  15. Simultaneous measurement of proline and related compounds in oak leaves by high-performance ligand-exchange chromatography and electrospray ionization mass spectrometry for environmental stress studies.

    Science.gov (United States)

    Oufir, Mouhssin; Schulz, Nadine; Sha Vallikhan, Patan Shaik; Wilhelm, Eva; Burg, Kornel; Hausman, Jean-Francois; Hoffmann, Lucien; Guignard, Cedric

    2009-02-13

    A mass spectrometer was coupled to high-performance ligand-exchange liquid chromatography (HPLEC) for simultaneous analysis of stress associated solutes such as proline, hydroxyproline, methylproline, glycine betaine and trigonelline extracted from leaves of drought stressed oaks and an internal standard namely N-acetylproline. Methanol/chloroform/water extracts were analyzed using an Aminex HPX-87C column and specifically quantified by the positive ion mode of an electrospray ionisation-mass spectrometry (ESI-MS) in single ion monitoring (SIM) mode. The recovery of N-acetyl proline added to oak leaf extracts ranged from 85.2 to 122.1% for an intra-day study. Standard calibration curves showed good linearity in the measured range from 0.3125 to 10micromolL(-1) with the lowest correlation coefficient of 0.99961 for trigonelline. The advantages of this alternative procedure, compared to previously published methods using fluorescence or amperometric detections, are the simultaneous and direct detection of osmoprotectants in a single chromatographic run, a minimal sample preparation, a good specificity and reduced limits of quantification, ranging from 0.1 to 0.6micromolL(-1). Fifty-six days of water deficit exposure resulted in increased foliar free proline levels (2.4-fold, P<0.001, 155micromolg(-1) FW) and glycine betaine contents (2.5-fold, P<0.05, 175micromolg(-1) FW) of drought stressed oak compared to control.

  16. Determination of Histamine in Silages Using Nanomaghemite Core (γ-Fe2O3-Titanium Dioxide Shell Nanoparticles Off-Line Coupled with Ion Exchange Chromatography

    Directory of Open Access Journals (Sweden)

    Natalia Cernei

    2016-09-01

    Full Text Available The presence of biogenic amines is a hallmark of degraded food and its products. Herein, we focused on the utilization of magnetic nanoparticles off-line coupled with ion exchange chromatography with post-column ninhydrin derivatization and Vis detection for histamine (Him separation and detection. Primarily, we described the synthesis of magnetic nanoparticles with nanomaghemite core (γ-Fe2O3 functionalized with titanium dioxide and, then, applied these particles to specific isolation of Him. To obtain further insight into interactions between paramagnetic particles’ (PMP surface and Him, a scanning electron microscope was employed. It was shown that binding of histamine causes an increase of relative current response of deprotonated PMPs, which confirmed formation of Him-PMPs clusters. The recovery of the isolation showed that titanium dioxide-based particles were able to bind and preconcentrate Him with recovery exceeding 90%. Finally, we successfully carried out the analyses of real samples obtained from silage. We can conclude that our modified particles are suitable for Him isolation, and thus may serve as the first isolation step of Him from biological samples, as it is demonstrated on alfalfa seed variety Tereza silage.

  17. Two Inexpensive and Non-destructive Techniques to Correct for Smaller-Than-Gasket Leaf Area in Gas Exchange Measurements

    Directory of Open Access Journals (Sweden)

    Andreas M. Savvides

    2018-04-01

    Full Text Available The development of technology, like the widely-used off-the-shelf portable photosynthesis systems, for the quantification of leaf gas exchange rates and chlorophyll fluorescence offered photosynthesis research a massive boost. Gas exchange parameters in such photosynthesis systems are calculated as gas exchange rates per unit leaf area. In small chambers (<10 cm2, the leaf area used by the system for these calculations is actually the internal gasket area (AG, provided that the leaf covers the entire AG. In this study, we present two inexpensive and non-destructive techniques that can be used to easily quantify the enclosed leaf area (AL of plant species with leaves of surface area much smaller than the AG, such as that of cereal crops. The AL of the cereal crop species studied has been measured using a standard image-based approach (iAL and estimated using a leaf width-based approach (wAL. iAL and wAL did not show any significant differences between them in maize, barley, hard and soft wheat. Similar results were obtained when the wAL was tested in comparison with iAL in different positions along the leaf in all species studied. The quantification of AL and the subsequent correction of leaf gas exchange parameters for AL provided a precise quantification of net photosynthesis and stomatal conductance especially with decreasing AL. This study provides two practical, inexpensive and non-destructive solutions to researchers dealing with photosynthesis measurements on small-leaf plant species. The image-based technique can be widely used for quantifying AL in many plant species despite their leaf shape. The leaf width-based technique can be securely used for quantifying AL in cereal crop species such as maize, wheat and barley along the leaf. Both techniques can be used for a wide range of gasket shapes and sizes with minor technique-specific adjustments.

  18. An Experimentally Validated Numerical Modeling Technique for Perforated Plate Heat Exchangers.

    Science.gov (United States)

    White, M J; Nellis, G F; Kelin, S A; Zhu, W; Gianchandani, Y

    2010-11-01

    Cryogenic and high-temperature systems often require compact heat exchangers with a high resistance to axial conduction in order to control the heat transfer induced by axial temperature differences. One attractive design for such applications is a perforated plate heat exchanger that utilizes high conductivity perforated plates to provide the stream-to-stream heat transfer and low conductivity spacers to prevent axial conduction between the perforated plates. This paper presents a numerical model of a perforated plate heat exchanger that accounts for axial conduction, external parasitic heat loads, variable fluid and material properties, and conduction to and from the ends of the heat exchanger. The numerical model is validated by experimentally testing several perforated plate heat exchangers that are fabricated using microelectromechanical systems based manufacturing methods. This type of heat exchanger was investigated for potential use in a cryosurgical probe. One of these heat exchangers included perforated plates with integrated platinum resistance thermometers. These plates provided in situ measurements of the internal temperature distribution in addition to the temperature, pressure, and flow rate measured at the inlet and exit ports of the device. The platinum wires were deposited between the fluid passages on the perforated plate and are used to measure the temperature at the interface between the wall material and the flowing fluid. The experimental testing demonstrates the ability of the numerical model to accurately predict both the overall performance and the internal temperature distribution of perforated plate heat exchangers over a range of geometry and operating conditions. The parameters that were varied include the axial length, temperature range, mass flow rate, and working fluid.

  19. Evaluating a nursing erasmus exchange experience: Reflections on the use and value of the Nominal Group Technique for evaluation.

    Science.gov (United States)

    Cunningham, Sheila

    2017-09-01

    This paper discusses the use of Nominal Group Technique (NGT) for European nursing exchange evaluation at one university. The NGT is a semi-quantitative evaluation method derived from the Delphi method popular in the 1970s and 1980s. The NGT was modified from the traditional version retaining the structured cycles and but adding a broader group discussion. The NGT had been used for 2 successive years but required analysis and evaluation itself for credibility and 'fit' for purpose which is presented here. It aimed to explore nursing students' exchange experiences and aid programme development futures exchanges and closure from exchange. Results varied for the cohorts and students as participants enthusiastically engaged generating ample data which they ranked and categorised collectively. Evaluation of the NGT itself was two fold: by the programme team who considered purpose, audience, inclusivity, context and expertise. Secondly, students were asked for their thoughts using a graffiti board. Students avidly engaged with NGT but importantly also reported an effect from the process itself as an opportunity to reflect and share their experiences. The programme team concluded the NGT offered a credible evaluation tool which made use of authentic student voice and offered interactive group processes. Pedagogially, it enabled active reflection thus aiding reorientation back to the United Kingdom and awareness of 'transformative' consequences of their exchange experiences. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. A classification system of intraocular lens dislocation sites under operating microscopy, and the surgical techniques and outcomes of exchange surgery.

    Science.gov (United States)

    Hayashi, Ken; Ogawa, Soichiro; Manabe, Shin-Ichi; Hirata, Akira; Yoshimura, Koichi

    2016-03-01

    The aim of this study was to examine the recent status of intraocular lens (IOL) dislocation according to a classification system based on vertical dislocation position, as well as the surgical techniques and outcomes of IOL exchange surgery. The medical records of 230 eyes from 214 consecutive patients who experienced IOL dislocation and underwent exchange surgery between 2006 and 2014 were reviewed. Vertical dislocation sites observed preoperatively under operating microscopy were examined, along with the surgical techniques and outcomes of IOL exchange. Dislocation sites included (1) the anterior chamber (12.2 %), (2) pseudophakodonesis (19.1 %), (3) the anterior vitreous cavity (47.4 %), (4) trap door-like dislocation (dangling in the peripheral vitreous cavity; 16.1 %), and (5) the retinal surface (5.2 %). The IOL retained in the anterior segment was moved onto the iris by pulling it up through the limbal side ports with an anterior vitrectomy (67.8 %), or by pushing it up from the pars plana with an anterior vitrectomy (26.5 %), while the IOL dropped on the retina was lifting it up from the retina after pars plana vitrectomy (5.7 %). Mean uncorrected and distance-corrected visual acuity significantly improved postoperatively (p system, approximately 95 % of dislocated IOLs were retained in the anterior segment, and these IOLs were exchanged using an anterior approach through limbal incisions with an anterior vitrectomy. Visual acuity improved significantly, and serious complications were uncommon, probably because the IOL exchange techniques were standardized and simplified without pars plana vitrectomy.

  1. Enantioresolution in electrokinetic chromatography-complete filling technique using sulfated gamma-cyclodextrin. Software-free topological anticipation.

    Science.gov (United States)

    Escuder-Gilabert, Laura; Martín-Biosca, Yolanda; Medina-Hernández, María José; Sagrado, Salvador

    2016-10-07

    Few papers have tried to predict the resolution ability of chiral selectors in capillary electrophoresis for the separation of the enantiomers of chiral compounds. In a previous work, we have used molecular information available on-line to establish enantioresolution levels of basic compounds using highly sulfated β-CD (HS-β-CD) as chiral selector in electrokinetic chromatography-complete filling technique (EKC-CFT). The present study is a continuation of this previous work, introducing some novelties. In this work, the ability of sulfated γ-cyclodextrin (S-γ-CD) as chiral selector in EKC-CFT is modelled for the first time. Thirty-three structurally unrelated cationic and neutral compounds (drugs and pesticides) are studied. Categorical enantioresolution levels (RsC, 0 or 1) are assigned from experimental enantioresolution values obtained at different S-γ-CD concentrations. Novel topological parameters connected to the chiral carbon (C * -parameters) are introduced. Four C * -parameters and a topological parameter of the whole molecule (aromatic atom count) are the most important variables according to a discriminant partial least squares-variable selection process. It suggests the preponderance of the topology adjacent to the chiral carbon to anticipate the RsC levels. A software-free anticipation protocol for new molecules is proposed. Over the current set of molecules evaluated, 100% of correct anticipations (resolved and non-resolved compounds) are obtained, while anticipation of some compounds remains undetermined. A criterion is introduced to alert on compounds which should not be anticipated. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. The use of ion exchange chromatography methods for the determination of {sup 93}Zr in the samples of radioactive wastes; Vyuzitie metod ionovymennej chromatografie pre stanovenie {sup 93}Zr vo vzorkach radioaktivnych odpadov

    Energy Technology Data Exchange (ETDEWEB)

    Gardonova, V; Dulanska, S; Remenec, B; Matel, L [Univerzita Komenskeho v Bratislave, Prirodovedecka fakulta, Katedra jadrovej chemie, 84215 Bratislava (Slovakia)

    2012-04-25

    A simple and rapid method of preconcentration, separation and purification of {sup 93}Zr based on the methods of ion exchange chromatography with ion exchangers made by Eichrom Technologies, Inc. was developed. Multi-stage method of {sup 93}Zr separation proved to be suitable for the analysis of samples highly contaminated with radioactive waste in a relatively short time and with a high decontamination factor. The use and effectiveness of the method was successfully tested by analysis of heterogeneous waste from Mochovce nuclear power plant, which belongs to the most complex matrixes of radiochemical analysis. (authors)

  3. A Comparison of Selected Statistical Techniques to Model Soil Cation Exchange Capacity

    Science.gov (United States)

    Khaledian, Yones; Brevik, Eric C.; Pereira, Paulo; Cerdà, Artemi; Fattah, Mohammed A.; Tazikeh, Hossein

    2017-04-01

    Cation exchange capacity (CEC) measures the soil's ability to hold positively charged ions and is an important indicator of soil quality (Khaledian et al., 2016). However, other soil properties are more commonly determined and reported, such as texture, pH, organic matter and biology. We attempted to predict CEC using different advanced statistical methods including monotone analysis of variance (MONANOVA), artificial neural networks (ANNs), principal components regressions (PCR), and particle swarm optimization (PSO) in order to compare the utility of these approaches and identify the best predictor. We analyzed 170 soil samples from four different nations (USA, Spain, Iran and Iraq) under three land uses (agriculture, pasture, and forest). Seventy percent of the samples (120 samples) were selected as the calibration set and the remaining 50 samples (30%) were used as the prediction set. The results indicated that the MONANOVA (R2= 0.82 and Root Mean Squared Error (RMSE) =6.32) and ANNs (R2= 0.82 and RMSE=5.53) were the best models to estimate CEC, PSO (R2= 0.80 and RMSE=5.54) and PCR (R2= 0.70 and RMSE=6.48) also worked well and the overall results were very similar to each other. Clay (positively correlated) and sand (negatively correlated) were the most influential variables for predicting CEC for the entire data set, while the most influential variables for the various countries and land uses were different and CEC was affected by different variables in different situations. Although the MANOVA and ANNs provided good predictions of the entire dataset, PSO gives a formula to estimate soil CEC using commonly tested soil properties. Therefore, PSO shows promise as a technique to estimate soil CEC. Establishing effective pedotransfer functions to predict CEC would be productive where there are limitations of time and money, and other commonly analyzed soil properties are available. References Khaledian, Y., Kiani, F., Ebrahimi, S., Brevik, E.C., Aitkenhead

  4. Development of techniques to dispose of the Windscale AGR heat exchangers

    International Nuclear Information System (INIS)

    Crossley, H.; Wakefield, J.R.

    1991-01-01

    In a gas-cooled nuclear power plant the gas side of the heat exchanger tubes becomes contaminated with radioactive deposits carried from the reactor in the coolant stream. In order to dispose of the heat exchangers in the safest and most cost-effective way during plant decommissioning, the deposits have to be removed. In situ chemical decontamination is considered to be the only viable method. This paper describes the research and development of chemical decontamination methods for the Windscale AGR heat exchangers, and the testing of a selected method on an in situ superheater. The research involved characterization of tube corrosion and radioactivity deposits, laboratory testing of chemical reagents on actual tube samples, and the provision and operation of a plant to apply the selected reagent. Disposal of radioactive effluent is an important consideration in chemical decontamination and in the present case was the major factor in determining the process

  5. Determination of mercury species by the diffusive gradient in thin film technique and liquid chromatography – atomic fluorescence spectrometry after microwave extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pelcová, Pavlína, E-mail: pavlina.pelcova@mendelu.cz; Dočekalová, Hana, E-mail: hana.docekalova@mendelu.cz; Kleckerová, Andrea, E-mail: andrea.kleckerova@mendelu.cz

    2015-03-25

    Highlights: • DGT–MAE–LC–CV-AFS method was developed for determination of four mercury species. • The microwave extraction was used for isolation of mercury species from resin gels. • Optimized DGT–MAE–LC–CV-AFS method provides low detection limits (13–38 ng L{sup −1}). • The diffusion coefficients of four mercury species were simultaneously determined. - Abstract: A diffusive gradient in thin films technique (DGT) was combined with liquid chromatography (LC) and cold vapor atomic fluorescence spectrometry (CV-AFS) for the simultaneous quantification of four mercury species (Hg{sup 2+}, CH{sub 3}Hg{sup +}, C{sub 2}H{sub 5}Hg{sup +}, and C{sub 6}H{sub 5}Hg{sup +}). After diffusion through an agarose diffusive layer, the mercury species were accumulated in resin gels containing thiol-functionalized ion-exchange resins (Duolite GT73, and Ambersep GT74). A microwave-assisted extraction (MAE) in the presence of 6 M HCl and 5 M HCl (55 °C, 15 min) was used for isolation of mercury species from Ambersep and Duolite resin gels, respectively. The extraction efficiency was higher than 95.0% (RSD 3.5%). The mercury species were separated with a mobile phase containing 6.2% methanol + 0.05% 2-mercaptoethanol + 0.02 M ammonium acetate with a stepwise increase of methanol content up to 80% in the 16th min on a Zorbax C18 reverse phase column. The LODs of DGT–MAE–LC–CV-AFS method were 38 ng L{sup −1} for CH{sub 3}Hg{sup +}, 13 ng L{sup −1} for Hg{sup 2+}, 34 ng L{sup −1} for C{sub 2}H{sub 5}Hg{sup +} and 30 ng L{sup −1} for C{sub 6}H{sub 5}Hg{sup +} for 24 h DGT accumulation at 25 °C.

  6. Determination of free sulfites (SO3-2) in dried fruits processed with sulfur dioxide by ion chromatography through anion exchange column and conductivity detection.

    Science.gov (United States)

    Liao, Benjamin S; Sram, Jacqueline C; Files, Darin J

    2013-01-01

    A simple and effective anion ion chromatography (IC) method with anion exchange column and conductivity detector has been developed to determine free sulfites (SO3-2) in dried fruits processed with sulfur dioxide. No oxidation agent, such as hydrogen peroxide, is used to convert sulfites to sulfates for IC analysis. In addition, no stabilizing agent, such as formaldehyde, fructose or EDTA, is required during the sample extraction. This method uses aqueous 0.2 N NaOH as the solvent for standard preparation and sample extraction. The sulfites, either prepared from standard sodium sulfite powder or extracted from food samples, are presumed to be unbound SO3-2 in aqueous 0.2 N NaOH (pH > 13), because the bound sulfites in the sample matrix are released at pH > 10. In this study, sulfites in the standard solutions were stable at room temperature (i.e., 15-25 degrees C) for up to 12 days. The lowest standard of the linear calibration curve is set at 1.59 microg/mL SO3-2 (equivalent to 6.36 microg/g sample with no dilution) for analysis of processed dried fruits that would contain high levels (>1000 microg/g) of sulfites. As a consequence, this method typically requires significant dilution of the sample extract. Samples are prepared with a simple procedure of sample compositing, extraction with aqueous 0.2 N NaOH, centrifugation, dilution as needed, and filtration prior to IC. The sulfites in these sample extracts are stable at room temperature for up to 20 h. Using anion IC, the sulfites are eluted under isocratic conditions with 10 mM aqueous sodium carbonate solution as the mobile phase passing through an anion exchange column. The sulfites are easily separated, with an analysis run time of 18 min, regardless of the dried fruit matrix. Recoveries from samples spiked with sodium sulfites were demonstrated to be between 81 and 105% for five different fruit matrixes (apricot, golden grape, white peach, fig, and mango). Overall, this method is simple to perform and

  7. Study of iodine-iodate isotopic exchange reaction in neutral aqueous solutions by radiotracer technique

    International Nuclear Information System (INIS)

    Tripathi, R.; Ram, K.D.

    1993-01-01

    The isotopic exchange of iodine atoms in neutral aqueous solutions of iodate ions and iodine (in KI) is found to obey the rate law R = k [IO 3 - ] 0.4 [I 2 ] 1.2 at 175 o C. The addition of neutral ionic salts, e.g. KCl and KNO 3 , in the reaction mixture showed a slight catalytic effect on the exchange rate. Further, the kinetic salt effect indicated the involvement of at least one neutral species on the rate-determining step. The activation energy in neutral aqueous solutions of iodate ions and iodine is found to be 86 ± 3 kJ mol -1 , which decreases in the presence of KCl (79 ± 3 kJ mol -1 and KNO 3 (82 + 3 kJ mol -1 ). The activation parameters, viz. free energy of activation, enthalpy of activation and entropy of activation, were also calculated. Based on these results, an association-dissociation type of reaction mechanism is proposed for this exchange reaction in neutral aqueous medium, similar to that proposed earlier for iodide-iodate isotopic exchange reaction in neutral aqueous solutions, nitrate eutectic melts and iodide-iodate melts. (author)

  8. Simultaneous separation and determination of six arsenic species in rice by anion-exchange chromatography with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Ma, Li; Yang, Zhaoguang; Tang, Jie; Wang, Lin

    2016-06-01

    The simultaneous separation and determination of arsenite As(III), arsenate As(V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB), and arsenocholine (AsC) in rice samples have been carried out in one single anion-exchange column run by high-performance liquid chromatography with inductively coupled plasma mass spectrometry. To estimate the effect of variables on arsenic (As) speciation, the chromatographic conditions including type of competing anion, ionic strength, pH of elution buffer, and flow rate of mobile phase have been investigated by a univariate approach. Under the optimum chromatographic conditions, baseline separation of six As species has been achieved within 10 min by gradient elution program using 4 mM NH4 HCO3 at pH 8.6 as mobile phase A and 4 mM NH4 HCO3 , 40 mM NH4 NO3 at pH 8.6 as mobile phase B. The method detection limits for As(III), As(V), MMA, DMA, AsB, and AsC were 0.4, 0.9, 0.2, 0.4, 0.5, and 0.3 μg/kg, respectively. The proposed method has been applied to separation and quantification of As species in real rice samples collected from Hunan Province, China. The main As species detected in all samples were As(III), As(V) and DMA, with inorganic As accounting for over 80% of total As in these samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Cholesterol concentrations in lipoprotein fractions separated by anion-exchange-high-performance liquid chromatography in healthy dogs and dogs with hypercholesterolemia.

    Science.gov (United States)

    Oda, Hitomi; Mori, Akihiro; Hirowatari, Yuji; Takoura, Toshie; Manita, Daisuke; Takahashi, Tomoya; Shono, Saori; Onozawa, Eri; Mizutani, Hisashi; Miki, Yohei; Itabashi, Yukiko; Sako, Toshinori

    2017-10-01

    Anion-exchange (AEX)-high-performance liquid chromatography (HPLC) for measurement of cholesterol can be used to separate serum lipoproteins (high-density lipoprotein (HDL); low-density lipoprotein (LDL); intermediate-density lipoprotein (IDL); very-low-density lipoprotein (VLDL)) in humans. However, AEX-HPLC has not been applied in veterinary practice. We had three objectives: (i) the validation of AEX-HPLC methods including the correlation of serum cholesterol concentration in lipoprotein fraction measured by AEX-HPLC and gel permeation-HPLC (GP-HPLC) in healthy dogs and those with hypercholesterolemia was investigated; (ii) the reference intervals of lipoprotein fractions measured by AEX-HPLC from healthy dogs (n=40) was established; (iii) lipoprotein fractions from the serum of healthy dogs (n=12) and dogs with hypercholesterolemia (n=23) were compared. Analytic reproducibility and precision of AEX-HPLC were acceptable. Positive correlation between serum concentrations of total cholesterol (Total-Chol), HDL cholesterol (HDL-Chol), LDL cholesterol (LDL-Chol)+IDL cholesterol (IDL-Chol), and VLDL cholesterol (VLDL-Chol) was noted for AEX-HPLC and GP-HPLC in healthy dogs and dogs with hypercholesterolemia. Reference intervals measured by AEX-HPLC for serum concentrations of Total-Chol, HDL-Chol, and LDL-Chol were determined to be 2.97-9.32, 2.79-6.57, 0.16-3.28mmol/L (2.5-97.5% interval), respectively. Furthermore, there was significant difference in lipoprotein profiles between healthy and dogs with hypercholesterolemia. These results suggest that AEX-HPLC can be used to evaluate lipoprotein profiles in dogs and could be a new useful indicator of hyperlipidemia in dogs. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Chiral speciation and determination of selenomethionine enantiomers in selenized yeast by ligand-exchange micellar electrokinetic capillary chromatography after solid phase extraction.

    Science.gov (United States)

    Duan, Jiankun; He, Man; Hu, Bin

    2012-12-14

    A new phenylalanine derivative (L-N-(2-hydroxy-propyl)-phenylalanine, L-HP-Phe) was synthesized and its chelate with Cu(II) (Cu(II)-(L-HP-Phe)(2)) was used as the chiral selector for the ligand-exchange (LE) chiral separation of D,L-selenomethionine (SeMet) in selenized yeast samples by micelle electrokinetic capillary chromatography (MEKC). In order to improve the sensitivity of MEKC-UV, two-step preconcentration strategy was employed, off-line solid phase extraction (SPE) and on-line large volume sample stacking (LVSS). D,L-SeMet was first retained on the Cu(II) loaded mesoporous TiO(2), then eluted by 0.1 mL of 5 mol L(-1) ammonia, and finally introduced for MEKC-UV analysis by LVSS injection after evaporation of NH(3). With the enrichment factors of 1400 and 1378, the LODs of 0.44 and 0.60 ng mL(-1) for L-SeMet and D-SeMet was obtained, respectively. The developed method was applied to the analysis of D,L-SeMet in a certified reference material of SELM-1 and a commercial nutrition yeast, and the results showed that most of SeMet in the SELM-1 selenized yeast was l isomer and the recovery for L and D isomers in the spiked commercial nutrition yeast was 96.3% and 103%, respectively. This method is featured with low running cost, high sensitivity and selectivity, and exhibits application potential in chiral analysis of seleno amino acids in real world samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Ion-exchange solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for the determination of veterinary drugs in organic fertilizers.

    Science.gov (United States)

    Zhao, Zhiyong; Zhang, Yanmei; Xuan, Yanfang; Song, Wei; Si, Wenshuai; Zhao, Zhihui; Rao, Qinxiong

    2016-06-01

    The analysis of veterinary drugs in organic fertilizers is crucial for an assessment of potential risks to soil microbial communities and human health. We develop a robust and sensitive method to quantitatively determine 19 veterinary drugs (amantadine, sulfonamides and fluoroquinolones) in organic fertilizers. The method involved a simple solid-liquid extraction step using the combination of acetonitrile and McIlvaine buffer as extraction solvent, followed by cleanup with a solid-phase extraction cartridge containing polymeric mixed-mode anion-exchange sorbents. Ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was used to separate and detect target analytes. We particularly focused on the optimization of sample clean-up step: different diluents and dilution factors were tested. The developed method was validated in terms of linearity, recovery, precision, sensitivity and specificity. The recoveries of all the drugs ranged from 70.9% to 112.7% at three concentration levels, with the intra-day and inter-day relative standard deviation lower than 15.7%. The limits of quantification were between 1.0 and 10.0μg/kg for all the drugs. Matrix effect was minimized by matrix-matched calibration curves. The analytical method was successfully applied for the survey of veterinary drugs contamination in 20 compost samples. The results indicated that fluoroquinolones had higher incidence rate and mean concentration levels ranging from 31.9 to 308.7μg/kg compared with other drugs. We expect the method will provide the basis for risk assessment of veterinary drugs in organic fertilizers. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Modeling of retention of some fission products and actinides by ion-exchange chromatography with a complexing agent. Application to the determination of selectivity coefficients

    International Nuclear Information System (INIS)

    Gurdale-Tack, K.; Aubert, M.; Chartier, F.

    2000-01-01

    For an accurate determination of the isotopic and elemental composition of americium (Am), curium (Cm), neodymium (Nd) and cesium (Cs) in spent nuclear fuels, performed by Thermal Ionization Mass Spectrometry (TIMS) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS), it is necessary to separate these elements before analysis. This separation is mandatory because of isobaric interferences between americium and curium, neodymium and samarium (Sm) and between cesium and barium (Ba). This is the reason why Ba and Sm are analyzed with the other four elements. Separation is carried out by cation-exchange chromatography on a silica-based stationary phase in the presence of a complexing eluent. The complexing agent is 2-hydroxy-2-methyl butanoic acid (HMB), a monoprotic acid (HL) with a pK a of 3.6. Cations (M n+ ) interact with it to form ML y (n-y)+ complexes. Optimization of chromatographic separation conditions requires monitoring of the pH and eluent composition. The influence of each parameter on metal ion retention and on selectivity was investigated. The first studies on standard solutions with Sm(III), Nd(III), Cs(I) and Ba(II) showed that four conditions allow efficient separation. However, only one allows good separation with a real solution of spent nuclear fuels. This condition is a chelating agent concentration of 0.1 mol.l -1 and a pH of 4.2. With the other conditions, co-elution is observed for Cs(I) and Am(III). The overall results were used to study the retention mechanisms. The aim of this modeling is a closer knowledge of the form in which (M n+ and/or ML y (n-y)+ ...) each cationic element is extracted into the stationary phase. In fact, while cations can exist in the eluent in various forms depending on the analytical conditions, their forms may be different in the stationary phase. (authors)

  13. 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.

  14. 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

  15. Thin layer chromatography: a simple and reliable technique for the determination of pesticides residue in environmental samples

    International Nuclear Information System (INIS)

    Asi, M.R.; Hussain, A.; Iqbal, Z.; Chaudhary, J.A.

    2000-01-01

    A method for the detection of pesticides by thin-layer chromatography is described. These pesticides on chlorination and treatment with 0-toluidine, yield an intensively colored blue product. Some of the organophosphates and carbonates can be determined at low level (mu g/ g) by this method. The limit of minimum detectable quantity is 10-100 ng. (author)

  16. Study of electron-molecule collisions via the finite-element method and R-matrix propagation technique: Model exchange

    International Nuclear Information System (INIS)

    Abdolsalami, F.; Abdolsalami, M.; Gomez, P.

    1994-01-01

    We have applied the finite-element method to electron-molecule collisions. All the calculations are done in the body frame within the fixed-nuclei approximation. A model potential, which is added to the static and polarization potential, has been used to represent the exchange effect. The method is applied to electron-H 2 scattering and the eigenphase sums and the cross sections obtained are in very good agreement with the corresponding results from the linear-algebraic approach. Finite-element calculations of the R matrix in the region where the static and exchange interactions are strong, however, has about one-half to one-fourth of the memory requirement of the linear-algebraic technique

  17. Determination of metallic elements in water by the combined preconcentration techniques of ion exchange and atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Paula, M.H. de.

    1981-01-01

    Having as an aim the utilization of atomic absorption method with flame's excitement, the limits of detection in water of six metals (Ag, Co, Cr, Cu, Ni, Zn) were determined in synthetical samples through atomic absorption spectroscopy. Techniques to optimize the data have been pointed out and presented their statistical treatment. By means of the routine and the addition methods three 'real' samples have also been analysed in order to determine the contents of Cu and Zn. Aiming a pre-concentration and by utilizing the 60 Co obtained activating a sample of cobalt in the CDTN/NUCLEBRAS TRIGA MARK-I reactor, the retainement of this cobalt in ion exchange resin and the variation of the factor of elution within different concentration of HCl in water have been determined. The limits of detection are presented and so are the quantitative ones, with and without pre-concentration in an ion exchanger resin and latter elution. (Author) [pt

  18. Chromatography of actinides on anion-exchange paper, behaviour of the elements U, Np Pu Am in acid, aqueous and alcohol-water solutions

    International Nuclear Information System (INIS)

    Collin, Michel

    1969-01-01

    A preliminary study of actinide migration on ion exchange paper has been carried out on trace amounts with a view to subsequent application in micro-analysis. The first tests have made it possible to define the factors having an effect on the migrational velocities of aqueous and alcohol-water solutions of HCl and HNO 3 . The behaviour, of actinides has then been studied in non-saline acid solutions. The results obtained for each element separately are interesting from the point of view of their mutual separation. This analytical technique has finally been applied successfully to the migration of 300 μg of uranium deposited from a 1 ml volume of solution. (author) [fr

  19. Optimization of fuel exchange machine operation for boiling water reactors using an artificial intelligence technique

    International Nuclear Information System (INIS)

    Sekimizu, K.; Araki, T.; Tatemichi, S.I.

    1987-01-01

    Optimization of fuel assembly exchange machine movements during periodic refueling outage is discussed. The fuel assembly movements during a fuel shuffling were examined, and it was found that the fuel assembly movements consist of two different movement sequences;one is the ''PATH,'' which begins at a discharged fuel assembly and terminates at a fresh fuel assembly, and the other is the ''LOOP,'' where fuel assemblies circulate in the core. It is also shown that fuel-loading patterns during the fuel shuffling can be expressed by the state of each PATH, which is the number of elements already accomplished in the PATH actions. Based on this fact, a scheme to determine a fuel assembly movement sequence within the constraint was formulated using the artificial intelligence language PROLOG. An additional merit to the scheme is that it can simultaneously evaluate fuel assembly movement, due to the control rods and local power range monitor exchange, in addition to normal fuel shuffling. Fuel assembly movements, for fuel shuffling in a 540-MW(electric) boiling water reactor power plant, were calculated by this scheme. It is also shown that the true optimization to minimize the fuel exchange machine movements would be costly to obtain due to the number of alternatives that would need to be evaluated. However, a method to obtain a quasi-optimum solution is suggested

  20. Chemical or electrochemical techniques, followed by ion exchange, for recycle of textile dye wastewater.

    Science.gov (United States)

    Raghu, S; Ahmed Basha, C

    2007-10-22

    This paper examines the use of chemical or electrocoagulation treatment process followed by ion-exchange process of the textile dye effluent. The dye effluent was treated using polymeric coagulant (cationic dye-fixing agent) or electrocoagulation (iron and aluminum electrode) process under various conditions such as various current densities and effect of pH. Efficiencies of COD reduction, colour removal and power consumption were studied for each process. The chemical or electrochemical treatment are indented primarily to remove colour and COD of wastewater while ion exchange is used to further improve the removal efficiency of the colour, COD, Fe concentration, conductivity, alkalinity and total dissolved solids (TDS). From the results chemical coagulation, maximum COD reduction of about 81.3% was obtained at 300 mg/l of coagulant whereas in electrocoagulation process, maximum COD removal of about 92.31% (0.25 A/dm2) was achieved with energy consumption of about 19.29 k Wh/kg of COD and 80% (1A/dm(2)) COD removal was obtained with energy consumption of about 130.095 k Wh/kg of COD at iron and aluminum electrodes, respectively. All the experimental results, throughout the present study, have indicated that chemical or electrocoagulation treatment followed by ion-exchange methods were very effective and were capable of elevating quality of the treated wastewater effluent to the reuse standard of the textile industry.

  1. Determination of lysergic acid diethylamide (LSD) in mouse blood by capillary electrophoresis/ fluorescence spectroscopy with sweeping techniques in micellar electrokinetic chromatography.

    Science.gov (United States)

    Fang, Ching; Liu, Ju-Tsung; Chou, Shiu-Huey; Lin, Cheng-Huang

    2003-03-01

    The separation and on-line concentration of lysergic acid diethylamide (LSD) in mouse blood was achieved by means of capillary electrophoresis/fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as the surfactant. Techniques involving on-line sample concentration, including sweeping micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were applied; the optimum on-line concentration and separation conditions were determined. In the analysis of an actual sample, LSD was found in a blood sample from a test mouse (0.1 mg LSD fed to a 20 g mouse; approximately 1/10 to the value of LD(50)). As a result, 120 and 30 ng/mL of LSD was detected at 20 and 60 min, respectively, after ingestion of the doses.

  2. On-line identification of lysergic acid diethylamide (LSD) in tablets using a combination of a sweeping technique and micellar electrokinetic chromatography/77 K fluorescence spectroscopy.

    Science.gov (United States)

    Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

    2003-03-01

    This work describes a novel method for the accurate determination of lysergic acid diethylamide (LSD) in tablets. A technique involving sweeping-micellar electrokinetic chromatography (MEKC) was used for the initial on-line concentration and separation, after which a cryogenic molecular fluorescence experiment was performed at 77 K. Using this approach, not only the separation of LSD from the tablet extract was achieved, but on-line spectra were readily distinguishable and could be unambiguously assigned. The results are in agreement with analyses by gas chromatography-mass spectrometry (GC-MS). Thus, this method, which was found to be accurate, sensitive and rapid, has the potential for use as a reliable complementary method to GC-MS in such analyses.

  3. The tritium labelling of ibuprofen by heterogeneous catalytic exchange

    International Nuclear Information System (INIS)

    Santamaria, J.; Rebollo, D.V.; Rivera, P.; Estaban, M.

    1986-01-01

    The tritium labelling of 2-(4-isobutylphenyl) propionic acid (ibuprofen) was performed. The method employed was heterogeneous catalytic exchange between ibuprofen and tritiated water. Prior to labelling, thermic stability of ibuprofen was studied. Purification was accomplished through thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Concentration, purity and specific activity of the labelled compound were determined by ultraviolet, HPLC and liquid scintillation techniques. (author)

  4. The development of RFT technique for carbon steel tubes in balance-of-plant heat exchangers

    International Nuclear Information System (INIS)

    Kim, Chang Soo; Kim, Han Jong; Moon, Yong Sick; Kim, Jae Dong; Kim, Wang Bae; Nam, Min Woo

    2005-01-01

    The NDT method of carbon steel tubes is applied RFT technique. As other NDT methods, It is surprising that RFT has been rapidly developed over the past decade. These improvements have resulted in multi-frequency system, dual driver probes and development of analysis technique. Also these improvements give some profit to power plants as well as general industry. Therefore, the purpose of this study is to improve the reliability of RFT technique for carbon steel tubes. To uplift RFT technique, probes, calibration standards and specimen was developed.

  5. Proton Exchange Membrane Fuel Cell Modelling Using Moving Least Squares Technique

    Directory of Open Access Journals (Sweden)

    Radu Tirnovan

    2009-07-01

    Full Text Available Proton exchange membrane fuel cell, with low polluting emissions, is a great alternative to replace the traditional electrical power sources for automotive applications or for small stationary consumers. This paper presents a numerical method, for the fuel cell modelling, based on moving least squares (MLS. Experimental data have been used for developing an approximated model of the PEMFC function of the current density, air inlet pressure and operating temperature of the fuel cell. The method can be applied for modelling others fuel cell sub-systems, such as the compressor. The method can be used for off-line or on-line identification of the PEMFC stack.

  6. Carbon dioxide exchange in subarctic ecosystems measured by a micrometeorological technique

    International Nuclear Information System (INIS)

    Aurela, M.

    2005-01-01

    The atmospheric CO 2 concentration and the surface air temperatures have increased since the pre-industrial era, and the increase in both is predicted to continue during the 21st century. The feedback mechanisms between the changing climate and the carbon cycle are complex, and more information is needed about carbon exchange in different ecosystems. Northern Finland lies in the transition zone between boreal forest and tundra where the ecosystems are especially sensitive to any changes in the climate. In 1995-2004, micrometeorological eddy covariance measurements were conducted to yield continuous data on the CO 2 exchange between the atmosphere and the biosphere in northern Finland on four different ecosystems: an aapa mire, a mountain birch forest, a Scots pine forest and a Norway spruce forest. A measurement system enabling year-round measurements in the harsh subarctic conditions was developed and shown to be suitable for long-term exchange studies. A comparison of the CO 2 flux components, photosynthesis and respiration, at different ecosystems in the European subarctic and arctic regions showed that the leaf area index (LAI) is the key determinant of the gross photosynthetic rates, explaining greatest part of the variation between these ecosystems. Respiration did not show such a strong correlation with LAI, but in general, high respiration rates were related to high values of LAI. The first continuous round-the-year measurements of net ecosystem CO 2 exchange on a subarctic wetland were conducted at Kaamanen. The winter-time CO 2 efflux (of about 90 g CO 2 m -2 yr -1 ) was shown to constitute an essential part of the annual CO 2 balance (of -79 g CO 2 m -2 yr -1 in 1997-2002). The annual CO 2 balances at all sites in northern Finland were relatively small compared with those in lower latitudes. The interannual variation of the CO 2 balance at Kaamanen was marked (-15 to -195 g CO 2 m -2 yr -1 ) during the years 1997-2002. The most important factor

  7. NMR characterization of segmental dynamics in poly(alkyl methacrylate) using CODEX and PUREX exchange techniques

    International Nuclear Information System (INIS)

    Becker-Guedes, Fabio; Azevedo, Eduardo R. de; Bonagamba, Tito J.; Schmidt-Rohr, Klaus

    2001-01-01

    Slow side group dynamics in a series of five poly(alkyl methacrylate)s with varying side group sizes (PMAA, PMMA, PEMA, PiBMA, and PcHMA, with -H, -CH 3 , -CH 2 CH 3 , -CH 2 CH(CH 3 ) 2 , and -cyclohexyl alkyl substituents, respectively) have been studied quantitatively by center band-only detection of exchange (CODEX) and pure exchange (PUREX) 13 C solid-state nuclear magnetic resonance (NMR). Flips and small-angle motions of the ester groups associated with the β-relaxation are observed distinctly, and the fraction of slowly flipping groups has been measured with 3% precision. In PMMA, 34% of side groups flip, while the fraction is 31% in PEMA at 25 C. Even the large isobutyl ether and cyclohexylester side groups can flip in the glassy state, although the flipping fraction is reduced to 22% and ∼10%, respectively. In poly methacrylic acid, no slow side group flips are detected. In PMMA, the flipping fraction is temperature-independent between 25 C and 80 C, while in Pemal it increases continuously from 31 to 60% between 25 C and 60 C. A similar doubling is also observed in Pi BMA. (author)

  8. Developing a technique to enhance durability of fibrous ion-exchange resin substrate for space greenhouses

    Science.gov (United States)

    Krivobok, A. S.; Berkovich, Yu. A.; Shcherbakova, V. A.; Chuvilskaya, N. A.

    2018-02-01

    One way to cut consumables for space plant growth facilities (PGF) with artificial soil in the form of fibrous ion-exchange resin substrate (FIERS) is on-board regeneration of the used medium. After crop harvest the procedure includes removal of the roots from the fibrous media with preservation of the exchanger properties and capillary structure. One type of FIERS, namely BIONA-V3ۛ, has been used in Russian prototypes of space conveyors. We describe a two-stage treatment of BIONA-V3ۛ including primary microwave heating of the used FIERS until (90 ± 5) °C in alkali-peroxide solution during 3.5 hrs. The second stage of the treatment is decomposition of root vestiges inside pores of BIONA-V3ۛ by using thermophilic and mesophilic anaerobic bacteria Clostridium thermocellum, Clostridium cellulolyticum and Cellulosilyticum lentocellum during 7-10 days at 55 °C. The two-stage procedure allows extraction of 90% dead roots from the FIERS' pores and the preservation of root zone hydro-physical properties. A posterior enrichment of the FIERS by minerals makes BIONA- V3ۛ reusable.

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

    Science.gov (United States)

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

    2017-07-07

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

  10. Development of an analytical method for polycyclic aromatic hydrocarbons in coffee beverages and dark beer using novel high-sensitivity technique of supercritical fluid chromatography/mass spectrometry.

    Science.gov (United States)

    Yoshioka, Toshiaki; Nagatomi, Yasushi; Harayama, Koichi; Bamba, Takeshi

    2018-07-01

    Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic substances that are mainly generated during heating in food; therefore, the European Union (EU) has regulated the amount of benzo[a]pyrene and PAH4 in various types of food. In addition, the Scientific Committee on Food of the EU and the Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives have recommended that 16 PAHs should be monitored. Since coffee beverages and dark beer are roasted during manufacture, monitoring these 16 PAHs is of great importance. On the other hand, supercritical fluid chromatography (SFC) is a separation method that has garnered attention in recent years as a complement for liquid and gas chromatography. Therefore, we developed a rapid high-sensitivity analytical method for the above-mentioned 16 PAHs in coffee beverages and dark beer involving supercritical fluid chromatography/atmospheric pressure chemical ionization-mass spectrometry (SFC/APCI-MS) and simple sample preparation. In this study, we developed a novel analytical technique that increased the sensitivity of MS detection by varying the back-pressure in SFC depending on the elution of PAHs. In addition, analysis of commercially available coffee and dark beer samples in Japan showed that the risk of containing the 16 PAHs may be low. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  11. Supercritical fluid chromatography coupled with tandem mass spectrometry: A high-efficiency detection technique to quantify Taxane drugs in whole-blood samples.

    Science.gov (United States)

    Jin, Chan; Guan, Jibin; Zhang, Dong; Li, Bing; Liu, Hongzhuo; He, Zhonggui

    2017-10-01

    We present a technique to rapid determine taxane in blood samples by supercritical fluid chromatography together with mass spectrometry. The aim of this study was to develop a supercritical fluid chromatography with mass spectrometry method for the analysis of paclitaxel, cabazitaxel, and docetaxel in whole-blood samples of rats. Liquid-dry matrix spot extraction was selected in sample preparation procedure. Supercritical fluid chromatography separation of paclitaxel, cabazitaxel, docetaxel, and glyburide (internal standard) was accomplished within 3 min by using the gradient mobile phase consisted of methanol as the compensation solvent and carbon dioxide at a flow rate of 1.0 mL/min. The method was validated regarding specificity, the lower limit of quantification, repeatability, and reproducibility of quantification, extraction recovery, and matrix effects. The lower limit of quantification was found to be 10 ng/mL since it exhibited acceptable precision and accuracy at the corresponding level. All interday accuracies and precisions were within the accepted criteria of ±15% of the nominal value and within ±20% at the lower limit of quantification, implying that the method was reliable and reproducible. In conclusion, this method is a promising tool to support and improve preclinical or clinical pharmacokinetic studies with the taxanes anticancer drugs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. New separation techniques of cesium by redox type ion exchange materials

    International Nuclear Information System (INIS)

    Tanihara, Koichi

    1998-01-01

    RIECS method, new cesium separation method, was developed in which a porous strong base anionic exchanger with copper ferrocyanide (CuFC) and inhibitor were used. Cesium could be separated from the high concentration nitric solution. By developing new impregnation method, large amount of CuFC was impregnated into the micropolar porous resin and silica gel pores. KFC adhered to outside of pores was recovered. Good complex with CuFC was prepared by use of copper chloride in ethyl alcohol solution. The adsorption ratio of cesium increased radically to 80% level in the very small range of hydrazine concentration 1.7 to 2.4x10 -4 M. The adsorption-desorption ratio of cesium did not decrease by repeating it seven times. The glassificated materials decreased large amount of γ-ray unless increase of volume could be produced by built RIECS method in the high level waste processing system. (S.Y.)

  13. Determination of Ni{sup 2+} using an equilibrium ion exchange technique: Important chemical factors and applicability to environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Worms, Isabelle A.M. [CABE - Analytical and Biophysical Environmental Chemistry, University of Geneva, 30 quai Ernest Ansermet 1211 Geneva 4 (Switzerland); Wilkinson, Kevin J. [Department of Chemistry, University of Montreal C.P. 6128, succursale Centre-ville Montreal, H3C 3J7 (Canada)], E-mail: KJ.Wilkinson@umontreal.ca

    2008-05-26

    In natural waters, the determination of free metal concentrations is a key parameter for studying bioavailability. Unfortunately, few analytical tools are available for determining Ni speciation at the low concentrations found in natural waters. In this paper, an ion exchange technique (IET) that employs a Dowex resin is evaluated for its applicability to measure [Ni{sup 2+}] in freshwaters. The presence of major cations (e.g. Na, Ca and Mg) reduced both the times that were required for equilibration and the partition coefficient to the resin ({lambda}{sup '}{sub Ni}). IET measurements of [Ni{sup 2+}] in the presence of known ligands (citrate, diglycolate, sulfoxine, oxine and diethyldithiocarbamate) were verified by thermodynamic speciation models (MINEQL{sup +} and VisualMINTEQ). Results indicated that the presence of hydrophobic complexes (e.g. Ni(DDC){sub 2}{sup 0}) lead to an overestimation of the Ni{sup 2+} fraction. On the other hand, [Ni{sup 2+}] measurements that were made in the presence of amphiphilic complexes formed with humic substances (standard aquatic humic acid (SRHA) and standard aquatic fulvic acid (SRFA)) were well correlated to free ion concentrations that were calculated using a NICA-DONNAN model. An analytical method is also presented here to reduce the complexity of the calibration (due to the presence of many other cations) for the use of Dowex equilibrium ion exchange technique in natural waters.

  14. New force replica exchange method and protein folding pathways probed by force-clamp technique.

    Science.gov (United States)

    Kouza, Maksim; Hu, Chin-Kun; Li, Mai Suan

    2008-01-28

    We have developed a new extended replica exchange method to study thermodynamics of a system in the presence of external force. Our idea is based on the exchange between different force replicas to accelerate the equilibrium process. This new approach was applied to obtain the force-temperature phase diagram and other thermodynamical quantities of the three-domain ubiquitin. Using the C(alpha)-Go model and the Langevin dynamics, we have shown that the refolding pathways of single ubiquitin depend on which terminus is fixed. If the N end is fixed then the folding pathways are different compared to the case when both termini are free, but fixing the C terminal does not change them. Surprisingly, we have found that the anchoring terminal does not affect the pathways of individual secondary structures of three-domain ubiquitin, indicating the important role of the multidomain construction. Therefore, force-clamp experiments, in which one end of a protein is kept fixed, can probe the refolding pathways of a single free-end ubiquitin if one uses either the polyubiquitin or a single domain with the C terminus anchored. However, it is shown that anchoring one end does not affect refolding pathways of the titin domain I27, and the force-clamp spectroscopy is always capable to predict folding sequencing of this protein. We have obtained the reasonable estimate for unfolding barrier of ubiquitin, using the microscopic theory for the dependence of unfolding time on the external force. The linkage between residue Lys48 and the C terminal of ubiquitin is found to have the dramatic effect on the location of the transition state along the end-to-end distance reaction coordinate, but the multidomain construction leaves the transition state almost unchanged. We have found that the maximum force in the force-extension profile from constant velocity force pulling simulations depends on temperature nonlinearly. However, for some narrow temperature interval this dependence becomes

  15. Column Liquid Chromatography.

    Science.gov (United States)

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  16. The high pressure liquid chromatography and its application to the separation of polynuclear aromatic hydrocarbons in atmospheric dust and burning residues

    International Nuclear Information System (INIS)

    Lopez, M.-C.

    1975-09-01

    A new technique of analysis is described: the high speed liquid chromatography or more exactly the high performance liquid chromatography because of the progress achieved on the new packings of the columns. The main types of chromatography, according to the phenomena involved are described: adsorption, partition, ion-exchange and exclusion chromatography. A brief outline is given of the theory for determination of stationary and mobile phases in order to obtain the optimum conditions of separation. Some exemples of possible applications are given, particularly the use of this technique for the separation of polycyclic aromatic hydrocarbons in atmospheric pollution and burning residues [fr

  17. Validation of an extraction paper chromatography (EPC) technique for estimation of trace levels of 90Sr in 90Y solutions obtained from 90Sr/90Y generator systems

    International Nuclear Information System (INIS)

    Usha Pandey; Yogendra Kumar; Ashutosh Dash

    2014-01-01

    While the extraction paper chromatography (EPC) technique constitutes a novel paradigm for the determination of few Becquerels of 90 Sr in MBq quantities of 90 Y obtained from 90 Sr/ 90 Y generator, validation of the technique is essential to ensure its usefulness as a real time analytical tool. With a view to explore the relevance and applicability of EPC technique as a real time quality control (QC) technique for the routine estimation of 90 Sr content in generator produced 90 Y, a systematic validation study was carried out diligently not only to establish its worthiness but also to broaden its horizon. The ability of the EPC technique to separate trace amounts of Sr 2+ in the presence of large amounts of Y 3+ was verified. The specificity of the technique for Y 3+ was demonstrated with 90 Y obtained by neutron irradiation. The method was validated under real experimental conditions and compared with a QC method described in US Pharmacopeia for detection of 90 Sr levels in 90 Y radiopharmaceuticals. (author)

  18. The tritium labeling of Butibufen by heterogeneous catalytic exchange

    International Nuclear Information System (INIS)

    Santamaria, J.; Rebollo, D.

    1986-01-01

    The labeling of a new non-steroidal antiinflammatory agent, Butibufen (2-(4-isobutylphenyl) butyric acid) was studied. The method used was heterogeneous catalytic exchange between Butibufen and tritiated water, obtained in situ. Purification was accomplished through thin layer chromatography. Concentration, purity and specific activity of the labeled drug were determined by ultraviolet and liquid scintillation techniques. (Author) 7 refs

  19. Use of variance techniques to measure dry air-surface exchange rates

    Science.gov (United States)

    Wesely, M. L.

    1988-07-01

    The variances of fluctuations of scalar quantities can be measured and interpreted to yield indirect estimates of their vertical fluxes in the atmospheric surface layer. Strong correlations among scalar fluctuations indicate a similarity of transfer mechanisms, which is utilized in some of the variance techniques. The ratios of the standard deviations of two scalar quantities, for example, can be used to estimate the flux of one if the flux of the other is measured, without knowledge of atmospheric stability. This is akin to a modified Bowen ratio approach. Other methods such as the normalized standard-deviation technique and the correlation-coefficient technique can be utilized effectively if atmospheric stability is evaluated and certain semi-empirical functions are known. In these cases, iterative calculations involving measured variances of fluctuations of temperature and vertical wind velocity can be used in place of direct flux measurements. For a chemical sensor whose output is contaminated by non-atmospheric noise, covariances with fluctuations of scalar quantities measured with a very good signal-to-noise ratio can be used to extract the needed standard deviation. Field measurements have shown that many of these approaches are successful for gases such as ozone and sulfur dioxide, as well as for temperature and water vapor, and could be extended to other trace substances. In humid areas, it appears that water vapor fluctuations often have a higher degree of correlation to fluctuations of other trace gases than do temperature fluctuations; this makes water vapor a more reliable companion or “reference” scalar. These techniques provide some reliable research approaches but, for routine or operational measurement, they are limited by the need for fast-response sensors. Also, all variance approaches require some independent means to estimate the direction of the flux.

  20. Study of electron-molecule collision via finite-element method and r-matrix propagation technique: Exact exchange

    International Nuclear Information System (INIS)

    Abdolsalami, F.; Abdolsalami, M.; Perez, L.; Gomez, P.

    1995-01-01

    The authors have applied the finite-element method to electron-molecule collision with the exchange effect implemented rigorously. All the calculations are done in the body-frame within the fixed-nuclei approximation, where the exact treatment of exchange as a nonlocal effect results in a set of coupled integro-differential equations. The method is applied to e-H 2 and e-N 2 scatterings and the cross sections obtained are in very good agreement with the corresponding results the authors have generated from the linear-algebraic approach. This confirms the significant difference observed between their results generated by linear-algebraic method and the previously published e-N 2 cross sections. Their studies show that the finite-element method is clearly superior to the linear-algebraic approach in both memory usage and CPU time especially for large systems such as e-N 2 . The system coefficient matrix obtained from the finite-element method is often sparse and smaller in size by a factor of 12 to 16, compared to the linear-algebraic technique. Moreover, the CPU time required to obtain stable results with the finite-element method is significantly smaller than the linear-algebraic approach for one incident electron energy. The usage of computer resources in the finite-element method can even be reduced much further when (1) scattering calculations involving multiple electron energies are performed in one computer run and (2) exchange, which is a short range effect, is approximated by a sparse matrix. 17 refs., 7 figs., 5 tabs

  1. Development of the gas puff charge exchange recombination spectroscopy (GP-CXRS) technique for ion measurements in the plasma edge

    International Nuclear Information System (INIS)

    Churchill, R. M.; Theiler, C.; Lipschultz, B.; Dux, R.; Pütterich, T.; Viezzer, E.

    2013-01-01

    A novel charge-exchange recombination spectroscopy (CXRS) diagnostic method is presented, which uses a simple thermal gas puff for its donor neutral source, instead of the typical high-energy neutral beam. This diagnostic, named gas puff CXRS (GP-CXRS), is used to measure ion density, velocity, and temperature in the tokamak edge/pedestal region with excellent signal-background ratios, and has a number of advantages to conventional beam-based CXRS systems. Here we develop the physics basis for GP-CXRS, including the neutral transport, the charge-exchange process at low energies, and effects of energy-dependent rate coefficients on the measurements. The GP-CXRS hardware setup is described on two separate tokamaks, Alcator C-Mod and ASDEX Upgrade. Measured spectra and profiles are also presented. Profile comparisons of GP-CXRS and a beam based CXRS system show good agreement. Emphasis is given throughout to describing guiding principles for users interested in applying the GP-CXRS diagnostic technique

  2. Development of the gas puff charge exchange recombination spectroscopy (GP-CXRS) technique for ion measurements in the plasma edge

    Energy Technology Data Exchange (ETDEWEB)

    Churchill, R. M.; Theiler, C.; Lipschultz, B. [MIT Plasma Science and Fusion Center, Cambridge, Massachusetts 02139 (United States); Dux, R.; Pütterich, T.; Viezzer, E. [Max-Planck-Institut für Plasmaphysik, EURATOM Association, Boltzmannstrasse 2, D-85748 Garching (Germany); Collaboration: Alcator C-Mod Team; ASDEX Upgrade Team

    2013-09-15

    A novel charge-exchange recombination spectroscopy (CXRS) diagnostic method is presented, which uses a simple thermal gas puff for its donor neutral source, instead of the typical high-energy neutral beam. This diagnostic, named gas puff CXRS (GP-CXRS), is used to measure ion density, velocity, and temperature in the tokamak edge/pedestal region with excellent signal-background ratios, and has a number of advantages to conventional beam-based CXRS systems. Here we develop the physics basis for GP-CXRS, including the neutral transport, the charge-exchange process at low energies, and effects of energy-dependent rate coefficients on the measurements. The GP-CXRS hardware setup is described on two separate tokamaks, Alcator C-Mod and ASDEX Upgrade. Measured spectra and profiles are also presented. Profile comparisons of GP-CXRS and a beam based CXRS system show good agreement. Emphasis is given throughout to describing guiding principles for users interested in applying the GP-CXRS diagnostic technique.

  3. Gas chromatography in space

    Science.gov (United States)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  4. A critical evaluation of multistage equilibration technique for preconcentration by ion-exchange

    International Nuclear Information System (INIS)

    Iyer, R.K.

    1994-01-01

    Capabilities of the method of preconcentration of heavy metal ions from aqueous samples by Chelex 100 using a successive equilibration technique has been evaluated. The process of successive equilibrations may be looked upon in one of the two ways: one of equilibrating a given amount of resin with n successive aliquots so that sample size increases n-fold. Alternatively one may consider this as dividing a large-sized sample into n equal aliquots and carrying out the equilibrations with a smaller amount of resin maintaining the v/m ratio. Expressions have been derived for overall recovery, percentage recovery and decontamination factor for the successive equilibration technique. The validity of the expressions has been checked with experimental data. The values for recovery and decontamination factor have been compared with those for a single equilibration using the whole sample. Finally the factors which affect the value of recovery have been examined and their effect on the recovery has been evaluated. (author). 12 refs., 4 tabs., 1 appendix

  5. Hybrid IgG4/IgG4 Fc antibodies form upon 'Fab-arm' exchange as demonstrated by SDS-PAGE or size-exclusion chromatography

    NARCIS (Netherlands)

    Rispens, Theo; den Bleker, Tamara H.; Aalberse, Rob C.

    2010-01-01

    Human IgG4 antibodies are dynamic molecules that in vivo exchange half-molecules to become bispecific antibodies. Here we show that IgG4 antibodies and IgG4 Fc fragments similarly exchange resulting in hybrid antibodies (a single Fab + Fc) with a molecular weight of ca. 100 kDa. These antibodies can

  6. Ion exchange chromatography on a new form of tin dioxide for the isolation of strontium radioisotopes from fission products: an application to milk samples

    International Nuclear Information System (INIS)

    Stella, R.; Valentini, M.T.G.; Maggi, L.

    1990-01-01

    An amorphous, partially-reduced tin dioxide, having properties of an inorganic exchanger, was tested for application to fission product separations. Due to the good sorption of both strontium and barium the application of the exchanger to radiostrontium isolation from fission product mixtures is subjected to important restrictions. An application to 90 Sr determination in milk is proposed. (author)

  7. An investigation of flow and resistance characteristics of heat exchanger with the 2-D LDV system and visualization technique

    International Nuclear Information System (INIS)

    Wang Zongsen; Shen Xiong; Xu Yuanhui; Bi Shuxun

    1987-12-01

    An experimental study of the heat exchanger which would be used in a nuclear reactor for low temperature heat-supplying is presented. A 2-D Laser Doppler Velocimeter was used as a unique technique to measure the mean velocity and turbulence intensity distributions in different sections of the model. The relationship between the resistance coefficient and Reynolds number also obtained in terms of the total pressure rakes covered by the casings and the wall static pressure pick-up holes. The flow visualization has realized by using a piece of light source with an Argon-Ion laser. It is apparent that the polystyrene particles seeded in the flow can trace the mean flow. The results showed that the self-similar phenomenon exists in the tube bundle flow system. There are some secondary vortices in the cross sections between two passages of the model

  8. Separation and sampling technique of light element isotopes by chemical exchange process

    International Nuclear Information System (INIS)

    Kato, Shunsaku; Oi, Kenta; Takagi, Norio; Hirotsu, Takafumi; Kano, Hirofumi; Sonoda, Akinari; Makita, Yoji

    2000-01-01

    Lithium and boron isotope separation technique were studied. Granulation of lithium isotope separation agent was carried out by cure covering in solution. Separation of lithium isotope was stepped up by ammonium carbonate used as elusion agent. Styrene and ester resin derived three kinds of agents such as 2-amino-1, 3-propanediol (1, 3-PD), 2-amino-2-methyl-1, 3-propanediol (Me-1,3-PD) and tris(2-hydroxyethyl)amine (Tris) were used as absorbent.The ester resin with Tris showed larger amount of adsorption (1.4 mmol/g) than other resins. However, all resins with agent indicated more large adsorption volume of boron than the objective value (0.5 mmol/g). Large isotope shift was shown by the unsymmetrical vibration mode of lithium ion on the basis of quantum chemical calculation of isotope effect on dehydration of hydrated lithium ion. (S.Y.)

  9. Field test of radioactive high efficiency filter and filter exchange techniques of fuel cycle examination facility

    International Nuclear Information System (INIS)

    Hwang, Yong Hwa; Lee, Hyung Kwon; Chun, Young Bum; Park, Dae Gyu; Ahn, Sang Bok; Chu, Yong Sun; Kim, Eun Ka.

    1997-12-01

    The development of high efficiency filter was started to protect human beings from the contamination of radioactive particles, toxic gases and bacillus, and its gradual performance increment led to the fabrication of Ultra Low Penetration Air Filter (ULPA) today. The application field of ULPA has been spread not only to the air conditioning of nuclear power facilities, semiconductor industries, life science, optics, medical care and general facilities but also to the core of ultra-precision facilities. Periodic performance test on the filters is essential to extend its life-time through effective maintenance. Especially, the bank test on HEPA filter of nuclear facilities handling radioactive materials is required for environmental safety. Nowadays, the bank test technology has been reached to the utilization of a minimized portable detecting instruments and the evaluation techniques can provide high confidence in the area of particle distribution and leakage test efficiency. (author). 16 refs., 13 tabs., 14 figs

  10. Information exchange mainly on HTGR operation and maintenance technique between JAEA and INET in 2005

    International Nuclear Information System (INIS)

    Tachibana, Yukio; Hino, Ryutaro; Yu Suyuan

    2006-06-01

    The worldwide interests in the HTGR (High Temperature Gas-cooled Reactor) have been growing because the high temperature heat produced by the reactor can be utilized not only for efficient power generation but also for broad process heat applications, especially for thermo-chemical hydrogen production to fuel a prospective hydrogen economy in future. Presently only two HTGR reactors are operational in the world, including the HTTR (High Temperature Engineering Test Reactor) in Japan Atomic Energy Agency (JAEA) and the HTR-10 in the Institute of Nuclear and New Energy Technology (INET) of Tsinghua University in China. JAEA and INET have cooperated since 1986 in the field of HTGR development, particularly on the HTTR and HTR-10 projects. This report describes the cooperation with emphasis on HTGR operation and maintenance techniques between JAEA and INET and outlines cooperation activities during the fiscal year 2005. (author)

  11. 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.

  12. Development of anion-exchange/reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry methods for the speciation of bio-available iodine and bromine from edible seaweed.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2012-05-04

    Anion exchange high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry has been novelly applied to assess inorganic (iodide and iodate) and organic (3-iodotyrosine - MIT, and 3,5-diiodotyrosine - DIT) iodine species in a single chromatographic run. The optimized operating conditions (Dionex IonPac AS7, gradient elution with 175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase and flow rates within the 0.5-1.5 mL min(-1) range) have also been used to perform inorganic bromine speciation analysis (bromide and bromate). The developed method has been applied for determining the bio-available contents of iodine and bromine species in dialyzates from edible seaweed. Reverse phase high performance liquid chromatography (Zorbax Eclipse XDB-C8, gradient elution with 0.2% (m/m) acetic acid, and 0.2% (m/m) acetic acid in methanol, as mobile phases, and a constant flow rate of 0.75 mL min(-1)) also hyphenated with inductively coupled plasma-mass spectrometry was used to confirm the presence of organic iodine species (MIT and DIT) in the dialyzates. The verification of the presence of iodinated amino acids (MIT and DIT) in the extracts was also performed by reverse phase high performance liquid chromatography-electrospray ionization-mass spectrometry (LTQ Orbitrap). The developed methods have provided good repeatability (RSD values lower than 10% for both anion exchange and reverse phase separations) and analytical recoveries within the 90-105% range for all cases. The in vitro bio-availability method consisted of a simulated gastric and an intestinal digestion/dialysis (10 kDa molecular weight cut-off - MWCO) two-stage procedure. Iodide and MIT were the main bio-available species quantified, whereas bromide was the major bromine species found in the extracts. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. The application of extraction chromatography to the determination of radionuclides in biological and environmental samples

    International Nuclear Information System (INIS)

    Testa, C.; Delle Site, A.

    1976-01-01

    The paper describe the application of extraction chromatography to the determination of several alpha and beta emitters in biological and environmental samples. Both column extraction chromatography and batch extraction process have been used to isolate the radionuclides from the samples. The effect of several parameters (extractant concentration, support granulometry, stirring time, temperature, presence of a complexing agent) on the extraction and elution has been examined. The application of redox extraction chromatography is also described. A very simple and rapid determination of the activity retained on the column can be obtained by transferring the slurry to a counting vial and by adding the scintillation liquid for a direct detection of the α or β emission. The counting efficiencies obtained with this technique are compared with those obtained with ion exchange resins. The organic polymers used for the extraction chromatography give about 100% counting efficiency. The conventional ion exchange resin cannot be used to this purpose because of their strong light absorption. (T.G.)

  14. Evidence for two compartments of exchangeable calcium in isolated rat liver mitochondria obtained using a 45Ca exchange technique in the presence of magnesium, phosphate, and ATPase at 370C

    International Nuclear Information System (INIS)

    Barritt, G.J.

    1981-01-01

    The distribution of calcium between isolated rat liver mitochondria and the extramitochondrial medium at 37 degrees C and in the presence of 2 mM inorganic phosphate, 3 mM ATP, 0.05 or 1.1 mM free magnesium and a calcium buffer, nitrilotriacetic acid, was investigated using a 45 Ca exchange technique. The amounts of 40 Ca in the mitochondria and medium were allowed to reach equilibrium before initiation of the measurement of 45 Ca exchange. At 0.05 mM free magnesium and initial extramitochondrial free calcium concentrations of between 0.15 and 0.5 microM, the mitochondria accumulated calcium until the extramitochondrial free calcium concentration was reduced to 0.15 microM. Control experiments showed that the mitochondria were stable under the incubation conditions employed. The 45 Ca exchange data were found to be consistent with a system in which two compartments of exchangeable calcium are associated with the mitochondria. Changes in the concentration of inorganic phosphate did not significantly affect the 45 Ca exchange curves, whereas an increase in the concentration of free magnesium inhibited exchange. The maximum rate of calcium outflow from the mitochondria was estimated to be 1.7 nmol/min per mg of protein, and the value of K0.5 for intramitochondrial exchangeable calcium to be about 1.6 nmol per mg of protein. Ruthenium Red decreased the fractional transfer rate for calcium inflow to the mitochondria while nupercaine affected principally the fractional transfer rates for the transfer of calcium between the two mitochondrial compartments. The use of the incubation conditions and 45 Ca exchange technique described in this report for studies of the effects of agents which may alter mitochondrial calcium uptake or release (e.g., the pre-treatment of cells with hormones) is briefly discussed

  15. Cleanup and analysis of sugar phosphates in biological extracts by using solid phase extraction and anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Smith, Hans Peter; Cohen, A.; Buttler, T.

    1998-01-01

    of Saccharomyces cerevisiae obtained by using cold methanol as quenching agent and chloroform as extraction solvent. It was shown that pretreatment of the cell extract with SPE markedly improved the quality of the liquid chromatography analysis with recoveries of the sugar phosphates close to 100%. Furthermore...

  16. Probing the mechanism of sister chromatid exchange formation with the fluorescent plus Giemsa technique

    International Nuclear Information System (INIS)

    Yu, L.C.

    1976-01-01

    The effects of x rays and light flashes on the SCE formation in BrdUrd-substituted Chinese hamster ovary (CHO) cells are examined using the fluorescent plus Giemsa (FPG) technique, which allows SCE's to be visualized with greater precision than 3 H autoradiography does. Near-diploid cells are selected and scoring SCE from every chromosome of near-diploid cells or from chromosome no. 1 is found to give a more accurate measure of the SCE induction. Double synchronous cells are used for the x ray study and asynchronous cells are used for the light flash study. The results indicate that x rays can induce SCE's throughout the cell cycle with S the most sensitive stage and G 2 the least sensitive stage. Light flashes can induce an appreciable amount of SCE's while no appreciable amount of chromosomal aberrations can be detected under conditions used in this study. For x-ray-induced chromosomal aberrations, G 2 is the most sensitive stage with G 1 being slightly more sensitive than S, which is consistent with other observations. Additionally, aberration induction is shown to be a more sensitive indicator of x-ray-induced cell damage than SCE induction, but SCE induction is a potentially good indicator of mutation induction. This study also suggests that symmetrically reunited isochromatid breaks can not be the sole source of SCE's and SCE induction is a different but not independent radiobiological effect from chromosomal aberration induction. SCE formation is proposed to be a consequence of specific type(s) of single strand breaks in DNA

  17. Determination of Four Anti-epileptic Drugs in Plasma Using Ultra Performance Liquid Chromatography with Mass Detection Technique.

    Science.gov (United States)

    Hassib, Sonia T; Hashem, Hanaa M A; Mahrouse, Marianne A; Mostafa, Eman A

    2018-04-10

    Status epilepticus (SE) is considered the second most frequent neurologic emergency. Its therapeutic management is performed using sequential anti-epileptic drug regimens. Diazepam (DIA), midazolam (MID), phenytoin (PHT) and phenobarbital (PB) are four drugs of different classes used sequentially in the management of SE. A sensitive, selective, accurate and precise method was developed and validated for simultaneous determination of the four anti-epileptic drugs in human plasma. Their separation and quantification were achieved using ultra performance liquid chromatography (UPLC) with mass detection using carbamazepine as internal standard (IS). For the first three drugs and IS, UPLC-MS/MS with electrospray ionization working in multiple reaction monitoring mode was used at the following transitions: m/z 285→193 for DIA, m/z 326→291 for MID, m/z 253→182 for PHT and m/z 237→194, 237→192 for IS. For the fourth drug (PB), molecular ion peak of PB [M+H] + at m/z 233 was used for its quantitation. The method was linear over concentration ranges of 5-500 ng/ml for DIA and MID and 0.25-20 μg/ml for PHT and PB, respectively. Bio-analytical validation of the developed method was carried out according to European Medicines Agency guidelines. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies. This article is protected by copyright. All rights reserved.

  18. 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.

  19. 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.

  20. Metabolite Analysis of Toosendanin by an Ultra-High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry Technique

    Directory of Open Access Journals (Sweden)

    Na Li

    2013-09-01

    Full Text Available Toosendanin is the major bioactive component of Melia toosendan Sieb. et Zucc., which is traditionally used for treatment of abdominal pain and as an insecticide. Previous studies reported that toosendanin possesses hepatotoxicity, but the mechanism remains unknown. Its bioavailability in rats is low, which indicates the hepatotoxicity might be induced by its metabolites. In this connection, in the current study, we examined the metabolites obtained by incubating toosendanin with human live microsomes, and then six of these metabolites (M1–M6 were identified for the first time by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF/MS. Further analysis on the MS spectra showed M1, M2, and M3 are oxidative products and M6 is a dehydrogenation product, while M4 and M5 are oxidative and dehydrogenation products of toosendanin. Moreover, their possible structures were deduced from the MS/MS spectral features. Quantitative analysis demonstrated that M1-M5 levels rapidly increased and reached a plateau at 30 min, while M6 rapidly reached a maximal level at 20 min and then decreased slowly afterwards. These findings have provided valuable data not only for understanding the metabolic fate of toosendanin in liver microsomes, but also for elucidating the possible molecular mechanism of its hepatotoxicity.

  1. Development of a gas chromatography-mass spectrometry technique to diagnose white snakeroot (Ageratina altissima) poisoning in a cow.

    Science.gov (United States)

    Meyerholtz, Kimberly A; Burcham, Grant N; Miller, Margaret A; Wilson, Christina R; Hooser, Stephen B; Lee, Stephen T

    2011-07-01

    An 8-year-old, crossbred beef cow was referred to the Indiana Animal Disease Diagnostic Laboratory at Purdue University for a complete necropsy in October 2009. The cow was the sixth to die in a 7-day period. Affected cows were reportedly stumbling and became weak, excitable, and recumbent. Histologically, myonecrosis was severe in the skeletal muscles and mild in the heart and tongue. According to the submitter, exposure to a poisonous plant was suspected, and a plant specimen received from this case was identified as white snakeroot (Ageratina altissima). Using the white snakeroot specimen, a gas chromatography-mass spectrometry analytical method for the detection of tremetone and dehydrotremetone (2 components of white snakeroot) was developed. Both tremetone and dehydrotremetone were detected in the plant specimen. Dehydrotremetone was recovered from the liver, while neither component was recovered in the rumen content. In the past, because of the lack of standard reference material, the diagnosis of white snakeroot poisoning was based mainly on history of exposure and the presence of the plant in the rumen. The analytical method described herein can be used to document exposure to tremetone or dehydrotremetone in cases of suspected white snakeroot poisoning when coupled with the appropriate clinical signs and lesions.

  2. Study to prepare 201Tl by irradiation of mercury with protons. Application of extraction chromatography technique in separation of thallium and mercury

    International Nuclear Information System (INIS)

    Fernandes, L.; Silva, C.P.G. da

    1986-01-01

    The extraction chromatography technique was used for the lig and 201 Tl separation. It was used glass columns of 5,0 cm height and 1,0 cm diameter filled with Voltalef powder impregnated with TBP/cyclohexane. By the Voltalef columns solutions of 203 Hg 2+ , 201 Tl 1+ and 20 1Te 3 were separately percolated in a nitric environment of 4 to 8 M concentration and in a hydrochloridric environment of 0,5 to 4 M. The separation of Hg and 201 Tl was obtained by the retention of 201 Tl3 + in the column during the elution of all the Hg with HCl 2 M. The 201 Tl 3+ was eluted from the column after its reduction with a hot hydrazine dichloride solution. (Author) [pt

  3. A novel approach to water polution monitoring by combining ion exchange resin and XRF-scanning technique

    Science.gov (United States)

    Huang, J. J.; Lin, S. C.; Löwemark, L.; Liou, Y. H.; Chang, Q. M.; Chang, T. K.; Wei, K. Y.; Croudace, I. W. C.

    2017-12-01

    Due to the rapid industrial expansion, environments are subject to irregular fluctuations and spatial distributions in pollutant concentrations. This study proposes to use ion exchange resin accompanied with the XRF-scanning technique to monitor environmental pollution. As a passive sampling sorbent, the use of ion exchange resin provides a rapid, low cost and simple method to detect episodic pollution signals with a high spatial sampling density. In order to digest large quantities of samples, the fast and non-destructive Itrax-XRF core scanner has been introduced to assess elemental concentrations in the resin samples. Although the XRF scanning results are often considered as a semi-quantitative measurement due to possible absorption or scattering caused by the physical variabilities of scanned materials, the use of resin can minimize such influences owing to the standarization of the sample matrix. In this study, 17 lab-prepared standard resin samples were scanned with the Itrax-XRF core scanner (at 100 s exposure time with the Mo-tube) and compared with the absolute elemental concentrations. Six elements generally used in pollution studies (Cr, Mn, Ni, Cu, Zn, and Pb) were selected, and their regression lines and correlation coefficients were determined. In addition, 5 standard resin samples were scanned at different exposure time settings (1 s, 5 s, 15 s, 30 s, 100 s) to address the influence of exposure time on the accuracy of the measurements. The results show that within the test range (from few ppm to thousands ppm), the correlation coefficients are higher than 0.97, even at the shortest exposure time (1 s). Furthermore, a pilot field survey with 30 resin samples has been conducted in a potentially polluted farm area in central Taiwan to demonstrate the feasibility of this novel approach. The polluted hot zones could be identified and the properties and sources of wastewater pollution can therefore be traced over large areas for the purposes of

  4. Different Techniques of Respiratory Support Do Not Significantly Affect Gas Exchange during Cardiopulmonary Resuscitation in a Newborn Piglet Model.

    Science.gov (United States)

    Mendler, Marc R; Maurer, Miriam; Hassan, Mohammad A; Huang, Li; Waitz, Markus; Mayer, Benjamin; Hummler, Helmut D

    2015-01-01

    There are no evidence-based recommendations on the use of different techniques of respiratory support and chest compressions (CC) during neonatal cardiopulmonary resuscitation (CPR). We studied the short-term effects of different ventilatory support strategies along with CC representing clinical practice on gas exchange [arterial oxygen saturation (SaO2), arterial partial pressure of oxygen (PaO2) and arterial partial pressure of carbon dioxide (PaCO2)], hemodynamics and cerebral oxygenation. We hypothesized that in newborn piglets with cardiac arrest, use of a T-piece resuscitator (TPR) providing positive end-expiratory pressure (PEEP) improves gas exchange as measured by SaO2 during CPR as compared to using a self-inflating bag (SIB) without PEEP. Furthermore, we explored the effects of a mechanical ventilator without synchrony to CC. Thirty newborn piglets with asystole were randomized into three groups and resuscitated for 20 min [fraction of inspired oxygen (FiO2) = 0.21 for 10 min and 1.0 thereafter]. Group 1 received ventilation using a TPR [peak inspiratory pressure (PIP)/PEEP of 20/5 cm H2O, rate 30/min] with inflations interposed between CC (3:1 ratio). Group 2 received ventilation using a SIB (PIP of 20 cm H2O without PEEP, rate 30/min) with inflations interposed between CC (3:1 ratio). Group 3 received ventilation using a mechanical ventilator (PIP/PEEP of 20/5 cm H2O, rate 30/min). CC were applied with a rate of 120/min without synchrony to inflations. We found no significant differences in SaO2 between the three groups. However, there was a trend toward a higher SaO2 [TPR: 28.0% (22.3-40.0); SIB: 23.7% (13.4-52.3); ventilator: 44.1% (39.2-54.3); median (interquartile range)] and a lower PaCO2 [TPR: 95.6 mm Hg (82.1-113.6); SIB: 100.8 mm Hg (83.0-108.0); ventilator: 74.1 mm Hg (68.5-83.1); median (interquartile range)] in the mechanical ventilator group. We found no significant effect on gas exchange using different respiratory support strategies

  5. Determination of 90Sr in radioactive liquid waste-a comparative study using 'SrCO3 precipitation, extraction chromatography and Cerenkov radiation counting' techniques

    International Nuclear Information System (INIS)

    Mani, A.G.S.; Renganathan, K.; Rao, S.V.S.; Sinha, P.K.

    2007-01-01

    In the wastes generated at nuclear power plants, 90 Sr and 90 Y are responsible for approximately 7% and 38% of the total fission product activity after 1 year and 10 years respectively. Monitoring of the liquid waste produced in nuclear facilities for 90 Sr before and after releasing to the aquatic environment is essential, as it can cause a long term biological hazard due to its chemical similarity with Ca, high fission yield (5.9%) and long radioactive and biological half lives of 28 and 49.3 years respectively. As conventional carbonate precipitation method for 90 Sr- 90 Y estimation is laborious and time consuming, the other methods like extraction chromatography technique using strontium selective crown ether and Cerenkov radiation counting by liquid scintillation analyser (LSA) were also investigated. This paper describe procedures involved in the estimation of strontium in low-level radioactive liquid effluent by using above methods and deals with the comparison of results. Cerenkov radiation counting by LSA has an edge over the other methods in the determination of 90 Sr as it is a simple and rapid technique. Experiences gained in the estimation of 90 Sr in low-level radioactive liquid effluent using Cerenkov radiation counting technique is discussed in detail in this paper. (author)

  6. Safety aspects in a chemical exchange process plant

    International Nuclear Information System (INIS)

    Sharma, B.K.

    2016-01-01

    Based on a chemical exchange process involving solid liquid exchange, studies have been undertaken to enrich 10 B isotope of boron using ion exchange chromatography in which a strong base anion exchange resin in hydroxyl form is equilibrated with boric acid solution in presence of mannitol (a complexing reagent to boric acid) to enhance the acidity and hence the isotopic exchange separation factor for 10 B = 11 B exchange reaction. Using the electrochemical techniques such as pH-metry and conductimetry, the choice of a suitable complexing reagent was made amongst ethylene glycol, propylene glycol, dextrose and mannitol for cost-effective separation of isotopes of boron and monitoring of band movements using these electrochemical techniques. 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. 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. This process is an industrially viable process. The various safety aspects followed during operation of this plant are described in this paper. (author)

  7. Recovery and reuse of hexavalent chromium from aqueous solutions by a hybrid technique of electrodialysis and ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Gayathri, R. [Sengunthar Engineering College, Tiruchengode (India). Dept. of Civil Engineering], e-mail: gay3civil@gmail.com; Senthil Kumar, P. [SSN College of Engineering, Chennai (India). Dept. of Chemical Engineering], E-mail: senthilkumarp@ssn.edu.in

    2010-01-15

    The chrome plating industry is one of the highly polluting industries whose effluent mainly consists of chromium(VI). This compound is highly toxic to aquatic life and human health. The rinse water constituents reflect the chrome plating bath characteristics; generally dead tank wash water contains about 1% of the plating bath concentration. Other metals and metal compounds usually considered as toxic can be precipitated out by suitably adjusting the pH of the wastewaters. However, Cr(VI) is soluble in almost all pH ranges and therefore an efficient treatment is required for the removal and recovery of chromium, and also for the reuse of wastewaters. The present study aims to recover the chromium by a hybrid technique of electrodialysis and ion exchange for the removal and concentration of chromate ions from the effluent. The different modes of operation like batch recirculation process, batch recirculation process with continuous dipping and continuous process were carried out to remove and recover the chromium from the effluent and the percentage reductions of chromium were found to be 98.69%, 99.18% and 100%, respectively. (author)

  8. Recovery and reuse of hexavalent chromium from aqueous solutions by a hybrid technique of electrodialysis and ion exchange

    International Nuclear Information System (INIS)

    Gayathri, R.; Senthil Kumar, P.

    2010-01-01

    The chrome plating industry is one of the highly polluting industries whose effluent mainly consists of chromium(VI). This compound is highly toxic to aquatic life and human health. The rinse water constituents reflect the chrome plating bath characteristics; generally dead tank wash water contains about 1% of the plating bath concentration. Other metals and metal compounds usually considered as toxic can be precipitated out by suitably adjusting the pH of the wastewaters. However, Cr(VI) is soluble in almost all pH ranges and therefore an efficient treatment is required for the removal and recovery of chromium, and also for the reuse of wastewaters. The present study aims to recover the chromium by a hybrid technique of electrodialysis and ion exchange for the removal and concentration of chromate ions from the effluent. The different modes of operation like batch recirculation process, batch recirculation process with continuous dipping and continuous process were carried out to remove and recover the chromium from the effluent and the percentage reductions of chromium were found to be 98.69%, 99.18% and 100%, respectively. (author)

  9. Recovery and reuse of hexavalent chromium from aqueous solutions by a hybrid technique of electrodialysis and ion exchange

    Directory of Open Access Journals (Sweden)

    R. Gayathri

    2010-03-01

    Full Text Available The chrome plating industry is one of the highly polluting industries whose effluent mainly consists of chromium(VI. This compound is highly toxic to aquatic life and human health. The rinse water constituents reflect the chrome plating bath characteristics; generally dead tank wash water contains about 1% of the plating bath concentration. Other metals and metal compounds usually considered as toxic can be precipitated out by suitably adjusting the pH of the wastewaters. However, Cr(VI is soluble in almost all pH ranges and therefore an efficient treatment is required for the removal and recovery of chromium, and also for the reuse of wastewaters. The present study aims to recover the chromium by a hybrid technique of electrodialysis and ion exchange for the removal and concentration of chromate ions from the effluent. The different modes of operation like batch recirculation process, batch recirculation process with continuous dipping and continuous process were carried out to remove and recover the chromium from the effluent and the percentage reductions of chromium were found to be 98.69%, 99.18% and 100%, respectively.

  10. Fabrication of gas diffusion layer based on x-y robotic spraying technique for proton exchange membrane fuel cell application

    International Nuclear Information System (INIS)

    Sitanggang, Ramli; Mohamad, Abu Bakar; Daud, Wan Ramli Wan; Kadhum, Abdul Amir H.; Iyuke, S.E.

    2009-01-01

    The x-y robotic spraying technique developed in the Universiti Kebangsaan Malaysia is capable of fabricating various sizes of thickness and porosity of gas diffusion layer (GDL) used in the proton exchange membrane fuel cell (PEMFC). These parameters are obtained by varying the characteristic spray numbers of the robotic spraying machine. This investigation results were adequately represented with mathematical equations for hydrogen gas distribution in GDL. Volumetric modulus (M) parameter is used to determine the value of current density produced on the electrode of a single cell PEMFC. Thus the M parameter can be employed as indicator for a successful GDL fabrication. GDL type 4 has three variables of layer design that can be optimized to function as gas distributor, gas storage, flooding preventer on GDL surface, to evacuate water from the electrode and to control the electrical conductivity. The gas distribution in GDL was mathematically represented with average error of 15.5%. The M value of GDL type 4 according to the model was 0.22 cm 3 /s and yielded a current density of 750 A/m 2 .

  11. Determination of mycophenolic acid in mest products using mixed mode reversed phase-anion exchange clean-up and liquid chromatography-high-resolution mass spectrometry

    DEFF Research Database (Denmark)

    Sørensen, Louise Marie; Nielsen, Kristian Fog; Jacobsen, Thomas

    2008-01-01

    A method for determination of mycophenolic acid (MPA) in dry-cured ham, fermented sausage and liver pate is described. MPA was extracted from meat with bicarbonate-acetonitrile, further cleaned-up by mixed mode reversed phase-anion exchange and detected using a LC-MS system with electrospray...

  12. Common Hemoglobin Variants in Southern Taiwan and Their Effect on the Determination of HbA1c by Ion-exchange High-performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Chih-Hsun Chu

    2009-07-01

    Conclusion: The existence of Hb variants may result in false HbA1c measurement. The possible presence of spuriously low HbA1c levels or abnormal HPLC chromatograms by using ion-exchange methods should be kept in mind.

  13. Rapid isolation of plutonium in environmental solid samples using sequential injection anion exchange chromatography followed by detection with inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Qiao Jixin, E-mail: jixin.qiao@risoe.d [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Hou Xiaolin; Roos, Per [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Miro, Manuel [Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, Carretera de Valldemossa km. 7.5, E-07122 Palma de Mallorca, Illes Balears (Spain)

    2011-01-31

    This paper reports an automated analytical method for rapid determination of plutonium isotopes ({sup 239}Pu and {sup 240}Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-x4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 10{sup 3} to 10{sup 4}. The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials.

  14. Characterization of oligosaccharides with capillary high performance anion exchange chromatography hyphenated to pulsed amperometric detection and ion trap mass spectrometry : application to the analysis of human lysosomal disorders

    NARCIS (Netherlands)

    Bruggink, Cornelis

    The development of a capillary ion chromatograph is described together with a matching desalter. This desalter made it possible to use on-line a mass spectrometer. The mass spectrometer enables partly to characterize carbohydrates eluting from the anion exchange column. This separation technology is

  15. Application of microscopy technique and high-performance liquid chromatography for quality assessment of the flower bud of Tussilago farfara L. (Kuandonghua)

    Science.gov (United States)

    Li, Da; Liang, Li; Zhang, Jing; Kang, Tingguo

    2015-01-01

    Background: Quality control is one of the bottleneck problems limiting the application and development of traditional Chinese medicine (TCM). In recent years, microscopy and high-performance liquid chromatography (HPLC) techniques have been frequently applied in the quality control of TCM. However, studies combining conventional microscopy and HPLC techniques for the quality control of the flower bud of Tussilago farfara L. (Kuandonghua) have not been reported. Objective: This study was undertaken to evaluate the quality of the flower bud of T. farfara L. and to establish the relationships between the quantity of pollen grains and four main bioactive constituents: tussilagone, chlorogenic acid, rutin and isoquercitrin. Materials and Methods: In this study, microscopic examination was used to quantify microscopic characteristics of the flower bud of T. farfara L., and the chemical components were determined by HPLC. The data were analyzed by Statistical Package for the Social Sciences statistics software. Results: The results of the analysis showed that tussilagone, chlorogenic acid, rutin and isoquercitrin were significantly correlated with the quantity of pollen grains in the flower bud of T. farfara L. There is a positive correlation between them. From these results, it can be deduced that the flower bud of T. farfara L. with a greater quantity of pollen grains should be of better quality. Conclusion: The study showed that the established method can be helpful for evaluating the quality of the flower bud of T. farfara L. based on microscopic characteristic constants and chemical quantitation. PMID:26246737

  16. [Online enrichment ability of restricted-access column coupled with high performance liquid chromatography by column switching technique for benazepril hydrochloride].

    Science.gov (United States)

    Zhang, Xiaohui; Wang, Rong; Xie, Hua; Yin, Qiang; Li, Xiaoyun; Jia, Zhengping; Wu, Xiaoyu; Zhang, Juanhong; Li, Wenbin

    2013-05-01

    The online enrichment ability of the restricted-access media (RAM) column coupled with high performance liquid chromatography by column switching technique for benazepril hydrochloride in plasma was studied. The RAM-HPLC system consisted of an RAM column as enrichment column and a C18 column as analytical column coupled via the column switching technique. The effects of the injection volume on the peak area and the systematic pressure were studied. When the injection volume was less than 100 microL, the peak area increased with the increase of the injection volume. However, when the injection volume was more than 80 microL, the pressure of whole system increased obviously. In order to protect the whole system, 80 microL was chosen as the maximum injection volume. The peak areas of ordinary injection and the large volume injection showed a good linear relationship. The enrichment ability of RAM-HPLC system was satisfactory. The system was successfully used for the separation and detection of the trace benazepril hydrochloride in rat plasma after its administration. The sensitivity of HPLC can be improved by RAM pre-enrichment. It is a simple and economic measurement method.

  17. Determination of aminopolycarboxylic acids at ultra-trace levels by means of online coupling ion exchange chromatography and inductively coupled plasma-mass spectrometry with indirect detection via their Pd2+-complexes

    International Nuclear Information System (INIS)

    Nette, David; Seubert, Andreas

    2015-01-01

    Highlights: • 8 important APCA’s analyzed in one run instead of 3 in the previous method. • Pd 2+ extents the methods applicability to 3 and more dentate amino carboxylic acids. • Separation system optimized for the isocratic determination of important APCA’s. • Thermodynamic stability of APCA–Pd 2+ complexes is higher than for Fe 3+ and In 3+ . • Pd 2+ is kinetically much slower than Fe 3+ and In 3+ and makes the method more rugged. - Abstract: A new indirect IC-ICP-MS method for the determination of aminopolycarboxylic acids in water samples is described. It is based on the addition of an excess of Pd(II) to water samples. The analytes are forced into very strong and negatively charged palladium complexes, separated by ion exchange chromatography and detected by their palladium content, utilizing an on-line coupled ICP-MS. This method is suitable to determine the concentration of 8 aminopolycarboxylic acids (nitrilotriacetic acid (NTA), (2-carboxyethyl) iminodiacetic acid (β-ADA), methylglycinediacetic acid (MGDA), 2-hydroxyethyl) ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA), ethylendiamine tetraacetic acid (EDTA), 1,3-diaminopropane tetraacetic acid (1,3-PDTA) and 1,2-diaminopropane tetraacetic acid (1,2-PDTA) at the ng kg −1 level. The method is faster and easier than the established gas chromatography (GC)-method ISO 16588:2002 [1] and up to two orders of magnitude more sensitive than the ion pair chromatography based method of DIN 38413-8. Analytic performance is superior to ISO 16588:2002 and the comparability is good

  18. Determination of aminopolycarboxylic acids at ultra-trace levels by means of online coupling ion exchange chromatography and inductively coupled plasma-mass spectrometry with indirect detection via their Pd{sup 2+}-complexes

    Energy Technology Data Exchange (ETDEWEB)

    Nette, David; Seubert, Andreas, E-mail: seubert@staff.uni-marburg.de

    2015-07-16

    Highlights: • 8 important APCA’s analyzed in one run instead of 3 in the previous method. • Pd{sup 2+} extents the methods applicability to 3 and more dentate amino carboxylic acids. • Separation system optimized for the isocratic determination of important APCA’s. • Thermodynamic stability of APCA–Pd{sup 2+} complexes is higher than for Fe{sup 3+} and In{sup 3+}. • Pd{sup 2+} is kinetically much slower than Fe{sup 3+} and In{sup 3+} and makes the method more rugged. - Abstract: A new indirect IC-ICP-MS method for the determination of aminopolycarboxylic acids in water samples is described. It is based on the addition of an excess of Pd(II) to water samples. The analytes are forced into very strong and negatively charged palladium complexes, separated by ion exchange chromatography and detected by their palladium content, utilizing an on-line coupled ICP-MS. This method is suitable to determine the concentration of 8 aminopolycarboxylic acids (nitrilotriacetic acid (NTA), (2-carboxyethyl) iminodiacetic acid (β-ADA), methylglycinediacetic acid (MGDA), 2-hydroxyethyl) ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA), ethylendiamine tetraacetic acid (EDTA), 1,3-diaminopropane tetraacetic acid (1,3-PDTA) and 1,2-diaminopropane tetraacetic acid (1,2-PDTA) at the ng kg{sup −1} level. The method is faster and easier than the established gas chromatography (GC)-method ISO 16588:2002 [1] and up to two orders of magnitude more sensitive than the ion pair chromatography based method of DIN 38413-8. Analytic performance is superior to ISO 16588:2002 and the comparability is good.

  19. Determination of glufosinate ammonium and its metabolite (AE F064619 and AE F061517) residues in water by gas chromatography with tandem mass spectrometry after ion exchange cleanup and derivatization.

    Science.gov (United States)

    Royer, A; Beguin, S; Sochor, H; Communal, P Y

    2000-11-01

    An analytical method for the determination of glufosinate ammonium and its principal metabolites, AE F064619 and AE F061517, in water of two different hardnesses (5 and 30 DH, French hardness) has been developed and validated. Samples were spiked at different levels (0. 05 and 0.5 microgram/L) and were purified by column chromatography on ion-exchange resins. After derivatization with glacial acetic acid and trimethylarthoacetate mixture, the derivatives were quantified by using capillary gas chromatography with an ion-trap tandem mass spectrometric detector. Analytical conditions for MS/MS detection were optimized, and the quantification was carried out on the areas of the most representative ions. The limit of quantification was validated at 0.05 microgram/L for each compound. The mean recovery value and the relative standard deviation (n = 20) were 92.0% and 17. 8% for glufosinate ammonium, 90.2% and 15.8% for AE F064619, and 89. 7% and 12.7% for AE F061517.

  20. Peak broadening in paper chromatography and related techniques VI. The efficiency of various kinds of chromatography paper and thin-layer cellulose powder for the separation of amino acids

    NARCIS (Netherlands)

    Ligny, C.L. de; Kok, E.C.M.

    1968-01-01

    The efficiency of several chromatography papers and thin-layer cellulose powders for the separation of amino acids is investigated, using the minimum elution time for a given resolution as the criterion.

  1. 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)

  2. Hydroxylapatite chromatography.

    Science.gov (United States)

    Broadhurst, A V

    2001-05-01

    Hydroxylapatite (also called hydroxyapatite), a form of calcium phosphate, can be used as a matrix for the chromatography of both proteins and nucleic acids. Protocols are provided for both standard low-pressure chromatography of a protein mixture using a hydroxylapatite column prepared in the laboratory, and an HPLC method, applicable to proteins and nucleic acids, that uses a commercially available column. Alternate protocols describe column chromatography using a step gradient or batch binding and step-gradient elution.

  3. A technique for extraction and Thin Layer Chromatography visualization of fecal bile acids applied to neotropical felid scats

    Directory of Open Access Journals (Sweden)

    Ada Virginia Cazón Narvaez

    1999-06-01

    Full Text Available Fecal bile acid patterns have been used successfully to identify scats. Neotropical felid scats are capable of this biochemical identification because they present low concentrations of plant pigments that would interfere in fecal bile acids detection. However, neotropical felid scats have poor quantities of bile acids, so we developed in this work a proper technique for their extraction, visualization and determination. Twenty eighth feces of seven different felid species, collected from Zoological and Wildlife Parks, were dried and pulverized. The procedure for analyzing feces is : Take one g of pulverized feces and shake for 3 hr at room temperature in 20 ml benzene : methanol; filter and evaporate to 5 ml. Spot on TLC plate and develop in toluene :acetic acid:water. Dry and visualize with anisaldehyde. Field collected scats could be identified by the bile acids pattern revealed by this specific technique and ,then, used as a source of information for distribution, density and food habits studies.Los patrones de ácidos biliares fecales han sido utilizados satisfactoriamente para identificar heces. Las heces de félidos neotropicales son propicias para ser identificadas bioquímicamente, ya que contienen baja concentración de pigmentos vegetales que pudieran interferir en la detección de ácidos biliares. Sin embargo los ácidos biliares se encuentran en bajas concentraciones en las heces, por lo cual desarrollamos en este trabajo una técnica apropiada para su extracción, visualización y determinación. Veintiocho heces de diferentes félidos recolectadas de Zoológicos y Estaciones de Fauna Silvestre fueron secadas y pulverizadas. El procedimiento para analizar las heces es : Tomar un gramo de feca pulverizada y agitar en 20 ml de benceno :metanol a temperatura ambiente durante 3 hr ; luego filtrar y evaporar hasta 5 ml. Sembrar en placa de TLC y desarrollar en tolueno :ác. acético :agua. Secar y revelar con anisaldehído. Las heces

  4. Size-exclusion chromatography (HPLC-SEC) technique optimization by simplex method to estimate molecular weight distribution of agave fructans.

    Science.gov (United States)

    Moreno-Vilet, Lorena; Bostyn, Stéphane; Flores-Montaño, Jose-Luis; Camacho-Ruiz, Rosa-María

    2017-12-15

    Agave fructans are increasingly important in food industry and nutrition sciences as a potential ingredient of functional food, thus practical analysis tools to characterize them are needed. In view of the importance of the molecular weight on the functional properties of agave fructans, this study has the purpose to optimize a method to determine their molecular weight distribution by HPLC-SEC for industrial application. The optimization was carried out using a simplex method. The optimum conditions obtained were at column temperature of 61.7°C using tri-distilled water without salt, adjusted pH of 5.4 and a flow rate of 0.36mL/min. The exclusion range is from 1 to 49 of polymerization degree (180-7966Da). This proposed method represents an accurate and fast alternative to standard methods involving multiple-detection or hydrolysis of fructans. The industrial applications of this technique might be for quality control, study of fractionation processes and determination of purity. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Chromatographic Techniques for Rare Earth Elements Analysis

    Science.gov (United States)

    Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

    2017-04-01

    The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

  6. Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

    Science.gov (United States)

    Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2011-01-01

    We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

  7. Nepem-211 ion exchange conductive membrane immobilized tris(2,2´-bipyridyl) ruthenium(II) electrogenerated chemiluminescence flow sensor for high-performance liquid chromatography and its application.

    Science.gov (United States)

    Li, Yongbo; Zhang, Zhujun

    2013-01-01

    We developed a sensitive and robust electrogenerated chemiluminescence (ECL) flow sensor based on Ru(bpy)3(2+) immobilized with a Nepem-211 perfluorinated ion exchange conductance membrane, which has robustness and stability under a wide range of chemical and physical conditions, good electrical conductivity, isotropy and a high exchange capacity for immobilization of Ru(bpy)3(2+). The flow sensor has been used as a post-column detector in high-performance liquid chromatography for determination of erythromycin and clarithromycin in honey and pork, and tricyclic antidepressant drugs in human urine. Under optimal conditions, the linear ranges were 0.03-26 ng/μL and 0.01-1 ng/μL for macrolides and tricyclic antidepressant drugs, respectively. The detection limits were 0.02, 0.01, 0.01, 0.06 and 0.003 ng/μL for erythromycin, clarithromycin, doxepin, amitriptyline and clomipramine, respectively. There is no post-column reagent addition. In addition to the conservation expensive reagents, the experimental setup was simplified. The flow sensor was used for 2 years with high sensitivity and stability. Copyright © 2013 John Wiley & Sons, Ltd.

  8. Long-chain alkylimidazolium ionic liquids, a new class of cationic surfactants coated on ODS columns for anion-exchange chromatography.

    Science.gov (United States)

    Qiu, Hongdeng; Zhang, Qinghua; Chen, Limei; Liu, Xia; Jiang, Shengxiang

    2008-08-01

    Separations of common inorganic anions were carried out on ODS columns coated with two long-chain alkylimidazolium ionic liquids ([C(12)MIm]Br and [C(14)MIm]Br) as new cationic surfactants for ion chromatography. With phthalate buffer solution as the mobile phases and non-suppressed conductivity detection, high column efficiencies and excellent selectivity were obtained in the separation of inorganic anions. Chromatographic parameters are calculated and the results show that the coated column possesses significant potential for the analysis of some inorganic anions such as CH(3)COO(-), IO(3)(-), Cl(-), BrO(3)(-), NO(2)(-), Br(-), NO(3)(-), SO(4)(2-), I(-), BF(4)(-), and SCN(-). The effect of eluent pH values on the separation of anions has been studied on the column coated with [C(12)MIm]Br. The stability of the coated columns was also examined.

  9. Characterization of new materials in chromatography and fuel cell development by modern NMR techniques; Charakterisierung neuer Materialien in der Chromatographie und Brennstoffzellen-Forschung mit Hilfe moderner NMR-Techniken

    Energy Technology Data Exchange (ETDEWEB)

    Schauff, S.

    2007-12-28

    New materials, suitable for the application in reversed phase liquid chromatography and fuel cell membranes, were characterized regarding their structure and dynamic properties using solid-state and suspended-state NMR spectroscopy. Both methods were found to be suitable to study the dynamic behaviour, the first to observe intrinsic mobilities of phosphonic acids, the second to monitor interaction processes taking place in a chromatography-like system. Several phosphonic acids, which are promising materials for high temperature fuel cell membranes, were investigated with respect to proton mobility and transport applying various solid-state NMR methods. In addition, water uptake and its effects on anhydride formation were studied on samples that were equilibrated with saturated salt solutions. For PVPA substantial, reversible anhydride formation was found, while MePA did not show condensation. These results show that the relation between hydrogen bond strength and proton mobility is complex. In particular, this work demonstrates that the application of simple 1D 1H and 2H NMR experiments provides easy access to information about proton/deuteron mobility on short time scales, needed for an identification of materials with high intrinsic proton conductivities. Stationary phases for reversed phase liquid chomatography were characterized by solid-state NMR spectroscopy, and their influence on different analytes was studied using suspendedstate HR-MAS NMR spectroscopy. Suspended-state HR-MAS NMR spectroscopy showed to be suitable to model the separation process of analytes on chromatographic sorbents. For this, the stationary phase was suspended in a solution of analyte dissolved in mobile phase. MePhSucc showed a peak doubling of the CH2 group in presence of monomeric C18 phase, leading to the coexistence of a narrow and a broadened peak. Thus, the dynamic interactions of MePhSucc towards the stationary phase, and under the influence of the mobile phase, could be

  10. Thin-Layer and Paper Chromatography.

    Science.gov (United States)

    Sherma, Joseph; Fried, Bernard

    1984-01-01

    Reviews literature on chromatography examining: books, reviews, student experiments; chromatographic systems, techniques, apparatus; detecting and identification of separated zones; preparative chromatography and radiochromatography; and applications related to specific materials (such as acids, alcohols, amino acids, antibiotics, enzymes, dyes,…

  11. Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

    Science.gov (United States)

    Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

    2014-10-01

    Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Incidence of Neonatal Hyperphenylalaninemia Based on High-performance Liquid Chromatography Confirmatory Technique in Mazandaran Province, Northern Iran (2007–2015

    Directory of Open Access Journals (Sweden)

    Ali Abbaskhanian

    2017-01-01

    Full Text Available Background: Classic phenylketonuria (PKU is a metabolic disorder. The purpose of this study was to assess epidemiological factors of PKU phenotypes in a neonatal screening program for Mazandaran, Iran. Methods: In this descriptive-retrospective study from 2007 to 2015, neonates PKU level was conducted by phenylalanine level based on a biochemical technique by ELISA and then by confirmatory methods high performance liquid chromatography. Results: Of the 407,244 screened newborns (48.7% girls and 51.3% boys, 14 girls and 13 boys were diagnosed definitely from 465 suspicious cases of PKU. The incidence of PKU was 0.66 in 10,000, which was noted in different severity (severe PKU - 1:67,874, mild PKU - 1:45,249, and HPA - 1:33,937. In addition, we did not detect any cases of nonclassic PKU. Conclusions: Although the consanguineous marriage pattern is a major cause of hyperphenylalaninemia (HPA particularly in Iranian, there was no significant difference between groups in this study. Now, screening should be executed for all of the family that they have the familial history of PKU in Iran. According to varies actual of prevalence and incidence rate of PKU reported a real patient and taking PKU with mild PKU and HPA, it is recommended, the will provide the PKU reports based on the severity of the disease.

  13. One-step derivatization and preconcentration microextraction technique for determination of bisphenol A in beverage samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fontana, Ariel R; Muñoz de Toro, Mónica; Altamirano, Jorgelina C

    2011-04-27

    A simple technique based on ultrasound-assisted emulsification microextraction in situ derivatization (USAEME-ISD) is proposed for the one-step derivatization, extraction, and preconcentration of bisphenol A (BPA) in beverage samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. BPA was in situ derivatized with acetic anhydride and simultaneously extracted and preconcentrated by using USAEME. Variables affecting the extraction efficiency of BPA were evaluated. Under optimal experimental conditions, the detection limit (LOD) was 38 ng L(-1) with a relative standard deviation (RSD) value of 11.6%. The linear working range was 100-1250 ng L(-1), and the coefficient of estimation (r(2)) of the calibration curve was ≥0.9971. The robustness of the proposed methodology was probed by developing a recovery study at two concentrations (125 and 500 ng L(-1)) over different beverage samples. This study led to a satisfactory result achieving recoveries of ≥82%, which showed acceptable robustness for determination of nanograms per liter of BPA in samples of food safety interest.

  14. Incidence of Neonatal Hyperphenylalaninemia Based on High-performance Liquid Chromatography Confirmatory Technique in Mazandaran Province, Northern Iran (2007–2015)

    Science.gov (United States)

    Abbaskhanian, Ali; Zamanfar, Daniel; Afshar, Parvaneh; Asadpoor, Einollah; Rouhanizadeh, Hamed; Jafarnia, Ali; Shokzadeh, Mohammad

    2017-01-01

    Background: Classic phenylketonuria (PKU) is a metabolic disorder. The purpose of this study was to assess epidemiological factors of PKU phenotypes in a neonatal screening program for Mazandaran, Iran. Methods: In this descriptive-retrospective study from 2007 to 2015, neonates PKU level was conducted by phenylalanine level based on a biochemical technique by ELISA and then by confirmatory methods high performance liquid chromatography. Results: Of the 407,244 screened newborns (48.7% girls and 51.3% boys), 14 girls and 13 boys were diagnosed definitely from 465 suspicious cases of PKU. The incidence of PKU was 0.66 in 10,000, which was noted in different severity (severe PKU - 1:67,874, mild PKU - 1:45,249, and HPA - 1:33,937). In addition, we did not detect any cases of nonclassic PKU. Conclusions: Although the consanguineous marriage pattern is a major cause of hyperphenylalaninemia (HPA) particularly in Iranian, there was no significant difference between groups in this study. Now, screening should be executed for all of the family that they have the familial history of PKU in Iran. According to varies actual of prevalence and incidence rate of PKU reported a real patient and taking PKU with mild PKU and HPA, it is recommended, the will provide the PKU reports based on the severity of the disease. PMID:29184644

  15. 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

  16. An enzymatic method for the determination of fructans in foods and food products - Comparison of the results by high performance anion exchange chromatography with pulsed amperemetric detection

    DEFF Research Database (Denmark)

    Andersen, Rikke; Sørensen, A.

    1999-01-01

    We report a new and non-equipment demanding method of measuring the content of fructans as well as the contents of free glucose, free fructose and sucrose in foods and food products enzymatically. This method comprises hydrolysis of fructans into D-glucose and D-fructose enzymatically...... effects than the fructanase reported as normally used. The method is tested on ten standard substances and five fructan products, and nine foods and food products are also analysed. The enzymatic measurement of the released sugars is confirmed by measurements done by high performance anion exchange...

  17. Temperature dependence of exchange bias in (NiFe/IrMn)n multilayer films studied through static and dynamic techniques

    Science.gov (United States)

    Adams, Daniel J.; Khanal, Shankar; Khan, Mohammad Asif; Maksymov, Artur; Spinu, Leonard

    2018-05-01

    The in-plane temperature dependence of exchange bias was studied through both dc magnetometry and ferromagnetic resonance spectroscopy in a series of [NiFe/IrMn]n multilayer films, where n is the number of layer repetitions. Major hysteresis loops were recorded in the temperature range of 300 K to 2 K to reveal the effect of temperature on the exchange bias in the static regime while temperature-dependent continuous-wave ferromagnetic resonance for frequencies from 3 to 16 GHz was used to determine the exchange bias dynamically. Strong divergence between the values of exchange bias determined using the two different types of measurements as well as a peak in temperature dependence of the resonance linewidth were observed. These results are explained in terms of the slow-relaxer mechanism.

  18. 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

  19. NON DESTRUCTIVE APPLICATION OF RADIOACTIVE TRACER TECHNIQUE FOR CHARACTERIZATION OF INDUSTRIAL GRADE ANION EXCHANGE RESINS INDION GS-300 AND INDION-860

    Directory of Open Access Journals (Sweden)

    P.U. SINGARE

    2014-02-01

    Full Text Available The paper deals with the application of radio isotopic non-destructive technique in the characterization of two industrial grade anion exchange resins Indion GS-300 and Indion-860. For the characterization of the two resins, 131I and 82Br were used as tracer isotopes to trace the kinetics of iodide and bromide ion-isotopic exchange reactions. It was observed that the values of specific reaction rate (min−1, amount of iodide ion exchanged (mmol, initial rate of iodide ion exchange (mmol/min and log Kd were calculated as 0.328, 0.577, 0.189 and 19.7 respectively for Indion GS-300 resin, which was higher than the respective values of 0.180, 0.386, 0.070 and 17.0 calculated for Indion-860 resins when measured under identical experimental conditions. Also at a constant temperature of 40.0 °C, as the concentration of labeled iodide ion solution increases 0.001 M to 0.004 M, the percentage of iodide ions exchanged increases from 75.16 % to 78.36 % for Indion GS-300 resins, which was higher than the increases from 49.65 % to 52.36 % compared to that obtained for Indion-860 resins. The overall results indicate that under identical experimental conditions, Indion GS-300 resins show superior performance over Indion-860 resins.

  20. Non Destructive Application of Radioactive Tracer Technique for Characterization of Industrial Grade Anion Exchange Resins Indio GS-300 and Indion-860

    International Nuclear Information System (INIS)

    Singare, P. U.

    2014-01-01

    The paper deals with the application of radio isotopic non-destructive technique in the characterization of two industrial grade anion exchange resins Indion GS-300 and Indion-860. For the characterization of the two resins, 131 I and 82 Br were used as tracer isotopes to trace the kinetics of iodide and bromide ion-isotopic exchange reactions. It was observed that the values of specific reaction rate (min -1 ), amount of iodide ion exchanged (mmol), initial rate of iodide ion exchange (mmol/min) and log K d were calculated as 0.328, 0.577, 0.189 and 19.7 respectively for Indion GS-300 resin, which was higher than the respective values of 0.180, 0.386, 0.070 and 17.0 calculated for Indion-860 resins when measured under identical experimental conditions. Also at a constant temperature of 40.0 .deg. C, as the concentration of labeled iodide ion solution increases 0.001 M to 0.004 M, the percentage of iodide ions exchanged increases from 75.16 % to 78.36 % for Indion GS-300 resins, which was higher than the increases from 49.65 % to 52.36 % compared to that obtained for Indion-860 resins. The overall results indicate that under identical experimental conditions, Indion GS-300 resins show superior performance over Indion-860 resins

  1. A Multidimensional System for Phosphopeptide Analysis Using TiO{sub 2} Enrichment and Ion-exchange Chromatography with Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Kun; Yoo, Jisun; Kim, Eunmin; Kim, Jin Young; Kim, Young Hwan; Yoo, Jong Shin [Korea Basic Science Institute, Ochang (Korea, Republic of); Oh, Han Bin [Sogang Univ., Seoul (Korea, Republic of)

    2012-10-15

    Although offline enrichment of phosphorylated peptides is widely used, enrichment for phosphopeptides using TiO{sub 2} is often performed manually, which is labor-intensive and can lead to irreproducible results. To address the problems associated with offline enrichment and to improve the effectiveness of phosphopeptide detection, we developed an automated online enrichment system for phosphopeptide analysis. A standard protein mixture comprising BSA, fetuin, crystalline, α-casein and β-casein, and ovalbumin was assessed using our new system. Our multidimensional system has four main parts: a sample pump, a 20-mm TiO{sub 2}-based column, a weak anion-exchange, and a strong cation-exchange (2:1 WAX:SCX) separation column with LC/MS. Phosphorylated peptides were successfully detected using the TiO{sub 2}-based online system with little interference from nonphosphorylated peptides. Our results confirmed that our online enrichment system is a simple and efficient method for detecting phosphorylated peptides.

  2. Ion-exclusion chromatography with conductimetric detection of aliphatic carboxylic acids on a weakly acidic cation-exchange resin by elution with benzoic acid-beta-cyclodextrin.

    Science.gov (United States)

    Tanaka, Kazuhiko; Mori, Masanobu; Xu, Qun; Helaleh, Murad I H; Ikedo, Mikaru; Taoda, Hiroshi; Hu, Wenzhi; Hasebe, Kiyoshi; Fritz, James S; Haddad, Paul R

    2003-05-16

    In this study, an aqueous solution consisting of benzoic acid with low background conductivity and beta-cyclodextrin (beta-CD) of hydrophilic nature and the inclusion effect to benzoic acid were used as eluent for the ion-exclusion chromatographic separation of aliphatic carboxylic acids with different pKa values and hydrophobicity on a polymethacrylate-based weakly acidic cation-exchange resin in the H+ form. With increasing concentration of beta-cyclodextrin in the eluent, the retention times of the carboxylic acids decreased due to the increased hydrophilicity of the polymethacrylate-based cation-exchange resin surface from the adsorption of OH groups of beta-cyclodextrin. Moreover, the eluent background conductivity decreased with increasing concentration of beta-cyclodextrin in 1 mM benzoic acid, which could result in higher sensitivity for conductimetric detection. The ion-exclusion chromatographic separation of carboxylic acids with high resolution and sensitivity was accomplished successfully by elution with a 1 mM benzoic acid-10 mM cyclodextrin solution without chemical suppression.

  3. Analysis of neutral volatile aroma components in Tilsit cheese using a combination of dynamic headspace technique, capillary gas chromatography and mass spectrometry

    International Nuclear Information System (INIS)

    Dillinger, K.H.

    2000-03-01

    Tilsit cheese is made by the influence of lab ferment and starter cultures on milk. The ripening is done by repeated inoculation of the surface of the Tilsit cheese with yeasts and read smear cultures. This surface flora forms the typical aroma of the Tilsit cheese during the ripening process. The aim of the work was to receive general knowledge about the kind and amount of the neutral volatile aroma components of Tilsit cheese. Beyond this the ability of forming aroma components by read smear cultures and the dispersion of these components in cheese was to be examined. The results were intended to evaluate the formation of aroma components in Tilsit cheese. The semi-quantitative analyses of the aroma components of all samples were done by combining dynamic headspace extraction, gas chromatography and mass spectrometry. In this process the neutral volatile aroma components were extracted by dynamic headspace technique, adsorbed on a trap, thermally desorbed, separated by gas chromatography, detected and identified by mass spectrometry. 63 components belonging to the chemical classes of esters, ketones, aldehydes, alcohols and sulfur containing substances as well as aromatic hydrocarbons, chlorinated hydrocarbons and hydrocarbons were found in the analysed cheese samples of different Austrian Tilsit manufacturing plants. All cheese samples showed a qualitative equal but quantitative varied spectrum of aroma components. The cultivation of pure cultures on a cheese agar medium showed all analysed aroma components to be involved in the biochemical metabolism of these cultures. The ability to produce aroma components greatly differed between the strains and it was not possible to correlate this ability with the taxonomic classification of the strains. The majority of the components had a non-homogeneous concentration profile in the cheese body. This was explained by effects of diffusion and temporal and spatial different forming of components by the metabolism of the

  4. Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2015-04-01

    Volcanoes are a large source for several reactive atmospheric trace gases including sulphur and halogen containing species. The detailed knowledge of volcanic plume chemistry can give insights into subsurface processes and can be considered as a useful geochemical tool for monitoring of volcanic activity, especially halogen to sulphur ratios (e.g. Bobrowski and Giuffrida, 2012; Donovan et al., 2014). The reactive bromine species bromine monoxide (BrO) is of particular interest, because BrO as well as SO2 are readily measurable by UV spectrometers at a safe distance. Furthermore it is formed in the plume by a multiphase reaction mechanism under depletion of ozone in the plume. The abundance of BrO changes as a function of the reaction time and therefore distance from the vent as well as the spatial position in the plume. Due to the lack of analytical approaches for the accurate speciation of certain halogens (HBr, Br2, Br, BrCl, HOBr etc.) there are still uncertainties about the magnitude of volcanic halogen emissions and in particular their specificationtheir species and therefore also in the understanding of the bromine chemistry in volcanic plumes (Bobrowski et al., 2007). In this study, the first application of a 1,3,5-trimethoxybenzene (1,3,5-TMB)-coated gas diffusion denuder (Huang and Hoffmann, 2008) on volcanic gases proved to be suitable to collect selectively gaseous bromine species with oxidation states of +1 or 0 (Br2 and BrO(H)), while being ignorant to HBr (OS -1). The reaction of 1,3,5-TMB with bromine gives 1-bromo-2,4,6-trimethoxybenzene (1-bromo-2,4,6-TMB) - other halogens give corresponding products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Choosing a flow rate of 500 mL-min-1 and a denuder length of 0.5 m a nearly quantitative collection efficiency was achieved. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography

  5. Optimal artificial neural network architecture selection for performance prediction of compact heat exchanger with the EBaLM-OTR technique

    Energy Technology Data Exchange (ETDEWEB)

    Wijayasekara, Dumidu, E-mail: wija2589@vandals.uidaho.edu [Department of Computer Science, University of Idaho, 1776 Science Center Drive, Idaho Falls, ID 83402 (United States); Manic, Milos [Department of Computer Science, University of Idaho, 1776 Science Center Drive, Idaho Falls, ID 83402 (United States); Sabharwall, Piyush [Idaho National Laboratory, Idaho Falls, ID (United States); Utgikar, Vivek [Department of Chemical Engineering, University of Idaho, Idaho Falls, ID 83402 (United States)

    2011-07-15

    Highlights: > Performance prediction of PCHE using artificial neural networks. > Evaluating artificial neural network performance for PCHE modeling. > Selection of over-training resilient artificial neural networks. > Artificial neural network architecture selection for modeling problems with small data sets. - Abstract: Artificial Neural Networks (ANN) have been used in the past to predict the performance of printed circuit heat exchangers (PCHE) with satisfactory accuracy. Typically published literature has focused on optimizing ANN using a training dataset to train the network and a testing dataset to evaluate it. Although this may produce outputs that agree with experimental results, there is a risk of over-training or over-learning the network rather than generalizing it, which should be the ultimate goal. An over-trained network is able to produce good results with the training dataset but fails when new datasets with subtle changes are introduced. In this paper we present EBaLM-OTR (error back propagation and Levenberg-Marquardt algorithms for over training resilience) technique, which is based on a previously discussed method of selecting neural network architecture that uses a separate validation set to evaluate different network architectures based on mean square error (MSE), and standard deviation of MSE. The method uses k-fold cross validation. Therefore in order to select the optimal architecture for the problem, the dataset is divided into three parts which are used to train, validate and test each network architecture. Then each architecture is evaluated according to their generalization capability and capability to conform to original data. The method proved to be a comprehensive tool in identifying the weaknesses and advantages of different network architectures. The method also highlighted the fact that the architecture with the lowest training error is not always the most generalized and therefore not the optimal. Using the method the testing

  6. Optimal artificial neural network architecture selection for performance prediction of compact heat exchanger with the EBaLM-OTR technique

    International Nuclear Information System (INIS)

    Wijayasekara, Dumidu; Manic, Milos; Sabharwall, Piyush; Utgikar, Vivek

    2011-01-01

    Highlights: → Performance prediction of PCHE using artificial neural networks. → Evaluating artificial neural network performance for PCHE modeling. → Selection of over-training resilient artificial neural networks. → Artificial neural network architecture selection for modeling problems with small data sets. - Abstract: Artificial Neural Networks (ANN) have been used in the past to predict the performance of printed circuit heat exchangers (PCHE) with satisfactory accuracy. Typically published literature has focused on optimizing ANN using a training dataset to train the network and a testing dataset to evaluate it. Although this may produce outputs that agree with experimental results, there is a risk of over-training or over-learning the network rather than generalizing it, which should be the ultimate goal. An over-trained network is able to produce good results with the training dataset but fails when new datasets with subtle changes are introduced. In this paper we present EBaLM-OTR (error back propagation and Levenberg-Marquardt algorithms for over training resilience) technique, which is based on a previously discussed method of selecting neural network architecture that uses a separate validation set to evaluate different network architectures based on mean square error (MSE), and standard deviation of MSE. The method uses k-fold cross validation. Therefore in order to select the optimal architecture for the problem, the dataset is divided into three parts which are used to train, validate and test each network architecture. Then each architecture is evaluated according to their generalization capability and capability to conform to original data. The method proved to be a comprehensive tool in identifying the weaknesses and advantages of different network architectures. The method also highlighted the fact that the architecture with the lowest training error is not always the most generalized and therefore not the optimal. Using the method the

  7. Technique employed to seal a tube leaking in a heat exchanger of the tube type by explosives with supporting means for the adjacent tubes

    International Nuclear Information System (INIS)

    Larson, G.C.

    1978-01-01

    This invention concerns the technique employed to seal a tube leaking in a heat exchanger of the tube and tube plate type by detonating metal plugs activated by an explosive and inserted in both ends of the tube. It refers in particular to an apparatus and process in which the deformation or distortion of the adjacent tubes and tube plate ties under the effect of the explosive forces is significantly reduced [fr

  8. Demonstration of a novel technique to measure two-photon exchange effects in elastic e±p scattering

    Science.gov (United States)

    Moteabbed, M.; Niroula, M.; Raue, B. A.; Weinstein, L. B.; Adikaram, D.; Arrington, J.; Brooks, W. K.; Lachniet, J.; Rimal, Dipak; Ungaro, M.; Afanasev, A.; Adhikari, K. P.; Aghasyan, M.; Amaryan, M. J.; Anefalos Pereira, S.; Avakian, H.; Ball, J.; Baltzell, N. A.; Battaglieri, M.; Batourine, V.; Bedlinskiy, I.; Bennett, R. P.; Biselli, A. S.; Bono, J.; Boiarinov, S.; Briscoe, W. J.; Burkert, V. D.; Carman, D. S.; Celentano, A.; Chandavar, S.; Cole, P. L.; Collins, P.; Contalbrigo, M.; Cortes, O.; Crede, V.; D'Angelo, A.; Dashyan, N.; De Vita, R.; De Sanctis, E.; Deur, A.; Djalali, C.; Doughty, D.; Dupre, R.; Egiyan, H.; Fassi, L. El; Eugenio, P.; Fedotov, G.; Fegan, S.; Fersch, R.; Fleming, J. A.; Gevorgyan, N.; Gilfoyle, G. P.; Giovanetti, K. L.; Girod, F. X.; Goetz, J. T.; Gohn, W.; Golovatch, E.; Gothe, R. W.; Griffioen, K. A.; Guidal, M.; Guler, N.; Guo, L.; Hafidi, K.; Hakobyan, H.; Hanretty, C.; Harrison, N.; Heddle, D.; Hicks, K.; Ho, D.; Holtrop, M.; Hyde, C. E.; Ilieva, Y.; Ireland, D. G.; Ishkhanov, B. S.; Isupov, E. L.; Jo, H. S.; Joo, K.; Keller, D.; Khandaker, M.; Kim, A.; Klein, F. J.; Koirala, S.; Kubarovsky, A.; Kubarovsky, V.; Kuhn, S. E.; Kuleshov, S. V.; Lewis, S.; Lu, H. Y.; MacCormick, M.; MacGregor, I. J. D.; Martinez, D.; Mayer, M.; McKinnon, B.; Mineeva, T.; Mirazita, M.; Mokeev, V.; Montgomery, R. A.; Moriya, K.; Moutarde, H.; Munevar, E.; Munoz Camacho, C.; Nadel-Turonski, P.; Nasseripour, R.; Niccolai, S.; Niculescu, G.; Niculescu, I.; Osipenko, M.; Ostrovidov, A. I.; Pappalardo, L. L.; Paremuzyan, R.; Park, K.; Park, S.; Phelps, E.; Phillips, J. J.; Pisano, S.; Pogorelko, O.; Pozdniakov, S.; Price, J. W.; Procureur, S.; Protopopescu, D.; Puckett, A. J. R.; Ripani, M.; Rosner, G.; Rossi, P.; Sabatié, F.; Saini, M. S.; Salgado, C.; Schott, D.; Schumacher, R. A.; Seder, E.; Seraydaryan, H.; Sharabian, Y. G.; Smith, E. S.; Smith, G. D.; Sober, D. I.; Sokhan, D.; Stepanyan, S.; Strauch, S.; Tang, W.; Taylor, C. E.; Tian, Ye; Tkachenko, S.; Voskanyan, H.; Voutier, E.; Walford, N. K.; Wood, M. H.; Zachariou, N.; Zana, L.; Zhang, J.; Zhao, Z. W.; Zonta, I.

    2013-08-01

    Background: The discrepancy between proton electromagnetic form factors extracted using unpolarized and polarized scattering data is believed to be a consequence of two-photon exchange (TPE) effects. However, the calculations of TPE corrections have significant model dependence, and there is limited direct experimental evidence for such corrections.Purpose: The TPE contributions depend on the sign of the lepton charge in e±p scattering, but the luminosities of secondary positron beams limited past measurement at large scattering angles, where the TPE effects are believe to be most significant. We present the results of a new experimental technique for making direct e±p comparisons, which has the potential to make precise measurements over a broad range in Q2 and scattering angles.Methods: We use the Jefferson Laboratory electron beam and the Hall B photon tagger to generate a clean but untagged photon beam. The photon beam impinges on a converter foil to generate a mixed beam of electrons, positrons, and photons. A chicane is used to separate and recombine the electron and positron beams while the photon beam is stopped by a photon blocker. This provides a combined electron and positron beam, with energies from 0.5 to 3.2 GeV, which impinges on a liquid hydrogen target. The large acceptance CLAS detector is used to identify and reconstruct elastic scattering events, determining both the initial lepton energy and the sign of the scattered lepton.Results: The data were collected in two days with a primary electron beam energy of only 3.3 GeV, limiting the data from this run to smaller values of Q2 and scattering angle. Nonetheless, this measurement yields a data sample for e±p with statistics comparable to those of the best previous measurements. We have shown that we can cleanly identify elastic scattering events and correct for the difference in acceptance for electron and positron scattering. Because we ran with only one polarity for the chicane, we are unable

  9. Non-Halal biomarkers identification based on Fourier Transform Infrared Spectroscopy (FTIR) and Gas Chromatography-Time of Flight Mass Spectroscopy (GC-TOF MS) techniques

    Science.gov (United States)

    Witjaksono, Gunawan; Saputra, Irwan; Latief, Marsad; Jaswir, Irwandi; Akmeliawati, Rini; Abdelkreem Saeed Rabih, Almur

    2017-11-01

    Consumption of meat from halal (lawful) sources is essential for Muslims. The identification of non-halal meat is one of the main issues that face consumers in meat markets, especially in non-Islamic countries. Pig is one of the non-halal sources of meat, and hence pig meat and its derivatives are forbidden for Muslims to consume. Although several studies have been conducted to identify the biomarkers for nonhalal meats like pig meat, these studies are still in their infancy stages, and as a result there is no universal biomarker which could be used for clear cut identification. The purpose of this paper is to use Fourier Transform Infrared Spectroscopy (FTIR) and Gas Chromatography-Time of Flight Mass Spectroscopy (GC-TOF MS) techniques to study fat of pig, cow, lamb and chicken to find possible biomarkers for pig fat (lard) identification. FTIR results showed that lard and chicken fat have unique peaks at wavenumbers 1159.6 cm-1, 1743.4 cm-1, 2853.1 cm-1 and 2922.5 cm-1 compared to lamb and beef fats which did not show peaks at these wavenumbers. On the other hand, GC/MS-TOF results showed that the concentration of 1,2,3-trimethyl-Benzene, Indane, and Undecane in lard are 250, 14.5 and 1.28 times higher than their concentrations in chicken fat, respectively, and 91.4, 2.3 and 1.24 times higher than their concentrations in cow fat, respectively. These initial results clearly indicate that there is a possibility to find biomarkers for non-halal identification.

  10. Toward rapid analysis, forecast and discovery of bioactive compounds from herbs by jointly using thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy technique.

    Science.gov (United States)

    Gu, Xiaoling; Jin, Yang; Dong, Fang; Cai, Yueqing; You, Zhengyi; You, Junhui; Zhang, Liying; Du, Shuhu

    2018-05-10

    Conventional isolation and identification of active compounds from herbs have been extensively reported by using various chromatographic and spectroscopic techniques. However, how to quickly discover new bioactive ingredients from natural sources still remains a challenging task due to the interference of their similar structures or matrices. Here, we present a grand approach for rapid analysis, forecast and discovery of bioactive compounds from herbs based on a hyphenated strategy of thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy. The performance of the hyphenated strategy is first evaluated by analyzing four protoberberine alkaloids, berberine (BER), coptisine (COP), palmatine (PAT) and jatrorrhizine (JAT), from a typical herb Coptidis Rhizoma as an example. It has been demonstrated that this coupling method can identify the four compounds by characteristic peaks at 728, 708, 736 and 732 cm -1 , and especially discriminate BER and COP (with similar migration distances) by ratiometric Raman intensity (I 708 /I 728 ). The corresponding limits of detection are 0.1, 0.05, 0.1 and 0.5 μM, respectively, which are about 1-2 orders of magnitude lower than those of direct observation method under 254 nm UV lamp. Based on these findings, the proposed method further guides forecast and discovery of unknown compounds from traditional Chinese herb Typhonii Rhizoma. Results infer that two trace alkaloids (BER and COP) from the n-butanol extract of Typhonii Rhizoma are found for the first time. Moreover, in vitro experiments manifest that BER can effectively decrease the viability of human glioma U87 cells by inducing cell cycle arrest in a concentration-dependent manner. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometric (LC/ESI-MS/MS) Study for the Identification and Characterization of In Vivo Metabolites of Cisplatin in Rat Kidney Cancer Tissues: Online Hydrogen/Deuterium (H/D) Exchange Study.

    Science.gov (United States)

    Bandu, Raju; Ahn, Hyun Soo; Lee, Joon Won; Kim, Yong Woo; Choi, Seon Hee; Kim, Hak Jin; Kim, Kwang Pyo

    2015-01-01

    In vivo rat kidney tissue metabolites of an anticancer drug, cisplatin (cis-diamminedichloroplatinum [II]) (CP) which is used for the treatment of testicular, ovarian, bladder, cervical, esophageal, small cell lung, head and neck cancers, have been identified and characterized by using liquid chromatography positive ion electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) in combination with on line hydrogen/deuterium exchange (HDX) experiments. To identify in vivo metabolites, kidney tissues were collected after intravenous administration of CP to adult male Sprague-Dawley rats (n = 3 per group). The tissue samples were homogenized and extracted using newly optimized metabolite extraction procedure which involves liquid extraction with phosphate buffer containing ethyl acetate and protein precipitation with mixed solvents of methanol-water-chloroform followed by solid-phase clean-up procedure on Oasis HLB 3cc cartridges and then subjected to LC/ESI-HRMS analysis. A total of thirty one unknown in vivo metabolites have been identified and the structures of metabolites were elucidated using LC-MS/MS experiments combined with accurate mass measurements. Online HDX experiments have been used to further support the structural characterization of metabolites. The results showed that CP undergoes a series of ligand exchange biotransformation reactions with water and other nucleophiles like thio groups of methionine, cysteine, acetylcysteine, glutathione and thioether. This is the first research approach focused on the structure elucidation of biotransformation products of CP in rats, and the identification of metabolites provides essential information for further pharmacological and clinical studies of CP, and may also be useful to develop various effective new anticancer agents.

  12. Clinical relevance of the discrepancy in phenylalanine concentrations analyzed using tandem mass spectrometry compared with ion-exchange chromatography in phenylketonuria

    Directory of Open Access Journals (Sweden)

    Bridget M. Stroup

    2016-03-01

    Conclusion: Use of DBS analyzed using MS/MS to monitor blood phe concentrations in individuals with PKU yields significantly lower phe levels compared to plasma phe levels analyzed using IEC. Optimization of current testing methodologies for measuring phe in DBS, along with patient education regarding the appropriate technique for spotting blood on filter paper is needed to improve the accuracy of using DBS to measure phe concentrations in PKU management.

  13. Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques.

    Science.gov (United States)

    Engida, Adam Mekonnen; Faika, Sitti; Nguyen-Thi, Bich Thuyen; Ju, Yi-Hsu

    2015-06-01

    In the present work, heat reflux extraction with ethanol/water (80:20; v/v) as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE) was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF) and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1) were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut. Copyright © 2014. Published by Elsevier B.V.

  14. Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques

    Directory of Open Access Journals (Sweden)

    Adam Mekonnen Engida

    2015-06-01

    Full Text Available In the present work, heat reflux extraction with ethanol/water (80:20; v/v as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1 were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut.

  15. Introduction to modern liquid chromatography

    National Research Council Canada - National Science Library

    Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

    2010-01-01

    "High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

  16. Gas chromatography: mass selective detector

    International Nuclear Information System (INIS)

    Lapinskas, R.

    1988-01-01

    The mechanism of mass spectrometry technique directed for detecting molecular structures is described, with some considerations about its operational features. This mass spectrometer is used as a gas chromatography detector. (author)

  17. 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

  18. Characterisation of uremic "Middle molecular"fractions by gas chromatography mass spectrometry, isotachophoresis, and liquid chromatography

    NARCIS (Netherlands)

    Schoots, A.C.; Mikkers, F.E.P.; Claessens, H.A.; Smet, de R.; Landschoot, van N.; Ringoir, S.M.G.

    1982-01-01

    Uremic ultrafiltrates (and normal serum, for comparison) were fractionated by means of gel filtration. The collected fractions were further investigated by combined analytical techniques: "high- performance" liquid chromatography, gas chromatography, mass spectrometry, and isotachophoresis.

  19. Metal-organic frameworks in chromatography.

    Science.gov (United States)

    Yusuf, Kareem; Aqel, Ahmad; ALOthman, Zeid

    2014-06-27

    Metal-organic frameworks (MOFs) emerged approximately two decades ago and are the youngest class of porous materials. Despite their short existence, MOFs are finding applications in a variety of fields because of their outstanding chemical and physical properties. This review article focuses on the applications of MOFs in chromatography, including high-performance liquid chromatography (HPLC), gas chromatography (GC), and other chromatographic techniques. The use of MOFs in chromatography has already had a significant impact; however, the utilisation of MOFs in chromatography is still less common than other applications, and the number of MOF materials explored in chromatography applications is limited. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. A simple method using on-line continuous leaching and ion exchange chromatography coupled to inductively coupled plasma mass spectrometry for the speciation analysis of bio-accessible arsenic in rice.

    Science.gov (United States)

    Horner, Nolan S; Beauchemin, Diane

    2012-03-02

    A simple method for the speciation analysis of bio-accessible arsenic (As) in rice was developed using a continuous on-line leaching method to release the bio-accessible fraction. The continuous on-line leaching method has several advantages over commonly used batch methods including quicker and easier sample preparation, reduced risk of contamination and access to real time leaching data. The bio-accessibility of As in the samples was monitored using inductively coupled plasma mass spectrometry (ICP-MS). Results from a certified reference material as well as cooked and uncooked white rice showed that the majority of As was leached by saliva. Results obtained using the continuous on-line leaching method were comparable to those obtained using a batch method. Speciation analysis of the saliva leachate was performed using ion exchange chromatography coupled to ICP-MS. The four most toxic forms of As (As(III), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and As(V)) were clearly separated within 5 min in a single chromatographic run. Over 92% of bio-accessible As in the certified reference material and uncooked white rice sample was in the form of DMA and As(V), whereas it was present as DMA and As(III) in the cooked white rice. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Separation and quantification of inulin in selected artichoke (Cynara scolymus L.) cultivars and dandelion (Taraxacum officinale WEB. ex WIGG.) roots by high-performance anion exchange chromatography with pulsed amperometric detection.

    Science.gov (United States)

    Schütz, Katrin; Muks, Erna; Carle, Reinhold; Schieber, Andreas

    2006-12-01

    The profile of fructooligosaccharides and fructopolysaccharides in artichoke heads and dandelion roots was investigated. For this purpose, a suitable method for high-performance anion exchange chromatography with pulsed amperometic detection was developed. The separation of monomers, oligomers and polymers up to a chain length of 79 sugar residues was achieved in one single run. Glucose, fructose, sucrose and individual fructooligosaccharides (kestose, nystose, fructofuranosylnystose) were quantified in six different artichoke cultivars and in dandelion roots. The contents ranged from 12.9 g/kg DM to 71.7 g/kg DM for glucose, from 15.8 g/kg DM to 67.2 g/kg DM for fructose, and from 16.8 g/kg DM to 55.2 g/kg DM for sucrose in the artichoke heads. Kestose was the predominant fructooligosaccharide, followed by nystose and fructofuranosylnystose. In four cultivars fructofuranosylnystose was only detectable in traces and reached its maximum value of 3.6 g/kg DM in the cultivar Le Castel. Furthermore, an average degree of polymerization of 5.3 to 16.7 was calculated for the individual artichoke cultivars, which is noticeably lower than hitherto reported. In contrast, the contents of kestose, nystose and fructofuranosylnystose in dandelion root exceeded that of artichoke, reflecting the short chain characteristic of the inulin, which was confirmed by chromatographic analysis. Copyright (c) 2006 John Wiley & Sons, Ltd.

  2. Effect of nebulizer/spray chamber interfaces on simultaneous, axial view inductively coupled plasma optical emission spectrometry for the direct determination of As and Se species separated by ion exchange high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Gettar, Raquel T.; Smichowski, Patricia; Garavaglia, Ricardo N.; Farias, Silvia; Batistoni, Daniel A.

    2005-01-01

    Different nebulizer/expansion chamber combinations were evaluated to assess their performance for sample introduction in the direct coupling with an axial view inductively coupled plasma multielement spectrometer for on-line determination of As and Se species previously separated by ion exchange-high performance liquid chromatography. The column effluents were injected into the plasma without prior derivatization. The instrument operation software was adapted for data acquisition and processing to allow multi-wavelength recording of the transient chromatographic peaks. After optimization of the chromatographic operating conditions, separation of mixtures of inorganic As and Se species, and of inorganic and two organic As species (monomethylarsonic and dimethylarsinic acids), was achieved with excellent resolution. Species discrimination from mixtures of As and Se oxyanions was further improved by the simultaneous element detection at specific analytical wavelengths. Three nebulizers and three spray chambers, employed in seven combinations, were tested as interfaces. Concentric nebulizers associated to a glass cyclonic chamber appear most suitable regarding sensitivity and signal to noise ratio. Measured element detection limits (3 σ) were around 10 ng ml -1 for all the species considered, making the method a viable alternative to similar procedures that employ volatile hydride generation previous to sample injection into the plasma. Analytical recoveries both for inorganic and organic species ranged between 92 and 107%. The method was demonstrated to be apt for the analysis of surface waters potentially subjected to natural contamination with arsenic

  3. Ion-exclusion/cation-exchange chromatography with dual detection of the conductivity and spectrophotometry for the simultaneous determination of common inorganic anionic species and cations in river and wastewater.

    Science.gov (United States)

    Nakatani, Nobutake; Kozaki, Daisuke; Mori, Masanobu; Hasebe, Kiyoshi; Nakagoshi, Nobukazu; Tanaka, Kazuhiko

    2011-01-01

    Simultaneous determinations of common inorganic anionic species (SO(4)(2-), Cl(-), NO(3)(-), phosphate and silicate) and cations (Na(+), NH(4)(+), K(+), Mg(2+) and Ca(2+)) were conducted using an ion-chromatography system with dual detection of conductivity and spectrophotometry in tandem. The separation of ionic species on a weakly acidic cation-exchange resin was accomplished using a mixture of 100 mM ascorbic acid and 4 mM 18-crown-6 as an acidic eluent (pH 2.6), after which the ions were detected using a conductivity detector. Subsequently, phosphate and silicate were analyzed based on derivatization with molybdate and spectrophotometry at 700 nm. The detection limits at S/N = 3 ranged from 0.11 to 2.9 µM for analyte ionic species. This method was applied to practical river water and wastewater with acceptable criteria for the anion-cation balance and comparisons of the measured and calculated electrical conductivity, demonstrating the usefulness of the present method for water quality monitoring.

  4. Uses of extraction and ion exchange chromatography in the thorium and rare earths separation from industrial residue generated in thorium purification unity at IPEN. Application of rare earths as catalysts for generation of hydrogen

    International Nuclear Information System (INIS)

    Zini, Josiane

    2010-01-01

    In the 70's a pilot plant for studies of different concentrates processing obtained from the chemical processing of monazite was operated at IPEN / CNEN-SP, with a view to obtaining thorium of nuclear purity. This unity was operated on an industrial scale since 1985, generating around 25 metric tons of residue and was closed in 2002. This waste containing thorium and rare earths was named Retoter (Rejeito de Torio e Terras Raras, in portuguese) and stored in the IPEN Safeguards shed. This paper studies the treatment of the waste, aimed at environmental, radiological and technology. Were studied two cases for the chromatographic separation of thorium from rare earths. One of them was the chromatographic extraction, where the extracting agent tributyl phosphate was supported on polymeric resins Amberlite XAD16. The other method is studied for comparison purposes, since the material used in chromatographic extraction is unprecedented with regard to the separation of thorium, was the ion-exchange chromatography using DOWEX 1-X8 strong cationic resin. Was studied also the chromatographic process of extraction with the extracting agent DEHPA supported on Amberlite XAD16 for the fractionation in groups of rare earths elements. Thorium was separated with high purity for strategic purposes and rare earths recovered free from thorium, were tested as a catalyst for ethanol reforming to hydrogen obtaining which is used in fuel cells for power generation. (author)

  5. Validation of methodologies for the analysis of lead and methyl-ether in gasoline, using the techniques of atomic emission with plasma source coupled inductively and micellar liquid chromatography

    International Nuclear Information System (INIS)

    Redondo Escalante, M.

    1995-01-01

    This study established and optimized the experimental variables for the lead quantization through the Icp-Aes technique, in aqueous media. A comparative study of several proposal methods, that appears in the literature for the extraction in aqueous media of the lead in gasoline was made. It determined that it is not possible, to make this procedure using the reaction of hydrolysis of tetraethyl lead. The op tim conditions were established, for the lead quantization in gasoline, using methyl-isobutyl-ketone and also ethanol as dis solvents. The conditions of the proposed methodologies were optimized, and the variables of analytical performance were defined. It was demonstrated, that it is possible to prepare lead dissolution patterns, in organic media, starting from inorganic salts of this metal. The techniques of chromatography of gases and of liquid chromatography of high pressure, in the analysis of methyl-ter butyl-ether (Mtbe), were compared. It demonstrated that it is possible, to quantize the Mtbe through the HPLC technique, and it found that the 'micellar' liquid chromatography. (author) [es

  6. High-performance liquid chromatography of oligoguanylates at high pH

    Science.gov (United States)

    Stribling, R.; Deamer, D. (Principal Investigator)

    1991-01-01

    Because of the stable self-structures formed by oligomers of guanosine, standard high-performance liquid chromatography techniques for oligonucleotide fractionation are not applicable. Previously, oligoguanylate separations have been carried out at pH 12 using RPC-5 as the packing material. While RPC-5 provides excellent separations, there are several limitations, including the lack of a commercially available source. This report describes a new anion-exchange high-performance liquid chromatography method using HEMA-IEC BIO Q, which successfully separates different forms of the guanosine monomer as well as longer oligoguanylates. The reproducibility and stability at high pH suggests a versatile role for this material.

  7. Removal of transmissible spongiform encephalopathy prion from large volumes of cell culture media supplemented with fetal bovine serum by using hollow fiber anion-exchange membrane chromatography.

    Science.gov (United States)

    Chou, Ming Li; Bailey, Andy; Avory, Tiffany; Tanimoto, Junji; Burnouf, Thierry

    2015-01-01

    Cases of variant Creutzfeldt-Jakob disease in people who had consumed contaminated meat products from cattle with bovine spongiform encephalopathy emphasize the need for measures aimed at preventing the transmission of the pathogenic prion protein (PrPSc) from materials derived from cattle. Highly stringent scrutiny is required for fetal bovine serum (FBS), a growth-medium supplement used in the production of parenteral vaccines and therapeutic recombinant proteins and in the ex vivo expansion of stem cells for transplantation. One such approach is the implementation of manufacturing steps dedicated to removing PrPSc from materials containing FBS. We evaluated the use of the QyuSpeed D (QSD) adsorbent hollow-fiber anion-exchange chromatographic column (Asahi Kasei Medical, Tokyo, Japan) for the removal of PrPSc from cell culture media supplemented with FBS. We first established that QSD filtration had no adverse effect on the chemical composition of various types of culture media supplemented with 10% FBS or the growth and viability characteristics of human embryonic kidney (HEK293) cells, baby hamster kidney (BHK-21) cells, African green monkey kidney (Vero) cells, and Chinese hamster ovary (CHO-k1) cells propagated in the various culture-medium filtrates. We used a 0.6-mL QSD column for removing PrPSc from up to 1000 mL of Dulbecco's modified Eagle's medium containing 10% FBS previously spiked with the 263K strain of hamster-adapted scrapie. The Western blot analysis, validated alongside an infectivity assay, revealed that the level of PrPSc in the initial 200mL flow-through was reduced by 2.5 to > 3 log10, compared with that of the starting material. These results indicate that QSD filtration removes PrPSc from cell culture media containing 10% FBS, and demonstrate the ease with which QSD filtration can be implemented in at industrial-scale to improve the safety of vaccines, therapeutic recombinant proteins, and ex vivo expanded stem cells produced using growth

  8. Exchange Options

    NARCIS (Netherlands)

    Jamshidian, F.

    2007-01-01

    The contract is described and market examples given. Essential theoretical developments are introduced and cited chronologically. The principles and techniques of hedging and unique pricing are illustrated for the two simplest nontrivial examples: the classical Black-Scholes/Merton/Margrabe exchange

  9. Tunable Subpicosecond Electron-Bunch-Train Generation Using a Transverse-To-Longitudinal Phase-Space Exchange Technique

    International Nuclear Information System (INIS)

    Sun, Y.-E; Piot, P.; Maxwell, T. J.; Johnson, A.; Lumpkin, A. H.; Ruan, J.; Thurman-Keup, R.

    2010-01-01

    We report on the experimental generation of a train of subpicosecond electron bunches. The bunch train generation is accomplished using a beam line capable of exchanging the coordinates between the horizontal and longitudinal degrees of freedom. An initial beam consisting of a set of horizontally separated beamlets is converted into a train of bunches temporally separated with tunable bunch duration and separation. The experiment reported in this Letter unambiguously demonstrates the conversion process and its versatility.

  10. The Development of a Patient-Identification-Oriented Nursing Shift Exchange Support System Using Wireless RFID PDA Techniques

    OpenAIRE

    Huang, Pin-Jen; She, Chien-Cheng; Chang, Polun

    2005-01-01

    The objectives of this study were to technically testing the feasibility of combining RFID and PDA technologies in nursing care and to develop a support system for the nursing shift exchange, which featured with “Positive Patient Identification” and “Point of Care” for patient’s safety and security. The most challenging part for the future work would be to embed the system into the real workflow. Future study would be to examine the practical effectiveness of the system....

  11. Progress in liquid ion exchangers

    International Nuclear Information System (INIS)

    Nakagawa, Genkichi

    1974-01-01

    Review is made on the extraction with anion exchangers and the extraction with liquid cation exchangers. On the former, explanation is made on the extraction of acids, the relation between anion exchange and the extraction of metals, the composition of the metallic complexes that are extracted, and the application of the extraction with anion exchangers to analytical chemistry. On the latter, explanation is made on the extraction of metals and its application to analytical chemistry. The extraction with liquid ion exchangers is suitable for the operation in chromatography, because the distribution of extracting agents into aqueous phase is small, and extraction equilibrium is quickly reached, usually within 1 to several minutes. The separation by means of anion exchangers is usually made from hydrochloric acid solution. For example, Brinkman et al. determined Rf values for more than 50 elements by thin layer chromatography. Tables are given for showing the structure of the liquid ion exchangers and the polymerized state of various amines. (Mori, K.)

  12. High Performance Liquid Chromatography Experiments to Undergraduate Laboratories

    Science.gov (United States)

    Kissinger, Peter T.; And Others

    1977-01-01

    Reviews the principles of liquid chromatography with electrochemical detection (LCEC), an analytical technique that incorporates the advantages of both liquids chromatography and electrochemistry. Also suggests laboratory experiments using this technique. (MLH)

  13. Tissue-specific metabolite profiling of Cyperus rotundus L. rhizomes and (+)-nootkatone quantitation by laser microdissection, ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry, and gas chromatography-mass spectrometry techniques.

    Science.gov (United States)

    Jaiswal, Yogini; Liang, Zhitao; Guo, Ping; Ho, Hing-Man; Chen, Hubiao; Zhao, Zhongzhen

    2014-07-23

    Cyperus rotundus L. is a plant species commonly found in both India and China. The caused destruction of this plant is of critical concern for agricultural produce. Nevertheless, it can serve as a potential source of the commercially important sesquiterpenoid (+)-nootkatone. The present work describes comparative metabolite profiling and (+)-nootkatone content determination in rhizome samples collected from these two countries. Laser dissected tissues, namely, the cortex, hypodermal fiber bundles, endodermis, amphivasal vascular bundles, and whole rhizomes were analyzed by ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Gas chromatography-mass spectrometry (GC-MS) analysis was used for profiling of essential oil constituents and quantitation of (+)-nootkatone. The content of (+)-nootkatone was found to be higher in samples from India (30.47 μg/10 g) compared to samples from China (21.72 μg/10 g). The method was validated as per International Conference on Harmonisation (ICH) guidelines (Q2 R1). The results from this study can be applied for quality control and efficient utilization of this terpenoid-rich plant for several applications in food-based industries.

  14. Application of anion-exchange techniques to the determination of traces of molybdenum in sea-water

    International Nuclear Information System (INIS)

    Kiriyama, T.; Kuroda, R.

    1984-01-01

    A combined ion-exchange spectrophotometric method has been developed for the determination of molybdenum in sea-water. Molybdenum is sorbed strongly on Amberlite CG 400 (Cl - ) at pH 3 from sea-water containing ascorbic acid and is easily eluted with 6 M nitric acid. Molybdenum in the effluent can be determined spectrophotometrically with potassium thiocyanate and stannous chloride. The combined method allows selective and sensitive determination of traces of molybdenum in sea-water. The precision of the method is 2% at a molybdenum level of approx. 10 μg/l. (author)

  15. An orientation sensitive approach in biomolecule interaction quantitative structure-activity relationship modeling and its application in ion-exchange chromatography.

    Science.gov (United States)

    Kittelmann, Jörg; Lang, Katharina M H; Ottens, Marcel; Hubbuch, Jürgen

    2017-01-27

    Quantitative structure-activity relationship (QSAR) modeling for prediction of biomolecule parameters has become an established technique in chromatographic purification process design. Unfortunately available descriptor sets fail to describe the orientation of biomolecules and the effects of ionic strength in the mobile phase on the interaction with the stationary phase. The literature describes several special descriptors used for chromatographic retention modeling, all of these do not describe the screening of electrostatic potential by the mobile phase in use. In this work we introduce two new approaches of descriptor calculations, namely surface patches and plane projection, which capture an oriented binding to charged surfaces and steric hindrance of the interaction with chromatographic ligands with regard to electrostatic potential screening by mobile phase ions. We present the use of the developed descriptor sets for predictive modeling of Langmuir isotherms for proteins at different pH values between pH 5 and 10 and varying ionic strength in the range of 10-100mM. The resulting model has a high correlation of calculated descriptors and experimental results, with a coefficient of determination of 0.82 and a predictive coefficient of determination of 0.92 for unknown molecular structures and conditions. The agreement of calculated molecular interaction orientations with both, experimental results as well as molecular dynamic simulations from literature is shown. The developed descriptors provide the means for improved QSAR models of chromatographic processes, as they reflect the complex interactions of biomolecules with chromatographic phases. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. The tritium labeling of Butibufen by heterogeneous catalytic exchange; Marcado del Butibufen con Tritio por inter- cambio catalitico en disolucion

    Energy Technology Data Exchange (ETDEWEB)

    Santamaria, J; Rebollo, D

    1986-07-01

    The labeling of a new non-steroidal antiinflammatory agent, Butibufen (2-(4-isobutylphenyl) butyric acid) was studied. The method used was heterogeneous catalytic exchange between Butibufen and tritiated water, obtained in situ. Purification was accomplished through thin layer chromatography. Concentration, purity and specific activity of the labeled drug were determined by ultraviolet and liquid scintillation techniques. (Author) 7 refs.

  17. 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

  18. Preparation of Polyimide/Zinc Oxide Nanocomposite Films via an Ion-Exchange Technique and Their Photoluminescence Properties

    Directory of Open Access Journals (Sweden)

    Shuxiang Mu

    2011-01-01

    Full Text Available Polyimide (PI composite films with ZnO nanoparticles embedded in the surface layer were prepared by alkali hydrolyzation following ion exchange in Zn(NO32 solution and thermal treatment of the zinc ion-doped PI films in air atmosphere. The effect of alkali treatment, ion exchange, and thermal treatment conditions was investigated in relation to the amount of zinc atomic loading, morphology, photoluminescence (PL, and thermal properties of the PI/ZnO composite films using ICP, XPS, FE-SEM, TEM, Raman microscope, TGA, and DSC. ZnO nanoparticles were formed slowly and dispersed uniformly in the surface-modified layers of PI films with an average diameter of 20 nm. The PL spectra of all the PI/ZnO nanocomposite films obtained at 350°C/7 h possessed a weak ultraviolet emission peak and a broad and strong visible emission band. The PI/ZnO nanocomposite films maintained the excellent thermal property of the host PI films.

  19. Net ecosystem exchange and energy fluxes measured with the eddy covariance technique in a western Siberian bog

    Directory of Open Access Journals (Sweden)

    P. Alekseychik

    2017-08-01

    Full Text Available Very few studies of ecosystem–atmosphere exchange involving eddy covariance data have been conducted in Siberia, with none in the western Siberian middle taiga. This work provides the first estimates of carbon dioxide (CO2 and energy budgets in a typical bog of the western Siberian middle taiga based on May–August measurements in 2015. The footprint of measured fluxes consisted of a homogeneous mixture of tree-covered ridges and hollows with the vegetation represented by typical sedges and shrubs. Generally, the surface exchange rates resembled those of pine-covered bogs elsewhere. The surface energy balance closure approached 100 %. Net CO2 uptake was comparatively high, summing up to 202 gC m−2 for the four measurement months, while the Bowen ratio was seasonally stable at 28 %. The ecosystem turned into a net CO2 source during several front passage events in June and July. The periods of heavy rain helped keep the water table at a sustainably high level, preventing a usual drawdown in summer. However, because of the cloudy and rainy weather, the observed fluxes might rather represent the special weather conditions of 2015 than their typical magnitudes.

  20. Enantioseparations in counter-current chromatography and centrifugal partition chromatography.

    Science.gov (United States)

    Foucault, A P

    2001-01-12

    Examples of chiral separations in counter-current chromatography (CCC) and centrifugal partition chromatography (CPC) are not numerous, due to the difficulty of finding chiral selectors highly selective in the liquid phase as well as a combination of solvents that does not destroy the selectivity and retains the capacity to elute chiral isomers of interest. New ideas and new chiral selectors generally come from other separation techniques, as will be highlighted in this review.

  1. Calcium-sensitive immunoaffinity chromatography

    DEFF Research Database (Denmark)

    Henriksen, Maiken L; Lindhardt Madsen, Kirstine; Skjoedt, Karsten

    2014-01-01

    Immunoaffinity chromatography is a powerful fractionation technique that has become indispensable for protein purification and characterization. However, it is difficult to retrieve bound proteins without using harsh or denaturing elution conditions, and the purification of scarce antigens...... to homogeneity may be impossible due to contamination with abundant antigens. In this study, we purified the scarce, complement-associated plasma protein complex, collectin LK (CL-LK, complex of collectin liver 1 and kidney 1), by immunoaffinity chromatography using a calcium-sensitive anti-collectin-kidney-1 m...... chromatography was superior to the traditional immunoaffinity chromatographies and resulted in a nine-fold improvement of the purification factor. The technique is applicable for the purification of proteins in complex mixtures by single-step fractionation without the denaturation of eluted antigens...

  2. Where the Rubber Meets the Road; Varied Techniques for Measuring the Land-Atmosphere Exchange of Water and Energy in a California Watershed and the Driving Influences on this Exchange

    Science.gov (United States)

    Kochendorfer, J.; Viers, J.; Niswonger, R.; Paw U, K.; Haas, E.; Reck, R. A.

    2005-12-01

    In conjunction with the Cosumnes Research Group, we performed a field study along the Cosumnes River in California's Central Valley. The study included tower-based evapotranspiration estimates, continuous hydrologic measurements, and analysis of remote sensing data. We estimated the effects of phreatophytic evapotranspiration on groundwater from scales as small as an individual stand of trees to as large as the watershed and explored the climactic and hydrologic controls over riparian evapotranspiration. Tower-based evapotranspiration measurements included one eddy covariance tower within a cottonwood forest (Populus fremontii), and one surface temperature/micrometeorological evapotranspiration tower within a willow stand (Salix lasiolepis). The technique used on the surface temperature/micrometeorological evapotranspiration tower was developed and chosen in preference to eddy covariance for a site where a considerable quantity of the riparian ecosystem to atmosphere exchange is advective. Hydrologic techniques included measurements of groundwater depth and volumetric soil moisture. We also examined multitemporal, multiresolution remotely sensed imagery to correlate evapotranspiration rates for a restored cottonwood forest with derived vegetation indices. These indices were evaluated for applicability to other restored riparian habitats within the Cosumnes River Preserve and to help guide future restoration actions as a function of hydrologic connectivity and water demand.

  3. Chemical exchange saturation transfer (CEST) MR technique for in-vivo liver imaging at 3.0 tesla

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Shu-Zhong; Deng, Min; Wang, Yi-Xiang J. [Chinese University of Hong Kong, Prince of Wales Hospital, Department of Imaging and Interventional Radiology, Faculty of Medicine (China); Yuan, Jing [Hong Kong Sanatorium and Hospital, Medical Physics and Research Department, Happy Valley, Hong Kong (China); Wei, Juan [Philips Healthcare Asia, Shanghai (China); Zhou, Jinyuan [Johns Hopkins University, Department of Radiology, Baltimore, MD (United States); Kennedy Krieger Institute, F.M. Kirby Research Center for Functional Brain Imaging, Baltimore, MD (United States)

    2016-06-15

    To evaluate Chemical Exchange Saturation Transfer (CEST) MRI for liver imaging at 3.0-T. Images were acquired at offsets (n = 41, increment = 0.25 ppm) from -5 to 5 ppm using a TSE sequence with a continuous rectangular saturation pulse. Amide proton transfer-weighted (APTw) and GlycoCEST signals were quantified as the asymmetric magnetization transfer ratio (MTR{sub asym}) at 3.5 ppm and the total MTR{sub asym} integrated from 0.5 to 1.5 ppm, respectively, from the corrected Z-spectrum. Reproducibility was assessed for rats and humans. Eight rats were devoid of chow for 24 hours and scanned before and after fasting. Eleven rats were scanned before and after one-time CCl4 intoxication. For reproducibility, rat liver APTw and GlycoCEST measurements had 95 % limits of agreement of -1.49 % to 1.28 % and -0.317 % to 0.345 %. Human liver APTw and GlycoCEST measurements had 95 % limits of agreement of -0.842 % to 0.899 % and -0.344 % to 0.164 %. After 24 hours, fasting rat liver APTw and GlycoCEST signals decreased from 2.38 ± 0.86 % to 0.67 ± 1.12 % and from 0.34 ± 0.26 % to -0.18 ± 0.37 % respectively (p < 0.05). After CCl4 intoxication rat liver APTw and GlycoCEST signals decreased from 2.46 ± 0.48 % to 1.10 ± 0.77 %, and from 0.34 ± 0.23 % to -0.16 ± 0.51 % respectively (p < 0.05). CEST liver imaging at 3.0-T showed high sensitivity for fasting as well as CCl4 intoxication. (orig.)

  4. Ion-exchange chromatographic protein refolding

    NARCIS (Netherlands)

    Freydell, E.; Wielen, van der L.; Eppink, M.H.M.; Ottens, M.

    2010-01-01

    The application of ion-exchange (IEX) chromatography to protein refolding (IExR) has been successfully proven, as supported by various studies using different model proteins, ion-exchange media and flow configurations. Ion-exchange refolding offers a relatively high degree of process

  5. Gas chromatography

    International Nuclear Information System (INIS)

    Cram, S.P.; Risby, T.H.; Field, L.R.; Yu, W.L.

    1980-01-01

    In addition to the published literature for the years 1978 - 79, this review of developments in the field of gas chromatography includes earlier articles of particular significance appearing in foreign journals and the patent literature which was not available at the time of the previous review. The articles cited were selected as presenting the most fundamental developments in theory, methodology, and instrumentation. Some applications are cited if they reflect an advance in the state-of-the-art or have particular relevance to new developments. 1149 references are cited

  6. The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Steven [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

  7. Chemical exchange saturation transfer (CEST) MR technique for in-vivo liver imaging at 3.0 tesla.

    Science.gov (United States)

    Chen, Shu-Zhong; Yuan, Jing; Deng, Min; Wei, Juan; Zhou, Jinyuan; Wáng, Yì-Xiáng J

    2016-06-01

    To evaluate Chemical Exchange Saturation Transfer (CEST) MRI for liver imaging at 3.0-T. Images were acquired at offsets (n = 41, increment = 0.25 ppm) from -5 to 5 ppm using a TSE sequence with a continuous rectangular saturation pulse. Amide proton transfer-weighted (APTw) and GlycoCEST signals were quantified as the asymmetric magnetization transfer ratio (MTRasym) at 3.5 ppm and the total MTRasym integrated from 0.5 to 1.5 ppm, respectively, from the corrected Z-spectrum. Reproducibility was assessed for rats and humans. Eight rats were devoid of chow for 24 hours and scanned before and after fasting. Eleven rats were scanned before and after one-time CCl4 intoxication. For reproducibility, rat liver APTw and GlycoCEST measurements had 95 % limits of agreement of -1.49 % to 1.28 % and -0.317 % to 0.345 %. Human liver APTw and GlycoCEST measurements had 95 % limits of agreement of -0.842 % to 0.899 % and -0.344 % to 0.164 %. After 24 hours, fasting rat liver APTw and GlycoCEST signals decreased from 2.38 ± 0.86 % to 0.67 ± 1.12 % and from 0.34 ± 0.26 % to -0.18 ± 0.37 % respectively (p 3.0-T showed high sensitivity for fasting as well as CCl4 intoxication. • CEST MRI of in-vivo liver was demonstrated at clinical 3 T field strength. • After 24-hour fasting, rat liver APTw and GlycoCEST signals decreased significantly. • After CCl4 intoxication both rat liver APTw and GlycoCEST signals decreased significantly. • Good scan-rescan reproducibility of liver CEST MRI was shown in healthy volunteers.

  8. Chromatography in Industry

    Science.gov (United States)

    Schoenmakers, Peter

    2009-07-01

    This review focuses on the chromatography research that has been carried out within industry or in close cooperation with industry and that has been reported in the scientific literature between 2006 and mid-2008. Companies in the health care sector, such as pharmaceutical and biotechnology companies, are the largest contributors. Industrial research seems to take place in an open environment in cooperation with academia, peer companies, and institutions. Industry appears ready to embrace new technologies as they emerge, but they focus strongly on making chromatography work robustly, reliably, rapidly, and automatically. “Hyphenated” systems that incorporate on-line sample-preparation techniques and mass-spectrometric detection are the rule rather than the exception. Various multidimensional separation methods are finding numerous applications. Strategies aimed at speeding up the development of new chromatographic methods remain the focus of attention. Also, there is a clear trend toward exploring chromatographic methods for parallel processing along with other strategies for high-throughput analysis.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-11-15

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

  10. Effects of hemoglobin variants HbJ Bangkok, HbE, HbG Taipei, and HbH on analysis of glycated hemoglobin via ion-exchange high-performance liquid chromatography.

    Science.gov (United States)

    Zhang, Xiu-Ming; Wen, Dong-Mei; Xu, Sheng-Nan; Suo, Ming-Huan; Chen, Ya-Qiong

    2018-01-01

    To explore the effects of HbJ Bangkok, HbE, HbG Taipei, and α-thalassemia HbH on the results of HbA1c assessment using ion-exchange high-performance liquid chromatography (IE-HPLC). We enrolled five patients in which the results of the IE-HPLC HbA1c assay were inconsistent with the average levels of FBG. We performed hemoglobin capillary (Hb) electrophoresis using whole-blood samples. We also sequenced the genes encoding Hb using dideoxy-mediated chain termination and analyzed HbA1c using borate affinity HPLC (BA-HPLC) and turbidimetric inhibition immunoassay (TINIA). Two patients had the HbJ Bangkok variant. Hb genotypes of these patients were β 41-42 /β J Bangkok and β N /β J Bangkok , and the content of HbJ Bangkok was 93.9% and 52.4%, respectively. The remaining three patients had the following: HbE (β N /β E Hb genotype, 23.6% HbE content), HbG Taipei (β N /β G Taipei Hb genotype, 39.4% HbG Taipei content), and α-thalassemia HbH (6.1% HbH content, 2.8% Hb Bart's content). In the patients with β-thalassemia and HbJ Bangkok variants, the presence of the variants interfered with the results of HbA1c analyses using IE-HPLC and TINIA; in the remaining four patients, there was interference with the results of HbA1c IE-HPLC but not with the TINIA assay. There was no interference with BA-HPLC HbA1c results. HbJ Bangkok, HbE, HbG Taipei Hb, and α-thalassemia HbH disease cause varying degrees of interference with the analysis of HbA1c using IE-HPLC. In these patients, we suggest using methods free from such interference for the analysis of HbA1c and other indicators to monitor blood glucose levels. © 2017 Wiley Periodicals, Inc.

  11. High perfomance liquid chromatography in pharmaceutical analyses.

    Science.gov (United States)

    Nikolin, Branko; Imamović, Belma; Medanhodzić-Vuk, Saira; Sober, Miroslav

    2004-05-01

    compounds often present in concentrations much greater than those of analyte. Analiyte concentrations are often low, and in the case of drugs, the endogenous compounds are sometimes structurally very similar to the drug to be measured. The binding of drugs to the plasma protein also may occur which decreases the amount of free compound that is measured. To undertake the analyses of drugs and metabolites in body fluids the analyst is facet with several problems. The first problem is due to the complex nature of the body fluid, the drugs must be isolated by an extraction technique, which ideally should provide a relatively clean extract, and the separation system must be capable of resolving the drugs of interest from co extractives. All mentioned when we are using high performance liquid chromatography require good selections of detectors, good stationary phase, eluents and adequate program during separation. UV/VIS detector is the most versatile detector used in high performance liquid chromatography it is not always ideal since it is lack of specificity means high resolution of the analyte that may be required. UV detection is preferred since it offers excellent linearity and rapid quantitative analyses can be performed against a single standard of the drug being determined. Diode array and rapid scanning detector are useful for peak identification and monitoring peak purity but they are somewhat less sensitive then single wavelength detectors. In liquid chromatography some components may have a poor UV chromophores if UV detection is being used or be completely retained on the liquid chromatography column. Fluorescence and electrochemical detector are not only considerably more sensitive towed appropriate analytes but also more selective than UV detectors for many compounds. If at all possible fluorescence detectors are sensitive, stable, selective and easy to operate. It is selectivity shows itself in the lack of frontal components observed in plasma extract whereas

  12. Study the Effect of the Flow on the Performance of a shell and Tube Type Heat Exchanger using Experimental Design Technique

    Directory of Open Access Journals (Sweden)

    Zuher Hassan Abdullah

    2016-10-01

    Full Text Available In the current research an experimental study was done to show the effect of pulse flow on the effectiveness of shell and tube type heat exchanger. the study was in the case of steady and pulse flows with a changing mass flow rate of hot water flowing inside the pipes of the heat exchanger for the range between (0.0273-0.0819 kg / s  at fix mass flow rate of cold water that flows through the shell and on the outer surface of the pipes when (0.0416 kg / s, to obtain pulsing a used was solenoid valve. The research aims to measure the percentage effect of independent factors which were presenting the mass flow rate of hot water, flow type and the surrounding environment conditions of the experimental side upon shell and tube type heat exchanger performance using experimental design technique at the significant level (0.05.The results derived from the experimental tests showed that pulse flow leads to increase internal heat transfer coefficient (hi comparing with its value in the steady flow and the highest increase was by (9.75% at a mass flow rate of hot water (0.0416 kg / s and increases the overall heat transfer coefficient (U, where the highest percentage was by 4.68% at a mass flow rate of hot water (0.0416kg/s. The results also showed increasing both the number of transmitted units (NTU and the effectiveness of the shell and tube type heat exchanger ( in the case of pulse flow of its value in the steady flow and the highest percentage of increase occurring was (4.75% and (1.85%, respectively, and at the mass flow rate of hot water (0.0416 kg / s. Percentage effect of mass flow rate of hot water was (97%, 97.42%, 95.5%, 99.48% and the percentage effect of each flow type and the errors were (2.8%, 2.25%, 2.44%, 0.4% and (0. 2, 0.33%, 2.06%, 0.12 respectively

  13. High performance liquid chromatography in pharmaceutical analyses

    Directory of Open Access Journals (Sweden)

    Branko Nikolin

    2004-05-01

    serum contains numerous endogenous compounds often present in concentrations much greater than those of analyte. Analiyte concentrations are often low, and in the case of drugs, the endogenous compounds are sometimes structurally very similar to the drug to be measured. The binding of drugs to the plasma protein also may occur which decreases the amount of free compound that is measured. To undertake the analyses of drugs and metabolites in body fluids the analyst is facet with several problems. The first problem is due to the complex nature of the body fluid, the drugs must be isolated by an extraction technique, which ideally should provide a relatively clean extract, and the separation system must be capable of resolving the drugs of interest from co extractives. All mentioned when we are using high performance liquid chromatography require good selections of detectors, good stationary phase, eluents and adequate program during separation. UV/VIS detector is the most versatile detector used in high performance liquid chromatography it is not always ideal since it is lack of specificity means high resolution of the analyte that may be required. UV detection is preferred since it offers excellent linearity and rapid quantitative analyses can be performed against a single standard of the drug being determined. Diode array and rapid scanning detector are useful for peak identification and monitoring peak purity but they are somewhat less sensitive then single wavelength detectors. In liquid chromatography some components may have a poor UV chromophores if UV detection is being used or be completely retained on the liquid chromatography column. Fluorescence and electrochemical detector are not only considerably more sensitive towed appropriate analytes but also more selective than UV detectors for many compounds. If at all possible fluorescence detectors are sensitive, stable, selective and easy to operate. It is selectivity shows itself in the lack of frontal

  14. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

  15. Application of the zone-melting technique to metal chelate systems-VI A new apparatus for zone-melting chromatography.

    Science.gov (United States)

    Maeda, S; Kobayashi, H; Ueno, K

    1973-07-01

    An improved apparatus has been constructed for zone-melting chromatography. An essential feature of the apparatus is that the length of the molten zone can be kept constant during a zone-melting operation, by employing heating and cooling compartments which are separated from each other by double partition plates. Each compartment is heated or cooled with jets of hot or cold air. The apparatus is suitable for organic materials melting in the range between 40 degrees and 180 degrees . The distribution of metal ion along the column after zone melting of copper acetylacetonate in 2-methoxynaphthalene was a smooth curve. The plot of the position of maximum concentration, x(max), against the number of zone passes, n, gave a relationship in accordance with theoretical prediction.

  16. ANALYSIS AND IDENTIFICATION SPIKING CHEMICAL COMPOUNDS RELATED TO CHEMICAL WEAPON CONVENTION IN UNKNOWN WATER SAMPLES USING GAS CHROMATOGRAPHY AND GAS CHROMATOGRAPHY ELECTRON IONIZATION MASS SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2010-06-01

    Full Text Available The identification and analysis of chemical warfare agents and their degradation products is one of important component for the implementation of the convention. Nowadays, the analytical method for determination chemical warfare agent and their degradation products has been developing and improving. In order to get the sufficient analytical data as recommended by OPCW especially in Proficiency Testing, the spiking chemical compounds related to Chemical Weapon Convention in unknown water sample were determined using two different techniques such as gas chromatography and gas chromatography electron-impact ionization mass spectrometry. Neutral organic extraction, pH 11 organic extraction, cation exchanged-methylation, triethylamine/methanol-silylation were performed to extract the chemical warfare agents from the sample, before analyzing with gas chromatography. The identification of chemical warfare agents was carried out by comparing the mass spectrum of chemicals with mass spectrum reference from the OPCW Central Analytical Database (OCAD library while the retention indices calculation obtained from gas chromatography analysis was used to get the confirmation and supported data of  the chemical warfare agents. Diisopropyl methylphosphonate, 2,2-diphenyl-2-hydroacetic acid and 3-quinuclidinol were found in unknown water sample. Those chemicals were classified in schedule 2 as precursor or reactant of chemical weapons compound in schedule list of Chemical Weapon Convention.   Keywords: gas chromatography, mass spectrometry, retention indices, OCAD library, chemical warfare agents

  17. Development of an air bleeding technique and specific duration to improve the CO tolerance of proton-exchange membrane fuel cells

    International Nuclear Information System (INIS)

    Chung, Chen-Chung; Chen, Chiun-Hsun; Weng, De-Zheng

    2009-01-01

    This study investigated transient CO poisoning of a proton-exchange membrane fuel cell under either a fixed cell voltage or fixed current density. During CO poisoning tests, the cell performance decreases over time. Experiments were performed to identify which method yields better performance in CO poisoning tests. The results revealed that a change in cell voltage did not affect the stable polarization behavior after CO poisoning of the cell. On the other hand, a higher fixed current density yielded better tolerance of 52.7 ppm CO. The air bleeding technique was then applied using different timings for air introduction during CO poisoning tests. Air bleeding significantly improved the CO tolerance of the cell and recovered the performance after poisoning, regardless of the timing of air introduction. The effects of different anode catalyst materials on cell performance were also investigated during poisoning tests. Without air bleeding, a Pt-Ru alloy catalyst exhibited better CO tolerance than a pure Pt catalyst. However, the air bleeding technique can effectively increase the CO tolerance of cells regardless of the type of catalyst used.

  18. Direct analysis of ultra-trace semiconductor gas by inductively coupled plasma mass spectrometry coupled with gas to particle conversion-gas exchange technique.

    Science.gov (United States)

    Ohata, Masaki; Sakurai, Hiromu; Nishiguchi, Kohei; Utani, Keisuke; Günther, Detlef

    2015-09-03

    An inductively coupled plasma mass spectrometry (ICPMS) coupled with gas to particle conversion-gas exchange technique was applied to the direct analysis of ultra-trace semiconductor gas in ambient air. The ultra-trace semiconductor gases such as arsine (AsH3) and phosphine (PH3) were converted to particles by reaction with ozone (O3) and ammonia (NH3) gases within a gas to particle conversion device (GPD). The converted particles were directly introduced and measured by ICPMS through a gas exchange device (GED), which could penetrate the particles as well as exchange to Ar from either non-reacted gases such as an air or remaining gases of O3 and NH3. The particle size distribution of converted particles was measured by scanning mobility particle sizer (SMPS) and the results supported the elucidation of particle agglomeration between the particle converted from semiconductor gas and the particle of ammonium nitrate (NH4NO3) which was produced as major particle in GPD. Stable time-resolved signals from AsH3 and PH3 in air were obtained by GPD-GED-ICPMS with continuous gas introduction; however, the slightly larger fluctuation, which could be due to the ionization fluctuation of particles in ICP, was observed compared to that of metal carbonyl gas in Ar introduced directly into ICPMS. The linear regression lines were obtained and the limits of detection (LODs) of 1.5 pL L(-1) and 2.4 nL L(-1) for AsH3 and PH3, respectively, were estimated. Since these LODs revealed sufficiently lower values than the measurement concentrations required from semiconductor industry such as 0.5 nL L(-1) and 30 nL L(-1) for AsH3 and PH3, respectively, the GPD-GED-ICPMS could be useful for direct and high sensitive analysis of ultra-trace semiconductor gas in air. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. A novel approach to measure elemental concentrations in cation exchange resins using XRF-scanning technique, and its potential in water pollution studies

    Science.gov (United States)

    Huang, Jyh-Jaan; Lin, Sheng-Chi; Löwemark, Ludvig; Liou, Ya-Hsuan; Chang, Queenie; Chang, Tsun-Kuo; Wei, Kuo-Yen; Croudace, Ian W.

    2016-04-01

    X-ray fluorescence (XRF) core-scanning is a fast, and convenient technique to assess elemental variations for a wide variety of research topics. However, the XRF scanning counts are often considered a semi-quantitative measurement due to possible absorption or scattering caused by down core variability in physical properties. To overcome this problem and extend the applications of XRF-scanning to water pollution studies, we propose to use cation exchange resin (IR-120) as an "elemental carrier", and to analyze the resins using the Itrax-XRF core scanner. The use of resin minimizes the matrix effects during the measurements, and can be employed in the field in great numbers due to its low price. Therefore, the fast, and non-destructive XRF-scanning technique can provide a quick and economical method to analyze environmental pollution via absorption in the resin. Five standard resin samples were scanned by the Itrax-XRF core scanner at different exposure times (1 s, 5 s, 15 s, 30 s, 100 s) to allow the comparisons of scanning counts with the absolute concentrations. The regression lines and correlation coefficients of elements that are generally used in pollution studies (Ca, Ti, Cr, Ni, Cu, Zn, and Pb) were examined for the different exposure times. The result shows that within the test range (from few ppm to thousands ppm), the correlation coefficients are all higher than 0.97, even at the shortest exposure time (1 s). Therefore, we propose to use this method in the field to monitor for example sewage disposal events. The low price of resin, and fast, multi elements and precise XRF-scanning technique provide a viable, cost- and time-effective approach that allows large sample numbers to be processed. In this way, the properties and sources of wastewater pollution can be traced for the purpose of environmental monitoring and environmental forensics.

  20. Boron isotopic enrichment by displacement chromatography

    International Nuclear Information System (INIS)

    Mohapatra, K.K.; Bose, Arun

    2014-01-01

    10 B enriched boron is used in applications requiring high volumetric neutron absorption (absorption cross section- 3837 barn for thermal and 1 barn for 1 MeV fast neutron). It is used in fast breeder reactor (as control rod material), in neutron counter, in Boron Neutron Capture Therapy etc. Owing to very small separation factor, boron isotopic enrichment is a complex process requiring large number of separation stages. Heavy Water Board has ventured in industrial scale production of 10 B enriched boron using Exchange Distillation Process as well as Ion Displacement Chromatography Process. Ion Displacement Chromatography process is used in Boron Enrichment Plant at HWP, Manuguru. It is based on isotopic exchange between borate ions (B(OH) 4 - ) on anion exchange resin and boric acid passing through resin. The isotopic exchange takes place due to difference in zero point energy of 10 B and 11 B

  1. Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

    2017-05-12

    A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Comparative study of different clean-up techniques for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with electron capture detection.

    Science.gov (United States)

    Muhamad, Halimah; Zainudin, Badrul Hisyam; Abu Bakar, Nor Kartini

    2012-10-15

    Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 μg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia. Copyright © 2012 Elsevier Ltd. All rights reserved.

  3. Separation of Transfer Ribonucleic Acids by Reverse Phase Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Kelmers, A. D.; Novelli, G. David; Stulberg, M. P.

    1965-10-01

    Numerous experimental techniques for the separation of transfer ribonucleic acids have been successful in preparing partially purified fractions of several specific t-RNAs. Many of the existing methods have depended upon the differential solubility of specific t-RNAs in complex two-phase systems (1-6) and the separation was achieved by means of counter-current extraction techniques. Column chromatography experiments using cellulose exchangers, (7,8) methylated albumin (9,10) or with solvent phases supported on inert material (11-13) have also shown partial separation of specific t-RNAs. Paper chromatographic procedures have produced partial resolutions of t-RNA.14 Methods involving chemical treatment of specific t-RNAs have been reported (15-19).

  4. Selectivity in microemulsion electrokinetic chromatography

    DEFF Research Database (Denmark)

    Pedersen-Bjergaard, S; Gabel-Jensen, Charlotte; Honoré Hansen, S

    2000-01-01

    Microemulsion electrokinetic chromatography (MEEKC) is a most promising separation technique providing good selectivity and high separation efficiency of anionic, cationic as well as neutral solutes. In MEEKC lipophilic organic solvents dispersed as tiny droplets in an aqueous buffer by the use...

  5. Liquid chromatography in migration studies

    International Nuclear Information System (INIS)

    Carlsen, L.; Batsberg, W.

    1982-01-01

    Liquid chromatography ahs been suggested as a facile experimental technique to determine important physico-chemical properties, as permeability, porosity, dispersion-, diffusion-, and sorption charcteristics for geological material as chalk samples. The feasibility of the trechnique as a rapid method to evaluate the possible influence of changes in ground water composition on the migration behavior of radionuclides has been demonstrated

  6. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    International Nuclear Information System (INIS)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H.

    2005-12-01

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here

  7. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  8. Detailed characterization of bio-oil from pyrolysis of non-edible seed-cakes by Fourier Transform Infrared Spectroscopy (FTIR) and gas chromatography mass spectrometry (GC-MS) techniques.

    Science.gov (United States)

    Sugumaran, Vatsala; Prakash, Shanti; Ramu, Emmandi; Arora, Ajay Kumar; Bansal, Veena; Kagdiyal, Vivekanand; Saxena, Deepak

    2017-07-15

    Bio-oil obtained from pyrolysis is highly complicated mixture with valued chemicals. In order to reduce the complexity for unambiguous characterization of components present in bio-oil, solvent extractions using different solvents with increasing polarity have been adopted. The fractions have been analyzed by Fourier transform infrared (FTIR) spectroscopy for identifying the functional groups and Gas chromatography-mass spectrometry (GC-MS), for detailed characterization of components present in various fractions, thereby providing in-depth information at molecular level of various components in bio-oil. This paper reveals the potential of the analytical techniques in identification and brings out the similarities as well as differences in the components present in the bio-oil obtained from two non-edible oil seed-cakes, viz., Jatropha and Karanjia. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Étude de la technique d'échange ionique avec compétition. Cas du dépôt de platine sur support solide acide par échange cationique Research on the Ion Exchange Technique with Competition. Case of Platinum Deposit on a Solid Acid Support by Cation Exchange

    Directory of Open Access Journals (Sweden)

    Ribeiro F.

    2006-11-01

    Full Text Available Cet article présente une étude détaillée de la technique de dépôt de platine sur support acide par échange cationique avec compétition. Cette technique permet d'obtenir à la fois une dispersion quasi atomique et une répartition macroscopique homogène du métal sur la surface du solide. En l'absence de limitations diffusionnelles extra-granulaires, les résultats expérimentaux sont en bon accord avec les prévisions théoriques . This article is a detailed examination of the technique of depositing platinum on an acid support by cation exchange with compétition. This technique produces both a quasi-atomic dispersion and a homogeneous macroscopic distribution of the métal onthe surface of the solid. In the absence of extragranular diffusion limitations, experimental findings are in good agreement with theoretical predictions.

  10. A novel extraction technique based on carbon nanotubes reinforced hollow fiber solid/liquid microextraction for the measurement of piroxicam and diclofenac combined with high performance liquid chromatography.

    Science.gov (United States)

    Song, Xin-Yue; Shi, Yan-Ping; Chen, Juan

    2012-10-15

    A novel design of carbon nanotubes reinforced hollow fiber solid/liquid phase microextraction (CNTs-HF-SLPME) was developed to determine piroxicam and diclofenac in different real water samples. Functionalized multi-walled carbon nanotubes (MWCNTs) were held in the pores of hollow fiber with sol-gel technology. The pores and lumen of carbon nanotubes reinforced hollow fiber were subsequently filled with a μL volume of organic solvent (1-octanol), and then the whole assembly was used for the extraction of the target analytes in direct immersion sampling mode. The target analytes were extracted from the sample by two extractants, one of which is organic solvent placed inside the pores and lumen of hollow fiber and the other one is CNTs held in the pores of hollow fiber. After extraction, the analytes were desorbed in acetonitrile and analyzed using high performance liquid chromatography. This novel extraction mode showed more excellent extraction performance in comparison with conventional hollow fiber liquid microextraction (without adding CNTs) and carbon nanotubes reinforced hollow fiber solid microextraction (CNTs held in the pores of hollow fiber, but no organic solvents placed inside the lumen of hollow fiber) under the respective optimum conditions. This method provided 47- and 184-fold enrichment factors for piroxicam and diclofenac, respectively, good inter-fiber repeatability and batch-to-batch reproducibility. Linearity was observed in the range of 20-960 μg L(-1) for piroxicam, and 10-2560 μg L(-1) for diclofenac, with correlation coefficients of 0.9985 and 0.9989, respectively. The limits of detection were 4.58 μg L(-1) for piroxicam and 0.40 μg L(-1) for diclofenac. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Determination of Phenolic Acids and Flavonoids in Taraxacum formosanum Kitam by Liquid Chromatography-Tandem Mass Spectrometry Coupled with a Post-Column Derivatization Technique

    Directory of Open Access Journals (Sweden)

    Hung-Ju Chen

    2011-12-01

    Full Text Available A liquid chromatography-tandem mass spectrometry method (LC-MS/MS was developed for the determination of phenolic acids and flavonoids in a medicinal Chinese herb Taraxacum formosanum Kitam. Initially, both phenolic acids and flavonoids were extracted with 50% ethanol in a water-bath at 60 °C for 3 h and eventually separated into acidic fraction and neutral fraction by using a C18 cartridge. A total of 29 compounds were separated within 68 min by employing a Gemini C18 column and a gradient solvent system of 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. Based on the retention behavior as well as absorption and mass spectra, 19 phenolic acids and 10 flavonoids were identified and quantified in T. formosanum, with the former ranging from 14.1 μg/g to 10,870.4 μg/g, and the latter from 9.9 μg/g to 325.8 μg/g. For further identification of flavonoids, a post-column derivatization method involving shift reagents such as sodium acetate or aluminum chloride was used and the absorption spectral characteristics without or with shift reagents were compared. An internal standard syringic acid was used for quantitation of phenolic acids, whereas (± naringenin was found suitable for quantitation of flavonoids. The developed LC-MS/MS method showed high reproducibility, as evident from the relative standard deviation (RSD values for intra-day and inter-day variability being 1.0–6.8% and 2.0–7.7% for phenolic acids and 3.7–7.4% and 1.5–8.1% for flavonoids, respectively, and thus may be applied for simultaneous determination of phenolic acids and flavonoids in Chinese herb and nutraceuticals.

  12. Thermal Stability of Oil Palm Empty Fruit Bunch (OPEFB) Nanocrystalline Cellulose: Effects of post-treatment of oven drying and solvent exchange techniques

    International Nuclear Information System (INIS)

    Indarti, E; Wanrosli, W D; Marwan

    2015-01-01

    Nanocrystallinecellulose (NCC) from biomass is a promising material with huge potentials in various applications. A big challenge in its utilization is the agglomeration of the NCC's during processing due to hydrogen bonding among the cellulose chains when in close proximity to each other. Obtaining NCC's in a non-agglomerated and non-aqueous condition is challenging. In the present work NCC's was isolated from oil palm empty fruit bunch (OPEFB) using TEMPO-oxidation reaction method. To obtain non-agglomerated and non-aqueous products, the NCC's underwent post-treatment using oven drying (OD) and solvent exchanged (SE) techniques. The thermal stability of all samples was determined from TGA and DTG profiles whilst FTIR was used to analyzethe chemical modifications that occurred under these conditions. NCC-SE has better thermal stability than the NCC-OD and its on-set degradation temperature and residue are also higher. FTIR analysis shows that NCC-SE has a slightly different chemical composition whereby the absorption band at 1300 cm -1 (due to C-O symmetric stretching) is absent as compared to NCC-OD indicating that in NCC-SE the carboxylate group is in acid form which contribute to its thermal stability (paper)

  13. Multiplex gas chromatography

    Science.gov (United States)

    Valentin, Jose R.

    1990-01-01

    The principles of the multiplex gas chromatography (GC) technique, which is a possible candidate for chemical analysis of planetary atmospheres, are discussed. Particular attention is given to the chemical modulators developed by present investigators for multiplex GC, namely, the thermal-desorption, thermal-decomposition, and catalytic modulators, as well as to mechanical modulators. The basic technique of multiplex GC using chemical modulators and a mechanical modulator is demonstrated. It is shown that, with the chemical modulators, only one gas stream consisting of the carrier in combination with the components is being analyzed, resulting in a simplified instrument that requires relatively few consumables. The mechanical modulator demonstrated a direct application of multiplex GC for the analysis of gases in atmosphere of Titan at very low pressures.

  14. Advances in chromatography of the rare earth elements (review)

    International Nuclear Information System (INIS)

    Oguma, Koichi; Kuroda, Rokuro; Shimizu, Tsuneo.

    1995-01-01

    A review is presented which covers liquid chromatography, gas chromatography, and related techniques. This article intends to describe the chromatographic methods playing an important role in the separation of the rare earth elements. Special attention is paid to the usefulness of various types of liquid chromatography which enable the complete mutual separation of the rare earth elements. Applications are also discussed. (author) 161 refs

  15. The tritium labelling of organic molecules by heterogeneous catalytic exchange

    International Nuclear Information System (INIS)

    Angoso, M.; Kaiser, F.

    1977-01-01

    The influence of the temperature at 65degC and 120degC on the labelling of three organic molecules with tritium was studied. The compounds were: benzoic acid, diphenyl glioxal and 2,3-tetramethylene-4-phenylthien-7-oxodiacetin. The method employed was the heterogeneous catalytic exchange between tritiaded water and the organic compound. The purification was made by thin-layer chromatography and the concentration, purity and specific activity of the products were determined by counting and ultraviolet techniques. The thermal stability and the radiolitic effects on labelled benzoic acid were also considered. (author) [es

  16. The tritium labelling of organic molecules by heterogeneous catalytic exchange

    International Nuclear Information System (INIS)

    Angoso Marina, M.; Kaiser Ruiz del Olmo, F.

    1977-01-01

    The influence of the temperature at 65 degree centigree and 120 degree centigree on the labelling of three organic molecules with tritium was studied. The compounds were: benzoic acid, de phenyl glyoxal and 2,3-tetramethylene-4-pantothenyl-7-oxo diacetin.The method employed was the heterogeneous catalytic exchange between tritiated water and the organic compound. The purification was made by thin-layer chromatography and the concentration, purity and specific activity of the products were determined by counting and ultraviolet techniques. The thermal stability and the radiolytic effects on labelled benzoic acid were also considered. (Author) 9 refs

  17. UHPLC: The Greening Face of Liquid Chromatography

    OpenAIRE

    Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

  18. Ultra-performance liquid chromatography MS/MS method for the determination of parabens in compost from sewage sludge: comparison of the efficiency of two extraction techniques.

    Science.gov (United States)

    Benítez-Villalba, Julio César; Zafra-Gómez, Alberto; Dorival-García, Noemí; Camino-Sánchez, Francisco Javier; Cantarero, Samuel; Vílchez, José Luis

    2013-08-01

    The efficiency of two extraction techniques--ultrasound-assisted extraction and pressurized liquid extraction--are compared and evaluated in the determination of parabens in compost samples. The extraction parameters for each technique were accurately optimized. The selected compounds were detected and quantified using ultra-performance LC MS/MS, operating in negative ESI and in SRM mode. The analytes were separated in less than 5 min. Ethylparaben (ring-(13)C6 labeled) was used as an internal standard. Two selective, sensitive, and accurate analytical methods were developed and validated. The LODs of the methods ranged from 3 to 7 ng/g and the LOQs from 10 to 23 ng/g, while inter- and intraday variability was under 6% in all cases. The methods were validated separately by using matrix-matched calibration and recovery assays with spiked samples. Recovery rates ranged from 94.0 to 105.0%. Compost samples were taken from different composting plants. Although the statistical comparison demonstrated no statistically significant differences between the two extraction techniques, the method based on pressurized liquid extraction was more sensitive than the ultrasound extraction based method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Nuclear magnetic resonance and high-performance liquid chromatography techniques for the characterization of bioactive compounds from Humulus lupulus L. (hop).

    Science.gov (United States)

    Bertelli, Davide; Brighenti, Virginia; Marchetti, Lucia; Reik, Anna; Pellati, Federica

    2018-06-01

    Humulus lupulus L. (hop) represents one of the most cultivated crops, it being a key ingredient in the brewing process. Many health-related properties have been described for hop extracts, making this plant gain more interest in the field of pharmaceutical and nutraceutical research. Among the analytical tools available for the phytochemical characterization of plant extracts, quantitative nuclear magnetic resonance (qNMR) represents a new and powerful technique. In this ambit, the present study was aimed at the development of a new, simple, and efficient qNMR method for the metabolite fingerprinting of bioactive compounds in hop cones, taking advantage of the novel ERETIC 2 tool. To the best of our knowledge, this is the first attempt to apply this method to complex matrices of natural origin, such as hop extracts. The qNMR method set up in this study was applied to the quantification of both prenylflavonoids and bitter acids in eight hop cultivars. The performance of this analytical method was compared with that of HPLC-UV/DAD, which represents the most frequently used technique in the field of natural product analysis. The quantitative data obtained for hop samples by means of the two aforementioned techniques highlighted that the amount of bioactive compounds was slightly higher when qNMR was applied, although the order of magnitude of the values was the same. The accuracy of qNMR was comparable to that of the chromatographic method, thus proving to be a reliable tool for the analysis of these secondary metabolites in hop extracts. Graphical abstract Graphical abstract related to the extraction and analytical methods applied in this work for the analysis of bioactive compounds in Humulus lupulus L. (hop) cones.

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

    Science.gov (United States)

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

    2017-09-05

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

  1. Continuous-flow IRMS technique for determining the 17O excess of CO2 using complete oxygen isotope exchange with cerium oxide

    NARCIS (Netherlands)

    Mrozek, D. J.; Van Der Veen, C.; Kliphuis, M.; Kaiser, J.; Wiegel, A. A.; Röckmann, T.

    2015-01-01

    This paper presents an analytical system for analysis of all single substituted isotopologues (12C16O17O, 12C16O18O, 13C16O16O) in nanomolar quantities of CO2 extracted from atmospheric air samples. CO2 is separated from bulk air by gas chromatography and CO2 isotope ratio measurements (ion masses

  2. Studies on the preparation of thallium-201 by irradiating mercury with protons using extraction chromatography technique to separate thallium from mercury

    International Nuclear Information System (INIS)

    Fernandes, L.

    1990-01-01

    Radionuclide sup(201)Tl is used in Nuclear Medicine to identify myocardial ischemia or myocardial infarct. It is a cyclotron-produced radioisotope, obtained indirectly from the decay of sup(202)Pb or directly by irradiating mercury with deuterons or protons. The usual technique to prepare sup(201)Tl makes use of the nuclear reaction: sup(203)(p,3n) → sup(201)Tl, which requires proton energy of around 28 MeV. Due to the limited proton energy of IPEN'S CV-28 cyclotron, studies on the irradiating conditions of natural mercury oxide pellets and drops of natural mercury metal were made in the range of 19 - 24 MeV. At the end of the bombardment of a 6 MeV thickness target of natural mercury metal with 19 MeV protons around 10 MBq sup(201)Tl/μ A h was obtained. (author)

  3. Report: Affinity Chromatography.

    Science.gov (United States)

    Walters, Rodney R.

    1985-01-01

    Supports, affinity ligands, immobilization, elution methods, and a number of applications are among the topics considered in this discussion of affinity chromatography. An outline of the basic principles of affinity chromatography is included. (JN)

  4. Kinetic ion exchange studies in ultramarines by the radioactive tracer method; Etudes cinetiques d'echanges d'ions dans les outremers par la technique des traceurs radioactifs

    Energy Technology Data Exchange (ETDEWEB)

    May, S; Goenvec, H; Pinte, G [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    The possibility of ion exchanges in various ultramarines has been studied in the aqueous phase. The kinetics of the exchange reactions is followed by studying the behaviour of a radioactive ion, either in the solution of the exchanging salt or in the ultramarine itself. The sodium in the make-up of the ultramarine, is found to exchange with various ions in solution. The reaction speeds appear to be governed by a diffusion process inside the grains of ultramarine. The diffusion coefficients and the activation energies are determined for the exchanges studied. Several exchange studies were carried out in an organic medium. The kinetics of ion exchange is also investigated in ultramarines from which most of the constituent sulphur has been eliminated. The results obtained in these ultramarines are compared with the exchange kinetics of the same ions in ordinary ultramarine. (author) [French] Nous avons etudie la possibilite d'echanges ioniques dans differents outremers, en phase aqueuse. L'etude cinetique des reactions d'echanges est suivie en etudiant le comportement d'ion radioactif, soit dans la solution du sel echangeant, soit dans l'outremer lui-meme. C'est le sodium de constitution de l'outremer qui s'echange avec differents ions en solution. Les vitesses de reactions semblent etre controlees par un processus de diffusion a l'interieur des grains d'outremer. Les coefficients de diffusion et les energies d'activation sont determines pour les echanges etudies. Quelques etudes sont realisees en milieu organique ou quelques echanges ont ete etudies. La cinetique d'echange d'ions est egalement etudie dans des outremers dans lesquels la majorite du soufre de constitution a ete eliminee. On compare les resultats obtenus dans ces outremers avec les cinetiques d'echanges des memes ions dans l'outremer ordinaire. (auteur)

  5. Chromatography on cellulose exchangers - microdetermination of Fe/sup 3 +/, UO/sub 2//sup 2 +/ and Cu/sup 2 +/ ions in aqueous solutions by means of small seperation columns

    Energy Technology Data Exchange (ETDEWEB)

    Barba, P; Lieser, K H [Technische Hochschule Darmstadt (Germany, F.R.). Fachbereich Anorganische Chemie und Kernchemie

    1978-07-01

    Small separation columns filled with a cellulose exchanger containing salicylic acid as anchor group are used for chromatographic determination of Fe/sup 3 +/, UO/sub 2//sup 2 +/, and Cu/sup 2 +/ in aqueous solutions. The preparation of the cellulose exchanger and the separation procedure are described. The detection limits are approximately /.2 ..mu..g Fe, 5 ..mu..g U and 10 ..mu..g Cu. Within certain concentration ranges chromatographic separation and simultaneous determination of several ions is possible, as shown by the examples Fe/sup 3 +//Cu/sup 2 +/ and UO/sub 2//sup 2 +//Cu/sup 2 +/.

  6. Analysis of the differentially expressed low molecular weight peptides in human serum via an N-terminal isotope labeling technique combining nano-liquid chromatography/matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Leng, Jiapeng; Zhu, Dong; Wu, Duojiao; Zhu, Tongyu; Zhao, Ningwei; Guo, Yinlong

    2012-11-15

    Peptidomics analysis of human serum is challenging due to the low abundance of serum peptides and interference from the complex matrix. This study analyzed the differentially expressed (DE) low molecular weight peptides in human serum integrating a DMPITC-based N-terminal isotope labeling technique with nano-liquid chromatography and matrix-assisted laser desorption/ionization mass spectrometry (nano-LC/MALDI-MS). The workflow introduced a [d(6)]-4,6-dimethoxypyrimidine-2-isothiocyanate (DMPITC)-labeled mixture of aliquots from test samples as the internal standard. The spiked [d(0)]-DMPITC-labeled samples were separated by nano-LC then spotted on the MALDI target. Both quantitative and qualitative studies for serum peptides were achieved based on the isotope-labeled peaks. The DMPITC labeling technique combined with nano-LC/MALDI-MS not only minimized the errors in peptide quantitation, but also allowed convenient recognition of the labeled peptides due to the 6 Da mass difference. The data showed that the entire research procedure as well as the subsequent data analysis method were effective, reproducible, and sensitive for the analysis of DE serum peptides. This study successfully established a research model for DE serum peptides using DMPITC-based N-terminal isotope labeling and nano-LC/MALDI-MS. Application of the DMPITC-based N-terminal labeling technique is expected to provide a promising tool for the investigation of peptides in vivo, especially for the analysis of DE peptides under different biological conditions. Copyright © 2012 John Wiley & Sons, Ltd.

  7. Separation of transfer ribonucleic acids on polystyrene anion exchangers

    Energy Technology Data Exchange (ETDEWEB)

    Singhal, R.P.; Griffin, G.D.; Novelli, G.D.

    1976-11-16

    The transfer RNA separation by chromatography on strong-base-polystyrene exchange materials is examined and compared with the widely used reversed-phase chromatography. Results indicate important differences in some transfer RNA (tRNA) elution patterns by the anion-exchange chromatography, as compared with the reversed-phase chromatography. Transfer RNAs containing hydrophobic groups are adsorbed more strongly. The anion exchanger has twice the number of theoretical plates. Single peaks of tRNA/sub 2//sup Glu/ and tRNA/sub 1//sup Phe/ obtained from the reversed-phase column give multiple peaks on polystyrene anion-exchange chromatography. All six leucine tRNAs (Escherichia coli) and differences in tRNA populations synthesized during early and late stages of the dividing lymphocytes from normal human blood can be characterized by the anion-exchange chromatography. Different separation profiles are obtained by two separation systems for tyrosine tRNAs from mouse liver and mouse-plasma-cell tumor. The results indicate that, in contrast to the reversed-phase chromatography, strong-base-polystyrene anion-exchange chromatography is capable of separating tRNAs with minor structural differences.

  8. An evaporation-assisted dispersive liquid-liquid microextraction technique as a simple tool for high performance liquid chromatography tandem-mass spectrometry determination of insecticides in wine.

    Science.gov (United States)

    Timofeeva, Irina; Kanashina, Daria; Moskvin, Leonid; Bulatov, Andrey

    2017-08-25

    A sample pre-treatment technique based on evaporation-assisted dispersive liquid-liquid microextraction (EVA-DLLME), followed by HPLC-MS/MS has been developed for the determination of organophosphate insecticides (malathion, diazinon, phosalone) in wine samples. The procedure includes the addition of mixture of organic solvents (with density higher than water), consisting of the extraction (low density) and volatile (high density) solvents, to aqueous sample followed by heating of the mixture obtained, what promotes the volatile solvent evaporation and moving extraction solvent droplets from down to top of the aqueous sample and, as a consequence, microextraction of target analytes. To initiate the evaporation process an initiator is required. It was established that hexanol (extraction solvent) and dichloromethane (volatile solvent) mixture (1:1, v/v) provides effective microextraction of the insecticides from wine samples with recovery from 92 to 103%. The conditions of insecticides' microextraction such as selection of extraction solvent, ratio of hexanol/dichloromethane and hexanol/sample, type and concentration of initiator, and effect of ethanol as one of the main components of wine have been studied. Under optimal experimental conditions the linear detection ranges were found to be 10 -7 -10 -3 gL -1 for malathion, 10 -9 -10 -4 gL -1 for diazinon, and 10 -6 -10 -2 gL -1 for phosalone. The LODs, calculated from a blank test, based on 3σ, found to be 3×10 -8 gL -1 for malathion, 3×10 -10 gL -1 for diazinon and 3×10 -7 gL -1 for phosalone. The advantages of EVA-DLLME are the rapidity, simplicity, high sample throughput and low cost. As an outcome, the analytical results agreed fairly well with the results obtained by a reference GC-MS method. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Analysis of sea water by difference chromatography. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Mangelsdorf, P.C. Jr.

    1977-02-01

    During the final period of this research contract the principal results obtained were: (a) the development of anion analysis by difference chromatography to the extent that SO/sub 4//sup =//Cl/sup -/ can be determined to better than 0.1 percent using an 0.5 ml seawater sample, (b) the determination of the ion-exchange cation complements of a variety of sediments in river water and in seawater, and (c) the discovery of a simple technique for the qualitative removal of NH/sub 4//sup +/ from seawater samples without altering the ratios of the other cations. This method supersedes the use of Cu-Chelex which has proved impossible to sustain.

  10. Applications of extraction chromatography in the development of radionuclide generator systems for nuclear medicine

    International Nuclear Information System (INIS)

    Dietz, M.L.; Horwitz, E.P.

    2000-01-01

    Numerous methods have been described for the separation and purification of radionuclides for application in diagnostic and therapeutic nuclear medicine, among them ion exchange, solvent extraction, and various forms of chromatography. Although extraction chromatography has previously been shown to provide a means of performing a number of separations of potential use in radionuclide generator systems, the application of the technique to generator development has thus far been limited. Recent work directed at improved methods for the determination of radionuclides in biological and environmental samples has led to the development of a series of novel extraction chromatographic resins exhibiting enhanced metal ion retention from strongly acidic media and excellent selectivity, among them materials suitable for the isolation of 212 Bi, 90 Y, and 213 Bi. These resins, along with extraction chromatographic materials employing functionalized supports to improve their physical stability or metal ion retention properties, are shown to offer promise in the development of improved radionuclide generators

  11. Chromatography on cellulose exchangers: microdetermination of Fe/sup 3 +/, UO/sub 2//sup 2 +/, and Cu/sup 2 +/ ions in aqueous solutions by means of small separation columns

    Energy Technology Data Exchange (ETDEWEB)

    Burba, P; Lieser, K H

    1978-01-01

    A study of the use of small separation columns filled with a cellulose exchanger containing salicylic acid as the anchor group for chromatographic determination of Fe/sup 3 +/ and Cu/sup 2 +/ in aqueous solution is described. The detection limits are Fe approx.0.2 and Cu 10 ..mu..g. The separation and simultaneous determination of several ions is possible.

  12. VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis. Program. Summary of reports

    International Nuclear Information System (INIS)

    2001-01-01

    Program and summary of reports of the VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis are performed. The meeting took place 15-19 October, 2001 in Moscow. Many problems of liquid and ion exchange chromatography, capillary electrophoresis, thin-layer chromatography have been discussed extensively. Reports covering properties of sorbents and devices for chromatography are incorporated in the collection [ru

  13. 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.

  14. Analytical chromatography. Methods, instrumentation and applications

    International Nuclear Information System (INIS)

    Yashin, Ya I; Yashin, A Ya

    2006-01-01

    The state-of-the-art and the prospects in the development of main methods of analytical chromatography, viz., gas, high performance liquid and ion chromatographic techniques, are characterised. Achievements of the past 10-15 years in the theory and general methodology of chromatography and also in the development of new sorbents, columns and chromatographic instruments are outlined. The use of chromatography in the environmental control, biology, medicine, pharmaceutics, and also for monitoring the quality of foodstuffs and products of chemical, petrochemical and gas industries, etc. is considered.

  15. Research of thermal stability of ion exchangers

    International Nuclear Information System (INIS)

    Stuchlik, S.; Srnkova, J.

    1983-01-01

    Prior to the fixation of radioactive ion exchangers into bitumen these exchangers have to be dried. The resulting gaseous products may generate explosive mixtures. An analysis was made of the thermal stability of two types of ion exchangers, the cation exchanger KU-2-8 cS and the anion exchanger AV-17-8 cS which are used in the V-1 nuclear power plant at Jaslovske Bohunice. The thermal stability of the anion exchangers was monitored using gas chromatography at temperatures of 100, 120, 140, 160 and 180 degC and by measuring weight loss by kiln-drying at temperatures of 120, 140, 160 and 180 degC. The ion exchanger was heated for 6 hours and samples were taken continuously at one hour intervals. The thermal stability of the cation exchanger was monitored by measuring the weight loss. Gas chromatography showed the release of trimethylamine from the anion exchanger in direct dependence on temperature. The measurement of weight losses, however, only showed higher losses of released products which are explained by the release of other thermally unstable products. The analysis of the thermal stability of the cation exchanger showed the release of SO 2 and the weight loss (following correction for water content) was found only after the fourth hour of decomposition. The experiment showed that the drying of anion exchanger AV-17-8 cS may cause the formation of explosive mixtures. (J.P.)

  16. Use of frontal analysis in ion exchange chromatography for the study of reactions of formation of complexes in solution. Application to hydrochloric complexes of nickel (II), cobalt (II) and copper (II)

    International Nuclear Information System (INIS)

    Tremillon, Bernard

    1959-01-01

    The ion exchanger column frontal analysis method provides a convenient way to study complex formation reactions when they are very unstable. It has the advantage of being much more sensitive and precise than the method (already used by other authors) of simple equilibrium between a solution and an ion exchanger. As an illustration of this method, the hydrochloric acid complexes NiCl + , CoCl + and CuCl + , have been studied, and their dissociation constants were determined (respectively 4.6 ± 0.1; 4.0 ± 0.1 and 2.5 ± 0.1, at an ionic strength substantially equal to 1.5). Reprint of a paper published in Bulletin de la Societe Chimique de France, 1958, p. 1483-1487 [fr

  17. Heat exchanger

    International Nuclear Information System (INIS)

    Dostatni, A.W.; Dostatni, Michel.

    1976-01-01

    In the main patent, a description was given of a heat exchanger with an exchange surface in preformed sheet metal designed for the high pressure and temperature service particularly encountered in nuclear pressurized water reactors and which is characterised by the fact that it is composed of at least one exchanger bundle sealed in a containment, the said bundle or bundles being composed of numerous juxtaposed individual compartments whose exchange faces are built of preformed sheet metal. The present addendun certificate concerns shapes of bundles and their positioning methods in the exchanger containment enabling its compactness to be increased [fr

  18. Automated exchange transfusion and exchange rate.

    Science.gov (United States)

    Funato, M; Shimada, S; Tamai, H; Taki, H; Yoshioka, Y

    1989-10-01

    An automated blood exchange transfusion (BET) with a two-site technique has been devised by Goldmann et al and by us, using an infusion pump. With this method, we successfully performed exchange transfusions 189 times in the past four years on 110 infants with birth weights ranging from 530 g to 4,000 g. The exchange rate by the automated method was compared with the rate by Diamond's method. Serum bilirubin (SB) levels before and after BET and the maximal SB rebound within 24 hours after BET were: 21.6 +/- 2.4, 11.5 +/- 2.2, and 15.0 +/- 1.5 mg/dl in the automated method, and 22.0 +/- 2.9, 11.2 +/- 2.5, and 17.7 +/- 3.2 mg/dl in Diamond's method, respectively. The result showed that the maximal rebound of the SB level within 24 hours after BET was significantly lower in the automated method than in Diamond's method (p less than 0.01), though SB levels before and after BET were not significantly different between the two methods. The exchange rate was also measured by means of staining the fetal red cells (F cells) both in the automated method and in Diamond's method, and comparing them. The exchange rate of F cells in Diamond's method went down along the theoretical exchange curve proposed by Diamond, while the rate in the automated method was significantly better than in Diamond's, especially in the early stage of BET (p less than 0.01). We believe that the use of this automated method may give better results than Diamond's method in the rate of exchange, because this method is performed with a two-site technique using a peripheral artery and vein.

  19. Ageing and structural effects on the sorption characteristics of Cd2+ by clinoptilolite and Y-type zeolite studied using isotope exchange technique

    International Nuclear Information System (INIS)

    Ahmed, I.A.M.; Young, S.D.; Crout, N.M.J.

    2010-01-01

    This research investigates the long-term kinetics of Cd 2+ sorption and desorption by calcium-exchanged clinoptilolite (CaCpt) and Y-type (CaY) zeolite using isotopic exchange with 109 Cd while maintaining pH at circumneutral values. The effects of Si/Al ratio and crystal structure of these zeolitic materials on intracrystalline transport of Cd are discussed. A first-order kinetic model was developed to describe the progressive transfer of Cd 2+ to a less reactive form within the zeolite structure, following initial sorption and subsequent desorption of Cd subject to different initial contact times. The kinetic model differentiates between two forms of sorbed Cd 2+ designated 'labile' and 'non-labile' in which the labile form is in immediate equilibrium with the free Cd 2+ ion activity in solution. A model combining diffusion and first-order kinetics for cation exchange was also employed to determine Cd 2+ diffusivity and intracrystalline exchange rates in CaY and CaCpt. The efficiency of Permeable Reactive Barriers (PRBs) containing zeolitic materials in protecting water systems against lateral flow of metal-contaminated leachate was simulated for three contrasting zeolites. The slow transfer of Cd between labile and non-labile forms was particularly important in moderating high concentration pulses of Cd traversing the PRB. In addition, the reversibility of Cd fixation effectively restored the sorption capability of the zeolite through slow leakage to drainage water.

  20. Determination of trace elements in high pure rare earth oxide by double focusing inductively coupled plasma mass spectrometry (HR ICP-MS) and high performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Pedreira Filho, Walter dos Reis

    2000-01-01

    Rare earth oxides are used in several technological fields whose applications can be observed in several areas of modern technology, among which are included: lasers, semiconductors semi, high purity materials and metallic alloys. The field of applications of the rare earth elements is quite wide. Several important industrial applications are ceramics, catalysts and metallurgical as well as research areas and high technology sectors. Such applications have been presenting an accentuated growth in the last years. Chemical characterization of rare earth oxides of high purity has been constituting one of the major challenges of analytical chemistry. Several analytical techniques were used for chemical characterization of high purity rare earth the oxides. Even so, those techniques present limitations when one needs to characterize materials of a high level of purity, as in the case of rare earth oxides. Some of those limitations are associated, for example, to spectral interference. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a powerful analytical tool for quantitative analysis of metal impurities in high purity materials. The Instituto de Pesquisas Energeticas e Nucleares (IPEN) has an unit of production and purification of rare earth oxides, with above 99,9% level of purity. In this work, the rare earth impurities were characterized in samples (La 2 O 3 ; CeO 2 ; Pr 6 O 11 ; Nd 2 O 3 ; Sm 2 O 3 ; Gd 2 O 3 ; Y 2 O 3 ) produced at the IPEN and certified standard materials produced by Johnson Matthey Chemical (JMC). The technique of high performance liquid chromatography (HPLC) was used in the separation of the impurities. Quantification of metallic impurities was carried out as inductively coupled plasma mass spectrometer (HR-ICP MS). In this work it is presented a new analytical methodology in the chemical characterization of metallic impurities in rare earth oxides of high purity (> 99,9%) with and without separation of the matrix. Analyses of standard

  1. Chromatography resin support

    Science.gov (United States)

    Dobos, James G.

    2002-01-01

    An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

  2. Development of high performance liquid chromatography for rapid determination of burn-up of nuclear fuels

    International Nuclear Information System (INIS)

    Joseph, M.; Karunasagar, D.; Saha, B.

    1996-01-01

    Burn-up an important parameter during evaluation of the performance of any nuclear fuel. Among the various techniques available, the preferred one for its determination is based on accurate measurement of a suitable fission product monitor and the residual heavy elements. Since isotopes of rare earth elements are generally used as burn-up monitors, conditions were standardized for rapid separation (within 15 minutes) of light rare earths using high performance liquid chromatography based on either anion exchange (Partisil 10 SAX) in methanol-nitric acid medium or by cation exchange on a reverse phase column (Spherisorb 5-ODS-2 or Supelcosil LC-18) dynamically modified with 1-octane sulfonate or camphor-10-sulfonic acid (β). Both these methods were assessed for separation of individual fission product rare earths from their mixtures. A new approach has been examined in detail for rapid assay of neodymium, which appears promising for faster and accurate measurement of burn-up. (author)

  3. Lipidomics by Supercritical Fluid Chromatography

    Directory of Open Access Journals (Sweden)

    Laurent Laboureur

    2015-06-01

    Full Text Available This review enlightens the role of supercritical fluid chromatography (SFC in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC. It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering or highly specific (mass spectrometry detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides defined by the LIPID MAPS consortium.

  4. Lipidomics by Supercritical Fluid Chromatography

    Science.gov (United States)

    Laboureur, Laurent; Ollero, Mario; Touboul, David

    2015-01-01

    This review enlightens the role of supercritical fluid chromatography (SFC) in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC). It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering) or highly specific (mass spectrometry) detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides) defined by the LIPID MAPS consortium. PMID:26090714

  5. A technique to simulate a tube break in a high-pressure gas/cooling water heat exchanger - HTR2008-58161

    International Nuclear Information System (INIS)

    Antwerpen, H. J. V.; Mulder, E. J.

    2008-01-01

    The gas cycles of most High Temperature Gas-Cooled Reactors (HTR's) reject heat to water at some stage. In the helium/water heat exchangers of HTR's with direct Brayton cycles, the helium is usually at a much higher pressure than the water. If the pressure boundary between the helium and the water fails inside the heat exchanger. the effect on the rest of the water system has to be established in order to do a proper system design. This can be done most efficiently by using a system simulation code, however, very few system simulation codes has the capability to do gas/liquid interface tracking as required for this problem. This study describes a calculation method with which a gas/liquid heat exchanger tube rupture can be calculated in a simulation code without interface tracking. The course of events after tube rupture is described and appropriate calculation models derived. A mathematical model for a pressure relief valve (PRV) was also created. The calculation models were implemented in the system simulation software Flownex and used to study a tube rupture on a 5000 kPa helium/water heat exchanger. The assembled calculation network solved stable and within reasonable time. The simulation provided insight into the course of events following the tube break. It was shown that the acceleration of water out of the helium cooler, by choked-flow helium, caused the main pressure pulses during the event. The maximum pressure in the water loop occurs on the opposite side of the helium cooler due to constructive interference of the initial pressure wave with itself. It was also shown that by changing only pipe lengths, the system could become prone to severe oscillations after a tube rupture event. (authors)

  6. Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

    International Nuclear Information System (INIS)

    Krupp, E.M.; Johnson, C.; Rechsteiner, C.; Moir, M.; Leong, D.; Feldmann, J.

    2007-01-01

    Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 μg/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 μg/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 μg As/m 3 natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes

  7. [Investigation of concentration levels of chromium(VI) in bottled mineral and spring waters by high performance ion chromatography technique with application of postcolumn reaction with 1,5-diphenylcarbazide and VIS detection].

    Science.gov (United States)

    Swiecicka, Dorota; Garboś, Sławomir

    2008-01-01

    The aim of this work was optimization and validation of the method of determination of Cr(VI) existing in the form of chromate(VI) in mineral and spring waters by High Performance Ion Chromatography (HPIC) technique with application of postcolumn reaction with 1,5-diphenylcarbazide and VIS detection. Optimization of the method performed with the use of initial apparatus parameters and chromatographic conditions from the Method 218.6 allowed to lowering detection limit for Cr(VI) from 400 ng/l to 2 ng/l. Thanks to very low detection limit achieved it was possible to determine of Cr(VI) concentrations in 25 mineral and spring waters presented at Polish market. In the cases of four mineral and spring waters analyzed, determined Cr(VI) concentrations were below of quantification limit (waters the concentrations of chromium(VI) were determined in the range of 5.6 - 1281 ng/l. The fact of existence of different Cr(VI) concentrations in investigated waters could be connected with secondary contamination of mineral and spring waters by chromium coming from metal installations and fittings. One should be underlined that even the highest determined concentration level of chromium(VI) was below of the maximum admissible concentration of total chromium presented in Polish Decree of Minister of Health from April 29th 2004. Therefore after taking into account determined in this work concentration of Cr(VI), the consumption of all waters analyzed in this study does not lead to essential human health risk.

  8. Application of pressurized ion exchange to separations of transplutonium elements

    International Nuclear Information System (INIS)

    Campbell, D.O.

    1980-01-01

    High-pressure ion exchange chromatography, used first for nucleic acid separations, was applied to the production of the heavier actinides, particularly the transcurium elements. Its use at the TRU plant is described. Future developments are considered briefly

  9. 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)

  10. Halogen speciation in volcanic plumes - Development of compact denuder sampling techniques with in-situ derivatization followed by gas chromatography-mass spectrometry and their application at Mt. Etna, Mt. Nyiragongo and Mt. Nyamulagira in 2015.

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2016-04-01

    products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography-mass spectrometry gives a limit of detection below 1 ng of bromine. The method was applied in 2015 on volcanic gas plumes at Mt. Etna (Italy), Mt. Nyiragongo and Mt. Nyamulagira (DR Congo) giving reactive bromine mixing ratios from 0.3 ppb (Nyiragongo) up to 22 ppb (Etna, NEC). Compared with total halogen data derived by alkaline trap sampling (Raschig-tube) and ion-chromatography analysis the reactive bromine mixing ratios allow the investigation of the conversion of HBr into reactive species due to plume chemistry with progressing plume age. The new method will be described in detail and the first results on the reactive halogen to total halogen output will be discussed (for bromine and chlorine) and compared to earlier volcanic plume chemistry model studies. References Bobrowski, N. and G. Giuffrida: Bromine monoxide / sulphur dioxide ratios in relation to volcanological observations at Mt. Etna 2006-2009. Solid Earth, 3, 433-445, 2012 Bobrowski, N., R. von Glasow, A. Aiuppa, S. Inguaggiato, I. Louban, O. W. Ibrahim and U. Platt: Reactive halogen chemistry in volcanic plumes. J. Geophys. Res., 112, 2007 Donovan A., V. Tsanev, C. Oppenheimer and M. Edmonds: Reactive halogens (BrO and OClO) detected in the plume of Soufrière Hills Volcano during an eruption hiatus. Geochem. Geophys. Geosyst., 15, 3346-3363, 2014 Rüdiger, J., N. Bobrowski, T. Hoffmann (2015), Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes (EGU2015-2392-2), EGU General Assembly 2015

  11. Microemulsion Electrokinetic Chromatography.

    Science.gov (United States)

    Buchberger, Wolfgang

    2016-01-01

    Microemulsion electrokinetic chromatography (MEEKC) is a special mode of capillary electrophoresis employing a microemulsion as carrier electrolyte. Analytes may partition between the aqueous phase of the microemulsion and its oil droplets which act as a pseudostationary phase. The technique is well suited for the separation of neutral species, in which case charged oil droplets (obtained by addition of an anionic or cationic surfactant) are present. A single set of separation parameters may be sufficient for separation of a wide range of analytes belonging to quite different chemical classes. Fine-tuning of resolution and analysis time may be achieved by addition of organic solvents, by changes in the nature of the surfactants (and cosurfactants) used to stabilize the microemulsion, or by various additives that may undergo some additional interactions with the analytes. Besides the separation of neutral analytes (which may be the most important application area of MEEKC), it can also be employed for cationic and/or anionic species. In this chapter, MEEKC conditions are summarized that have proven their reliability for routine analysis. Furthermore, the mechanisms encountered in MEEKC allow an efficient on-capillary preconcentration of analytes, so that the problem of poor concentration sensitivity of ultraviolet absorbance detection is circumvented.

  12. Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

    Science.gov (United States)

    Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

    2017-09-01

    A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. High-performance liquid chromatography - Ultraviolet method for the determination of total specific migration of nine ultraviolet absorbers in food simulants based on 1,1,3,3-Tetramethylguanidine and organic phase anion exchange solid phase extraction to remove glyceride.

    Science.gov (United States)

    Wang, Jianling; Xiao, Xiaofeng; Chen, Tong; Liu, Tingfei; Tao, Huaming; He, Jun

    2016-06-17

    The glyceride in oil food simulant usually causes serious interferences to target analytes and leads to failure of the normal function of the RP-HPLC column. In this work, a convenient HPLC-UV method for the determination of the total specific migration of nine ultraviolet (UV) absorbers in food simulants was developed based on 1,1,3,3-tetramethylguanidine (TMG) and organic phase anion exchange (OPAE) SPE to efficiently remove glyceride in olive oil simulant. In contrast to the normal ion exchange carried out in an aqueous solution or aqueous phase environment, the OPAE SPE was performed in the organic phase environments, and the time-consuming and challenging extraction of the nine UV absorbers from vegetable oil with aqueous solution could be readily omitted. The method was proved to have good linearity (r≥0.99992), precision (intra-day RSD≤3.3%), and accuracy(91.0%≤recoveries≤107%); furthermore, the lower limit of quantifications (0.05-0.2mg/kg) in five types of food simulants(10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol and olive oil) was observed. The method was found to be well suited for quantitative determination of the total specific migration of the nine UV absorbers both in aqueous and vegetable oil simulant according to Commission Regulation (EU) No. 10/2011. Migration levels of the nine UV absorbers were determined in 31 plastic samples, and UV-24, UV-531, HHBP and UV-326 were frequently detected, especially in olive oil simulant for UV-326 in PE samples. In addition, the OPAE SPE procedure was also been applied to efficiently enrich or purify seven antioxidants in olive oil simulant. Results indicate that this procedure will have more extensive applications in the enriching or purification of the extremely weak acidic compounds with phenol hydroxyl group that are relatively stable in TMG n-hexane solution and that can be barely extracted from vegetable oil. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Heat exchanger

    International Nuclear Information System (INIS)

    Leigh, D.G.

    1976-01-01

    The arrangement described relates particularly to heat exchangers for use in fast reactor power plants, in which heat is extracted from the reactor core by primary liquid metal coolant and is then transferred to secondary liquid metal coolant by means of intermediate heat exchangers. One of the main requirements of such a system, if used in a pool type fast reactor, is that the pressure drop on the primary coolant side must be kept to a minimum consistent with the maintenance of a limited dynamic head in the pool vessel. The intermediate heat exchanger must also be compact enough to be accommodated in the reactor vessel, and the heat exchanger tubes must be available for inspection and the detection and plugging of leaks. If, however, the heat exchanger is located outside the reactor vessel, as in the case of a loop system reactor, a higher pressure drop on the primary coolant side is acceptable, and space restriction is less severe. An object of the arrangement described is to provide a method of heat exchange and a heat exchanger to meet these problems. A further object is to provide a method that ensures that excessive temperature variations are not imposed on welded tube joints by sudden changes in the primary coolant flow path. Full constructional details are given. (U.K.)

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

    NARCIS (Netherlands)

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

    2006-01-01

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

  16. New technique for synthesizing AMP : precipitation inside an ion-exchange resin and its application to separation of cesium from fission-products and to A137sub(m) Ba generator

    International Nuclear Information System (INIS)

    Matsuda, H.T.; Abrao, A.

    1980-06-01

    A new technique for synthesizing ammonium molybdophosphate, an inorganic ion exchanger which retains selectively cesium-137 from a mixture of fission products, is dealt with. Normally the use of this exchanger in column operation requires the use of asbestos, silica-gel or organic polymers as binder, due to its microcrystalline form. The new process employs a strong anionic resin, saturated with molybdate anions. This method enables the precipitation of ammonium molybdophosphate directly into the resinous structure by adding dihydrogen ammonium phosphate in 7,5M HNO 3 . The reactants maintened at 60 0 C for a period of four hours has been found to be the optimum condition for a maximum yield of this compound (anionic resin-ammonium molybdophosphate=R-AMP). The tests performed for characterizing this compound are: molybdenum-phosphorus ratio determination, electronic absorption spectra, infra-red absorption spectra, reflection microscopy observations, electron probe micro-analysis and X-ray powder patterns. The mentioned analysis confirmed the presence of the ammonium molybdophosphate in the resinous structure, permitting, thereby, its use as a cation exchanger. R-AMP showed a capacity of 0,48mE/g of dry material. The cesium retention studies were made using columns charged with R-AMP compound. The behavior of some polivalent fission products was also studied. The R-AMP columns was finally applied to separate cesium from irradiated uranium solutions. A method for the isolation of sup(137m)Ba by successive elutions from R-AMP ( 137 Cs) exchanger (generator) is described. (Author) [pt

  17. 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.

  18. The reversed-flow gas chromatography technique as a tool for the study of the evaporation retardation of SO2 and (CH3)2S from water by soluble surfactants.

    Science.gov (United States)

    Sevastos, D; Kotsalos, E; Koliadima, A

    2017-02-01

    In the present work the evaporation retardation of SO 2 and (CH 3 ) 2 S (=DMS) from water by soluble surfactants was studied by the Reversed-Flow Gas Chromatography (R.F.G.C.) technique. Using suitable mathematical analysis, rate coefficients, k c , for the transfer of SO 2 and DMS from pure or artificial sea water to the atmospheric environment were determined in the presence or the absence of surfactants. The efficiency of the three surfactants used (CTAB, TRITON X-100 and SDS) to retard the evaporation rate of SO 2 and DMS from water was estimated by the decrease of the k c values in the presence of the three surfactants, compared to those in the absence of surfactants. The more efficient surfactant for the retardation evaporation of SO 2 from both the pure and the artificial sea water was found to be the cationic CTAB surfactant, as the maximum decreases of the k c values were found to be 4.61×10 -3 cms -1 (number of films, n=1) and 3.07×10 -3 cms -1 (n=3), respectively. On the other hand, more efficient surfactant for the retardation evaporation of DMS from pure water was found to be the non-ionic TRITON X-100, in which the decrease of the k c value was estimated to be 18.20×10 -3 cms -1 (n=3) and from artificial sea water the cationic CTAB surfactant in which the decrease of the k c value was found to be 8.24×10 -3 cms -1 (n=3). Finally, the precision of the R.F.G.C. method in studying the retardation effect of various surfactants in the transfer of SO 2 and DMS from the water body to the atmosphere is estimated (mean value 96.69%), and the experimental values of k c are compared with those given in the literature. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Radial Chromatography for the Separation of Nitroaniline Isomers

    Science.gov (United States)

    Miller, Robert B.; Case, William S.

    2011-01-01

    Separation techniques are usually presented in the undergraduate organic laboratory to teach students how to purify and isolate compounds. Often the concept of liquid chromatography is introduced by having students create "silica gel columns" to separate components of a reaction mixture. Although useful, column chromatography can be a laborious…

  20. Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

    Directory of Open Access Journals (Sweden)

    Ball James W

    2003-06-01

    Full Text Available A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad™ AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan. Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad™ AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns.

  1. Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

    Science.gov (United States)

    Druschel, G.K.; Schoonen, M.A.A.; Nordstorm, D.K.; Ball, J.W.; Xu, Y.; Cohn, C.A.

    2003-01-01

    A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad??? AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab) and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern) and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan). Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad??? AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns. ?? The Royal Society of Chemistry and the Division of Geochemistry of the American Chemical Society 2003.

  2. Exchange Network

    Science.gov (United States)

    The Environmental Information Exchange Network (EN) is an Internet-based system used by state, tribal and territorial partners to securely share environmental and health information with one another and EPA.

  3. Optimization of an anion-exchange high performance liquid chromatography-inductively coupled plasma-mass spectrometric method for the speciation analysis of oxyanion-forming metals and metalloids in leachates from cement-based materials.

    Science.gov (United States)

    Mulugeta, Mesay; Wibetoe, Grethe; Engelsen, Christian J; Lund, Walter

    2010-10-01

    A method was developed for the speciation analysis of the oxyanions of As(III), As(V), Cr(VI), Mo(VI), Sb(III), Sb(V), Se(IV), Se(VI) and V(V) in leachates from cement-based materials, based on anion-exchange HPLC coupled with ICP-MS. The method was optimized in a two-step multivariate approach: the effect of sample pH and mobile phase composition on resolution, peak symmetry and analysis time was studied. Optimum conditions were then identified for the significant experimental factors by studying their interdependence. A mobile phase composition of 20 mM ammonium nitrate, 50 mM ammonium tartrate and pH 9.5 was found to be a compromise optimum for the separation of the target analytes using isocratic elution. The optimum condition provided separation of the analytes in less than 6 min, at a mobile phase flow rate of 1.0 mL/min. The signal intensities of the analytes were improved by adding 1% methanol to the mobile phase. The limit of detection of the method was in the range 0.2-2.2 μg/L for the various species. The effect of sample constituents was studied using spiked concrete leachates. The method was used to determine the target oxyanionic species in leachates generated from a concrete material in the pH range 3.5-12.4; CrO(4)(2-), MoO(4)(2-) and VO(4)(3-) were detected in most of the leachates. Copyright © 2010 Elsevier B.V. All rights reserved.

  4. Open gas exchange system for simultaneous determination of the apparent CO2 assimilation by means of URAS technique and incorporation of 14C into plants

    International Nuclear Information System (INIS)

    Schumann, F.; Merbach, W.; Freye, E.; Schilling, G.

    1988-01-01

    Apparent CO 2 assimilation and 14 C incorporation into intact plants (Hordeum distichon L., Beta vulgaris L., and Vicia faba L.) were simultaneously measured on the same leaf, using a simple combination of the URAS technique (infrared absorption recorder) and 14 CO 2 fumigation in an open system. As a result of 14 C discrimination during the CO 2 incorporation and respiration losses during harvest and post-harvest treatment, the 14 C method gave always lower CO 2 assimilation values (by 17 to 25%) than the URAS technique. Nevertheless, the results obtained by both methods were closely correlated. Therefore, for quantifying the assimilated CO 2 properly and simultaneously tracing the assimilates synthesized from CO 2 , it is not sufficient to measure solely 14 C incorporation, but to combine both techniques. The system presented is qualified to meet these requirements. (author)

  5. Novel preconcentration technique for on-line coupling to high-speed narrow-bore capillary gas chromatography: sample enrichment by equilibrium (ab)sorption, I: Principles and theoretical aspects

    NARCIS (Netherlands)

    Pham Tuan, H.; Janssen, J.G.M.; Cramers, C.A.M.G.

    1997-01-01

    In recent years, there has been substantial progress in the field of high-speed narrow-bore capillary gas chromatography (GC) in general, and in the development of (trans)portable gas chromatographs for fast and accurate analysis in field applications in particular. Due to the limited

  6. Dehydroepiandrosterone sulfate quantification in serum using high-performance liquid chromatography/mass spectrometry and a deuterated internal standard: a technique suitable for routine use or as a reference method

    International Nuclear Information System (INIS)

    Shackleton, C.H.; Kletke, C.; Wudy, S.; Pratt, J.H.

    1990-01-01

    A thermospray high-performance liquid chromatography/mass spectrometry method for determination of serum dehydroepiandrosterone sulfate is described. The steroid was measured intact using [7,7-2H2]dehydroepiandrosterone sulfate as internal standard. The analysis was carried out in the negative ion mode by determining the peak height ratio of the molecular anions of the analyte and internal standard. The method was used to determine the steroid in serum from 15 male and female normal adults and the following values were obtained: males, 272 +/- 45 micrograms/dl (range, 197 to 331 micrograms/dl) and females, 215 +/- 67 micrograms/dl (range, 107 to 347 micrograms/dl). In addition, dehydroepiandrosterone sulfate was measured by high-performance liquid chromatography/mass spectrometry and radioimmunoassay (a commercial kit) on 25 individuals of all age groups. There was strong correlation between the values obtained, but the radioimmunoassay values were generally double those obtained by high-performance liquid chromatography/mass spectrometry. Three other steroid sulfates, androsterone sulfate, epiandrosterone sulfate, and androst-5-ene-3 beta, 17 beta-diol sulfate, were also assayed. In males, these had mean values of 112, 44, and 13 micrograms/dl and, in females, they had mean values of 84, 25, and 6 micrograms/dl, respectively. Radioimmunoassay cross-reactivity measurement for these steroids (as reference compounds) showed that they were unlikely to contribute greatly to the discrepancy between radioimmunoassay and high-performance liquid chromatography/mass spectrometry values

  7. Lipid exchange by ultracentrifugation

    DEFF Research Database (Denmark)

    Drachmann, Nikolaj Düring; Olesen, Claus

    2014-01-01

    , and the complex interplay between the lipids and the P-type ATPases are still not well understood. We here describe a robust method to exchange the majority of the lipids surrounding the ATPase after solubilisation and/or purification with a target lipid of interest. The method is based on an ultracentrifugation...... step, where the protein sample is spun through a dense buffer containing large excess of the target lipid, which results in an approximately 80-85 % lipid exchange. The method is a very gently technique that maintains protein folding during the process, hence allowing further characterization...

  8. Supercritical fluid chromatography

    Science.gov (United States)

    Vigdergauz, M. S.; Lobachev, A. L.; Lobacheva, I. V.; Platonov, I. A.

    1992-03-01

    The characteristic features of supercritical fluid chromatography (SCFC) are examined and there is a brief historical note concerning the development of the method. Information concerning the use of supercritical fluid chromatography in the analysis of objects of different nature is presented in the form of a table. The roles of the mobile and stationary phases in the separation process and the characteristic features of the apparatus and of the use of the method in physicochemical research are discussed. The bibliography includes 364 references.

  9. Stock price forecasting for companies listed on Tehran stock exchange using multivariate adaptive regression splines model and semi-parametric splines technique

    Science.gov (United States)

    Rounaghi, Mohammad Mahdi; Abbaszadeh, Mohammad Reza; Arashi, Mohammad

    2015-11-01

    One of the most important topics of interest to investors is stock price changes. Investors whose goals are long term are sensitive to stock price and its changes and react to them. In this regard, we used multivariate adaptive regression splines (MARS) model and semi-parametric splines technique for predicting stock price in this study. The MARS model as a nonparametric method is an adaptive method for regression and it fits for problems with high dimensions and several variables. semi-parametric splines technique was used in this study. Smoothing splines is a nonparametric regression method. In this study, we used 40 variables (30 accounting variables and 10 economic variables) for predicting stock price using the MARS model and using semi-parametric splines technique. After investigating the models, we select 4 accounting variables (book value per share, predicted earnings per share, P/E ratio and risk) as influencing variables on predicting stock price using the MARS model. After fitting the semi-parametric splines technique, only 4 accounting variables (dividends, net EPS, EPS Forecast and P/E Ratio) were selected as variables effective in forecasting stock prices.

  10. Surface modification of chromatography adsorbents by low temperature low pressure plasma

    DEFF Research Database (Denmark)

    Arpanaei, Ayyoob; Winther-Jensen, Bjørn; Theodosiou, E.

    2010-01-01

    In this study we show how low temperature glow discharge plasma can be used to prepare bi-layered chromatography adsorbents with non-adsorptive exteriors. The commercial strong anion exchange expanded bed chromatography matrix, Q HyperZ, was treated with plasmas in one of two general ways. Using ...

  11. Comparative Analysis of A, B Type and Exchange Traded Funds Performances with Mutual Fund Performance Measures, Regression Analysis and Manova Technique.

    Directory of Open Access Journals (Sweden)

    Mehmet Arslan

    2010-06-01

    Full Text Available The objective of the study is to evaluate risk- reward relationship and relative performances of the 4 different groups of mutual funds. To this end, daily return data of these 12 mutual funds (3 type variable fund; 3 B type variable fund; 3 A type stock fund and 3 A type Exchange traded fund together with daily market index (imkb100 return and daily return of riskless rate for the period from January 2006 to Feb 2010. The 180-day maturity T-Bill has been selected to represent riskless rate. To determine performances of mutual funds; Sharpe ratio, M2 measure, Treynor index, Jensen index, Sortino ratio, T2 ratio, Valuation ratio has been applied and these indicators produced conflicting results in ranking mutual funds. Then timingand selection capability of the fund manager has been determined by applying simple regression and Quadratic regression. Interestingly all funds found to have positive coefficient, indicating positive election capability of managers; but in terms of timing capability only one fund managers showed success. Finally, to determine extent to which mean returns are differs between mutual funds, market index (imkb100 and riskless rate (180 day TBill results of the analysis revealed that mean returns of individual security returns differs at P≤0,01 level. That shows instability in returns and poor ex-ante forecast modeling capability.

  12. Chromatographic techniques used in the laboratory scale fractionation and purification of plasma

    International Nuclear Information System (INIS)

    Siti Najila Mohd Janib; Wan Hamirul Bahrin Wan Kamal; Shaharuddin Mohd

    2004-01-01

    Chromatography is a powerful technique used in the separation as well as purification of proteins for use as biopharmaceuticals or medicines. Scientists use many different chromatographic techniques in biotechnology as they bring a molecule from its initial identification stage to the stage of it becoming a marketed product. The most commonly used of these techniques is liquid chromatography (1,C). This technique can be used to separate the target molecule from undesired contaminants, as well as to analyse the final product for the requisite purity as established by governmental regulatory groups such as the FDA. Some examples of LC techniques include: ion exchange (IEC), hydrophobic interaction (HIC), gel filtration (GF), affinity (AC) and reverse phase (RPC) chromatography. These techniques are very versatile and can be used at any stage of the purification process i.e. capture, intermediate purification phase and polishing. The choice of a particular technique is dependent upon the nature of the target protein as well as its intended final use. This paper describes the preliminary work done on the chromatographic purification of factor VIII (FVIII), factor IX (FIX), albumin and IgG from plasma. Results, in particular, in the isolation of albumin and IgG using IEC, have been promising. Preparation and production of cryoprecipitate to yield FVIII and FIX have also been successful. (Author)

  13. Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

    African Journals Online (AJOL)

    Prof. Ogunji

    The use of gas chromatography mass spectrometry (GC MS) as a sensitive and specific technique ... cold flow properties and stability of the fuel to oxidation, peroxidation and polymerization .... determinants of both the physical and chemical ...

  14. The thermodynamic principles of ligand binding in chromatography and biology

    DEFF Research Database (Denmark)

    Mollerup, Jørgen

    2007-01-01

    the general thermodynamic principles of ligand binding. Models of the multi-component adsorption in ion-exchange and hydrophobic chromatography, HIC and RPLC, are developed. The parameters in the models have a well-defined physical significance. The models are compared to the Langmuir model...

  15. Hydrogen exchange

    DEFF Research Database (Denmark)

    Jensen, Pernille Foged; Rand, Kasper Dyrberg

    2016-01-01

    Hydrogen exchange (HX) monitored by mass spectrometry (MS) is a powerful analytical method for investigation of protein conformation and dynamics. HX-MS monitors isotopic exchange of hydrogen in protein backbone amides and thus serves as a sensitive method for probing protein conformation...... and dynamics along the entire protein backbone. This chapter describes the exchange of backbone amide hydrogen which is highly quenchable as it is strongly dependent on the pH and temperature. The HX rates of backbone amide hydrogen are sensitive and very useful probes of protein conformation......, as they are distributed along the polypeptide backbone and form the fundamental hydrogen-bonding networks of basic secondary structure. The effect of pressure on HX in unstructured polypeptides (poly-dl-lysine and oxidatively unfolded ribonuclease A) and native folded proteins (lysozyme and ribonuclease A) was evaluated...

  16. The effects of real exchange rate misalignment and real exchange volatility on exports

    OpenAIRE

    Diallo, Ibrahima Amadou

    2011-01-01

    This paper uses panel data cointegration techniques to study the impacts of real exchange rate misalignment and real exchange rate volatility on total exports for a panel of 42 developing countries from 1975 to 2004. The results show that both real exchange rate misalignment and real exchange rate volatility affect negatively exports. The results also illustrate that real exchange rate volatility is more harmful to exports than misalignment. These outcomes are corroborated by estimations on s...

  17. Impulse Response of the Exchange Rate Volatility to a Foreign Exchange Intervention Shock

    OpenAIRE

    Hoshikawa, Takeshi

    2009-01-01

    This paper uses Lin's technique (1997) to report on the impulse response function analysis that traces the dynamics of exchange rate volatility from innovations in Japanese foreign exchange intervention. Using a multivariate GARCH model, we employed a volatility impulse response function based on Lin (1997) to detect the impulse response of exchange rate volatility on a one-unit foreign exchange intervention shock. The main findings of t his paper are as follows: (1) a foreign exchange inter...

  18. Phosphorus fertility recapitalization of nutrient-depleted tropical acid soils with reactive phosphate rock: An assessment using the isotopic exchange technique

    International Nuclear Information System (INIS)

    Fardeau, J.-C.; Zapata, F.

    2002-01-01

    A 'soil P fertility recapitalization' initiative utilizing large rates of phosphate rocks (PRs) was proposed to improve the soil P status and increase the sustainable food production in acid and P-deficient tropical soils. Two series of experiments were carried out using five tropical acid soils treated with heavy applications of Gafsa phosphate rock (GPR). In the first series, the soils were mixed with GPR at the following application rates: 0, 500, 1000 and 2000 mg P·kg -1 , and incubated for one month in moist conditions. In another series, 1000 mg P kg -1 applied as GPR was added to three soils and incubated for 1.5 month; thereafter 50 mg P kg -1 as triple superphosphate (TSP) were added. The 32 P isotopic exchange method was utilized to assess the contribution of GPR to the available soil P. Changes in amounts, E, of P transferred with time as phosphate ions from the soil particles to the soil solution as well as changes in pH, calcium and phosphate concentrations in soil suspensions were determined. It was found that: (i) the contribution of P from GPR to recapitalization of soil P fertility was mainly assessed by E pool size, pH, calcium and phosphate concentrations; other variables were not significant at the 0.1 level; (ii) heavy applications of GPR did not saturate all the P sorption sites, P freshly applied as water-soluble P was still sorbed; (iii) recapitalization of soil P fertility using GPR was partly obtained in some acid tropical soils; (iv) Upon dissolution, GPR provided calcium ions to crops and to soils, thus reducing Al toxicity, but its liming effect was limited. To explain these effects with heavy application rates of GPR, it was postulated that a coating of Al and Fe compounds is formed around PR particles with time, thus reducing further dissolution. (author)

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

    NARCIS (Netherlands)

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

    2012-01-01

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

  20. Heat exchanger

    International Nuclear Information System (INIS)

    Drury, C.R.

    1988-01-01

    A heat exchanger having primary and secondary conduits in heat-exchanging relationship is described comprising: at least one serpentine tube having parallel sections connected by reverse bends, the serpentine tube constituting one of the conduits; a group of open-ended tubes disposed adjacent to the parallel sections, the open-ended tubes constituting the other of the conduits, and forming a continuous mass of contacting tubes extending between and surrounding the serpentine tube sections; and means securing the mass of tubes together to form a predetermined cross-section of the entirety of the mass of open-ended tubes and tube sections

  1. Detection in superheated water chromatography

    International Nuclear Information System (INIS)

    Chienthavorn, O.

    1999-11-01

    Superheated water has been used successfully as an eluent in liquid chromatography and has been coupled to various modes of detection, ultraviolet (UV), fluorescence, and nuclear magnetic resonance spectroscopy (NMR) and mass spectrometry (MS). A number of compounds were examined on poly(styrene-divinylbenzene) (PS-DVB), polybutadiene (PBD), and octadecylsilyl bonded silica (ODS) column with isothermal and temperature programmes. The PS-DVB column was mostly used throughout the project as it was the most stable. Not only pure water could serve as superheated water mobile phase; inorganic buffered water and ion-pairing reagent with a concentration of 1-3 mM of the buffer and reagent were also exploited. It was shown that the pH could be controlled during the separation without salt precipitation and the separations followed a conventional reversed-phase HPLC method. Results from fluorescence detection showed good separation of a series of vitamins, such as pyridoxine, riboflavin, thiamine, and some analgesics. The relationship of riboflavin using the detection was linear and the detection limit was seven times higher than that of a conventional method. Simultaneous separation and identification using superheated water chromatography-NMR was demonstrated. With using a stop flow method, NMR spectra of model drugs, namely barbiturates, paracetamol, caffeine and phenacetin were obtained and the results agreed with reference spectra, confirming a perfect separation. A demonstration to obtain COSY spectrum of salicylamide was also performed. The method was expanded to the coupling of superheated water LC to NMR-MS. Results from the hyphenated detection method showed that deuteration and degradation happened in the superheated water conditions. The methyl group hydrogens of pyrimidine ring of sulfonamide and thiamine were exchanged with deuterium. Thiamine was decomposed to 4-methyl-5-thiazoleethanol and both were deuterated under the conditions. (author)

  2. Heat exchanger

    Science.gov (United States)

    Wolowodiuk, Walter

    1976-01-06

    A heat exchanger of the straight tube type in which different rates of thermal expansion between the straight tubes and the supply pipes furnishing fluid to those tubes do not result in tube failures. The supply pipes each contain a section which is of helical configuration.

  3. Heat exchangers

    International Nuclear Information System (INIS)

    1975-01-01

    The tubes of a heat exchanger tube bank have a portion thereof formed in the shape of a helix, of effective radius equal to the tube radius and the space between two adjacent tubes, to tangentially contact the straight sections of the tubes immediately adjacent thereto and thereby provide support, maintain the spacing and account for differential thermal expansion thereof

  4. Exchange rates.

    Science.gov (United States)

    Mills, Bev

    2003-09-01

    IN MAY this year, I was lucky enough to go to Larissa in northern Greece as part of Hope Exchange 2003, an annual study tour organised by the European Union's hospital committee and administered by the Institute of Healthcare Management (IHM).

  5. Heat exchanger

    Science.gov (United States)

    Daman, Ernest L.; McCallister, Robert A.

    1979-01-01

    A heat exchanger is provided having first and second fluid chambers for passing primary and secondary fluids. The chambers are spaced apart and have heat pipes extending from inside one chamber to inside the other chamber. A third chamber is provided for passing a purge fluid, and the heat pipe portion between the first and second chambers lies within the third chamber.

  6. Heat exchanger

    International Nuclear Information System (INIS)

    Wolowodiuk, W.

    1976-01-01

    A heat exchanger of the straight tube type is described in which different rates of thermal expansion between the straight tubes and the supply pipes furnishing fluid to those tubes do not result in tube failures. The supply pipes each contain a section which is of helical configuration

  7. UHPLC: The Greening Face of Liquid Chromatography.

    Science.gov (United States)

    Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

  8. Gas chromatography of β-diketonates

    International Nuclear Information System (INIS)

    Burgett, C.A.

    1976-01-01

    The history of separation of metal complexes by gas chromatography is reviewed. The greatest success has been achieved with metal halides or metal β-diketonates, particularly with chelates of the small elements, Be and Al, and the extremely inert chromium diketonates. Many problems still remain concerning the development of suitable chromatographic techniques for many chelates; however, the technique of synergic solvent extraction, mixed-ligand complex chromatography, the synthesis of new heteroatomic ligands, and the advent of new liquid phases are discussed as means to increase the number of unique techniques for separation and analysis of metals. Methods are suggested and references are cited for chromatographic analysis of elements in the following groups: alkali metals, alkaline earths, Group IIIA, IVB, VB, VIB, VIIB, VIII, IB, and IIB. Special attention is given to separation of the volatile complexes of Sc, Y, the lanthanides, the actinides, and Pb. 156 references

  9. High-Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  10. Laser induced pyrolysis techniques

    International Nuclear Information System (INIS)

    Vanderborgh, N.E.

    1976-01-01

    The application of laser pyrolysis techniques to the problems of chemical analysis is discussed. The processes occurring during laser pyrolysis are first briefly reviewed. The problems encountered in laser pyrolysis gas chromatography are discussed using the analysis of phenanthrene and binary hydrocarbons. The application of this technique to the characterization of naturally occurring carbonaceous material such as oil shales and coal is illustrated

  11. Extraction chromatography of actinides

    International Nuclear Information System (INIS)

    Muller, W.

    1978-01-01

    Extraction chromatography of actinides in the oxidation state from 2 to 6 is reviewed. Data on using neutral (tbp), basic (substituted ammonium salts) and acidic [di-(2-ethylhexyl)-phosphoric acid (D2EHPA)] extracting agents ketones, esters, alcohols and β-diketones in this method are given. Using the example of actinide separation using D2EHPA, discussed are factors influencing the efficiency of their chromatography separation (nature and particle size of the carrier materials, extracting agents amount on the carrier, temperature and elution rate)

  12. Micellar liquid chromatography

    International Nuclear Information System (INIS)

    Basova, Elena M; Ivanov, Vadim M; Shpigun, Oleg A

    1999-01-01

    Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

  13. H- charge exchange injection systems

    International Nuclear Information System (INIS)

    Ankenbrandt, C.; Curtis, C.; Hojvat, C.; Johnson, R.P.; Owen, C.; Schmidt, C.; Teng, L.; Webber, R.C.

    1980-01-01

    The techniques and components required for injection of protons into cyclic accelerators by means of H - charge exchange processes are reviewed, with emphasis on the experience at Fermilab. The advantages of the technique are described. The design and performance of the system of injection of H - ions into the Fermilab Booster are detailed. (Auth.)

  14. Ion exchange equilibrium constants

    CERN Document Server

    Marcus, Y

    2013-01-01

    Ion Exchange Equilibrium Constants focuses on the test-compilation of equilibrium constants for ion exchange reactions. The book first underscores the scope of the compilation, equilibrium constants, symbols used, and arrangement of the table. The manuscript then presents the table of equilibrium constants, including polystyrene sulfonate cation exchanger, polyacrylate cation exchanger, polymethacrylate cation exchanger, polysterene phosphate cation exchanger, and zirconium phosphate cation exchanger. The text highlights zirconium oxide anion exchanger, zeolite type 13Y cation exchanger, and

  15. Heat exchanger

    International Nuclear Information System (INIS)

    Bennett, J.C.

    1975-01-01

    A heat exchanger such as forms, for example, part of a power steam boiler is made up of a number of tubes that may be arranged in many different ways, and it is necessary that the tubes be properly supported. The means by which the tubes are secured must be as simple as possible so as to facilitate construction and must be able to continue to function effectively under the varying operating conditions to which the heat exchanger is subject. The arrangement described is designed to meet these requirements, in an improved way. The tubes are secured to a member extending past several tubes and abutment means are provided. At least some of the abutment means comprise two abutment pieces and a wedge secured to the supporting member, that acts on these pieces to maintain the engagement. (U.K.)

  16. Gas chromatography at the Tritium Laboratory Karlsruhe

    International Nuclear Information System (INIS)

    Laesser, R.; Gruenhagen, S.

    2003-08-01

    Among the analytical techniques (mass spectrometry, laser Raman spectroscopy, gas chromatography, use of ionisation chambers) employed at the Tritium Laboratory Karlsruhe (TLK), gas chromatography plays a prominent role. The main reasons for that are the simplicity of the gas chromatographic separation process, the small space required for the equipment, the low investment costs in comparison to other methods, the robustness of the equipment, the simple and straightforward analysis and the fact that all gas species of interest (with the exception of water) can easily be detected by gas chromatographic means. The conventional gas chromatographs GC1 and GC2 used in the Tritium Measurement Techniques (TMT) System of the TLK and the gas chromatograph GC3 of the experiment CAPER are presented in detail, by discussing their flow diagrams, their major components, the chromatograms measured by means of various detectors, shortcomings and possible improvements. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures. To overcome this disadvantage, micro gas chromatography for hydrogen analysis was developed. Reduction of the retention times by one order of magnitude was achieved. (orig.)

  17. Heat exchangers

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, E L; Eisenmann, G; Hahne, E [Stuttgart Univ. (TH) (F.R. Germany). Inst. fuer Thermodynamik und Waermetechnik

    1976-04-01

    A survey is presented on publications on design, heat transfer, form factors, free convection, evaporation processes, cooling towers, condensation, annular gap, cross-flowed cylinders, axial flow through a bundle of tubes, roughnesses, convective heat transfer, loss of pressure, radiative heat transfer, finned surfaces, spiral heat exchangers, curved pipes, regeneraters, heat pipes, heat carriers, scaling, heat recovery systems, materials selection, strength calculation, control, instabilities, automation of circuits, operational problems and optimization.

  18. A simple and rapid technique for recovery of 99mTc from low specific activity (n,γ)99Mo based on solid-liquid extraction and column chromatography methodologies

    International Nuclear Information System (INIS)

    Chattopadhyay, Sankha; Das, Sujata Saha; Barua, Luna

    2010-01-01

    A simple and inexpensive method has been developed for the separation of 99m Tc from 99 Mo produced from the neutron activation of 98 Mo by 98 Mo(n,γ) 99 Mo nuclear reaction. The recovery of 99m Tc was performed by solid-liquid extraction based on alumina column chromatography. The overall radiochemical yield for the complete separation of 99m Tc was 85-97% (n=5). The separated Na[ 99m Tc]TcO 4 was of high radionuclidic, radiochemical and chemical purities. The method can be adopted for routine processing and use of 99m Tc in radiopharmacy operations.

  19. Ion exchange purification of scandium

    Science.gov (United States)

    Herchenroeder, Laurie A.; Burkholder, Harvey R.

    1990-10-23

    An improvement in purification of scandium through ion exchange chromatography is disclosed in which the oxidation potential of the eluting solution is altered by the addition of potassium chlorate or ammonium chloride so that removal of contaminants is encouraged. The temperature, pH and concentration of the eluent HEDTA are controlled in order to maintain the scandium in the column while minimizing dilution of the scandium band. Recovery of scandium is improved by pumping dilute scandium over the column prior to stripping the scandium and precipitation. This eliminates the HEDTA ion and other monovalent cations contaminating the scandium band. This method maximizes recovery of scandium while maintaining purity.

  20. A new technique of ion beam tritium labelling

    International Nuclear Information System (INIS)

    Zhang Nianbao; Sheng Shugang; Yao Fuzeng

    1990-01-01

    In this paper a new technique is reported for tritium labelling of proteins, peptides and other nonvolatile organic compounds. A tritium ion beam is accelerated to bombard solid sample target for producing tritium exchange with hydrogen. The tritium labelling method has been applied to tritiated soybean trypsin inhibitor, ribonuclease A, elastin, pachyman and others totalled 11. After purifying by dialysis, ion exchange chromatography and gel filtration, the tritiated proteins and polysaccharide were obtained with specific activity over 37 GBq/mmol, without decomposition and with biological activity well preserved. By amino acid analysis of tritiated protein it was shown that the relative specific radioactivities for His., Tyr. and Phe. residues were higher while those for Val., Ile. and Ser. residues were lower