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Sample records for chromatographic cation exchange

  1. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column.

    Science.gov (United States)

    Arai, Kaori; Mori, Masanobu; Hironaga, Takahiro; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-04-01

    A combination of hydrophilic interaction chromatographic (HILIC) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography (IC). Firstly, the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions. The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10). When using tartaric acid as the eluent, the HILIC columns indicated strong retentions for anions, based on ion-pair interaction. Especially, HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I(-) > NO3(-) > Br(-) > Cl(-) > H2PO4(-). However, since HILIC-10 could not separate analyte cations, a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series. The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+, NH4+, K+, Mg2+, Ca2+, H2PO4(-), Cl(-), Br(-), NO3(-) and I(-)) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6. The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections. The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 micromol/L for the cations and 0.31 - 1.2 micromol/L for the anions. This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  2. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column

    Institute of Scientific and Technical Information of China (English)

    Kaori ARAI; Masanobu MORI; Takahiro HIRONAGA; Hideyuki ITABASHI; Kazuhiko TANAKA

    2012-01-01

    A combination of hydrophilic interaction chromatographic ( HILIC ) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography ( IC ).Firstly,the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions.The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetainezwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10).When using tartaric acid as the eluent,the HILIC columns indicated strong retentions for anions,based on ion-pair interaction.Especially,HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I- > NO3- > Br- > Cl- >H2PO4-.However,since HILIC-10 could not separate analyte cations,a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series.The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+,NH4+,K+,Mg2+,Ca2+,H2PO4-,Cl-,Br-,NO3- and I-) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6.The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections.The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 μmol/L for the cations and 0.31 - 1.2 μmol/L for the anions.This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  3. Preparation of Medium Cation Exchange Stationary Phase of Polymeric Matrix and Their Chromatographic Properties

    Institute of Scientific and Technical Information of China (English)

    CHEN,Gang; GONG,Bo-Lin; BAI,Quan; GENG,Xin-Du

    2007-01-01

    Based on the monodisperse poly(glycidyl methacrylate-co-ethylenedimethacrylate) beads (PGMA/EDMA) with macropore as a medium, a new hydrophilic medium cation exchange (MCX) stationary phase for HPLC was synthesized by a new chemically modified method. The stationary phase was evaluated with the property of ion exchange, separability, reproducibility, hydrophilicity, effect of salt concentration, salt types, column loading and pH on the separation and retention of proteins in detail. It was found that it follows ion exchange chromatographic (IEC)retention mechanism. The measured bioactivity recovery for lysozyme was (96±5)%. The dynamic protein loading capacity of the synthesized MCX packings was 21.8 mg/g. Five proteins were almost completely separated within 6.0 min at a flow rate of 4 mL/min using the synthesized MCX resin. The MCX resin was also used for the rapid separation and purification of lysozyme from egg white with only one step. The purity and specific bioactivity of the purified lysozyme was found more than 95% and 70345 U/mg, respectively.

  4. Preparation of weak cation exchange packings for chromatographic separation of proteins using "click chemistry''.

    Science.gov (United States)

    Zhao, Kailou; Bai, Quan; Song, Chao; Wang, Fei; Yang, Fan

    2012-04-01

    "Click chemistry" is defined as a class of robust and selective chemical reactions affording high yields and is tolerant to a variety of solvents (including water), functional groups, and air. In this study, click chemistry was used as an effective strategy for coupling three alkyne-carboxylic acids onto the azide-silica to obtain three novel stationary phases of weak cation exchange chromatography, which were characterized with FTIR and elemental analysis. Six kinds of standard proteins, such as myoglobin, RNase A, RNase B, cytochrome C, α-chymotrypsin A, and lysozyme, were separated completely with the three novel weak cation exchange chromatography stationary phases. Compared with commercial weak cation exchange chromatography columns, the three kinds of novel weak cation exchange chromatography packings prepared by click chemistry approach have better resolution and selectivity. The mass recovery of more than 97% was obtained for all the tested proteins, and the bioactivity recovery of lysozyme on the prepared column was determined to be 96%. In addition, lysozyme was purified successfully from egg white with the novel weak cation exchange chromatography column by one step. The purity was more than 97% and a high specific activity was achieved to be 81 435 U/mg. The results illustrate the potential of click chemistry for preparing stationary phase for ion-exchange chromatography.

  5. Preparation of Weak Cation Exchange Packings Based on Monodisperse Poly (chloromethylstyrene-co-divinylbenzene) Particles and Its Chromatographic Properties

    Institute of Scientific and Technical Information of China (English)

    卫引茂; 陈强; 耿信笃

    2001-01-01

    Monodisperse poly ( chloromethylstyrene-co-divinylbenzene )particles were firstly prepared by a two-step swelling method.Based on this media, one kind of weak cation ion exchange packings was prepared. It was demonstrated that the prepared packings have comparative advantages for biopolymer separation with high column efficiency, low interstitial volume and low column backpressure, and have good resolution to proteins. The effects of salt concentration and pH of mobile phase on protein retentions were investigated. The properties of the weak cation ion exchange packings were evaluated by the unified retention model for mixed-mode interaction mechanison in ion exchange and hydrophobic interaction chromatography.

  6. On-line coupling of an ion chromatograph to the ICP-MS: Separations with a cation exchange chromatography column

    Energy Technology Data Exchange (ETDEWEB)

    Roellin, Stefan [Studsvik Nuclear AB, Nykoeping (Sweden)

    1999-12-01

    An ion chromatography system was coupled on-line to the ICP-MS. All separations were made with a cation exchange chromatography column. Fundamental laws about elution parameters affecting individual retention times and elution forms are explained by applying a proper ion exchange mechanism for the isocratic elution (separations with constant eluent concentration) of mono-, di-, tri-, and tetravalent cations and the actinide species MO{sub 2}{sup +} and MO{sub 2}{sup 2+}. A separation method with two eluents has been investigated to separate mono- from divalent ions in order to separate isobaric overlaps of Rb/Sr and Cs/Ba. The ions normally formed by actinides in aqueous solutions in the oxidation states III to VI are M{sup 3+}, M{sup 4+}, MO{sub 2}{sup +} and MO{sub 2}{sup 2+} respectively. Elution parameters were investigated to separate all four actinide species from each other in order to separate isobaric overlaps of the actinides Np, Pu, U and Am. A major question of concern over the possible release of actinides to the environment is the speciation of actinides within their four possible oxidation states. To check the possibility of speciation analysis with ion chromatography, a separation method was investigated to separate U{sup 4+} and UO{sub 2}{sup 2+} without changing the redox species composition during the separation. First results of Pu speciation analysis showed that Pu could be eluted as three different species. Pu(VI) was always eluting at the same time as Np(V). This was surprising as Pu(VI) is expected to have the same chemical characteristics as U(VI) and thus was expected to elute at the same time as U(VI)

  7. Denatured Thermodynamics of Proteins in Weak Cation-exchange Chromatography

    Institute of Scientific and Technical Information of China (English)

    LI Rong; CHEN Guo-Liang

    2003-01-01

    The thermostability of some proteins in weak cation-exchange chromatography was investigated at 20-80 ℃. The results show that there is a fixed thermal denaturation transition temperature for each protein. The appearance of the thermal transition temperature indicates that the conformations of the proteins are destroyed seriously. The thermal behavior of the proteins in weak cation-exchange and hydrophobic interaction chromatographies were compared in a wide temperature range. It was found that the proteins have a higher thermostability in a weak cation-exchange chromatography system. The thermodynamic parameters(ΔH0, ΔS0) of those proteins were determined by means of Vant Hoff relationship(lnk-1/T). According to standard entropy change(ΔS0), the conformational change of the proteins was judged in the chromatographic process. The linear relationships between ΔH0 and ΔS0 can be used to evaluate "compensation temperature"(β) at the protein denaturation and identify the identity of the protein retention mechanism in weak cation-exchange chromatography.

  8. Advancements in Anion Exchange Membrane Cations

    Energy Technology Data Exchange (ETDEWEB)

    Sturgeon, Matthew R. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Long, Hai [National Renewable Energy Lab. (NREL), Golden, CO (United States); Park, Andrew M. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Pivovar, Bryan S. [National Renewable Energy Lab. (NREL), Golden, CO (United States)

    2015-10-15

    Anion-exchange membrane fuel cells (AME-FCs) are of increasingly popular interest as they enable the use of non-Pt fuel cell catalysts, the primary cost limitation of proton exchange membrane fuel cells. Benzyltrimethyl ammonium (BTMA) is the standard cation that has historically been utilized as the hydroxide conductor in AEMs. Herein we approach AEMs from two directions. First and foremost we study the stability of several different cations in a hydroxide solution at elevated temperatures. We specifically targeted BTMA and methoxy and nitro substituted BTMA. We've also studied the effects of adding an akyl spacer units between the ammonium cation and the phenyl group. In the second approach we use computational studies to predict stable ammonium cations, which are then synthesized and tested for stability. Our unique method to study cation stability in caustic conditions at elevated temperatures utilizes Teflon Parr reactors suitable for use under various temperatures and cation concentrations. NMR analysis was used to determine remaining cation concentrations at specific time points with GCMS analysis verifying product distribution. We then compare the experimental results with calculated modeling stabilities. Our studies show that the electron donating methoxy groups slightly increase stability (compared to that of BTMA), while the electron withdrawing nitro groups greatly decrease stability in base. These results give insight into possible linking strategies to be employed when tethering a BTMA like ammonium cation to a polymeric backbone; thus synthesizing an anion exchange membrane.

  9. 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 intensification

  10. Ion-exchange chromatographic analysis of peroxynitric acid.

    Science.gov (United States)

    Nakashima, Yoichi; Ikawa, Satoshi; Tani, Atsushi; Kitano, Katsuhisa

    2016-01-29

    Ion-exchange chromatographic analysis of peroxynitric acid (O2NOOH) was performed by combining an acidic eluate with an UV-vis detector and immersing the separation column in an ice-water bath. The decomposition behavior of peroxynitric acid in the solution was also studied using this system. The fraction for the peroxynitric acid peak was collected. Ion-exchange chromatographic analysis of this fraction, after standing at room temperature for 24h, showed that the decomposition products were mainly nitrate ions with a very small amount of nitrous acid. The peroxynitric acid peak area correlated perfectly with the total amount of decomposition products. The ion-exchange chromatographic isolation allowed us to evaluate the molar extinction coefficient of peroxynitric acid precisely in a wider wavelength range than previous reports. The value decreases monotonically from 1729±26M(-1)cm(-1) at 200nm to 12.0±0.5M(-1)cm(-1) at 290nm.

  11. Chromatographic separation of inorganic ions on thin layers of titanium phosphate ion-exchanger

    Institute of Scientific and Technical Information of China (English)

    Vanik GHOULIPOUR; Moharram SAFARI

    2014-01-01

    The chromatographic behavior of 30 inorganic cations has been studied on thin layers of titanium phosphate ion-exchanger using several aqueous,organic and mixed mobile phases. The separation of one ion from several other ions and also ternary and binary separations have been developed. Some important analytical separations are reported. The effect of pH of the mobile phase on retention factor(Rf)values of the cations in the presence of complex-forming anion along with the separation power of the ion-exchanger were studied. This ion-exchanger exhibits high sorption capacity and varying selectivity towards metal ions and makes it a suitable stationary phase in thin layer chromatography.

  12. Chromatographic separation of inorganic ions on thin layers of titanium phosphate ion-exchanger.

    Science.gov (United States)

    Ghoulipour, Vanik; Safari, Moharram

    2014-12-01

    The chromatographic behavior of 30 inorganic cations has been studied on thin layers of titanium phosphate ion-exchanger using several aqueous, organic and mixed mobile phases. The separation of one ion from several other ions and also ternary and binary separations have been developed. Some important analytical separations are reported. The effect of pH of the mobile phase on retention factor (Rf) values of the cations in the presence of complex-forming anion along with the separation power of the ion-exchanger were studied. This ion-exchanger exhibits high sorption capacity and varying selectivity towards metal ions and makes it a suitable stationaiy phase in thin layer chromatography.

  13. Recent progress and applications of ion-exclusion/ion-exchange chromatography for simultaneous determination of inorganic anions and cations.

    Science.gov (United States)

    Nakatani, Nobutake; Kozaki, Daisuke; Mori, Masanobu; Tanaka, Kazuhiko

    2012-01-01

    One of the ultimate goals of ion chromatography is to determine both anions and cations found in samples with a single chromatographic run. In the present article, recent progress in ion-exclusion/ion-exchange chromatography for the simultaneous determinations of inorganic anions and cations are reviewed. Firstly, the principle and the control for the simultaneous separation and detection of analyte ions using ion-exclusion/cation-exchange chromatography with a weakly acidic cation-exchange column are outlined. Then, advanced chromatographic techniques in terms of analytical time, selectively and sensitivity are summarized. As a related method, ion-exclusion/anion-exchange chromatography with an anion-exchange column could be used for the simultaneous determination of inorganic nitrogen species, such as ammonium, nitrite and nitrate ions. Their usefulness and applications to water-quality monitoring and related techniques are also described.

  14. Production of sulfonated cation-exchangers from petroleum asphaltites

    Energy Technology Data Exchange (ETDEWEB)

    Pokonova, Yu.V.; Pol' kin, G.B.; Proskuryakov, V.A.; Vinogradov, M.V.

    1982-02-10

    Continuing our studies of the preparation of products of practical value from asphaltite, a new by-product of oil refining, we obtained sulfonated cation-exchangers from a mixture of asphaltite and acid tar. It is shown that these cation-exchangers have good kinetic properties and are superior in thermal and thermohydrolytic stability to the commercial cation-exchange resin KU-2.

  15. Ion-exchange chromatographic protein refolding.

    Science.gov (United States)

    Freydell, Esteban J; van der Wielen, Luuk; Eppink, Michel; Ottens, Marcel

    2010-11-12

    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 intensification, represented by the possibility of performing protein refolding, product purification and product concentration, in one unit operation. Besides its high degree of process intensification, IExR offers an additional set of key advantages including: spatial isolation of the bound protein molecules and the controllable change in chemical composition using gradients. Despite of the acknowledgement of the former advantages, the lack of mechanistic understanding on how they influence the process performance of the ion-exchange refolding reactor, limits the ability to exploit them in order to optimize the performance of the unit. This paper presents a quantitative analysis that assesses the effect that the spatial isolation and the urea gradient, have on the IExR performance, judged on the basis of the refolding yield (Y(N)) and the fractional mass recovery (f(Prot,Rec)). Additionally, this work discusses the effect of the protein load, the protein loading state (i.e., native, denatured, denatured and reduced (D&R)) and the adsorbent type on f(Prot,Rec). The presented work shows: (1) that the protein load has a direct effect on f(Prot,Rec), and the magnitude of this effect depends on the loading state of the protein solution and the adsorbent type; (2) that irrespectively of the type of adsorbent used, the saturation capacity of a denatured protein is less than the native protein and that this difference can be linked to differences in accessible binding surface area; (3) that there is a clear correlation between fractional surface coverage (θ) and f(Prot,Rec), indicating that the former could serve as a good descriptor to assess spatial isolation, and (4) that the urea

  16. Cation exchange properties of zeolites in hyper alkaline aqueous media.

    Science.gov (United States)

    Van Tendeloo, Leen; de Blochouse, Benny; Dom, Dirk; Vancluysen, Jacqueline; Snellings, Ruben; Martens, Johan A; Kirschhock, Christine E A; Maes, André; Breynaert, Eric

    2015-02-03

    Construction of multibarrier concrete based waste disposal sites and management of alkaline mine drainage water requires cation exchangers combining excellent sorption properties with a high stability and predictable performance in hyper alkaline media. Though highly selective organic cation exchange resins have been developed for most pollutants, they can serve as a growth medium for bacterial proliferation, impairing their long-term stability and introducing unpredictable parameters into the evolution of the system. Zeolites represent a family of inorganic cation exchangers, which naturally occur in hyper alkaline conditions and cannot serve as an electron donor or carbon source for microbial proliferation. Despite their successful application as industrial cation exchangers under near neutral conditions, their performance in hyper alkaline, saline water remains highly undocumented. Using Cs(+) as a benchmark element, this study aims to assess the long-term cation exchange performance of zeolites in concrete derived aqueous solutions. Comparison of their exchange properties in alkaline media with data obtained in near neutral solutions demonstrated that the cation exchange selectivity remains unaffected by the increased hydroxyl concentration; the cation exchange capacity did however show an unexpected increase in hyper alkaline media.

  17. Cu Vacancies Boost Cation Exchange Reactions in Copper Selenide Nanocrystals.

    Science.gov (United States)

    Lesnyak, Vladimir; Brescia, Rosaria; Messina, Gabriele C; Manna, Liberato

    2015-07-29

    We have investigated cation exchange reactions in copper selenide nanocrystals using two different divalent ions as guest cations (Zn(2+) and Cd(2+)) and comparing the reactivity of close to stoichiometric (that is, Cu2Se) nanocrystals with that of nonstoichiometric (Cu(2-x)Se) nanocrystals, to gain insights into the mechanism of cation exchange at the nanoscale. We have found that the presence of a large density of copper vacancies significantly accelerated the exchange process at room temperature and corroborated vacancy diffusion as one of the main drivers in these reactions. Partially exchanged samples exhibited Janus-like heterostructures made of immiscible domains sharing epitaxial interfaces. No alloy or core-shell structures were observed. The role of phosphines, like tri-n-octylphosphine, in these reactions, is multifaceted: besides acting as selective solvating ligands for Cu(+) ions exiting the nanoparticles during exchange, they also enable anion diffusion, by extracting an appreciable amount of selenium to the solution phase, which may further promote the exchange process. In reactions run at a higher temperature (150 °C), copper vacancies were quickly eliminated from the nanocrystals and major differences in Cu stoichiometries, as well as in reactivities, between the initial Cu2Se and Cu(2-x)Se samples were rapidly smoothed out. These experiments indicate that cation exchange, under the specific conditions of this work, is more efficient at room temperature than at higher temperature.

  18. Cation-exchange high-performance liquid chromatography: Separation of highly basic proteins using volatile acidic solvents

    NARCIS (Netherlands)

    Eijnden-van Raaij, A.J.M. van den; Koornneef, I.; Oostwaard, Th.M.J.; Laat, S.W. de; Zoelen, E.J.J. van

    1987-01-01

    The chromatographic behavior of a number of globular proteins was studied on a Bio-Sil TSK CM-2-SW weak cation exchange HPLC column under acidic conditions. A linear gradient of O-I M NH₄Ac in I M HOAc, inducing a convex pH gradient from 2.4-4.8, resulted in an excellent separation of highly basic p

  19. Preparation of sulfonated cation exchangers from petroleum asphaltites

    Energy Technology Data Exchange (ETDEWEB)

    Pokonova, Yu.V.; Pol' kin, G.B.; Proskuryakov, V.A.

    1980-01-01

    It was established that the reaction of petroleum asphaltite sulfonation is determined in the first step by the chemical reaction rate, and in the last --- by diffusion factors. The kinetic constants were found for each reaction step. Sulfonated cation exchangers were obtained having the characteristics: specific volume of the swollen cation exchanger 3.30 mL/g, bulk density of the air-dry product 0.58 g/mL., moisture content 23.4%, swelling in water 41.6%, mechanical strength 80.0%, static exchange capacity with respect to 0.1N NaOH solution 2.76 mg equiv/g, dynamic exchange capacity with respect to 0.0035N CaC1/sub 2/ solution for a specific load of 10 L/L.h 465 mg equiv/L.

  20. New cation-exchange membranes for hyperfiltration processes

    NARCIS (Netherlands)

    Velden, van der P.M.; Smolders, C.A.

    1977-01-01

    A new route for the preparation of cation exchange membranes from polystyrene-polyisoprene-polystyrene (SIS) block copolymers has been studied, using N-chlorosulfonyl isocyanate. At temperatures of 0° to 20°C, N-chlorosulfonyl isocyanate reacts readily with the olefin group in polyisoprenes, resulti

  1. Transesterification of propylene glycol methyl ether in chromatographic reactors using anion exchange resin as a catalyst.

    Science.gov (United States)

    Oh, Jungmin; Sreedhar, Balamurali; Donaldson, Megan E; Frank, Timothy C; Schultz, Alfred K; Bommarius, Andreas S; Kawajiri, Yoshiaki

    2016-09-30

    Reactive chromatography using an anion exchange resin is proposed for a transesterification reaction of propylene glycol methyl ether (DOWANOL™ PM) with ethyl acetate to produce propylene glycol methyl ether acetate (DOWANOL™ PMA). This reaction is studied in batch and chromatographic reactors catalyzed by an anion exchange resin. Several anion exchange resins are tested and compared based on the performance of resin as an adsorbent and a catalyst. A chromatographic column is packed with a selected catalyst, AMBERLITE™ IRA904, and both reaction and chromatographic elution are studied at different temperatures and feed concentrations. The resulting chromatograms are fitted to a mathematical model to obtain adsorption equilibrium and reaction kinetic parameters by the inverse method. Compared to esterification investigated in a previous study, transesterification has advantages such as a higher conversion at lower temperature and easy removal of the byproduct which may lead to higher productivity. Deactivation of anion exchange resins is observed and potential solutions are suggested.

  2. Properties of sulfonated cation-exchangers made from petroleum asphaltites

    Energy Technology Data Exchange (ETDEWEB)

    Pokonova, Yu.V.; Pol' kin, G.B.; Proskuryakov, V.A.

    1982-01-10

    The use of ion-exchangers in radiochemical technology is accompanied by changes of their properties under the influence of ionizing radiation. The rate of development of these processes depends on the nature and structure of the matrix and on the nature and amount of ionic groups. We have proposed a method of synthesis of ion-exchangers resistant to ..gamma.. radiation from petroleum asphaltites. Continuing these investigations, we prepared cation-exchangers by sulfonation of a mixture of petroleum asphaltites and acid asphalt. An investigation of their radiation resistance is described in this paper.

  3. Chromatographic Separation of Glucose and Fructose

    Science.gov (United States)

    Kuptsevich, Yu E.; Larionov, Oleg G.; Stal'naya, I. D.; Nakhapetyan, L. A.; Pronin, A. Ya

    1987-03-01

    The structures, mutarotation, and the physicochemical properties of glucose and fructose as well as methods for their separation are examined. Their chromatographic separation on cation exchangers in the calcium-form is discussed in detail. A theory of the formation of complexes of carbohydrates with metal cations is described and the mechanism of the separation of glucose and fructose on cation exchangers in the calcium-form is discussed in detail. Factors influencing the chromatographic separation of glucose and fructose on sulphonic acid cation-exchange resins are also considered. The bibliography includes 138 references.

  4. Selective Facet Reactivity During Cation Exchange in Cadmium Sulfide Nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Sadtler, Bryce; Demchenko, Denis; Zheng, Haimei; Hughes, Steven; Merkle, Maxwell; Dahmen, Ulrich; Wang, Lin-Wang; Alivisatos, A. Paul

    2008-12-18

    The partial transformation of ionic nanocrystals through cation exchange has been used to synthesize nanocrystal heterostructures. We demonstrate that the selectivity for cation exchange to take place at different facets of the nanocrystal plays an important role in determining the resulting morphology of the binary heterostructure. In the case of copper I (Cu+) cation exchange in cadmium sulfide (CdS) nanorods, the reaction starts preferentially at the ends of the nanorods such that copper sulfide (Cu2S) grows inwards from either end. The resulting morphology is very different from the striped pattern obtained in our previous studies of silver I (Ag+) exchange in CdS nanorods where non-selective nucleation of silver sulfide (Ag2S) occurs. From interface formation energies calculated for several models of epitaxialconnections between CdS and Cu2S or Ag2S, we infer the relative stability of each interface during the nucleation and growth of Cu2S or Ag2S within the CdS nanorods. The epitaxial connections of Cu2S to the end facets of CdS nanorods minimize the formation energy, making these interfaces stable throughout the exchange reaction. However, as the two end facets of wurtzite CdS nanorods are crystallographically nonequivalent, asymmetric heterostructures can be produced.

  5. Protein adsorption in polyelectrolyte brush type cation-exchangers.

    Science.gov (United States)

    Khalaf, Rushd; Coquebert de Neuville, Bertrand; Morbidelli, Massimo

    2016-11-04

    Ion exchange chromatography materials functionalized with polyelectrolyte brushes (PEB) are becoming an integral part of many protein purification steps. Adsorption onto these materials is different than that onto traditional materials, due to the 3D partitioning of proteins into the polyelectrolyte brushes. Despite this mechanistic difference, many works have described the chromatographic behavior of proteins on polyelectrolyte brush type ion exchangers with much of the same methods as used for traditional materials. In this work, unconventional chromatographic behavior on polyelectrolyte brush type materials is observed for several proteins: the peaks shapes reveal first anti-Langmuirian and then Langmuirian types of interactions, with increasing injection volumes. An experimental and model based description of these materials is carried out in order to explain this behavior. The reason for this behavior is shown to be the 3D partitioning of proteins into the polyelectrolyte brushes: proteins that fully and readily utilize the 3D structure of the PEB phase during adsorption show this behavior, whereas those that do not show traditional ion exchange behavior.

  6. Sulfonated polyvinyl chloride fibers for cation-exchange microextraction.

    Science.gov (United States)

    Xu, Li; Lee, Hian Kee

    2009-09-18

    Polyvinyl chloride (PVC) fiber was derivatized by concentrated sulfuric acid to yield sulfonated PVC (PVC-SO3H). The PVC-SO3H fiber had dual properties as a sorbent, based on cation-exchange and hydrophobicity. In the present study, the novel fiber was used directly as an individual device for extraction purposes in the cation-exchange microextraction of anaesthetics, followed by high-performance liquid chromatography-UV analysis. The results demonstrated that this PVC-SO3H fiber-based microextraction afforded convenient operation and cost-effective application to basic analytes. The limits of detection for four anaesthetics ranged from 1.2 to 6.0 ng/mL. No carryover (because of its disposable usage), and no loss of sorbent phase (which normally occurs in stir-bar sorptive extraction) during extraction were observed.

  7. Alloyed copper chalcogenide nanoplatelets via partial cation exchange reactions.

    Science.gov (United States)

    Lesnyak, Vladimir; George, Chandramohan; Genovese, Alessandro; Prato, Mirko; Casu, Alberto; Ayyappan, S; Scarpellini, Alice; Manna, Liberato

    2014-08-26

    We report the synthesis of alloyed quaternary and quinary nanocrystals based on copper chalcogenides, namely, copper zinc selenide-sulfide (CZSeS), copper tin selenide-sulfide (CTSeS), and copper zinc tin selenide-sulfide (CZTSeS) nanoplatelets (NPLs) (∼20 nm wide) with tunable chemical composition. Our synthesis scheme consisted of two facile steps: i.e., the preparation of copper selenide-sulfide (Cu2-xSeyS1-y) platelet shaped nanocrystals via the colloidal route, followed by an in situ cation exchange reaction. During the latter step, the cation exchange proceeded through a partial replacement of copper ions by zinc or/and tin cations, yielding homogeneously alloyed nanocrystals with platelet shape. Overall, the chemical composition of the alloyed nanocrystals can easily be controlled by the amount of precursors that contain cations of interest (e.g., Zn, Sn) to be incorporated/alloyed. We have also optimized the reaction conditions that allow a complete preservation of the size, morphology, and crystal structure as that of the starting Cu2-xSeyS1-y NPLs. The alloyed NPLs were characterized by optical spectroscopy (UV-vis-NIR) and cyclic voltammetry (CV), which demonstrated tunability of their light absorption characteristics as well as their electrochemical band gaps.

  8. Review on cation exchange selectivity coefficients for MX-80 bentonite

    Energy Technology Data Exchange (ETDEWEB)

    Domenech, C.; Arcos, D.; Duro, L. [ENVIROS, Passeig de Rubi, 29-31, 08197 Valldoreix (Spain); Sellin, P. [SKB, Brahegatan 47, SE-102 40 Stockholm (Sweden)

    2005-07-01

    Full text of publication follows: Bentonite is considered as engineered barrier in the near field of a nuclear waste repository due to its low permeability, what impedes groundwater flow to the nuclear waste, and its high retention capacity (sorption) of radionuclides in the eventuality of groundwater intrusion. One of the main retention processes occurring at the bentonite surface is ion exchange. This process may exert a strong control on the mobility of major pore water cations. Changes in major cation concentration, especially calcium, can affect the dissolution-precipitation of calcite, which in turn controls one of the key parameters in the system: pH. The cation exchange process is usually described according to the Gaines-Thomas convention: Ca{sup 2+} + 2 NaX = CaX{sub 2} + 2 Na{sup +}, K{sub Ca} = (N{sub Ca} x a{sup 2}{sub Na{sup +}})/(N{sup 2}{sub Na} x a{sub Ca{sup 2+}}) where K{sub Ca} is the selectivity coefficient for the Ca by Na exchange, ai is the activity of cation 'i' in solution and NJ the equivalent fractional occupancy of cation 'J' in bentonite. Parameters such as solid to liquid (S:L) ratio and dry density of the solid have an important influence on the value of selectivity coefficients (K{sub ex}). Although in most geochemical modelling works, K{sub ex} values are directly taken from experiments conducted at low S:L ratios and low dry densities, the expected conditions in a deep geological nuclear waste repository are higher S:L and higher bentonite density (1.6 g.cm{sup -3} in the SKB design to obtain a fully water saturated density of around 2.0 g.cm{sup -3}). Experiments focused at obtaining selectivity coefficients under the conditions of interest face the difficulty of achieving a proper extraction and analyses of pore water without disturbing the system by the sampling method itself. In this work we have conducted a complete analyses of published data on MX-80 bentonite cationic exchange in order to assess the

  9. Spontaneous Superlattice Formation in Nanorods through PartialCation Exchange

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, Richard D.; Sadtler, Bryce; Demchenko, Denis O.; Erdonmez, Can K.; Wang, Lin-Wang; Alivisatos, A. Paul

    2007-03-14

    Lattice mismatch strains are widely known to controlnanoscale pattern formation in heteroepitaxy, but such effects have notbeen exploited in colloidal nanocrystal growth. We demonstrate acolloidal route to synthesizing CdS-Ag2S nanorod superlattices throughpartial cation exchange. Strain induces the spontaneous formation ofperiodic structures. Ab initio calculations of the interfacial energy andmodeling of strain energies show that these forces drive theself-organization. The nanorod superlattices exhibit high stabilityagainst ripening and phase mixing. These materials are tunablenear-infrared emitters with potential applications as nanometer-scaleoptoelectronic devices.

  10. Analysis of Adsorption, Ion Exchange, Thermodynamic Behaviour of Some Organic Cations on Dowex 50WX4-50/H+ Cation Exchanger in Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Ehteram A. Noor

    2011-01-01

    Full Text Available The equilibrium adsorption, ion exchange characteristics of various concentrations of some organic cations from aqueous solutions onto dowex 50WEX/H+ cation exchanger were studied at different temperatures in the range of 30-50 °C. The studied cations showed good adsorptive properties onto dowex 50WX4-5/H+ at different concentrations and temperatures. Main adsorption behaviour was ion exchange between hydrogen ions and the organic cations as indicated from the linear relation between the initial concentration of the organic cations and the released hydrogen ions. It was found that the adsorption affinity of dowex 50WX4-50/H+ towards the studied organic cations depends on the substituent type of the organic cations giving the following increasing order: 1-H < 2-OH < 3-OCH3. Thermodynamic parameters for the adsorption of the studied organic cations were evaluated and discussed. It was found that the adsorption 1-H organic cation was spontaneous, ordered, exothermic and favored with decreasing temperature. On the other hand the adsorption of both 2-OH and 3-OCH3 organic cations was found to be spontaneous and disordered with enthalpy change varies significantly with increasing organic cation concentration, suggesting dipole-dipole adsorption forces as new active sites for adsorption under conditions of relatively high concentrations. Freundlich and Dubinin-Radushkevich adsorption isotherm models reasonably describe the adsorption of the studied organic cations onto dowex 50WX4-50/H+ by segmented straight lines depending on the studied range of concentration, indicating the existence of two different sets of adsorption sites with substantial difference in energy of adsorption. According to Dubinin-Radushkevich adsorption isotherm model, physical-ion exchange mechanism was suggested for the adsorption of 1-H organic cation and both physical and chemical-ion exchange mechanisms were suggested for the adsorption of 2-OH and 3-OCH3 organic cations

  11. Computer simulation of methanol exchange dynamics around cations and anions

    Energy Technology Data Exchange (ETDEWEB)

    Roy, Santanu; Dang, Liem X.

    2016-03-03

    In this paper, we present the first computer simulation of methanol exchange dynamics between the first and second solvation shells around different cations and anions. After water, methanol is the most frequently used solvent for ions. Methanol has different structural and dynamical properties than water, so its ion solvation process is different. To this end, we performed molecular dynamics simulations using polarizable potential models to describe methanol-methanol and ion-methanol interactions. In particular, we computed methanol exchange rates by employing the transition state theory, the Impey-Madden-McDonald method, the reactive flux approach, and the Grote-Hynes theory. We observed that methanol exchange occurs at a nanosecond time scale for Na+ and at a picosecond time scale for other ions. We also observed a trend in which, for like charges, the exchange rate is slower for smaller ions because they are more strongly bound to methanol. This work was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences, and Biosciences. The calculations were carried out using computer resources provided by the Office of Basic Energy Sciences.

  12. Thin-layer chromatographic specification and separation of Cu(1+), Cu(2+), Ni(2+), and Co(2+) cations.

    Science.gov (United States)

    Savasci, Sahin; Akçay, Mehmet; Ergül, Soner

    2010-07-01

    The M(PyDTC)(2) (M: Cu, Co, or Ni) and CuPyDTC complexes, prepared by reactions of ammonium pyrrolidinedithiocarbamate with metal nitrates, are examined for qualitative analysis, speciation, and mutual separation using thin-layer chromatography systems. These complexes and their mixtures are spotted to the activated and non-activated thin layers of silica gel 60GF(254) (Si-60GF(254)) with a 250-microm thickness. Toluene-dichloromethane mixtures (4:1, 1:1, 1:4 v/v) are used as mobile phases for running of the complexes. All of these chromatographic systems are successfully used for speciation of Cu(2+) and Cu(1+) cations. The best analytical separation for the qualitative analysis of corresponding metal cations and mutual separation of components in M(PyDTC)(2) and CuPyDTC complexes are obtained when using pure toluene-dichloromethane (1:1 v/v) on the activated layer. This study shows that it is possible to qualitatively analyze and satisfactorily separate a mixture of Cu(1+), Cu(2+), Ni(2+), and Co(2+) cations on cited chromatographic systems. These results may be also said for the adaptability or validity on column chromatography.

  13. Comparison among three anion exchange chromatographic supports to capture erythropoietin from cell culture supernatant

    Institute of Scientific and Technical Information of China (English)

    Lourdes HERNNDEZ; Diobel STEWART; Lourdes ZUMALACRREGUI; Daniel AMARO

    2015-01-01

    Affinity and ion exchange conventional chromatography have been used to capture erythropoietin ( EPO)from mammalian cell culture supernatant. Currently,chromatographic adsorbent perfusion is available, however a limited number of applications have been found in the literature. In this work,three anion exchange chromatographic supports( gel,membrane and monolithic)were evaluated in the capture step of the recombi-nant erythropoietin purification process. The influences of load and flow rate on each support performance were analyzed. Also the purity of the EPO molecules was determined. A productivity analysis,as a decision tool for larger scale implementation,was done. As a conclusion,the evaluated supports are technically suitable to cap-ture EPO with adequate recovery and good purity. However,the monolithic column admits high operating velocity,showing the highest adsorption capacity and productivity.

  14. Synthesis and rheological properties of cation-exchanged Laponite suspensions

    Energy Technology Data Exchange (ETDEWEB)

    Phuoc, Tran X. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Univ. of Pittsburgh, PA (United States); Howard, Bret H. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Chyu, Minking K. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Univ. of Pittsburgh, PA (United States)

    2009-11-01

    In this paper we report our new approach to synthesize cation-exchanged Laponite suspensions. General observations of the prepared samples indicated that an aqueous suspension of 1 wt.% Laponite retained its free flowing liquid phase characteristics even after aging for several weeks. When bivalent cationic metals (Cu, Co, Ni) were ablated into the suspension, the strong charge of the crystal face was reduced and, on standing, the suspension gelled becoming highly viscous. This sol-gel transition was induced by the formation of a space-filled structure due to both van der Waals and electrostatic bonds between the positively charged rims and negatively charged faces. Rheological properties of such prepared suspensions were measured using a Brookfield DV-II Pro Viscometer with a small sample adapter (SSA18/13RPY). The yield strengths of 2.2 N/m2, 3.2 N/m2, and 1.7 N/m2 were measured for Ni-, Co-, and Cumodified Laponite suspensions, respectively. These yield strengths are sufficiently high for suspending weighting materials such as barite which requires the gel strength of about 0.5 N/m2.

  15. Synthesis and rheological properties of cation exchanged Laponite suspensions

    Energy Technology Data Exchange (ETDEWEB)

    Tran, X P; Howard, B; Chyu, M K

    2009-01-01

    In this paper we report our new approach to synthesize cation-exchanged Laponite suspensions. General observations of the prepared samples indicated that an aqueous suspension of 1 wt% Laponite retained its free flowing liquid phase characteristics even after aging for several weeks. When bivalent cationic metals (Cu, Co, Ni) were ablated into the suspension, the strong charge of the crystal face was reduced and, on standing, the suspension gelled becoming highly viscous. This sol-gel transition was induced by the formation of a space-filled structure due to both van derWaals and electrostatic bonds between the positively charged rims and negatively charged faces. Rheological properties of such prepared suspensions were measured using a Brookfield DV-H Pro Viscometer with a small sample adapter{SSA18/13RPY). The yield strengths of2.2 N/m2, 3.2 N/m2, and 1.7 N/m2 were measured for Ni-, Co-, and Cu-modified Laponite suspensions, respectively. These yield strengths are sufficiently high for suspending weighting materials such as barite which requires the gel strength of about 0.5 N/m2.

  16. DETERMINATION OF ION EXCHANGE EQUILIBRIUM CONSTANTS FOR THE WEAK ACID CATION AND THE WEAK BASE ANION EXCHANGE RESINS

    Institute of Scientific and Technical Information of China (English)

    TAOZuyi; WANGChangshou

    1992-01-01

    The general procedure based on the potentiometric titration has developed.According to the procedure,the rational equilibrium constants of the ion exchange reactions RH/Na,RH/Ca,RH/Sr,RH/Ba for the weak acid cation exchange resin D725 and ROH/Cl for the weak base anion exchange resin D705 have been determined.

  17. Cation immobilization in pyrolyzed simulated spent ion exchange resins

    Energy Technology Data Exchange (ETDEWEB)

    Luca, Vittorio, E-mail: vluca@cnea.gov.ar [Programa Nacional de Gestion de Residuos Radiactivos, Centro Atomico Constituyentes, Comision Nacional de Energia Atomica, Av. General, Paz 1499, 1650 San Martin, Provincia de Buenos Aires (Argentina); Bianchi, Hugo L. [Gerencia de Quimica, Centro Atomico Constituyentes, Comision Nacional de Energia Atomica, Av. General, Paz 1499, 1650 San Martin, Provincia de Buenos Aires (Argentina); ECyT, Universidad Nacional de General San Martin, Campus Miguelete, Ed. Tornavias, Martin de Irigoyen 3100, 1650 San Martin (Argentina); Conicet, Av. Rivadavia 1917, 1033 Buenos Aires (Argentina); Manzini, Alberto C. [Programa Nacional de Gestion de Residuos Radiactivos, Comision Nacional de Energia Atomica, Av. Del Libertador 8250, CP 1429, Ciudad Autonoma de Buenos Aires (Argentina)

    2012-05-15

    Significant quantities of spent ion exchange resins that are contaminated by an assortment of radioactive elements are produced by the nuclear industry each year. The baseline technology for the conditioning of these spent resins is encapsulation in ordinary Portland cement which has various shortcomings none the least of which is the relatively low loading of resin in the cement and the poor immobilization of highly mobile elements such as cesium. The present study was conducted with cationic resin samples (Lewatit S100) loaded with Cs{sup +}, Sr{sup 2+}, Co{sup 2+}, Ni{sup 2+} in roughly equimolar proportions at levels at or below 30% of the total cation exchange capacity. Low temperature thermal treatment of the resins was conducted in inert (Ar), or reducing (CH{sub 4}) gas atmospheres, or supercritical ethanol to convert the hydrated polymeric resin beads into carbonaceous materials that contained no water. This pyrolytic treatment resulted in at least a 50% volume reduction to give mechanically robust spherical materials. Scanning electron microscope investigations of cross-sections of the beads combined with energy dispersive analysis showed that initially all elements were uniformly distributed through the resin matrix but that at higher temperatures the distribution of Cs became inhomogeneous. Although Cs was found in the entire cross-section, a significant proportion of the Cs occurred within internal rings while a proportion migrated toward the outer surfaces to form a crustal deposit. Leaching experiments conducted in water at 25 Degree-Sign C showed that the divalent contaminant elements were very difficult to leach from the beads heated in inert atmospheres in the range 200-600 Degree-Sign C. Cumulative fractional loses of the order of 0.001 were observed for these divalent elements for temperatures below 500 Degree-Sign C. Regardless of the processing temperature, the cumulative fractional loss of Cs in water at 25 Degree-Sign C reached a plateau or

  18. Water quality monitoring system for determination of ionic nutrients by ion-exclusion chromatography with spectrophotometric detection on cation- and anion-exchange resin columns using water eluent.

    Science.gov (United States)

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

    2012-07-01

    A unified ion-exclusion chromatography (IEC) system for monitoring anionic and cationic nutrients like NH4+, NO2-, NO3-, phosphate ion, silicate ion and HCO3- was developed and applied to several environmental waters. The IEC system consisted of four IEC methodologies, including the IEC with ultraviolet (UV) form connected with detection at 210 nm for determining NH4+ on anion-exchange separation column in OH anion-exchange UV-conversion column in I- form in tandem, the IEC with UV-detection at 210 nm for determining simultaneously NO3- and NO3- on cation-exchange separation column in H+ form, the IEC with UV-detection at 210 nm for determining HCO3- on cation-exchange separation column in H+ form connected with anion-exchange UV-conversion column in I- form in tandem, and the IEC with visible-detection based on molybdenum-blue reaction for determining simultaneously silicate and phosphate ions on cation-exchange separation column in H+ form. These IEC systems were combined through three manually-driven 6-port column selection valves to select each separation column to determine selectively the ionic nutrients. Using this sequential water quality monitoring system, the analytical performances such as calibration linearity, reproducibility, detection limit and recovery were also tested under the optimized chromatographic conditions. This novel water quality monitoring system has been applied successfully for the determination of the ionic eutrophication components in sub-urban river waters.

  19. Indirect UV detection-ion-exclusion/cation-exchange chromatography of common inorganic ions with sulfosalicylic acid eluent.

    Science.gov (United States)

    Kozaki, Daisuke; Mori, Masanobu; Nakatani, Nobutake; Arai, Kaori; Masuno, Tomoe; Koseki, Masakazu; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2013-01-01

    Herein, we describe indirect UV detection-ion-exclusion/cation-exchange chromatography (IEC/CEC) on a weakly acidic cation-exchange resin in the H(+)-form (TSKgel Super IC-A/C) using sulfosalicylic acid as the eluent. The goal of the study was to characterize the peaks detected by UV detector. The peak directions of analyte ions in UV at 315 nm were negative because the molar absorbance coefficients of analyte anions and cations were lower than that of the sulfosalicylic acid eluent. Good chromatographic resolution and high signal-to-noise ratios of analyte ions were obtained for the separations performed using 1.1 mM sulfosalicylic acid and 1.5 mM 18-crown-6 as the eluent. The relative standard deviations (RSDs) of the peak areas ranged from 0.6 to 4.9%. Lower detection limits of the analytes were achieved using indirect UV detection at 315 nm (0.23 - 0.98 μM) than those obtained with conductometric detection (CD) (0.61 - 2.1 μM) under the optimized elution conditions. The calibration curves were linear in the range from 0.01 to 1.0 mM except for Cl(-), which was from 0.02 to 2.0 mM. The present method was successfully applied to determine common inorganic ions in a pond water sample.

  20. Purification of Monoclonal Antibodies Using a Fiber Based Cation-Exchange Stationary Phase: Parameter Determination and Modeling

    Directory of Open Access Journals (Sweden)

    Jan Schwellenbach

    2016-10-01

    Full Text Available Monoclonal antibodies (mAb currently dominate the market for protein therapeutics. Because chromatography unit operations are critical for the purification of therapeutic proteins, the process integration of novel chromatographic stationary phases, driven by the demand for more economic process schemes, is a field of ongoing research. Within this study it was demonstrated that the description and prediction of mAb purification on a novel fiber based cation-exchange stationary phase can be achieved using a physico-chemical model. All relevant mass-transport phenomena during a bind and elute chromatographic cycle, namely convection, axial dispersion, boundary layer mass-transfer, and the salt dependent binding behavior in the fiber bed were described. This work highlights the combination of model adaption, simulation, and experimental parameter determination through separate measurements, correlations, or geometric considerations, independent from the chromatographic cycle. The salt dependent binding behavior of a purified mAb was determined by the measurement of adsorption isotherms using batch adsorption experiments. Utilizing a combination of size exclusion and protein A chromatography as analytic techniques, this approach can be extended to a cell culture broth, describing the salt dependent binding behavior of multiple components. Model testing and validation was performed with experimental bind and elute cycles using purified mAb as well as a clarified cell culture broth. A comparison between model calculations and experimental data showed a good agreement. The influence of the model parameters is discussed in detail.

  1. Fabrication of patterned calcium cross-linked alginate hydrogel films and coatings through reductive cation exchange.

    Science.gov (United States)

    Bruchet, Marion; Melman, Artem

    2015-10-20

    Calcium cross-linked alginate hydrogels are widely used in targeted drug delivery, tissue engineering, wound treatment, and other biomedical applications. We developed a method for preparing homogeneous alginate hydrogels cross-linked with Ca(2+) cations using reductive cation exchange in homogeneous iron(III) cross-linked alginate hydrogels. Treatment of iron(III) cross-linked alginate hydrogels with calcium salts and sodium ascorbate results in reduction of iron(III) cations to iron(II) that are instantaneously replaced with Ca(2+) cations, producing homogeneous ionically cross-linking hydrogels. Alternatively, the cation exchange can be performed by photochemical reduction in the presence of calcium chloride using a sacrificial photoreductant. This approach allows fabrication of patterned calcium alginate hydrogels through photochemical patterning of iron(III) cross-linked alginate hydrogel followed by the photochemical reductive exchange of iron cations to calcium.

  2. Cation exchange displacement batch chromatography of proteins guided by screening of protein purification parameters.

    Science.gov (United States)

    Kotasińska, Marta; Richter, Verena; Thiemann, Joachim; Schlüter, Hartmut

    2012-11-01

    Displacement chromatography has been shown to be an effective alternative for protein purification. We investigated in this study sample displacement chromatography, which does not require a displacer molecule. Furthermore, we performed a screening for determination of parameters for an optimal sample displacement chromatography. We screened the affinities of cytochrome C, lysozyme, myoglobin, and ribonuclease A toward a cation exchange material as a function of different pH values and to presence of different concentrations of sodium chloride in the sample application buffer. Sample displacement chromatography in batch chromatography mode for the separation of the protein mixture was studied with a sample application buffer with a pH of 5 and 7. As predicted by the screening experiments, sample displacement chromatography was most effective at pH 7 since this pH guaranteed the largest differences of the affinities of the four proteins toward the stationary phase. In summary, we describe here sample displacement chromatography in the batch chromatography mode for the separation of proteins, which is a simple and fast alternative to conventional displacement chromatography. Systematic screening of chromatographic parameters prior to sample displacement chromatography promises a successful separation of a target protein.

  3. Ion-exclusion chromatography with the direct UV detection of non-absorbing inorganic cations using an anion-exchange conversion column in the iodide-form.

    Science.gov (United States)

    Mori, Masanobu; Itabashi, Hideyuki; Ikedo, Mikaru; Tanaka, Kazuhiko

    2006-08-15

    An ion-exclusion chromatographic method for the direct UV detection of non-absorbing inorganic cations such as sodium (Na(+)), ammonium (NH(4)(+)) and hydrazine (N(2)H(5)(+)) ions was developed by connecting an anion-exchange column in the I(-)-form after the separation column. For example, NH(4)(+) is converted to a UV-absorbing molecule, NH(4)I, by the anion-exchange column in the I(-)-form after the ion-exclusion separation on anion-exchange column in the OH(-)-form with water eluent. As a result, the direct UV detection of Na(+), NH(4)(+) and N(2)H(5)(+) could be successfully obtained as well as the well-resolved separation. The calibration graphs of the analyte cations detected with UV at 230nm were linear in the range of 0.001-5.0mM. The detection limits at S/N=3 of the cations were below 0.1muM. This method was applied to real water analysis, the determination of NH(4)(+) in river and rain waters, or that of N(2)H(5)(+) in boiler water, with the satisfactory results. This could be applied also to low- or non-absorbing anions such as fluoride or hydrogencarbonate ions by the combination of a weakly acidic cation-exchange resin in the H(+)-form as the separation column and the anion-exchange conversion column.

  4. Full automation of {sup 68}Ga labelling of DOTA-peptides including cation exchange prepurification

    Energy Technology Data Exchange (ETDEWEB)

    Ocak, M. [Clinical Department of Nuclear Medicine, Medical University Innsbruck, Anichstrasse 35, A-6020 Innsbruck (Austria); Department of Pharmaceutical Technology, Pharmacy Faculty, Istanbul University, Istanbul (Turkey); Antretter, M. [Clinical Department of Nuclear Medicine, Medical University Innsbruck, Anichstrasse 35, A-6020 Innsbruck (Austria); Knopp, R.; Kunkel, F. [Eckert and Ziegler Eurotope GmbH, Berlin (Germany); Petrik, M. [Clinical Department of Nuclear Medicine, Medical University Innsbruck, Anichstrasse 35, A-6020 Innsbruck (Austria); Bergisadi, N. [Department of Pharmaceutical Technology, Pharmacy Faculty, Istanbul University, Istanbul (Turkey); Decristoforo, C. [Clinical Department of Nuclear Medicine, Medical University Innsbruck, Anichstrasse 35, A-6020 Innsbruck (Austria)], E-mail: Clemens.Decristoforo@uki.at

    2010-02-15

    Here we describe a fully automated approach for the synthesis of {sup 68}Ga-labelled DOTA-peptides based on pre-concentration and purification of the generator eluate by using a cation exchange-cartridge and its comparison with fully automated direct labelling applying fractionated elution. Pre-concentration of the eluate on a cation exchange cartridge both using a resin-based and a disposable cation-exchange cartridge efficiently removed {sup 68}Ge as well as major metal contaminations with Fe and Zn. This resulted in a high labelling efficiency of DOTA-peptides at high specific activity (SA) with short synthesis times.

  5. Determining the cation exchange capacity of montmorillonite by simultaneous thermal analysis method

    Science.gov (United States)

    Boeva, N. M.; Bocharnikova, Yu. I.; Belousov, P. E.; Zhigarev, V. V.

    2016-08-01

    A way of determining the cation exchange capacity of montmorillonite by simultaneous thermal analysis is developed using as an example the bentonites of the 10th Khutor deposit (Republic of Khakassia) and the Vodopadnyi area (Sakhalin Island). A correlation is established between the cation exchange capacity of smectite and its weight loss upon heating in the range of dehydration; the enthalpy of dehydration of montmorillonite; and the weight loss and the enthalpy of thermal dissociation of ethylene glycol contained in the interlayer space of the mineral's crystal structure. These data open up new possibilities for determining the cation exchange capacity of montmorillonite, the most important technological indicator of the natural clay nanomineral.

  6. Sulphonic acid strong cation-exchange restricted access columns in sample cleanup for profiling of endogenous peptides in multidimensional liquid chromatography. Structure and function of strong cation-exchange restricted access materials.

    Science.gov (United States)

    Machtejevas, E; Denoyel, R; Meneses, J M; Kudirkaite, V; Grimes, B A; Lubda, D; Unger, K K

    2006-08-04

    In this work, the pore structural parameters and size exclusion properties of LiChrospher strong cation-exchange and reverse phase restricted access materials (RAM) are analysed. The molecular weight size exclusion limit for polystyrenes was found to be about 17.7 kDa, while for standard proteins, the molecular weight size exclusion limit was higher, at approximately 25 kDa. The average pore diameter on a volume basis calculated from the pore network model changes from 8.5 nm (native LiChrospher) to 8.6 nm (diol derivative) to 8.2 nm (sulphonic acid derivative) to 6.9 nm (n-octadecyl derivative). Additional characterisations were performed on restricted access materials with nitrogen sorption at 77 K, water adsorption at 25 degrees C, intrusion-extrusion of water (in order to evaluate the hydrophobic properties of the pores of the hydrophobic RAM), and zeta potential measurements by microelectrophoresis. For peptide analysis out of the biofluids, the strong cation-exchange functionality seems to be particularly suitable mainly because of the high loadability of the strong cation-exchange restricted access material (SCX-RAM) and the fact that one can work under non-denaturing conditions to perform effective chromatographic separations. For bacitracin, the dynamic capacity of the SCX-RAM columns does not reach its maximum value in the analysed range. For lysozyme, the dynamic capacity reaches a value of 0.08 mg/ml of column volume before column is overloaded. Additionally, the proper column operating conditions that lead to the total effective working time of the RAM column to be equal to approximately 500 injections (depending on the type of sample), is comprehensively described. The SCX-RAM column was used in the same system analysing urine samples for the period of 1 month (approximately 150 injections) with run-to-run reproducibility below 5% RSD and below 10% RSD for the relative fractions.

  7. High-Performance Liquid Chromatographic Resolution of Neutral and Cationic Hetero[6]Helicenes.

    Science.gov (United States)

    Labrador, Geraldine M; Bosson, Johann; Breitbach, Zachary S; Lim, Yeeun; Francotte, Eric R; Sabia, Rocchina; Villani, Claudio; Armstrong, Daniel W; Lacour, Jérôme

    2016-04-01

    Cationic hetero[6]helicenes 1+, 2+ and 3+ have been recently disclosed. Herein we report on their enantiomeric separation using high-performance liquid chromatography. Separation of the antipodes can be achieved in preparative scale on neutral adducts with Chiralcel OD-I or Chiralpak ID CSP. Selectivity factors of 1.90, 1.67, and 1.96 were obtained for 1-H, 2-H, and 3-H, respectively. Separation can also be performed on the carbenium ions on regular Chiralpak IA CSP using water-containing eluents, thus allowing for enantiomeric purity determinations in aqueous environments. Resolution of neutral and cationic helicenes is also achieved on more recently developed LARIHC columns. The versatility of the cyclofructan phases allows for baseline separations for both cases and their loading capabilities are demonstrated. Finally, the configurational stability of 1+, 2+, and 3+ was measured. For each replacement of an oxygen atom by an amino group, the racemization barrier increases significantly (ΔG‡ = 29.8, 36.3 and >37 kcal mol(-1) for 1+, 2+, and 3+ respectively).

  8. Ammonia vapor sensing properties of polyaniline-titanium(IV)phosphate cation exchange nanocomposite.

    Science.gov (United States)

    Khan, Asif Ali; Baig, Umair; Khalid, Mohd

    2011-02-28

    In this study, the electrically conducting polyaniline-titanium(IV)phosphate (PANI-TiP) cation exchange nanocomposite was synthesized by sol-gel method. The cation exchange nanocomposite based sensor for detection of ammonia vapors was developed at room temperature. It was revealed that the sensor showed good reversible response towards ammonia vapors ranging from 3 to 6%. It was found that the sensor with p-toluene sulphonic acid (p-TSA) doped exhibited higher sensing response than hydrochloric acid doped. This sensor has detection limit ≤1% ammonia. The response of resistivity changes of the cation exchange nanocomposite on exposure to different concentrations of ammonia vapors shows its utility as a sensing material. These studies suggest that the cation exchange nanocomposite could be a good material for ammonia sensor at room temperature.

  9. High-speed ion-exclusion chromatography of dissolved carbon dioxide on a small weakly acidic cation-exchange resin column with ion-exchange enhancement columns of conductivity detection.

    Science.gov (United States)

    Mori, Masanobu; Ikedo, Mikaru; Hu, Wenzhi; Helaleh, Murad I H; Xu, Qun; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2005-10-28

    The high-speed ion-exclusion chromatographic determination of dissolved carbon dioxide, i.e., carbonic acid, hydrogencarbonate or carbonate, with conductivity detection was obtained using a small column packed with a weakly acidic cation-exchange resin in the H+-form (40 mm long x 4.6 mm i.d., 3 microm-particle and 0.1 meq./ml-capacity). Two different ion-exchange resin columns, which were a strongly acidic cation-exchange resin in the K+-form and a strongly basic anion-exchange resin in the OH- -form, were connected after the separation column. The sequence of columns could convert dissolved carbon dioxide to KOH having high conductivity response. The enhancement effect for dissolved carbon dioxide could retain even on the vast chromatographic runs, by using the enhancement columns with high ion-exchange capacity above 1.0 meq./ml. The retention time was in 60 s at flow-rate of 1.2 ml/min. The calibration graph of dissolved carbon dioxide estimated as H2CO3- was linear in the range of 0.005-10 mM. The detection limit at signal to noise of 3 was 0.15 microM as H2CO3-. This method was applicable to several rainwater and tap water samples.

  10. Cation exchange at the secondary building units of metal–organic frameworks

    OpenAIRE

    Brozek, Carl Kavanaugh; Dinca, Mircea

    2014-01-01

    Cation exchange is an emerging synthetic route for modifying the secondary building units (SBUs) of metal–organic frameworks (MOFs). This technique has been used extensively to enhance the properties of nanocrystals and molecules, but the extent of its applications for MOFs is still expanding. To harness cation exchange as a rational tool, we need to elucidate its governing factors. Not nearly enough experimental observations exist for drawing these conclusions, so we provide a conceptual fra...

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

    Energy Technology Data Exchange (ETDEWEB)

    Chiarizia, R.; Horwitz, E.P.

    2000-01-01

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

  12. Chromatographic separation of vanadium, tungsten and molybdenum with a liquid anion-exchanger.

    Science.gov (United States)

    Fritz, J S; Topping, J J

    1971-09-01

    In acidic solution only molybdenum(VI), tungsten(VI), vanadium(V), niobium(V) and tantalum(V) form stable, anionic complexes with dilute hydrogen peroxide. This fact has been used in developing an analytical method of separating molybdenum(VI), tungsten(VI) and vanadium(V) from other metal ions and from each other. Preliminary investigations using reversed-phase paper chromatography and solvent extraction led to a reversed-phase column Chromatographic separation technique. These metal-peroxy anions are retained by a column containing a liquid anion-exchanger (General Mills Aliquat 336) in a solid support. Then molybdenum(VI), tungsten(VI) and vanadium(V) are selectively eluted with aqueous solutions containing dilute hydrogen peroxide and varying concentrations of sulphuric acid.

  13. Separation of Clay Minerals from Host Sediments Using Cation Exchange Resins

    Institute of Scientific and Technical Information of China (English)

    I.S. Ismael; H.M. Baioumy

    2003-01-01

    Classic physical and chemical treatments applied to separating clay minerals from the host sediments are often difficult or aggressive for clay minerals. A technique using cation exchange resins (amberlite IRC-50H and amberlite IR-120) is used to separate clay minerals from the host sediments. The technique is based on the exchange of cations in the minerals that may be associated clay minerals in sediments,such as Ca and Mg from dolomite; Ca from calcite,gypsum and francolite with cations carried by resin radicals. The associated minerals such as gypsum,calcite,dolomite and francolite are removed in descending order. Separation of clay minerals using cation exchange resins is less aggressive than that by other classic treatments.The efficiency of amberlite IRC-50H in the removal of associated minerals is greater than that of amberlite IR-120.

  14. Ion transport resistance in Microbial Electrolysis Cells with anion and cation exchange membranes

    NARCIS (Netherlands)

    Sleutels, T.H.J.A.; Hamelers, H.V.M.; Rozendal, R.A.; Buisman, C.J.N.

    2009-01-01

    Previous studies have shown that Microbial Electrolysis Cells (MECs) perform better when an anion exchange membrane (AEM) than when a cation exchange membrane (CEM) separates the electrode chambers. Here, we have further studied this phenomenon by comparing two analysis methods for bio-electrochemic

  15. Exchangeable cations-mediated photodegradation of polycyclic aromatic hydrocarbons (PAHs) on smectite surface under visible light

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Hanzhong, E-mail: jiahz@ms.xjb.ac.cn [Laboratory of Environmental Sciences and Technology, Xinjiang Technical Institute of Physics & Chemistry, Key Laboratory of Functional Materials and Devices for Special Environments, Chinese Academy of Sciences, Urumqi 830011 (China); Li, Li [Laboratory of Environmental Sciences and Technology, Xinjiang Technical Institute of Physics & Chemistry, Key Laboratory of Functional Materials and Devices for Special Environments, Chinese Academy of Sciences, Urumqi 830011 (China); Chen, Hongxia; Zhao, Yue [Laboratory of Environmental Sciences and Technology, Xinjiang Technical Institute of Physics & Chemistry, Key Laboratory of Functional Materials and Devices for Special Environments, Chinese Academy of Sciences, Urumqi 830011 (China); School of Geology and Mining Engineering, Xinjiang University, Urumqi 830046 (China); Li, Xiyou [Laboratory of Environmental Sciences and Technology, Xinjiang Technical Institute of Physics & Chemistry, Key Laboratory of Functional Materials and Devices for Special Environments, Chinese Academy of Sciences, Urumqi 830011 (China); Wang, Chuanyi, E-mail: cywang@ms.xjb.ac.cn [Laboratory of Environmental Sciences and Technology, Xinjiang Technical Institute of Physics & Chemistry, Key Laboratory of Functional Materials and Devices for Special Environments, Chinese Academy of Sciences, Urumqi 830011 (China)

    2015-04-28

    Graphical abstract: Roles of exchangeable cations in PAHs photodegradation on clay surafces under visible light. - Highlights: • Photolysis rate are strongly dependent on the type of cations on clay surface. • The strength of “cation–π” interactions governs the photodegradation rate of PAHs. • Several exchangeable cations could cause a shift in the absorption spectrum of PAHs. • Exchangeable cations influence the type and amount of reactive intermediates. - Abstract: Clay minerals saturated with different exchangeable cations are expected to play various roles in photodegradation of polycyclic aromatic hydrocarbons (PAHs) via direct and/or indirect pathways on clay surfaces. In the present study, anthracene and phenanthrene were selected as molecule probes to investigate the roles of exchangeable cations on their photodegradation under visible light irradiation. For five types of cation-modified smectite clays, the photodegradation rate of anthracene and phenanthrene follows the order: Fe{sup 3+} > Al{sup 3+} > Cu{sup 2+} >> Ca{sup 2+} > K{sup +} > Na{sup +}, which is consistent with the binding energy of cation–π interactions between PAHs and exchangeable cations. The result suggests that PAHs photolysis rate depends on cation–π interactions on clay surfaces. Meanwhile, the deposition of anthracene at the Na{sup +}-smectite and K{sup +}-smectite surface favors solar light absorption, resulting in enhanced direct photodecomposition of PAHs. On the other hand, smectite clays saturated with Fe{sup 3+}, Al{sup 3+}, and Cu{sup 2+} are highly photoreactive and can act as potential catalysts giving rise to oxidative radicals such as O{sub 2}{sup −}· , which initiate the transformation of PAHs. The present work provides valuable insights into understanding the transformation and fate of PAHs in the natural soil environment and sheds light on the development of technologies for contaminated land remediation.

  16. INTRAPARTICLE DIFFUSION OF RARE EARTHS IN POROUS CATION EXCHANGERS

    Institute of Scientific and Technical Information of China (English)

    LINGDaren; ZHENGZuying; 等

    1993-01-01

    Experiments for determining cerium isotope ion exchange rates with macroporous resins Amberlyst 15,D001 and XN1010 are discribed.The kinetics of the isotope ion exchange reaction has been examined by a simple theoretical equation of intraparticle effective diffustivity De in a porous ion exchanger.The ion exchange proceedes by diffusion within the macropores and the solid phase of the resin,De of cerium was affected by the concentration of the bulk solution C and was separated into a macropore diffusivity D-p and a solid phase diffusivity D-g by the equation.The diffusion coefficients of the exchanging ion are shown to have the values in the macropores comparable with those in the bulk solution and to have the values in the solid phase comparable with those in gel resin with the same crosslinkage as the resins used for the experiments.

  17. Effect of Lanthanum Accumulation on Cation Exchange Capacity and Solution Composition of Red Soil

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Pot and adsorption-exchange experiments were carried out by collecting the soil samples from the surface layer (0~15 cm) of red soil at the Ecological Experiment Station of Red Soil, the Chinese Academy of Sciences, in Jiangxi Province of China. When concentration of the exogenous La3+ exceeded 400 mg kg-1, there was less non-exchangeable La3+ than exchangeable La3+ in the soil. Cation exchange capacity of the soil changed slightly with increasing concentration of the exogenous La3+ in both experiments. However, in the adsorption-exchange experiment, when concentration of the exogenous La3+ was higher than 300 mg kg-1, exchangeable basic cations decreased significantly, while exchangeable hydrogen and exchangeable aluminum increased significantly compared with the control treatments. The amounts of base cations (Ca2+, Mg2+, K+ and Na+) exchanged by La3+ in the supernatant solution increased with the concentration of the exogenous La3+, especially when concentration of the exogenous La3+ was higher than 50 mg kg-1.

  18. Formation of cobalt hydrotalcite by cation exchange of Co2+-substitued zeolite X

    Science.gov (United States)

    Jeong, H. Y.; Lee, K.

    2013-12-01

    Zeolite has been utilized to sequester heavy metals and nuclides due to the high cation exchange capacity. However, once-immobilized cations by zeolite tend to be re-exchanged by other cations (Ca2+, Mg2+, Na+, etc) present in groundwater. Thus, it is important to understand the mechanism associated with re-exchange reactions to predict the environmental fate and behavior of the metal cations sequestered by zeolite. In this study, we performed a series of cation exchange experiments using Co2+-substituted zeolite X (Co-X) in concentrated CaCl2 solutions. The radioactive isotope of cobalt (60Co2+), commonly found in low-to-intermediate level nuclear wastes, undergoes radioactive decay, likely altering the physicochemical properties of zeolite by generating heat and irradiation. To simulate such effects, Co-X was thermally treated at 400 and 600oC before re-exchange experiments. At the higher treatment temperature, the re-exchanged amount of Co2+ in Co-X by Ca2+ was found to decrease. According to X-ray diffraction, the re-exchange led to little change in the zeolite crystallinity for thermally untreated samples, but the significantly decreased crystallinity was noted for re-exchanged, thermally treated samples. Nonetheless, 27Al MAS NMR spectra of all re-exchanged samples revealed that the peaks corresponding to 4-fold coordinated Al became broader with their position shifting as a result of the re-exchange, suggesting that the re-exchange caused a short-range order structural distortion for both thermally untreated and treated samples. Also, Co-K edge X-ray absorption spectroscopy (XAS) was employed to examine the mechanism(s) involved in the re-exchange. By comparison of XAS spectra between re-exchanged samples and model compounds, Co2+ was likely to be either present as an extraframwork cation within zeolite or incorporated into a cobalt hydrotalcite (Co6Al2(OH)16(An-)2/n where An- is an interlayer anion) phase. The relative contribution of an extraframwork Co2

  19. Sulfonated hydrocarbon graft architectures for cation exchange membranes

    DEFF Research Database (Denmark)

    Nielsen, Mads Møller; Jankova Atanasova, Katja; Hvilsted, Søren

    2013-01-01

    A synthetic strategy to hydrocarbon graft architectures prepared from a commercial polysulfone and aimed as ion exchange membrane material is proposed. Polystyrene is grafted from a polysulfone macroinitiator by atom transfer radical polymerization, and subsequently sulfonated with acetyl sulfate...

  20. Synthesis and adsorption properties of the cation exchange forms of OFF-type zeolite

    Science.gov (United States)

    Gorshunova, K. K.; Travkina, O. S.; Kustov, L. M.; Kutepov, B. I.

    2016-03-01

    The possibility of the ion-exchange of Na+ and K+ cations contained in OFF-type zeolite for H+, Ni2+, Cu2+, Co2+, and La3+ cations is investigated. Chemical and phase compositions, the morphology of crystals, and the adsorption properties of synthesized samples are studied via X-ray fluorescence and X-ray diffraction analysis, IR spectroscopy, scanning electron microscopy, and adsorption measurements.

  1. The effect of exchangeable cations in clinoptilolite and montmorillonite on the adsorption of aflatoxin B1

    Directory of Open Access Journals (Sweden)

    DRAGAN STOJSIC

    2001-08-01

    Full Text Available The adsorption of aflatoxin B1 (AFB1 by cation-exchanged clinoptilolite zeolitic tuff and montmorillonite was investigated at 37°C and pH 3.8 from an aqueous electrolyte having a composition similar to that of gastric juices of animals. Both minerals were exchanged from the natural form to the sodium form and then to the Cu2+, Zn2+ and Co2+-rich forms. The cation exchange was different for the different cations, but in all cases the exchanges were larger on montmorillonite than on clinoptilolite. The degree of exchange on montmorillonite was 76 % for copper (from a total of CEC 0.95 meq/g, Cu2+ –0.73 meq/g and 85 % for zinc and cobalt. Under the same conditions (concentration, temperature, pH, contact time, the degree of exchange on zeolitic tuff was 12 % for Cu2+ (from a total CEC of 1.46 meq/g, Cu2+ –0.17 meq/g, 8 % for Zn2+ and 10 % for Co2+. Both groups of mineral adsorbents showed high AFB1 chemisorption indexes (ca. For the montmorillonite forms, ca ranged from 0.75 for the Cu-exchanged montmorillonite to 0.89 for the natural Ca-form, 0.90 for the Zn-exchanged form and 0.93 for the Co-exchanged montmorillonite. The adsorption of AFB1 on the different exchanged forms of clinoptilolite gave similar values of ca for the Cu and Ca forms (0.90 and values of 0.94 and 0.95 for the Zn- and Co-exchanged form. The impact of the mineral adsorbents on the reduction of essential nutrients present in animal feed (Cu, Zn, Mn and Co showed that the Ca-rich montmorillonite had a higher capability for the reduction of the microelements than the Ca-rich clinoptilolite.

  2. Sulfonation Process and Desalination Effect of Polystyrene/PVDF Semi-Interpenetrating Polymer Network Cation Exchange Membrane

    Directory of Open Access Journals (Sweden)

    Yin-lin Lei

    2014-07-01

    Full Text Available With the classical sulfonation method of polystyrene-based strongly acidic cation exchange resins, polystyrene/polyvinylidene fluoride (PVDF alloy particles were sulfonated to obtain a cation exchange resin, which was then directly thermoformed to prepare a semi-interpenetrating polymer network (semi-IPN cation exchange membrane. The effects of the swelling agent, sulfonation time and temperature and the relative contents of polystyrene and divinylbenzene (DVB in the alloy particles on the feasibility of the membrane formation are discussed. The results indicate that a favorable sulfonation degree above 80% and a suitable ion exchange capacity of 1.5–2.4 mmol/g can be gained, with concentrated sulfuric acid as the sulfonation agent and 1,2-dichloroethane as the swelling agent. The running electrical resistance and desalination effect of the prepared cation exchange membrane were measured in a pilot-scale electrodialyser and not only obviously exceeded a commercial heterogeneous cation exchange membrane, but was also very close to a commercial homogenous membrane. In this way, the authors have combined the classical sulfonation method of polystyrene-based cation exchange resins with the traditional thermoforming manufacturing process of heterogeneous cation exchange membranes, to successfully develop a novel, low-price, but relatively high-performance polystyrene/PVDF cation exchange membrane with the semi-IPN structure.

  3. 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.

  4. Impact of sediment-seawater cation exchange on Himalayan chemical weathering fluxes

    Science.gov (United States)

    Lupker, Maarten; France-Lanord, Christian; Lartiges, Bruno

    2016-08-01

    Continental-scale chemical weathering budgets are commonly assessed based on the flux of dissolved elements carried by large rivers to the oceans. However, the interaction between sediments and seawater in estuaries can lead to additional cation exchange fluxes that have been very poorly constrained so far. We constrained the magnitude of cation exchange fluxes from the Ganga-Brahmaputra river system based on cation exchange capacity (CEC) measurements of riverine sediments. CEC values of sediments are variable throughout the river water column as a result of hydrological sorting of minerals with depth that control grain sizes and surface area. The average CEC of the integrated sediment load of the Ganga-Brahmaputra is estimated ca. 6.5 meq 100 g-1. The cationic charge of sediments in the river is dominated by bivalent ions Ca2+ (76 %) and Mg2+ (16 %) followed by monovalent K+ (6 %) and Na+ (2 %), and the relative proportion of these ions is constant among all samples and both rivers. Assuming a total exchange of exchangeable Ca2+ for marine Na+ yields a maximal additional Ca2+ flux of 28 × 109 mol yr-1 of calcium to the ocean, which represents an increase of ca. 6 % of the actual river dissolved Ca2+ flux. In the more likely event that only a fraction of the adsorbed riverine Ca2+ is exchanged, not only for marine Na+ but also Mg2+ and K+, estuarine cation exchange for the Ganga-Brahmaputra is responsible for an additional Ca2+ flux of 23 × 109 mol yr-1, while ca. 27 × 109 mol yr-1 of Na+, 8 × 109 mol yr-1 of Mg2+ and 4 × 109 mol yr-1 of K+ are re-absorbed in the estuaries. This represents an additional riverine Ca2+ flux to the ocean of 5 % compared to the measured dissolved flux. About 15 % of the dissolved Na+ flux, 8 % of the dissolved K+ flux and 4 % of the Mg2+ are reabsorbed by the sediments in the estuaries. The impact of estuarine sediment-seawater cation exchange appears to be limited when evaluated in the context of the long-term carbon cycle and

  5. A method for the production of weakly acidic cation exchange resins

    Science.gov (United States)

    Heller, H.; Werner, F.; Mitschker, A.; Diehl, H. V.; Schaefer, A.

    1991-12-01

    The invention relates to a nonpolluting method for the production of weakly acidic cation exchange resins by saponification of cross-linked acrylonitrile bead polymers, with an alkaline saponification agent at elevated temperature, according to which method the bead polymer and alkaline saponification agent are jointly added only at elevated temperature.

  6. Synthesis and cation-exchange properties of a bis-zwitterionic lamellar hybrid material

    Energy Technology Data Exchange (ETDEWEB)

    Besson, E. [ICSM Marcoule, UMR 5257, F-30207 Bagnols Sur Ceze, (France); Mehdi, A.; Reye, C.; Corriu, Robert J. P. [Univ Montpellier 2, Inst Charles Gerhardt Montpellier, CNRS-UM2-ENSCM-UM1, UMR 5253, Chim Mol et Org Sol, F-34095 Montpellier 5, (France); Chollet, H. [CEA Valduc, Dept Traitement Mat Nucl, F-21120 Is Sur Tille, (France); Guilard, R. [ICMUB, CNRS, UMR 5260, F-21078 Dijon, (France)

    2008-07-01

    The synthesis of a bis-zwitterionic lamellar hybrid material containing ammonium carboxylate groups is described. Cation-exchange properties of this material towards transition metal and lanthanide ions were studied as well as the regeneration and reuse of the material. (authors)

  7. Nongeminate Radiative Recombination of Free Charges in Cation-Exchanged PbS Quantum Dot Films

    Energy Technology Data Exchange (ETDEWEB)

    Marshall, Ashley R.; Beard, Matthew C.; Johnson, Justin C.

    2016-06-01

    Using photoluminescence (PL) spectroscopy we explore the radiative recombination pathways in PbS quantum dots (QDs) synthesized by two methods. We compare conventionally synthesized PbS from a PbO precursor to PbS synthesized using cation-exchange from CdS QDs. We show that strongly coupled films of PbS QDs from the cation-exchange luminesce with significant efficiency at room temperature. This is in stark contrast to conventional PbS QDs, which have exceedingly weak room temperature emission. Moreover, the power dependence of the emission is quadratic, indicating bimolecular radiative recombination that is reasonably competitive with trap-assisted recombination, a feature previously unreported in coupled PbS QD films. We interpret these results in terms of a greatly reduced defect concentration for cation-exchanged QDs that mitigates the influence of trap-assisted recombination. Cation-exchanged QDs have recently been employed in highly efficient and air-stable lead chalcogenide QD devices, and the reduced number of trap states inferred here may lead to improved current collection and higher open circuit voltage.

  8. Behavior of human serum albumin on strong cation exchange resins: I. experimental analysis.

    Science.gov (United States)

    Voitl, Agnes; Butté, Alessandro; Morbidelli, Massimo

    2010-08-20

    Experiments with human serum albumin on the strong cation exchange resin Fractogel EMD SE Hicap (M) were carried out. Even though human serum albumin was used at high purity, two peaks in gradient elution experiments occurred. The obtained data can be explained by considering that human serum albumin binds to Fractogel EMD SE Hicap (M) in two different binding conformations: the protein adsorbs instantaneously in the first conformation and then changes into the second one with a kinetic limitation. The two-peak behavior of human serum albumin was analyzed in detail, especially at various gradient lengths, concentrations and temperatures. Breakthrough curves were performed at four modifier concentrations and three velocities. The characteristic adsorption behavior, found for gradient experiments, was confirmed by the breakthrough curves. The two-peak elution pattern of human serum albumin was also found for other strong cation exchange resins, but not for weak cation exchange resins. It is concluded that the described behavior is peculiar for the interaction of human serum albumin with the strong cation exchange ligand of the resin.

  9. Selective separation of sodium ions from a mixture with phenylalanine by Donnan dialysis with a profiled sulfogroup cation exchange membrane

    Science.gov (United States)

    Vasil'eva, V. I.; Goleva, E. A.

    2013-11-01

    The possibility of separating ions of metal from a mixture with ampholyte (an amino acid) by Donnan dialysis with an MK-40 sulfogroup cation exchange membrane is demonstrated. Conditions ensuring the selectivity and intensity of the mass transfer of sodium ions from a mixture with bipolar phenylalanine ions into a diffusate containing hydrochloric acid through a cation exchange membrane are found.

  10. Calcium Solubility and Cation Exchange Properties in Zeoponic Soil

    Science.gov (United States)

    Beiersdorfer, Raymond E.

    1999-01-01

    An important aspect of a regenerative life support system at a Lunar or Martian outpost is the ability to produce food. Essential plant nutrients, as well as a solid support substrate, can be provided by: (1) treated Lunar or Martian regolith; (2) a synthetic soil or (3) some combination of both. A synthetic soil composed of ammonium- and potassium-saturated chinoptlolite (a zeolite mineral) and apatite, can provide slow-release fertilization of plants via dissolution and ion-exchange reactions. Previous equilibrium studies (Beiersdorfer, 1997) on mixtures of synthetic hydroxyapatite and saturated-clinoptilolite indicate that the concentrations of macro-nutrients such as ammonium, phosphorous, potassium, magnesium, and calcium are a function of the ratio of chinoptilolite to apatite in the sample and to the ratio of potassium to ammonium on the exchange sites in the clinoptilolite. Potassium, ammonium, phosphorous, and magnesium are available to plants at sufficient levels. However, calcium is deficient, due to the high degree of calcium adsorption by the clinoptilolite. Based on a series of batch-equilibration experiments, this calcium deficiency can be reduced by (1) treating the clinoptilolite with CaNO3 or (2) adding a second Ca-bearing mineral (calcite, dolomite or wollastonite) to the soil. Treating the Cp with CaNO3 results in increased Ca in solution, decreased P in solution and decreased NH4 in solution. Concentrations of K were not effected by the CaNO3 treatment. Additions of Cal, Dol and Wol changed the concentrations of Ca and P in solution in a systematic fashion. Cal has the greatest effect, Dol the least and Wol is intermediate. The changes are consistent with changes expected for a common ion effect with Ca. Higher concentrations of Ca in solution with added Cal, Dol or Wol do not result in changes in K or NH4 concentrations.

  11. Surface-orientation-dependent distribution of subsurface cation-exchange defects in olivine-phosphate nanocrystals.

    Science.gov (United States)

    Chung, Sung-Yoon; Choi, Si-Young; Kim, Tae-Hwan; Lee, Seongsu

    2015-01-27

    Atomic-scale exchange between two different cations of similar size in crystalline oxides is one of the major types of point defects when multiple cations in oxygen interstitials are arrayed in an ordered manner. Although a number of studies have been performed on a variety of Li-intercalation olivine phosphates to determine the distribution of exchange defects in bulk, understanding of the thermodynamic stability of the defects in subsurface regions and its dependency on the crystallographic orientation at the surface has remained elusive. Through a combination of small-angle neutron scattering, atomic-scale direct probing with scanning transmission electron microscopy, and theoretical ab initio calculations, we directly demonstrate that the antisite exchange defects are distributed in a highly anisotropic manner near the surfaces of LiFePO4 crystals. Moreover, a substantial amount of cation exchanges between Li and Fe sites is identified as an energetically favorable configuration in some surface regions, showing excellent agreement with the calculation results of negative defect formation energies. The findings in this study provide insight into developing better ways to avoid degradation of lithium mobility through the surface as well as scientifically notable features regarding the distribution of exchange defects in olivine phosphates.

  12. Strong cation exchange monoliths for HPLC by Reactive Gelation.

    Science.gov (United States)

    Brand, Bastian; Krättli, Martin; Storti, Giuseppe; Morbidelli, Massimo

    2011-08-01

    Polymeric monolithic stationary phases for HPLC can be produced by Reactive Gelation. Unlike the conventional method of using porogens, such novel process consists of a number of separate steps, thus enabling a better control of the quality of the final material. A suspension of polymer nanoparticles in water is produced and subsequently swollen with hydrophobic monomers. The particles are then destabilised (usually by salt addition) to make them aggregate into a large percolating structure, the so-called monolith. Finally, the added monomer can then be polymerised to harden the structure. In this work, a polystyrene latex is used as the base material and functionalised by introduction of epoxide groups on the surface and subsequent reaction to sulphonic acid groups, yielding a SO3(-) density of 0.7 mmol/g dry material. Morphological investigations show 54% porosity made of 300 nm large pores. Van Deemter measurements of a large protein show no practical influence of diffusion limitations on the plate number. Finally, a preliminary separation of a test protein mixture is shown, demonstrating the potential of using ion-exchange chromatography on Reactive Gelation monoliths.

  13. First principles derived, transferable force fields for CO2 adsorption in Na-exchanged cationic zeolites.

    Science.gov (United States)

    Fang, Hanjun; Kamakoti, Preeti; Ravikovitch, Peter I; Aronson, Matthew; Paur, Charanjit; Sholl, David S

    2013-08-21

    The development of accurate force fields is vital for predicting adsorption in porous materials. Previously, we introduced a first principles-based transferable force field for CO2 adsorption in siliceous zeolites (Fang et al., J. Phys. Chem. C, 2012, 116, 10692). In this study, we extend our approach to CO2 adsorption in cationic zeolites which possess more complex structures. Na-exchanged zeolites are chosen for demonstrating the approach. These methods account for several structural complexities including Al distribution, cation positions and cation mobility, all of which are important for predicting adsorption. The simulation results are validated with high-resolution experimental measurements of isotherms and microcalorimetric heats of adsorption on well-characterized materials. The choice of first-principles method has a significant influence on the ability of force fields to accurately describe CO2-zeolite interactions. The PBE-D2 derived force field, which performed well for CO2 adsorption in siliceous zeolites, does not do so for Na-exchanged zeolites; the PBE-D2 method overestimates CO2 adsorption energies on multi-cation sites that are common in cationic zeolites with low Si/Al ratios. In contrast, a force field derived from the DFT/CC method performed well. Agreement was obtained between simulation and experiment not only for LTA-4A on which the force field fitting is based, but for other two common adsorbents, NaX and NaY.

  14. Influence of the Ion Coordination Number on Cation Exchange Reactions with Copper Telluride Nanocrystals.

    Science.gov (United States)

    Tu, Renyong; Xie, Yi; Bertoni, Giovanni; Lak, Aidin; Gaspari, Roberto; Rapallo, Arnaldo; Cavalli, Andrea; Trizio, Luca De; Manna, Liberato

    2016-06-01

    Cu2-xTe nanocubes were used as starting seeds to access metal telluride nanocrystals by cation exchanges at room temperature. The coordination number of the entering cations was found to play an important role in dictating the reaction pathways. The exchanges with tetrahedrally coordinated cations (i.e., with coordination number 4), such as Cd(2+) or Hg(2+), yielded monocrystalline CdTe or HgTe nanocrystals with Cu2-xTe/CdTe or Cu2-xTe/HgTe Janus-like heterostructures as intermediates. The formation of Janus-like architectures was attributed to the high diffusion rate of the relatively small tetrahedrally coordinated cations, which could rapidly diffuse in the Cu2-xTe NCs and nucleate the CdTe (or HgTe) phase in a preferred region of the host structure. Also, with both Cd(2+) and Hg(2+) ions the exchange led to wurtzite CdTe and HgTe phases rather than the more stable zinc-blende ones, indicating that the anion framework of the starting Cu2-xTe particles could be more easily deformed to match the anion framework of the metastable wurtzite structures. As hexagonal HgTe had never been reported to date, this represents another case of metastable new phases that can only be accessed by cation exchange. On the other hand, the exchanges involving octahedrally coordinated ions (i.e., with coordination number 6), such as Pb(2+) or Sn(2+), yielded rock-salt polycrystalline PbTe or SnTe nanocrystals with Cu2-xTe@PbTe or Cu2-xTe@SnTe core@shell architectures at the early stages of the exchange process. In this case, the octahedrally coordinated ions are probably too large to diffuse easily through the Cu2-xTe structure: their limited diffusion rate restricts their initial reaction to the surface of the nanocrystals, where cation exchange is initiated unselectively, leading to core@shell architectures. Interestingly, these heterostructures were found to be metastable as they evolved to stable Janus-like architectures if annealed at 200 °C under vacuum.

  15. Influence of the Ion Coordination Number on Cation Exchange Reactions with Copper Telluride Nanocrystals

    CERN Document Server

    Tu, Renyong; Bertoni, Giovanni; Lak, Aidin; Gaspari, Roberto; Rapallo, Arnaldo; Cavalli, Andrea; De Trizio, Luca; Manna, Liberato

    2016-01-01

    Cu2-xTe nanocubes were used as starting seeds to access metal telluride nanocrystals by cation exchanges at room temperature. The coordination number of the entering cations was found to play an important role in dictating the reaction pathways. The exchanges with tetrahedrally coordinated cations (i.e. with coordination number 4), such as Cd2+ or Hg2+, yielded monocrystalline CdTe or HgTe nanocrystals with Cu2-xTe/CdTe or Cu2-xTe/HgTe Janus-like heterostructures as intermediates. The formation of Janus-like architectures was attributed to the high diffusion rate of the relatively small tetrahedrally coordinated cations, which could rapidly diffuse in the Cu2-xTe NCs and nucleate the CdTe (or HgTe) phase in a preferred region of the host structure. Also, with both Cd2+ and Hg2+ ions the exchange led to wurtzite CdTe and HgTe phases rather than the more stable zinc-blende ones, indicating that the anion framework of the starting Cu2- xTe particles could be more easily deformed to match the anion framework of t...

  16. Effect of quinidine on cation exchange in cultured cells.

    Science.gov (United States)

    McCall, D

    1976-06-01

    The effects of quinidine on membrane ion exchange were examined using monolayer cultures of mammalian cells. Quinidine, in concentrations from 10(-6) to 10(-3) M, produced a prompt inhibition of the passive Na influx, dose-dependent along a sigmoid log dose-response curve. This effect was at a maximum for each concentration of the drug within 30 seconds of application. Passive Na influx (pmol/cm2/sec) decreased from 18.8 to 17.6 (P less than .05) and 10.5 (P less than .001) in the presence of 10(-6) and 10(-3) M quinidine, respectively. In the continued presence of quinidine, there was no further time-dependent effect on the Na influx, nor was there any tendency for the influx to recover. Washing the cells free of quinidine, however, resulted in a return of Na influx to control levels within 1 to 3 minutes. After 1 to 2 minute of quinidine treatment, coupled active Na efflux/K influx rapidly declined, reaching minimum values for each concentration between 2 to 4 minutes of drug treatment. Beyond that time, active Na/K fluxes again increased, but to values which remained significantly less than control, for up to 4 hours. Ten minutes of exposure to quinidine were required before any demonstrable effect on the passive K efflux could be recorded. In the presence of quinidine, there was reduced membrane turnover of both Na and K, but such that after a brief initial period (10 minutes or less) both ions were in flux equilibrium, explaining the absence of change in [Nai] and [Ki] in the presence of quinidine. Calculations of Ec1 indicated that, when present for 4 hours, quinidine did not change the Em in these cells although significant (P less than .001) reductions in apparent PNa and Pk values were recorded. The effect on PNa was much greater than that on Pk. The quinidine-induced flux changes occurred in a definite temporal sequence suggesting that they could all be explained on the basis of one direct initial action. This initial direct action, namely the prompt

  17. Acarbose Isolation with Gel Type Strong Acid Cation Exchange Resin:Equilibrium, Kinetic and Thermodynamic Studies

    Institute of Scientific and Technical Information of China (English)

    王亚军; 于蕾; 郑裕国; 王远山; 沈寅初

    2013-01-01

    Acarbose, a potentα-glucosidase inhibitor, is widely used as an oral anti-diabetic drug for the treatment of the type 2, non-insulin-dependent diabetes. In this work, a gel type strong acid cation exchange resin 001×4 was applied to isolate acarbose from fermentation broth. It was demonstrated that cation exchanger 001×4 displayed a large adsorption capacity and quick exchange rate for acarbose. The static adsorption equilibrium data were well fitted to the Langmuir equation. Column adsorption experiments demonstrated that high dynamic adsorption capacity was reached at bed height of 104.4 mm, feed flow rate of 1.0 ml·min-1 and acarbose concentration of 4.0 mg·ml-1. Under the optimized conditions, the column chromatography packed with cation exchanger 001×4 recovered 74.3%(by mass) of acarbose from Actinoplanes utahensis ZJB-08196 fermentation broth with purity of 80.1%(by mass), demonstrating great potential in the practical applications in acarbose separation.

  18. Strong cation-exchange chromatography of proteins on a sulfoalkylated monolithic cryogel.

    Science.gov (United States)

    Perçin, Işık; Khalaf, Rushd; Brand, Bastian; Morbidelli, Massimo; Gezici, Orhan

    2015-03-20

    A new strong cation exchanger (SCX) monolithic column was synthesized by at-line surface modification of a cryogel prepared by copolymerization of 2-hydroxyethylmethacrylate (HEMA) and glycidylmethacrylate (GMA). Sodium salt of 3-Mercaptopropane sulfonic acid (3-MPS) was used as the ligand to transform the surface of the monolith into a strong cation exchanger. The obtained material was characterized in terms of elemental analysis, infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Brunauer-Emmett-Teller (BET) N2 adsorption, and used as a stationary phase for strong-cation exchange chromatography of some proteins, such as α-chymotrypsinogen, cytochrome c and lysozyme. Water permeability of the column was calculated according to Darcy's law (2.66×10(-13)m(2)). The performance of the monolithic cryogel column was evaluated on the basis of Height Equivalent to a Theoretical Plate (HETP). Retention behavior of the studied proteins was modeled on the basis of Yamamoto model to understand the role of the ion-exchange mechanism in retention behaviors. The considered proteins were successfully separated, and the obtained chromatogram was compared with that obtained with a non-functionalized cryogel column.

  19. 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.

  20. Radial variations in cation exchange capacity and base saturation rate in the wood of pedunculate oak and European beech

    Energy Technology Data Exchange (ETDEWEB)

    Herbauts, J.; Penninckx, V.; Gruber, W.; Meerts, P. [Universite Libre de Bruxelles, Laboratoire de genetique et d' ecologie vegetales, Brussels (Belgium)

    2002-10-01

    Visual observation of pedunculate oak trees and European beech trees in a mixed forest stand in the Belgian Ardennes revealed decreasing cation concentration profiles in wood. In order to determine whether these profiles are attributable to endogenous factors or to decreased availability of cations in the soil, radial profiles of water-soluble, exchangeable and total cations were investigated. Cation exchange capacity of wood was also determined. Results showed wood cation exchange capacity to decrease from pith to bark in European beech and from pith to outer heartwood in pedunculate oak. Decreasing profiles of exchangeable calcium and magnesium in peduncular oak and exchangeable calcium in European beech were found to be strongly constrained by cation exchange capacity, and thus not related to environmental change. Base cation saturation rate showed no consistent radial change in either species. It was concluded that the results did not provide convincing evidence to attribute the decrease in divalent cation concentration in pedunculate oak and European beech in this location to be due to atmospheric pollution. 42 refs., 1 tab., 4 figs.

  1. Chromatographic behaviour of alkaloids on thin layers of anion and cation exhangers. I. AG 1-X4 and cellex D.

    Science.gov (United States)

    Lepri, L; Desideri, P G; Lepori, M

    1976-01-07

    The chromatographic behaviour of 48 alkaloids has been studied on Bio-Rad AG 1-X4, Cellex D and microcrystalline cellulose, eluting with solutions of different pH but constant ionic strength (0.5). Many interesting separations were effected on both AG 1-X4 and Cellex D layers. The influence of pH on the chromatographic behaviour of alkaloids has been quantitatively studied and an equation was used that expresses the behaviour of the alkaloids on both AG 1-X4 (AcO-) and microcrystalling cellulose layers. The nonapplicability of this equation to Cellex D layers is discussed.

  2. Study by XPS of different conditioning processes to improve the cation exchange in clinoptilolite

    Science.gov (United States)

    Ruiz-Serrano, D.; Flores-Acosta, M.; Conde-Barajas, E.; Ramírez-Rosales, D.; Yáñez-Limón, J. M.; Ramírez-Bon, R.

    2010-09-01

    We report the X-ray photoelectron spectroscopy (XPS) analysis of natural clinoptilolite from a mine in Sonora, México. From these measurements we determined the chemical state and binding energy of the elements in the zeolite framework and of those in the extra framework sites. The analysis was done on natural clinoptilolite and on cation-exchanged clinoptilolites with Na + and NH4+ ions. Complementary analysis by several experimental techniques was performed to determine the structural, chemical composition and chemical state modifications experimented by clinoptilolite samples processed by the two types of cation exchange. The clinoptilolite samples were studied by X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) to determine their structural composition, Energy Dispersive Spectroscopy (EDS) to measure the chemical composition and electronic paramagnetic resonance (EPR) spectroscopy to determine the chemical state of iron inside the natural zeolites.

  3. Multicolour synthesis in lanthanide-doped nanocrystals through cation exchange in water

    KAUST Repository

    Han, Sanyang

    2016-10-04

    Meeting the high demand for lanthanide-doped luminescent nanocrystals across a broad range of fields hinges upon the development of a robust synthetic protocol that provides rapid, just-in-time nanocrystal preparation. However, to date, almost all lanthanide-doped luminescent nanomaterials have relied on direct synthesis requiring stringent controls over crystal nucleation and growth at elevated temperatures. Here we demonstrate the use of a cation exchange strategy for expeditiously accessing large classes of such nanocrystals. By combining the process of cation exchange with energy migration, the luminescence properties of the nanocrystals can be easily tuned while preserving the size, morphology and crystal phase of the initial nanocrystal template. This post-synthesis strategy enables us to achieve upconversion luminescence in Ce3+ and Mn2+-activated hexagonal-phased nanocrystals, opening a gateway towards applications ranging from chemical sensing to anti-counterfeiting.

  4. Effect of Simulated N Deposition on Soil Exchangeable Cations in Three Forest Types of Subtropical China

    Institute of Scientific and Technical Information of China (English)

    LU Xian-Kai; MO Jiang-Ming; P.GUNDERSERN; ZHU Wei-Xing; ZHOU Guo-Yi; LI De-Jun; ZHANG Xu

    2009-01-01

    The effects of simulated nitrogen (N) deposition on soil exchangeable cations were studied in three forest types of subtropical China.Four N treatments with three replications were designed for the monsoon evergreen broadleaf forest (mature forest):control (0 kg N ha-1 year-1),low N (50 kg N ha-1 year-1),medium N (100 kg N ha-1 year-1) and high N (150 kg N ha-1 ycar-1),and only three treatments (i.e.,control,low N,medium N) were established for the pine and mixed forests.Nitrogen had been applied continuously for 26 months before the measurement.The mature forest responded more rapidly and intensively to N additions than the pine and mixed forests,and exhibited some significant negative symptoms,e.g.,soil acidification,Al mobilization and leaching of base cations from soil.The pine and mixed forests responded slowly to N additions and exhibited no significant response of soil cations.Response of soil exchangeable cations to N deposition varied in the forests of subtropical China,depending on soil N status and land-nse history.

  5. Influence of the type of exchangeable cation on the electrolytic conductivity of bentonite suspensions

    Directory of Open Access Journals (Sweden)

    Daković Aleksandra S.

    2003-01-01

    Full Text Available The electrolytic conductivity of bentonite aqueous suspensions was investigated. The starting material (Ca-Mont was exchanged with sodium ions, using an ion exchange column. The sodium form of bentonite (Na-Mont was used to obtain organobentonites. The electrolytic conductivity of the starting material, Na-Mont and organobentonites was studied for different suspension concentration. The highest value of the electrolytic conductivity was obtained for Na-Mont, while the organic cation in the bentonite structure decreased the electrolytic conductivity.

  6. Solubility and cation exchange in phosphate rock and saturated clinoptilolite mixtures

    Science.gov (United States)

    Allen, E. R.; Hossner, L. R.; Ming, D. W.; Henninger, D. L.

    1993-01-01

    Mixtures of zeolite and phosphate rock (PR) have the potential to provide slow-release fertilization of plants in synthetic soils by dissolution and ion-exchange reactions. This study was conducted to examine solubility and cation-exchange relationships in mixtures of PR and NH4- and K-saturated clinoptilolite (Cp). Batch-equilibration experiments were designed to investigate the effect of PR source, the proportion of exchangeable K and NH4, and the Cp to PR ratio on solution N, P, K, and Ca concentrations. The dissolution and cation-exchange reactions that occurred after mixing NH4- and K-saturated Cp with PR increased the solubility of the PR and simultaneously released NH4 and K into solution. The more reactive North Carolina (NC) PR rendered higher solution concentrations of NH4 and K when mixed with Cp than did Tennessee (TN) PR. Solution P concentrations for the Cp-NC PR mixture and the Cp-TN PR mixture were similar. Solution concentrations of N, P, K, and Ca and the ratios of these nutrients in solution varied predictably with the type of PR, the Cp/PR ratio, and the proportions of exchangeable K and NH4 on the Cp. Our research indicated that slow-release fertilization using Cp/PR media may provide adequate levels of N, P, and K to support plant growth. Solution Ca concentrations were lower than optimum for plant growth.

  7. Cation Exchange Resins and colonic perforation. What surgeons need to know

    OpenAIRE

    María Rita Rodríguez-Luna; Enrique Fernández-Rivera; Joaquín E. Guarneros-Zárate; Jorge Tueme-Izaguirre; José Roberto Hernández-Méndez

    2015-01-01

    Introduction: Since 1961 the use of Cation Exchange Resins has been the mainstream treatment for chronic hyperkalemia. For the past 25 years different kind of complications derived from its clinical use have been recognized, being the colonic necrosis the most feared and lethal of all. Presentation of case: We report a case of a 72-year-old patient with chronic kidney disease, treated with calcium polystyrene sulfonate for hyperkalemia treatment who presented in the emergency department wi...

  8. Tuning light emission of PbS nanocrystals from infrared to visible range by cation exchange

    KAUST Repository

    Binetti, Enrico

    2015-10-27

    Colloidal semiconductor nanocrystals, with intense and sharp-line emission between red and near-infrared spectral regions, are of great interest for optoelectronic and bio-imaging applications. The growth of an inorganic passivation layer on nanocrystal surfaces is a common strategy to improve their chemical and optical stability and their photoluminescence quantum yield. In particular, cation exchange is a suitable approach for shell growth at the expense of the nanocrystal core size. Here, the cation exchange process is used to promote the formation of a CdS passivation layer on the surface of very small PbS nanocrystals (2.3 nm in diameter), blue shifting their optical spectra and yielding luminescent and stable nanostructures emitting in the range of 700–850 nm. Structural, morphological and compositional investigation confirms the nanocrystal size contraction after the cation-exchange process, while the PbS rock-salt crystalline phase is retained. Absorption and photoluminescence spectroscopy demonstrate the growth of a passivation layer with a decrease of the PbS core size, as inferred by the blue-shift of the excitonic peaks. The surface passivation strongly increases the photoluminescence intensity and the excited state lifetime. In addition, the nanocrystals reveal increased stability against oxidation over time. Thanks to their absorption and emission spectral range and the slow recombination dynamics, such highly luminescent nano-objects can find interesting applications in sensitized photovoltaic cells and light-emitting devices.

  9. Insights into cation exchange selectivity of a natural clinoptilolite by means of dielectric relaxation spectroscopy

    Science.gov (United States)

    Rodríguez-Fuentes, Gerardo; Devautour-Vinot, Sabine; Diaby, Sekou; Henn, François

    2011-09-01

    Purified natural clinoptilolite from the Tasajeras deposit, Cuba, and some of its metal exchanged forms are studied, at the dehydrated state, by means of dielectric relaxation spectroscopy (DRS) using two different modus operandi: complex impedance spectroscopy and dielectric dynamic thermal analysis. Data analysis yields the determination of the extra-framework cation (EFC) population into the various possible crystallographic sites of the zeolitic framework as well as of the activation energy characterizing the localized hopping mechanism of EFC. First, it is shown that the DRS responses obtained here match well with the previous reported data, which were previously localized EFCs in positions close to M1 and M2 sites when the clinoptilolite is modified to almost homoionic form. From this outcome, it can be concluded that all EFCs are in the same crystallographic situation regarding solvation or, in other terms, that no steric effect can be taken into account to explain cationic selectivity. Second, based on the assumption that the activation energy for EFC hopping is directly connected to the EFC/framework interaction and on simple thermodynamics consideration, we show this interaction does not govern the EFC exchange reaction. So, it is emphasized that EFC/H2O interaction is the key factor for cation exchange selectivity.

  10. Cation exchange on the nanoscale: an emerging technique for new material synthesis, device fabrication, and chemical sensing.

    Science.gov (United States)

    Rivest, Jessy B; Jain, Prashant K

    2013-01-01

    Cation exchange is an age-old technique for the chemical conversion of liquids or extended solids by place-exchanging the cations in an ionic material with a different set of cations. The technique is undergoing a major revival with the advent of high-quality nanocrystals: researchers are now able to overcome the limitations in bulk systems and fully exploit cation exchange for materials synthesis and discovery via rapid, low-temperature transformations in the solid state. In this tutorial review, we discuss cation exchange as a promising materials synthesis and discovery tool. Exchange on the nanoscale exhibits some unique attributes: rapid kinetics at room temperature (orders of magnitude faster than in the bulk) and the tuning of reactivity via control of nanocrystal size, shape, and surface faceting. These features make cation exchange a convenient tool for accessing nanocrystal compositions and morphologies for which conventional synthesis may not be established. A simple exchange reaction allows extension of nanochemistry to a larger part of the periodic table, beyond the typical gamut of II-VI, IV-VI, and III-V materials. Cation exchange transformations in nanocrystals can be topotactic and size- and shape-conserving, allowing nanocrystals synthesized by conventional methods to be used as templates for production of compositionally novel, multicomponent, or doped nanocrystals. Since phases and compositions resulting from an exchange reaction can be kinetically controlled, rather than governed by the phase diagram, nanocrystals of metastable and hitherto inaccessible compositions are attainable. Outside of materials synthesis, applications for cation exchange exist in water purification, chemical staining, and sensing. Since nanoscale cation exchange occurs rapidly at room temperature, it can be integrated with sensitive environments such as those in biological systems. Cation exchange is already allowing access to a variety of new materials and processes

  11. Unfolding and aggregation of monoclonal antibodies on cation exchange columns: effects of resin type, load buffer, and protein stability.

    Science.gov (United States)

    Guo, Jing; Carta, Giorgio

    2015-04-03

    The chromatographic behavior of a monoclonal antibody (mAb) that exhibits a pronounced two-peak elution behavior is studied for a range of strong cation exchange resins and with varying load buffer pH and composition. Six stationary phases are considered, including two tentacle-type resins (Fractogel EMD SO3-(M) and Eshmuno S), a resin with grafted polymeric surface extenders (Nuvia S), a resin with a bimodal pore size distribution (POROS HS 50), and two macroporous resins without polymer grafts (Source 30S and UNOsphere Rapid S). The two-peak elution behavior is very pronounced for the tentacle and polymer-grafted resins and for POROS HS 50, but is essentially absent for the two macroporous resins. The extent of this behavior decreases as the buffer pH and concentration increase and, consequently, mAb binding becomes weaker. Replacing sodium with arginine as the buffer counterion, which is expected to decrease the mAb binding strength, nearly completely eliminates the two-peak behavior, while replacing sodium with tetra-n-butylammonium hydroxide, which is expected to increase the mAb binding strength, dramatically exacerbate the effect. As shown by hydrogen-deuterium exchange mass spectrometry (HX-MS), the two-peak elution behavior is related to conformational changes that occur when the mAb binds. These changes result in increased solvent exposure of specific peptides in the Fc-region for either the Fractogel or the Nuvia resin. No significant conformational changes were seen by HX-MS when the mAb was bound to the UNOsphere resin or on the Fractogel resin when arginine was used in lieu of sodium as the load buffer counterion. Experiments with two additional mAbs on the Fractogel resin show that the two-peak elution behavior is dependent on the particular antibody. Circular dichroism suggests that the propensity of different mAbs to either precipitate directly or to form stabilizing intermolecular structures upon exposure to thermal stress can be related to their

  12. Anion and cation mixed-bed ion exchange for enhanced multidimensional separations of peptides and phosphopeptides.

    Science.gov (United States)

    Motoyama, Akira; Xu, Tao; Ruse, Cristian I; Wohlschlegel, James A; Yates, John R

    2007-05-15

    Shotgun proteomics typically uses multidimensional LC/MS/MS analysis of enzymatically digested proteins, where strong cation-exchange (SCX) and reversed-phase (RP) separations are coupled to increase the separation power and dynamic range of analysis. Here we report an on-line multidimensional LC method using an anion- and cation-exchange mixed bed for the first separation dimension. The mixed-bed ion-exchange resin improved peptide recovery over SCX resins alone and showed better orthogonality to RP separations in two-dimensional separations. The Donnan effect, which was enhanced by the introduction of fixed opposite charges in one column, is proposed as the mechanism responsible for improved peptide recovery by producing higher fluxes of salt cations and lower populations of salt anions proximal to the SCX phase. An increase in orthogonality was achieved by a combination of increased retention for acidic peptides and moderately reduced retention of neutral to basic peptides by the added anion-exchange resin. The combination of these effects led to approximately 100% increase in the number of identified peptides from an analysis of a tryptic digest of a yeast whole cell lysate. The application of the method to phosphopeptide-enriched samples increased by 94% phosphopeptide identifications over SCX alone. The lower pKa of phosphopeptides led to specific enrichment in a single salt step resolving acidic phosphopeptides from other phospho- and non-phosphopeptides. Unlike previous methods that use anion exchange to alter selectivity or enrich phosphopeptides, the proposed format is unique in that it works with typical acidic buffer systems used in electrospray ionization, making it feasible for online multidimensional LC/MS/MS applications.

  13. Synthesis, characterization and ion exchange properties of zirconium(IV) tungstoiodophosphate, a new cation exchanger

    Indian Academy of Sciences (India)

    Weqar Ahmad Siddiqui; Shakeel Ahmad Khan

    2007-02-01

    Zirconium(IV) tungstoiodophosphate has been synthesized under a variety of conditions. The most chemically and thermally stable sample is prepared by adding a mixture of aqueous solutions of 0.5 mol L-1 sodium tungstate, potassium iodate and 1 mol L-1 orthophosphoric acid to aqueous solution of 0.1 mol L-1 zirconium(IV) oxychloride. Its ion exchange capacity for Na+ and K+ was found to be 2.20 and 2.35 meq g-1 dry exchanger, respectively. The material has been characterized on the basis of chemical composition, pH titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. The effect on the exchange capacity of drying the exchanger at different temperatures has been studied. The analytical importance of the material has been established by quantitative separation of Pb2+ from other metal ions.

  14. CATION-EXCHANGE MEMBRANES WITH POLYANILINE SURFACE LAYER FOR WATER TREATMENT

    Directory of Open Access Journals (Sweden)

    Dinar Dilshatovich Fazullin

    2014-01-01

    Full Text Available Ion-exchange membranes are widely used in modern technologies, particularly in the field of water treatment and make it possible to considerably reduce expenses for wastewater treatment and ensure high degree of purification. Currently, perfluorinated sulfated proton-conducting membranes are often used, such as NAFION and its Russian analogue, MF-4SK based on co-polymerization product of a perfluorinated vinyl ether with tetrafluoroethylene. However, with development of the industry, materials with improved properties and lower cost are required. The aim is to obtain ion-exchange membranes for water treatment from metal ions and to study physico-chemical properties of obtained membranes. In this study, cation exchange composite membranes with modified polyaniline surface layer on nylon and PTFE substrate have been obtained. Changes in the structure of membranes were recorded using a microscope. Throughput capacity of the membranes was determined by passing a certain volume of distilled water through the membrane. The experiment intended to determine electivity of membranes was performed by passing a certain volume of metal salt solutions of a known concentration, after which the filtrate was collected. Concentrations of the studied metal ions in the original solution and in the filtrate were determined by the method of atomic adsorptive spectrometry with electro thermal atomization "Quantum Z.ETA". Prepared highly selective ion exchange membranes. Properties of modified membranes, such as selective permeability and ion-exchange capacity have been determined. The membranes feature high selectivity for heavy metal ions. Moisture-retaining power and swelling ability of the membranes have been studied. Selectivity of the membrane to heavy metal ions is between 70 and 99%. Ion-exchange capacity of the obtained nylon polyaniline membrane is not inferior to some commercially available cation-exchange membranes. Use of the modified membranes in the

  15. Analyzing freely dissolved concentrations of cationic surfactant utilizing ion-exchange capability of polyacrylate coated solid-phase microextraction fibers

    NARCIS (Netherlands)

    Chen, Y.; Droge, S.T.J.; Hermens, J.L.M.

    2012-01-01

    A 7-μm polyacrylate (PA) coated fiber was successfully employed to determine freely dissolved concentrations of cationic surfactants by solid-phase microextraction (SPME) and utilizing the capability of the PA-coating to sorb organic cations via ion-exchange at carboxylic groups. Measured fiber-wate

  16. Preparation of a Cation Exchanger from Cork Waste: Thermodynamic Study of the Ion Exchange Processes

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    An ion exchanger was prepared by sulfonation of cork-waste chars. The exchange properties of the resultant materialwere characterized using Na+, Ca2+ or Fe3+ aqueous solutions, The content of metal ions in the solutions weredetermined by atomic absorption spectrometry. On the basis of the results obtained, the chemical equilibrium andits thermodynamic aspects related to the ion exchange process were studied. It was found that equilibrium constantK varies by the order: Na+<Ca2+<Fe3+, its value increasing with increasing temperature, and that △H°>0 and△S°>0, with -△G° following the sequence: Ca2+>Na+>Fe3+,

  17. Hydrogeochemical evolution of confined groundwater in northeastern Osaka Basin, Japan: estimation of confined groundwater flux based on a cation exchange mass balance method

    Energy Technology Data Exchange (ETDEWEB)

    Yamanaka, Masaru [Department of Geosystem Sciences, College of Humanities and Sciences, Nihon University, Setagaya-ku, Tokyo 156-8550 (Japan)]. E-mail: yamanaka@chs.nihon-u.ac.jp; Nakano, Takanori [Research Institute for Humanity and Nature, Kamigyo-ku, Kyoto 602-0878 (Japan); Tase, Norio [Institute of Geoscience, University of Tsukuba, Tsukuba, Ibaraki 305-8571 (Japan)

    2005-02-01

    A confined aquifer system has developed in argillaceous marine and freshwater sediments of Pliocene-Holocene age in the northeastern Osaka Basin (NEOB) in central Japan. The shallow groundwater (<100 m) in the system is recharged in a northern hilly to mountainous area with dominantly Ca-HCO{sub 3} type water, which changes as it flows toward the SW to Mg-HCO{sub 3} type and then to Na-HCO{sub 3} type water. Comparison of the chemical and Sr isotopic compositions of the groundwater with those of the bulk and exchangeable components of the underground sediments indicates that elements leached from the sediments contribute negligibly to the NEOB aquifer system. Moreover, model calculations show that contributions of paleo-seawater in the deep horizon and of river water at the surface are not major factors of chemical change of the groundwater. Instead, the zonal pattern of the HCO{sub 3}-dominant groundwater is caused by the loss of Ca{sup 2+} from the water as it is exchanged for Mg{sup 2+} in clays, followed by loss of Mg + Ca as they are exchanged for Na + K in clays between the Ca-HCO{sub 3} type recharge water and the exchangeable cations in the clay layers, which were initially enriched in Na{sup +}. Part of this process was reproduced in a chromatographic experiment in which Na type water with high {sup 87}Sr/{sup 86}Sr was obtained from Mg type water with low {sup 87}Sr/{sup 86}Sr by passing it through marine clay packed in a column. The flux of recharge water into the confined aquifer system according to this chromatographic model is estimated to be 0.99 mm/day, which is compatible with the average recharge flux to unconfined groundwater in Japan (1 mm/day)

  18. Chabazite: stable cation-exchanger in hyper alkaline concrete pore water.

    Science.gov (United States)

    Van Tendeloo, Leen; Wangermez, Wauter; Kurttepeli, Mert; de Blochouse, Benny; Bals, Sara; Van Tendeloo, Gustaaf; Martens, Johan A; Maes, André; Kirschhock, Christine E A; Breynaert, Eric

    2015-02-17

    To avoid impact on the environment, facilities for permanent disposal of hazardous waste adopt multibarrier design schemes. As the primary barrier very often consists of cement-based materials, two distinct aspects are essential for the selection of suitable complementary barriers: (1) selective sorption of the contaminants in the repository and (2) long-term chemical stability in hyperalkaline concrete-derived media. A multidisciplinary approach combining experimental strategies from environmental chemistry and materials science is therefore essential to provide a reliable assessment of potential candidate materials. Chabazite is typically synthesized in 1 M KOH solutions but also crystallizes in simulated young cement pore water, a pH 13 aqueous solution mainly containing K(+) and Na(+) cations. Its formation and stability in this medium was evaluated as a function of temperature (60 and 85 °C) over a timeframe of more than 2 years and was also asessed from a mechanistic point of view. Chabazite demonstrates excellent cation-exchange properties in simulated young cement pore water. Comparison of its Cs(+) cation exchange properties at pH 8 and pH 13 unexpectedly demonstrated an increase of the KD with increasing pH. The combined results identify chabazite as a valid candidate for inclusion in engineered barriers for concrete-based waste disposal.

  19. CATION EXCHANGE CAPACITY OF DOMINANT SOIL TYPES IN THE REPUBLIC OF CROATIA

    Directory of Open Access Journals (Sweden)

    Marija Tomasic

    2013-09-01

    Full Text Available The study was conducted on 18 locations and 11 dominant soil types in the Republic of Croatia including their evolution-genetic horizons. In total, 51 soil samples were examined. Analysis of soil was done by saturating patterns using barium chloride solution in three replications. Descriptive statistics of the analyzed data was conducted. Basic statistical parameters were calculated, and functional dependence between the base saturation (V% of analyzed soil samples and their pH was observed. The correlation coefficient (r between base saturation (V% and pH for all examined soils was r=0.79 (n=51; very strong correlation. For acid soils it was r=0.82 (n=17; very strong correlation, for neutral soils r=0.75 (n=8; very strong correlation, and finally for alkaline soils r=0.15 (n=26; very weak correlation. Cation exchange capacity values ranged from 2.39 cmol+*kg-1 to 33.8 cmol+*kg-1 depending on soil type, pH, organic content and other soil parameters. The content of exchangeable cations in the sum of basic cations ranged from: Ca2+ (16% - 94%, Mg2+ (2% - 41%, K+ (1% - 68% and Na+ (<0.01% also depending on soil type, depth, location and other physical and chemical soil parameters.

  20. Carbon dioxide and nitrogen adsorption on cation-exchanged SSZ-13 zeolites.

    Science.gov (United States)

    Pham, Trong D; Liu, Qingling; Lobo, Raul F

    2013-01-15

    Samples of high-silica SSZ-13, ion exchanged with protons and alkali-metal cations Li(+), Na(+), and K(+), were investigated using adsorption isotherms of CO(2) and N(2). The results show that Li-, Na-SSZ-13 have excellent CO(2) capacity at ambient temperature and pressure; in general, Li-SSZ-13 shows the highest capacity for N(2), CO(2) particularly in the low-pressure region. The effect of cation type and Si/Al ratio (6 and 12) on the adsorption properties was investigated through analysis of adsorption isotherms and heats of adsorption. The separation of CO(2) in a flue gas mixture was evaluated for these adsorbents in the pressure swing adsorption and vacuum pressure adsorption processes.

  1. Cation exchange resin nanocomposites based on multi-walled carbon nanotubes

    Science.gov (United States)

    Fathy, Mahmoud; Abdel Moghny, Th.; Awad Allah, Ahmed Elsayed; Alblehy, AbdElhamid

    2014-01-01

    Carbon nanotubes (CNTs) are of great interest due to their potential applications in different fields such as water treatment and desalination. The increasing exploitation of multi-walled carbon nanotubes (MWCNTs) into many industrial processes has raised considerable concerns for environmental applications. The interactions of soluble salt with MWNCTs influence in the total salt content in saline water. In this work, we synthesized two cation exchange resins nano composites from polystyrene divinylbenzene copolymer (PSDVB) and pristine MWNCTs. The prepared compounds were characterized using infra red spectroscopy, thermal stability, X-ray diffraction, and electro scan microscope. Also, the ion capacities of prepared cation exchange resins were determined by titration. Based on the experimental results, it was found that the thermal stability of prepared nanocomposites in the presence of MWNCTs increased up to 617 °C. The X-ray of PSDVB and its sulfonated form exhibits amorphous pattern texture structure, whereas the nano composite exhibits amorphous structure with indication peak at 20° and 26° for the PSDVB and MWCNTs, respectively. The ion-exchange capacity increased from 225.6 meq/100 g to 466 mg/100 g for sulfonated PSDVB and sulfonated PSDVB MWNCTs-pristine, respectively.

  2. On the real performance of cation exchange resins in wastewater treatment under conditions of cation competition: the case of heavy metal pollution.

    Science.gov (United States)

    Prelot, Benedicte; Ayed, Imen; Marchandeau, Franck; Zajac, Jerzy

    2014-01-01

    Sorption performance of cation-exchange resins Amberlite® IRN77 and Amberlite™ IRN9652 toward Cs(I) and Sr(II) has been tested in single-component aqueous solutions and simulated waste effluents containing other monovalent (Effluent 1) or divalent (Effluent 2) metal cations, as well as nitrate, borate, or carbonate anions. The individual sorption isotherms of each main component were measured by the solution depletion method. The differential molar enthalpy changes accompanying the ion-exchange between Cs+ or Sr2+ ions and protons at the resin surface from single-component nitrate solutions were measured by isothermal titration calorimetry and they showed a higher specificity of the two resins toward cesium. Compared to the retention limits of both resins under such idealized conditions, an important depression in the maximum adsorption capacity toward each main component was observed in multication systems. The overall effect of ion exchange process appeared to be an unpredictable outcome of the individual sorption capacities of the two resins toward various cations as a function of the cation charge, size, and concentration. The cesium retention capacity of the resins was diminished to about 25% of the "ideal" value in Effluent 1 and 50% in Effluent 2; a further decrease to about 15% was observed upon concomitant strontium addition. The uptake of strontium by the resins was found to be less sensitive to the addition of other metal components: the greatest decrease in the amount adsorbed was 60% of the ideal value in the two effluents for Amberlite® IRN77 and 75% for Amberlite™ IRN9652. It was therefore demonstrated that any performance tests carried out under idealized conditions should be exploited with much caution to predict the real performance of cation exchange resins under conditions of cation competition.

  3. Determination of organoarsenic species in marine samples using gradient elution cation exchange HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, Kåre

    2003-01-01

    A method for the determination of arsenic species in marine samples using high performance liquid chromatography coupled to inductively coupled mass spectrometry (HPLC-ICP-MS) has been developed. Cation exchange HPLC with gradient elution using pyridine formate as the mobile phase was employed...... the certified limits and low detection limits of 0.002-0.005 mug g(-1) dry mass (as As) for the different arsenic species were obtained. At least 23 different organic arsenic species were detected in a scallop kidney in one analytical run of 25 min duration. The ability of our analytical method to detect...

  4. Refolding of Denatured/Reduced Lysozyme Using Weak-Cation Exchange Chromatography

    Institute of Scientific and Technical Information of China (English)

    Yan WANG; Bo Lin GONG; Xin Du GENG

    2003-01-01

    Oxidative refolding of the denatured/reduced lysozyme was investigated by using weak-cation exchange chromatography (WCX). The stationary phase of WCX binds to the reduced lysozyme and prevented it from forming intermolecular aggregates. At the same time urea and ammonium sulfate were added to the mobile phase to increase the elution strength for lysozyme. Ammonium sulfate can more stabilize the native protein than a common eluting agent, sodium chloride. Refolding of lysozyme by using this WCX is successfully. It was simply carried out to obtain a completely and correctly refolding of the denatured lysozyme at high concentration of 20.0 mg/mL.

  5. PREPARATION OF SA-Fe CATION EXCHANGE MEMBRANE AND IT'S APPLICATION IN ELECTRODIALYSIS FOR TREATING WASTEWATER

    Institute of Scientific and Technical Information of China (English)

    GENG Yamin; CHEN Zhen; ZHENG Xi; HUANG Xuehong; CHEN Riyao

    2006-01-01

    An insoluble SA-Fe membrane was prepared by being linked soluble sodium alginate with FeCl3. SEM was used to observe its surface structure. IR spectrum indicated that Fe3+ was linked with -COOH and -OH in SA membrane. As a cationic exchanging membrane in electrodialysis the membrane was applied in treating inorganic wastewater with high concentration of inorganic ammonia and azote. The results of experiment showed that it was well-selective to ammonia and azote. The percentage of the removal of ammonia and azote in wastewater was up to 80%.

  6. 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.

  7. Modified DIX model for ion-exchange equilibrium of L-phenylalanine on a strong cation-exchange resin☆

    Institute of Scientific and Technical Information of China (English)

    Jinglan Wu; Pengfei Jiao; Wei Zhuang; Jingwei Zhou; Hanjie Ying

    2016-01-01

    L-phenylalanine, one of the nine essential amino acids for the human body, is extensively used as an ingredient in food, pharmaceutical and nutrition industries. A suitable equilibrium model is required for purification of L-phenylalanine based on ion-exchange chromatography. In this work, the equilibrium uptake of L-phenylalanine on a strong acid-cation exchanger SH11 was investigated experimental y and theoretical y. A modified Donnan ion-exchange (DIX) model, which takes the activity into account, was established to predict the uptake of L-phenyl-alanine at various solution pH values. The model parameters including selectivity and mean activity coefficient in the resin phase are presented. The modified DIX model is in good agreement with the experimental data. The optimum operating pH value of 2.0, with the highest L-phenylalanine uptake on the resin, is predicted by the model. This basic information combined with the general mass transfer model wil lay the foundation for the prediction of dynamic behavior of fixed bed separation process.

  8. Model Simulations of a Field Experiment on Cation Exchange-affected Multicomponent Solute Transport in a Sandy Aquifer

    DEFF Research Database (Denmark)

    Bjerg, Poul Løgstrup; Ammentorp, Hans Christian; Christensen, Thomas Højlund

    1993-01-01

    A large-scale and long-term field experiment on cation exchange in a sandy aquifer has been modelled by a three-dimensional geochemical transport model. The geochemical model includes cation-exchange processes using a Gaines-Thomas expression, the closed carbonate system and the effects of ionic...... of 800 days due to a substantially attenuation in the aquifer. The observed and the predicted breakthrough curves showed a reasonable accordance taking the duration of the experiment into account. However, some discrepancies were observed probably caused by the revealed non-ideal exchange behaviour of K+....

  9. A simple method for estimating cation exchange capacity from water vapor sorption

    DEFF Research Database (Denmark)

    Arthur, Emmanuel; Tuller, Markus

    2016-01-01

    Knowledge of soil cation exchange capacity (CEC) is crucial for soil fertility considerations, sorption and release of polar and non-polar compounds, engineering applications, and other biogeochemical processes. Standard procedures such as the ammonium acetate or the BaCl2 compulsive exchange...... methods are expensive and laborious, and in previous studies the CEC has been predicted from parameters such as particle size distribution and organic matter content, specific surface area, clay content, and from Atterberg limits. In this study, relative humidity (RH)-dependent pedotransfer functions...... (PTFs) for estimating CEC from soil water content considering hysteresis have been developed based on 203 differently-textured soils. Furthermore, we compared the performance of the new PTFs with existing PTFs that predict CEC from clay content, organic carbon, soil pH and specific surface area. The new...

  10. Measurement of (90)Sr in environmental samples by cation-exchange and liquid scintillation counting.

    Science.gov (United States)

    Amano, H; Yanase, N

    1990-06-01

    A new method for the measurement of (90)Sr in environmental samples by cation-exchange and liquid scintillation counting is described. Strontium carbonate is purified by precipitation and ion-exchange, weighed for the determination of chemical yield, dissolved in hydrochloric acid and mixed with the liquid scintillator, Aquasol-2. Two channels of a low-background liquid scintillation counter are used to determine (90)Sr, (90)Y and (89)Sr, free from the effects of environmental tritium. The values of (90)Sr obtained by this method are in good agreement with those from ordinary (90)Y milking and the gas proportional counting method. The concentration of (90)Sr in the air at Tokai-mura in Japan has been measured by the new method.

  11. Kinetics of Isovalent (Cd(2+)) and Aliovalent (In(3+)) Cation Exchange in Cd1-xMnxSe Nanocrystals.

    Science.gov (United States)

    Chakraborty, Pradip; Jin, Yu; Barrows, Charles J; Dunham, Scott T; Gamelin, Daniel R

    2016-10-05

    Ion exchange, in which an in-diffusing ion replaces a lattice ion, has been widely exploited as a synthetic tool for semiconductor doping and solid-to-solid chemical transformations, both in bulk and at the nanoscale. Here, we present a systematic investigation of cation-exchange reactions that involve the displacement of Mn(2+) from CdSe nanocrystals by Cd(2+) or In(3+). For both incoming cations, Mn(2+) displacement is spontaneous but thermally activated, following Arrhenius behavior over a broad experimental temperature range. At any given temperature, cation exchange by In(3+) is approximately 2 orders of magnitude faster than that by Cd(2+), illustrating a critical dependence on the incoming cation. Quantitative analysis of the kinetics data within a Fick's-law diffusion model yields diffusion barriers (ED) and limiting diffusivities (D0) for both incoming ions. Despite their very different kinetics, indistinguishable diffusion barriers of ED ≈ 1.1 eV are found for both reactions (In(3+) and Cd(2+)). A dramatically enhanced diffusivity is found for Mn(2+) cation exchange by In(3+). Overall, these findings provide unique experimental insights into cation diffusion within colloidal semiconductor nanocrystals, contributing to our fundamental understanding of this rich and important area of nanoscience.

  12. On-line cation-exchange preconcentration and capillary electrophoresis coupled by tee joint interface.

    Science.gov (United States)

    Zhang, Zhao-Xiang; He, You-Zhao

    2005-02-25

    An on-line preconcentration method based on ion exchange solid phase extraction was developed for the determination of cationic analytes in capillary electrophoresis (CE). The preconcentration-separation system consisted of a preconcentration capillary bonded with carboxyl cation-exchange stationary phase, a separation capillary for zone electrophoresis and a tee joint interface of the capillaries. Two capillaries were connected closely inside a 0.3 mm i.d. polytetrafluoroethylene tube with a side opening and fixed together by the interface. The preparations of the preconcentration capillaries and interface were described in detail in this paper. The on-line preconcentration and separation procedure of the analysis system included washing and conditioning the capillaries, loading analytes, filling with buffer solution, eluting analytes and separating by capillary zone electrophoresis (CZE). Several analysis parameters, including sample loading flow rate and time, eluting solution and volume, inner diameter and length of preconcentration capillary etc., were investigated. The proposed method enhanced the detection sensitivity of CE-UV about 5000 times for propranolol and metoprolol compared with normally electrokinetic injection. The detection limits of propranolol and metoprolol were 0.02 and 0.1 microg/L with the proposed method respectively, whereas those were 0.1 and 0.5 mg/L with conventional electrokinetic injection. The experiment results demonstrate that the proposed technique can increase the preconcentration factor evidently.

  13. Morphologically Aligned Cation-Exchange Membranes by a Pulsed Electric Field for Reverse Electrodialysis.

    Science.gov (United States)

    Lee, Ju-Young; Kim, Jae-Hun; Lee, Ju-Hyuk; Kim, Seok; Moon, Seung-Hyeon

    2015-07-21

    A low-resistance ion-exchange membrane is essential to achieve the high-performance energy conversion or storage systems. The formation methods for low-resistance membranes are various; one of the methods is the ion channel alignment of an ion-exchange membrane under a direct current (DC) electric field. In this study, we suggest a more effective alignment method than the process with the DC electric field. First, an ion-exchange membrane was prepared under a pulsed electric field [alternating current (AC) mode] to enhance the effectiveness of the alignment. The membrane properties and the performance in reverse electrodialysis (RED) were then examined to assess the membrane resistance and ion selectivity. The results show that the membrane electrical resistance (MER) had a lower value of 0.86 Ω cm(2) for the AC membrane than 2.13 Ω cm(2) observed for the DC membrane and 4.30 Ω cm(2) observed for the pristine membrane. Furthermore, RED achieved 1.34 W/m(2) of maximum power density for the AC membrane, whereas that for the DC membrane was found to be 1.14 W/m(2) [a RED stack assembled with CMX, used as a commercial cation-exchange membrane (CEM), showed 1.07 W/m(2)]. Thereby, the novel preparation process for a remarkable low-resistance membrane with high ion selectivity was demonstrated.

  14. Solubility and Cation Exchange Properties of Synthetic Hydroxyapatite and Clinoptilolite Mixtures

    Science.gov (United States)

    Beiersdorfer, Raymond E.; Ming, Douglas W.

    2003-01-01

    A zeoponic plant growth system is defined as the cultivation of plants in artificial soils, which have zeolites as a major component. These systems: 1) can serve as a controllable and renewable fertilization system to provide plant growth nutrients; 2) can mitigate the adverse effects of contamination due to leaching of highly soluble and concentrated fertilizers; and 3) are being considered as substrates for plant growth in regenerative life-support systems for long-duration space missions. Batch-equilibrium studies of the dissolution and ion-exchange properties of mixtures of naturally-occurring Wyoming clinoptilolite (a zeolite) exchanged with K(+) or NH4(+); and synthetic hydroxyapatite were conducted to determine: 1) the plant availability of the macro-nutrients NH4-N, P, K, Ca, and Mg and 2) the effects of varying the clinoptilolite to hydroxyapatite ratio and the ratio of exchangeable cations (K(+) vs. NH4(+)) on clinoptilolite extraframework sites. The nutrients NH4-N (19.7 to 73.6 mg L(sup -1), P (0.57 to 14.99 mg L(sup- 1), K (14.8 to 104.9 mg L(sup -1), and Mg (0.11 to 6.68mg L(sup -1) are available to plants at sufficient levels. Solution Ca concentrations (0.47 to 3.40 mg L(sup -1) are less than optimal. Solution concentrations of NH4(+), K(+), Ca(2+), and Mg(2+) all decreased with increasing clinoptilolite to hydroxyapatite ratio in the sample. Solution concentrations of phosphorous initially increased, reached a maximum value and then decreased with increasing clinoptilolite to hydroxyapatite ratio in the sample. The NH4(+) -exchanged clinoptilolite is more efficient in dissolving synthetic hydroxyapatite than the K(+) -exchanged clinoptilolite. This suggests that NH4(+), which is less selective at clinoptilolite extraframework sites than K(+) is exchanged more readily by Ca(2+) and thereby enhances the dissolution of the synthetic hydroxyapatite.

  15. Cu2Se and Cu Nanocrystals as Local Sources of Copper in Thermally Activated In Situ Cation Exchange

    KAUST Repository

    Casu, Alberto

    2016-01-27

    Among the different synthesis approaches to colloidal nanocrystals a recently developed toolkit is represented by cation exchange reactions, where the use of template nanocrystals gives access to materials that would be hardly attainable via direct synthesis. Besides, post-synthetic treatments, such as thermally activated solid state reactions, represent a further flourishing route to promote finely controlled cation exchange. Here, we report that, upon in situ heating in a transmission electron microscope, Cu2Se nanocrystals deposited on an amorphous solid substrate undergo partial loss of Cu atoms, which are then engaged in local cation exchange reactions with Cu “acceptors” phases represented by rod- and wire- shaped CdSe nanocrystals. This thermal treatment slowly transforms the initial CdSe nanocrystals into Cu2-xSe nanocrystals, through the complete sublimation of Cd and the partial sublimation of Se atoms. Both Cu “donor” and “acceptor” particles were not always in direct contact with each other, hence the gradual transfer of Cu species from Cu2Se or metallic Cu to CdSe nanocrystals was mediated by the substrate and depended on the distance between the donor and acceptor nanostructures. Differently from what happens in the comparably faster cation exchange reactions performed in liquid solution, this study shows that slow cation exchange reactions can be performed at the solid state, and helps to shed light on the intermediate steps involved in such reactions.

  16. Sorption of Ni(II) ions from aqueous solution by Lewatit cation-exchange resin.

    Science.gov (United States)

    Dizge, Nadir; Keskinler, Bülent; Barlas, Hulusi

    2009-08-15

    Ion-exchange is an alternative process for uptake of heavy metals from aqueous solutions. In the present study, the sorption of nickel(II) ions from aqueous solution was investigated by using Lewatit MonoPlus SP 112 (strongly acidic, macroporous cation-exchange resin) in a batch adsorption system as a function of pH (2.0-8.0), initial nickel concentration (50-200 mg/L), resin dosage (0.5-2.0 g/L), contact time (0.5-3h), and temperatures (298-318K). The data were analyzed on the basis of Lagergren pseudo-first order, pseudo-second order (Types 1-5), Elovich and external, Weber-Morris intraparticle, pore-surface mass diffusion models. The experimental data showed that the maximum pH for efficient sorption of nickel(II) was 6.0. At the optimal conditions, nickel(II) ions sorption on the resin was decreased when the initial metal concentration increased. The results indicated that the resin dosage strongly affected the amount of nickel(II) ions removed from aqueous solution. The adsorption process was very fast due to 80% of nickel(II) sorption was occurred within 30 min and equilibrium was reached at about 90 min. Freundlich and Langmuir adsorption isotherm models were used for sorption equilibrium data and the maximum adsorption capacity (171 mg/g) of Lewatit MonoPlus SP 112 was obtained from Langmuir isotherm. The thermodynamic parameters (DeltaG degrees, free energy change; DeltaS degrees, enthalpy change; and DeltaH degrees, entropy change) for sorption of nickel(II) ions were evaluated. The rise in temperature caused a partly increase in the value of the equilibrium constant (K(c)) for the sorption of nickel(II) ions. Moreover, column flow adsorption study was also studied. Breakthrough curves were obtained from column flow studies by using both synthetic solution and rinsing bath water of filter industry. The column regeneration was carried out for two sorption-desorption cycles. The eluant used for regeneration of the cation-exchange resin was 7% (w/w) HCl. The

  17. Effects of exchangeable cation composition on the thermal expansion/contraction of clinoptilolite

    Energy Technology Data Exchange (ETDEWEB)

    Bish, D.L.

    1984-12-31

    To understand and predict the effects of a thermal pulse induced by a radioactive waste repository on clinoptilolite-bearing rocks, the lattice parameters of 6 natural and 3 cation-exchanged (Ca, K, Na) clinoptilolites were studied as a function of temperature. The samples were examined at room temperature, under vacuum, and at 50{sup 0}C increments to 300{sup 0}C using a high-temperature x-ray powder diffractometer. The unit cell of all samples decreased in volume between 20 and 300{sup 0}C; Na-saturated clinoptilolite underwent the greatest volume decrease (8.4%) and K-saturated clinoptilolite the smallest (1.6%), of the clinoptilolites studied. The volume decrease for the Ca-saturated clinoptilolite was 3.6%. The highest percentage decrease for each sample was along the b axis, generally 80 to 90% of the total volume decrease. The change in the a axis was the smallest and was usually <5%, although 26.5% of the contraction of the Na-exchanged clinoptilolite was along a. The bulk of the volume contraction of many samples occurred on evacuation at room temperature, demonstrating that the observed changes were due to water loss and not to temperature-induced structural changes. Low-angle scattering was significantly reduced upon evacuation for every sample, and the 110 reflection of clinoptilolite at 7.35{sup 0}2 {theta} became obvious, whereas it was not in the untreated samples. These data show that the effects of heating on the unit-cell volume of clinoptilolite depend strongly on the exchangeable cation content. Significant reductions in the unit-cell volumes of natural, mixed Na-K-Ca clinoptilolites could take place in rocks in a repository environment, particularly if the clinoptilolites occurred in unsaturated, dehydrated rock. The unit-cell volumes of clinoptilolites in partially saturated rocks at temperatures below 100{sup 0}C, however, should not decrease significantly.

  18. Preparation and chromatographic performance of polymer-based anion exchangers for ion chromatography: A review.

    Science.gov (United States)

    Zatirakha, A V; Smolenkov, A D; Shpigun, O A

    2016-01-21

    In the last decade the developments in the field of ion chromatography (IC) were aimed at increasing the efficiency, sensitivity and rapidity of analysis, as well as on improving separation selectivity. Since selectivity and efficiency to the large extent depend on the surface chemistry of the stationary phase, the development of novel anion exchangers remains one of the priority tasks in modern IC. The exact chemistry of commercially available resins is not known and not many literature data devoted to the procedures of preparing anion exchangers for IC have become available in the last 10-15 years. However, the knowledge about the surface chemistry of anion exchangers can provide understanding of the trends in selectivity and efficiency changes, as well as help with the choice of the stationary phase type suitable for solving a particular analytical task. The current review is devoted to the methods of preparing anion exchangers based on polystyrene-divinylbenzene (PS-DVB) and ethylvinylbenzene-divinylbenzene (EVB-DVB) for IC of inorganic and small organic anions and is aimed at demonstrating the improvement of their performance over the years, which was brought by the development of the new types of stationary phase architecture.

  19. Stagnant mobile phase mass transfer in chromatographic media: Intraparticle diffusion and exchange kinetics

    NARCIS (Netherlands)

    Tallarek, U.; Vergeldt, F.J.; As, van H.

    1999-01-01

    Pulsed field gradient nuclear magnetic resonance has been successfully applied to a direct and detailed experimental study of topological and dynamic aspects involved in the exchange of small, nonsorbed fluid molecules between the intraparticle pore network and the interparticle void space in chroma

  20. Effect of blastfurnace slag addition to Portland cement for cationic exchange resins encapsulation

    Directory of Open Access Journals (Sweden)

    Stefan L.

    2013-07-01

    Full Text Available In the nuclear industry, cement-based materials are extensively used to encapsulate spent ion exchange resins (IERs before their final disposal in a repository. It is well known that the cement has to be carefully selected to prevent any deleterious expansion of the solidified waste form, but the reasons for this possible expansion are not clearly established. This work aims at filling the gap. The swelling pressure of IERs is first investigated as a function of ions exchange and ionic strength. It is shown that pressures of a few tenths of MPa can be produced by decreases in the ionic strength of the bulk solution, or by ion exchanges (2Na+ instead of Ca2+, Na+ instead of K+. Then, the chemical evolution of cationic resins initially in the Na+ form is characterized in CEM I (Portland cement and CEM III (Portland cement + blastfurnace slag cements at early age and an explanation is proposed for the better stability of CEM III material.

  1. Adsorptional removal of methylene blue by guar gum-cerium (IV) tungstate hybrid cationic exchanger.

    Science.gov (United States)

    Gupta, V K; Pathania, Deepak; Singh, Pardeep; Kumar, Amit; Rathore, B S

    2014-01-30

    Guar gum-cerium (IV) tungstate nanocomposite (GG/CTNC) cationic exchanger was synthesized using simple sol gel method. The GG/CTNC was characterized using X-ray diffraction (XRD), Fourier transmission infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and energy dispersive X-ray spectrophotometer (EDX). The XRD studies confirmed amorphous and fibrous in nature of GG/CTNC. The high percentage of oxygen in the nanocomposite material confirmed the functionality tungstate (WO4(-)). The ion exchange capacity of GG/CTNC for Na(+) ion was observed to be 1.30 mequivg(-1). The hybrid exchanger was used as potential adsorbent for the removal of methylene blue (MB) from aqueous system. The correlation coefficients value indicated a good fit of monolayer Langmuir model to the adsorption of methylene blue onto GG/CTNC. The adsorption kinetic study revealed that the adsorption process followed the pseudo second order kinetic. The Gibbs free energy (ΔG) values confirmed the spontaneous nature of adsorption process.

  2. Independent control of the shape and composition of ionic nanocrystals through sequential cation exchange reactions

    Energy Technology Data Exchange (ETDEWEB)

    Luther, Joseph Matthew; Zheng, Haimei; Sadtler, Bryce; Alivisatos, A. Paul

    2009-07-06

    Size- and shape-controlled nanocrystal growth is intensely researched for applications including electro-optic, catalytic, and medical devices. Chemical transformations such as cation exchange overcome the limitation of traditional colloidal synthesis, where the nanocrystal shape often reflects the inherent symmetry of the underlying lattice. Here we show that nanocrystals, with established synthetic protocols for high monodispersity, can be templates for independent composition control. Specifically, controlled interconversion between wurtzite CdS, chalcocite Cu2S, and rock salt PbS occurs while preserving the anisotropic dimensions unique to the as-synthesized materials. Sequential exchange reactions between the three sulfide compositions are driven by the disparate solubilites of the metal ion exchange pair in specific coordinating molecules. Starting with CdS, highly anisotropic PbS nanorods are created, which serve as an important material for studying strong 2-dimensional quantum confinement, as well as for optoelectronic applications. Furthermore, interesting nanoheterostructures of CdS|PbS are obtained by precise control over ion insertion and removal.

  3. CO 2 adsorption in mono-, di- and trivalent cation-exchanged metal-organic frameworks: A molecular simulation study

    KAUST Repository

    Chen, Yifei

    2012-02-28

    A molecular simulation study is reported for CO 2 adsorption in rho zeolite-like metal-organic framework (rho-ZMOF) exchanged with a series of cations (Na +, K +, Rb +, Cs +, Mg 2+, Ca 2+, and Al 3+). The isosteric heat and Henry\\'s constant at infinite dilution increase monotonically with increasing charge-to-diameter ratio of cation (Cs + < Rb + < K + < Na + < Ca 2+ < Mg 2+ < Al 3+). At low pressures, cations act as preferential adsorption sites for CO 2 and the capacity follows the charge-to-diameter ratio. However, the free volume of framework becomes predominant with increasing pressure and Mg-rho-ZMOF appears to possess the highest saturation capacity. The equilibrium locations of cations are observed to shift slightly upon CO 2 adsorption. Furthermore, the adsorption selectivity of CO 2/H 2 mixture increases as Cs + < Rb + < K + < Na + < Ca 2+ < Mg 2+ ≈ Al 3+. At ambient conditions, the selectivity is in the range of 800-3000 and significantly higher than in other nanoporous materials. In the presence of 0.1% H 2O, the selectivity decreases drastically because of the competitive adsorption between H 2O and CO 2, and shows a similar value in all of the cation-exchanged rho-ZMOFs. This simulation study provides microscopic insight into the important role of cations in governing gas adsorption and separation, and suggests that the performance of ionic rho-ZMOF can be tailored by cations. © 2012 American Chemical Society.

  4. Formation of ZnSe/Bi2Se3 QDs by surface cation exchange and high photothermal conversion

    Directory of Open Access Journals (Sweden)

    Guozhi Jia

    2015-08-01

    Full Text Available Water-dispersed core/shell structure ZnSe/Bi2Se3 quantum dots were synthesized by ultrasonicwave-assisted cation exchange reaction. Only surface Zn ion can be replaced by Bi ion in ZnSe quantum dots, which lead to the ultrathin Bi2Se3 shell layer formed. It is significance to find to change the crystal of QDs due to the acting of ultrasonicwave. Cation exchange mechanism and excellent photothermal conversion properties are discussed in detail.

  5. The Cation Exchange Capacity of Fibrous Feedstuff and Its Nutritive Characteristics

    Institute of Scientific and Technical Information of China (English)

    XING Ting-xian

    2003-01-01

    Current researches on the nutritive characteristics of fibrous feedstuff through determining thefeedstuff cation exchange capacity (CEC) to evaluate its nutritive value at home and abroad were comprehen-sively discribed, and the methods of determining CEC value and the correlation between CEC value and chemi-cal compositions, pH value, and the effect of CEC value on the digestion kinetics in ruminants were also em-phatically introduced. The results of research showed that the CEC values of different feedstuff are different,closely correlated with nitrogen and acid detergent fibre (ADF) and lignin (LIG) content of the feedstuff. Atthe same time, there are markedly effect of CEC value in diet on the nutrients flow of digesta in the digestivetract of ruminants, the degradation rate and digestibility of nutrients in the rumen.

  6. Controlled methyl-esterification of pectin catalyzed by cation exchange resin.

    Science.gov (United States)

    Peng, Xiaoxia; Yang, Guang; Fan, Xingchen; Bai, Yeming; Ren, Xiaomeng; Zhou, Yifa

    2016-02-10

    This study developed a new method to methyl-esterify pectin using a cation exchange resin. Homogalacturonan (HG)-type pectin (WGPA-3-HG) and rhamnogalacturonan (RG)-I-type pectin (AHP-RG) obtained from the roots of Panax ginseng and sunflower heads, respectively, were used as models. Compared to commonly used methyl-esterification methods that use either methyl iodide or acidified methanol, the developed method can methyl-esterify both HG- and RG-I-type pectins without degrading their structures via β-elimination or acid hydrolysis. In addition, by modifying reaction conditions, including the mass ratio of resin to pectin, reaction time, and temperature, the degree of esterification can be controlled. Moreover, the resin and methanol can be recycled to conserve resources, lower costs, and reduce environmental pollution. This new methodology will be highly useful for industrial esterification of pectin.

  7. Behavior of human serum albumin on strong cation exchange resins: II. model analysis.

    Science.gov (United States)

    Voitl, Agnes; Butté, Alessandro; Morbidelli, Massimo

    2010-08-20

    Experiments with human serum albumin on a strong cation exchange resin exhibit a peculiar elution pattern: the protein elutes with two peaks in a modifier gradient. This behavior is modeled with a general rate model, where the two elution peaks are modeled with two binding conformations, one of which is at equilibrium conditions, while for the other, the adsorption process is rate limited. Isocratic experiments under nonadsorbing conditions were used to characterize the mass transfer process. The isotherm of both adsorption conformations as well as the kinetic of adsorption and desorption for the second conformation are functions of the modifier concentration. They are evaluated with linear modifier gradient experiments and step experiments with various adsorption times. All experimental features are well reproduced by the proposed modified general rate model.

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

    Directory of Open Access Journals (Sweden)

    Mariola J. Edelmann

    2011-01-01

    Full Text Available 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.

  9. Synthesis of high capacity cation exchangers from a low-grade Chinese natural zeolite.

    Science.gov (United States)

    Wang, Yifei; Lin, Feng

    2009-07-30

    The Chinese natural zeolite, in which clinoptilolite coexists with quartz was treated hydrothermally with NaOH solutions, either with or without fusion with NaOH powder as pretreatment. Zeolite Na-P, Na-Y and analcime were identified as the reacted products, depending on the reaction conditions such as NaOH concentration, reaction time and hydrothermal temperature. The products were identified by X-ray diffraction, and characterized by Fourier transform IR and ICP. With hydrothermal treatment after fusion of natural zeolite with NaOH, high purity of zeolite Na-Y and Na-P can be selectively formed, their cation exchange capacity (CEC) are 275 and 355 meq/100g respectively, which are greatly higher than that of the natural zeolite (97 meq/100g). Furthermore, the ammonium removal by the synthetic zeolite Na-P in aqueous solution was also studied. The equilibrium isotherms have been got and the influence of other cations present in water upon the ammonia uptake suggested an order of preference Ca(2+)>K(+)>Mg(2+).

  10. Synthesis of high capacity cation exchangers from a low-grade Chinese natural zeolite

    Energy Technology Data Exchange (ETDEWEB)

    Wang Yifei, E-mail: yifeiwang0206@yahoo.com.cn [College of Biology and Chemical Engineering, Jiaxing University, Jiaxing, Zhejiang 314001 (China); Department of Chemistry, XiXi Campus, Zhejiang University, Hangzhou, Zhejiang 310028 (China); Lin Feng [Department of Chemistry, XiXi Campus, Zhejiang University, Hangzhou, Zhejiang 310028 (China)

    2009-07-30

    The Chinese natural zeolite, in which clinoptilolite coexists with quartz was treated hydrothermally with NaOH solutions, either with or without fusion with NaOH powder as pretreatment. Zeolite Na-P, Na-Y and analcime were identified as the reacted products, depending on the reaction conditions such as NaOH concentration, reaction time and hydrothermal temperature. The products were identified by X-ray diffraction, and characterized by Fourier transform IR and ICP. With hydrothermal treatment after fusion of natural zeolite with NaOH, high purity of zeolite Na-Y and Na-P can be selectively formed, their cation exchange capacity (CEC) are 275 and 355 meq/100 g respectively, which are greatly higher than that of the natural zeolite (97 meq/100 g). Furthermore, the ammonium removal by the synthetic zeolite Na-P in aqueous solution was also studied. The equilibrium isotherms have been got and the influence of other cations present in water upon the ammonia uptake suggested an order of preference Ca{sup 2+} > K{sup +} > Mg{sup 2+}.

  11. Safety evaluation of cation-exchange resins. [For use in separating and processing radionuclides

    Energy Technology Data Exchange (ETDEWEB)

    Kalkwarf, D.R.

    1977-08-01

    Results are presented of a study to evaluate whether sufficient information is available to establish conservative limits for the safe use of cation-exchange resins in separating radionuclides and, if not, to recommend what new data should be acquired. The study was also an attempt to identify in-line analytical techniques for the evaluation of resin degradation during radionuclide processing. The report is based upon a review of the published literature and upon discussions with many people engaged in the use of these resins. It was concluded that the chief hazard in the use of cation-exchange resins for separating radionuclides is a thermal explosion if nitric acid or other strong oxidants are present in the process solution. Thermal explosions can be avoided by limiting process parameters so that the rates of heat and gas generation in the system do not exceed the rates for their transfer to the surroundings. Such parameters include temperature, oxidant concentration, the amounts of possible catalysts, the radiation dose absorbed by the resin and the diameter of the resin column. Current information is not sufficient to define safe upper limits for these parameters. They can be evaluated, however, from equations derived from the Frank-Kamenetskii theory of thermal explosions provided the heat capacities, thermal conductivities and rates of heat evolution in the relevant resin-oxidant mixtures are known. It is recommended that such measurements be made and the appropriate limits be evaluated. A list of additional safety precautions are also presented to aid in the application of these limits and to provide additional margins of safety. In-line evaluation of resin degradation to assess its safety hazard is considered impractical. Rather, it is recommended that the resin be removed from use before it has received the limiting radiation dose, evaluated as described above.

  12. Analysis of statistical thermodynamic model for binary protein adsorption equilibria on cation exchange adsorbent

    Institute of Scientific and Technical Information of China (English)

    ZHOU Xiaopeng; SU Xueli; SUN Yan

    2007-01-01

    A study of nonlinear competitive adsorption equilibria of proteins is of fundamental importance in understanding the behavior of preparative chromatographic separation.This work describes the nonlinear binary protein adsorption equilibria on ion exchangers by the statistical thermodynamic (ST) model.The single-component and binary protein adsorption isotherms of bovine hemoglobin (Hb) and bovine serum albumin(BSA)on SP Sepharose FF were determined by batch adsorption experiments in 0.05 mol/L sodium acetate buffer at three pH values(4.5,5.0 and 5.5)and three NaCl concentrations(0.05,0.10 and 0.15 mol/L)at pH 5.0.The ST model was found to depict the effects of pH and ionic strength on the single-component equilibria well,with model parameters depending on the pH and ionic strength.Moreover,the ST model gave acceptable fitting to the binary adsorption data with the fltted singlecomponent model parameters,leading to the estimation of the binary ST model parameter.The effects of pH and ionic strength on the model parameters are reasonably interpreted by the electrostatic and thermodynamic theories.Results demonstrate the availability of the ST model for describing nonlinear competitive protein adsorption equilibria in the presence of two proteins.

  13. A DFT-D study of the interaction of methane, carbon monoxide, and nitrogen with cation-exchanged SAPO-34

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, Michael [Bremen Univ. (Germany). Fachgebiet Kristallographie; University College London (United Kingdom). Dept. of Chemistry; Bell, Robert G. [University College London (United Kingdom). Dept. of Chemistry

    2015-07-01

    Density-functional theory calculations including a semi-empirical dispersion correction (DFT-D) are employed to study the interaction of small guest molecules (CH{sub 4}, CO, N{sub 2}) with the cation sites in the silicoaluminophosphate SAPO-34. Eight different cations from three different groups (alkali cations, alkaline earth cations, transition metals) are included in the study. For each case, the total interaction energy as well as the non-dispersive contribution to the interaction are analysed. Electron density difference plots are used to investigate the nature of this non-dispersive contribution in more detail. Despite a non-negligible contribution of polarisation interactions, the total interaction remains moderate in systems containing main group cations. In SAPOs exchanged with transition metals, orbital interactions between the cations and CO and N{sub 2} lead to a very strong interaction, which makes these systems attractive as adsorbents for the selective adsorption of these species. A critical comparison with experimental heats of adsorption shows reasonable quantitative agreement for CO and N{sub 2}, but a pronounced overestimation of the interaction strength for methane. While this does not affect the conclusions regarding the suitability of TM-exchanged SAPO-34 materials for gas separations, more elaborate computational approaches may be needed to improve the quantitative accuracy for this guest molecule.

  14. Surface modification of cation exchange membranes by graft polymerization of PAA-co-PANI/MWCNTs nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Nemati, Mahsa; Hosseini, Sayed Mohsen; Bagheripour, Ehsan [Faculty of Engineering, Arak University, Arak (Iran, Islamic Republic of); Madaeni, Sayed Siavash [Faculty of Engineering, Razi University, Kermanshah (Iran, Islamic Republic of)

    2016-03-15

    Surface modification of polyvinylchloride based heterogeneous cation exchange membrane was performed by graft polymerization of PAA and PAA-co-PANI/MWCNTs nanoparticles. The ion exchange membranes were prepared by solution casting technique. Spectra analysis confirmed graft polymerization clearly. SEM images illustrated that graft polymerization covers the membranes by simple gel network entanglement. The membrane water content was decreased by graft polymerization of PAA-co-PANI/MWCNTs nanoparticles on membrane surface. Membrane transport number and selectivity declined initially by PAA graft polymerization and then began to increase by utilizing of composite nanoparticles in modifier solution. The sodium and barium flux was improved sharply by PAA and PAAco- 0.01%wt PANI/MWCNTs graft polymerization on membrane surface and then decreased again by more increase of PANI/MWCNTs nanoparticles content ratio in modifier solution. The electrodialysis experiment results in laboratory scale showed higher dialytic rate in heavy metals removal for grafted-PAA and grafted-PAA-co-PANI/MWCNTs modified membrane compared to pristine one. Membrane areal electrical resistance was also decreased by introducing graft polymerization of PAA and PAA-co-PANI/MWCNTs NPs on membrane surface.

  15. Simultaneous isolation of lactoferrin and lactoperoxidase from bovine colostrum by SPEC 70 SLS cation exchange resin.

    Science.gov (United States)

    Liang, Yafei; Wang, Xuewan; Wu, Mianbin; Zhu, Wanping

    2011-09-01

    In this work, simultaneous isolation of lactoferrin (Lf) and lactoperoxidase (Lp) from defatted bovine colostrum by one-step cation exchange chromatography with SPEC 70 SLS ion-exchange resin was investigated. A RP-HPLC method for Lf and Lp determination was developed and optimized as the following conditions: detection wavelength of 220 nm, flow rate of 1 mL/min and acetonitrile concentration from 25% to 75% within 20 min. The adsorption process of Lf on SPEC 70 SLS resin was optimized using Lf standard as substrate. The maximum static binding capacity of SPEC 70 SLS resin was of 22.0 mg/g resin at 15 °C, pH 7.0 and adsorption time 3 h. The Lf adsorption process could be well described by the Langmuir adsorption isotherm model, with a maximum adsorption capacity of 21.73 mg/g resin at 15 °C. In batch fractionation of defatted colostrum, the binding capacities of SPEC 70 SLS resin for adsorbing Lf and Lp simultaneously under the abovementioned conditions were 7.60 and 6.89 mg/g resin, respectively, both of which were superior to those of CM Sepharose F.F. or SP Sepharose F.F. resins under the same conditions. As a result, SPEC 70 SLS resin was considered as a successful candidate for direct and economic purification of Lf and Lp from defatted colostrum.

  16. Simultaneous Isolation of Lactoferrin and Lactoperoxidase from Bovine Colostrum by SPEC 70 SLS Cation Exchange Resin

    Directory of Open Access Journals (Sweden)

    Mianbin Wu

    2011-09-01

    Full Text Available In this work, simultaneous isolation of lactoferrin (Lf and lactoperoxidase (Lp from defatted bovine colostrum by one-step cation exchange chromatography with SPEC 70 SLS ion-exchange resin was investigated. A RP-HPLC method for Lf and Lp determination was developed and optimized as the following conditions: detection wavelength of 220 nm, flow rate of 1 mL/min and acetonitrile concentration from 25% to 75% within 20 min. The adsorption process of Lf on SPEC 70 SLS resin was optimized using Lf standard as substrate. The maximum static binding capacity of SPEC 70 SLS resin was of 22.0 mg/g resin at 15 °С, pH 7.0 and adsorption time 3 h. The Lf adsorption process could be well described by the Langmuir adsorption isotherm model, with a maximum adsorption capacity of 21.73 mg/g resin at 15 °С. In batch fractionation of defatted colostrum, the binding capacities of SPEC 70 SLS resin for adsorbing Lf and Lp simultaneously under the abovementioned conditions were 7.60 and 6.89 mg/g resin, respectively, both of which were superior to those of CM Sepharose F.F. or SP Sepharose F.F. resins under the same conditions. As a result, SPEC 70 SLS resin was considered as a successful candidate for direct and economic purification of Lf and Lp from defatted colostrum.

  17. Ultrathin Sicopion Composite Cation-Exchange Membranes: Characteristics and Electrodialytic Performance following a Conditioning Procedure

    Directory of Open Access Journals (Sweden)

    Erik Ayala-Bribiesca

    2012-01-01

    Full Text Available The aim of this work was to investigate the properties of Sicopion membranes: an ultrathin (≈20 μm composite cation-exchange membrane (CEM made from sulphonated poly(ether-ether-ketone (SPEEK containing different levels of sulphonic-functionalized silica particles (SFSPs. Sicopion membranes were conditioned according to the French Normalization Association procedure, consisting in a series of acid and alkaline washes, and their electrodialytic characteristics were compared to an existent commercial food-grade membrane (CMX-SB. Electrical conductivity of Sicopion membranes was higher than that of CMX-SB membranes (9.92 versus 6.98 mS/cm, as well as their water content (34.0 versus 27.6%. As the SFSP level was reduced, the ion-exchange capacity (IEC of Sicopion membranes increased. Concerning their electrodialytic performances, Sicopion membranes presented a lower demineralization rate than CMX-SB membranes (35.9 versus 45.5%, due to an OH− leakage through the pores created by dislodging the SFSP particles during the conditioning procedure.

  18. Effects of Acetate on Cation Exchange Capacity of a Zn-Containing Montmorillonite : Physicochemical Significance and Metal Uptake

    NARCIS (Netherlands)

    Stathi, P.; Papadas, I. T.; Enotiadis, A.; Gengler, R. Y. N.; Gournis, D.; Rudolf, P.; Deligiannakis, Y.

    2009-01-01

    Fundamental properties such as cation exchange capacity (CEC), permanent charge, pH(PZC), and metal uptake of a Zn-containing montmorillonite are modified, in a predictable manner, by a mild chemical treatment using acetate. Acetate treatment allows a controllable increase of the CEC of montmorillon

  19. SYNTHESIS OF 1—(N—BENZYLOXYCARBONYLAMINO)ALKANEPHOSPHATES AND—PHOSPHINIC ACIDS CATALYZED BY A CATION EXCHANGE RESIN

    Institute of Scientific and Technical Information of China (English)

    ZHANGYuehua; HUANGWenqiang; 等

    1993-01-01

    An improved method is developed by using strongly acidic cation exchange resin(001×1,H+ form) as a catalyst for the synthesis of diphenyl 1-(N-benzyloxycarbonyl-amino) alkanephosphonates and 1-(N-benzyloxycarbonylamino) alkanephenyl phosphinic acids in high yields.

  20. Luminescent CuInS2 quantum dots by partial cation exchange in Cu2- xS nanocrystals

    NARCIS (Netherlands)

    Van Der Stam, Ward; Berends, Anne C.; Rabouw, Freddy T.; Willhammar, Tom; Ke, Xiaoxing; Meeldijk, Johannes D.; Bals, Sara; De Mello Donega, Celso

    2015-01-01

    Here, we show successful partial cation exchange reactions in Cu2-xS nanocrystals (NCs) yielding luminescent CuInS2 (CIS) NCs. Our approach of mild reaction conditions ensures slow Cu extraction rates, which results in a balance with the slow In incorporation rate. With this method, we obtain CIS NC

  1. Preparation and characterisation of monovalent ion selective cation exchange membranes based on sulphonated poly(ether ether ketone)

    NARCIS (Netherlands)

    Balster, J.; Krupenko, O.; Punt, I.G.M.; Stamatialis, D.; Wessling, M.

    2005-01-01

    This paper analyses the separation properties of various commercial cation exchange membranes (CEMs) and tailor made membranes based on sulphonated poly(ether ether ketone) and poly(ether sulphone) for binary electrolyte solutions containing protons and calcium ions. All membranes are thoroughly cha

  2. SYNTHESIS OF 2—HYDROXYETHYL ACRYLATE BY USING STRONG ACIDIC CATION ION EXCHANGE RESIN AS CATALYST

    Institute of Scientific and Technical Information of China (English)

    GAODabin

    1992-01-01

    2-Hydroxyethyl acrylate is synthesized from acrylic acid and ethylene glycol under a simple and mild condition by using strong acidic cation ion exchange resin as a catalyst,which could be recycled as long as 10 times with high activation.

  3. Industrial scale chromatographic separation of valuable compounds from biomass hydrolysates and side streams

    Energy Technology Data Exchange (ETDEWEB)

    Saari, P.

    2011-06-15

    Carbohydrates are composed of a number of various monosaccharides, glucose being the most abundant. Some of the monosaccharides are valuable compounds used in the food and pharmaceutical industries. They can be separated from biomass hydrolysates e.g. by chromatographic methods. In this thesis, chromatographic separation of valuable compounds using ion exchange resins was studied on an industrial scale. Of special interest were rare monosaccharides in biomass hydrolysates. A novel chromatographic separation process was developed for fucose, starting from pre-processed spent sulfite liquor. The core of the process consists of three chromatographic separations with different types of ion exchange resins. Chromatographic separation of galactose was tested with three biomass hydrolysates; lactose, gum arabic and hemicellulose hydrolysates. It was demonstrated that also galactose can be separated from complex carbohydrate mixtures. A recovery process for arabinose from citrus pectin liquid residual and for mannose from wood pulp hydrolysate were also developed and experimentally verified. In addition to monosaccharides, chromatographic separation of glycinebetaine from vinasse was examined with a hydrogen form weak acid cation exchange resin. The separation involves untypical peak formation depending, for example, on the pH and the cation composition. The retention mechanism was found to be hydrogen bonding between glycinebetaine and the resin. In the experimental part, all four resin types - strong acid cation, strong base anion, weak acid cation and weak base anion exchange resins - were used. In addition, adsorption equilibria data of seven monosaccharides and sucrose were measured with the resins in sodium and sulfate forms because such data have been lacking. It was found out that the isotherms of all sugars were linear under industrial conditions. A systematic method for conceptual process design and sequencing of chromatographic separation steps were developed

  4. Influence of Sulfonated-Kaolin On Cationic Exchange Capacity Swelling Degree and Morphology of Chitosan/Kaolin Composites

    Directory of Open Access Journals (Sweden)

    Ozi Adi Saputra

    2016-06-01

    Full Text Available Preparation of sulfonated-kaolin (sKao has been conducted and used as filler on chitosan matrix via solution casting method, namely chitosan/sKao (Cs/sKao. Swelling degree, cationic exchange capacity and thermal stability were evaluated to determine chitosan/sKao membranes performance as proton exchange membrane in fuel cell. Functional group analysis of chitosan, sKao and synthesized products were studied using Fourier Transform Infra-Red (FTIR spectroscopy. In this study, swelling degree and swelling area of Cs/sKao are also studied to determine of membrane ability to swelling which compare to unmodified chitosan/kaolin (Cs/Kao. The presence of sKao in chitosan matrix was able to improve cationic exchange capacity (CEC which proved by morphological study of membrane surface after CEC test. Moreover, Thermal stability of Cs/sKao showed the membrane has meet requirement for PEM application.

  5. A study on equilibrium and kinetics of ion exchange of alkaline earth metals using an inorganic cation exchanger - zirconium titanium phosphate

    Indian Academy of Sciences (India)

    Amin Jignasa; Thakkar Rakesh; Chudasama Uma

    2006-03-01

    An advanced inorganic cation exchange material of the class of tetravalent metal acid (TMA) salt, zirconium titanium phosphate (ZTP), has been synthesized by a modified sol-gel technique. ZTP has been characterized by elemental analysis (ICP-AES), thermal analysis (TGA), FTIR and X-ray diffraction studies. The Nernst-Planck equation has been used to study the forward and reverse ion exchange kinetics of Mg (II), Ca (II), Sr (II) and Ba (II) with H (I) at four different temperatures. The mechanism of exchange is particle diffusion, as confirmed by the linear (dimensionless time parameter) vs (time) plots. The exchange process is thus controlled by the diffusion within the exchanger particles for the systems studied herein. Further, various kinetic parameters like self-diffusion coefficient (0), energy of activation () and entropy of activation (*) have been evaluated under conditions favouring a particle diffusion-controlled mechanism.

  6. On the Structure-Property Relationships of Cation-Exchanged ZK-5 Zeolites for CO2 Adsorption.

    Science.gov (United States)

    Pham, Trong D; Hudson, Matthew R; Brown, Craig M; Lobo, Raul F

    2017-03-09

    The CO2 adsorption properties of cation-exchanged Li-, Na-, K-, and Mg-ZK-5 zeolites were correlated to the molecular structures determined by Rietveld refinements of synchrotron powder X-ray diffraction patterns. Li-, K-, and Na-ZK-5 all exhibited high isosteric heats of adsorption (Qst ) at low CO2 coverage, with Na-ZK-5 having the highest Qst (ca. 49 kJ mol(-1) ). Mg(2+) was located at the center of the zeolite hexagonal prism with the cation inaccessible to CO2 , leading to a much lower Qst (ca. 30 kJ mol(-1) ) and lower overall uptake capacity. Multiple CO2 adsorption sites were identified at a given CO2 loading amount for all four cation-exchanged ZK-5 adsorbents. Site A at the flat eight-membered ring windows and site B/B* in the γ-cages were the primary adsorption sites in Li- and Na-ZK-5 zeolites. Relatively strong dual-cation adsorption sites contributed significantly to an enhanced electrostatic interaction for CO2 in all ZK-5 samples. This interaction gives rise to a migration of Li(+) and Mg(2+) cations from their original locations at the center of the hexagonal prisms toward the α-cages, in which they interact more strongly with the adsorbed CO2 .

  7. Analyzing freely dissolved concentrations of cationic surfactant utilizing ion-exchange capability of polyacrylate coated solid-phase microextraction fibers.

    Science.gov (United States)

    Chen, Yi; Droge, Steven T J; Hermens, Joop L M

    2012-08-24

    A 7-μm polyacrylate (PA) coated fiber was successfully employed to determine freely dissolved concentrations of cationic surfactants by solid-phase microextraction (SPME) and utilizing the capability of the PA-coating to sorb organic cations via ion-exchange at carboxylic groups. Measured fiber-water partitioning coefficients (K(fw)) were constant below a fiber loading of 2mmol per liter polyacrylate, allowing for simple and accurate analysis in a concentration range that is relevant from a risk assessment point of view. Ion-exchange was confirmed to be the main sorption mechanism because of a decreasing K(fw) with either higher CaCl(2) concentrations or lower pH, and maximum fiber uptake at the polyacrylate cation-exchange capacity (CEC, at 30mmol/L PA). Fiber-water sorption isotherms were established in various aqueous media in toxicological relevant concentrations. The developed SPME method has a high potential for application in ecotoxicological studies, as demonstrated in sorption studies with humic acid in different electrolyte solutions at aqueous concentrations down to the sub nM range. Cationic surfactant sorption affinities for humic acid also depend on medium composition but are orders of magnitude higher than to the PA fiber on a sorbent weight basis.

  8. 1H and 23Na MAS NMR spectroscopy of cationic species in CO2 selective alkaline earth metal porous silicoaluminophosphates prepared via liquid and solid state ion exchange

    Science.gov (United States)

    Arévalo-Hidalgo, Ana G.; Dugar, Sneha; Fu, Riqiang; Hernández-Maldonado, Arturo J.

    2012-07-01

    The location of extraframework cations in Sr2+ and Ba2+ ion-exchanged SAPO-34 was estimated by means of 1H and 23Na MAS NMR spectroscopy and spectral deconvolution. Incorporation of the alkaline earth metal cations onto the SAPO framework was achieved via liquid state ion exchange, coupled partial detemplation/solid-state ion exchange, and combination of both techniques. MAS NMR revealed that the level of ion exchange was limited by the presence of protons and sodium cations near hexagonal prisms (site SI), which are relatively difficult to exchange with the alkaline earth metal due to steric and charge repulsion criteria. In addition, the presence of ammonium cations in the supercages facilitated the exchange of otherwise tenacious hydrogen as corroborated by unit cell compositional data as well as enhanced CO2 adsorption at low partial pressures. The extraframework ammonium species were produced from partial detemplation of the structure-directing agent employed for the SAPO-34 synthesis, tetraethylammonium.

  9. Alkali recovery using PVA/SiO2 cation exchange membranes with different -COOH contents.

    Science.gov (United States)

    Hao, Jianwen; Gong, Ming; Wu, Yonghui; Wu, Cuiming; Luo, Jingyi; Xu, Tongwen

    2013-01-15

    By changing -COOH content in poly(acrylic acid-co-methacryloxypropyl trimethoxy silane (poly(AA-co-γ-MPS)), a series of PVA/SiO(2) cation exchange membranes are prepared from sol-gel process of poly(AA-co-γ-MPS) in presence of poly(vinyl alcohol) (PVA). The membranes have the initial decomposition temperature (IDT) values of 236-274 °C. The tensile strength (TS) ranges from 17.4 MPa to 44.4 MPa. The dimensional stability in length (DS-length) is in the range of 10%-25%, and the DS-area is in the range of 21%-56% in 65 °C water. The water content (W(R)) ranges from 61.2% to 81.7%, the ion exchange capacity (IEC) ranges from 1.69 mmol/g to 1.90 mmol/g. Effects of -COOH content on diffusion dialysis (DD) performance also are investigated for their potential applications. The membranes are tested for recovering NaOH from the mixture of NaOH/Na(2)WO(4) at 25 - 45 °C. The dialysis coefficients of NaOH (U(OH)) are in the range of 0.006-0.032 m/h, which are higher than those of the previous membranes (U(OH): 0.0015 m/h, at 25 °C). The selectivity (S) can reach up to 36.2. The DD performances have been correlated with the membrane structure, especially the continuous arrangement of -COOH in poly(AA-co-γ-MPS) chain.

  10. Cationic Polymerization of 1,2-Epoxypropane by an Acid Exchanged Montmorillonite Clay in the Presence of Ethylene Glycol

    Directory of Open Access Journals (Sweden)

    Aïcha Hachemaoui

    2003-10-01

    Full Text Available Abstract: The polymerization of propylene oxide (PO catalysed by maghnite-H+ (mag-H+ in the presence of ethylene glycol was investigated. Mag-H+ is a montmorillonite silicate sheet clay was prepared through a straight forward proton exchange process. It was found that the cationic polymerization of PO was initiated by mag-H+ at 20 °C both in bulk and in solution. The effect of the amount of mag-H+ and solvent was studied. These results indicated the cationic nature of the polymerization A possible initiation pathway, via the transfer of protons from mag-H+ to the monomer, is proposed.

  11. Influence of competing inorganic cations on the ion exchange equilibrium of the monovalent organic cation metoprolol on natural sediment.

    Science.gov (United States)

    Niedbala, Anne; Schaffer, Mario; Licha, Tobias; Nödler, Karsten; Börnick, Hilmar; Ruppert, Hans; Worch, Eckhard

    2013-02-01

    The aim of this study was to systematically investigate the influence of the mono- and divalent inorganic ions Na(+) and Ca(2+) on the sorption behavior of the monovalent organic cation metoprolol on a natural sandy sediment at pH=7. Isotherms for the beta-blocker metoprolol were obtained by sediment-water batch tests over a wide concentration range (1-100000 μg L(-1)). Concentrations of the competing inorganic ions were varied within freshwater relevant ranges. Data fitted well with the Freundlich sorption model and resulted in very similar Freundlich exponents (n=0.9), indicating slightly non-linear behavior. Results show that the influence of Ca(2+) compared to Na(+) is more pronounced. A logarithmic correlation between the Freundlich coefficient K(Fr) and the concentration or activity of the competing inorganic ions was found allowing the prediction of metoprolol sorption on the investigated sediment at different electrolyte concentrations. Additionally, the organic carbon of the sediment was completely removed for investigating the influence of organic matter on the sorption of metoprolol. The comparison between the experiments with and without organic carbon removal revealed no significant contribution of the organic carbon fraction (0.1%) to the sorption of metoprolol on the in this study investigated sediment. Results of this study will contribute to the development of predictive models for the transport of organic cations in the subsurface.

  12. Adsorption behavior and mechanism of cadmium on strong-acid cation exchange resin

    Institute of Scientific and Technical Information of China (English)

    WANG Fei; WANG Lian-jun; LI Jian-sheng; SUN Xiu-yun; HAN Wei-qing

    2009-01-01

    The adsorption behavior of Cd2+ on 001×7 strong-acid cation exchange resin was studied with the static adsorption method. The adsorption process was analyzed from thermodynamics and kinetics aspects. The influences of experimental parameters such as pH, temperature, initial concentration and adsorption rate were investigated. The experimental results show that in the studied concentration range, 001×7 resin has a good sorption ability for Cd2+, and the equilibrium adsorption data fit to Freundlich isotherms. The adsorption is an exothermic process which runs spontaneously. Kinetic analysis shows that the adsorption rate is mainly governed by liquid film diffusion. The best adsorption condition is pH 4-5. The saturated resin can be regenerated by 3 mol/L nitric acid, and the desorption efficiency is over 98%. The maximal static saturated adsorption capacity is 355 mg/g (wet resin) at 293 K. The adsorption mechanism of Cd2+ on 001×7 resin was discussed based on IR spectra.

  13. Use of Cation Exchange Membrane in Soil Potassium Release and Wheat Response to Potassium

    Institute of Scientific and Technical Information of China (English)

    LIGUI-BAO; J.J.SCHOENAU; 等

    1995-01-01

    A pot experiment was conducted in the growth chamber on Saskatchewan soils with different texture to determine the K release status and wheat K demand.The relationship between K uptake and soil available K extracted by cation exchange membrane(CEM-K) and the effcet of K fertilizer on wheat growth and soil available K was also evaluated.Treatments of 0,60 and 120mg K/kg were applied to sandy,low and high K loamy and clay soils,The highest yields were acieved with the application of 120mg K/kg in sandy soil and 60 mg K/kg in other soils.On the whole,the clay soil contributed K more than other soils from slowly available fraction.Regression revealed a linear relationship between the soil available K extracted by NH4OAc(Ka) and CEM-K in suspensions(r=0.93).Results also showed that CEM-K in burial and in suspensions were different not only in the amount but also in correlation with Ka or K uptake.

  14. Strong cation exchange resin for improving physicochemical properties and sustaining release of ranitidine hydrochloride

    Directory of Open Access Journals (Sweden)

    Khan S

    2007-01-01

    Full Text Available In the present study strong cation exchange resin (Amberlite IRP69 was used to improve the physicochemical properties of ranitidine hydrochloride such as taste and bulk properties and to sustain dissolution rate. Drug-resin complexes were prepared using batch method. Drug loading was done under different processing conditions such as temperature, pH, drug-resin ratio, and drug concentration to get the optimum condition for resinate preparation. Resinate prepared under optimized condition was tested for taste, bulk properties and release rate. Degree of bitterness of ranitidine was found to reduce to zero after complexation with resin. Improvement in flow properties was also observed. Angle of repose for resinate was found to be 33.21 o as compared to 42.27 o for ranitidine HCl. Effect of dissolution medium and particle size on in vitro release of drug from resinate was also investigated. Resinate with drug to resin ratio of 2:3 and particle size> 90 µm showed about 90% of drug release within 12 h. The orodispersible tablet formulated from the resinate containing 10% croscarmellose sodium disintegrated within 35 sec in oral cavity and showed similar dissolution profile as the resinate. Tablets were found stable after stability studies with no change in dissolution profile.

  15. Assessing Soil Available Potassium by Cation Exchange Membrane and COnventional Chemical Extractions

    Institute of Scientific and Technical Information of China (English)

    LIUZHAOHUI; J.SCHOENAU; 等

    1999-01-01

    Four testing methods using cation exchange membrane (CEM),ammonium acetate,ASI(0.25mol L-1 NaHCO3+0.01mol L-1 EDTA +0.01 molL-1 NH4F) and 1.0molL-1 boiling nitric acid,respectively,were used to evaluate soil available K.The soil K tested by CEM was significantly correlated with that by the other (conventional)methods(r2=0.43**-0.95***).The soil K tested by CEM saturated with NH4HCO3(15min extraction)was most closely correlated with that by the other methods(r2=0.60**-0.95***),Potassium availability,as predicted by soil test,was comparable to actual K uptake by canola and wheat grown on the soils in growth chamber.Regression analyses showed that plant K uptake was more closely correlated wiht K extracted by CEM(r2=0.56**-0.81***)than that by the conventional methods(r2=0.46***-0.81***),most colsely correlated with that by NH4HCO3-saturated CEM for 15 min (r2=0.81***).and worst correlated with that by HNO3(r2=0.45**-0.72***)

  16. Mineral carbonation of gaseous carbon dioxide using a clay-hosted cation exchange reaction.

    Science.gov (United States)

    Kang, Il-Mo; Roh, Ki-Min

    2013-01-01

    The mineral carbonation method is still a challenge in practical application owing to: (1) slow reaction kinetics, (2) high reaction temperature, and (3) continuous mineral consumption. These constraints stem from the mode of supplying alkaline earth metals through mineral acidification and dissolution. Here, we attempt to mineralize gaseous carbon dioxide into calcium carbonate, using a cation exchange reaction of vermiculite (a species of expandable clay minerals). The mineralization is operated by draining NaCI solution through vermiculite powders and continuously dropping into the pool of NaOH solution with CO2 gas injected. The mineralization temperature is regulated here at 293 and 333 K for 15 min. As a result of characterization, using an X-ray powder diffractometer and a scanning electron microscopy, two types of pure CaCO3 polymorphs (vaterite and calcite) are identified as main reaction products. Their abundance and morphology are heavily dependent on the mineralization temperature. Noticeably, spindle-shaped vaterite, which is quite different from a typical vaterite morphology (polycrystalline spherulite), forms predominantly at 333 K (approximately 98 wt%).

  17. Cation- and anion-exchanges induce multiple distinct rearrangements within metallosupramolecular architectures.

    Science.gov (United States)

    Riddell, Imogen A; Ronson, Tanya K; Clegg, Jack K; Wood, Christopher S; Bilbeisi, Rana A; Nitschke, Jonathan R

    2014-07-01

    Different anionic templates act to give rise to four distinct Cd(II)-based architectures: a Cd2L3 helicate, a Cd8L12 distorted cuboid, a Cd10L15 pentagonal prism, and a Cd12L18 hexagonal prism, which respond to both anionic and cationic components. Interconversions between architectures are driven by the addition of anions that bind more strongly within a given product framework. The addition of Fe(II) prompted metal exchange and transformation to a Fe4L6 tetrahedron or a Fe10L15 pentagonal prism, depending on the anionic templates present. The equilibrium between the Cd12L18 prism and the Cd2L3 triple helicate displayed concentration dependence, with higher concentrations favoring the prism. The Cd12L18 structure serves as an intermediate en route to a hexafluoroarsenate-templated Cd10L15 complex, whereby the structural features of the hexagonal prism preorganize the system to form the structurally related pentagonal prism. In addition to the interconversion pathways investigated, we also report the single-crystal X-ray structure of bifluoride encapsulated within a Cd10L15 complex and report solution state data for J-coupling through a CH···F(-) hydrogen bond indicating the strength of these interactions in solution.

  18. Isolation of lactoperoxidase using different cation exchange resins by batch and column procedures.

    Science.gov (United States)

    Fweja, Leonard Wt; Lewis, Michael J; Grandison, Alistair S

    2010-08-01

    Lactoperoxidase (LP) was isolated from whey protein by cation-exchange using Carboxymethyl resin (CM-25C) and Sulphopropyl Toyopearl resin (SP-650C). Both batch and column procedures were employed and the adsorption capacities and extraction efficiencies were compared. The resin bed volume to whey volume ratios were 0.96:1.0 for CM-25C and 0.64:1.0 for SP-650 indicating higher adsorption capacity of SP-650 compared with CM-25C. The effluent LP activity depended on both the enzyme activity in the whey and the amount of whey loaded on the column within the saturation limits of the resin. The percentage recovery was high below the saturation point and fell off rapidly with over-saturation. While effective recovery was achieved with column extraction procedures, the recovery was poor in batch procedures. The whey-resin contact time had little impact on the enzyme adsorption. SDS PAGE and HPLC analyses were also carried out, the purity was examined and the proteins characterised in terms of molecular weights. Reversed phase HPLC provided clear distinction of the LP and lactoferrin (LF) peaks. The enzyme purity was higher in column effluents compared with batch effluents, judged on the basis of the clarity of the gel bands and the resolved peaks in HPLC chromatograms.

  19. Oxidative decomposition properties of cationic exchange resins producing SO4(2-) in power plants.

    Science.gov (United States)

    Zhu, Zhiping; Dai, Chenlin; Liu, Sen; Tian, Ye

    2015-01-01

    The sulphate content of a system increases when strong-acid cationic exchange resins leak into a system or when sulphonic acid groups on the resin organic chain detach. To solve this problem, a dynamic cycle method was used in dissolution experiments of several resins under H2O2 or residual chlorine conditions. Results show that after performing dynamic cycle experiments for 120 hours under oxidizing environments, the SO4(2-) and total organic carbon (TOC) released by four kinds of resins increased with time, contrary to their release velocity. The quantity of released SO4(2-) increased as the oxidizing ability of oxidants was enhanced. Results showed that the quantity and velocity of released SO4(2-) under residual chlorine condition were larger than those under H2O2 condition. Data analysis of SO4(2-) and TOC released from the four kinds of resins by the dynamic cycle experiment revealed that the strength of oxidation resistance of the four resins were as follows: 650C>1500H>S200>SP112H.

  20. Ionic polymer-metal composite actuators obtained from radiation-grafted cation- and anion-exchange membranes.

    Science.gov (United States)

    Park, Jong Hyuk; Han, Man Jae; Song, Dae Seock; Jho, Jae Young

    2014-12-24

    Two series of ionic polymer-metal composites (IPMCs), one cationic and one anionic, are designed and prepared from radiation-grafted ion-exchange membranes. Through examination of the properties of the membranes synthesized from the two grafting monomers and the two base polymers, acrylic acid-grafted poly(vinylidene fluoride-co-hexafluoropropylene) and quarternized 4-vinylpyridine-grafted poly(ethylene-co-tetrafluoroethylene) with the appropriate amount of ionic groups are employed for the fabrication of cation and anion IPMCs, respectively. The bending displacement of the cation IPMC is comparable to Nafion-based IPMC under direct- and alternating-current voltage, but back-relaxation is not observed. The actuation performance of the anion IPMC is highly improved over those reported earlier in the literature for the other anion IPMCs.

  1. Separation of matrine and oxymatrine from Sophora flavescens extract through cation exchange resin coupled with macroporous absorption resin

    Directory of Open Access Journals (Sweden)

    Chen Haohao

    2016-06-01

    Full Text Available A simple method for separation of matrine and oxymatrine from Sophora flavescens was developed with cation exchange resin coupled with macroporous resin. Based on the adsorption characteristics of matrine and oxymatrine, 001×732 cation exchange resin was used to absorb target alkaloids for removing most of the foreign matter, while BS-65 macroporous resin was chosen to purify these alkaloids. The result showed that the equilibrium adsorption data of matrine and oxymatrine on 001×732 resin and BS-65 resin at 30°C was fitted to Langmuir isotherm and Freundlich isotherm, respectively. The contents of matrine and oxymatrine were increased from 0.73% and 2.2% in the crude extract of the root of Sophora flavescens to 67.2% and 66.8% in the final eluent products with the recoveries of 90.3% and 86.9%, respectively.

  2. Improved high performance liquid chromatographic separation of anthocyanin compounds from grapes using a novel mixed-mode ion-exchange reversed-phase column.

    Science.gov (United States)

    McCallum, Jason L; Yang, Raymond; Young, J Christopher; Strommer, Judith N; Tsao, Rong

    2007-04-27

    A novel mixed mode HPLC method using a column combining both ion-exchange and reversed-phase separation mechanisms has been developed to facilitate analysis of anthocyanins in grapes. Chromatographic performance and subsequent analysis of anthocyanidin diglucosides and acylated compounds are significantly improved using the new column, compared to those associated with conventional C18 reversed-phase methods. The mixed mode column produces a distinctive eluting pattern for the different anthocyanin subgroups, avoiding overlaps found with C18 columns. The enhanced chromatographic resolution provides nearly complete separation of 37 anthocyanin types, and permits detection of delphinidin 3-O-(6''-O-caffeoyl) beta-D-glucoside for the first time in extracts of skins from Concord grapes.

  3. The load and release characteristics on a strong cationic ion-exchange fiber: kinetics, thermodynamics, and influences.

    Science.gov (United States)

    Yuan, Jing; Gao, Yanan; Wang, Xinyu; Liu, Hongzhuo; Che, Xin; Xu, Lu; Yang, Yang; Wang, Qifang; Wang, Yan; Li, Sanming

    2014-01-01

    Ion-exchange fibers were different from conventional ion-exchange resins in their non-cross-linked structure. The exchange was located on the surface of the framework, and the transport resistance reduced significantly, which might mean that the exchange is controlled by an ionic reaction instead of diffusion. Therefore, this work aimed to investigate the load and release characteristics of five model drugs with the strong cationic ion-exchange fiber ZB-1. Drugs were loaded using a batch process and released in United States Pharmacopoeia (USP) dissolution apparatus 2. Opposing exchange kinetics, suitable for the special structure of the fiber, were developed for describing the exchange process with the help of thermodynamics, which illustrated that the load was controlled by an ionic reaction. The molecular weight was the most important factor to influence the drug load and release rate. Strong alkalinity and rings in the molecular structures made the affinity between the drug and fiber strong, while logP did not cause any profound differences. The drug-fiber complexes exhibited sustained release. Different kinds and concentrations of counter ions or different amounts of drug-fiber complexes in the release medium affected the release behavior, while the pH value was independent of it. The groundwork for in-depth exploration and further application of ion-exchange fibers has been laid.

  4. Superparamagnetic cation-exchange adsorbents for bioproduct recovery from crude process liquors by high-gradient magnetic fishing

    DEFF Research Database (Denmark)

    Heebøll-Nielsen, Anders; Justesen, S.F.L; Hobley, Timothy John;

    2004-01-01

    Different routes were screened for the preparation of superparamagnetic cation-exchange adsorbents for the capture of proteins using high-gradient magnetic fishing. Starting from a polyglutaraldehyde-coated base particle, the most successful of these involved attachment of sulphite to oligomers...... from sweet bovine whey. Subsequently, a high-gradient magnetic fishing process was constructed for the fractionation of whey, in which lactoperoxidase was purified 36-fold and concentrated 4.7-fold...

  5. FACTORS AFFECT THE RELEASE OF PSEUDOEPHDRINE HYDROCHLORIDE FROM THE UNCOATED CATION EXCHANGE RESIN-BASED DRUG DELIVERY SYSTEM IN VITRO

    Institute of Scientific and Technical Information of China (English)

    LI Zhenhua; PI Hongqiong; HE Binglin

    2001-01-01

    In this paper, it was investigated that the effect of parameters such as the ionic strength,pH, counter-ion type of release medium, particle size, and cross linkage of cation exchange resin on the release of model drug pseudoephedrine hydrochloride (PE) from uncoated drug-resin complex.The drug-resin complex was prepared by the reaction of PE with strongly acidic cation exchange resin (001 ×4, 001 ×7, 001 ×14). The result showed that the loading of PE increased with the increase of temperatures. The release of PE from drug-resin complex at 37 ℃ was monitored in vitro.From the experiments, it was found that the release rate of PE depends on the pH, composition of the releasing media, increased at lower pH media or with increase of ionic strength of media. Moreover,the release rate of PE was inversely proportional to the cross-linkage and particle size of the cation exchange resin.

  6. A weak cation-exchange monolith as stationary phase for the separation of peptide diastereomers by CEC.

    Science.gov (United States)

    Ludewig, Ronny; Nietzsche, Sandor; Scriba, Gerhard K E

    2011-01-01

    A CEC weak cation-exchange monolith has been prepared by in situ polymerization of acrylamide, methylenebisacrylamide and 4-acrylamidobutyric acid in a decanol-dimethylsulfoxide mixture as porogen. The columns were evaluated by SEM and characterized with regard to the separation of diastereomers and α/β-isomers of aspartyl peptides. Column preparation was reproducible as evidenced by comparison of the analyte retention times of several columns prepared simultaneously. Analyte separation was achieved using mobile phases consisting of acidic phosphate buffer and ACN. Under these conditions the peptides migrated due to their electrophoretic mobility but the EOF also contributed as driving force as a function of the pH of the mobile phase due to increasing dissociation of the carboxyl groups of the polymer. Raising the pH of the mobile phase also resulted in deprotonation of the peptides reducing analyte mobility. Due to these mechanisms each pair of diastereomeric peptides displayed the highest resolution at a different pH of the buffer component of the mobile phase. Comparing the weak-cation exchange monolith to an RP monolith and a strong cation-exchange monolith different elution order of some peptide diastereomers was observed, clearly illustrating that interactions with the stationary phase contribute to the CEC separations.

  7. FACTORS AFFECT THE RELEASE OF PSEUDOEPHDRINE HYDROCHLORIDE FROM THE UNCOATED CATION EXCHANGE RESIN—BASED DRUG DELIVERY SYSTEM IN VITRO

    Institute of Scientific and Technical Information of China (English)

    LIZhenhua; PIHongqiong; 等

    2001-01-01

    In this paper,it was investigated that the effect of parameters such as the ionic strength,pH.counter-ion type of release medium,particle size.and cross linkage of cation exchange resin on the release of model drug pseudoephedrine hydrochloride(PE) from uncoated drug-resin complex.The drug-resin complex was pepared by the reaction of PE with strongly acidic cation exchange resin(001×4,001×7,001×14) .The result showed that the loading of PE increased with the increase of temperatures.The release of PE from drug-resin complex at 37℃ was monitored in vitro.From the experiments,it was found that the release rate of PE depends on the pH.comosition of the releasing media,increased at lower pH media or with increase of ionic strength of media.Moreover,the release rate of PE was inversely proportional to the cross-linkage and particle size of the cation exchange resin.

  8. Sorption of chlorimuron-ethyl on montmorillonite clays: effects of exchangeable cations, pH, and ionic strength.

    Science.gov (United States)

    Ren, Wenjie; Teng, Ying; Zhou, Qixing; Paschke, Albrecht; Schüürmann, Gerrit

    2014-10-01

    Sorption interaction of chlorimuron-ethyl with montmorillonite clays was investigated under varied types of exchangeable cation, pH, and ionic strength conditions. Chlorimuron-ethyl sorption on bentonites exhibited pronounced cation dependency, and the sorption ability increased as the sequence Ca(2+)- clay type and much weaker for montmorillonites. The decrease of pH at the range of 4.0-6.0 prominently increased sorption of chlorimuron-ethyl on all cation-exchanged montmorillonite clays, and nearly a neglected sorption (about 2 %) can be observed at pH over 7.0. In the presence of CaCl2, sorption of chlorimuron-ethyl on Fe(3+)-bentonite was promoted because of complexion of Ca(2+) and the surface of Fe(3+)-bentonite. However, as the concentration of CaCl2 increased, chlorimuron-ethyl sorption on Ca(2+)- and Fe(3+)-exchanged bentonite decreased, suggesting that Ca bridging was not the prevailing mechanism for sorption of chlorimuron-ethyl on these clays. Furthermore, chlorimuron-ethyl sorption was relatively sensitive to pH, and the change of pH may obscure effect of other factors on the sorption, so it was quite necessary to control pH at a constant value when the effect of other factor was being studied.

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

    Science.gov (United States)

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

    2013-03-01

    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 complexity is prefractionation by use of strong cation exchange chromatography. Here, we have compared SCX-LC-MS/MS with LC-FAIMS-MS/MS for the identification of peptides and proteins from whole cell lysates from the breast carcinoma SUM52 cell line. Two FAIMS approaches are considered: (1) multiple compensation voltages within a single LC-MS/MS analysis (internal stepping) and (2) repeat LC-MS/MS analyses at different and fixed compensation voltages (external stepping). We also consider the consequence of the fragmentation method (electron transfer dissociation or collision-induced dissociation) on the workflow performance. The external stepping approach resulted in a greater number of protein and peptide identifications than the internal stepping approach for both ETD and CID MS/MS, suggesting that this should be the method of choice for FAIMS proteomics experiments. The overlap in protein identifications from the SCX method and the external FAIMS method was ~25 % for both ETD and CID, and for peptides was less than 20 %. The lack of overlap between FAIMS and SCX highlights the complementarity of the two techniques. Charge state analysis of the peptide assignments showed that the FAIMS approach identified a much greater proportion of triply-charged ions.

  10. Spatial Variability of Soil Cation Exchange Capacity in Hilly Tea Plantation Soils Under Different Sampling Scales

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Studies on the spatial variability of the soil cation exchange capacity (CEC) were made to provide a theoretical basis for an ecological tea plantation and management of soil fertilizer in the tea plantation. Geostatistics were used to analyze the spatial variability of soil CEC in the tea plantation site on Mengding Mountain in Sichuan Province of China on two sampling scales. It was found that, (1) on the small scale, the soil CEC was intensively spatially correlative, the rate of nugget to sill was 18.84% and the spatially dependent range was 1 818 m, and structural factors were the main factors that affected the spatial variability of the soil CEC; (2) on the microscale, the soil CEC was also consumingly spatially dependent,and the rate of nugget to sill was 16.52%, the spatially dependent range was 311 m, and the main factors affecting the spatial variability were just the same as mentioned earlier. On the small scale, soil CEC had a stronger anisotropic structure on the slope aspect, and a weaker one on the lateral side. According to the ordinary Kriging method, the equivalence of soil CEC distributed along the lateral aspect of the slope from northeast to outhwest, and the soil CEC reduced as the elevation went down. On the microscale, the anisotropic structure was different from that measured on the small scale. It had a stronger anisotropic structure on the aspect that was near the aspect of the slope, and a weaker one near the lateral aspect of the slope. The soil CEC distributed along the lateral aspect of the slope and some distributed in the form of plots.From the top to the bottom of the slope, the soil CEC increased initially, and then reduced, and finally increased.

  11. Cation Exchange Resins and colonic perforation. What surgeons need to know

    Science.gov (United States)

    Rodríguez-Luna, María Rita; Fernández-Rivera, Enrique; Guarneros-Zárate, Joaquín E.; Tueme-Izaguirre, Jorge; Hernández-Méndez, José Roberto

    2015-01-01

    Introduction Since 1961 the use of Cation Exchange Resins has been the mainstream treatment for chronic hyperkalemia. For the past 25 years different kind of complications derived from its clinical use have been recognized, being the colonic necrosis the most feared and lethal of all. Presentation of case We report a case of a 72-year-old patient with chronic kidney disease, treated with calcium polystyrene sulfonate for hyperkalemia treatment who presented in the emergency department with constipation treated with hypertonic cathartics. With clinical deterioration 48 h later progressed with colonic necrosis requiring urgent laparotomy, sigmoidectomy and open abdomen management with subsequent rectal stump perforation and dead. The histopathology finding: calcium polystyrene sulfonate embedded in the mucosa, consistent with the cause of perforation. Discussion Lillemoe reported the first case series of five uremic patients with colonic perforation associated with the use of SPS in sorbitol in 1987 and in 2009 the FDA removed from the market the SPS containing 70% of sorbitol. The pathophysiologic change of CER goes from mucosal edema, ulcers, pseudomembranes, and the most severe case transmural necrosis. Up to present day, some authors have questioned the use of CER in the setting of lowering serum potassium. Despite its worldwide use in hyperkalemia settings, multiple studies have not demonstrated a significant potassium excretion by CER. Conclusion Despite the low incidence of colonic complication and lethal colonic necrosis associated with the CER clinical use, the general surgeon needs a high index of suspicion when dealing with patients treated with CER and abdominal pain. PMID:26439420

  12. A new cation-exchange method for accurate field speciation of hexavalent chromium

    Science.gov (United States)

    Ball, J.W.; McCleskey, R.B.

    2003-01-01

    A new method for field speciation of Cr(VI) has been developed to meet present stringent regulatory standards and to overcome the limitations of existing methods. The method consists of passing a water sample through strong acid cation-exchange resin at the field site, where Cr(III) is retained while Cr(VI) passes into the effluent and is preserved for later determination. The method is simple, rapid, portable, and accurate, and makes use of readily available, inexpensive materials. Cr(VI) concentrations are determined later in the laboratory using any elemental analysis instrument sufficiently sensitive to measure the Cr(VI) concentrations of interest. The new method allows measurement of Cr(VI) concentrations as low as 0.05 ??g 1-1, storage of samples for at least several weeks prior to analysis, and use of readily available analytical instrumentation. Cr(VI) can be separated from Cr(III) between pH 2 and 11 at Cr(III)/Cr(VI) concentration ratios as high as 1000. The new method has demonstrated excellent comparability with two commonly used methods, the Hach Company direct colorimetric method and USEPA method 218.6. The new method is superior to the Hach direct colorimetric method owing to its relative sensitivity and simplicity. The new method is superior to USEPA method 218.6 in the presence of Fe(II) concentrations up to 1 mg 1-1 and Fe(III) concentrations up to 10 mg 1-1. Time stability of preserved samples is a significant advantage over the 24-h time constraint specified for USEPA method 218.6.

  13. Use of potassium-form cation-exchange resin as a conductimetric enhancer in ion-exclusion chromatography of aliphatic carboxylic acids.

    Science.gov (United States)

    Iwata, Tomotaka; Mori, Masanobu; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2009-09-15

    In this study, a cation-exchange resin (CEX) of the K(+)-form, i.e., an enhancer resin, is used as a postcolumn conductimetric enhancer in the ion-exclusion chromatography of aliphatic carboxylic acids. The enhancer resin is filled in the switching valve of an ion chromatograph; this valve is usually used as a suppressor valve in ion-exchange chromatography. An aliphatic carboxylic acid (e.g., CH(3)COOH) separated by a weakly acidic CEX column of the H(+)-form converts into that of the K(+)-form (e.g., CH(3)COOK) by passing through the enhancer resin. In contrast, the background conductivity decreases because a strong acid (e.g., HNO(3)) with a higher conductimetric response in an eluent converts into a salt (e.g., KNO(3)) with a lower conductimetric response. Since the pH of the eluent containing the resin enhancer increases from 3.27 to 5.85, the enhancer accelerates the dissociations of analyte acids. Consequently, peak heights and peak areas of aliphatic carboxylic acids (e.g., acetic acid, propionic acid, butyric acid, and valeric acid) with the enhancer resin are 6.3-8.0 times higher and 7.2-9.2 times larger, respectively, than those without the enhancer resin. Calibrations of peak areas for injected analytes are linear in the concentration range of 0.01-1.0mM. The detection limits (signal-to-noise ratio=3) range from 0.10 microM to 0.39 microM in this system, as opposed to those in the range of 0.24-7.1 microM in the separation column alone. The developed system is successfully applied to the determination of aliphatic carboxylic acids in a chicken droppings sample.

  14. On the Structure-Property Relationships of Cation-Exchanged ZK-5 Zeolites for CO 2 Adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Pham, Trong D. [Department of Chemical and Biomolecular Engineering, University of Delaware, Newark Delaware 19716 USA; Hudson, Matthew R. [Center for Neutron Research, National Institute of Standards and Technology, Gaithersburg Maryland 20899 USA; Brown, Craig M. [Department of Chemical and Biomolecular Engineering, University of Delaware, Newark Delaware 19716 USA; Center for Neutron Research, National Institute of Standards and Technology, Gaithersburg Maryland 20899 USA; Lobo, Raul F. [Department of Chemical and Biomolecular Engineering, University of Delaware, Newark Delaware 19716 USA

    2017-02-16

    The CO2 adsorption properties of cation-exchanged Li-, Na-, K-, and Mg-ZK-5 zeolites were correlated to the molecular structures determined by Rietveld refinements of synchrotron powder X-ray diffraction patterns. Li-, K-, and Na-ZK-5 all exhibited high isosteric heats of adsorption (Qst) at low CO2 coverage, with Na-ZK-5 having the highest Qst (ca. 49 kJ mol-1). Mg2+ was located at the center of the zeolite hexagonal prism with the cation inaccessible to CO2, leading to a much lower Qst (ca. 30 kJ mol-1) and lower overall uptake capacity. Multiple CO2 adsorption sites were identified at a given CO2 loading amount for all four cation-exchanged ZK-5 adsorbents. Site A at the flat eight-membered ring windows and site B/B* in the γ-cages were the primary adsorption sites in Li- and Na-ZK-5 zeolites. Relatively strong dual-cation adsorption sites contributed significantly to an enhanced electrostatic interaction for CO2 in all ZK-5 samples. This interaction gives rise to a migration of Li+ and Mg2+ cations from their original locations at the center of the hexagonal prisms toward the α-cages, in which they interact more strongly with the adsorbed CO2.

  15. Modification of the cation exchange resin properties by impregnation in polyethyleneimine solutions: application to the separation of metallic ions.

    Science.gov (United States)

    Amara, Mourad; Kerdjoudj, Hacène

    2003-07-27

    A commercial cation exchange resin Amberlite 200 has been modified after immersion in solutions of polyethyleneimine (PEI). The kinetic of fixation of the metallic ions have been determined. The modification of the surface of the resin deals with a change in the order of the affinities of the resins towards cations. The retention is the function of the formation and the stability of the complex. The conditions of modification (pH, PEI concentration and time of immersion) have been examined and the modification was confirmed by the determination of the exchange capacities, the distribution coefficient (P) and the selectivity factors (S). The obtained results revealed the effect of PEI on the exchange properties of the resin. The pH range selected (6-8) permitted a good adherence of PEI onto the resin surface. The quantity of the adsorbed PEI was increased by raising the initial concentration and the immersion period. The exchange capacity for copper ion passed from 2.6 mmol g(-1), in the case of unmodified resin, to 3.9 mmol g(-1) for the modified one.

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

    Science.gov (United States)

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

    2016-02-01

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

  17. An Investigation into the Effect of Cation-exchange on the Adsorption Performance of Indium-based Sodalite-ZMOF

    KAUST Repository

    Samin, Umer A.

    2016-04-13

    There is a pressing need for advanced solid-state materials that can be implemented in industrial gas separation processes to achieve separations with a significantly reduced energy input compared to what is typically required from current technologies. Although certain porous materials like zeolites bear some commercial significance for gas separation; their inherent lack of tunability limits the extent to which these materials may be exploited in industry. Zeolite-like Metal-Organic Frameworks (ZMOFs) are a sub-class of Metal-Organic Framework materials (MOFs) that show a structural semblance to zeolites while possessing the tunability advantages of MOF materials. ZMOFs which are topologically similar to certain zeolites can be functionalised and tuned in numerous ways to improve their gas separation properties. In this work, indium-based sod-ZMOF was tuned by cation-exchange and then characterised by different experimental tools such as single-crystal x-ray diffraction, elemental analysis and gas adsorption. It was found that various parameters like the choice of cation, the concentration of salt solution and the choice of solvent had a significant bearing on the cation-exchange of sod-ZMOF and its subsequent adsorption properties.

  18. Synthesis of cation-exchanged laponite suspensions by laser ablation of microsized-metal particles in liquid

    Science.gov (United States)

    Phuoc, Tran X.; Chen, Ruey-Hung

    2011-03-01

    Laser ablation in the liquid technique has been used to synthesize cation-exchanged laponite suspensions. In summary, laser ablation of the microsize-metal powder (Co, Al, and Cu) dispersed in an aqueous solution containing deionized water laponite crystals was carried out using laser beam generated by a single-mode, Q-switched Nd-Yag laser operating at 532 nm with a pulse duration of 5.5 ns and 10 Hz repetition rate. Laser fluence was 0.265 J/cm 2 for all tests. For all samples, the mass fraction of laponite was 1%. General observations of the prepared samples indicated that an aqueous suspension of 1 wt% laponite retained its free flowing liquid phase characteristics even after aging for several weeks. When bivalent cationic metals (Cu, Co, Al) were ablated in it for about 1 h, even with a small amount of the metal (0.025% and 0.050%) were generated, the suspension became highly viscous and behaved as a shear-thinning and thixotropic material. That is, the suspension gelled strongly when it was allowed to rest. The gels, however, could easily be reverted to a low viscosity liquid with simple shaking. Information from TEM and XRD analysis indicated that such a sol-gel transformation might be due to the charge exchange between the cationic species produced during the laser ablation and the sodium ions in the interlayers of the clay sheets.

  19. Comparison between methods using copper, lanthanum, and colorimetry for the determination of the cation exchange capacity of plant cell walls.

    Science.gov (United States)

    Wehr, J Bernhard; Blamey, F Pax C; Menzies, Neal W

    2010-04-28

    The determination of the cation exchange capacity (CEC) of plant cell walls is important for many physiological studies. We describe the determination of cell wall CEC by cation binding, using either copper (Cu) or lanthanum (La) ions, and by colorimetry. Both cations are strongly bound by cell walls, permitting fast and reproducible determinations of the CEC of small samples. However, the dye binding methods using two cationic dyes, Methylene Blue and Toluidine Blue, overestimated the CEC several-fold. Column and centrifugation methods are proposed for CEC determination by Cu or La binding; both provide similar results. The column method involves packing plant material (2-10 mg dry mass) in a chromatography column (10 mL) and percolating with 20 bed volumes of 1 mM La or Cu solution, followed by washing with deionized water. The centrifugation method uses a suspension of plant material (1-2 mL) that is centrifuged, and the pellet is mixed three times with 10 pellet volumes of 1 mM La or Cu solution followed by centrifugation and final washing with deionized water. In both methods the amount of La or Cu bound to the material was determined by spectroscopic methods.

  20. 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

  1. Consistent effects of canopy vs. understory nitrogen addition on the soil exchangeable cations and microbial community in two contrasting forests.

    Science.gov (United States)

    Shi, Leilei; Zhang, Hongzhi; Liu, Tao; Zhang, Weixin; Shao, Yuanhu; Ha, Denglong; Li, Yuanqiu; Zhang, Chuangmao; Cai, Xi-an; Rao, Xingquan; Lin, Yongbiao; Zhou, Lixia; Zhao, Ping; Ye, Qing; Zou, Xiaoming; Fu, Shenglei

    2016-05-15

    Anthropogenic N deposition has been well documented to cause substantial impacts on the chemical and biological properties of forest soils. In most studies, however, atmospheric N deposition has been simulated by directly adding N to the forest floor. Such studies thus ignored the potentially significant effect of some key processes occurring in forest canopy (i.e., nitrogen retention) and may therefore have incorrectly assessed the effects of N deposition on soils. Here, we conducted an experiment that included both understory addition of N (UAN) and canopy addition of N (CAN) in two contrasting forests (temperate deciduous forest vs. subtropical evergreen forest). The goal was to determine whether the effects on soil exchangeable cations and microbial biomass differed between CAN and UAN. We found that N addition reduced pH, BS (base saturation) and exchangeable Ca and increased exchangeable Al significantly only at the temperate JGS site, and reduced the biomass of most soil microbial groups only at the subtropical SMT site. Except for soil exchangeable Mn, however, effects on soil chemical properties and soil microbial community did not significantly differ between CAN and UAN. Although biotic and abiotic soil characteristics differ significantly and the responses of both soil exchangeable cations and microbial biomass were different between the two study sites, we found no significant interactive effects between study site and N treatment approach on almost all soil properties involved in this study. In addition, N addition rate (25 vs. 50 kg N ha(-1) yr(-1)) did not show different effects on soil properties under both N addition approaches. These findings did not support previous prediction which expected that, by bypassing canopy effects (i.e., canopy retention and foliage fertilization), understory addition of N would overestimate the effects of N deposition on forest soil properties, at least for short time scale.

  2. Modification of Nafion Membranes by IL-Cation Exchange: Chemical Surface, Electrical and Interfacial Study

    Directory of Open Access Journals (Sweden)

    V. Romero

    2012-01-01

    A study of time evolution of the impedance curves measured in the system “IL aqueous solution/Nafion-112 membrane/IL aqueous solution” was also performed. This study allows us monitoring the electrical changes associated to the IL-cation incorporation in both the membrane and the membrane/IL solution interface, and it provides supplementary information on the characteristic of the Nafion/DTA+ hybrid material. Moreover, the results also show the significant effect of water on the electrical resistance of the Nafion-112/IL-cation-modified membrane.

  3. Highly Emissive Divalent-Ion-Doped Colloidal CsPb1–xMxBr3 Perovskite Nanocrystals through Cation Exchange

    Science.gov (United States)

    2017-01-01

    Colloidal CsPbX3 (X = Br, Cl, and I) perovskite nanocrystals (NCs) have emerged as promising phosphors and solar cell materials due to their remarkable optoelectronic properties. These properties can be tailored by not only controlling the size and shape of the NCs but also postsynthetic composition tuning through topotactic anion exchange. In contrast, property control by cation exchange is still underdeveloped for colloidal CsPbX3 NCs. Here, we present a method that allows partial cation exchange in colloidal CsPbBr3 NCs, whereby Pb2+ is exchanged for several isovalent cations, resulting in doped CsPb1–xMxBr3 NCs (M= Sn2+, Cd2+, and Zn2+; 0 50%), sharp absorption features, and narrow emission of the parent CsPbBr3 NCs. The blue-shift in the optical spectra is attributed to the lattice contraction that accompanies the Pb2+ for M2+ cation exchange and is observed to scale linearly with the lattice contraction. This work opens up new possibilities to engineer the properties of halide perovskite NCs, which to date are demonstrated to be the only known system where cation and anion exchange reactions can be sequentially combined while preserving the original NC shape, resulting in compositionally diverse perovskite NCs. PMID:28260380

  4. Suitability of the methylene blue test for determination of cation exchange capacity of clay minerals related to ammonium acetate method

    Science.gov (United States)

    Milošević, Maja; Logar, Mihovil; Dojčinović, Biljana; Erić, Suzana

    2015-04-01

    Cation exchange capacity (CEC) represents one of the most important parameters of clay minerals which reflects their ability to exchange cations with liquid phases in near contact. Measurement of CEC is used for characterizing sample plasticity, adsorbing and swelling properties which later define their usage in industrial purposes. Several methods have been developed over the years for determination of layer charge, charge density, charge distribution, etc. and have been published in numerous papers (Czimerova et al., 2006; Yukselen and Kaya, 2008). The main goal of present study is comparison of suitability of more recent method - methylene blue test in regard to older method - ammonium acetate for determination of CEC. For this study, we selected one montmorillonite clay (Bogovina, Serbia) and two mainly kaolinite clays (Miličinica, Serbia). Chemicals used for CEC determinations were solution of methylene blue (MB)(14*10-6M/ml) and ammonium acetate (AA) solution (1M). The obtained results are showing generally lower values in case of MB method. The main difference is due to molecular aggregation of MB on the clay surface. AA method is highly sensitive to the presence of CaO. Release of Ca ion from the sample into the solution can limit the saturation of exchange sites by the ammonium ion. This is clearly visible in case of montmorillonite clay. Fe2+ and Mg ions are difficult to move by the ammonium ion because of their ion radius, but in case of MB molecule there is no such restriction in removing them from the exchange sites. MB solution, even in a low concentration (2*10-6M/ml), is showing preferable results in moving the ions from their positions which is already visible after adding a small quantity of solution (25cm3). Both MB-titration and MB-spot test yield similar results and are much simpler methods than AA and they also give other information such as specific surface area (external and internal) whereas AA method only provides information about

  5. Uncertainties of Gaseous Oxidized Mercury Measurements Using KCl-Coated Denuders, Cation-Exchange Membranes, and Nylon Membranes: Humidity Influences.

    Science.gov (United States)

    Huang, Jiaoyan; Gustin, Mae Sexauer

    2015-05-19

    Quantifying the concentration of gaseous oxidized mercury (GOM) and identifying the chemical compounds in the atmosphere are important for developing accurate local, regional, and global biogeochemical cycles. The major hypothesis driving this work was that relative humidity affects collection of GOM on KCl-coated denuders and nylon membranes, both currently being applied to measure GOM. Using a laboratory manifold system and ambient air, GOM capture efficiency on 3 different collection surfaces, including KCl-coated denuders, nylon membranes, and cation-exchange membranes, was investigated at relative humidity ranging from 25 to 75%. Recovery of permeated HgBr2 on KCl-coated denuders declined by 4-60% during spikes of relative humidity (25 to 75%). When spikes were turned off GOM recoveries returned to 60 ± 19% of permeated levels. In some cases, KCl-coated denuders were gradually passivated over time after additional humidity was applied. In this study, GOM recovery on nylon membranes decreased with high humidity and ozone concentrations. However, additional humidity enhanced GOM recovery on cation-exchange membranes. In addition, reduction and oxidation of elemental mercury during experiments was observed. The findings in this study can help to explain field observations in previous studies.

  6. Comparison of gaseous oxidized Hg measured by KCl-coated denuders, and nylon and cation exchange membranes.

    Science.gov (United States)

    Huang, Jiaoyan; Miller, Matthieu B; Weiss-Penzias, Peter; Gustin, Mae Sexauer

    2013-07-02

    The chemical compounds that make up gaseous oxidized mercury (GOM) in the atmosphere, and the reactions responsible for their formation, are not well understood. The limitations and uncertainties associated with the current method applied to measure these compounds, the KCl-coated denuder, are not known due to lack of calibration and testing. This study systematically compared the uptake of specific GOM compounds by KCl-coated denuders with that collected using nylon and cation exchange membranes in the laboratory and field. In addition, a new method for identifying different GOM compounds using thermal desorption is presented. Different GOM compounds (HgCl2, HgBr2, and HgO) were found to have different affinities for the denuder surface and the denuder underestimated each of these compounds. Membranes measured 1.3 to 3.7 times higher GOM than denuders in laboratory and field experiments. Cation exchange membranes had the highest collection efficiency. Thermodesorption profiles for the release of GOM compounds from the nylon membrane were different for HgO versus HgBr2 and HgCl2. Application of the new field method for collection and identification of GOM compounds demonstrated these vary as a function of location and time of year. Understanding the chemistry of GOM across space and time has important implications for those developing policy regarding this environmental contaminant.

  7. Toward Separating Alpha-lactalbumin and Beta-lactoglobulin Proteins from Whey through Cation-exchange Adsorption

    Science.gov (United States)

    El-Sayed, Mayyada; Chase, Howard

    2009-05-01

    This paper describes the cation-exchange adsorption of the two major whey proteins, alpha-lactalbumin (ALA) and beta-lactoglobulin (BLG) with the purpose of establishing a process for isolating them from cow's milk whey. The single- and two-component adsorption of 1.5 mg/ml ALA and 3 mg/ml BLG to the cation-exchanger SP Sepharose FF at 20° C using 0.1 M acetate buffer of pH 3.7 was studied. Langmuir isotherm parameters were determined for the pure proteins. In two-component systems, BLG breakthrough curve exhibited an overshoot phenomenon that gave evidence for the presence of a competitive adsorption between the two proteins. Complete separation occurred and it was possible to obtain each of the two proteins in a pure form. The process was then applied to a whey concentrate mixture where incomplete separation took place. However, BLG was produced with 95% purity and a recovery of 80%, while ALA showed an 84% recovery with low purity.

  8. Radiometric Determination of Uranium in Natural Waters after Enrichment and Separation by Cation-Exchange and Liquid-Liquid Extraction

    CERN Document Server

    Pashalidis, I

    2003-01-01

    The alpha-radiometric determination of uranium after its pre-concentration from natural water samples using the cation-exchange resin Chelex-100, its selective extraction by tributylphosphate and electrodeposition on stainless steel discs is reported. The validity of the separation procedure and the chemical recoveries were checked by addition of uranium standard solution as well as by tracing with U-232. The average uranium yield was determined to be (97 +- 2) % for the cation-exchange, (95 +- 2) % for the liquid-liquid extraction, and more than 99% for the electrodeposition. Employing high-resolution alpha-spectroscopy, the measured activity of the U-238 and U-234 radioisotopes was found to be of similar magnitude; i.e. ~7 mBq/L and ~35 mBq/L for ground- and seawater samples, respectively. The energy resolution (FWHM) of the alpha-peaks was 22 keV, while the Minimum Detectable Activity (MDA) was estimated to be 1 mBq/L (at the 95% confidence limit).

  9. Changes of Soil Water, Organic Matter, and Exchangeable Cations Along a Forest Successional Gradient in Southern China

    Institute of Scientific and Technical Information of China (English)

    YAN Jun-Hua; ZHOU Guo-Yi; ZHANG De-Qiang; CHU Guo-Wei

    2007-01-01

    Information on the distribution patterns of soil water content (SWC), soil organic matter (SOM), and soil exchangeable cations (SEC) is important for managing forest ecosystems in a sustainable manner. This study investigated how SWC, SOM, and SEC were influenced in forests along a successional gradient, including a regional climax (monsoon evergreen broad-leaved forest, or MEBF), a transitional forest (coniferous and broad-leaved mixed forest, or MF), and a pioneer forest (coniferous Masson pine (Pinus massoniana) forest, or MPF) of the Dinghushan Biosphere Reserve in the subtropical region of southern China. SWC, SOM, and SEC excluding Ca2+ were found to increase in the soil during forest succession, being highest in the top soil layer (0 to 15 cm depth) except for Na+. The differences between soil layers were largest in MF. This finding also suggested that the nutrients were enriched in the topsoil when they became increasingly scarce in the soil. There were no significant differences (P = 0.05) among SWC, SOM, and SBC. A linear, positive correlation was found between SWC and SOM. The correlation between SOM and cation exchange capacity (CEC) was statistically significant, which agreed with the theory that the most important factor determining SEC is SOM. The ratio of K+ to Na+ in the topsoil was about a half of that in the plants of each forest. MF had the lowest exchangeable Ca2+ concentration among the three forests and Ca2+:K+ in MPF was two times higher than that in MF. Understanding the changes of SWC, SOM, and CEC during forest succession would be of great help in protecting all three forests in southern China.

  10. Selective cation exchange in the core region of Cu2-xSe/Cu2-xS core/shell nanocrystals.

    Science.gov (United States)

    Miszta, Karol; Gariano, Graziella; Brescia, Rosaria; Marras, Sergio; De Donato, Francesco; Ghosh, Sandeep; De Trizio, Luca; Manna, Liberato

    2015-09-30

    We studied cation exchange (CE) in core/shell Cu2-xSe/Cu2-xS nanorods with two cations, Ag(+) and Hg(2+), which are known to induce rapid exchange within metal chalcogenide nanocrystals (NCs) at room temperature. At the initial stage of the reaction, the guest ions diffused through the Cu2-xS shell and reached the Cu2-xSe core, replacing first Cu(+) ions within the latter region. These experiments prove that CE in copper chalcogenide NCs is facilitated by the high diffusivity of guest cations in the lattice, such that they can probe the whole host structure and identify the preferred regions where to initiate the exchange. For both guest ions, CE is thermodynamically driven as it aims for the formation of the chalcogen phase characterized by the lower solubility under the specific reaction conditions.

  11. Synthesis of silver embedded poly(o-anisidine molybdophosphate nano hybrid cation-exchanger applicable for membrane electrode.

    Directory of Open Access Journals (Sweden)

    Anish Khan

    Full Text Available Poly(o-anisidine molybdophosphate was expediently obtained by sol-gel mixing of Poly(o-anisidine into the inorganic matrices of molybdophosphate, which was allowed to react with silver nitrate to the formation of poly(o-anisidine molybdophosphate embedded silver nano composite. The composite was characterized by Fourier Transform Infrared Spectroscopy, X-ray powder diffraction, UV-Vis Spectrophotometry, Fluorescence Spectroscopy, Scanning Electron Microscopy/Energy-dispersive X-ray Spectroscopy and Thermogravimertic Analysis. Ion exchange capacity and distribution studies were carried out to understand the ion-exchange capabilities of the nano composite. On the basis of highest distribution studies, this nano composite cation exchanger was used as preparation of heavy metal ion selective membrane. Membrane was characterized for its performance as porosity and swelling later on was used for the preparation of membrane electrode for Hg(II, having better linear range, wide working pH range (2-4.5 with fast response in the real environment.

  12. Design of a fixed-bed ion-exchange process for the treatment of rinse waters generated in the galvanization process using Laminaria hyperborea as natural cation exchanger.

    Science.gov (United States)

    Mazur, Luciana P; Pozdniakova, Tatiana A; Mayer, Diego A; Boaventura, Rui A R; Vilar, Vítor J P

    2016-03-01

    In this study, the removal of zinc from galvanization wastewaters was performed in a fixed bed column packed with brown macro-algae Laminaria hyperborea, acting as a natural cation exchanger (resin). The rinse wastewater presents a zinc concentration between 9 and 22 mg/L, a high concentration of light metals (mainly Na and Ca), a high conductivity (0.5-1.5 mS/cm) and a low organic content (DOC = 7-15 mg C/L). The zinc speciation diagram showed that approximately 80% of zinc is in the form of Zn(2+) and ≅20% as ZnSO4, considering the effluent matrix. From all operational conditions tested for zinc uptake (17 treatment of 2.4 m(3)/day of galvanization wastewater, resulting in an estimated reactants cost of 2.44 €/m(3).

  13. Formation of ZnSe/Bi{sub 2}Se{sub 3} QDs by surface cation exchange and high photothermal conversion

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Guozhi; Wang, Peng; Zhang, Yanbang [School of science, Tianjin Chengjian University, Tianjin 300384 (China); Wu, Zengna; Li, Qiang; Yao, Jianghong [Key Laboratory of Weak-Light Nonlinear Photonics, Ministry of Education, School of Physics and TEDA Applied Physics School, Nankai University, Tianjin 300457 (China); Chang, Kai [Institute of Semiconductors, Chinese Academy of Sciences, P.O. Box 912, Beijing 100083 (China)

    2015-08-15

    Water-dispersed core/shell structure ZnSe/Bi{sub 2}Se{sub 3} quantum dots were synthesized by ultrasonicwave-assisted cation exchange reaction. Only surface Zn ion can be replaced by Bi ion in ZnSe quantum dots, which lead to the ultrathin Bi{sub 2}Se{sub 3} shell layer formed. It is significance to find to change the crystal of QDs due to the acting of ultrasonicwave. Cation exchange mechanism and excellent photothermal conversion properties are discussed in detail.

  14. Membrane resistance : The effect of salinity gradients over a cation exchange membrane

    NARCIS (Netherlands)

    Galama, A. H.; Vermaas, D. A.; Veerman, J.; Saakes, M.; Rijnaarts, H. H. M.; Post, J. W.; Nijmeijer, K.

    2014-01-01

    Ion exchange membranes (IEMs) are used for selective transport of ions between two solutions. These solutions are often different in concentration or composition. The membrane resistance (R-M) is an important parameter affecting power consumption or power production in electrodialytic processes. In

  15. Colorimetric Humidity and Solvent Recognition Based on a Cation-Exchange Clay Mineral Incorporating Nickel(II)-Chelate Complexes.

    Science.gov (United States)

    Hosokawa, Hitoshi; Mochida, Tomoyuki

    2015-12-01

    Solvatochromic nickel(II) complexes with diketonato and diamine ligands were incorporated into a saponite clay by ion exchange, and their colorimetric humidity- and solvent-recognition properties were investigated. These powders exhibit color change from red to blue-green depending on humidity, and the detection range can be controlled by modifying the metal complex. The humidity response takes advantage of the humidity-dependent water content in clay and the coordination of water molecules to the metal complex in equilibrium. The addition of organic solvents to the powders causes a color change to occur, varying from red to blue-green depending on the donor number of the solvent, thereby enabling solvent recognition. In the clay, the affinity of less sterically hindered complexes to water or solvent molecules is decreased compared with that in solution because the cationic complexes interact with the anionic layers in the clay. Incorporating diethylene glycol into the materials produced thermochromic powders.

  16. Perfluorinated carbon-chain copolymers with functional groups and cation exchange membranes based on them: synthesis, structure and properties

    Science.gov (United States)

    Kirsh, Yu E.; Smirnov, S. A.; Popkov, Yu M.; Timashev, Sergei F.

    1990-06-01

    The review is devoted to perfluorinated polymers with sulphonic and carboxylic acid groups and to cation exchange membranes based on them. The synthesis is described of copolymers of tetrafluoroethylene with perfluorovinyl ethers containing functional groups by radical copolymerisation in an organic medium and in aqueous emulsions. Special features of the copolymerisation and approaches to obtaining copolymers with set characteristics are discussed. Data are presented on the structure and physicochemical properties of the polymeric films. Attempts to form membranes from the polymers obtained, the means of strengthening them and methods for chemical modification are described. Data are correlated on the influence of structure and polymer composition and the nature of the functional groups on the electrochemical characteristics of membranes. Special features of the functioning of perfluorinated membranes in the process for making chlorine and alkali by the electrolysis of sodium chloride solution are considered. The bibliography has 104 references.

  17. Common Ion Effects In Zeoponic Substrates: Dissolution And Cation Exchange Variations Due to Additions of Calcite, Dolomite and Wollastonite

    Science.gov (United States)

    Beiersdorfer, R. E.; Ming, D. W.; Galindo, C., Jr.

    2003-01-01

    c1inoptilolite-rich tuff-hydroxyapatite mixture (zeoponic substrate) has the potential to serve as a synthetic soil-additive for plant growth. Essential plant macro-nutrients such as calcium, phosphorous, magnesium, ammonium and potassium are released into solution via dissolution of the hydroxyapatite and cation exchange on zeolite charged sites. Plant growth experiments resulting in low yield for wheat have been attributed to a Ca deficiency caused by a high degree of cation exchange by the zeolite. Batch-equilibration experiments were performed in order to determine if the Ca deficiency can be remedied by the addition of a second Ca-bearing, soluble, mineral such as calcite, dolomite or wollastonite. Variations in the amount of calcite, dolomite or wollastonite resulted in systematic changes in the concentrations of Ca and P. The addition of calcite, dolomite or wollastonite to the zeoponic substrate resulted in an exponential decrease in the phosphorous concentration in solution. The exponential rate of decay was greatest for calcite (5.60 wt. % -I), intermediate for wollastonite (2.85 wt.% -I) and least for dolomite (1.58 wt.% -I). Additions of the three minerals resulted in linear increases in the calcium concentration in solution. The rate of increase was greatest for calcite (3.64), intermediate for wollastonite (2.41) and least for dolomite (0.61). The observed changes in P and Ca concentration are consistent with the solubilities of calcite, dolomite and wollastonite and with changes expected from a common ion effect with Ca. Keywords: zeolite, zeoponics, common-ion effect, clinoptilolite, hydroxyapatite

  18. Controlling electron beam-induced structure modifications and cation exchange in cadmium sulfide–copper sulfide heterostructured nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Haimei [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Sadtler, Bryce; Habenicht, Carsten [Department of Chemistry, University of California, Berkeley, CA 94720 (United States); Freitag, Bert [FEI Company, P.O. Box 80066, KA 5600 Eindhoven (Netherlands); Alivisatos, A. Paul [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Department of Chemistry, University of California, Berkeley, CA 94720 (United States); Kisielowski, Christian, E-mail: CFKisielowski@lbl.gov [National Center for Electron Microcopy, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Joint Center for Artificial Photosynthesis, Berkeley, CA 94720 (United States)

    2013-11-15

    The atomic structure and interfaces of CdS/Cu{sub 2}S heterostructured nanorods are investigated with the aberration-corrected TEAM 0.5 electron microscope operated at 80 kV and 300 kV applying in-line holography and complementary techniques. Cu{sub 2}S exhibits a low-chalcocite structure in pristine CdS/Cu{sub 2}S nanorods. Under electron beam irradiation the Cu{sub 2}S phase transforms into a high-chalcocite phase while the CdS phase maintains its wurtzite structure. Time-resolved experiments reveal that Cu{sup +}–Cd{sup 2+} cation exchange at the CdS/Cu{sub 2}S interfaces is stimulated by the electron beam and proceeds within an undisturbed and coherent sulfur sub-lattice. A variation of the electron beam current provides an efficient way to control and exploit such irreversible solid-state chemical processes that provide unique information about system dynamics at the atomic scale. Specifically, we show that the electron beam-induced copper–cadmium exchange is site specific and anisotropic. A resulting displacement of the CdS/Cu{sub 2}S interfaces caused by beam-induced cation interdiffusion equals within a factor of 3–10 previously reported Cu diffusion length measurements in heterostructured CdS/Cu{sub 2}S thin film solar cells with an activation energy of 0.96 eV. - Highlights: • Heterostructured nanorods were investigated at atomic resolution showing that they are free of extended defects. • Beam–sample interactions are controlled by current and voltage variations to provide pristine crystal structures. • Beam-induced migration of heterointerfaces are measured time-resolved and compared with Cu diffusion coefficients. • Beam–sample interaction overwrite possible signal improvements that can be expected by sample cooling.

  19. Physical characterization of the state of motion of the phenalenyl spin probe in cation-exchanged faujasite zeolite supercages with pulsed EPR

    Science.gov (United States)

    Doetschman, D. C.; Dwyer, D. W.; Fox, J. D.; Frederick, C. K.; Scull, S.; Thomas, G. D.; Utterback, S. G.; Wei, J.

    1994-08-01

    The molecular motion of the phenalenyl (PNL) spin probe in the supercages of cation-exchanged X and Y zeolites (faujasites) has been physically characterized by pulsed and continuous wave (CW) electron paramagnetic resonance (EPR). Both X and Y zeolites, whose cation sites were exchanged with the alkali metal ions, Li +, Na +, K +, Rb + and Cs + were examined. There is a good correspondence between the temperature dependences of the PNL electron spin phase memory time and the CW EPR spectra. Both display evidence of a thermal activation from a stationary, non-rotating molecular state to a low-temperature state of in-plane rotation (Das et al., Chem Phys. 143 (1990) 253). The rate of in-plane rotation is an activated process, with E* | / R=1289 |+- 35 K and 1462 ± 47 K in NaX and KX zeolites, respectively. The rotation appears to be about an axis along which the half-filled, non-bonding π orbital interacts with the exchanged cation in the supercage. Both CW and pulsed EPR also show a higher temperature activation from the in-plane rotating state to an effectively isoptropic state of rotation of PNL in which the PNL-cation bond is thought to be broken, with E* ⊥ / R=2050 ± 110 K, 1956 ± 46K, 1335 ± 97 K in LiX, NaX and KX zeolites, respectively. The strength of the PNL-cation bonding decreases with increasing cation atomic number as indicated by E* ⊥ and the peripheral repulsion (crowding) of PNL increases with cation size as indicated E* |. There are qualitative indications that the binding of PNL to the cations in the Y zeolite is stronger than in the X zeolite.

  20. Preparation and Cation Exchange Properties of Zeolitic Adsorbents Using Fused Coal Fly Ash and Seawater

    Science.gov (United States)

    Hirai, Takashi; Wajima, Takaaki; Yoshizuka, Kazuharu

    For the development of functional material using coal fly ash discharged from thermal power plants, we have prepared zeolitic adsorbents derived from alkaline fused coal fly ash in several aqueous saline media to obtain the optimized preparation condition. The NH4+ exchange capacity of the product prepared at 80°C for 12 hours in diluted seawater using the precursor fused at 500°C was 4.6 mmol⁄g which is equivalent that of product prepared in deionized water. Zeolite-X and zeolite-A were produced in all aqueous media, in addition hydroxysodalite was produced over 12 hours. It was suggested that zeolite-A transform into hydroxysodalite in the products. The zeolitic adsorbents having high ion exchange capacity could be prepared in twice diluted seawater at 6-12 hours in 80°C using a precursor fused at 500°C.

  1. Structure and resistance of concentration polar layer on cation exchange membrane-solution interface

    Institute of Scientific and Technical Information of China (English)

    SANG Shang-bin; HUANG Ke-long; LI Xiao-gang; WANG Xian

    2006-01-01

    Membrane/solution interface consists of a neutral concentration polar layer(CPL) and a charge layer(CL) under external electrical field, and the neutral CPL can be neglected under high frequency AC electrical field. The relationship of CL thickness e with electrolyte concentration C and fixed ion exchange sites density σ in membrane surface layer can be expressed as e=σ/C.According to this model, the thickness of the CL on Nafion1135 membrane/solution interface(ec) was calculated under different membrane surface charge quantity Q and variable electrolyte concentration C. The membrane/solution interface CL thickness(em) is obviously related with the membrane properties, and decreases dramatically in a higher electrolyte concentration, em values are 76.3nm and 110.3 nm respectively for Nafion1135 and PE01 ion exchange membrane in 0.05 mol/L H2SO4 solution, and em values for both membrane tend to 2 nm in 2 mol/L H2SO4 solution. For Nafion1135 membrane, the comparison of ec and em gives the result that CL thickness em obtained by resistance measurement fits well with the calculated CPL thickness ec while proton in CL transferred to membrane surface is 14.56 × l0-10 mol, which corresponds to the fixed exchange group number in a surface layer with a thickness τ=2 nm for Nafion1135 membrane.

  2. Solution-membrane equilibrium at metal-deposited cation-exchange membranes: Chronopotentiometric characterization of metal-modified membranes

    Energy Technology Data Exchange (ETDEWEB)

    Shahi, V.K.; Prakash, R.; Ramachandraiah, G.; Rangarajan, R. [Central Salt and Marine Chemical Research Inst., Bhavnagar (India); Vasudevan, D. [Central Electrochemical Research Inst., Karaikudi (India)

    1999-08-01

    Ion-exchange membranes such as Nafion with suitable metal catalysts entrapped in the body have been found applications in fuel cells, water electrolysis, and also electroorganic synthesis. Copper- and lead-deposited interpolymer cationic membranes have been prepared by electroless plating by an ion-exchange method and characterized by chronopotentiometry and cyclic voltammetry. The parameters such as transition time ({tau}), I{tau}{sup 1/2}, the potential drop (E{sub 0}) across these membranes immediately after the application of constant current (I), and the height of the potential jump ({Delta}E) across the membrane at {tau} have been measured by chronopotentiometry and compared with those of plain membranes. The approximate percentage of metal coverage and the number of ionic sites masked by the deposited metal in terms of NaCl concentration have been estimated from the differences in I{tau}{sup 1/2} values of plain and metal-deposited membranes. The quantity of metal deposited in a unit area of the membrane surface was measured by differential pulse polarography. The oxidation and reduction peak potentials corresponding to Cu(0)/Cu(II) and Pb(0)/Pb(II) couples were identified by cyclic voltammetry at pH 2.8 and 4.5 of 0.2 M CH{sub 3}COONa-H{sub 2}SO{sub 4}.

  3. Comparing the short and long term stability of biodegradable, ceramic and cation exchange membranes in microbial fuel cells.

    Science.gov (United States)

    Winfield, Jonathan; Chambers, Lily D; Rossiter, Jonathan; Ieropoulos, Ioannis

    2013-11-01

    The long and short-term stability of two porous dependent ion exchange materials; starch-based compostable bags (BioBag) and ceramic, were compared to commercially available cation exchange membrane (CEM) in microbial fuel cells. Using bi-directional polarisation methods, CEM exhibited power overshoot during the forward sweep followed by significant power decline over the reverse sweep (38%). The porous membranes displayed no power overshoot with comparably smaller drops in power during the reverse sweep (ceramic 8%, BioBag 5.5%). The total internal resistance at maximum power increased by 64% for CEM compared to 4% (ceramic) and 6% (BioBag). Under fixed external resistive loads, CEM exhibited steeper pH reductions than the porous membranes. Despite its limited lifetime, the BioBag proved an efficient material for a stable microbial environment until failing after 8 months, due to natural degradation. These findings highlight porous separators as ideal candidates for advancing MFC technology in terms of cost and operation stability.

  4. Simultaneous determinations of Cr(VI) and Cr(III) by ion-exclusion/cation-exchange chromatography with an unmodified silica-gel column.

    Science.gov (United States)

    Hirata, Shizuko; Kozaki, Daisuke; Sakanishi, Kinya; Nakagoshi, Nobukazu; Tanaka, Kazuhiko

    2010-01-01

    In order to characterize the ion-exclusion and cation-exchange properties of an unmodified silica-gel column, the retention behaviors of Cr(VI) and Cr(III) ions were investigated using a Develosil 30-5 (150 x 4.6 mm i.d.) in the acidic region. Cr(VI) was separated from other anions by an ion-exclusion and ion-adsorption mechanism, and Cr(III) was separated from other cations with a cation-exchange mechanism. When using 2.0 mM oxalic acid (pH 2.6) as an eluent, a good separation of Cr(VI) and Cr(III) was obtained using conductimetric detection in 12 min. The method was successfully applied to the simultaneous determinations of Cr(VI) and Cr(III) added into tap-water and river-water samples.

  5. Acceptable levels of heavy metals (Cd, Cr, Cu, Ni, Pb, Zn) in soils, depending on their clay and humus content and cation-exchange capacity

    NARCIS (Netherlands)

    Haan, de S.; Rethfeld, H.; Driel, van W.

    1985-01-01

    Three sandy soils differing in humus content and three clay soils differing in clay content were supplied with heavy metals to determine which loading rate of each single metal should be regarded as critical from the viewpoint of crop yield and metal content dependent on soil cation exchange capacit

  6. Effect of a cation exchange resin on the uptake of heavy metals by grapevines and other cultivated plants grown in contaminated soils

    Energy Technology Data Exchange (ETDEWEB)

    Mohr, H.D.

    1982-12-01

    The effect of a cation exchange resin on the growth and heavy metal content of grapevine, sun flower, cress, wheat and Italian rye-grass was investigated in potted vineyard soil, contaminated by Cu-containing (total Cu content of the soil: 628 ppm), or a soil contaminated artificially with 20 ppm Cd. Roots of cress seedlings grown in a vineyard soil mixed with a cation exchange resin were 2.2 times longer than in the untreated soil. Rye-grass was not injured, whereas grapevine, sun flower and wheat showed varying degrees of growth reduction, chlorosis and necrosis when grown in untreated vineyard soil. However, wheat and sunflower grown in vineyard soil containing a cation exchange resin showed no injury and grapevines exhibited markedly reduced symptoms. The Zn, Cu and Cd content of the plants decreased considerably, whereas their Fe and Mn content was not influenced. Grapevine, grown in a calcareous soil contaminated with 20 ppm Cd, contained 447 ppm Cd in the roots and 0,20 ppm Cd in the leaves. The Cd content of the roots declined to 113 ppm, that of the leaves to 0,15 ppm when grown in the contaminated soil containing a cation exchanger.

  7. Effects of disodium cromoglycate on cationic exchange of deoxygenated sickle cells.

    Science.gov (United States)

    Bizumukama, Léonidas; Ferster, Alina; Gulbis, Béatrice; Kumps, Alain; Cotton, Frédéric

    2011-08-31

    In the present work, we explored the way in which cromoglycate, a drug used to treat allergies acts on ion movements in sickle cells. Cells were either slowly deoxygenated by overnight exposure to nitrogen or acutely deoxygenated by exposure to metabisulfite, a strong reducing agent which induces sickling of red blood sickle cells. Flushing the cells with nitrogen increased the intracellular concentration of Na(+) and decreased the intracellular concentration of K(+) and the sum of the concentrations of the two cations. One hundred nM cromoglycate inhibited the decrease of intracellular K(+) and the increase of intracellular Na(+) induced by deoxygenation (n=17). Metabisulfite (100mM) increased the intracellular concentration of Ca(2+) (measured by Fura Red) (n=15) and the shape of the cells (measured by light scattering) (n=9). One μM cromoglycate partially inhibited these two responses. In conclusion, cromoglycate partially inhibits abnormal K(+) loss, Ca(2+) entry pathways or Ca(2+) channels opened by cell deoxygenation and ensuing membrane modifications and prevents cell sickling.

  8. Disintegration and dissolution of spent radioactive cationic exchange resins using Fenton-like oxidation process

    Energy Technology Data Exchange (ETDEWEB)

    Wan, Zhong; Xu, Lejin [Collaborative Innovation Center for Advanced Nuclear Energy Technology, INET, Tsinghua University, Beijing 100084 (China); Wang, Jianlong, E-mail: wangjl@tsinghua.edu.cn [Collaborative Innovation Center for Advanced Nuclear Energy Technology, INET, Tsinghua University, Beijing 100084 (China); Beijing Key Laboratory of Radioactive Wastes Treatment, Tsinghua University, Beijing 100084 (China)

    2015-09-15

    Highlights: • The spent radioactive resins could be oxidized by Fenton-like process. • The influencing factors on resin oxidation were evaluated. • Chemical oxygen demand (COD) reduction rate was more than 99%. • SEM and Raman spectrum were used to analyze the resins morphological change. - Abstract: The treatment and disposal of the spent radioactive resins is essential for the sustainable development of the nuclear industry. In this paper, the disintegration and dissolution of spent cationic resins were studied by Fenton-like process. The influencing factors on resin dissolution, such as pH, temperature, type and concentration of catalysts were evaluated. The results showed that the spent resins could be effectively dissolved at pH < 1, [Fe{sup 2+}] = 0.2 M and T = 97 ± 2 °C. Chemical oxygen demand (COD) reduction rate was more than 99%. The scanning electron microscopy and the Raman spectrum were used to observe the morphological changes of the spent resins during the dissolution process. Fenton-like oxidation is an efficient method for the volume reduction and stabilization of the spent resins before further immobilization.

  9. Exchangeable sodium induced changes in yield, water relation and cation composition of fennel (Foeniculum vulgare Mill).

    Science.gov (United States)

    Garg, V K; Singh, P K; Pushpangadan, P

    2005-06-01

    A pot experiment was conducted with the objectives to assess the adaptation potential of fennel crop grown at 10, 20, 25, 35 and 40 ESP (exchangeable sodium percentage) levels. Results showed that the rate of seed germination, plant growth including branching pattern, umbels per plant and 1000 test seed weight were adversely affected by sodic soils. Assuming that fifty percent reduction in seed yield and Na+/K+ ratio in leaf tissue as an index of alkali tolerance revealed that fennel was tolerant up to 25 ESP. The cell sap pH and EC reflected optimum osmoticum maintenance to withstand sodicity stress at this level and beyond this leaf water potential decreased (negatively) more to impede water uptake.

  10. Reversible dissociation and ligand-glutathione exchange reaction in binuclear cationic tetranitrosyl iron complex with penicillamine.

    Science.gov (United States)

    Syrtsova, Lidia; Sanina, Natalia; Lyssenko, Konstantin; Kabachkov, Evgeniy; Psikha, Boris; Shkondina, Natal'ja; Pokidova, Olesia; Kotelnikov, Alexander; Aldoshin, Sergey

    2014-01-01

    This paper describes a comparative study of the decomposition of two nitrosyl iron complexes (NICs) with penicillamine thiolic ligands [Fe2(SC5H11NO2)2(NO)4]SO4 ·5H2O (I) and glutathione- (GSH-) ligands [Fe2(SC10H17N3O6)2(NO)4]SO4 ·2H2O (II), which spontaneously evolve to NO in aqueous medium. NO formation was measured by a sensor electrode and by spectrophotometric methods by measuring the formation of a hemoglobin- (Hb-) NO complex. The NO evolution reaction rate from (I)  k 1 = (4.6 ± 0.1)·10(-3) s(-1) and the elimination rate constant of the penicillamine ligand k 2 = (1.8 ± 0.2)·10(-3) s(-1) at 25°C in 0.05 M phosphate buffer,  pH 7.0, was calculated using kinetic modeling based on the experimental data. Both reactions are reversible. Spectrophotometry and mass-spectrometry methods have firmly shown that the penicillamine ligand is exchanged for GS(-) during decomposition of 1.5·10(-4) M (I) in the presence of 10(-3) M GSH, with 76% yield in 24 h. As has been established, such behaviour is caused by the resistance of (II) to decomposition due to the higher affinity of iron to GSH in the complex. The discovered reaction may impede S-glutathionylation of the essential enzyme systems in the presence of (I) and is important for metabolism of NIC, connected with its antitumor activity.

  11. Modification of polyamide-CdS-CdSe composite material films with Ag using a cation–cation exchange reaction

    Energy Technology Data Exchange (ETDEWEB)

    Krylova, V.; Žalenkienė, S.; Dukstienė, N. [Department of Physical and Inorganic Chemistry, Kaunas University of Technology, Radvilenu st. 19, LT-50254, Kaunas (Lithuania); Baltrusaitis, J., E-mail: job314@lehigh.edu [Department of Chemical and Biomolecular Engineering, Lehigh University, B336 Iacocca Hall, 111 Research Drive, Bethlehem, PA 18015 (United States)

    2015-10-01

    Highlights: • We investigated deposition of a mixed CdSe-CdS-Ag{sub 2}Se-Ag{sub 2}S on polyamide. • A single chalcogen precursor – K{sub 2}SeS{sub 2}O{sub 6} – was used. • AAS showed five- to ten-fold excess of chalcogens diffused into PA. • Addition of AgNO{sub 3} resulted in subsurface Ag{sub 2}Se–Ag{sub 2}S formation. - Abstract: Thin mixed CdSe-CdS-Ag{sub 2}Se-Ag{sub 2}S films were deposited on a polyamide 6 (PA) surface by successfully using a cation-exchange reaction between Cd{sup 2+} and Ag{sup +} to convert CdSe-CdS into Ag{sub 2}Se-Ag{sub 2}S. These were deposited using a K{sub 2}SeS{sub 2}O{sub 6} precursor solution at 60 °C followed by cadmium acetate (Cd(CH{sub 3}COO){sub 2}). An aqueous AgNO{sub 3} solution was used as the Ag source. XRD patterns showed a complex PA-Cd-S-Se-Ag film crystalline composition with CdS, CdSe, Ag{sub 2}S and Ag{sub 2}Se peaks. Calculated dislocation density ranged within 5–15 × 10{sup 13} lines·m{sup −2} indicating high quality atomic layers. Atomic Absorption Spectroscopy (AAS) showed five- to ten-fold excess of chalcogens to metals in the thin films formed. No chalcogenides were observed on the sample surface during XPS analysis after Ag exchange due to the desorption of CdS and CdSe layers, not diffused into the bulk of the polymer suggesting that silver chalcogenides were located subsurface, as opposed to the outermost layer, likely comprised of Ag{sub 2}O.

  12. Proteomics-based, multivariate random forest method for prediction of protein separation behavior during cation-exchange chromatography.

    Science.gov (United States)

    Swanson, Ryan K; Xu, Ruo; Nettleton, Dan; Glatz, Charles E

    2012-08-01

    The most significant cost of recombinant protein production lies in the optimization of the downstream purification methods, mainly due to a lack of knowledge of the separation behavior of the host cell proteins (HCP). To reduce the effort required for purification process development, this work was aimed at modeling the separation behavior of a complex mixture of proteins in cation-exchange chromatography (CEX). With the emergence of molecular pharming as a viable option for the production of recombinant pharmaceutical proteins, the HCP mixture chosen was an extract of corn germ. Aqueous two phase system (ATPS) partitioning followed by two-dimensional electrophoresis (2DE) provided data on isoelectric point, molecular weight and surface hydrophobicity of the extract and step-elution fractions. A multivariate random forest (MVRF) method was then developed using the three characterization variables to predict the elution pattern of individual corn HCP. The MVRF method achieved an average root mean squared error (RMSE) value of 0.0406 (fraction of protein eluted in each CEX elution step) for all the proteins that were characterized, providing evidence for the effectiveness of both the characterization method and the analysis approach for protein purification applications.

  13. COMPOSITE OF CHITOSAN VANILIN / SULFONATED POLYSTYRENE AS POLYMER ELECTROLYTE MEMBRANES : CATIONIC EXCHANGE CAPACITY, SWELLING DEGREE AND THERMAL PROPERTIES

    Directory of Open Access Journals (Sweden)

    Edi Pramono

    2016-08-01

    Full Text Available Research on the preparation and characterization of sulfonated polystyrene (PST /chitosan vanillin (KV composite as electrolyte membranes has been conducted in order to investigate the effect of PST and KV composition to its chemical and physical properties. Polystyrene was modified by sulfonation reaction to produces PST, meanwhile chitosan was modified by schift base reaction to produces KV. The composite membranes were prepared by casting method and were characterized in order to identify the functional groups contained in the composite, the cation exchange capacity (CEC, the Swelling Degree (SD, the thermal properties and the morphology. The peak of imine vibration in the FTIR spectrum indicates that the chitosan vanilin was succesfully synthesized. Meanwhile, the peak of sulfonate vibration indicates the product of sulfonation on polystyrene. The result of CEC analysis shows that the addition of sulfonate groups on polystyrene and the addition of phenolic groups on chitosan increase the CEC value. The increasing of PST and KV concentration in membrane enhance the CEC value. However, the increasing of PST concentration in membrane composition even decrease the Swelling Degree of membranes. Meanwhile, the increasing of KV concentration increase the swelling degree of membranes. Thermal analysis shows that the thermal decomposition of membranes occurs in three stages i.e. the dehydration of water molecules, the degradation of the subtituen groups and the plasticizer and the degradation of the back bone of chitosan and polystyrene.

  14. Role of tentacles and protein loading on pore accessibility and mass transfer in cation exchange materials for proteins.

    Science.gov (United States)

    Thomas, Helen; Coquebert de Neuville, Bertrand; Storti, Giuseppe; Morbidelli, Massimo; Joehnck, Matthias; Schulte, Michael

    2013-04-12

    In protein chromatography, the size of the protein determines which fraction of pores it can access within a resin and at which rate of diffusion. Moreover, in the presence of grafted polymers like in advanced materials, adsorbed proteins and electrolytes complicate the interaction pore-protein. In this study, we evaluated in a comparative way the behavior of Fractogel EMD SO3 (M) and (S), "tentacle"-type, strong cation exchangers, as well as a reference material without tentacles, all of which are commonly used for protein purification. ISEC experiments were carried out with a set of Dextran tracers of largely different molecular size covering the typical range of protein sizes. Experimental values of porosity (internal and external to the particles) as well as of pore diffusion coefficients have been measured at different NaCl concentrations and under protein loading. These results provide useful insights into the complex interplay among mentioned factors: first, the presence of tentacles induces size exclusion selectivity in the materials; second, the salt induces conformational changes of the tentacles, leading to porosities larger than expected in tentacle materials; third, protein adsorption mainly leads to a reduction of porosity due to pore space occupied by the protein and to a decrease of pore diffusion coefficient.

  15. Advanced analytical method of nereistoxin using mixed-mode cationic exchange solid-phase extraction and GC/MS.

    Science.gov (United States)

    Park, Yujin; Choe, Sanggil; Lee, Heesang; Jo, Jiyeong; Park, Yonghoon; Kim, Eunmi; Pyo, Jaesung; Jung, Jee H

    2015-07-01

    Nereistoxin(NTX) was originated from a marine annelid worm Lumbriconereis heteropoda and its analogue pesticides including cartap, bensultap, thiocyclam and thiobensultap have been commonly used in agriculture, because of their low toxicity and high insecticidal activity. However, NTX has been reported about its inhibitory neuro toxicity in human and animal body, by blocking nicotinic acetylcholine receptor and it cause significant neuromuscular toxicity, resulting in respiratory failure. We developed a new method to determine NTX in biological fluid. The method involves mixed-mode cationic exchange based solid phase extraction and gas chromatography/mass spectrometry for final identification and quantitative analysis. The limit of detection and recovery were substantially better than those of other methods using liquid-liquid extraction or headspace solid phase microextraction. The good recoveries (97±14%) in blood samples were obtained and calibration curves over the range 0.05-20 mg/L have R2 values greater than 0.99. The developed method was applied to a fatal case of cartap intoxication of 74 years old woman who ingested cartap hydrochloride for suicide. Cartap and NTX were detected from postmortem specimens and the cause of the death was ruled to be nereistoxin intoxication. The concentrations of NTX were 2.58 mg/L, 3.36 mg/L and 1479.7 mg/L in heart, femoral blood and stomach liquid content, respectively. The heart blood/femoral blood ratio of NTX was 0.76.

  16. Improving stability of virus-like particles by ion-exchange chromatographic supports with large pore size: advantages of gigaporous media beyond enhanced binding capacity.

    Science.gov (United States)

    Yu, Mengran; Li, Yan; Zhang, Songping; Li, Xiunan; Yang, Yanli; Chen, Yi; Ma, Guanghui; Su, Zhiguo

    2014-02-28

    Limited binding capacity and low recovery of large size multi-subunits virus-like particles (VLPs) in conventional agarose-gel based chromatographic supports with small pores have long been a bottleneck limiting the large scale purification and application of VLPs. In this study, four anion exchange media including DEAE-Sepharose FF (DEAE-FF), DEAE-Capto, gigaporous DEAE-AP-120nm and DEAE-AP-280nm with average pore diameters of 32nm, 20nm, 120nm and 280nm, respectively, were applied for purification of hepatitis B virus surface antigen (HBsAg) VLPs. Pore size effects of media on the VLPs adsorption equilibrium, adsorption kinetics, dynamic binding capacity (DBC), and recovery were investigated in detail. According to the confocal laser scanning microscopy observation, adsorption of the VLPs in DEAE-FF and DEAE-Capto was mostly confined to a thin shell on the outer surface of the beads, leaving the underlying pore space and the binding sites inaccessibly, while the large pores in gigaporous media enabled the VLPs to access to the interior pore spaces by diffusion transport efficiently. Compared to the most widely used DEAE-FF, gigaporous media DEAE-AP-280nm gained about 12.9 times increase in static adsorption capacity, 8.0 times increase in DBC, and 11.4 times increase in effective pore diffusivity. Beyond increasing the binding capacity and enhancing the mass transfer, the gigaporous structure also significantly improved the stability of the VLPs during intensive adsorption-desorption process by lowing the multi-point interaction between the VLPs and binding sites in the pores. At 2.0mg/mL-media loading quantity, about 85.5% VLPs were correctly self-assembled after the chromatography with DEAE-AP-280nm media; oppositely about 85.2% VLPs lost their normal assembly with DEAE-FF due to irreversible disassembly. Comparative investigation was made to study the purifying performance of these four chromatographic media for actual VLPs purification from recombinant

  17. A comparative study of chelating and cationic ion exchange resins for the removal of palladium(II) complexes from acidic chloride media.

    Science.gov (United States)

    Hubicki, Zbigniew; Wołowicz, Anna

    2009-05-30

    The increasing demand for palladium for technological application requires the development of ion exchange chromatography. Recently ion exchange chromatography has developed largely as a result of new types of ion exchangers available on the market of which two types are widely applied. One of them are selective (chelating) and modified ion exchangers and the other one are liquid exchangers. Two types of ion exchange resins such as chelating (Lewatit TP 214, Purolite S 920) and cationic (Chelite S, Duolite GT 73) ion exchangers are used for the recovery of palladium(II) complexes from chloride media (0.1-2.0M HCl-1.0M NaCl-0.0011 M Pd(II); 0.1-2.0M HCl-2.0M NaCl-0.0011M Pd(II)). The influence of concentration of hydrochloric acid, sodium chloride as well as the phase contact time on the degree of recovery of palladium(II) complexes was studied. Moreover, the amount of palladium(II) chlorocomplexes sorbed onto ion exchangers, the working ion exchange capacities and the weight and bed distribution coefficients were calculated in order to judge which of two types of resins possesses the best performance towards palladium(II) complexes.

  18. Ion Exchange and Thin Layer Chromatographic Separation and Identification of Amino Acids in a Mixture: An Experiment for General Chemistry and Biotechnology Laboratories

    Science.gov (United States)

    Brunauer, Linda S.; Caslavka, Katelyn E.; Van Groningen, Karinne

    2014-01-01

    A multiday laboratory exercise is described that is suitable for first-year undergraduate chemistry, biochemistry, or biotechnology students. Students gain experience in performing chromatographic separations of biomolecules, in both a column and thin layer chromatography (TLC) format. Students chromatographically separate amino acids (AA) in an…

  19. {sup 1}H and {sup 23}Na MAS NMR spectroscopy of cationic species in CO{sub 2} selective alkaline earth metal porous silicoaluminophosphates prepared via liquid and solid state ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Arevalo-Hidalgo, Ana G. [Department of Chemical Engineering, University of Puerto Rico-Mayagueez Campus, Mayagueez, PR 00681-9000 (Puerto Rico); Dugar, Sneha; Fu, Riqiang [National High Magnetic Field Laboratory, Florida State University, Tallahassee, FL 32310 (United States); Hernandez-Maldonado, Arturo J., E-mail: arturoj.hernandez@upr.edu [Department of Chemical Engineering, University of Puerto Rico-Mayagueez Campus, Mayagueez, PR 00681-9000 (Puerto Rico)

    2012-07-15

    The location of extraframework cations in Sr{sup 2+} and Ba{sup 2+} ion-exchanged SAPO-34 was estimated by means of {sup 1}H and {sup 23}Na MAS NMR spectroscopy and spectral deconvolution. Incorporation of the alkaline earth metal cations onto the SAPO framework was achieved via liquid state ion exchange, coupled partial detemplation/solid-state ion exchange, and combination of both techniques. MAS NMR revealed that the level of ion exchange was limited by the presence of protons and sodium cations near hexagonal prisms (site SI), which are relatively difficult to exchange with the alkaline earth metal due to steric and charge repulsion criteria. In addition, the presence of ammonium cations in the supercages facilitated the exchange of otherwise tenacious hydrogen as corroborated by unit cell compositional data as well as enhanced CO{sub 2} adsorption at low partial pressures. The extraframework ammonium species were produced from partial detemplation of the structure-directing agent employed for the SAPO-34 synthesis, tetraethylammonium. - Graphical abstract: MAS NMR was used to elucidate the position the cationic species in alkaline earth metal exchanged silicoaluminophosphates. These species played a significant role during the ion exchange process and, therefore, the materials ultimate CO{sub 2} adsorption performance. Highlights: Black-Right-Pointing-Pointer Location of extraframework Sr{sup 2+} or Ba{sup 2+} cations was estimated by means of {sup 1}H and {sup 23}Na MAS NMR. Black-Right-Pointing-Pointer Level of Sr{sup 2+} or Ba{sup 2+} ion exchange was limited by the presence of protons and sodium cations. Black-Right-Pointing-Pointer Presence of ammonium cations in the supercages facilitated the exchange. Black-Right-Pointing-Pointer Sr{sup 2+} and Ba{sup 2+} ion exchanged SAPOs are outstanding CO{sub 2} adsorbents.

  20. The partitioning of sulfur and chlorine between andesite melts and magmatic volatiles and the exchange coefficients of major cations

    Science.gov (United States)

    Zajacz, Zoltán; Candela, Philip A.; Piccoli, Philip M.; Sanchez-Valle, Carmen

    2012-07-01

    Andesite melts were equilibrated with an H-O-S-bearing volatile phase to determine the partition coefficients for S and Cl as a function of melt composition and oxygen fugacity. The experiments were conducted in rapid-quench MHC vessel assemblies at 200 MPa and 1000 °C, and over a range of imposed fO2 between NNO-1.2 and NNO+1.8. High fluid/melt mass ratios (∼15) were employed, allowing precise and accurate partition coefficients to be obtained by mass balance calculations. Chlorine exhibits Henrian behavior at ClO-0.5 activities typical for arc magmas, with D Cl volatile/melt = 1.36 ± 0.06 (1σ) below 0.2 wt.% Cl in the melt; at higher ClO-0.5 activities, D Cl volatile/melt increases linearly to 2.11 ± 0.02 at 1 wt.% Cl in the melt. In the volatile phase: FeCl2 ∼ NaCl > KCl ∼ HCl. The determination of cation exchange coefficients for major cations yielded: K K,Na volatile/melt = 1.23 ± 0.10 (1σ) and ∗K Fe,Na volatile/melt = D Fe volatile/melt / D Na volatile/melt = 1.08 ± 0.16 (1σ). Under these conditions, the concentration of HCl in the vapor is negatively correlated with the (Na + K)/(Al + Fe3+) ratio in the melt. Reduced sulfur (S2-) appears to obey Henry's law in andesite melt-volatile system at fH2S below pyrrhotite saturation. The partition coefficient for S at fO2 = NNO-0.5 correlates negatively with the FeO concentration in the melt, changing from 254 ± 25 at 4.0 wt.% FeO to 88 ± 6 at 7.5 wt.% FeO. Pyrrhotite saturation is reached when approximately 3.2 mol% S is present in the volatile phase at fO2 = NNO-0.5. At the sulfide/sulfate transition, the partition coefficient of S drops from 171 ± 23 to 21 ± 1 at a constant FeO content of ∼6 wt.% in the melt. At fO2 = NNO+1.8, anhydrite saturation is reached at ∼3.3 mol% S present in the volatile phase. Aqueous volatiles exsolving from intermediate to mafic magmas can efficiently extract S, and effect its transfer to sites of magmatic-hydrothermal ore deposit formation.

  1. Dynamics of the separation of amino acid and mineral salt in the stationary dialysis of solutions with an MK-40 profiled sulfo group cation exchange membrane

    Science.gov (United States)

    Vasil'eva, V. I.; Vorob'eva, E. A.

    2012-11-01

    The conjugated diffusion transport of amino acid and mineral salt through a profiled sulfo group cation exchange membrane that simulates the extraction of amino acid from wash waters of microbiological production containing mineral components not used in synthesis is studied. The competitive nature of the conjugation of flows resulting in a decrease in the rate of the mass transfer of components and their separation factor is established from a comparative analysis of experimental data on the diffusion transfer of phenylalanine and sodium chloride in the form of hydrogen from individual and mixed solutions through a profiled sulfo group cation exchange membrane. The range of concentrations and the ratio of components in solution corresponding to the effective separation of phenylalanine and sodium chloride are determined.

  2. Characteristics of Lipoprotein Peak x Eluted from a Column with the Eluent of High-magnesium Ion Concentration in Lipoprotein Analysis Using the Cation-exchange Chromatography

    OpenAIRE

    Yuji Hirowatari; Hiroshi Yoshida; Yutaka Ogura; Hidekastu Yanai; Hideo Kurosawa; Norio Tada

    2005-01-01

    The new lipoprotein analysis method using a cation-exchange chromatography, which contains a sulfopropyl-ligand column and two magnesium ion-containing eluents was previously reported. This method can separate serum lipoproteins on the column gel with a magnesium ion concentration gradient and high-density lipoprotein (HDL), low-density lipoprotein (LDL), very-low-density lipoprotein (VLDL) and an unspecified lipoprotein peak are eluted in order from the column. We have now characterize...

  3. High pH reversed-phase chromatography with fraction concatenation as an alternative to strong-cation exchange chromatography for two-dimensional proteomic analysis

    OpenAIRE

    Yang, Feng; Shen, Yufeng; Camp, David G.; Smith, Richard D.

    2012-01-01

    Orthogonal high-resolution separations are critical for attaining improved analytical dynamic range and protein coverage in proteomic measurements. High pH reversed-phase liquid chromatography (RPLC) followed by fraction concatenation affords better peptide analysis than conventional strong-cation exchange (SCX) chromatography applied for the two-dimensional proteomic analysis. For example, concatenated high pH reversed-phase liquid chromatography increased identification for peptides (1.8-fo...

  4. Controllable conversion of plasmonic Cu2-xS nanoparticles to Au2S by cation exchange and electron beam induced transformation of Cu2-xS-Au2S core/shell nanostructures.

    Science.gov (United States)

    Wang, Xianliang; Liu, Xin; Zhu, Dewei; Swihart, Mark T

    2014-08-01

    Self-doped Cu2-xS nanocrystals (NCs) were converted into monodisperse Cu2-xS-Au2S NCs of tunable composition, including pure Au2S, by cation exchange. The near-infrared (NIR) localized surface plasmon resonance (LSPR) was dampened and red-shifted with increasing Au content. Cation exchange was accompanied by elimination of cation vacancies and a change in crystal structure. Partially exchanged Cu2-xS-Au2S core/shell structures evolved to dumbbell-like structures under electron irradiation in the transmission electron microscope (TEM).

  5. Influence of lime, peat and cation exchanger on the heavy-metal-uptake of vine (Vitis vinifera L. ) from contaminated soils

    Energy Technology Data Exchange (ETDEWEB)

    Mohr, H.D.

    1980-10-01

    In pot experiments with heavy-metal-contaminated soils, the influence of different soil admixtures on growth and heavy-metal-uptake of vine cuttings was investigated. The following results were obtained: 1. The heavy metal uptake of vines from mixtures of soil and garbage-sewage-compost was strongly reduced by a cation exchanger. The heavy metal content of the roots decreased as follows: Cu68-77%; Zn36-74%; Cd29-81%; Mn20-45%; Pb13-52%; Cr7-58%. The Mn-, Zn- and Cu-content of wood, tendrils and leaves also decreased considerably. 2. Vine cuttings, which were cultivated on an acid, artificially Cd-contaminated soil, showed heavy damages and high Cd-contents. Admixtures of lime, cation exchanger or garbage-sewage-sludge-compost strongly reduced the injury of vines and their Cd-content. A combined addition of lime and cation exchanger was most effectful. On the contrary, the toxic effect of Cd was intensified by the acid reaction of peat.

  6. Effect of the intercalated cation-exchanged on the properties of nanocomposites prepared by 2-aminobenzene sulfonic acid with aniline and montmorillonite

    Energy Technology Data Exchange (ETDEWEB)

    Toumi, I. [Laboratoire de Chimie Organique, Macromoleculaire et des Materiaux, Universite de Mascara, Bp 763 Mascara 29000 (Algeria); Benyoucef, A., E-mail: ghani29000@yahoo.fr [Laboratoire de Chimie Organique, Macromoleculaire et des Materiaux, Universite de Mascara, Bp 763 Mascara 29000 (Algeria); Yahiaoui, A. [Laboratoire de Chimie Organique, Macromoleculaire et des Materiaux, Universite de Mascara, Bp 763 Mascara 29000 (Algeria); Quijada, C. [Departamento de Ingenieria Textil y Papelera, Universidad Politecnica de Valencia, Pza Ferrandiz i Carbonel, E-03801 Alcoy, Alicante (Spain); Morallon, E. [Departamento de Quimica Fisica e Instituto Universitario de Materiales, Universidad de Alicante, Apartado 99, E-03080 Alicante (Spain)

    2013-02-25

    Polymer/montmorillonite nanocomposites were prepared. Intercalation of 2-aminobenzene sulfonic acid with aniline monomers into montmorillonite modified by cation was followed by subsequent oxidative polymerization of monomers in the interlayer spacing. The clay was prepared by cation exchange process between sodium cation in (M-Na) and copper cation (M-Cu). XRD analyses show the manifestation of a basal spacing (d-spacing) for M-Cu changes depending on the inorganic cation and the polymer intercalated in the M-Cu structure. TGA analyses reveal that polymer/M-Cu composites is less stable than M-Cu. The conductivity of the composites is found to be 10{sup 3} times higher than that for M-Cu. The microscopic examinations including TEM picture of the nanocomposite demonstrated an entirely different and more compatible morphology. Remarkable differences in the properties of the polymers have also been observed by UV-Vis and FTIR, suggesting that the polymer produced with presence of aniline has a higher degree of branching. The electrochemical behavior of the polymers extracted from the nanocomposites has been studied by cyclic voltammetry which indicates the electroactive effect of nanocomposite gradually increased with aniline in the polymer chain.

  7. Tuning Equilibrium Compositions in Colloidal Cd1-xMnxSe Nanocrystals Using Diffusion Doping and Cation Exchange.

    Science.gov (United States)

    Barrows, Charles J; Chakraborty, Pradip; Kornowske, Lindsey M; Gamelin, Daniel R

    2016-01-26

    The physical properties of semiconductor nanocrystals can be tuned dramatically via composition control. Here, we report a detailed investigation of the synthesis of high-quality colloidal Cd1-xMnxSe nanocrystals by diffusion doping of preformed CdSe nanocrystals. Until recently, Cd1-xMnxSe nanocrystals proved elusive because of kinetic incompatibilities between Mn(2+) and Cd(2+) chemistries. Diffusion doping allows Cd1-xMnxSe nanocrystals to be prepared under thermodynamic rather than kinetic control, allowing access to broader composition ranges. We now investigate this chemistry as a model system for understanding the characteristics of nanocrystal diffusion doping more deeply. From the present work, a Se(2-)-limited reaction regime is identified, in which Mn(2+) diffusion into CdSe nanocrystals is gated by added Se(2-), and equilibrium compositions are proportional to the amount of added Se(2-). At large added Se(2-) concentrations, a solubility-limited regime is also identified, in which x = xmax = ∼0.31, independent of the amount of added Se(2-). We further demonstrate that Mn(2+) in-diffusion can be reversed by cation exchange with Cd(2+) under exactly the same reaction conditions, purifying Cd1-xMnxSe nanocrystals back to CdSe nanocrystals with fine tunability. These chemistries offer exceptional composition control in Cd1-xMnxSe NCs, providing opportunities for fundamental studies of impurity diffusion in nanocrystals and for development of compositionally tuned nanocrystals with diverse applications ranging from solar energy conversion to spin-based photonics.

  8. Recommandations pour la détermination expérimentale de la capacité d'échange de cations des milieux argileux Recommendations for Experimentally Determining the Cation-Exchange Capacity of Shaly Media

    Directory of Open Access Journals (Sweden)

    Chambre Syndicale du Pétrole$

    2006-11-01

    Full Text Available Cet article présente une méthode relativement simple et précise destinée à la détermination de la capacité d'échanges de cations des milieux argileux qui permet de caractériser la réactivité des argiles. Cette mesure présente une certaine importance en raison des problèmes posés par les réservoirs argileux (interprétation des diagraphies, efficacité des méthodes de récupération améliorée par voie chimique. . . . Après avoir brièvement rappelé les propriétés fondamentales des argiles, la capacité d'échanges de cations (CEC est définie et la méthode recommandée de mesure de celle-ci (dosage par le chlorure de cobaltihexammine est décrite. Trois exemples viennent ensuite illustrer cette méthode dans le cas d'une argile pure, d'un sable argileux et d'un échantillon de grès argileux consolidé. This article describes a relatively simple and accurate method for determining the cation-exchange capacity of shaly media, which enables the characterization of the clay reactivity. This measurement is of some importance because of the problems posed by shaly reservoirs (interpreting well logs, effectiveness of improved-recovery methods by chemical means, etc. . After a brief review of the fondamental properties of shales, the cation-exchange capacity (CEC is defined, and the recommended measurement method by using cobaltihexammine chloride is described. Three examples are then given to illustrate this method for pure clay, for a shaly Band and for a consolidated shaly sandstone.

  9. Cation exchange synthesis of uniform PbSe/PbS core/shell tetra-pods and their use as near-infrared photodetectors

    Science.gov (United States)

    Mishra, N.; Mukherjee, B.; Xing, G.; Chakrabortty, S.; Guchhait, A.; Lim, J. Y.

    2016-07-01

    In this work we explore the preparation of complex-shaped semiconductor nanostructures composed of different materials via a cationic exchange process in which the cations of the original semiconductor nanostructure are replaced by cations of different metals with preservation of the shape and the anionic framework of the nanocrystals. Utilizing this cation exchange method, we synthesized two new tetrapods for the first time: Cu2-xSe/Cu2-xS and PbSe/PbS, both prepared from CdSe/CdS tetrapods as `templates'. We also fabricated near-infrared (NIR) photodetectors with a very simple architecture comprising a PbSe/PbS tetrapod layer between two Au electrodes on a glass substrate. When illuminated by a NIR laser, these devices are capable of achieving a responsivity of 11.9 A W-1 without the use of ligand-exchange processes, thermal annealing or hybrid device architecture. Transient absorption spectroscopy was carried out on these PbSe/PbS tetrapods, the results of which suggest that the branched morphology contributes in part to device performance. Investigation of the charge dynamics of the PbSe/PbS tetrapods revealed an extremely long-lived exciton recombination lifetime of ~17 ms, which can result in enhanced photoconductive gain. Overall, these heterostructured tetrapods showcase simultaneously the importance of nanoparticle shape, band structure, and surface chemistry in the attainment of NIR photodetection.In this work we explore the preparation of complex-shaped semiconductor nanostructures composed of different materials via a cationic exchange process in which the cations of the original semiconductor nanostructure are replaced by cations of different metals with preservation of the shape and the anionic framework of the nanocrystals. Utilizing this cation exchange method, we synthesized two new tetrapods for the first time: Cu2-xSe/Cu2-xS and PbSe/PbS, both prepared from CdSe/CdS tetrapods as `templates'. We also fabricated near-infrared (NIR) photodetectors

  10. Insights in understanding aggregate formation and dissociation in cation exchange chromatography for a structurally unstable Fc-fusion protein.

    Science.gov (United States)

    Chen, Zhiqiang; Huang, Chao; Chennamsetty, Naresh; Xu, Xuankuo; Li, Zheng Jian

    2016-08-19

    Cation-exchange chromatography (CEX) of a structurally unstable Fc-fusion protein exhibited multi-peak elution profile upon a salt-step elution due to protein aggregation during intra-column buffer transition where low pH and high salt coexisted. The protein exhibited a single-peak elution behavior during a pH-step elution; nevertheless, the levels of soluble aggregates (i.e. high molecular weight species, HMW) in the CEX eluate were still found up to 12-fold higher than that for the load material. The amount of the aggregates formed upon the pH-step elution was dependent on column loading with maximum HMW achieved at intermediate loading levels, supporting the hypothesis that the aggregation was the result of both the conformational changes of the bound protein and the solution concentration of the aggregation-susceptible proteins during elution. Factors such as high load pH, short protein/resin contact time, hydrophilic resin surface, and weak ionizable ligand were effective, to some extent, to reduce aggregate formation by improving the structural integrity of the bound protein. An orthogonal technique, differential scanning fluorimetry (DSF) using Sypro Orange dye confirmed that the bound protein exposed more hydrophobic area than the native molecule in free solution, especially in the pH 4-5 range. The Sypro Orange dye study of resin surface property also demonstrated that the poly[styrene-divinylbenzene]-based Poros XS with polyhydroxyl surface coating is more hydrophobic compared to the agarose-based CM Sepharose FF and SP Sepharose FF. The hydrophobic property of Poros XS contributed to stronger interactions with the partially unfolded bound protein and consequently to the higher aggregate levels seen in Poros XS eluate. This work also investigates the aggregation reversibility in CEX eluate where up to 66% of the aggregates were observed to dissociate into native monomers over a period of 120h, and links the aggregate stability to such conditions as resin

  11. Influência da matéria orgânica na capacidade de troca de cations do solo Cation-exchange capacity of the organic fraction of soils

    Directory of Open Access Journals (Sweden)

    F. da Costa Verdade

    1956-01-01

    . The cation-exchange capacity and other data on these soils show that the organic fraction must play an important role in the cation-exchange process. The study of the adsorptive capacity of the organic matter was done by destruction of the organic fraction of the soil by 12% hydrogen peroxide. For heavy textured soils the results show that the organic fraction most resistant to oxidation had a higher cation-exchange capacity than the portion first oxidized. For sandy soils all organic fractions had the same magnitude in the base adsorbing power. It was observed that the organic matter seems to inhibit the base-exchange capacity of the mineral fraction. Plotting the percentage of cation-exchange capacity of the organic fraction against the percentage of organic carbon in the soil, a curve is determined which shows the inhibition phenomenon. The results were rather scattered and the experiments are now being repeated to elucidate these observations. The organic cation-exchange capacity of soils in São Paulo is 30-40% for fine textured soils and 50-60% for sandy soils. Since most of the farming land in São Paulo belongs to the sandy soil group called Bauru, the problem of maintaining or increasing the fertility of these soils is dependent on their organic matter content.

  12. Obtention of the cation exchange capacity of a natural kaolinite with radioactive tracers; Obtencion de la capacidad de intercambio cationico de una kaolinita natural con trazadores radioactivos

    Energy Technology Data Exchange (ETDEWEB)

    Uribe I, A.; Badillo A, V.E. [Universidad Autonoma de Zacatecas, 98000 Zacatecas (Mexico); Monroy G, F. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)]. e-mail: Adrya81@hotmail.com

    2005-07-01

    One of the more used techniques for the elimination of the heavy metals present in water systems is to use adsorbent mineral phases like zeolites and clays, among others. The clays are able to exchange easily the fixed ions in the external surface of its crystals or well the ions present in the interlaminar spaces of the structures, for other existent ones in the encircling aqueous solutions for that the Cation exchange capacity (CIC) is defined as the sum of all the cations exchange that a mineral can possess independent to the physicochemical conditions. The CIC is equal to the measure of the total of negative charges of the mineral by mass of the solid (meq/g). In this investigation work, the value of the CIC equal to 2.5 meq/100 g is obtained, of a natural kaolinite from the State of Hidalgo studying the retention of the sodium in the kaolinite with the aid of the radioactive isotope {sup 24} Na and of the selective electrodes technique, making vary the pH value. So is experimentally demonstrated that the CIC is an intrinsic property of the mineral independent of the pH value of the solution and of the charges origin. (Author)

  13. Tunable separation of anions and cations by column switching in ion chromatography.

    Science.gov (United States)

    Amin, Muhammad; Lim, Lee Wah; Takeuchi, Toyohide

    2007-03-15

    A convenient ion chromatography method has been proposed for the routine and simple determination of anions (Cl(-), SO(4)(2-) and NO(3)(-)) and/or cations (Na(+), NH(4)(+), K(+), Mg(2+) and Ca(2+)) using a single pump, a single eluent and a single detector. The present system used cation-exchange and anion-exchange columns connected in series via two 6-port switching valves or a single 10-port valve. The connection order of the ion-exchange columns could be varied by switching the valve(s). The present system therefore allowed the separation of either cations or anions in a single chromatographic run. While one ion-exchange column is being operated, the other ion-exchange column is being conditioned, i.e., the columns are always ready for analysis at any time. When 2.4mM 5-sulfosalicylic acid was used as the eluent, the three anions and the five cations could be separated on the anion-exchange column and cation-exchange column, respectively. In order to obtain the separations of the target ions, the injection valve was placed between the two columns. Complete separations of the above anions or cations were demonstrated within 10min each. The detection limits at S/N=3 were 19-50ppb (mug/l) for cations and 10-14ppb for anions. The relative standard deviations of the analyte ions were less than 1.1, 2.9 and 2.8% for retention time, peak area and peak height, respectively. This proposed technique was applied to the determination of common anions and cations in river water samples.

  14. Hybrid organic-inorganic silica monolith with hydrophobic/strong cation-exchange functional groups as a sorbent for micro-solid phase extraction.

    Science.gov (United States)

    Zheng, Ming-Ming; Ruan, Ge-Deng; Feng, Yu-Qi

    2009-11-06

    A hybrid organic-inorganic silica monolith with hydrophobic and strong cation-exchange functional groups was prepared and used as a sorbent for micro-solid phase extraction (micro-SPE). The hybrid silica monolith functionalized with octyl and thiol groups was conveniently synthesized by hydrolysis and polycondensation of a mixture of tetraethoxysilane (TEOS), n-octyltriethoxysilane (C8-TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) via a two-step catalytic sol-gel process. Due to the favorable chemical reactivity of mercapto pendant moieties, the obtained hybrid monolith was oxidized using hydrogen peroxide (30%, w/w) to yield sulfonic acid groups, which provided strong cation-exchange sites. The obtained hybrid monolith was characterized by diffused infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The results show that the resulting monolith contains much higher carbon (31.6%) and sulfur (4.8%) contents than traditionally bonded silica materials. The extraction performance of the hybrid monolith was evaluated using sulfonamides as testing analytes by micro-SPE on-line coupled to HPLC. The results show that the hybrid monolith with hydrophobic and strong cation-exchange functional groups exhibits high extraction efficiency towards the testing analytes. The column-to-column RSD values were 1.3-9.8% for the extraction of SAs investigated. The extraction performance of the hybrid silica monolith remained practically unchanged after treated with acid (pH 1.0) and basic solutions (pH 10.5). Finally, the application of the hybrid monolith was demonstrated by micro-SPE of sulfonamide residues from milk followed by HPLC-UV analysis. The limits of detection (S/N=3) for eight SAs were found to be 1.0-3.0ng/mL in milk. The recoveries of eight SAs spiked in milk sample ranged from 80.2% to 115.6%, with relative standard deviations less than 11.8%.

  15. Near-Infrared Emitting CuInSe2/CuInS2 Dot Core/Rod Shell Heteronanorods by Sequential Cation Exchange

    OpenAIRE

    2015-01-01

    The direct synthesis of heteronanocrystals (HNCs) combining different ternary semiconductors is challenging and has not yet been successful. Here, we report a sequential topotactic cation exchange (CE) pathway that yields CuInSe2/CuInS2 dot core/rod shell nanorods with near-infrared luminescence. In our approach, the Cu+ extraction rate is coupled to the In3+ incorporation rate by the use of a stoichiometric trioctylphosphine-InCl3 complex, which fulfills the roles of both In-source and Cu-ex...

  16. Near-infrared emitting CuInSe_{2}/CuInS_{2} dot core/rod shell heteronanorods by sequential cation exchange

    OpenAIRE

    2015-01-01

    Abstract: The direct synthesis of heteronanocrystals (HNCs) combining different ternary semiconductors is challenging and has not yet been successful. Here, we report a sequential topotactic cation exchange (CE) pathway that yields CuInSe2/CuInS2 dot core/rod shell nanorods with near-infrared luminescence. In our approach, the Cu+ extraction rate is coupled to the In3+ incorporation rate by the use of a stoichiometric trioctylphosphine-InCl3 complex, which fulfills the roles of both In-source...

  17. 阳离子交换毛细管整体柱的制备及其在毛细管离子色谱中的应用%Preparation and Application of Cation-exchange Capillary Monolithic Column in Capillary Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    李晶; 朱岩

    2013-01-01

    Polymer-based cation exchange capillary monolithic column was prepared for capillary ion chromatography (CIC) by radical polymerization in a 320-μm-i. d. fused-silica capillary tube, taking glycidyl methacrylate ( GMA ) as the functional monomer, ethylene dimethacrylate ( EDMA) as the cross-linking agent and in the presence of 1 ,4-butanediol, 1-propanol and water as the porogen solvents and azobisisobutyronitrile (AIBN) as a suitable initiator. Introduction of cation exchange sites was achieved by reacting with Na2SO3. Coupled with the prepared cation exchange capillary monolithic column, a capillary ion chromatography system was constructed with a pump (in μL/min level) , a capillary detection cell and a UV detector, on which more chromatographic characteristics were further studied. With the CIC system, 9 common univalent and divalent cations (Li+ , Na+ , NH4+ , K+ , Cs+ , Mg2+, Ca2+ , Sr2+, Ba2+) were successfully separated and determined by flow rate gradient. Another interesting separation of cations and melamine was also tested on the prepared column.%以甲基丙烯酸缩水甘油酯(GMA)为功能单体,亚乙基二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为自由基引发剂,在三元致孔剂(正丙醇,1,4-丁二醇,水)的存在下,在320μm内径的弹性石英毛细管柱内制备得到带有环氧功能基团的聚合物整体柱基质;利用Na2SO3对其改性,制备得到磺酸基型阳离子交换毛细管整体柱.采用微流泵、毛细管检测池和紫外检测器构建了毛细管离子色谱系统,并对所制备的整体柱的流体力学参数、色谱性能参数进行评价;采用流速梯度洗脱的方式实现9种常见阳离子(Li+,Na+,NH4+,K+,Cs+,Mg2+,Ca2+,Sr2+,Ba2+)的分离分析;此色谱系统还可应用于牛奶中阳离子和三聚氰胺的分离检测.

  18. Determination of some aliphatic carboxylic acids in anaerobic digestion process waters by ion-exclusion chromatography with conductimetric detection on a weakly acidic cation-exchange resin column.

    Science.gov (United States)

    Ito, Kazuaki; Takayama, Yohichi; Ikedo, Mikaru; Mori, Masanobu; Taoda, Hiroshi; Xu, Qun; Hu, Wenzhi; Sunahara, Hiroshi; Hayashi, Tsuneo; Sato, Shinji; Hirokawa, Takeshi; Tanaka, Kazuhiko

    2004-06-11

    The determination of seven aliphatic carboxylic acids, formic, acetic, propionic, isobutyric, n-butyric, isovaleric and n-valeric acids in anaerobic digestion process waters was examined using ion-exclusion chromatography with conductimetric detection. The analysis of these biologically important carboxylic acids is necessary as a measure for evaluating and controlling the process. The ion-exclusion chromatography system employed consisted of polymethacrylate-based weakly acidic cation-exchange resin columns (TSKgel OApak-A or TSKgel Super IC-A/C). weakly acidic eluent (benzoic acid), and conductimetric detection. Particle size and cation-exchange capacity were 5 microm and 0.1 meq./ml for TSKgel OApak-A and 3 microm and 0.2 meq./ml for TSKgel Super IC-A/C, respectively. A dilute eluent (1.0-2.0 mM) of benzoic acid was effective for the high resolution and highly conductimetric detection of the carboxylic acids. The good separation of isobutyric and n-butyric acids was performed using the TSKgel Super IC-A/C column (150 mm x 6.0 mm i.d. x 2). The simple and good chromatograms were obtained by the optimized ion-exclusion chromatography conditions for real samples from mesophilic anaerobic digestors, thus the aliphatic carboxylic acids were successfully determined without any interferences.

  19. Fabrication, characterization and photocatalytic properties of Ag/AgI/BiOI heteronanostructures supported on rectorite via a cation-exchange method

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Yunfang [School of Chemistry and Environment, South China Normal University, Guangzhou 510006, Guangdong (China); Fang, Jianzhang, E-mail: fangjzh@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Guangzhou 510006, Guangdong (China); Guangdong Technology Research Center for Ecological Management and Remediation of Urban Water System, Guangzhou 510006 (China); Lu, Shaoyou [Shenzhen Center for Disease Control and Prevention, Shenzhen 518055 (China); Wu, Yan; Chen, Dazhi; Huang, Liyan [Institute of Engineering Technology of Guangdong Province, Key Laboratory of Water Environmental Pollution Control of Guangdong Province, Guangzhou 510440 (China); Xu, Weicheng; Zhu, Ximiao [School of Chemistry and Environment, South China Normal University, Guangzhou 510006, Guangdong (China); Fang, Zhanqiang [School of Chemistry and Environment, South China Normal University, Guangzhou 510006, Guangdong (China); Guangdong Technology Research Center for Ecological Management and Remediation of Urban Water System, Guangzhou 510006 (China)

    2015-04-15

    Highlights: • Ag/AgI/BiOI-rectorite was prepared by twice cation-exchange process. • Ag/AgI/BiOI-rectorite photocatalyst possessed SPR and adsorption capacity. • Ag/AgI/BiOI-rectorite exhibited highly photocatalytic activity. • Trapped holes and ·O{sub 2}{sup −} were formed active species in the photocatalytic system. - Abstract: In this work, a new plasmonic photocatalyst Ag/AgI/BiOI-rectorite was prepared via a cation exchange process. The photocatalyst had been characterized by X-ray powder diffraction (XRD), Raman spectra, nitrogen sorption (BET), field-emission scanning electron microscope (FE-SEM), X-ray photoelectron spectroscopy (XPS) and UV–vis diffuse reflectance spectroscopy (DRS). The photocatalytic activity, which was evaluated by degradation of rhodamine B (RhB) and bisphenol A (BPA) under visible light irradiation, was enhanced significantly by loading Ag/AgI/BiOI nanoparticles onto rectorite. The photogenerated holes and superoxide radical (·O{sub 2}{sup −}) were both formed as active species for the photocatalytic reactions under visible light irradiation. The existence of metallic Ag particles, which possess the surface plasmon resonance effect, acted as an indispensable role in the photocatalytic reaction.

  20. Effect of Zeolite Modification via Cationic Exchange Method on Mechanical, Thermal, and Morphological Properties of Ethylene Vinyl Acetate/Zeolite Composites

    Directory of Open Access Journals (Sweden)

    N. D. Zaharri

    2013-01-01

    Full Text Available In this research, organozeolite filled ethylene vinyl acetate (EVA composites were prepared in a melt-mixing process and followed by compression molding using hot press machine according to standard test specimen. Prior to mixing process, zeolite was modified via cationic exchange of alkylammonium ions. The effect of zeolite or organozeolite loading from 5 up to 25 volume percentages on the properties of EVA/zeolite composites was evaluated. A combination of Fourier Transform Infrared Radiation (FTIR and scanning electron microscopy (SEM coupled with energy dispersive X-ray (EDX analysis were done to characterize the resultant organoclay. Tensile test was performed in order to study the mechanical properties of the composites. EVA filled with organozeolite showed better tensile properties compared to EVA filled with unmodified zeolite, which might be an indication of enhanced dispersion of organophilic clay in the composites. Meanwhile, morphological study using SEM revealed the fibrillation effect of organozeolite. Besides, thermal properties of the composites were also characterized by using thermogravimetric analysis (TGA and differential scanning calorimetry (DSC. The results showed that the application of the cation exchange treatment increases both decomposition and melting temperature of EVA/zeolite composites.

  1. Cation exchange applications of synthetic tobermorite for the immobilization and solidification of cesium and strontium in cement matrix

    Indian Academy of Sciences (India)

    O P Shrivastava; Rashmi Shrivastava

    2000-12-01

    Immobilization and solidification of hazardous cations like Cs137 and Sr90 are required while handling the radioactive waste of nuclear power plants. Efforts are on to find a fail proof method of safe disposal of nuclear wastes. In this context, various materials like borosilicate glass, zeolites, cements and synthetic rocks have been tried by several workers. This communication deals with the synthesis, characterization, cesium uptake capacity and leaching behaviour of synthetic alumina-substituted calcium silicate hydroxy hydrate, which are close to that obtained for the natural mineral, 11 Å tobermorite. The synthetic mineral show cation selectivity for Cs+ in presence of 500–1000 times concentrated solutions of Na+ , K+ , Mg2+, Ca2+ , Ba2+ and Sr2+. Although the ordinary portland cement (OPC) which is often used in waste management operations alone holds negligible amounts of Cs+ and Sr2+, the addition of alumina-substituted tobermorite to OPC enhances the retention power of cement matrix by drastically lowering the leach rate of cations.

  2. Magnetic graphene - polystyrene sulfonic acid nano composite: A dispersive cation exchange sorbent for the enrichment of aminoalcohols and ethanolamines from environmental aqueous samples.

    Science.gov (United States)

    Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Dubey, D K; Pardasani, Deepak

    2015-12-04

    Present study aimed at graphene surface modification to achieve selective analyte binding in dispersive solid phase extraction. Magnetic graphene - polystyrene sulfonic acid (MG-PSS) cation exchange nano-composite was prepared by non-covalent wrapping method. Composite was characterized by FT-IR and zeta potential. Material exhibited good dispersion in water and high exchange capacity of 1.97±0.16mMg(-1). Prepared nano-sorbent was then exploited for the cation exchange extraction and gas chromatography mass spectrometric analysis of Chemical Weapons Convention relevant aminoalcohols and ethanolamines from aqueous samples. Extraction parameters such as sorbent amount, extraction time, desorption conditions and sample pH were optimized and effect of common matrix interferences such as polyethylene glycol and metal salts was also studied. Three milligram of sorbent per mL of sample with 20min of extraction time at room temperature afforded 70-81% recoveries of the selected analytes spiked at concentration level of 1μgmL(-1). Method showed good linearity in the studied range with r(2)≥0.993. The limits of detection and limits of quantification ranged from 23 to 54ngmL(-1) and 72 to 147ngmL(-1), respectively. The relative standard deviation for intra- and inter-day precision ranged from 4.6 to 10.2% and 7.4 to 14.8% respectively. Applicability of the method to different environmental samples as well as the proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons (OPCW) was also ascertained.

  3. Separation behavior of U(VI) and Th(IV) on a cation exchange column using 2,6-pyridine dicarboxylic acid as a complexing agent and its application for the rapid separation and determination of U and Th by ion chromatography.

    Science.gov (United States)

    Jeyakumar, Subbiah; Mishra, Vivekchandra Guruprasad; Das, Mrinal Kanti; Raut, Vaibhavi Vishwajeet; Sawant, Ramesh Mahadev; Ramakumar, Karanam Lakshminarayana

    2011-03-01

    The retention behavior of U and Th as their 2,6-pyridine dicarboxylic acid (PDCA) complexes on a cation exchange column was investigated under low pH conditions. Based on the observed retention characteristics, an ion chromatographic method for the rapid separation of uranium and thorium in isocratic elution mode using 0.08 mM PDCA and 0.24 M KNO(3) in 0.22 M HNO(3) as the eluent was developed. Both uranium and thorium were eluted as their PDCA complexes within 2 min, whereas the transition and lanthanide metal cations were eluted as an unresolved broad peak after thorium. Under the optimized conditions both U and Th have no interference either from alkali and alkaline earth elements up to a concentration ratio of 1:500 or from other elements up to 1:100. The detection limits (LOD) of U and Th were calculated as 0.04 and 0.06 ppm, respectively (S/N=3). The precision in the measurement of peak area of 0.5 ppm of both U and Th was better than 5% and a linear calibration in the concentration range of 0.25-25 ppm of U and Th was obtained. The method was successfully applied to determine U and Th in effluent water samples.

  4. Chromatographic separation of three monoclonal antibody variants using multicolumn countercurrent solvent gradient purification (MCSGP).

    Science.gov (United States)

    Müller-Späth, Thomas; Aumann, Lars; Melter, Lena; Ströhlein, Guido; Morbidelli, Massimo

    2008-08-15

    Multicolumn countercurrent solvent gradient purification (MCSGP) is a continuous chromatographic process developed in recent years (Aumann and Morbidelli, 2007a; Aumann et al., 2007) that is particularly suited for applications in the field of bioseparations. Like batch chromatography, MCSGP is suitable for three-fraction chromatographic separations and able to perform solvent gradients but it is superior in terms of solvent consumption, yield, purity, and productivity due to the countercurrent movement of the liquid and the solid phases. In this work, the MCSGP process is applied to the separation of three monoclonal antibody variants on a conventional preparative cation exchange resin. The experimental process performance was compared to simulations based on a lumped kinetic model. Yield and purity values of the target variant of 93%, respectively were obtained experimentally. The batch reference process was clearly outperformed by the MCSGP process.

  5. Investigations on Cationic Exchange Capacity and Unused Bed Zone according to operational conditions in a Fixed Bed Reactor for water lead removal by a natural zeolite

    Directory of Open Access Journals (Sweden)

    Barthélemy JP.

    2006-01-01

    Full Text Available In this study, attention has been focused on the behaviour of the Cationic Exchange Capacity (CEC and the Unused Bed Zone (UBZ, according to the operating parameters (bed length: L, column diameter: D, particle diameter: d and fl ow rate: Q in a Fixed Bed Reactor (FBR. The investigations are performed for a single-component study of lead on New Zealand clinoptilolite at 25 ± 1°C. The results show a constant operating CEC of 1.00 ± 0.015 meq.g-1 which is independent of the operational parameters listed above. The performance of the operations expressed as UBZ, shows an optimum for the ratio L/D (bed length and column diameter fi xed at 18.1, for Q = 2.9 BV.h-1 (bed volume per hour and particle diameter d = 0.38 mm (the ratio particle diameter on column diameter d/D at 0.057. This maximum performance is reached with the lowest UBZ value of 5.6% of the operating CEC. Overall interpretation drawn from the results according to UBZ shows that decreasing the particles size improves the performance of ion exchange process; as well as decreasing the fl ow rate. Nevertheless, the increase of L/D to a certain extent does not improve ion exchange performances.

  6. Synthesis of Strong Acid Cation Exchange Resin with High Exchange Capacity%高交换容量强酸型阳离子交换树脂的合成研究

    Institute of Scientific and Technical Information of China (English)

    罗旻; 赵兴

    2014-01-01

    Strong acid cation exchange resin has many important applications in most fields. Exchange capacity is an important parameter which influences the effect of the resin applied, the better performance of the resin due to its higher exchange capacity mostly. In this paper, the method of synthesis of strong acid cation exchange resin with high exchange capacity was discussed. Based on the influence of the pore-forming agent on the physical structure of the polymer, a small amount of the pore-forming agent was added to the monomer to modify the styrene-divinylbenzene copolymer which was then sulfonated to form the resin. The Na-type exchange capacity of 4.82 mmol/g (dried resin) of the gel type resin (the crosslinkage is 7%) with good mechanical strength was obtained while the experimental optimization was adopted.%强酸型阳离子交换树脂在许多领域有着重要用途。交换容量是影响树脂应用效果的重要参数,更高的交换容量往往赋予树脂更好的应用性能。本文探讨了高交换容量强酸型阳离子交换树脂的合成方法,结合致孔剂对聚合物内部物理结构的影响机理,采用在单体中加入少量致孔剂的方法得到改性的苯乙烯-二乙烯苯共聚物,再经磺化制备树脂。通过实验优化,得到了钠型交换容量为4.82 mmol/g(干树脂)的凝胶型树脂(交联度为7%),且机械强度好。

  7. Investigation of the swelling behavior of cationic exchange resins saturated with Na{sup +} ions in a C{sub 3}S paste

    Energy Technology Data Exchange (ETDEWEB)

    Lafond, E. [CEA, DEN, DTCD, SPDE, F-30207 Bagnols-sur-Cèze cedex (France); Cau Dit Coumes, C., E-mail: celine.cau-dit-coumes@cea.fr [CEA, DEN, DTCD, SPDE, F-30207 Bagnols-sur-Cèze cedex (France); Gauffinet, S. [UMR5209 Institut Carnot de Bourgogne, Université de Bourgogne Dijon, Faculté des Sciences Mirande, 9 Avenue Alain Savary, BP 47870, 21078 Dijon cedex (France); Chartier, D. [CEA, DEN, DTCD, SPDE, F-30207 Bagnols-sur-Cèze cedex (France); Le Bescop, P. [CEA, DEN, DPC, SECR, F-91192 Gif-sur-Yvette (France); Stefan, L. [AREVA, Back End Business Group, Dismantling & Services, 1 place Jean Millier, 92084 Paris La Défense (France); Nonat, A. [UMR5209 Institut Carnot de Bourgogne, Université de Bourgogne Dijon, Faculté des Sciences Mirande, 9 Avenue Alain Savary, BP 47870, 21078 Dijon cedex (France)

    2015-03-15

    Ion exchange resins (IERs) are widely used by the nuclear industry to decontaminate radioactive effluents. Spent products are usually encapsulated in cementitious materials. However, the solidified waste form can exhibit strong expansion, possibly leading to cracking, if the appropriate binder is not used. In this work, the interactions between cationic resins in the Na{sup +} form and tricalcium silicate are investigated during the early stages of hydration in order to gain a better understanding of the expansion process. It is shown that the IERs exhibit a transient swelling of small magnitude due to the decrease in the osmotic pressure of the external solution. This expansion, which occurs just after setting, is sufficient to damage the material which is poorly consolidated for several reasons: low degree of hydration, precipitation of poorly cohesive sodium-bearing C–S–H, and very heterogeneous microstructure with zones of high porosity.

  8. Zwitterionic and cationic bis(phosphine) platinum(II) complexes: structural, electronic, and mechanistic comparisons relevant to ligand exchange and benzene C-H activation processes.

    Science.gov (United States)

    Thomas, J Christopher; Peters, Jonas C

    2003-07-23

    Structurally similar but charge-differentiated platinum complexes have been prepared using the bidentate phosphine ligands [Ph(2)B(CH(2)PPh(2))(2)], ([Ph(2)BP(2)], [1]), Ph(2)Si(CH(2)PPh(2))(2), (Ph(2)SiP(2), 2), and H(2)C(CH(2)PPh(2))(2), (dppp, 3). The relative electronic impact of each ligand with respect to a coordinated metal center's electron-richness has been examined using comparative molybdenum and platinum model carbonyl and alkyl complexes. Complexes supported by anionic [1] are shown to be more electron-rich than those supported by 2 and 3. A study of the temperature and THF dependence of the rate of THF self-exchange between neutral, formally zwitterionic [Ph(2)BP(2)]Pt(Me)(THF) (13) and its cationic relative [(Ph(2)SiP(2))Pt(Me)(THF)][B(C(6)F(5))(4)] (14) demonstrates that different exchange mechanisms are operative for the two systems. Whereas cationic 14 displays THF-dependent, associative THF exchange in benzene, the mechanism of THF exchange for neutral 13 appears to be a THF independent, ligand-assisted process involving an anchimeric, eta(3)-binding mode of the [Ph(2)BP(2)] ligand. The methyl solvento species 13, 14, and [(dppp)Pt(Me)(THF)][B(C(6)F(5))(4)] (15), each undergo a C-H bond activation reaction with benzene that generates their corresponding phenyl solvento complexes [Ph(2)BP(2)]Pt(Ph)(THF) (16), [(Ph(2)SiP(2))Pt(Ph)(THF)][B(C(6)F(5))(4)] (17), and [(dppp)Pt(Ph)(THF)][B(C(6)F(5))(4)] (18). Examination of the kinetics of each C-H bond activation process shows that neutral 13 reacts faster than both of the cations 14 and 15. The magnitude of the primary kinetic isotope effect measured for the neutral versus the cationic systems also differs markedly (k(C(6)H(6))/k(C(6)D(6)): 13 = 1.26; 14 = 6.52; 15 approximately 6). THF inhibits the rate of the thermolysis reaction in all three cases. Extended thermolysis of 17 and 18 results in an aryl coupling process that produces the dicationic, biphenyl-bridged platinum dimers [[(Ph(2)SiP(2))Pt](2

  9. 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....... It is capable of separating and quantifying both C8-isomers of ergocornine, alpha-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61% +/- 10% with limits of detection from 0.2 to 1.1 mu g kg(-1). Twenty-four unknown rye flour samples from Danish mills contained on average 46 mu...... g kg(-1) with a maximum content of 234 mu g kg(-1). The most common ergot alkaloids were ergotamine and alpha-ergocryptine including their C8-isomers. A total of 54% of the ergot alkaloids were detected as C(8)-S isomers....

  10. Effect of temperature and pH value on cation exchange performance of a natural clay for selective (Cu2þ, Co2þ) removal:Equilibrium, sorption and kinetics

    Institute of Scientific and Technical Information of China (English)

    Ramzi Chalghaf; Walid Oueslati; Marwa Ammar; Hafsia Ben Rhaiem; Abdesslem Ben Haj Amara

    2013-01-01

    This work aims at investigating the strain effect, created by varying pH solution and continuous heating cycle, on the cation exchange process in the case of Na-rich montmorillonite sample in contact with bi-ionic solution with variable concentration, saturated respectively by Co2þ and Cu2þ cations. The ionic exchange process is characterized using XRD analysis obtained through the comparison of experimental XRD patterns with calculated ones, which allowed us to determine several structural parameters related to the nature, abundance, size, position and organization of exchangeable cation and water molecule in the interlamellar space along the cn axis. Indeed, the proposed theoretical models, for the stressed samples, show that the structure presents an interstratified hydration character and proves the coexistence of more than two ‘‘crystallite’’ specie in the structure. The perturbation types have an obvious effect on the selective exchange process for all stressed samples, where the interlayer space is characterized by the coexistence of more one exchangeable cation.

  11. Review of the thermal stability and cation exchange properties of the zeolite minerals clinoptilolite, mordenite, and analcime; applications to radioactive waste isolation in silicic tuff

    Energy Technology Data Exchange (ETDEWEB)

    Smyth, J.R.; Caporuscio, F.A.

    1981-06-01

    Silicic tuffs of the southern Great Basin and basalts of the Columbia River Plateau are under investigation as potential host rocks for high- and intermediate-level radioactive wastes. Nonwelded and partially welded tuffs may contain major amounts (> 50%) of the zeolite minerals clinoptilolite, mordenite, and analcime. Densely welded tuffs and some basalt flows may contain clinoptilolite as fracture filling that limits the permeability of these rocks. The cation exchange properties of these zeolite minerals allow them to pose a formidable natural barrier to the migration of cationic species of various radionuclides in aqueous solutions. However, these minerals are unstable at elevated temperatures and at low water-vapor pressures and may break down either by reversible dehydration or by irreversible mineralogical reactions. All the breakdown reactions occurring at increased temperature involve a net volume reduction and evolution of fluids. Thus, they may provide a pathway (shrinkage fractures) and a driving force (fluid pressure) for release of radionuclides to the biosphere. These reactions may be avoided by keeping zeolite-bearing horizons saturated with water and below about 85{sup 0}C. This may restrict allowable gross thermal loadings in waste repositories in volcanic rocks.

  12. PROPYLENE OLIGOMERIZATION CATALYZED BY HIGHLY ACIDIC CATION EXCHANGE RESIN%强酸性阳离子交换树脂催化丙烯齐聚

    Institute of Scientific and Technical Information of China (English)

    佟春雨; 陈群; 孙富安; 陈亮; 何明阳

    2012-01-01

    A catalyst of cation exchange resin was selected to catalyze propylene oligomerization. The relationship between resin properties and catalytic activities were studied and the optimal reaction conditions of the typical resin LC001 were investigated. The propylene oligomerization was catalyzed by cation resin LC001 with macroporous and high exchange capacity. The once through conversion of propylene kept at about 64.7%, and the selectivity of nonene and dodecene in liquid products were about 58% under the optimized conditions of reaction temperature 150℃, reaction pressure 4.0MPa and the LHSV 1.5h'\\ This catalyst displayed good stability, high activity and simple process. It showed a good prospect in industrial production.%筛选了可用于丙烯齐聚的阳离子交换树脂催化剂,研究了树脂性质与催化性能间的关系,并考察了自制LC001树脂催化丙烯齐聚的工艺条件.结果发现,采用大孔、高交换量的LC001树脂在150℃、4.0MPa、液时空速为1.5h-1条件下反应,丙烯单程转化率达到64.7%,C9和C12烯烃的选择性能达到58%.催化剂性能稳定,催化活性高,工艺流程简单,有很好的工业应用前景.

  13. A Generalized Adsorption Rate Model Based on the Limiting-Component Constraint in Ion-Exchange Chromatographic Separation for Multicomponent Systems

    DEFF Research Database (Denmark)

    In species exchange processes (e.g., ion-exchange chromatography column), conventional adsorption rate models describe mass transfer (or exchange) between phases, assuming the existence of a counterpart species. In contrast, the adsorption models may not be useful in an inert environment (or...... move with time. Hence, the moving active and inactive zones are mixed over the column length. If a conventional adsorption rate model is employed in the inactive zone, computational solutions show that such a model can lead to unphysical negative concentrations. This study aims to develop a model...

  14. Studies on the Thermodenaturation Behavior of Bacillus subtilis α-Amylase on Chromatographic Media

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    The thermodenaturation behavior of Bacillus subtilis α-amylase on some chromatographic media was studied by determining their adsorption parameters with frontal analysis. The experimental results show that on a RP-C18 reversed-phase medium, a Chelating Sepharose Fast-Flow chelated by Zn2+ affinity medium and a WCX-1 cation-exchange medium, a stable conformation of a-amylase molecule separately exists below or over 30℃; while on a PEG-400 hydrophobic medium and a modified PEG-400 medium, a stable conformation of α-amylase mole-cule separately exists below 40 and 30℃, and when the experimental temperatures are separately over 40 and 30℃,a drastically conformational change of α-amylase molecules can continuously take place. And by combining the in-trinsic fluorescence emission spectrum and thermal inactivation profile of α-amylase in free solution and on the PEG-400 and modified PEG-400 hydrophobic media, it can be concluded that in liquid chromatographic procedure,chromatographic media can induce the conformational change of a-amylase molecules and promote their ther-modenaturation; and in hydrophobic interaction chromatography, the higher the hydrophobicity of chromatographicmedium, the lower the conformational change temperature of a-amylase molecules on the chromatographic me-dium.

  15. A two-layer ONIOM study of thiophene cracking catalyzed by proton- and cation-exchanged FAU zeolite.

    Science.gov (United States)

    Sun, Yingxin; Mao, Xinfeng; Pei, Supeng

    2016-02-01

    A two-layer ONIOM study on the hydrodesulfurization mechanism of thiophene in H-FAU and M-FAU (M = Li(+), Na(+), and K(+)) has been carried out. The calculated results reveal that in H-FAU, for a unimolecular mechanism, the rate-determining step is hydrogenation of alkoxide intermediate. The assistance of H2O and H2S molecules does not reduce the difficulty of the C-S bond cracking step more effectively. A bimolecular hydrodesulfurization mechanism is more favorable due to the lower activation barriers. The rate-determining step is the formation of 2-methylthiophene, not the C-S bond cracking of thiophene. Moreover, the ring opening of thiophene is much easier to occur than the desulfurization step. A careful analysis of energetics indicates that H2S, propene, and methyl thiophene are the major products for the hydrodesulfurization process of thiophene over H-FAU zeolite, in good agreement with experimental findings. In M-FAU zeolites, both unimolecular and bimolecular cracking processes are difficult to occur because of the high energy barriers. Compared to the case on H-FAU, the metal cations on M-FAU increase the difficulty of occurrence of bimolecular polymerization and subsequent C-S bond cracking steps. Graphical abstract Hydrodesulfurization process of thiophene can take place in H-FAU zeolite. Two different mechanisms, unimolecular and bimolecular ones, have been proposed and evaluated in detail. The bimolecular mechanism is more favorable due to lower activation barrier as described in the picture above. Our calculated data indicate that H2S, propene, and methylthiophene are the major products, in good agreement with experimental observations. The effect of metal cations on the reaction mechanism is also investigated in this work.

  16. Cation exchanged and impregnated Ti-pillared clays for selective catalytic reduction of NO{sub x} by propylene

    Energy Technology Data Exchange (ETDEWEB)

    Valverde, J.L.; De Lucas, A.; Sanchez, P.; Dorado, F.; Romero, A. [Facultad de Quimicas, Departamento de Ingenieria Quimica, Universidad Castilla-La Mancha, 13004 Ciudad Real (Spain)

    2003-06-20

    Ti-pillared interlayer clay (PILC)-based catalysts ion exchanged with Cu, Ni and Fe were prepared and used for the selective catalytic reduction of NO{sub x} using propylene as the reducing agent. The influence of the metal loading in the SCR activity was studied. Likewise, catalytic activity of Cu-ion exchanged samples was compared to that of Cu-ones. In both cases, the catalytic activity increased with increasing metal loading, reaching a maximum of NO{sub x} conversion, and then decreased at higher loading. The maximum of NO{sub x} conversion was achieved in each set of catalysts for the samples NiTi-3.4, FeTi-8.0 and CuTi-7.4. Ti-PILCs-ion exchanged with Cu was the most active catalyst for the SCR of NO{sub x} by propylene. H{sub 2}-TPR results showed that Ni{sup 2+} in Ti-PILC-based catalysts was harder to reduce than Cu{sup 2+} in the same material. It was observed that, as the Cu content is increased, CuO and isolated Cu{sup 2+} species became easier to reduce in ion exchanged samples. Likewise, it was also noted that the relative H{sub 2} consumption decreased with the Cu content, due to a lower accessibility of H{sub 2} to the metal. It can be verified a correlation between NO{sub x} conversion and the H{sub 2} consumption for the Cu{sup 2+} -> Cu{sup +} reduction process, reaching the maximum for the sample CuTi-7.4. Finally, it was observed that the presence of 10% water in the feed inhibited the SCR of NO activity of this catalyst. However, this effect was completely reversible following the removal of water from the gas stream.

  17. Selective sorption of lead, cadmium and zinc ions by a polymeric cation exchanger containing nano-Zr(HPO3S)2.

    Science.gov (United States)

    Zhang, Qingrui; Pan, Bingcai; Pan, Bingjun; Zhang, Weiming; Jia, Kun; Zhang, Quanxing

    2008-06-01

    A novel polymeric hybrid sorbent, namely ZrPS-001, was fabricated for enhanced sorption of heavy metal ions by impregnating Zr(HPO3S)2 (i.e., ZrPS) nanoparticles within a porous polymeric cation exchanger D-001. The immobilized negatively charged groups bound to the polymeric matrix D-001 would result in preconcentration and permeation enhancement of target metal ions prior to sequestration, and ZrPS nanoparticles are expected to sequester heavy metals selectively through an ion-exchange process. Highly effective sequestration of lead, cadmium, and zinc ions from aqueous solution can be achieved by ZrPS-001 even in the presence of competing calcium ion at concentration several orders of magnitude greater than the target species. The exhausted ZrPS-001 beads are amenable to regeneration with 6 M HCI solution for repeated use without any significant capacity loss. Fixed-bed column treatment of simulated waters containing heavy metals at high or trace levels was also performed. The content of heavy metals in treated effluent approached or met the WHO drinking water standard.

  18. Preparation and characterization of electrically conducting polypyrrole Sn(IV phosphate cation-exchanger and its application as Mn(II ion selective membrane electrode

    Directory of Open Access Journals (Sweden)

    A.A. Khan

    2011-10-01

    Full Text Available Polypyrrole Sn(IV phosphate, an organic–inorganic composite cation-exchanger was synthesized via sol-gel mixing of an organic polymer, polypyrrole, into the matrices of the inorganic precipitate of Sn(IV phosphate. The physico-chemical properties of the material were determined using Atomic Absorption Spectrometry (AAS, CHN elemental analysis (inductively coupled plasma mass spectrometry, ICP-MS, UV–VIS spectrophotometry, FTIR (Fourier Transform Infra-Red, SEM (Scanning Electron Microscopy, TGA–DTA (Thermogravimetric Analysis–Differential Thermal Analysis, and XRD (X-ray diffraction. Ion-exchange behavior was observed to characterize the material. On the basis of distribution studies, the material was found to be highly selective for toxic heavy metal ion Mn2+. Due to its selective nature, the material was used as an electroactive component for the construction of an ion-selective membrane electrode. The proposed electrode shows fairly good discrimination of mercury ion over several other inorganic ions. The analytical utility of this electrode was established by employing it as an indicator electrode in electrometric titrations for Mn(II in water.

  19. 阳离子树脂净化铂族金属溶液的研究%Purification of Platinum Group Metals Solution by Cation Exchange

    Institute of Scientific and Technical Information of China (English)

    毕向光; 余建民; 杨金富; 贺洪亮; 李权

    2015-01-01

    研究了阳离子交换树脂净化含大量贱金属的铂族金属溶液的工艺条件,结果表明,在pH=1~1.5时001×7阳离子交换树脂吸附贱金属的次序为:Ni>Cu>Co>Fe;Fe、Ni、Co、Cu的穿透容量分别为(g/kg):0.13,1.25,0.42,0.87;饱和容量分别为(g/kg):0.32,6.65,2.33,4.72,合计为14.02 g/kg;贱金属的分离效率主要取决于贵贱金属浓度及交换柱的数量;吸附在树脂上的贱金属极易被6 mol/L HCl洗脱,所有贱金属的最大洗脱均发生在洗脱液体积与床体积之比为1.0/1.7处,当洗脱液体积为床体积的2.0倍时贱金属被完全洗脱。实验结果为离子交换分离贱金属净化铂族金属溶液的工业化应用提供了强有力的理论依据。%The platimum group metals ( PGMs) solution containing a large amount of base metals purified with cation exchange resin had been investigated. The results showed that the adsorption of base metals by 001 × 7 cation ion exchange resin at pH=1~1.5 was in the order of Ni>Cu>Co>Fe. From the tests, the breakthrough capacities ( g/kg) of Fe, Ni, Co and Cu were 0.13, 1.25, 0.42 and 0.87, respectively, while the saturated capacities ( g/kg) were 0.32, 6.65, 2.33 and 4.72, respectively and 14.02 g/kg in total. It is shown that the separation efficiency of the base metals depends largely on the concentrations of the precious and base metals, as well as the number of exchange columns. The base metals absorbed on the resin could be easily eluted by adding HCl solution at the amount of 6 mol/L, with the elution reaching the maximum as the eluent volume and bed volume at the ratio of 1.0/1.7 and completely finished as the eluent volume being 2. 0 times the bed volume. The experimental results can definitely provide a theoretical basis favorably for the industrial application of PGMs solution purified by cation exchange resin.

  20. Use of Cation Exchange Resins for Production of U{sub 3}O{sub 8} Suitable for the Al-U{sub 3}O{sub 8} Powder Metallurgy Process

    Energy Technology Data Exchange (ETDEWEB)

    Mosley, W.C.

    2001-09-17

    This report describes the production of U{sub 3}O{sub 8} powders from three types of cation exchange resins: Dowex 50W, a strong acid, sulfonate resin; AG MP-50, a macroporous form of sulfonate resin; and Bio-Rex 70, a weak acid, carboxylic resin.

  1. EXCHANGE

    Energy Technology Data Exchange (ETDEWEB)

    Boltz, J.C. (ed.)

    1992-09-01

    EXCHANGE is published monthly by the Idaho National Engineering Laboratory (INEL), a multidisciplinary facility operated for the US Department of Energy (DOE). The purpose of EXCHANGE is to inform computer users about about recent changes and innovations in both the mainframe and personal computer environments and how these changes can affect work being performed at DOE facilities.

  2. Squalamine, a novel cationic steroid, specifically inhibits the brush-border Na+/H+ exchanger isoform NHE3.

    Science.gov (United States)

    Akhter, S; Nath, S K; Tse, C M; Williams, J; Zasloff, M; Donowitz, M

    1999-01-01

    Squalamine, an endogenous molecule found in the liver and other tissues of Squalus acanthias, has antibiotic properties and causes changes in endothelial cell shape. The latter suggested that its potential targets might include transport proteins that control cell volume or cell shape. The effect of purified squalamine was examined on cloned Na+/H+ exchanger isoforms NHE1, NHE2, and NHE3 stably transfected in PS120 fibroblasts. Squalamine (1-h pretreatment) decreased the maximal velocity of rabbit NHE3 in a concentration-dependent manner (13, 47, and 57% inhibition with 3, 5, and 7 micrograms/ml, respectively) and also increased K'[H+]i. Squalamine did not affect rabbit NHE1 or NHE2 function. The inhibitory effect of squalamine was 1) time dependent, with no effect of immediate addition and maximum effect with 1 h of exposure, and 2) fully reversible. Squalamine pretreatment of the ileum for 60 min inhibited brush-border membrane vesicle Na+/H+ activity by 51%. Further investigation into the mechanism of squalamine's effects showed that squalamine required the COOH-terminal 76 amino acids of NHE3. Squalamine had no cytotoxic effect at the concentrations studied, as indicated by monitoring lactate dehydrogenase release. These results indicate that squalamine 1) is a specific inhibitor of the brush-border NHE isoform NHE3 and not NHE1 or NHE2, 2) acts in a nontoxic and fully reversible manner, and 3) has a delayed effect, indicating that it may influence brush-border Na+/H+ exchanger function indirectly, through an intracellular signaling pathway or by acting as an intracellular modulator.

  3. Catalysis in a Cage: Condition-Dependent Speciation and Dynamics of Exchanged Cu Cations in SSZ-13 Zeolites.

    Science.gov (United States)

    Paolucci, Christopher; Parekh, Atish A; Khurana, Ishant; Di Iorio, John R; Li, Hui; Albarracin Caballero, Jonatan D; Shih, Arthur J; Anggara, Trunojoyo; Delgass, W Nicholas; Miller, Jeffrey T; Ribeiro, Fabio H; Gounder, Rajamani; Schneider, William F

    2016-05-11

    The relationships among the macroscopic compositional parameters of a Cu-exchanged SSZ-13 zeolite catalyst, the types and numbers of Cu active sites, and activity for the selective catalytic reduction (SCR) of NOx with NH3 are established through experimental interrogation and computational analysis of materials across the catalyst composition space. Density functional theory, stochastic models, and experimental characterizations demonstrate that within the synthesis protocols applied here and across Si:Al ratios, the volumetric density of six-membered-rings (6MR) containing two Al (2Al sites) is consistent with a random Al siting in the SSZ-13 lattice subject to Löwenstein's rule. Further, exchanged Cu(II) ions first populate these 2Al sites before populating remaining unpaired, or 1Al, sites as Cu(II)OH. These sites are distinguished and enumerated ex situ through vibrational and X-ray absorption spectroscopies (XAS) and chemical titrations. In situ and operando XAS follow Cu oxidation state and coordination environment as a function of environmental conditions including low-temperature (473 K) SCR catalysis and are rationalized through first-principles thermodynamics and ab initio molecular dynamics. Experiment and theory together reveal that the Cu sites respond sensitively to exposure conditions, and in particular that Cu species are solvated and mobilized by NH3 under SCR conditions. While Cu sites are spectroscopically and chemically distinct away from these conditions, they exhibit similar turnover rates, apparent activation energies and apparent reaction orders at the SCR conditions, even on zeolite frameworks other than SSZ13.

  4. Standardization of method for determining glycosylated hemoglobin (Hb A1c by cation exchange high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Marina Venzon Antunes

    2009-12-01

    Full Text Available Hemoblobin A1c is the most important parameter for the monitoring of metabolic control of patients with diabetes mellitus. The purpose of this study was to adapt the Mono S method to a conventional HPLC system, allowing highly selective HbA1c determination without the acquisition of kits or the use of dedicated systems The results obtained were compared to the Tinaquant® immune turbidimetric method and the Bio-Rad Variant® chromatographic method. The developed method presented intra-study precision (C.V. % of 1.39-3.65 and inter-study precision (C.V. % of 2.80-3.02%. The determination coefficients among methods were: HPLC Mono S x Tinaquant®: r²: 0.9856 (n=60 and HPLC Mono S x HPLC Bio-Rad Variant®: r²: 0.9806 (n=16. A conversion equation between HPLC Mono S and Bio-Rad Variant® was calculated allowing yielding comparable and interchangeable values. The HPLC Mono-S is a precise, low-cost method which yields similar values to the Bio-Rad Variant® method on conventional HPLC equipment.A hemoglobina A1c é o parâmetro laboratorial mais importante no monitoramento do controle metabólico de pacientes portadores de diabetes melito. Dentre as metodologias existentes para a quantificação desta fração de hemoglobina, a cromatografia líquida de alta eficiência (CLAE baseada em troca catiônica apresenta a melhor precisão, sendo o método de escolha. O objetivo deste trabalho foi adaptar o método Mono S a um sistema de CLAE convencional permitindo a disponibilidade da determinação altamente seletiva de Hb A1c sem a aquisição de kits e comparar os resultados obtidos com o método imunoturbidimétrico Tinaquant® (Roche® e com o método de cromatografia líquida Bio-Rad Variant®. O método desenvolvido apresentou precisão intra-ensaio de 1,39-3,65% e inter-ensaio de 2,80-3,02%. Os coeficientes de determinação entre os métodos foram: CLAE Mono S x Tinaquant®: r² = 0,9856 (n=60 e CLAE Mono S x Bio-Rad Variant®: r² = 0,9806 (n=16

  5. L—PROLINE—FUNCTIONALIZED POLYSTYRENE WITH 1—METHYLDECYLENE SPACER AS A CHIRAL STATIONARY PHASE FOR LIGAND—EXCHANGE CHROMATOGRAPHIC RESOLUTION OF AMINO ACID RECEMATES

    Institute of Scientific and Technical Information of China (English)

    MaJianbiao; ChenLi; 等

    1995-01-01

    The L-proline-functionalized polystyrene with 1-methyldecylene spacer was synthesized from 2% divinylbenzene-crosslinked polystyrene gel via 10-bromo-1-methyldecyl polystyrene intermediate.After complexed with copper(Ⅱ) ion,the polymer with L-proline ligand was used as the chiral stationary phase (CSP) for ligand exchange chromatography of amino acid racemates.The results showed that the CSP possessed powerful enantioselectivity and all racemates of the fifteen tried amino acids were completely separated.

  6. 2-Acrylamido-2-methyl-1-propanesulfonic Acid Grafted Poly(vinylidene fluoride-co-hexafluoropropylene)-Based Acid-/Oxidative-Resistant Cation Exchange for Membrane Electrolysis.

    Science.gov (United States)

    Pandey, Ravi P; Das, Arindam K; Shahi, Vinod K

    2015-12-30

    For developing acid-/oxidative-resistant aliphatic-polymer-based cation-exchange membrane (CEM), macromolecular modification of poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-co-HFP) was carried out by controlled chemical grafting of 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS). To introduce the unsaturation suitable for chemical grafting, dehydrofluorination of commercially available PVDF-co-HFP was achieved under alkaline medium. Sulfonated copolymer (SCP) was prepared by the free radical copolymerization of dehydofluorinated PVDF-co-HFP (DHPVDF-co-HFP) and AMPS in the presence of free radical initiator. Prepared SCP-based CEMs were analyzed for their morphological characteristics, ion-exchange capacity (IEC), water uptake, conductivity, and stabilities (mechanical, chemical, and thermal) in comparison with state-of-art Nafion117 membrane. High bound water content avoids the membrane dehydration, and most optimal (SCP-1.33) membrane exhibited about ∼2.5-fold high bound water content in comparison with that of Nafion117 membrane. Bunsen reaction of iodine-sulfur (I-S) was successfully performed by direct-contact-mode membrane electrolysis in a two-compartment electrolytic cell using different SCP membranes. High current efficiency (83-99%) confirmed absence of any side reaction and 328.05 kJ mol-H2(-1) energy was required for to produce 1 mol of H2 by electrolytic cell with SCP-1.33 membrane. In spite of low conductivity for reported SCP membrane in comparison with that of Nafion117 membrane, SCP-1.33 membrane was assessed as suitable candidate for electrolysis because of its low-cost nature and excellent stabilities in highly acidic environment may be due to partial fluorinated segments in the membrane structure.

  7. Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS.

    Science.gov (United States)

    Pyo, Jae Sung

    2016-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX) cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ) of propofol was 25 ng/mL. The validated method exhibited good linearity (R (2) = 0.9989) with accuracy and precision -5.8%~11.7% and 3.7%~11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes.

  8. Iminodiacetic acid functionalized cation exchange resin for adsorptive removal of Cr(VI), Cd(II), Ni(II) and Pb(II) from their aqueous solutions.

    Science.gov (United States)

    Misra, R K; Jain, S K; Khatri, P K

    2011-01-30

    Iminodiacetic acid functionality has been introduced on styrene-divinyl benzene co-polymeric beads and characterized by FT-IR in order to develop weak acid based cation exchange resin. This resin was evaluated for the removal of different heavy metal ions namely Cd(II), Cr(VI), Ni(II) and Pb(II) from their aqueous solutions. The results showed greater affinity of resin towards Cr(VI) for which 99.7% removal achieved in optimal conditions following the order Ni(II)>Pb(II)>Cd(II) with 65%, 59% and 28% removal. Experiments were also directed towards kinetic studies of adsorption and found to follow first order reversible kinetic model with the overall rate constants 0.3250, 0.2393, 0.4290 and 0.2968 for Cr(VI), Ni(II), Pb(II) and Cd(II) removal respectively. Detailed studies of Cr(VI) removal has been carried out to see the effect of pH, resin dose and metal ion concentration on adsorption and concluded that complexation enhanced the chromium removal efficacy of resin drastically, which is strongly pH dependent. The findings were also supported by the comparison of FT-IR spectra of neat resin with the chromium-adsorbed resin.

  9. Characteristics of Lipoprotein Peak x Eluted from a Column with the Eluent of High-magnesium Ion Concentration in Lipoprotein Analysis Using the Cation-exchange Chromatography

    Directory of Open Access Journals (Sweden)

    Yuji Hirowatari

    2005-01-01

    Full Text Available The new lipoprotein analysis method using a cation-exchange chromatography, which contains a sulfopropyl-ligand column and two magnesium ion-containing eluents was previously reported. This method can separate serum lipoproteins on the column gel with a magnesium ion concentration gradient and high-density lipoprotein (HDL, low-density lipoprotein (LDL, very-low-density lipoprotein (VLDL and an unspecified lipoprotein peak are eluted in order from the column. We have now characterized the unspecified lipoproteins, designated peak x, which is last eluted from the column with the eluent of high-magnesium ion concentration. The peak x was small size chylomicron fraction with a part of VLDL. Furthermore, the cholesterol values in the peak x were significantly correlated with remnant-like particle (RLP-cholesterol values. The peak x separated from a hyperlipidemic patient included apolipoprotein B-100, B-48, E, A-1 and Cs (C-I, C-II, C-III and its composition of free cholesterol, cholesteryl esters, triglyceride (TG and phospholipids in total lipids were 6, 15, 66 and 13%, respectively. These results suggest that a major part of the lipoprotein peak X may be composed of remnants of chylomicron and VLDL, but it remains to be elucidated.

  10. Analysis of amphetamine-type stimulants and their metabolites in plasma, urine and bile by liquid chromatography with a strong cation-exchange column-tandem mass spectrometry.

    Science.gov (United States)

    Kuwayama, Kenji; Inoue, Hiroyuki; Kanamori, Tatsuyuki; Tsujikawa, Kenji; Miyaguchi, Hajime; Iwata, Yuko T; Miyauchi, Seiji; Kamo, Naoki

    2008-05-01

    The aim of this work was to develop and validate a method for analysing amphetamine-type stimulants (ATSs) and their metabolites in plasma, urine and bile by liquid chromatography with a strong cation-exchange column-tandem mass spectrometry, and to apply it to the pharmacokinetic study of ATSs. 3,4-Methylenedioxymethamphetamine, methamphetamine, ketamine and their main metabolites, 4-hydroxy-3-methoxymethamphetamine, 3,4-methylenedioxyamphetamine, p-hydroxymethamphetamine, amphetamine and norketamine, were simultaneously quantified by the new method (50-5000 ng/ml). The coefficients of variation and the percent deviations for the eight compounds were in the range of 0.2 to 5.3% and -9.4 to +12.8%, respectively. The recoveries were over 90% in all biological samples tested. This method was effective for the separation and the identification of ATSs and their main metabolites having amine moieties in plasma, urine and bile, and was applicable to pharmacokinetic analysis of methamphetamine, ketamine and their main metabolites in biological samples. This analytical method should be useful for the pharmacokinetic analysis of ATSs.

  11. Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS

    Directory of Open Access Journals (Sweden)

    Jae Sung Pyo

    2016-01-01

    Full Text Available A gas chromatography-mass spectrometry (GC-MS method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ of propofol was 25 ng/mL. The validated method exhibited good linearity (R2=0.9989 with accuracy and precision −5.8%~11.7% and 3.7%~11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes.

  12. Quantitative determination of corticosteroids in bovine milk using mixed-mode polymeric strong cation exchange solid-phase extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tölgyesi, Adám; Tölgyesi, László; Sharma, Virender K; Sohn, Mary; Fekete, Jeno

    2010-12-01

    A new method was developed to identify and quantify corticosteroids (prednisolone, methylprednisone, flumetasone, dexamethasone, and methylprednisolone) in raw bovine milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS) utilizing mixed-mode polymeric strong cation exchange and reversed-phase (MCX) solid-phase extraction (SPE) to reduce ion effects in a multimode ion (MMI) source. The main advantage of this method over other commonly used methods includes the use of a single SPE cartridge with a low volume for sample preparation and fast separation on the HPLC system with reduced ion suppression. This study is the first to report the determination of methylprednisone, a metabolite of methylprednisolone, in bovine milk. This method was validated in accordance with the European Union (EU) Commission Decision 2002/657/EC. The recoveries vary between 90% and 105%. The within-laboratory reproducibility (precision) is less than 30%. The decision limits and detection capabilities were calculated along with LODs, which ranged from 0.02 to 0.07 microg/kg. The method was further enhanced by its successful adaptation to other LC-MS/MS systems equipped with the newly developed ion source, Agilent Jet Stream (AJS). After optimization of the AJS ion source and MS parameters, even lower LOD values were achieved (0.001-0.006 microg/kg) for the corticosteroids. Analytical results obtained with the AJS were characterized by an enhanced area response and similar noise level comparable to those obtained with conventional orthogonal atmospheric ionization (API).

  13. Double-peak elution profile of a monoclonal antibody in cation exchange chromatography is caused by histidine-protonation-based charge variants.

    Science.gov (United States)

    Luo, Haibin; Cao, Mingyan; Newell, Kelcy; Afdahl, Christopher; Wang, Jihong; Wang, William K; Li, Yuling

    2015-12-11

    We have systemically investigated unusual elution behaviors of an IgG4 (mAb A) in cation exchange chromatography (CEX). This mAb A exhibited two elution peaks under certain conditions when being purified by several strong CEX columns. When either of the two peaks was isolated and re-injected on the same column, the similar pattern was observed again during elution. The protein distribution between the two peaks could be altered by NaCl concentration in the feed, or NaCl concentration in wash buffer, or elution pH, suggesting two pH-associated strong-and-weak binding configurations. The protein distributions under different pH values showed good correlation with protonated/un-protonated fractions of a histidine residue. These results suggest that the double-peak elution profile associates with histidine-protonation-based charge variants. By conducting pepsin digestion, amino-acid specific chemical modifications, peptide mapping, and measuring the effects of elution residence time, a histidine in the variable fragment (Fab) was identified to be the root cause. Besides double-peak pattern, mAb A can also exhibit peak-shouldering or single elution peak on different CEX resins, reflecting different resins' resolving capability on protonated/un-protonated forms. This work characterizes a novel cause for unusual elution behaviors in CEX and also provides alternative avenues of purification development for mAbs with similar behaviors.

  14. Isolation of cross-linked peptides by diagonal strong cation exchange chromatography for protein complex topology studies by peptide fragment fingerprinting from large sequence databases.

    Science.gov (United States)

    Buncherd, Hansuk; Roseboom, Winfried; Ghavim, Behrad; Du, Weina; de Koning, Leo J; de Koster, Chris G; de Jong, Luitzen

    2014-06-27

    Knowledge of spatial proximity of amino acid residues obtained by chemical cross-linking and mass spectrometric analysis provides information about protein folding, protein-protein interactions and topology of macromolecular assemblies. We show that the use of bis(succinimidyl)-3-azidomethyl glutarate as a cross-linker provides a solution for two major analytical problems of cross-link mapping by peptide fragment fingerprinting (PFF) from complex sequence databases, i.e., low abundance of protease-generated target peptides and lack of knowledge of the masses of linked peptides. Tris(carboxyethyl)phosphine (TCEP) reduces the azido group in cross-linked peptides to an amine group in competition with cleavage of an amide bond formed in the cross-link reaction. TCEP-induced reaction products were separated by diagonal strong cation exchange (SCX) from unmodified peptides. The relation between the sum of the masses of the cleavage products and the mass of the parent cross-linked peptide enables determination of the masses of candidate linked peptides. By reversed phase LC-MS/MS analysis of secondary SCX fractions, we identified several intraprotein and interprotein cross-links in a HeLa cell nuclear extract, aided by software tools supporting PFF from the entire human sequence database. The data provide new information about interacting protein domains, among others from assemblies involved in splicing.

  15. Liquid Anion Exchange Chromatographic Extraction and Separation of Platinum(IV with n-Octylaniline as a Metallurgical Reagent: Analysis of Real Samples

    Directory of Open Access Journals (Sweden)

    Ashwini P. Gaikwad

    2013-01-01

    Full Text Available A simple and selective method was developed for the determination of platinum(IV with n-octylaniline in toluene. In present study, the use of n-octylaniline in toluene for the extraction of platinum(IV from ascorbate media was carried out. The effect of various parameters, such as pH, equilibrium time, extractant concentration, and organic solvent on the extraction has been discussed. The back extraction of platinum(IV has been performed. On the basis of slope analysis, the composition of the extracted species was determined as [RR′NH2+ Pt(Succinate2−](org. The interfering effects of various cations and anions were also studied, and the selectivity of the method is enhanced by using suitable masking agents. The proposed method is rapid, reproducible and successfully applied for the determination of platinum(IV in binary and synthetic mixtures. The separation of pt(IV from other associated metals has been studied. Comparison of the results with those obtained using an atomic absorption spectrophotometer also tested the validity of the method.

  16. Water-Chemistry Evolution and Modeling of Radionuclide Sorption and Cation Exchange during Inundation of Frenchman Flat Playa

    Energy Technology Data Exchange (ETDEWEB)

    Hershey, Ronald; Cablk, Mary; LeFebre, Karen; Fenstermaker, Lynn; Decker, David

    2013-08-01

    dioxide and calcite; dissolution of sodium chloride, gypsum, and composite volcanic glass; and precipitation of composite clay and quartz represented changes in water as it disappeared from the playa. This modeling provided an understanding of the water-soil geochemical environment, which was then used to evaluate the potential mobility of residual radionuclides into the playa soils by water. Because there is no information on the chemical forms of anthropogenic radionuclides in Frenchman Flat playa soil, it was assumed that soil radionuclides go into solution when the playa is inundated. In mobility modeling, a select group of radionuclides were allowed to sorb onto, or exchange with, playa soil minerals to evaluate the likelihood that the radionuclides would be removed from water during playa inundation. Radionuclide mobility modeling suggested that there would be minimal sorption or exchange of several important radionuclides (uranium, cesium, and technetium) with playa minerals such that they may be mobile in water when the playa is inundated and could infiltrate into the subsurface. Mobility modeling also showed that plutonium may be much less mobile because of sorption onto calcite, but the amount of reactive surface area of playa soil calcite is highly uncertain. Plutonium is also known to sorb onto colloidal particles suspended in water, suspended colloidal particles will move with the water, providing a mechanism to redistribute plutonium when Frenchman Flat playa is inundated. Water chemistry, stable isotopes, and geochemical modeling showed that residual radionuclides in Frenchman Flat playa soils could be mobilized in water when the playa is inundated with precipitation. Also, there is potential for these radionuclides to infiltrate into the subsurface with water. As a result of the information obtained both during this study and the conclusions drawn from it, additional data collection, investigation, and modeling are recommended. Specifically: sampling the

  17. Evaluation of selectivity in homologous multimodal chromatographic systems using in silico designed antibody fragment libraries.

    Science.gov (United States)

    Karkov, Hanne Sophie; Woo, James; Krogh, Berit Olsen; Ahmadian, Haleh; Cramer, Steven M

    2015-12-24

    This study describes the in silico design, surface property analyses, production and chromatographic evaluations of a diverse set of antibody Fab fragment variants. Based on previous findings, we hypothesized that the complementarity-determining regions (CDRs) constitute important binding sites for multimodal chromatographic ligands. Given that antibodies are highly diversified molecules and in particular the CDRs, we set out to examine the generality of this result. For this purpose, four different Fab fragments with different CDRs and/or framework regions of the variable domains were identified and related variants were designed in silico. The four Fab variant libraries were subsequently generated by site-directed mutagenesis and produced by recombinant expression and affinity purification to enable examination of their chromatographic retention behavior. The effects of geometric re-arrangement of the functional moieties on the multimodal resin ligands were also investigated with respect to Fab variant retention profiles by comparing two commercially available multimodal cation-exchange ligands, Capto MMC and Nuvia cPrime, and two novel multimodal ligand prototypes. Interestingly, the chromatographic data demonstrated distinct selectivity trends between the four Fab variant libraries. For three of the Fab libraries, the CDR regions appeared as major binding sites for all multimodal ligands. In contrast, the fourth Fab library displayed a distinctly different chromatographic behavior, where Nuvia cPrime and related multimodal ligand prototypes provided markedly improved selectivity over Capto MMC. Clearly, the results illustrate that the discriminating power of multimodal ligands differs between different Fab fragments. The results are promising indications that multimodal chromatography using the appropriate multimodal ligands can be employed in downstream bioprocessing for challenging selective separation of product related variants.

  18. High-pH anion-exchange chromatographic analysis of phosphorylated compounds: application to isolation and characterization of nonpeptide mycobacterial antigens.

    Science.gov (United States)

    Poquet, Y; Constant, P; Peyrat, M A; Poupot, R; Halary, F; Bonneville, M; Fournié, J J

    1996-12-01

    A rapid and sensitive high-pH anion-exchange chromatography (HPAEC) method for the separation and quantification of phosphorylated antigens in mycobacterial extracts has been developed. This method provides the separation of mono-, di-, or triphosphonucleotides and of various other phosphorylated molecules. Dual detection by conductimetry and UV absorption downstream of a chemical suppressor constitute nondegradative and highly sensitive tools for the physical detection and the quantification of phosphorylated compounds in biological samples. The lower limit of accurate quantification is around 1 nmol per sample. This method was used for the separation of several phosphorylated antigens activating human gamma delta T lymphocytes from semipurified mycobacterial fractions. Their quantification revealed that the minimal concentration activating a gamma delta T cell clone is between 1 and 5 nM. This approach can be used for more general preparative purposes with samples where minute amounts of biologically active phosphoanions are analyzed.

  19. Prepared polymethacrylate-based monoliths for the separation of cations by non-suppressed capillary ion chromatography.

    Science.gov (United States)

    Li, Jing; Zhu, Yan

    2014-01-01

    This paper describes a novel analytical system for non-suppressed capillary ion chromatography. Methacrylate monolithic columns were prepared from silanized fused-silica capillaries of 320 µm i.d. by in situ polymerization of glycidyl methacrylate and ethylene dimethacrylate in the presence of 1,4-butanediol, 1-propanol and water as the porogen solvents. The introduction of cation-exchange sites was achieved by sulfonating the matrix with sodium sulfite to produce total cation-exchange capacities in the range of 45-105 μequiv/mL for a 25 cm column. The conditions (concentrations of sodium sulfite solution, reacting time and modified flow rate) of sulfonation were optimized. The hydrodynamic and chromatographic performances were estimated. Coupled with a conductivity detector, a capillary ion chromatography system was set up with the prepared column. Finally, the resultant column was used for the separations of five common univalent cations (Li(+), Na(+), NH4(+), K(+) and Cs(+)) using methanesulfonic acid as the eluent and four divalent cations (Mg(2+), Ca(2+), Sr(2+) and Ba(2+)) by non-suppressed capillary ion chromatography; the chromatographic parameters were further researched.

  20. Chromatographic separation of fructose from date syrup.

    Science.gov (United States)

    Al Eid, Salah M

    2006-01-01

    The objective of this study is to provide a process for separating fructose from a mixture of sugars containing essentially fructose and glucose, obtained from date palm fruits. The extraction procedure of date syrup from fresh dates gave a yield of 86.5% solids after vacuum drying. A process for separating fructose from an aqueous solution of date syrup involved adding the date syrup solutions (20, 30 and 40% by weight) to a chromatographic column filled with Dowex polystyrene strong cation exchange gel matrix resin Ca2 + and divinylbenzene, a functional group, sulfonic acid, particle size 320 microm, with a flow rate of 0.025 and 0.05 bed volume/min, under 30 and 70 degrees C column temperature. After the date sugar solution batch, a calculated quantity of water was added to the column. Glucose was retained by the resin more weakly than fructose and proceeded faster into the water batch flowing ahead. Three fractions were collected: a glucose-rich fraction, a return fraction, and a fructose-rich fraction. The return fraction is based on when the peaks of fructose and glucose were reached, which could be determined by means of an analyzer (polarimeter) based on the property of glucose and fructose solutions to turn the polarization level of polarized light. A high yield of fructose is obtained at 70 degrees C column temperature with a flow rate of 0.025 bed volume/min and date syrup solution containing 40% sugar concentration. The low recovery by weight obtained using date syrup solutions having a sugar concentration of 20 and 30%, encourages the use of a concentration of 40%. However, with the 40% date syrup supply the average concentrations of glucose and fructose in the return fractions were more than 40%, which can be used for diluting the thick date syrup solution extracted from dates.

  1. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...... and dimethylarsinate and the cations arsenobetaine, trimethylarsine oxide, arsenocholine and the tetramethylarsonium ion. Hexahydroxyantimonate(III) was co-chromatographed with the arsenic anions but detected at m/z 121 and used as an internal standard for their qualitative analysis. Arsenite was prone to oxidation...... to arsenate in urine but was stable after at least 4-fold dilution of the urine with water. Arsenite was unstable in both urine samples and standard mixtures when diluted with the basic (pH 10.3) mobile phase used for anion chromatography. This could not be prevented by adding ascorbic acid as antioxidant...

  2. New reversed phase-high performance liquid chromatographic method for selective separation of yttrium from all rare earth elements employing nitrilotriacetate complexes in anion exchange mode.

    Science.gov (United States)

    Dybczyński, Rajmund S; Kulisa, Krzysztof; Pyszynska, Marta; Bojanowska-Czajka, Anna

    2015-03-20

    Separation of Y from other rare earth elements (REE) is difficult because of similarity of its ionic radius to ionic radii of Tb, Dy and Ho. In the new RP-HPLC system with C18 column, tetra-n-butyl ammonium hydroxide (TBAOH) as an ion interaction reagent (IIR), nitrilotriacetic acid (NTA) as a complexing agent at pH=2.8-3.5, and post column derivatization with Arsenazo III, yttrium is eluted in the region of light REE, between Nd and Sm and is base line separated from Nd and Sm and even from promethium. Simple model employing literature data on complex formation of REE with NTA and based on anion exchange mechanism was developed to foresee the order of elution of individual REE. The model correctly predicted that lanthanides up to Tb will be eluted in the order of increasing Atomic Number (At.No.) but all heavier REE will show smaller retention factors than Tb. Concurrent UV/VIS detection at 658nm and the use of radioactive tracers together with γ-ray spectrometric measurements made possible to establish an unique elution order of elution of REE: La, Ce, Pr, Nd, Pm, Y, Sm, Er, Ho, Tm, Yb, Eu, Lu, Dy+Gd, Tb, Sc. The real place of Y however, in this elution series differs from that predicted by the model (Y between Sm and Eu). The method described in this work enables selective separation of Y from La, Ce, Pr, Nd, Pm, Sm and all heavier REE treated as a group.

  3. Preparation of a novel weak cation exchange/hydrophobic interaction chromatography dual-function polymer-based stationary phase for protein separation using "thiol-ene click chemistry".

    Science.gov (United States)

    Yang, Fan; Bai, Quan; Zhao, Kailou; Gao, Dong; Tian, Lei

    2015-02-01

    A novel dual-function mixed-mode stationary phase based on poly(glycidyl methacrylate-co-ethylene dimethacrylate) microspheres was synthesized by thiol-ene click chemistry and characterized by infrared spectroscopy and elemental analysis. The new system displays both hydrophobic interaction chromatography (HIC) character in a high salt concentration mobile phase, and weak cation exchange (WCX) chromatography character in a low salt concentration mobile phase. It can be used to separate proteins in both ion-exchange chromatography (IEC) mode and HIC mode. The resolution and selectivity of the stationary phase were evaluated in both HIC mode and IEC mode using protein standards. In comparison with the conventional WCX and HIC columns, the results were satisfactory and acceptable. Protein mass and bioactivity recoveries of more than 96% can be achieved in both HIC mode and IEC mode using this column. The results indicate that the novel dual-function mixed-mode column in many cases can replace the use of two individual WCX and HIC columns. In addition, the effects on protein separation of different ligand structures in the dual-function stationary phase and the pH of the mobile phase used were also investigated in detail. The results show that electrostatic interaction of the ligand with proteins must match the hydrophobicity of the ligand, which is an important factor to prepare the dual-function stationary phase. On the basis of this dual-function mixed-mode chromatography column, a new two-dimensional liquid chromatography technology with a single column system was also developed in this study, and was used to renature and purify recombinant human interferon-γ from inclusion bodies. The mass recovery, purity, and specific bioactivity obtained for the purified recombinant human interferon-γ were 87.2%, 92.4%, and 2.8 × 10(7) IU/mg, respectively, in IEC mode, and 83.4%, 95.2%, and 4.3 × 10(7) IU/mg, respectively, in HIC mode. The results indicate that the

  4. Synthesis of cyclohexyl acetate by catalytic action of cation exchange resin%阳离子交换树脂催化合成乙酸环己酯

    Institute of Scientific and Technical Information of China (English)

    董森; 彭胜; 郭学华

    2012-01-01

    Cyclohexyl acetate was synthesized by cyclohexene and acetic acid as starting materials with polystyrene sulfonate cation exchange resin as catalyst. Effects of reaction temperature,reaction time,dosage of catalyst and molar ratio of acetic acid to cyclohexene on the reaction yield were investigated. Results showed that the optimum conditions were identified as follows; amount of cyclohexene 0. 1 mol, molar ratio of acetic acid to cyclohexene 4: 1 .dosage of catalyst 0. 96 g,reaction temperature 90 ℃ ,reaction time 5 h. Under these conditions,the yield of cyclohexyl acetate reaches 83.2%. The catalyst can be used for 5 times without significant yield declining.%以磺化苯乙烯阳离子交换树脂为催化剂,催化环己烯和乙酸反应合成乙酸环己酯,考察了反应温度、反应时间、催化剂用量和原料配比对反应的影响.结果表明,较适宜的反应条件为:环己烯用量为0.1 mol,酸烯摩尔比为4∶1,催化剂用量为0.96g,反应温度为90℃,反应时间为5h.在此条件下酯收率为83.2%,催化剂使用5次仍保持较高活性.

  5. Monoclonal antibody heterogeneity analysis and deamidation monitoring with high-performance cation-exchange chromatofocusing using simple, two component buffer systems.

    Science.gov (United States)

    Kang, Xuezhen; Kutzko, Joseph P; Hayes, Michael L; Frey, Douglas D

    2013-03-29

    The use of either a polyampholyte buffer or a simple buffer system for the high-performance cation-exchange chromatofocusing of monoclonal antibodies is demonstrated for the case where the pH gradient is produced entirely inside the column and with no external mixing of buffers. The simple buffer system used was composed of two buffering species, one which becomes adsorbed onto the column packing and one which does not adsorb, together with an adsorbed ion that does not participate in acid-base equilibrium. The method which employs the simple buffer system is capable of producing a gradual pH gradient in the neutral to acidic pH range that can be adjusted by proper selection of the starting and ending pH values for the gradient as well as the buffering species concentration, pKa, and molecular size. By using this approach, variants of representative monoclonal antibodies with isoelectric points of 7.0 or less were separated with high resolution so that the approach can serve as a complementary alternative to isoelectric focusing for characterizing a monoclonal antibody based on differences in the isoelectric points of the variants present. Because the simple buffer system used eliminates the use of polyampholytes, the method is suitable for antibody heterogeneity analysis coupled with mass spectrometry. The method can also be used at the preparative scale to collect highly purified isoelectric variants of an antibody for further study. To illustrate this, a single isoelectric point variant of a monoclonal antibody was collected and used for a stability study under forced deamidation conditions.

  6. High-purity isolation of anthocyanins mixtures from fruits and vegetables--a novel solid-phase extraction method using mixed mode cation-exchange chromatography.

    Science.gov (United States)

    He, Jian; Giusti, M Monica

    2011-11-04

    Research on biological activity of anthocyanins requires the availability of high purity materials. However, current methods to isolate anthocyanins or anthocyanin mixtures are tedious and expensive or insufficient for complete isolation. We applied a novel cation-exchange/reversed-phase combination solid-phase extraction (SPE) technique, and optimized the use of water/organic buffer mobile phases to selectively separate anthocyanins. Crude extracts of various representative anthocyanin sources were purified with this technique and compared to 3 commonly used SPE techniques: C(18), HLB, and LH-20. Purified anthocyanin fractions were analyzed with high performance liquid chromatography (HPLC) coupled to photodiode array (PDA) and mass spectrometry (MS) detectors and by Fourier transform infrared (FT-IR) spectroscopy. The UV-visible chromatograms quantitatively demonstrated that our novel technique achieved significantly higher (Panthocyanin purity than the C(18) cartridge, the next best method, for 11 of the 12 anthocyanin sources tested. Among them, eight were purified to greater than 99% purity (based on UV-visible chromatograms). The new method efficiently removed non-anthocyanin phenolics. MS and FT-IR results semi-quantitatively confirmed extensive reduction of impurities. Due to strong ionic interaction, our sorbent capacity was superior to others, resulting in the highest throughput and least use of organic solvents. This new methodology for isolation of anthocyanin mixtures drastically increased purity and efficiency while maintaining excellent recovery rate and low cost. The availability of high purity anthocyanin mixtures will facilitate anthocyanin studies and promote the application of anthocyanins in the food and nutraceutical industries.

  7. Variability of Cation-Exchange Capacity (CEC of Fen Peats in Vertical Profiles from Eastern and Central Poland in Relation to Function of Peatlands as Natural Geological Barriers

    Directory of Open Access Journals (Sweden)

    Rydelek Paweł

    2016-12-01

    Full Text Available An analysis of cation-exchange capacity(CEC variability of peats is presented in vertical pro files from eastern and central Po land. CEC values were com pared with ash con tent (Ac, pH and CaCO3 content. Eight peatlands were selected for re search in the fol lowingareas: War saw Plateau (2 objects, Siedlce Plateau (2 objects, Lubartów Plateau (2 objects, Nałęczów Table land (1 object and Dobrohusk Depression (1 object. The peatlands represented a fen peat type of similar botanic compositions of sediments, but they differed in the area, peat thickness and drain age conditions. Characteristic regular i ties in CEC variability were noted in the peatlands and there were three types of CEC variability in vertical pro files. Carbonate peats (types 1 and 2 had the high est pH and definitely the high est values of CEC. In vertical pro files, there was also a zonation, but the regularities similar to non-carbonate peats were not observed. Different distribution of phys i cal and chem i cal parameters were establishedin vertical pro files in partly drained peatlands (with a muck layer on top with non-carbonate peats (type 3 and there were three distinct zones in vertical pro files, with different Ac and CEC. Determination of the vertical CEC variability and other phys i cal and chem i cal parameters in peatlands made it possible to distinguish zones with potentially most beneficial isolation conditions.

  8. Online coupling of hydrophilic interaction/strong cation exchange/reversed-phase liquid chromatography with porous graphitic carbon liquid chromatography for simultaneous proteomics and N-glycomics analysis.

    Science.gov (United States)

    Zhao, Yun; Law, Henry C H; Zhang, Zaijun; Lam, Herman C; Quan, Quan; Li, Guohui; Chu, Ivan K

    2015-10-09

    In this study we developed a fully automated three-dimensional (3D) liquid chromatography methodology-comprising hydrophilic interaction separation as the first dimension, strong cation exchange fractionation as the second dimension, and low-pH reversed-phase (RP) separation as the third dimension-in conjunction downstream with additional complementary porous graphitic carbon separation, to capture non-retained hydrophilic analytes, for both shotgun proteomics and N-glycomics analyses. The performance of the 3D system alone was benchmarked through the analysis of the total lysate of Saccharomyces cerevisiae, leading to improved hydrophilic peptide coverage, from which we identified 19% and 24% more proteins and peptides, respectively, relative to those identified from a two-dimensional hydrophilic interaction liquid chromatography and low-pH RP chromatography (HILIC-RP) system over the same mass spectrometric acquisition time; consequently, the 3D platform also provided enhanced proteome and protein coverage. When we applied the integrated technology to analyses of the total lysate of primary cerebellar granule neurons, we characterized a total of 2201 proteins and 16,937 unique peptides for this primary cell line, providing one of its most comprehensive datasets. Our new integrated technology also exhibited excellent performance in the first N-glycomics analysis of cynomolgus monkey plasma; we successfully identified 122 proposed N-glycans and 135 N-glycosylation sites from 122 N-glycoproteins, and confirmed the presence of 38 N-glycolylneuraminic acid-containing N-glycans, a rare occurrence in human plasma, through tandem mass spectrometry for the first time.

  9. Retention of PWR primary coolant trace elements by cation exchange resins during cold shutdown with oxygenation: modelling and experimental results for silver behavior; Retention des elements traces du fluide primaire des REP par les resines echangeuses de cations lors des mises en arret a froid avec oxygenation: modelisation et resultats experimentaux relatifs au comportement de l'argent

    Energy Technology Data Exchange (ETDEWEB)

    Elain, L.; Doury-Berthod, M. [CEA Saclay, INSTN, Institut National des Sciences et Techniques Nucleaires, 91 - Gif-sur-Yvette (France); Genin, J.B. [CEA Cadarache, Dir. de l' Energie Nucleaire (DEN), 13 - Saint-Paul-lez-Durance (France); Berger, M. [Electricite de France (EDF/SEPTEN), 69 - Villeurbanne (France)

    2004-07-01

    In order to minimize the radiochemical impact of the corrosion products on the operation of Pressurized Water Reactors, on-line purification of the primary coolant is carried out. The purification system arranged on the Chemical and Volume Control System is made up of mechanical filters and demineralizers packed with a mixed bed of cation and anion exchange resins. This paper proposes an update on the retention of primary coolant trace elements by the cation exchange resins of the demineralizers during cold shutdowns with oxygenation. The study is first of all devoted to the description of the concentration profiles of the various cation constituents which settle in the demineralizer during purification after oxygenation. For a number of trace elements, localized enrichment zones at the Li{sup +}/Ni(Il) exchange zone are expected to appear in the column. The case of silver is afterwards discussed in detail. Thermodynamic modelling shows that the theoretical retention volume of the metallic element and its degree of enrichment in the column are dependent on the basic composition of the primary coolant and the specific characteristics of the demineralizer cation exchanger. At the Ag{sup +} ion concentration expected in the reactor coolant after oxygenation (between 10{sup -8} mol.L{sup -1} and 10{sup -6} mol.L{sup -1}), the breakthrough of silver should be near-simultaneous with that of nickel. The experimental results, obtained in the laboratory and with a 'Mini-CVCS' pilot instrumentation recently used during the cold shutdown of Tricastin Unit 2,900 MWe PWR NPP, confirm the validity of these theoretical forecasts and enable new hypotheses to be advanced for explaining silver release from a demineralizer. (authors)

  10. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Science.gov (United States)

    2010-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  11. 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.

  12. 阳离子交换树脂催化水解大豆糖蜜的研究%Hydrolysis of soy molasses catalyzed by cation exchange resin

    Institute of Scientific and Technical Information of China (English)

    郭紫光; 张永忠

    2011-01-01

    Strong acid styrene cation exchange resin was used to catalyze the hydrolysis of soy molasses.Through single factor and orthogonal experiments, the best conditions were determined as follows: ratio of liquid to solid 3: 1, time 120 min, temperature 60 ℃, concentration of substrate 0.2 g/mL. After hydrolysis under the optimum conditions, the ratio of reducing sugar to total sugar was 0.91, reducing sugar yield was 36.85% and reducing sugar content reached 368.46 mg/g, which was 4. 4 times higher than that before hydrolysis ( 83.93 mg/g). When the molasses was hydrolyzed at the optimal conditions, the reducing sugar yield of the resin catalysis method was almost the same with that of the acid catalysis method, but the resin method avoided the high temperature and low pH, and the resin method had the advantages of easy operation and less wastewater emissions.%采用强酸性苯乙烯系阳离子交换树脂催化水解大豆糖蜜.通过单因素及正交试验得到优化条件为:水解时间120 min,水解温度60℃,液固比3:1,底物质量浓度0.2 g/mL.水解后还原糖与总糖比率达到0.91,还原糖得率为36.85%,还原糖含量达到368.46 mg/g,比水解前的83.93 mg/g提高了3.4倍.与传统酸催化法对比得知,分别在最优条件下水解大豆糖蜜,还原糖得率相差无几,但树脂法避免了高温,pH低,操作简便,废水排放量减少.

  13. Effects of Land Use Practices on the Organic Carbon Content, Cation Exchange Capacity and Aggregate Stability of Soils in the Catchment Zones

    Directory of Open Access Journals (Sweden)

    Mosayeb Heshmati

    2011-01-01

    Full Text Available Problem statement: Land use practice leads to changes in the physico-chemical properties of soils, such as Soil Organic Carbon (SOC, Cation Exchange Capacity (CEC and Soil Aggregate Stability (SAS that cause soil erosion. Approach: Merek catchment, Iran suffers from land degradation due to poor land use practice. A study was carried out with the objectives: (i to determine soil nutrient status in different agro-ecological zones in Merek catchment; and (ii to evaluate the influence of land use practices on SOC, CEC and SAS. Results: It was found that soil texture was silty and clay, while soil reaction was alkaline (pH was 7.75. The respective amount of carbonates was 32 and 36% in the top-soil and sub-soil respectively, indicating high level of alkalinity in the soils of the study area. The mean SAS of the surface soil layer for agriculture, rangeland and forest was 53, 61 and 64%, respectively with its mean in the topsoil of agriculture is significantly lower (P≤0.05 than the other zones. SOC level in the agriculture, rangeland and forest were 1.35, 1.56, 2.14 % in the topsoil and 1.03, 1.33 and 1.45%, in the subsoil of the respective areas. The results of t-test and ANOVA analyses showed that SOC means are significantly different from each other within soil depth and among agro-ecological zones. The CEC in the agriculture, rangeland and forest areas were 25.8, 24.6 and 35.1 cmolckg-1 for the top-soil and 31.1, 26.8 and 26.9 cmolckg-1 in the sub-soil, respectively. All the above changes are due to the negative effects of agricultural activities. Conclusion: Improper tillage practice (up-down the slope, conversion of the rangeland and forest to rain-fed areas, crop residue burning, over grazing and forest clearance contribute to reduction in SOC and SAS in the Merek catchment, Iran.

  14. Multi-cycle recovery of lactoferrin and lactoperoxidase from crude whey using fimbriated high-capacity magnetic cation exchangers and a novel "rotor-stator" high-gradient magnetic separator.

    Science.gov (United States)

    Brown, Geoffrey N; Müller, Christine; Theodosiou, Eirini; Franzreb, Matthias; Thomas, Owen R T

    2013-06-01

    Cerium (IV) initiated "graft-from" polymerization reactions were employed to convert M-PVA magnetic particles into polyacrylic acid-fimbriated magnetic cation exchange supports displaying ultra-high binding capacity for basic target proteins. The modifications, which were performed at 25 mg and 2.5 g scales, delivered maximum binding capacities (Qmax ) for hen egg white lysozyme in excess of 320 mg g(-1) , combined with sub-micromolar dissociation constants (0.45-0.69 µm) and "tightness of binding" values greater than 49 L g(-1) . Two batches of polyacrylic acid-fimbriated magnetic cation exchangers were combined to form a 5 g pooled batch exhibiting Qmax values for lysozyme, lactoferrin, and lactoperoxidase of 404, 585, and 685 mg g(-1) , respectively. These magnetic cation exchangers were subsequently employed together with a newly designed "rotor-stator" type HGMF rig, in five sequential cycles of recovery of lactoferrin and lactoperoxidase from 2 L batches of a crude sweet bovine whey feedstock. Lactoferrin purification performance was observed to remain relatively constant from one HGMF cycle to the next over the five operating cycles, with yields between 40% and 49% combined with purification and concentration factors of 37- to 46-fold and 1.3- to 1.6-fold, respectively. The far superior multi-cycle HGMF performance seen here compared to that observed in our earlier studies can be directly attributed to the combined use of improved high capacity adsorbents and superior particle resuspension afforded by the new "rotor-stator" HGMS design.

  15. The elution of erbium from a cation exchanger bed by means of the N-hydroxyethyl-ethylene-diamine triacetic acid; Mecanismo de la elucion del erbio en un cambiador cationico con el acido n-hidroxietil-etilen-diamono-triacetico

    Energy Technology Data Exchange (ETDEWEB)

    Amer Amezaga, S.

    1963-07-01

    A physicochemical study of the phenomena resulting when erbium is eluted from a cation-exchanger bed at a steady by means of the N-hydroxyethyl-ethylene-diamine-triacetic acid (HEDTA) is made. Two different retaining beds are used, a hydrogen bed, in which no ammonium passes through, and a zinc bed, which leaks ammonium ion. Good agreement between experimental and calculated values by using the equations deduced for the concentrations of the main species has been achieved, with errors around 1-2% in most of the experiments. (Author) 69 refs.

  16. Simple setup for gas-phase H/D exchange mass spectrometry coupled to electron transfer dissociation and ion mobility for analysis of polypeptide structure on a liquid chromatographic time scale.

    Science.gov (United States)

    Mistarz, Ulrik H; Brown, Jeffery M; Haselmann, Kim F; Rand, Kasper D

    2014-12-01

    Gas-phase hydrogen/deuterium exchange (HDX) is a fast and sensitive, yet unharnessed analytical approach for providing information on the structural properties of biomolecules, in a complementary manner to mass analysis. Here, we describe a simple setup for ND3-mediated millisecond gas-phase HDX inside a mass spectrometer immediately after ESI (gas-phase HDX-MS) and show utility for studying the primary and higher-order structure of peptides and proteins. HDX was achieved by passing N2-gas through a container filled with aqueous deuterated ammonia reagent (ND3/D2O) and admitting the saturated gas immediately upstream or downstream of the primary skimmer cone. The approach was implemented on three commercially available mass spectrometers and required no or minor fully reversible reconfiguration of gas-inlets of the ion source. Results from gas-phase HDX-MS of peptides using the aqueous ND3/D2O as HDX reagent indicate that labeling is facilitated exclusively through gaseous ND3, yielding similar results to the infusion of purified ND3-gas, while circumventing the complications associated with the use of hazardous purified gases. Comparison of the solution-phase- and gas-phase deuterium uptake of Leu-Enkephalin and Glu-Fibrinopeptide B, confirmed that this gas-phase HDX-MS approach allows for labeling of sites (heteroatom-bound non-amide hydrogens located on side-chains, N-terminus and C-terminus) not accessed by classical solution-phase HDX-MS. The simple setup is compatible with liquid chromatography and a chip-based automated nanoESI interface, allowing for online gas-phase HDX-MS analysis of peptides and proteins separated on a liquid chromatographic time scale at increased throughput. Furthermore, online gas-phase HDX-MS could be performed in tandem with ion mobility separation or electron transfer dissociation, thus enabling multiple orthogonal analyses of the structural properties of peptides and proteins in a single automated LC-MS workflow.

  17. Cation exchange capacity of an oxisol amended with an effluent from domestic sewage treatment Capacidade de troca catiônica de um latossolo tratado com efluente de tratamento de esgoto doméstico

    Directory of Open Access Journals (Sweden)

    Adriel Ferreira da Fonseca

    2005-12-01

    Full Text Available The addition of Na-rich anthropogenic residues to tropical soils has stimulated the scientific community to study the role of sodium in both the soil solution and the exchange complex. In this study, several different methods were used to calculate the concentration of exchangeable and soluble cations and this data was then used to establish correlations between the level of these cations and both the accumulation of various elements and the dry weight of maize grown in a greenhouse under different conditions. In the closed environments of the pots, the most suitable method for calculating the effective cation exchange capacity (ECEC was the cation exchange capacity calculated by cations removed with barium chloride solution (CEC S. Then again, the actual cation exchange capacity (CEC A should be measured by using Mg adsorption to prevent ionic force from influencing electric charges. A strong positive correlation was obtained between the concentrations of Na in the 1:2 soil:water extracts and the accumulation of Na in the maize plants, indicating saline or double acid extractors are not needed when monitoring the Na concentration only.A disposição de resíduos antropogênicos ricos em sódio nos solos tropicais tem despertado o interesse da comunidade científica em estudar a participação deste elemento no complexo de troca, bem como na solução no solo. Objetivou-se neste trabalho estabelecer correlações entre as concentrações de cátions trocáveis e de cátions solúveis, obtidos por diferentes métodos, com o acúmulo de elementos e com a massa seca no milho. O experimento foi conduzido em casa de vegetação, sob diferentes condições. Para experimentos em ambiente fechado (vasos, o método mais indicado para o cálculo da capacidade de troca catiônica efetiva (CTCe é a capacidade de troca catiônica calculada a partir dos cátions removidos com solução de cloreto de bário. Ainda, a capacidade de troca catiônica atual deve

  18. Chromatographic and Related Reactors.

    Science.gov (United States)

    1988-01-07

    special information about effects of surface heteroge- neity in the methanation reaction. Studies of an efficient multicolumn assembly for measuring...of organic basic catalysts such as pyridine and 4-methylpicoline. It was demonstrated that the chromatographic reactor gave special information about...Programmed Reaction to obtain special information about surface heterogeneity in the methanation reaction. Advantages of stopped flow over steady state

  19. Thermodynamics and Extra-thermodynamics of Bacillus subtilis α-Amylase in Some Chromatographic Systems

    Institute of Scientific and Technical Information of China (English)

    BIAN,Liujiao; WANG,Xiaohua; YANG,Xiaoyan; LIU,Li; CHEN,Chao

    2009-01-01

    The thermodynamics and extra-thermodynamics of Bacillus subtilis a-amylase in five kinds of chromatographic systems were studied by determining their adsorption equilibrium constant KsL,enthalpy change,entropy change,free energy change and compensation temperature under different temperature areas.The results showed that on anRP.C18 reversed-phase medium,a Zn-chelated Sepharose fast-flow affinity medium and a WCX-l cation-exchange medium,their In KsL separately linearly changed with the reciprocal of absolute temperatures under two different temperature ranges of 13-30 and 30-50℃:and on PEG-400 and modified PEG-400 hydrophobic media,their ln KsL separately linearly decreased with the reciprocal of absolute temperatures under the temperature areas of 13-40 and 13-30℃.while when the temperatures were separately over 40 and 30℃,they violently decreased with the reciprocal of absolute temperatures.Through studying the relations among the enthalpy change,entropy change.free energy change and the conformational change of a-amylase under the different temperature areas,it was found that on the RP-C18 reversed-phase medium and Zn-chelated Sepharose fast-flow affinity medium under the temperature range of 30-50℃and on the WCX-l cation-exchange medium under the temperature range of 13-30℃.their adsorption procedures were driven by both the enthalpy change and the entropy change;while on the Zn-chelated Sepharose fast-flow affinity medium under the temperature range of 13-30℃.on the WCX-1cation.exchange medium under the temperature range of 30-50℃and on the PEG-400 and modified PEG-400 hydrophobic media under the temperature range of 13-65℃.their adsorption procedures were driven only by the entropy change.Finally, by comparing the compensation temperatures of a-amylase in these chromatographic sys-terns each other,it Was further found that their enthalpy changes could be compensated only with their entropy changes rising from their conformational change.

  20. Cation diffusion in the natural zeolite clinoptilolite

    Energy Technology Data Exchange (ETDEWEB)

    Dyer, A.; White, K.J. [Science Research Institute, Chemistry Division, Cockcroft Building, University of Salford, Salford (United Kingdom)

    1999-12-14

    The natural zeolite clinoptilolite is mined commercially in many parts of the world. It is a selective exchanger for the ammonium cation and this has prompted its use in waste water treatment, swimming pools and in fish farming. It is also used to scavenge radioisotopes in nuclear waste clean-up. Further potential uses for clinoptilolite are in soil amendment and remediation. The work described herein provides thermodynamic data on cation exchange processes in clinoptilolite involving the NH{sub 4}, Na, K, Ca, and Mg cations. The data includes estimates of interdiffusion coefficients together with free energies, entropies and energies of activation for the cation exchanges studied. Suggestions are made as to the mechanisms of cation-exchanges involved.

  1. Chromatographic speciation of Cr(III)-species, inter-species equilibrium isotope fractionation and improved chemical purification strategies for high-precision isotope analysis.

    Science.gov (United States)

    Larsen, K K; Wielandt, D; Schiller, M; Bizzarro, M

    2016-04-22

    Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of these species can result in incomplete Cr recovery during chromatographic purification. Because of large mass-dependent inter-species isotope fractionation, incomplete recovery can affect the accuracy of high-precision Cr isotope analysis. Here, we demonstrate widely differing cation distribution coefficients of Cr(III)-species (Cr(3+), CrCl(2+) and CrCl2(+)) with equilibrium mass-dependent isotope fractionation spanning a range of ∼1‰/amu and consistent with theory. The heaviest isotopes partition into Cr(3+), intermediates in CrCl(2+) and the lightest in CrCl2(+)/CrCl3°. Thus, for a typical reported loss of ∼25% Cr (in the form of Cr(3+)) through chromatographic purification, this translates into 185 ppm/amu offset in the stable Cr isotope ratio of the residual sample. Depending on the validity of the mass-bias correction during isotope analysis, this further results in artificial mass-independent effects in the mass-bias corrected (53)Cr/(52)Cr (μ(53)Cr* of 5.2 ppm) and (54)Cr/(52)Cr (μ(54)Cr* of 13.5 ppm) components used to infer chronometric and nucleosynthetic information in meteorites. To mitigate these fractionation effects, we developed strategic chemical sample pre-treatment procedures that ensure high and reproducible Cr recovery. This is achieved either through 1) effective promotion of Cr(3+) by >5 days exposure to HNO3H2O2 solutions at room temperature, resulting in >∼98% Cr recovery for most types of sample matrices tested using a cationic chromatographic retention strategy, or 2) formation of Cr(III)-Cl complexes through exposure to concentrated HCl at high temperature (>120 °C) for several hours, resulting in >97.5% Cr recovery using a

  2. The influence of hydrogen- and cation-underpotential deposition on oxide-mediated Pt dissolution in proton-exchange membrane fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seokkoo [Texas Materials Institute and Center for Electrochemistry, University of Texas at Austin, University Station, C2200 Austin, TX 78712-0292 (United States); Meyers, Jeremy P., E-mail: jeremypmeyers@austin.utexas.edu [Texas Materials Institute and Center for Electrochemistry, University of Texas at Austin, University Station, C2200 Austin, TX 78712-0292 (United States)

    2011-10-01

    Highlights: > Pt dissolution has a maximum value around E{sub L} = 0.5-0.6 V vs. RHE at CV, SW experiments. > The addition of Zn cation (5 mM) in acid solution increase Pt dissolution rate on the region E{sub L} < 0.2 V at E{sub H} = 1.6 V. > Pt dissolution is accelerated by convection flow at over 1.2 V vs. RHE. > The amount of Pt dissolution during Pt oxide reduction reaction is measured by RRDE experiment. - Abstract: In order to fully understand the influence of a lower potential limit on platinum dissolution and the likely mechanism for mass and surface-area loss under potential cycling conditions, the dissolution of a Pt catalyst in a N{sub 2}-saturated 0.5 M H{sub 2}SO{sub 4} solution was examined using an electrochemical quartz nanobalance (EQCN) flow cell, a rotating ring-disk electrode (RRDE) and inductively coupled plasma mass spectroscopy (ICP-MS). Due to the observation that cycling to a lower potential limit, which coincides with the hydrogen under-potential (H{sub UPD}) region, results in a decrease in the dissolution rate, cations capable of interfering with the hydrogen UPD process (Zn{sup 2+}, Li{sup +}, Na{sup +}, K{sup +}, and Cd{sup 2+}) were introduced to the solution. Larger rates of mass loss were observed in the presence of these cations during the cycling process in the UPD region, despite apparently negligible effects on the behavior with more positive lower potential limits or on oxide formation and stripping. It was found that the quantity of soluble Pt species produced during the electrochemical reduction of PtO{sub 2} was proportional to the charge associated with oxide stripping at the disk electrode during the RRDE experiment.

  3. Continuous melting and ion chromatographic analyses of ice cores.

    Science.gov (United States)

    Huber, T M; Schwikowski, M; Gäggele, H W

    2001-06-22

    A new method for determining concentrations of organic and inorganic ions in ice cores by continuous melting and contemporaneous ion chromatographic analyses was developed. A subcore is melted on a melting device and the meltwater produced is collected in two parallel sample loops and then analyzed simultaneously by two ion chromatographs, one for anions and one for cations. For most of the analyzed species, lower or equal blank values were achieved with the continuous melting and analysis technique compared to the conventional analysis. Comparison of the continuous melting and ion chromatographic analysis with the conventional analysis of a real ice core segment showed good agreement in concentration profiles and total amounts of ionic species. Thus, the newly developed method is well suited for ice core analysis and has the advantages of lower ice consumption, less time-consuming sample preparation and lower risk of contamination.

  4. Detachable strong cation exchange monolith, integrated with capillary zone electrophoresis and coupled with pH gradient elution, produces improved sensitivity and numbers of peptide identifications during bottom-up analysis of complex proteomes.

    Science.gov (United States)

    Zhang, Zhenbin; Yan, Xiaojing; Sun, Liangliang; Zhu, Guijie; Dovichi, Norman J

    2015-04-21

    A detachable sulfonate-silica hybrid strong cation-exchange monolith was synthesized in a fused silica capillary, and used for solid phase extraction with online pH gradient elution during capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) proteomic analysis. Tryptic digests were prepared in 50 mM formic acid and loaded onto the strong cation-exchange monolith. Fractions were eluted using a series of buffers with lower concentration but higher pH values than the 50 mM formic acid background electrolyte. This combination of elution and background electrolytes results in both sample stacking and formation of a dynamic pH junction and allows use of relatively large elution buffer volumes while maintaining reasonable peak efficiency and resolution. A series of five pH bumps were applied to elute E. coli tryptic peptides from the monolith, followed by analysis using CZE coupled to an LTQ-Orbitrap Velos mass spectrometer; 799 protein groups and 3381 peptides were identified from 50 ng of the digest in a 2.5 h analysis, which approaches the identification rate for this organism that was obtained with an Orbitrap Fusion. We attribute the improved numbers of peptide and protein identifications to the efficient fractionation by the online pH gradient elution, which decreased the complexity of the sample in each elution step and improved the signal intensity of low abundance peptides. We also performed a comparative analysis using a nanoACQUITY UltraPerformance LCH system. Similar numbers of protein and peptide identifications were produced by the two methods. Protein identifications showed significant overlap between the two methods, whereas peptide identifications were complementary.

  5. Esterification of Waste Frying Oil Using Styrene Type Cation Exchange Resin Catalyst%苯乙烯型阳离子交换树脂催化废煎炸油的酯化反应

    Institute of Scientific and Technical Information of China (English)

    吕鹏梅; 刘莉梅; 杨玲梅; 袁振宏; 陈子博

    2014-01-01

    Porous polystyrene-divinylbenzene was prepared by suspension polymerization,and then sulfonie acid ion exchange resin was obtained by sulfonated porous polystyrene-divinylbenzene.The resin' s morphology and degree of sulfonation were characterized with SEM/EDS,BET,IR respectively.Esterification of waste frying oils with acid value of 63.0 mg/g was studied using cation exchange resin as catalyst to investigate its catalytic activity.40.0% dosage of porogen was preferred when the polymerization conditions were 360 r/min,1.0% dispersant,1.0% initiator,75℃ for 4 h and the heat to 85 ℃ for 6 h,while the sulfonation conditions were 1.0 mL/g dichloroethane,5.0 mL/g sulfuric acid,70℃ sulfonated for 1 h and the heat to 80 ~ 85℃ for 3 h,the optimum swelling time was 1 h,and the concentration of sulfuric acid was 98%.The maximum exchange capacity of the cation exchange resin W2 was 5.2 mmol/g in that condition.When the esterification was performed in the condition of 40.0% methanol,10.0% W2,70℃ stirring.for 1.5 h,the crushing rate of W2 was only 10.0% and the conversion rate of FFA reached to 86.8%.W2 is better than commercially available cation exchange resin PC101,and could be reused for 5 times.%以液体石蜡、邻苯二甲酸二丁酯为混合致孔剂,采用悬浮聚合法制备多孔聚苯乙烯-二乙烯苯,磺化后得到磺酸型阳离子交换树脂.利用SEM/EDS、BET、IR等手段对其形貌、磺化程度进行表征,并通过酸值为63.0 mg/g(以KOH计)煎炸油的酯化反应考察催化剂的活性.结果表明:磺酸根基团成功接到PS分子链上;在聚合条件为360 r/min、1.0%分散剂、1.0%引发剂、75℃保温4h、升温至85℃保温6h时,混合致孔剂的最佳添加量为40.0%液体石蜡、50.0%邻苯二甲酸二丁酯;在磺化条件为二氯乙烷1.0 mL/g、硫酸5.0 mL/g、70℃磺化1h后升温至80~85℃磺化3h时的最佳溶胀时间为1h、硫酸体积分数98%,

  6. Controlled porosity monolithic material as permselective ion exchange membranes.

    Science.gov (United States)

    Huang, Xiaojia; Dasgupta, Purnendu K

    2011-03-18

    Ion exchange membranes (IEMs) are used in a variety of analytical devices, including suppressors, eluent generators and other components used in ion chromatography. Such membranes are flexible and undergo substantial dimensional changes on hydration. Presently the push to miniaturization continues; a resurgent interest in open tubular ion chromatography requires microscale adaptation of these components. Incorporating IEMs in microscale devices is difficult. Although both macroporous and microporous ion exchange materials have been made for use as chromatographic packing, ion exchange material used as membranes are porous only on a molecular scale. Because such pores have vicinal ion exchange sites, ions of the same charge sign as those of the fixed sites are excluded from the IEMs. Monolithic polymers, including ion exchangers derived therefrom, are presently extensively used. When used in a separation column, such a monolithic structure contains an extensively connected porous network. We show here that by controlling the amount of porogen added during the synthesis of monolithic polymers derived from ethylene dimethacrylate - glycidyl methacrylate, which are converted to an anion exchanger by treatment with trimethylamine, it is possible to obtain rigid ion exchange polymers that behave like IEMs and allow only one charge type of ions to pass through, i.e., are permselective. We demonstrate successful open tubular cation chromatography suppressor performance.

  7. 离子交换型缓蚀填料在防腐蚀涂层中的应用Ⅰ阳离子交换型填料%Application of Ion-exchange Compounds as Corrosion Inhibiting Pigments to Organic Anticorrosion Coatings Ⅰ Cation-exchange Pigments

    Institute of Scientific and Technical Information of China (English)

    吴俊升; 肖葵; 李欣荣; 董超芳; 李晓刚

    2011-01-01

    铬酸盐等重金属类缓蚀性颜填料会对环境造成严重的污染,未来该类有害物质在防腐蚀涂层中的应用将被禁止。新型的离子交换型填料因其具有可同时释放缓蚀性离子和吸附固定侵蚀性离子(H+、Cl-、SO24-等)的双重功效,被认为是替代传统重金属类颜填料的理想材料。本文对Zn2+、Ce3+、Ca2+等缓蚀性阳离子改性膨润土、氧化硅、分子筛等新型离子交换型缓蚀填料在有机防腐蚀涂层中的应用进行了综述。%It is well documented that chromate pigments and other heavy metal compounds must be eliminated from organic anticorrosion coatings due to their toxic nature and carcinogenic effects in the future. The novel ion-exchange pigments can play a double role of absorbing the harmful ions such as H+ ,C1- ,SO24- and releasing the inhibiting ions on contact with aggressive electrolyte invading the coating. The released inhibitors can provide active corrosion protection to the defects in the coating and substrate, on the other hand, the uptake of harmful ions decreases the aggressiveness of the corrosive medium, and thereby reduces the rate of ecorrosion processes. Therefore, such new inhibiting compounds have been developed as the potential alternate materials of the traditional toxic pigments, and have attracted a lot of attention. In this paper, the application of ion-exchange pigments, such as Ce3+ , Znz+ cation-exchanged bentonite, Ca2+ cation-exchanged silica and MoO22+ cation-exchanged zeolite, to organic anticorrosion coatings is reviewed.

  8. Anion exchange membrane

    Science.gov (United States)

    Verkade, John G; Wadhwa, Kuldeep; Kong, Xueqian; Schmidt-Rohr, Klaus

    2013-05-07

    An anion exchange membrane and fuel cell incorporating the anion exchange membrane are detailed in which proazaphosphatrane and azaphosphatrane cations are covalently bonded to a sulfonated fluoropolymer support along with anionic counterions. A positive charge is dispersed in the aforementioned cations which are buried in the support to reduce the cation-anion interactions and increase the mobility of hydroxide ions, for example, across the membrane. The anion exchange membrane has the ability to operate at high temperatures and in highly alkaline environments with high conductivity and low resistance.

  9. Furosine as a pasta quality marker: evaluation by an innovative and fast chromatographic approach.

    Science.gov (United States)

    Giannetti, Vanessa; Mariani, Maurizio Boccacci; Mannino, Paola

    2013-07-01

    A fast and simple high-performance liquid chromatography method suitable for determining furosine level in heat-treated food samples was developed. The analysis of furosine was performed by a novel mixed-mode column that provides multiple and simultaneous retention mechanisms including cation-exchange, anion-exchange, reversed-phase, or hydrophilic interaction. Each retention mechanism could be independently controlled by setting chromatographic conditions. Adequate retention and selectivity of polar charged furosine were achieved by adjusting mobile phase pH, buffer concentration, organic content, and ionic strength. The optimized method was successfully applied to determinate furosine in durum wheat semolina pasta samples. Furosine level in pasta may be used as a reliable marker of health and nutritional damage occurring during pasta manufacture. Indeed, a low content of furosine is generally related to high nutritional quality of food and application of mild heat treatments. A wide range of dry pasta samples, collected from both supermarkets (large-scale retail trade) and shops selling local products, were analyzed. Variable amounts of furosine, ranging from 107 to 506 mg/100 g of protein, were found in pasta samples. The proposed method allows to discriminate products submitted to different time-temperature conditions during the drying process. At the same time, it may be used to highlight potential label fraud.

  10. Development and characterization of cation exchange sorbent of St - DVB copolymer support for solid-phase extraction%St-DVB基质阳离子交换固相萃取填料的研制及应用

    Institute of Scientific and Technical Information of China (English)

    申书昌; 李媛媛; 柏叶春

    2011-01-01

    以玉米淀粉为分散剂,偶氮二异丁腈 (AIBN)为引发剂,二乙烯基苯(DVB)为交联剂,在在氮气保护下,用悬浮聚合法制备了交联苯乙烯-二乙烯苯(St-DVB )高分子微球,用浓硫酸进行磺化,制成了以St-DVB为基质的阳离子交换固相萃取填料.考察了搅拌速度对交联聚苯乙烯微球粒径大小及分布的影响.分别用TEM,SEM/EDS和傅里叶红外光谱法对填料进行了形貌及结构分析,测定了磺化物的磺化度.自制阳离子交换固相萃取小柱,对水中的莠去津进行了应用试验,考察了性能.%In this paper, used eom-starch as dispersing agent, 2,2-azobisisobutyronitrile as initiator of polymerization, divinyl benzene as cross-linking agent,polystyrene-divinyl benzene microspheres were prepared by suspension polymerization under nitrogen.The polystyrene-divinyl benzene microspheres were sulfonated by concentrated sulfuric acid, the polystyrene-divinyl benzene sulphonic acid material as a cation exchange sorbent for solid phase extraction packing. stirring speed were investigated to cress-linked polystyrene partiele size and distribution. The form , structure and composition of the polystyrene-divinyl benzene and the polystyrene -divinyl benzene sulphonie acid mierospheres were characterized by means of transmission electron mieraseope , scanning electron microscope/energy dispersive X-ray spectrometer and fourier transform infrared spectroscopy measurement respectively the sulfonate sulfonation degree was Determinated by acid-soda titration method. The cation exchange solid phase extraction column made using the self-made and a plastic syringe. The atrazine in water was detected by solid phase extraetion-HPLC

  11. Profile Distribution of Exchangeable Cations under No-till and Conventional Tillage in An Aquic Brown Soil%免耕与常规耕作潮棕壤交换性阳离子的剖面分布特征

    Institute of Scientific and Technical Information of China (English)

    孙良杰; 张晓珂; 梁文举

    2009-01-01

    The effects of tillage systems on exchangeable cations of different layers to a 1 m depth in an aquic brown soil were studied in a field experiment. The results showed that no-tillage, compared with conventional tillage, significantly increased soil pH and reduced electronic conductivity (EC) in the 0- 5 cm layer. Soil exchangeable K~+ was improved in no-tillage treatment,while exchangeable Na was declined. However, there was no significant effect of tillage practices on soil exchangeable Ca~(2+) , Mg~(2+) and cation exchange capacity. Correlation analysis showed that no significant correlations were observed between exchangeable K and soil nutrients, whereas exchangeable Na~+ , Ca~(2+) , Mg~(2+) , as well as cation exchange capacity had significant negative correlations with organic matter (OM) and total nitrogen (TN), respectively.%通过田间定位试验.研究了不同耕作方式对潮棕壤0-100 cm深度6个土层土壤交换性阳离子的影响.结果表明,与常规耕作相比,免耕使土壤表层pH显著增,.而电导率下降;同时,免耕增加了表层土壤可交换性K~+含量,降低了可交换性Na~+含量,但对可交换性Ca~(2+),Mg~(2+)和阳离子交换量没有产生显著影响.相关分析结果表明,可交换性K~+与土壤养分含量没有显著相关性,而可交换性Na~+,Ca~(2+),Mg~(2+)和阳离子交换量与有机质和全氮含量均呈负相关关系.

  12. Mercury(II) removal from aqueous solutions and wastewaters using a novel cation exchanger derived from coconut coir pith and its recovery

    Energy Technology Data Exchange (ETDEWEB)

    Anirudhan, T.S. [Department of Chemistry, University of Kerala, Kariavattom, Trivandrum 695581 (India)], E-mail: tsani@rediffmail.com; Divya, L.; Ramachandran, M. [Department of Chemistry, University of Kerala, Kariavattom, Trivandrum 695581 (India)

    2008-09-15

    A new adsorbent (PGCP-COOH) having carboxylate functional group at the chain end was synthesized by grafting poly(hydroxyethylmethacrylate) onto coconut coir pith, CP (a coir industry-based lignocellulosic residue), using potassium peroxydisulphate as an initiator and in the presence of N,N'-methylenebisacrylamide as a cross-linking agent. The adsorbent was characterized with the help of infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, and potentiometric titrations. The ability of PGCP-COOH to remove Hg(II) from aqueous solutions was assessed using batch adsorption technique under kinetic and equilibrium conditions. Adsorbent exhibits very high adsorption potential for Hg(II) and more than 99.0% removal was achieved in the pH range 5.5-8.0. Adsorption process was found to follow first-order-reversible kinetics. An increase of ionic strength of the medium caused a decrease in metal removal, indicating the occurrence of outer-sphere surface complex mechanism. The equilibrium data were fitted well by the Freundlich isotherm model (R{sup 2} = 0.99; {chi}{sup 2} 1.81). The removal efficiency was tested using chlor-alkali industry wastewater. Adsorption isotherm experiments were also conducted for comparison using a commercial carboxylate-functionalized ion exchanger, Ceralite IRC-50. Regeneration experiments were tried for four cycles and results indicate a capacity loss of <9.0%.

  13. Mercury(II) removal from aqueous solutions and wastewaters using a novel cation exchanger derived from coconut coir pith and its recovery.

    Science.gov (United States)

    Anirudhan, T S; Divya, L; Ramachandran, M

    2008-09-15

    A new adsorbent (PGCP-COOH) having carboxylate functional group at the chain end was synthesized by grafting poly(hydroxyethylmethacrylate) onto coconut coir pith, CP (a coir industry-based lignocellulosic residue), using potassium peroxydisulphate as an initiator and in the presence of N,N'-methylenebisacrylamide as a cross-linking agent. The adsorbent was characterized with the help of infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, and potentiometric titrations. The ability of PGCP-COOH to remove Hg(II) from aqueous solutions was assessed using batch adsorption technique under kinetic and equilibrium conditions. Adsorbent exhibits very high adsorption potential for Hg(II) and more than 99.0% removal was achieved in the pH range 5.5-8.0. Adsorption process was found to follow first-order-reversible kinetics. An increase of ionic strength of the medium caused a decrease in metal removal, indicating the occurrence of outer-sphere surface complex mechanism. The equilibrium data were fitted well by the Freundlich isotherm model (R(2)=0.99; chi(2)=1.81). The removal efficiency was tested using chlor-alkali industry wastewater. Adsorption isotherm experiments were also conducted for comparison using a commercial carboxylate-functionalized ion exchanger, Ceralite IRC-50. Regeneration experiments were tried for four cycles and results indicate a capacity loss of <9.0%.

  14. Effect of Clay Mineralogy and Exchangeable Cations on Permeability of Saudi Sandstone Reservoirs Effet de la minéralogie des argiles et des cations échangeables sur la perméabilité des réservoirs gréseux d'Arabie Saoudite

    Directory of Open Access Journals (Sweden)

    Dahab A. S.

    2006-11-01

    Full Text Available Reservoir rocks are susceptible to formation damage during secondary recovery operations due to the particular mineralogical, textural and electrochemical properties of the clay minerals they contain. This damage can be explained by the swelling of indigeneous clays present, resulting in the constricting of pores, or by the dispersion of indigeneous nonswelling particle rearrangements during fluid flow, resulting in the plugging of the pore system, or by a combination of the two. This article describes a laboratory study showing the effect of clay mineralogy on the permeability of actual Saudi sandstone reservoirs during water flooding operations. The study shows that the permeability damage of Saudi sandstone reservoirs depends upon the amount of swelling clays and exchangeable ions as well as on the nature of these ions. Monovalent cations cause more damage than multivalent ones but within the same group of metals, those with smaller atomic mass cause more damage. Les roches réservoirs peuvent être endommagées pendant les opérations de récupération secondaire à cause des propriétés minéralogiques, texturales et électrochimiques particulières des minéraux argileux qu'elles contiennent. Cet endommagement peut s'expliquer, soit par le gonflement des argiles qui conduit à un rétrécissement des pores, soit par la migration de particules non gonflantes pendant l'écoulement des fluides qui entraîne le colmatage des milieux poreux, soit par une combinaison des deux mécanismes. Cet article présente une étude de laboratoire montrant l'effet de la minéralogie des argiles sur la perméabilité des roches réservoirs réelles d'Arabie Saoudite pendant des opérations d'injection d'eau. L'étude montre que l'endommagement de la perméabilité des roches réservoirs d'Arabie Saoudite dépend de la quantité d'argiles gonflantes et d'ions échangeables, ainsi que de la nature de ces ions. Les cations monovalents provoquent plus d

  15.  Pressure-induced Fe↔Cu cationic valence exchange and its structural consequences: High-pressure studies of delafossite CuFeO2

    Science.gov (United States)

    Xu, W. M.; Rozenberg, G. Kh.; Pasternak, M. P.; Kertzer, M.; Kurnosov, A.; Dubrovinsky, L. S.; Pascarelli, S.; Munoz, M.; Vaccari, M.; Hanfland, M.; Jeanloz, R.

    2010-03-01

    The present high-pressure studies of CuFeO2 to 30 GPa using x-ray diffraction, along with F57e Mössbauer and Fe and CuK -edge x-ray absorption spectroscopy methods, reveal a sequence of intricate structural/electronic-magnetic pressure-induced transitions. The low-pressure R3¯m structure (0-18 GPa) is composed of sheets of FeS=5/23+ ions alternating with layers of O-CuS=01+-O dumbbells, the latter oriented along the c axis. This structure is characterized by an unusual positive d(c/a)/dP . At 18 GPa a structural transition takes place to a more isotropic C2/c structure with the O-CuS=01+-O axis tilted 28° from the c axis and with negative d(c/a)/dP . This transition corroborates with the onset of long-range antiferromagnetic order. Starting at ˜23GPa , with an initial volume reduction in ˜|ΔV/V0|=0.16 , the Cu-Fe bands overlap and this leads to a (CuS=01+FeS=5/23+)→(CuS=1/22+FeS=22+) interionic valence exchange in about 1/3 of the C2/c-CuFeO2 at 27 GPa. As a result: (i) the Cu2+-O becomes fourfold coordinated and is in a new crystallographic structure with space group P3¯m , and (ii) the Néel temperature increases above twofold [TN(CuS=1/22+FeS=22+)≈2.2TN(CuS=01+FeS=5/23+)] . This sequence of transitions is reversible with minimal hysteresis.

  16. Bulk derivatization and cation exchange restricted access media-based trap-and-elute liquid chromatography–mass spectrometry method for determination of trace estrogens in serum

    Energy Technology Data Exchange (ETDEWEB)

    Beinhauer, Jana [Department of Biochemistry, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Centre of the Region Haná for Biotechnological and Agricultural Research - Department of Protein Biochemistry and Proteomics, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Bian, Liangqiao [Shimadzu Center for Advanced Analytical Chemistry, The University of Texas at Arlington, Arlington, TX (United States); Shimadzu Institute for Research Technologies, The University of Texas at Arlington, Arlington, TX (United States); Fan, Hui [Department of Chemistry and Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); Šebela, Marek [Department of Biochemistry, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Centre of the Region Haná for Biotechnological and Agricultural Research - Department of Protein Biochemistry and Proteomics, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Kukula, Maciej [Shimadzu Center for Advanced Analytical Chemistry, The University of Texas at Arlington, Arlington, TX (United States); Shimadzu Institute for Research Technologies, The University of Texas at Arlington, Arlington, TX (United States); Barrera, Jose A. [Shimadzu Institute for Research Technologies, The University of Texas at Arlington, Arlington, TX (United States); and others

    2015-02-09

    Highlights: • Analysis of estrogens in small volume samples at low parts-per-trillion concentration. • Charged bulk derivatization facilitates on-line ion exchange sample preparation. • On-line WCX restricted access media traps analytes, but not proteins and lipids. • Complete preparation and LC–MS/MS analysis completed in 30 min/sample. - Abstract: Estrone (E1), estradiols (α/β-E2), and estriol (E3) are four major metabolically active estrogens exerting strong biological activities at very low circulating concentrations. This paper reports a sensitive and efficient method with automated, on-line clean-up and detection to determine trace estrogens in a small volume of serum samples using liquid chromatography–electrospray ionization–tandem mass spectrometry directly, without off-line liquid–liquid or solid-phase extraction pretreatments. Serum aliquots (charcoal stripped fetal bovine serum, 100 μL) were spiked with four estrogen standards and their corresponding isotope-labeled internal standards, then bulk derivatized with 2-fluoro-1-methyl-pyridium p-toluenesulfonate (2-FMP) to establish the calibration curves and perform method validation. Calibration was established in the concentration ranges of 5–1000 pg mL{sup −1}, and demonstrated good linearity of R{sup 2} from 0.9944 to 0.9997 for the four derivatized estrogens. The lower detection limits obtained were 3–7 pg mL{sup −1}. Good accuracy and precision in the range of 86–112% and 2.3–11.9%, respectively, were observed for the quality control (QC) samples at low, medium, and high concentration levels. The stability tests showed that the derivatized serum samples were stable 8 h after derivatization at room temperature and at least to 48 h if stored at −20 °C. The method was applied to measure trace estrogens in real human and bovine serum samples, and three of four estrogen compounds studied were observed and quantified.

  17. Thermally induced conversion of Mg2+ cation exchanged LTA, FAU, GIS and SOD zeolites: syntheses and characterization of γ-cordierite, a new Mg2Al4Si5O18 polymorph

    Directory of Open Access Journals (Sweden)

    RADOVAN DIMITRIJEVIC

    2007-12-01

    Full Text Available The thermal behaviours of fully Mg2+ cation exchanged LTA, FAU (X and Y species, GIS and SOD zeolites were investigated in the temperature range from ambient to 1400 °C. The initial zeolite frameworks collapsed into amorphous intermediate substances after air heating between 800–850 °C. Prolonged annealing of these products above 850 °C induced recrystallization into sapphirine-like phases (Mg–LTA and Mg–FAUx zeolites and μ-cordierite (Mg–FAUy and Mg–GIS zeolites phases. These phases were unstable during further temperature/time treatment and between 1000–1100 °C, they polymorphously transformed into γ-cordierite, a new Mg2Al4Si5O18 polymorph. γ-Cordierite was formed as a transformation product from the investigated zeolite precursors, except for the Mg–SOD zeolite. Structurally the γ-cordierite phase is a modulated, Mg-stuffed derivative of cristobalite with the approximate composition Mg2Al4Si5O18, which precedes the appearance of α-cordierite. The orthorhombic unit cell dimensions calculated from X-ray powder diffraction pattern are: a = 16.387(7 Å, b = 8.835(4 Å, c = 7.853(3 Å. γ-Cordierite has a narrow range of temperature stability (1100–1200 °C and during prolonged temperature/time treatment, it is polymorphously transformed to the α-cordierite phase.

  18. Matrix-assisted refolding of autoprotease fusion proteins on an ion exchange column.

    Science.gov (United States)

    Schmoeger, Elisabeth; Berger, Eva; Trefilov, Alexandru; Jungbauer, Alois; Hahn, Rainer

    2009-11-27

    Refolding of proteins must be performed under very dilute conditions to overcome the competing aggregation reaction, which has a high reaction order. Refolding on a chromatography column partially prevents formation of the intermediate form prone to aggregation. A chromatographic refolding procedure was developed using an autoprotease fusion protein with the mutant EDDIE from the N(pro) autoprotease of pestivirus. Upon refolding, self-cleavage generates a target peptide with an authentic N-terminus. The refolding process was developed using the basic 1.8-kDa peptide sSNEVi-C fused to the autoprotease EDDIE or the acidic peptide pep6His, applying cation and anion exchange chromatography, respectively. Dissolved inclusion bodies were loaded on cation exchange chromatographic resins (Capto S, POROS HS, Fractogel EMD SO(3)(-), UNOsphere S, SP Sepharose FF, CM Sepharose FF, S Ceramic HyperD F, Toyopearl SP-650, and Toyopearl MegaCap II SP-550EC). A conditioning step was introduced in order to reduce the urea concentration prior to the refolding step. Refolding was initiated by applying an elution buffer containing a high concentration of Tris-HCl plus common refolding additives. The actual refolding process occurred concurrently with the elution step and was completed in the collected fraction. With Capto S, POROS HS, and Fractogel SO(3)(-), refolding could be performed at column loadings of 50mg fusion protein/ml gel, resulting in a final eluate concentration of around 10-15 mg/ml, with refolding and cleavage step yields of around 75%. The overall yield of recovered peptide reached 50%. Similar yields were obtained using the anion exchange system and the pep6His fusion peptide. This chromatographic refolding process allows processing of fusion peptides at a concentration range 10- to 100-fold higher than that observed for common refolding systems.

  19. [Preparation of an agglomerated ion chromatographic stationary phase with 2,3-ionene and its application in SO4(2-) analysis].

    Science.gov (United States)

    Wang, Muhua; Liu, Junwei; Huang, Zhongping; Zhang, Jiajie; Zhu, Yan

    2015-07-01

    The poly-electrolyte cation functional group of 2,3-ionene was synthesized with tetramethyl ethylenediamine and 1,3-dibromopropane as the raw materials. Multiporous polystyrene-divinylbenzene microsphere particles (PS-DVB) were produced by swelling method with polystyrene as seeds and sulfonated. Then the 2,3-ionene was bonded on the sulfonated multi-porous polystyrene-divinylbenzene microsphere particles by agglomeration to get the agglomerative ion-exchange stationary phase. After optimizing the synthetic conditions, the new stationary phase was characterized by the techniques including scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and elemental analysis. The chromatographic column was packed by slurry method and applied in the analysis of SO4(2-) with a conductivity detector. SO4(2-) and other six common anions including F-, Cl-, NO2(-), Br-, NO3(-), PO4(3-), were separated and analyzed rapidly on the self-regulating chromatographic column within 8 min. The linear range was from 0.5 to 50 mg/L with correlation coefficient (r) of 0.9992. The LOD was 0.04 mg/L with S/N of 3. The relative standard deviations (RSDs, n = 6) were 2.4% and 3.1% for the peak area and retention time, respectively. The recoveries were between 99.2% and 101.8%. The retention times of SO4(2-) did not change significantly after long time use of the self-regulating chromatographic column. The self-regulating chromatographic column is suitable for the detection of SO4(2-) in complex matrix samples.

  20. Chiral Ionic Liquids in Chromatographic Separation and Spectroscopic Discrimination

    Science.gov (United States)

    Li, Min; Bwambok, David K.; Fakayode, Sayo O.; Warner, Isiah M.

    Chiral ionic liquids (CILs) are a subclass of ionic liquids (ILs) in which the cation, anion, or both may be chiral. The chirality can be central, axial, or planar. CILs possess a number of unique advantageous properties which are inherited from ionic liquids including negligible vapor pressure, wide liquidus temperature range, high thermal stability, and high tunability. Due to their dual functionalities as chiral selectors and chiral solvents simultaneously, CILs recently have been widely used both in enantiomeric chromatographic separation and in chiral spectroscopic discrimination. In this chapter, the various applications of CILs in chiral chromatographic separations such as GC, HPLC, CE, and MEKC are reviewed. The applications of CILs in enantiomeric spectroscopic discrimination using techniques such as NMR, fluorescence, and NIR are described. In addition, chiral recognition and separation mechanism using the CILs as chiral selectors or chiral solvents is also discussed.

  1. Divalent cation shrinks DNA but inhibits its compaction with trivalent cation

    Science.gov (United States)

    Tongu, Chika; Kenmotsu, Takahiro; Yoshikawa, Yuko; Zinchenko, Anatoly; Chen, Ning; Yoshikawa, Kenichi

    2016-05-01

    Our observation reveals the effects of divalent and trivalent cations on the higher-order structure of giant DNA (T4 DNA 166 kbp) by fluorescence microscopy. It was found that divalent cations, Mg(2+) and Ca(2+), inhibit DNA compaction induced by a trivalent cation, spermidine (SPD(3+)). On the other hand, in the absence of SPD(3+), divalent cations cause the shrinkage of DNA. As the control experiment, we have confirmed the minimum effect of monovalent cation, Na(+) on the DNA higher-order structure. We interpret the competition between 2+ and 3+ cations in terms of the change in the translational entropy of the counterions. For the compaction with SPD(3+), we consider the increase in translational entropy due to the ion-exchange of the intrinsic monovalent cations condensing on a highly charged polyelectrolyte, double-stranded DNA, by the 3+ cations. In contrast, the presence of 2+ cation decreases the gain of entropy contribution by the ion-exchange between monovalent and 3+ ions.

  2. 邻氯苯乙烯-二乙烯基苯强酸性阳离子交换树脂的合成工艺%SYNTHESIS TECHNOLOGY OF o-CHLOROSTYRENE-DIVINYLBENZENE STRONGLY ACIDIC CATION EXCHANGE RESIN

    Institute of Scientific and Technical Information of China (English)

    陈亮; 孙富安; 何明阳; 佟春雨; 张海涛; 陈群

    2012-01-01

    o-chlorostyrene and divinylbenzene occurred suspension copolymerization could obtain high quality copolymer beads. The effects of water-oil ratio, dispersants, assist dispersants and other factors were studied. The optimum reaction conditions: water-oil ratio was from 3:1 to 4:1; poly vinyl alcohol, gelatin, secondary dispersants and electrolyte were respectively 0.1%, 1.0%, 0.5% and 10% ratio of water, the heating rate should be controlled at 20℃/h during the critical period of 40~80℃. Beads sulfonated at 80~110℃ by oleum could be made into strongly acidic cation exchange resin. The exchange capacity was more than 4mmol/g and the synthesis technology of resin has been optimized.%以邻氯苯乙烯和二乙烯基苯为原料制备了邻氯苯乙烯-二乙烯基苯强酸性阳离子交换树脂,考察了水油比、分散剂、助分散剂等因素对合成树脂的影响.研究表明,该树脂的合成最佳工艺条件为:水油比3:1~4:1,聚乙烯醇与明胶分别为水相质量的0.1%和1.0%,助分散剂为水相质量的0.5%,电解质为水相质量的10%,在40~80℃的成球关键期控制升温速率为20℃/h,在80~110℃以发烟硫酸辅助磺化,得到交换量大于4mmol/g的树脂,优化了该树脂的合成工艺.

  3. 强酸性阳离子交换树脂催化合成乙酰水杨酸的研究%Synthesis of acetylsalicylic acid using strong-acidic cation-exchange resin as catalyst

    Institute of Scientific and Technical Information of China (English)

    赵志刚; 谢志融; 陈靠山

    2012-01-01

    目的:探讨001×7强酸性阳离子交换树脂催化合成乙酰水杨酸的方法和最佳工艺.方法:通过正交试验探讨了乙酸酐与水杨酸的摩尔比、反应时间、催化剂用量和反应温度对乙酰水杨酸产率的影响,并探讨催化剂的催化能力与使用次数的关系.结果:乙酸酐与水杨酸的摩尔比为3:1、催化剂用量为水杨酸质量的14.50%、反应时间120 min、反应温度60 ℃时,乙酰水杨酸产率最高,为77.93%.结论:001×7强酸性苯乙烯系阳离子交换树脂对酯化反应催化效果好,副反应少,对环境污染小,能重复使用,值得大力推广.%Objective:To optimize the technology of synthesizing acetylsalicylic acid using 001 × 7 strong-acidic cation-exchange resin as catalyst . Methods : Orthogonal experiment was performed to examine the effect of molar ratio of reactants,reaction time, dosage of catalyst, and reaction temperature on the yield of product as well as the efficiency and frequencies of the resin recycled and shifted on the synthesis. Results :The optimal reaction conditions were 3:1 (the ratio of acetic anhydride to salicylic acid,n:n),in a dosage of the resin 14. 50% of salicylic acid,for the reaction time of 120 min at temperature of 60 ℃ , which led to a yield of 77.93 % . Conclusion: 001 × 7 strong-acidic cat ion-exchange resin works well on esterification reaction as a environmentally friendly catalyst and is worthy of wider use, for it has efficient activity, less adverse reaction and recyclable advantages.

  4. Evaluation of glycidyl methacrylate-based monolith functionalized with weak anion exchange moiety inside 0.5 mm i.d. column for liquid chromatographic separation of DNA

    Directory of Open Access Journals (Sweden)

    Aprilia Nur Tasfiyati

    2016-03-01

    Full Text Available In this study, the organic polymer monolith was developed as a weak anion exchanger column in high performance liquid chromatography for DNA separation. Methacrylate-based monolithic column was prepared in microbore silicosteel column (100 × 0.5 mm i.d. by in-situ polymerization reaction using glycidyl methacrylate as monomer; ethylene dimethacrylate as crosslinker; 1-propanol, 1,4-butanediol, and water as porogenic solvents, with the presence of initiator α,α′-azobisisobutyronitrile (AIBN. The monolith matrix was modified with diethylamine to create weak anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by SEM. The properties of the monolithic column, such as permeability, mechanical stability, binding capacity and pore size distribution, were characterized in detail. From the results of the characterization, monoliths poly-(GMA-co-EDMA with total monomer percentage (%T 40 and crosslinker percentage (%C 25 was found to be the ideal composition of monomer and crosslinker. It has good mechanical stability and high permeability, adequate molecular recognition sites (represented with binding capacity value of 36 mg ml−1, and has relatively equal proportion of flow-through pore and mesopores (37.2% and 41.1% respectively. Poly-(GMA-co-EDMA with %T 40 and %C 25 can successfully separate oligo(dT12–18 and 50 bp DNA ladder with good resolution.

  5. 强酸阳树脂在过氧化氢中的氧化分解特性研究%Characteristics of oxidation and decomposition of strong acidic cation exchange resin in hydrogen peroxide

    Institute of Scientific and Technical Information of China (English)

    朱志平; 周瑜; 赵永福; 郭小翠

    2012-01-01

    在核电站,SO42-会引起镍基金属的晶间应力腐蚀破裂,对核电站的安全经济运行造成严重危害.为探索核电站SO42-的来源,研究了几种进口阳树脂在H2O2溶液中的动态溶出特性,采用离子色谱仪和TOC仪对溶出液的SO42-、TOC进行测定.研究结果表明,过氧化氢对大孔型和凝胶型树脂的影响不同,且氧化剂浓度越高,对树脂的影响越大,溶出的SO42-也越多;脱磺化速率随着时间推移而降低,而有机物溶出速率变化相对较小.%SO42- may cause intergranular stress corrosion cracking of nickel-based metal in nuclear power stations, resulting in serious hazards to the economically running of the nuclear power stations. To explore the source of SO42-of nuclear power stations, dynamic dissolving characteristics of several kinds of imported cation exchange resins in hydrogen peroxide solution have been researched. The dissolved liquid of S042- ,TOC are determined by ion chro-matography and TOC meter. The results show that the effects of hydrogen peroxide on macro-porous resin and gel-type resin are different. The higher the oxidant concentration is,the higher the influence on resin is,and the more SO42- is dissolved. And it is very likely that the desulfonation rate decreases with time, and the change of dissolving rate of organisms is relatively small.

  6. Development and validation of a UHPLC-MS/MS assay for colistin methanesulphonate (CMS) and colistin in human plasma and urine using weak-cation exchange solid-phase extraction.

    Science.gov (United States)

    Zhao, Miao; Wu, Xiao-Jie; Fan, Ya-Xin; Guo, Bei-Ning; Zhang, Jing

    2016-05-30

    A rapid ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) assay method was developed for determination of CMS and formed colistin in human plasma and urine. After extraction on a 96-well SPE Supra-Clean Weak Cation Exchange (WCX) plate, the eluents were mixed and injected into the UHPLC-MS/MS system directly. A Phonomenex Kinetex XB-C18 analytical column was employed with a mobile phase consisting of solution "A" (acetonitrile:methanol, 1:1, v/v) and solution "B" (0.1% formic acid in water, v/v). The flow rate was 0.4 mL/min with gradient elution over 3.5 min. Ions were detected in ESI positive ion mode and the precursor-product ion pairs were m/z 390.7/101.3 for colistin A, m/z 386.0/101.2 for colistin B, and m/z 402.3/101.2 for polymyxin B1 (IS), respectively. The lower limit of quantification (LLOQ) was 0.0130 and 0.0251 mg/L for colistin A and colistin B in both plasma and urine with accuracy (relative error, %) <± 12.6% and precision (relative standard deviation, %) <± 10.8%. Stability of CMS was demonstrated in biological samples before and during sample treatment, and in the extract. This new analytical method provides high-throughput treatment and optimized quantification of CMS and colistin, which offers a highly efficient tool for the analysis of a large number of clinical samples as well as routine therapeutic drug monitoring.

  7. Research on removal of metal impurities from wet-process phosphoric acid with macroporous strong acid cation exchange resin%大孔阳离子树脂脱除湿法磷酸中阳离子的研究

    Institute of Scientific and Technical Information of China (English)

    熊祥祖; 徐彪; 王威; 杜文; 胡利锋

    2011-01-01

    采用D001大孔强酸性阳离子交换树脂三级处理湿法磷酸中的金属杂质,考察了搅拌速度、温度、树脂用量及反应时间对金属阳离子去除率的影响.结果表明,在搅拌速度为200 r/min、树脂质量磷酸质量为12、反应温度为400 ℃、反应时间为10 min时,效果最好,铁的去除率可达到86.75%、铝的去除率可达到76.13%、镁的去除率可到达40.38%、钙的去除率可到达47.49%.%The removal rate of metal impurities in Wet-Process Phosphoric Acid with D001 macroporous strong acid cation exchange resin was researched.Some important factors which affect the removal rate of metal impurities such as stirring speed, temperature, the mass ratio of resin to phosphoric acid and reaction time were studied respectively.The results show that the removal efficiency of iron,aluminum,magnesium,calcium can be up to 86.75%, 76.13%, 40.38%, 47.49%, respectively, when the stirring speed was 200 r/min, the mass ratio of resin to phosphoric acid was 1:2, the temperature was 40 ℃,the reaction time was 10min.

  8. Effect of water pollutants to copper ion removal bv using cation exchange membrane%水中污染物对阳离子交换膜分离去除Cu2+的影响

    Institute of Scientific and Technical Information of China (English)

    谢德华; 施周; 陈世洋

    2012-01-01

    Baesd on Donnan dialysis mechanism, copper ion separation and removing experiments in raw water using exchange membrane was conducted under voltage free condition. The copper ion removing effects of cation exchange membrane cuased by various potential pollutants in raw water such as inorganic particles, organic matters, EDTA acid, ammonia, ferric ion and surfacatant etc, were studied. The results showed that upon addition any one of the above pollutants to raw water, would influence on the copper ions removing effects more or less after a long time operation procedure. To pollutants with no physical and chemical interaction with copper ion and membrane, such as silica and non-ionic surfactant, there were little influences on the copper ion separation of the cation exchange membrane and the Cu2+ removal decreased only by about 4% compared to that of blank control experiments; Cu2+ could be precipitated by ammonia and anionic surfaceactive agent, or adsorbed by humic acid which made the concentration of free Cu2+ in the solution reduce by about 50%; While to pollutants which could form complex compounds with Cu2+, serious effects on Cu2+ removal efficiency were observed. For EDTA acid, ammonia and anionic surfaceactive agent, the Cu2+ removal effects decreased by approximately 100%, 78% and 56% respectively; Cationic surfactants may occupy a lot of space of film render Cu2+ remove difficulty; ferric ion easily hydrolyzed into iron hydroxide colloids in weak acid or neutral solution induced Cu2+ removal effect decreased to certain extend, by about 12% compared to the blank.%基于Donnan dialysis原理,在无外加电压作用下采用阳离子交换膜分离去除原水中的Cu2+,研究原水中可能出现的无机颗粒物,有机物质,EDTA酸、氨水、Fe3+、表面活性剂等对阳离子交换膜分离去除Cu2+效果的影响.研究表明:原水中添加二氧化硅、腐殖酸、EDTA酸、氨水、Fe3+、表面活性剂等物质,在长时间运行后均

  9. Trace adsorption of positively charged proteins onto Sepharose FF and Sepharose FF-based anion exchangers.

    Science.gov (United States)

    Yu, Lin-Ling; Sun, Yan

    2012-08-31

    Agarose-based matrices have been widely used in ion exchange chromatography (IEC). We have herein observed that positively charged proteins (lysozyme and cytochrome c) are adsorbed on the agarose-based anion-exchangers (Q and DEAE Sepharose FF gels) in a capacity of 10-40 μg/mL. In contrast, negatively charged protein (bovine serum albumin) is not adsorbed to Sepharose FF and SP Sepharose FF gels. Elemental analysis of the gel indicated that the residual anionic sulfate groups in agarose would have worked as the cation exchange groups for the positively charged proteins. The trace adsorption behavior of lysozyme onto Sepharose FF and Sepharose FF-based anion exchangers was studied and the effects of NaCl concentration and cation group density on the adsorption were examined for better understanding of the trace adsorption in chromatographic processes. At NaCl concentrations less than 0.05 mol/L, which is the normal adsorption condition in IEC, the trace adsorption kept at a high level, so this trace adsorption cannot be avoided in the ionic strength range of routine IEC operations. Grafting poly(ethylenimine) (PEI) chain of 60 kDa to a cation group density of 700 mmol/L could reduce the adsorption capacity to about 20 μg/mL, but further reduction was not possible by increasing the cation group density to 1200 mmol/L. Therefore, attentions need to be paid to the phenomenon in protein purification practice using agarose-based matrices. The research is expected to call attentions to the trace adsorption on agarose-based matrices and to the importance in the selection of the suitable solid matrices in the production of high-purity protein products in large-scale bioprocesses.

  10. 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.

  11. Review of UV spectroscopic, chromatographic, and electrophoretic methods for the cholinesterase reactivating antidote pralidoxime (2-PAM).

    Science.gov (United States)

    John, Harald; Blum, Marc-Michael

    2012-01-01

    Pralidoxime (2-PAM) belongs to the class of monopyridinium oximes with reactivating potency on cholinesterases inhibited by phosphylating organophosphorus compounds (OPC), for example, pesticides and nerve agents. 2-PAM represents an established antidote for the therapy of anticholinesterase poisoning since the late 1950s. Quite high therapeutic concentrations in human plasma (about 13 µg/ml) lead to concentrations in urine being about 100 times higher allowing the use of less sensitive analytical techniques that were used especially in the early years after 2-PAM was introduced. In this time (mid-1950s until the end of the 1970s) 2-PAM was most often analyzed by either paper chromatography or simple UV spectroscopic techniques omitting any sample separation step. These methods were displaced completely after the establishment of column liquid chromatography in the early 1980s. Since then, diverse techniques including cation exchange, size-exclusion, reversed-phase, and ligand-exchange chromatography have been introduced. Today, the most popular method for 2-PAM quantification is ion pair chromatography often combined with UV detection representing more than 50% of all column chromatographic procedures published. Furthermore, electrophoretic approaches by paper and capillary zone electrophoresis have been successfully used but are seldom applied. This review provides a commentary and exhaustive summary of analytical techniques applied to detect 2-PAM in pharmaceutical formulations and biological samples to characterize stability and pharmacokinetics as well as decomposition and biotransformation products. Separation techniques as well as diverse detectors are discussed in appropriate detail allowing comparison of individual preferences and limitations. In addition, novel data on mass spectrometric fragmentation of 2-PAM are provided.

  12. Kinetic simulation of complex decomposition as a tool for the ion chromatographic determination of elemental speciation of less inert metal ions.

    Science.gov (United States)

    Winter, Christian; Seubert, Andreas

    2016-01-15

    Species decomposition is an often occurring artefact during the chromatographic determination of elemental speciation. The decomposition follows a simple path to lower coordinated compounds. Therefore a simulation is developed for those decomposition reactions. The simulation separates the isochronal processes of the separation itself and the ongoing reaction and delivers thermodynamic and kinetic information about the species present in the original sample. This shifts the boundaries of separation based elemental speciation to less inert metal ions which are typically not analyzable by this approach. The less inert gallium monooxalato complex [GaOx](+) is used as example for testing the simulation software as this complex decomposes only to Ga(3+) and both species are retained on cation exchange columns. We extracted thermodynamic and kinetic information from flow rate experiments by the analysis of the peak areas in the chromatogram. The results show that some of our assumptions such as the irreversibility under the applied chromatographic conditions are not ultimately true, but good accordance of simulation and measured data was achieved.

  13. Mineral Separation in a CELSS by Ion-exchange Chromatography

    Science.gov (United States)

    Ballou, E. V.; Spitze, L. A.; Wong, F. W.; Wydeven, T.; Johnson, C. C.

    1982-01-01

    Operational parameters pertinent to ion exchange chromatography separation were identified. The experiments were performed with 9 mm diameter ion exchange columns and conventional column accessories. The cation separation beds were packed with AG 50W-X2 strong acid cation exchange resin in H(+) form and 200-400 dry mesh particle size. The stripper beds used in some experiments were packed with AG 1-XB strong base cation exchange resin in OH(-) form and 200-400 dry mesh particle size.

  14. Cationic ruthenium alkylidene catalysts bearing phosphine ligands.

    Science.gov (United States)

    Endo, Koji; Grubbs, Robert H

    2016-02-28

    The discovery of highly active catalysts and the success of ionic liquid immobilized systems have accelerated attention to a new class of cationic metathesis catalysts. We herein report the facile syntheses of cationic ruthenium catalysts bearing bulky phosphine ligands. Simple ligand exchange using silver(i) salts of non-coordinating or weakly coordinating anions provided either PPh3 or chelating Ph2P(CH2)nPPh2 (n = 2 or 3) ligated cationic catalysts. The structures of these newly reported catalysts feature unique geometries caused by ligation of the bulky phosphine ligands. Their activities and selectivities in standard metathesis reactions were also investigated. These cationic ruthenium alkylidene catalysts reported here showed moderate activity and very similar stereoselectivity when compared to the second generation ruthenium dichloride catalyst in ring-closing metathesis, cross metathesis, and ring-opening metathesis polymerization assays.

  15. Hidrólise parcial da superfície do polyethylene terephthalate (PET: transformando um rejeito em um material de troca catiônica para aplicação ambiental Partial hydrolysis of pet surface: transforming a plastic waste into a material with cationic exchange properties for environmental application

    Directory of Open Access Journals (Sweden)

    Marcelo G. Rosmaninho

    2009-01-01

    Full Text Available In this work it is proposed a simple and versatile undergraduate chemical experiment in polymer and environmental technology based on the process of polyethylene terephthalate (PET hydrolysis. Polyethylene terephthalate from post-consume bottles is submitted to a controlled partial hydrolysis which allows the students to follow the reaction by a simple procedure. The students can explore the reaction kinetics, the effect of catalysts and the exposed polyethylene terephthalate surface area on the hydrolysis reaction. The second and innovative part of this experiment is the technological and environmental application of the hydrolyzed polyethylene terephthalate as a material with cation exchange properties. The surface hydrolyzed polyethylene terephthalate can be used as adsorbent for cationic contaminants.

  16. Determination of Morpholinium Ionic Liquid Cations by Ion Chromatography with Direct Conductivity Detection%离子色谱-直接电导检测法分离测定吗啉离子液体阳离子

    Institute of Scientific and Technical Information of China (English)

    孙晓娇; 于泓; 张仁庆

    2013-01-01

    An ion chromatographic method with direct conductivity detection for the determination of N-methyl,ethyl morpholinium cation([MEMo] +),N-methyl,propyl morpholinium cation([MP-Mo] +) two morpholinium ionic liquid cations was developed using a cation-exchange column and ethylenediamine-acetonitrile as mobile phase.The effects of column type,mobile phase and column temperature on retention and separation of the cations were investigated.The retention rules of the cations under different chromatographic conditions were formulated.The results indicated that the retention process of morpholinium cations retained in line with the ion-exchange mode,wihich was an exothermic process.The successful separation of the two morpholinium ionic liquid cations was achieved using the optimized mobile phase of 0.1 mmol/L ethylenediamine-0.5% acetonitrile (adjusted to pH 5.0 with hydrochloric acid) at a flow rate of 1.0 mL/min and a column temperature of 30 ℃.Under the optimal conditions,the two morpholinium ionic liquid cations could be successfully separated in 4 min.The detection limits(S/N =3) for [MEMo] + and [MPMo] + were 0.08 mg/L and 0.13 mg/L,respectively.The relative standard deviations(RSDs,n =5) of the chromatographic peak areas for the cations were no more than 1.5%.The method was successfully applied in the determination of morpholinium bromide ionic liquid samples synthesized by chemistry laboratory.The recoveries of morpholinium cations after spiked were in the range of 94.0%-106.0%.The method was proved to be accurate,reliable and rapid,and could meet the requirements for quantitative analysis of morpholinium ionic liquid samples.%建立了离子色谱-直接电导检测法分析N-甲基乙基吗啉([MEMo]+)、N-甲基丙基吗啉([MPMo]+)2种吗啉离子液体阳离子的方法.采用磺酸型阳离子交换色谱柱,以乙二胺-乙腈为流动相,研究了色谱柱、流动相、色谱柱温度对吗啉阳离子保留的影响,并讨论了保留规律.结

  17. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  18. Cation locations and dislocations in zeolites

    Science.gov (United States)

    Smith, Luis James

    The focus of this dissertation is the extra-framework cation sites in a particular structural family of zeolites, chabazite. Cation sites play a particularly important role in the application of these sieves for ion exchange, gas separation, catalysis, and, when the cation is a proton, acid catalysis. Structural characterization is commonly performed through the use of powder diffraction and Rietveld analysis of powder diffraction data. Use of high-resolution nuclear magnetic resonance, in the study of the local order of the various constituent nuclei of zeolites, complements well the long-range order information produced by diffraction. Recent developments in solid state NMR techniques allow for increased study of disorder in zeolites particularly when such phenomena test the detection limits of diffraction. These two powerful characterization techniques, powder diffraction and NMR, offer many insights into the complex interaction of cations with the zeolite framework. The acids site locations in SSZ-13, a high silica chabazite, and SAPO-34, a silicoaluminophosphate with the chabazite structure, were determined. The structure of SAPO-34 upon selective hydration was also determined. The insensitivity of X-rays to hydrogen was avoided through deuteration of the acid zeolites and neutron powder diffraction methods. Protons at inequivalent positions were found to have different acid strengths in both SSZ-13 and SAPO-34. Other light elements are incorporated into zeolites in the form of extra-framework cations, among these are lithium, sodium, and calcium. Not amenable by X-ray powder diffraction methods, the positions of such light cations in fully ion-exchanged versions of synthetic chabazite were determined through neutron powder diffraction methods. The study of more complex binary cation systems were conducted. Powder diffraction and solid state NMR methods (MAS, MQMAS) were used to examine cation site preferences and dislocations in these mixed-akali chabazites

  19. Study on influence factors of the flux for strong cation-exchange monolithic electroosmotic pump%强阳离子交换整体电渗泵流量影响因素研究

    Institute of Scientific and Technical Information of China (English)

    崔瑞红; 尤慧艳

    2011-01-01

    采用丙烯酸,2-丙烯酰胺-2-甲基丙磺酸为功能单体,N,N’-亚甲基双丙烯酰胺为交联剂,正十二醇、1,4-丁二醇及二甲基亚砜为致孔剂,偶氮二异丁腈为引发剂在原位聚合,制备出了以丙烯酰胺类强阳离子交换整体柱为核心的电渗泵.在乙腈-磷酸盐二元流动相体系下,考察了驱动电压,有机调节剂,盐浓度,pH对该泵流量的影响.流量与驱动电压呈线性关系(0.9991);当有机调节剂乙腈的浓度低于70%时,固定相溶胀为主要因素,流量随乙腈浓度的增加而有下降的趋势,但随着有机调节剂浓度的增加(>70%),此时粘度起主要作用,流量开始缓慢地增加;随着磷酸盐浓度逐渐增加,流量随之降低;在pH 3~9范围内,流量基本上保持恒定.%A strong cation-exchange monolithic electroosmotic column was prepared inside the fused-silica capillary bypolymerization. The solution was consisted of acrylanide, 2-acrylamido-2-methyl-l -propanesulfonicacid as a functional monomer, N, N' -methylenebisacrylanide as a cross-linking agent, dimethyl sulphoxide and dodecanol, 1, 4-Butanediol as organic porogenic reagents and azobisisobutyronitrile as an initiator. The monolithic column was severed as a key part of electroosmotic pump. Effects of applied voltage, the concentrations of organic modifier and salt solution, pH value on the flux were investigated. A good linear relationship between the applied voltage and the flux was obtained (0. 9991 ). The concentration of the organic modifier (CAN)was less than 70%. The swelling degree of stationary phase played a main role, and the flux decreased with increase of the concentration of CAN. However, its concentration was more than 70% , at this time the viscosity of mobile phase was the main influence factor, the flux began to increase slightly. The flux decreased as the concentration of phosphate increased. pH value was in the range of 3 ~ 9, it did not exert a significant change in

  20. Multi-modal applicability of a reversed-phase/weak-anion exchange material in reversed-phase, anion-exchange, ion-exclusion, hydrophilic interaction and hydrophobic interaction chromatography modes.

    Science.gov (United States)

    Lämmerhofer, Michael; Nogueira, Raquel; Lindner, Wolfgang

    2011-06-01

    We recently introduced a mixed-mode reversed-phase/weak anion-exchange type separation material based on silica particles which consisted of a hydrophobic alkyl strand with polar embedded groups (thioether and amide functionalities) and a terminal weak anion-exchange-type quinuclidine moiety. This stationary phase was designed to separate molecules by lipophilicity and charge differences and was mainly devised for peptide separations with hydroorganic reversed-phase type elution conditions. Herein, we demonstrate the extraordinary flexibility of this RP/WAX phase, in particular for peptide separations, by illustrating its applicability in various chromatographic modes. The column packed with this material can, depending on the solute character and employed elution conditions, exploit attractive or repulsive electrostatic interactions, and/or hydrophobic or hydrophilic interactions as retention and selectivity increments. As a consequence, the column can be operated in a reversed-phase mode (neutral compounds), anion-exchange mode (acidic compounds), ion-exclusion chromatography mode (cationic solutes), hydrophilic interaction chromatography mode (polar compounds), and hydrophobic interaction chromatography mode (e.g., hydrophobic peptides). Mixed-modes of these chromatographic retention principles may be materialized as well. This allows an exceptionally flexible adjustment of retention and selectivity by tuning experimental conditions. The distinct separation mechanisms will be outlined by selected examples of peptide separations in the different modes.

  1. 聚苯乙烯磺酸钠阳离子交换树脂(高温磺化)制备浅色高纯树脂的方法%Method for the Preparation of Lighted Colored Sodium Polystyrene Sulfonate Cation-ion-exchange Resin of High Purity Sulfonated at High Temperature

    Institute of Scientific and Technical Information of China (English)

    杨光; 顾浩

    2009-01-01

    Sodium polystyrene sulfonate ion-exchange resin(SPSR) is a medicine used as lowering kalieraia. Using commercial dark colored sodium polystyrene sulfonate cation-ion-exchange resin prepared by the conventional process at the sulfonated temperature higher than 100℃as raw material, light colored SPSR of high purity was prepared by the bleaching-purifying combined process. The resin reached the criterion of medicinal SPSR of Japanese pharmacopoeia(14 ed. ).%聚苯乙烯磺酸钠阳离子交换树脂(SPSR)是降血钾药.以市售的高于100℃的高温磺化工艺生产的深棕色SPSR为原料,经过漂白和净化联合工艺处理,得到了浅色高纯SPSR,该浅色树脂达到日本药典(第14版)规定的药用SPSR标准.

  2. Water quality monitoring system for determination of ionic nutrients by ion-exclusion chromatography with spectrophotometric detection on cationand anion-exchange resin columns using water eluent

    Institute of Scientific and Technical Information of China (English)

    Daisuke KOZAKI; Nobutakc NAKATANI; Masanobu MORI; Nobukazu NAKAGOSHI; Kazuhiko TANAKA

    2012-01-01

    A unified ion-exclusion chromatography(IEC)system for monitoring anionic and cationic nutrients like NH+4,NO-2,NO-3,phosphate ion,silicate ion and HCO-3 was developed and applied to several environmental waters.The IEC system consisted of four IEC methodologies,including the IEC with ultraviolet(UV)detection at 210 nm for determining NH-4 on anion-exchange separation column in OH form connected with anion-exchange UV-conversion column in I-form in tandem,the IEC with UV-detection at 210 nm for determining simultaneously NO-2 and NO-3 on cation-exchange separation column in H+ form,the IEC with UV-detection at 210 nm for determining HCO-3 on cation-exchange separation column in H+ form connected with anionexchange UV-conversion column in I-form in tandem,and the IEC with visible-detection based on molybdenum-blue reaction for determining simultaneously silicate and phosphate ions on cation-exchange separation column in H + form.These IEC systems were combined through three manually-driven 6-port column selection valves to select each separation column to determine selectively the ionic nutrients.Using this sequential water quality monitoring system,the analytical performances such as calibration linearity,reproducibility,detection limit and recovery were also tested under the optimized chromatographic conditions.This novel water quality monitoring system has been applied successfully for the determination of the ionic eutrophication components in sub-urban river waters.

  3. Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha.

    Science.gov (United States)

    Liu, Ying; Xie, Daotao; Kang, Yun; Wang, Yaqin; Yang, Ping; Guo, Jixian; Huang, Jianming

    2016-04-01

    A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE-SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE-SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE-SPE-HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha.

  4. Chromatographic removal and heat inactivation of hepatitis A virus during manufacture of human albumin.

    Science.gov (United States)

    Adcock, W L; MacGregor, A; Davies, J R; Hattarki, M; Anderson, D A; Goss, N H

    1998-08-01

    CSL Limited, an Australian biopharmaceutical company, has recently converted its method of manufacture for human albumin from a traditional Cohn-ethanol fractionation method to a method employing chromatographic techniques. Studies were undertaken to determine the efficiency of the chromatographic and pasteurization steps used in the manufacture of Albumex(R) (CSL's trade name for albumin) in removing and inactivating the potential viral contaminant, hepatitis A virus (HAV). The manufacturing process for Albumex(R) includes three chromatographic steps, two of which are ion-exchange steps (DEAE-Sepharose(R) Fast Flow and CM-Sepharose(R) Fast Flow) and the third is a gel-filtration step (Sephacryl(R) S200 HR). The final stage of the Albumex(R) process involves a bulk pasteurization step where product is held at 60 degrees C for 10 h. HAV partitioning experiments on the DEAE-Sepharose(R) FF and CM-Sepharose(R) FF ion-exchange and Sephacryl(R) S200 HR gel-filtration columns were performed with scaled-down models of the production-scale chromatographic Albumex(R) process. Production samples collected before each of the chromatographic steps were spiked with HAV and processed through each of the scaled-down chromatographic columns. Samples collected during processing were assayed and the log10 reduction factors calculated. Inactivation kinetics of HAV were examined during the pasteurization of Albumex(R) 5 and 20 [5% and 20% (w/v) albumin solutions] held at 60 degrees C for 10 h. Log10 reductions for HAV through the DEAE-Sepharose(R) FF, CM-Sepharose(R) FF and Sephacryl(R) S200 HR chromatographic columns were 5.3, 1.5 and 4.2 respectively, whereas a 4.4 and a greater than 3.9 log10 reduction in HAV in Albumex(R) 5 and 20 respectively were achieved during pasteurization.

  5. Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

    Directory of Open Access Journals (Sweden)

    Nataša Gros

    2013-06-01

    Full Text Available This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as completely as possible. The sections—Selected Anions, Selected Cations and Metals—follow. The most essential experimental conditions used in different methods are summarized in tables for a rapid comparison. Techniques encountered in the reviewed articles comprise: direct determinations of ions in untreated samples with ion- or ion-exclusion chromatography, or electrostatic ion chromatography; matrix elimination with column-switching; pre-concentration with a chelation ion chromatography and purge-and-trap pre-concentration. Different detection methods were used: non-suppressed conductometric or suppressed conductometric, direct spectrometric or spectrometric after a post-column derivetization, and inductively coupled plasma in combination with optical emission or mass spectrometry.

  6. Interpretative optimization of the isocratic ion chromatographic separation of anions

    Directory of Open Access Journals (Sweden)

    Todorović Žaklina N.

    2016-01-01

    Full Text Available Interpretive retention modeling was utilized to optimize the isocratic ion chromatographic (IC separation of the nine anions (formate, fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfate, oxalate. The carbonate-bicarbonate eluent was used and separation was done on a Dionex AS14 ion-exchange column. The influence of combined effects of two mobile phase factors, the total eluent concentration (2 - 6 mM and the carbonate/bicaronate ratio from 1:9 to 9:1 (which corespondent to pH range 9.35 - 11.27, on the IC separation was studied. The multiple species analyte/eluent model that takes into account ion-exchange equilibria of the eluent and sample anions was used. In order to estimate the parameters in the model, a non-linear fitting of the retention data, obtained at two-factor three-level experimental design, was applied. To find the optimal conditions in the experimental design, the normalized resolution product as a chromatographic objective function was employed. This criterion includes both the individual peak resolution and the total analysis time. A good agreement between experimental and simulated chromatograms was obtained. [Projekat Ministarstva nauke Republike Srbije, br. III43009

  7. Adsorption behavior of plasmid DNA onto perfusion chromatographic matrix

    Institute of Scientific and Technical Information of China (English)

    Miladys LIMONTA; Lourdes ZUMALACARREGUI; Dayana SOLER

    2012-01-01

    Anion exchange chromatography is the most popular chromatographic method for plasmid separa-tion.POROS RI 50 is a perfusion chromatographic support which is a reversed phase matrix and is an alterna-tive to conventional ones due to its mass transfer properties.The adsorption and elution of the pIDKE2 plasmidonto reversed phase POROS RI 50 was studied.Langmuir isotherm model was adjusted in order to get the max-imum adsorption capacity and the dissociation constant for POROS RI 50-plasmid DNA (pDNA) system.Break-through curves were obtained for volumetric flows between 0.69-3.33mL/min,given dynamic capacity up to2.3 times higher than those reported for ionic exchange matrix used during the purification process of plasmidswith similar size to that of pIDKE2.The efficiency was less than 45% for the flow conditions and initial concen-tration studied,which means that the support will not be operated under saturation circumstances.

  8. Development, modelling, optimisation and scale-up of chromatographic purification of a therapeutic protein

    DEFF Research Database (Denmark)

    Mollerup, Jørgen; Hansen, Thomas Budde; Kidal, Steffen;

    2007-01-01

    Development of a chromatographic purification step proceeds through a number of stages. High-throughput screening techniques are used to identify suitable resins. This technique is also suitable for the design of a capture step and some intermediate chromatographic steps, but development and true...... optimisation of a purification step necessitate simulations and thus models of the adsorption isotherm. A model for ion-exchange is reviewed and the strategy for estimation of model parameters is reported. Examples are shown where computer simulations are used for development and optimisation...

  9. Purification of recombinant virus-like particles of porcine circovirus type 2 capsid protein using ion-exchange monolith chromatography.

    Science.gov (United States)

    Zaveckas, Mindaugas; Snipaitis, Simas; Pesliakas, Henrikas; Nainys, Juozas; Gedvilaite, Alma

    2015-06-01

    Diseases associated with porcine circovirus type 2 (PCV2) infection are having a severe economic impact on swine-producing countries. The PCV2 capsid (Cap) protein expressed in eukaryotic systems self-assemble into virus-like particles (VLPs) which can serve as antigens for diagnostics or/and as vaccine candidates. In this work, conventional adsorbents as well as a monolithic support with large pore sizes were examined for the chromatographic purification of PCV2 Cap VLPs from clarified yeast lysate. Q Sepharose XL was used for the initial separation of VLPs from residual host nucleic acids and some host cell proteins. For the further purification of PCV2 Cap VLPs, SP Sepharose XL, Heparin Sepharose CL-6B and CIMmultus SO3 monolith were tested. VLPs were not retained on SP Sepharose XL. The purity of VLPs after chromatography on Heparin Sepharose CL-6B was only 4-7% and the recovery of VLPs was 5-7%. Using ion-exchange chromatography on the CIMmultus SO3 monolith, PCV2 Cap VLPs with the purity of about 40% were obtained. The recovery of VLPs after chromatography on the CIMmultus SO3 monolith was 15-18%. The self-assembly of purified PCV2 Cap protein into VLPs was confirmed by electron microscopy. Two-step chromatographic purification procedure of PCV2 Cap VLPs from yeast lysate was developed using Q Sepharose XL and cation-exchange CIMmultus SO3 monolith.

  10. 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.

  11. The magnetic Curie temperature and exchange coupling between cations in tetragonal spinel oxide Mn{sub 2.5}M{sub 0.5}O{sub 4} (M = Co, Ni, Mn, Cr, and Mg) films

    Energy Technology Data Exchange (ETDEWEB)

    Kuo, K.; Cheng, C. W.; Chern, G. [Physics Department and SPIN Research Center, National Chung Cheng University, Chia-Yi, Taiwan, 621 (China)

    2012-04-01

    Mn{sub 3}O{sub 4} is a Jahn-Taller tetragonal ferrite that has a relatively low Curie temperature (T{sub c}) of {approx}43 K due to weak coupling between the canting spins. In this study, we fabricated a series of 100-nm-thick Mn{sub 2.5}M{sub 0.5}O{sub 4} (M = Co, Ni, Mn, Cr, and Mg) films via oxygen-plasma-assisted molecular beam epitaxy and measured the structural and magnetic properties of these films. These films show single phase quality, and the c-axis lattice parameter of pure Mn{sub 3}O{sub 4} is 0.944 nm, with a c/a ratio {approx}1.16, consistent with the bulk values. The replacement of Mn by M (M = Co, Ni, Cr, and Mg) changes the lattice parameters, and the c/a ratio varies between 1.16 and 1.06 depending upon the cation distribution of the films. The magnetic Curie temperatures of these films also vary in the range of 25-66 K in that Ni and Co enhance the T{sub c} whereas Mg reduces the T{sub c} (Cr shows no effect on the T{sub c}). These changes to the T{sub c} are related to both the element electronic state and the cation distributions in these compounds. As a non-collinear spin configuration can induce electrical polarization, the present study provides a systematic way to enhance the magnetic transition temperature in tetragonal spinel ferrites.

  12. Cation exchange for mercury and cadmium of xanthated, sulfonated, activated and non-treated subbituminous coal, commercial activated carbon and commercial synthetic resin:effect of pre-oxidation on xanthation of subbituminous coal

    Institute of Scientific and Technical Information of China (English)

    Lewis M. Gomez; Fredy Colpas-Castillo; Roberto Fernandez-Maestre

    2014-01-01

    A subbituminous coal was oxidized with air at 150 ?C on a fixed bed for 4 h and xanthated with carbon disulfide in a basic solution, at 30 or 5–10 ?C. This xanthated coal was evaluated for the removal of Hg2? and Cd2? from 7,000 mg/L aqueous solutions; metal concentrations were determined by atomic absorption spectrometry. The ion exchange of the xanthated coal was compared against those of the original subbituminous coal, a sulfonated subbituminous coal, activated carbon, commercial activated carbon, and commercial synthetic resin. The commercial synthetic resin showed the highest exchange capacity (concentration factor 98%) followed by the xanthated coal (concentration factor 96%). The retention of cadmium on the sulfonated subbituminous coal was lower (exchange capacity 0.56 meq/g) than that of xanthated coals (1.85 ± 0.09 meq/g). Our xanthated coal showed a better Cd2? removal (81%against 15%) than a non preoxidized 40-h-xanthated coal, which shows that oxidation of coal increased the amount of oxygenated groups which enhanced xanthation.

  13. Purification of Transglutaminase from High Salt Culture by Gel and Cation Exchange Chromatography%凝胶层析和离子交换层析结合法纯化高盐发酵液中谷氨酰胺转胺酶

    Institute of Scientific and Technical Information of China (English)

    张莉丽; 张兰威; 杜明; 韩雪; 易华西; 张英春; 张艳禾; 马微

    2012-01-01

    To purify the transglutaminase from high-salt medium, gel filtration combined with ion exchange chromatography method was employed. Two-step chromatographic conditions (flow rate and the sample volume) were optimized. The final sample volume and a flow rate for Gel chromatography were 6 mL and 0. 25 mL/min, respectively. Conditions for ion-exchange chromatography were a sample volume of 50 mL and flow rate of 3 mL/min. Enzyme was purified 4.22-fold, the specific activity and the recovery rate were 17. 33 U/mg protein and 77. 5%, respectrively. A comparison between liquid chromatography/tandem mass spectrometric identification and the protein database was carried out and the results showed that the purified enzyme had high homology with AAN01353.%采用凝胶层析和离子交换层析相结合的方法分离纯化高盐培养基中的谷氨酰胺转胺酶,优化的凝胶层析的条件,上样量6mL,流速为0.25 mL/min;离子交换层析的上样量50 mL,流速为3 mL/min.酶被纯化了4.22倍,比活力达17.33 U/mg蛋白,回收率为77.5%.液相色谱-串联质谱鉴定、蛋白质数据库比对结果表明,纯酶与AAN01353是同种蛋白质.

  14. Selective arsenic speciation analysis of human urine reference materials using gradient elution ion-exchange HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2004-01-01

    Arsenic speciation analysis was performed in two human urine certified reference materials (NIES No. 18 and NIST SRM2670a) and three human urine control materials (Seronorm, Medisafe and Lyphocheck). The samples were diluted 1 + 3 prior to analysis by gradient elution anion or cation exchange high-performance...... liquid chromatography ( HPLC) coupled with inductively coupled plasma mass spectrometry (ICP-MS). Nine arsenic species, including arsenic acid, arsenous acid, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine, trimethylarsine oxide, dimethylarsinoylacetic acid, trimethylarsoniopropionate...... and dimethylarsinoylethanol, were determined in the urines. Additionally, several unknown arsenicals were detected. This is the first time that dimethylarsinoylacetic acid and trimethylarsoniopropionate have been reported in human urine. The sums of the species concentrations determined by the chromatographic approaches were...

  15. Chromatographic separation process with pellicular ion exchange resins that can be used for ion or isotope separation and resins used in this process. Procede de separation chromatographique au moyen de resines echangeuses d'ions pelliculaires, utilisable notamment pour la separation des isotopes ou des ions, et resines utilisables dans ce procede

    Energy Technology Data Exchange (ETDEWEB)

    Carles, M.; Neige, R.; Niemann, C.; Michel, A.; Bert, M.; Bodrero, S.; Guyot, A.

    1989-01-06

    For separation of uranium, boron or nitrogen isotopes, an isotopic exchange is carried out betwen an isotope fixed on an ion exchange resin and another isotope of the same element in the liquid phase contacting the resin. Pellicular resins are used comprising composite particulates with an inert polymeric core and a surface layer with ion exchange groups.

  16. CHROMATOGRAPHIC REFOLDING OF PROTEINS: MOLECULAR ACTION AND COLUMN CONTROL

    Institute of Scientific and Technical Information of China (English)

    Fangwei Wang; Yongdong Liu; Jing Chen; Zhiguo Su

    2005-01-01

    Protein expression in E. coli often results in the formation of a kind of protein aggregate called inclusion body. Conversion of the inactive protein aggregate into biologically active protein is a key step in production of recombinant products. Conventional dilution refolding technique suffers from disadvantages of low recovery and low concentration. Various chromatographic refolding techniques have been developed over the last few years. These include size-exclusion chromatography, ion exchange chromatography, hydrophobic interaction chromatography and different affinity chromatography. A successful strategy is the use of gradient elution in column control which provides a gentle and gradual change of the solution environment for the macromolecule to refold at nano-scale. The gradient refolding at column scale could minimize misfolding and aggregation which are induced by sudden change of the solution in conventional refolding operation.

  17. Zebrafish ("Danio rerio") endomembrane antiporter similar to a yeast cation/H(+) transporter is required for neural crest development

    Science.gov (United States)

    CAtion/H (+) eXchangers (CAXs) are integral membrane proteins that transport Ca (2+) or other cations by exchange with protons. While several yeast and plant CAX proteins have been characterized, no functional analysis of a vertebrate CAX homologue has yet been reported. In this study, we further ch...

  18. Effect of polyamine reagents on exchange capacity in ion exchangers

    Science.gov (United States)

    Petrova, T. I.; Dyachenko, F. V.; Bogatyreva, Yu. V.; Borodastov, A. K.; Ershova, I. S.

    2016-05-01

    Effect of compounds involved in complex reagents is described using Helamin 906H reagent as an example. The working exchange capacity of KU-2-8chs cation exchanger in hydrogen form and Amberlite IRA 900Cl anion exchanger in OH form remained almost unchanged when they were used repeatedly to purify water that contained Helamin 906H reagent; in addition, this capacity was the same upon filtration of water that did not contain this reagent. Leakage of total organic carbon was observed earlier than that of calcium ions upon filtration of the solution through the cation exchanger layer. The test results obtained in industrial conditions indicated that using H-OH filters to purify turbine condensate enables the decrease of the concentration of organic and other impurities therein.

  19. Electrochromatographic properties of synthetic poly(styrene-divinylbenzene) encapsulated packing material and sulphonic cation-exchange phase based on the former%合成聚(苯乙烯-二乙烯苯)包覆填料及基于此填料经磺酰化得到的阳离子交换型固定相的色谱行为考察

    Institute of Scientific and Technical Information of China (English)

    李菠; 李永山; 韩南银; 徐秉玖

    2003-01-01

    Objective: To develop new kinds of stationary phases suitable for applications in capillary electrochromatography (CEC), as well as in LC, which can be tailored to realize selective separations of solutes difficult to separate with conventional stationary phases. Methods:Purchased spherical silica particles (5 μm) were refluxed in anhydrous toluene with vinyl-triethoxysilane for 18 h, to modify the surface with vinylsilyl groups. The silylated silica particles were subsequently stirred in an n-henanol-acetonitril mixture (1∶ 4, volume fraction) for 18 h. Styrene and divinylbenzene in the mixture co-polymerized to form a crosslinked encapsulation layer on the silica surface, and bonded on the surface vinyl groups at the same time, both reactions were initiated by azo-iso-butyronitrile. The poly(Styrene-divinylbenzene) encapsulated silica(PS-DES) produced can be used as a non-conventional stationary phase for CEC itself. By sulphonation of the PS-DES phase with chlorosulphonic acid, strong cation-exchange stationary phase of sulphonic type was obtained. Results: The manufactured PS-DES as well as the sulphonated phases were respectively packed into capillaries,and the columns thus prepared were tested for their chromatographic characteristics. It was found that the PS-DES phase showed reversed-phase characteristics. Due to the phenyl groups in the encapsulated polymer, it introduced π-π electronic interaction between the solutes molecules and stationary phase during the chromatographic separation process, therefore it showed unique selectivity on separating aromatic compounds, also polar- as well as some alkaline drugs was analyzed on the column packed with the phase. It was demonstrated that the sulphonated phase could be used to prepare columns for the separation of alkaline drugs, symmetric peaks were obtained for them and base-line separation was realized. Conclusion: It is possible that these stationary phases prepared can be used for solving the analytical

  20. Role of extracellular cations in cell motility, polarity, and chemotaxis

    Directory of Open Access Journals (Sweden)

    Soll D

    2011-04-01

    Full Text Available David R Soll1, Deborah Wessels1, Daniel F Lusche1, Spencer Kuhl1, Amanda Scherer1, Shawna Grimm1,21Monoclonal Antibody Research Institute, Developmental Studies, Hybridoma Bank, Department of Biology, University of Iowa, Iowa City; 2Mercy Medical Center, Surgical Residency Program, Des Moines, Iowa, USAAbstract: The concentration of cations in the aqueous environment of free living organisms and cells within the human body influence motility, shape, and chemotaxis. The role of extracellular cations is usually perceived to be the source for intracellular cations in the process of homeostasis. The role of surface molecules that interact with extracellular cations is believed to be that of channels, transporters, and exchangers. However, the role of Ca2+ as a signal and chemoattractant and the discovery of the Ca2+ receptor have demonstrated that extracellular cations can function as signals at the cell surface, and the plasma membrane molecules they interact with can function as bona fide receptors that activate coupled signal transduction pathways, associated molecules in the plasma membrane, or the cytoskeleton. With this perspective in mind, we have reviewed the cationic composition of aqueous environments of free living cells and cells that move in multicellular organisms, most notably humans, the range of molecules interacting with cations at the cell surface, the concept of a cell surface cation receptor, and the roles extracellular cations and plasma membrane proteins that interact with them play in the regulation of motility, shape, and chemotaxis. Hopefully, the perspective of this review will increase awareness of the roles extracellular cations play and the possibility that many of the plasma membrane proteins that interact with them could also play roles as receptors.Keywords: extracellular cations, chemotaxis, transporters, calcium, receptors

  1. Sorption of the organic cation metoprolol on silica gel from its aqueous solution considering the competition of inorganic cations.

    Science.gov (United States)

    Kutzner, Susann; Schaffer, Mario; Börnick, Hilmar; Licha, Tobias; Worch, Eckhard

    2014-05-01

    Systematic batch experiments with the organic monovalent cation metoprolol as sorbate and the synthetic material silica gel as sorbent were conducted with the aim of characterizing the sorption of organic cations onto charged surfaces. Sorption isotherms for metoprolol (>99% protonated in the tested pH of around 6) in competition with mono- and divalent inorganic cations (Na(+), NH4(+), Ca(2+), and Mg(2+)) were determined in order to assess their influence on cation exchange processes and to identify the role of further sorptive interactions. The obtained sorption isotherms could be described well by an exponential function (Freundlich isotherm model) with consistent exponents (about 0.8). In general, a decreasing sorption of metoprolol with increasing concentrations in inorganic cations was observed. Competing ions of the same valence showed similar effects. A significant sorption affinity of metoprolol with ion type dependent Freundlich coefficients KF,0.77 between 234.42 and 426.58 (L/kg)(0.77) could still be observed even at very high concentrations of competing inorganic cations. Additional column experiments confirm this behavior, which suggests the existence of further relevant interactions beside cation exchange. In subsequent batch experiments, the influence of mixtures with more than one competing ion and the effect of a reduced negative surface charge at a pH below the point of zero charge (pHPZC ≈ 2.5) were also investigated. Finally, the study demonstrates that cation exchange is the most relevant but not the sole mechanism for the sorption of metoprolol on silica gel.

  2. 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.

  3. Recycling asymmetric hydrogenation catalysts by their immobilisation onto ion-exchange resins.

    Science.gov (United States)

    Barbaro, Pierluigi; Bianchini, Claudio; Giambastiani, Giuliano; Oberhauser, Werner; Bonzi, Laura Morassi; Rossi, Filippo; Dal Santo, Vladimiro

    2004-06-21

    New systems based on cationic chiral phosphine-rhodium complexes anchored to a commercial cation-exchange gel-type resin showed high efficiency and easy recycling in the asymmetric hydrogenation of prochiral olefins.

  4. Chemically modified polymeric resins for separation of cations, organic acids, and small polar moleculea by high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Morris, J.B.

    1993-07-01

    This thesis is divided into 4 parts: a review, ion chromatography of metal cations on carboxylic resins, separation of hydrophilic organic acids and small polar compounds on macroporous resin columns, and use of eluent modifiers for liquid chromatographic separation of carboxylic acids using conductivity detection.

  5. Two different cationic positions in Cu-SSZ-13?

    Science.gov (United States)

    Hun Kwak, Ja; Zhu, Haiyang; Lee, Jong H; Peden, Charles H F; Szanyi, János

    2012-05-16

    H(2)-TPR and FTIR were used to characterize the nature of the Cu ions present in the Cu-SSZ-13 zeolite at different ion exchange levels. The results obtained are consistent with the presence of Cu ions at two distinct cationic positions in the SSZ-13 framework.

  6. Two different cationic positions in Cu-SSZ-13?

    Energy Technology Data Exchange (ETDEWEB)

    Kwak, Ja Hun; Zhu, Haiyang; Lee, Jong H.; Peden, Charles HF; Szanyi, Janos

    2012-04-18

    H2-TPR and FTIR were used to characterize the Cu ions present in Cu-SSZ-13 zeolite at different ion exchange levels. The results obtained are consistent with the presence of Cu ions in two distinct cationic positions of the SSZ-13 framework.

  7. Functional chromatographic technique for natural product isolation†

    OpenAIRE

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.; La Clair, James J.; Chapman, Eli

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation.

  8. Chromatographic methods in the study of autism.

    Science.gov (United States)

    Żurawicz, Ewa; Kałużna-Czaplińska, Joanna; Rynkowski, Jacek

    2013-10-01

    Research into biomarkers of autism is a new means of medical intervention in this disease. Chromatographic techniques, especially coupled with mass spectrometry, are widely used in determination of biomarkers and assessment of effectiveness of autism therapy owing to their sensitivity and selectivity. Among the chromatographic techniques gas chromatography and liquid chromatography, especially high-performance liquid chromatography, have found application in clinical trials. The high-performance liquid chromatography technique allows an analysis of liquid samples with a wide range of molecules, small and large, providing an opportunity to perform advanced assays within a short time frame. Gas chromatography with the appropriate preparation of samples (gaseous and liquid) and a selection of analysis conditions enables the separation of thermally stable, volatile and non-volatile organic substances in short runtimes. The chromatographic techniques that are currently used in metabolic studies in autism are designed to identify abnormalities in three areas: the metabolism of neurotransmitters, nutritional and metabolic status and manifestations of oxidative stress. This review presents a necessary theoretical introduction and examples of applications of chromatographic studies of disorder markers in autism.

  9. 40 CFR 1065.267 - Gas chromatograph.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  10. Cyclic electrophoretic and chromatographic separation methods

    NARCIS (Netherlands)

    Eijkel, Jan C.T.; Berg, van den Albert; Manz, Andreas

    2004-01-01

    A review is given of the application of cyclic analytical methods in capillary electroseparation (CE) and liquid chromatography (LC) systems. Cyclic methods have been used since the early sixties in chromatographic systems to overcome pressure limitations to resolution. From the early nineties on th

  11. Functional chromatographic technique for natural product isolation†

    Science.gov (United States)

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation. PMID:25588099

  12. Effects of hydrochloric acid modification on the channel characteristics, composition, surface potential and cation exchange behavior of natural clinoptilolite%盐酸改性对天然斜发沸石孔道特征、成分、表面电位及阳离子交换性能的影响

    Institute of Scientific and Technical Information of China (English)

    霍汉鑫; 林海; 董颖博; 刘泉利; 曹丽霞; 程皝; 汪涵; 傅川

    2015-01-01

    采用不同浓度盐酸对天然斜发沸石进行改性,并系统地研究了改性沸石的孔道特征、化学成分、表面电位及阳离子交换性能的变化.盐酸改性后,沸石晶体结构破坏较小,表面变得疏松粗糙,K+、Na+、Ca2+和Mg2+元素含量均小幅下降;表面负电荷增加,阳离子交换容量减小;比表面积和总孔体积均有所提高,最高分别从原沸石的35.97 m2·g -1和0.0761 m3·g-1提高至64.46 m2·g-1和0.1156 m3·g-1.盐酸改性对沸石微孔、介孔和大孔的分布影响明显.从迟滞回线形状判断沸石孔道类型均为不均匀狭缝型孔道,盐酸改性不会改变沸石孔道类型.%ABSTRACT Natural clinoptilolite was modified by different concentrations of hydrochloric acid. Systemic investigations were performed on the channel characteristics, chemical composition, surface potential, and cation exchange behavior of the modified clinoptilolite. It is found that the surface of the modified clinoptilolite becomes loose and rough, the contents of K+, Na+, Ca2+, and Mg2+ slightly decrease, the surface negative charges increases, and the cation exchange capacity decreases to some extent. The specif-ic surface area and total pore volume are improved and the maximum values of them increase from 35.97 m2·g-1 and 0.0761 m3·g-1 to 64.46 m2·g-1 and 0.1156 m3·g-1 , respectively. The distribution of micropores, mesopores, and macropores is obviously impacted, and the type of zeolite cavities is determined to be uneven slits by the hysteresis loop shape, indicating that this acid modification cannot change zeolite cavities.

  13. 基于大肠杆菌蛋白质质谱鉴定的阳离子交换色谱优化研究%Optimization of conditions for the separation with strong cation exchange chromatography based on Escherichia coli protein for mass spectrometry identification

    Institute of Scientific and Technical Information of China (English)

    朱平川; 岑卫健; 付强; 胡炜; 卢洁

    2014-01-01

    As a research of tryptic digestion products from Escherichia coli protein , on the extraction efficiency of protein were studied in this paper ,The focus is on the separation conditions of strong cation used multidimensional chromatography exchange chromatography . The conditions included the buffer species ,pH ,the type of the salt in mobile phase ,the proportion of organic solvent added in the elution solution ,and the loading amount of the sample .The results showed that ,in the power of 400 W ,ultrasonic time was 15 minutes ,achieved the highest extraction efficiency of protein . In the strong cation exchange chromatography separation of linear sample volume range ,10 mmol/L potassium dihydrogen phosphate (pH = 3 .0 ) of mobile phases and 30% (V/V ) organic solvent in mobile phases as buffer system ,as washing desalination in potassium chloride solution ,can obtain the best separation results .%以大肠杆菌蛋白质的胰蛋白酶切产物为研究对象,对蛋白质的提取效率进行初步探讨,重点是对多维色谱分离中常用的强阳离子交换色谱的分离条件,包括缓冲液的种类、pH值,洗脱盐的种类、有机溶剂的比例以及上样量进行了考察和比较.结果表明:功率为400 W ,超声时间为15 min ,蛋白质的提取效率达到最高.在强阳离子交换色谱分离线性上样量范围内,10 mmol/L磷酸二氢钾(pH=3.0)作为缓冲体系,在氯化钾溶液作为洗脱盐、流动相中乙腈的体积分数为30%的条件下进行梯度洗脱时,可获得最佳的分离结果.

  14. Tadpole toxicity prediction using chromatographic systems.

    Science.gov (United States)

    Fernández-Pumarega, Alejandro; Amézqueta, Susana; Fuguet, Elisabet; Rosés, Martí

    2015-10-30

    Toxicity has been emulated in tadpole species through chromatographic systems. The parameter studied to evaluate the non-specific toxicity of a compound is the narcosis concentration (Cnar), which is defined as the concentration needed for the immobilization of the organism. Because experimental investigation with animals is lengthy, costly, technically difficult, and ethically questionable, there is a great interest in developing surrogate physicochemical systems able to emulate biological systems to obtain the same information in a faster, more economic, and easier manner. In order to see which chromatographic systems would be able to emulate tadpole narcosis, both, tadpole narcosis data and data in several chromatographic and electrophoretic systems, were fitted to a linear solvation energy relationship (LSER) model. Thus, by comparison of the models it was possible to see which of the chromatographic systems were more similar to the biological one. The physicochemical systems that best emulate tadpole narcosis were an HPLC system based on an immobilized artificial membrane (IAM) column, and two micellar electrokinetic chromatography (MEKC) systems based on sodium taurocholate (STC) and a mixture of sodium dodecylsulphate (SDS) and Brij 35 as surfactants. A system based on a RP18 HPLC column also was selected for comparison because it is a common column in most analytical laboratories. To establish the models, a set of compounds with known Cnar values were analyzed in the chromatographic, and electrophoretic selected systems and, then, the retention factor (k) was correlated to the concentration of narcosis. Statistics showed that the system based on STC micelles was the best to emulate toxicity in tadpoles. The robustness and predictive ability of the developed models were validated.

  15. Competitive Effects of 2+ and 3+ Cations on DNA Compaction

    CERN Document Server

    Tongu, C; Yoshikawa, Y; Zinchenko, A A; Chen, N; Yoshikawa, K

    2016-01-01

    By using single-DNA observation with fluorescence microscopy, we observed the effects of divalent and trivalent cations on the higher-order structure of giant DNA (T4 DNA with 166 kbp). It was found that divalent cations, such as Mg(2+) and Ca(2+), inhibit DNA compaction induced by a trivalent cation, spermidine (SPD(3+)). On the other hand, in the absence of SPD(3+), divalent cations cause the shrinkage of DNA. These experimental observations are inconsistent with the well-established Debye-Huckel scheme regarding the shielding effect of counter ions, which is given as the additivity of contributions of cations with different valences. We interpreted the competition between 2+ and 3+ cations in terms of the change in the translational entropy of the counter ions before and after the folding transition of DNA. For the compaction with SPD(3+), we considered the increase in translational entropy due to the ion-exchange of the intrinsic monovalent cations condensing on a highly-charged polyelectrolyte, double-st...

  16. Atmospheric CO2 enrichment facilitates cation release from soil.

    Science.gov (United States)

    Cheng, L; Zhu, J; Chen, G; Zheng, X; Oh, N-H; Rufty, T W; Richter, D deB; Hu, S

    2010-03-01

    Atmospheric CO(2) enrichment generally stimulates plant photosynthesis and nutrient uptake, modifying the local and global cycling of bioactive elements. Although nutrient cations affect the long-term productivity and carbon balance of terrestrial ecosystems, little is known about the effect of CO(2) enrichment on cation availability in soil. In this study, we present evidence for a novel mechanism of CO(2)-enhancement of cation release from soil in rice agricultural systems. Elevated CO(2) increased organic C allocation belowground and net H(+) excretion from roots, and stimulated root and microbial respiration, reducing soil redox potential and increasing Fe(2+) and Mn(2+) in soil solutions. Increased H(+), Fe(2+), and Mn(2+) promoted Ca(2+) and Mg(2+) release from soil cation exchange sites. These results indicate that over the short term, elevated CO(2) may stimulate cation release from soil and enhance plant growth. Over the long-term, however, CO(2)-induced cation release may facilitate cation losses and soil acidification, negatively feeding back to the productivity of terrestrial ecosystems.

  17. Rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography using a monolithic column

    Institute of Scientific and Technical Information of China (English)

    Xu Huang; Hong Yu; Ying Jie Dong

    2012-01-01

    A method for rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography with ultraviolet detection was developed.Chromatographic separations were performed on a reversed-phase silica-based monolithic column using 1-heptanesulfonic acid sodium-acetonitrile as mobile phase.The effects of ion-pair reagent and acetonitrile concentration on retention of the cations were investigated.The retention times of the cations accord with carbon number rule.The method has been successfully applied to the determination of four ionic liquids synthesized by organic chemistry laboratory.

  18. 阳离子交换法制备稳定的近红外区核/壳型PbS/CdS量子点%Utilizing Cation Exchange Method to Produce Core/Shell PbS/CdS Quantum Dots with Stable Infrared Emission

    Institute of Scientific and Technical Information of China (English)

    李谦; 张腾; 古宏伟; 丁发柱; 屈飞; 彭星煜; 王洪艳; 吴战鹏

    2013-01-01

    硫化铅量子点(PbS QDs)的光氧化稳定性差是其应用于太阳能电池等领域的主要限制因素之一.采用阳离子交换法在合成的PbS量子点表面包裹一层具有更稳定、更大禁带宽度的硫化镉(CdS)壳层,制备出稳定的核/壳型PbS/CdS量子点;同时,研究了反应温度和反应时间对阳离子交换过程的影响规律.通过透射电子显微镜和高分辨透射电子显微镜(TEM/HRTEM)、X射线衍射仪(XRD)、吸收光谱和荧光光谱考察了所制备PbS/CdS量子点的结构、光学特性和光氧化稳定性,结果表明:阳离子交换过程中,离子交换反应程度有限、仅发生在量子点的表面层,但极薄的CdS壳层已能有效钝化PbS量子点的表面缺陷、显著提高其光氧化稳定性.%PbS quantum dots (QDs) have enormous potential for applications ranging from tunable infrared lasers to solar cells due to their efficient emission over a large spectral range in the infrared.Especially,multiple exciton generation has been observed in PbS QDs,which makes PbS QDs have great potential for high-efficiency solar cells.However,these applications have been limited by instability in emission quantum yield and peak position on exposure to ambient conditions.An effective strategy to improve PbS QDs' stability is overgrowth with a shell of a more stable semiconductor,such as CdS,resulting in core/shell PbS/CdS QDs.The PbS/CdS QDs were fabricated in a two-step method.In the first step,PbS QDs with a 4.8 nm diameter were prepared by using organic metal.Second,PbS/CdS QDs with 3.8 nm PbS core and 0.5 nm CdS shell were fabricated by exposing PbS QDs in Cd2+ solution for 24 h at 65 ℃.In this article,cation exchange method was adopted to moderate reaction temperature in a low temperature,so that Ostwald ripening in high temperature was avoided.The results of transmission electron microscopy (TEM) and high resolution TEM showed that PbS QDs were sphere and in a cubic cystal without obvious

  19. Effects of ionizing radiation on modern ion exchange materials

    Energy Technology Data Exchange (ETDEWEB)

    Marsh, S.F.; Pillay, K.K.S.

    1993-10-01

    We review published studies of the effects of ionizing radiation on ion exchange materials, emphasizing those published in recent years. A brief overview is followed by a more detailed examination of recent developments. Our review includes styrene/divinylbenzene copolymers with cation-exchange or anion-exchange functional groups, polyvinylpyridine anion exchangers, chelating resins, multifunctional resins, and inorganic exchangers. In general, strong-acid cation exchange resins are more resistant to radiation than are strong-base anion exchange resins, and polyvinylpyridine resins are more resistant than polystyrene resins. Cross-linkage, salt form, moisture content, and the surrounding medium all affect the radiation stability of a specific exchanger. Inorganic exchangers usually, but not always, exhibit high radiation resistance. Liquid ion exchangers, which have been used so extensively in nuclear processing applications, also are included.

  20. Determination of effective capacities of ion-exchangeable materials by measuring the equilibrium conductivity.

    Science.gov (United States)

    Okabe, Toshiaki; Yokoyama, Yukio

    2010-01-01

    The effective ion-exchange capacities of ion-exchange materials were determined by measuring the change in the equilibrium conductivity of a column packed with analyte. The developed instrumental method can provide effective ion-exchange capacities for both cation and anion exchangers with simple operations. The cation-exchange capacity of a weak-acid cation-exchange resin (TSKgel SuperIC-Cation column) depended on the conditioning pH and the molar concentration of the conditioning agent. Plots of effective cation-exchange capacities over the conditioning pH exhibited three inflection points, suggesting the presence of two carboxy groups and one phenolic OH group in the resin, probably due to the inherent base polymer. This method was applied to several commercial analytical columns for ion chromatography, and could provide scientifically useful results for characterizing the resin properties.

  1. Controlling chemistry with cations: photochemistry within zeolites.

    Science.gov (United States)

    Ramamurthy, V; Shailaja, J; Kaanumalle, Lakshmi S; Sunoj, R B; Chandrasekhar, J

    2003-08-21

    The alkali ions present in the supercages of zeolites X and Y interact with included guest molecules through quadrupolar (cation-pi), and dipolar (cation-carbonyl) interactions. The presence of such interactions can be inferred through solid-state NMR spectra of the guest molecules. Alkali ions, as illustrated in this article, can be exploited to control the photochemical and photophysical behaviors of the guest molecules. For example, molecules that rarely phosphoresce can be induced to do so within heavy cation-exchanged zeolites. The nature (electronic configuration) of the lowest triplet state of carbonyl compounds can be altered with the help of light alkali metal ions. This state switch (n pi*-pi pi*) helps to bring out reactivity that normally remains dormant. Selectivity obtained during the singlet oxygen oxidation of olefins within zeolites illustrates the remarkable control that can be exerted on photoreactions with the help of a confined medium that also has active sites. The reaction cavities of zeolites, like enzymes, are not only well-defined and confined, but also have active sites that closely guide the reactant molecule from start to finish. The examples provided here illustrate that zeolites are far more useful than simple shape-selective catalysts.

  2. Media selection in ion-exchange chromatography in a single microplate.

    Science.gov (United States)

    Cabanne, Charlotte; Santarelli, Xavier

    2014-01-01

    High-throughput process development is more and more used in chromatography. Limitations are the tools provided by the manufacturers. Here, we describe a method to select chromatographic media for ion-exchange chromatography using a 96-well filter microplate.

  3. Chromatographic fingerprint analysis of Pycnogenol dietary supplements.

    Science.gov (United States)

    Chen, Pei; Song, Fenhong; Lin, Long-Ze

    2009-01-01

    The bark of maritime pine (Pinus pinaster Aiton) has been widely used as a remedy for various degenerative diseases. A standard high-performance liquid chromatographic (HPLC) procedure for Pycnogenol analysis is a method specified in the United States Pharmacopeia (USP) monograph, which requires measurement of peak areas and identification of four components of the extract: caffeic acid, catechin, ferulic acid, and taxifolin. In this study, a fingerprint analysis using an HPLC method based on the USP monograph has been developed to provide additional qualitative information for the analysis of Pycnogenol-containing dietary supplements (PDS). Twelve commercially available PDS samples were purchased and analyzed along with a standard Pycnogenol extract. Their chromatographic fingerprints were analyzed using principal component analysis. The results showed that two of the samples were not consistent with the standard reference Pycnogenol extract. One contained other active ingredients in addition to Pycnogenol, and the other may have resulted from a quality control issue in manufacturing.

  4. [Effect of emulsion on chromatographic process].

    Science.gov (United States)

    Jiang, Yulei; Li, Xi

    2004-11-01

    The types and features of concentration wave of the chromatographic process in which the mobile phase was emulsion were studied theoretically by the method of characteristics and the concept of multi mobile phase chromatography. When the mobile phase is an emulsion, solute is partitioned between the inner and outer phases of the emulsion as well as simultaneously adsorbed on the stationary phase resulting in the great difference of concentration profiles from the case in which the mobile phase is homogenous. The various profiles and mechanisms of concentration wave of the chromatographic process in which the partition relationship between the inner and outer phases of the emulsion and the adsorption isotherm on the stationary phase were both Langmuir-like were analyzed and discussed with corresponding examples, and the comparison with the case in which the mobile phase is homogenous is also done. It is shown that the chromatographic progress with emulsion is more complicated and multiple. The existence of multi mobile phases may sharpen simple wave to be shock wave or diffuse shock wave to be simple wave.

  5. Trigonal tricationic ionic liquids: a generation of gas chromatographic stationary phases.

    Science.gov (United States)

    Payagala, Tharanga; Zhang, Ying; Wanigasekara, Eranda; Huang, Ke; Breitbach, Zachary S; Sharma, Pritesh S; Sidisky, Leonard M; Armstrong, Daniel W

    2009-01-01

    Trigonal tricationic ionic liquids (ILs) are a new class of ILs that appear to be unique when used as gas chromatographic stationary phases. They consist of four core structures; (1) A = mesitylene core, (2) B = benzene core, (3) C = triethylamine core, and (4) D = tri(2-hexanamido)ethylamine core; to which three identical imidazolium or phosphonium cationic moieties were attached. These were coated on fused silica capillaries, and their gas chromatographic properties were evaluated. They were characterized using a linear solvation parameter model and a number of test mixtures. On the basis of the literature, it is known that both monocationic and dicationic ILs possess almost identical polarities, solvation characteristics, and chromatographic selectivities. However, some of the trigonal tricationic ILs were quite different. The different solvation parameters and higher apparent polarities appear to generate from the more rigid trigonal geometry of these ILs, as well as their ability to retain the positive charges in relatively close proximity to one another in some cases. Their unique selectivities, retention behaviors, and separation efficiencies were demonstrated using the Grob mixture, a flavor and fragrance test mixture, alcohols/alkanes test, and FAME isomer separations. Two ILs C1 (methylimidazolium substitution) and C4 (2-hydroxyethylimidazolium substitution) had higher apparent polarities than any know IL (mono, di, and tricationic ILs) or commercial stationary phases. The tri(2-hexanamido)ethylamine core IL series proved to be very interesting in that it not only showed the highest separation efficiency for all test mixtures, but it also is the first IL stationary phase (containing NTf(2)(-) anions) that eliminates peak tailing for alcohols and other H-bonding analytes. The thermal stabilities were investigated using three methods: thermogravimetric analysis (TGA) method, temperature programmed gas chromatographic method (TPGC), and isothermal gas

  6. Computer simulation of alkali metal cation-montmorillonite hydrates

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Fang-Ru Chou [Columbia Univ., Palisades, NY (United States); Skipper, N.T. [Univ. College, London (United Kingdom); Sposito, G. [Lawrence Berkeley National Lab., CA (United States)

    1997-12-31

    Molecular structure in the interlayers of Li-, Na-, or K-Wyoming montmorillonite with one, two, or three adsorbed water layers was investigated for the first time by concurrent Monte Carlo and molecular dynamics (MD) simulation, based on the Matsouka-Clementi-Yoshimine, (MCY) model of water-water interactions. Calculated layer spacings, as well as interlayer-species self-diffusion coefficients, were in good agreement with available experimental data. Inner-sphere surface complexes of the cations with tetrahedral charge sites were observed for all hydrates, whereas outer-sphere surface complexes of the cations with octahedral charge sites, found also in the one-layer hydrate, tended to dissociate from the clay mineral basal planes into a diffuse layer in the two- and three-layer hydrates. Differences in the interlayer water structure among the hydrates mainly reflected cation solvation, although some water molecules were entrapped within cavities in the montmorillonite surface. All of the interlayer cation and water species exchanged on the time scale (0.2 ns) of the MD simulations. Comparisons with results obtained using, instead of the MCY model, the TIP4P model for water-water, cation-water, and cation-clay interactions indicated that layer spacings and interlayer species mobilities tend to be under-predicted by the TIP4P model.

  7. Thin layer chromatographic separation of cobalt from nickel on impregnated silica gel layers:quantitative determination by digital image analysis%Thin layer chromatographic separation of cobalt from nickel on impregnated silica gel layers: quantitative determination by digital image analysis

    Institute of Scientific and Technical Information of China (English)

    P A MOHAMED NAJAR; R G SONALI; M T NIMJE; K V RAMANA RAO

    2012-01-01

    Thin layer chromatography (TLC) of cobalt and nickel has been performed on silica gel layers induced with alkali mediated cellulose extract.A novel combination of 10% aqueous solutions of Tween-20 and potassium thiocyanate in 1∶ 1 (v/v) was identified as the best mobile phase for the selective separation of Co2+ from Ni2+ on the impregnated Silica Gel G layers.The chromatographic characteristics of the cations were studied and the limits of detection as well as the limits of quantification for Co2+ and Ni2+ were determined.The quantitative estimation of the cations was achieved from the digital image analysis of respective chromatograms.The proposed quantitative method was successfully applied with 0-0.50% error for the determination of Co2+ from Ni2+ in spiked samples of bauxite,soil and rock containing common cations such as Al3+,Fe2+,Ti4+,Zn2+,Mn2+,Cu2+,Cr6+,Mg2+ etc.under the optimized chromatographic conditions.

  8. Cation-{pi}-interaction promoted aggregation of aromatic molecules and energy transfer within Y zeolites

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, K.J.; Sunoj, R.B.; Chandrasekhar, J.; Ramamurthy, V.

    2000-05-30

    Photophysical studies of naphthalene confirm that aromatic molecules tend to aggregate within cation exchanged Y zeolites. Ground-state aggregation is traced to the presence of cation-aromatic {pi}-interaction. Solvents that can coordinate to the cation turn off the cation-aromatic interaction, and consequently aggregation does not occur in zeolites that are impregnated with the above solvents. The solvent that exhibits a maximum in such an effect is water. MP2 calculations on cation-benzene dimer indicate that cation-{pi}-interaction results in stabilization of the {pi}-stacked benzene dimer. Results of MP2 calculations are consistent with the formation of ground-state {pi}-stacked aggregates of naphthalene molecules within Y zeolites.

  9. Kafirin adsorption on ion-exchange resins: isotherm and kinetic studies.

    Science.gov (United States)

    Kumar, Prashant; Lau, Pei Wen; Kale, Sandeep; Johnson, Stuart; Pareek, Vishnu; Utikar, Ranjeet; Lali, Arvind

    2014-08-22

    Kafirin is a natural, hydrophobic and celiac safe prolamin protein obtained from sorghum seeds. Today kafirin is found to be useful in designing delayed delivery systems and coatings of pharmaceuticals and nutraceuticals where its purity is important and this can be obtained by adsorptive chromatography. This study is the first scientific insight into the isotherm and kinetic studies of kafirin adsorption on anion- and cation-exchange resins for practical applications in preparative scale chromatography. Adsorption isotherms of kafirin were determined for five anion- and two cation-exchange resins in batch systems. Isotherm parameters such as maximum binding capacity and dissociation constant were determined from Langmuir isotherm, and adsorptive capacity and affinity constant from Freundlich isotherm. Langmuir isotherm was found to fit the adsorption equilibrium data well. Batch uptake kinetics for kafirin adsorption on these resins was also carried out and critical parameters including the diffusion coefficient, film mass transfer coefficient, and Biot number for film-pore diffusion model were calculated. Both the isotherm and the kinetic parameters were considered for selection of appropriate resin for kafirin purification. UNOsphere Q (78.26 mg/ml) and Toyopearl SP-650M (57.4 mg/ml) were found to offer better kafirin binding capacities and interaction strength with excellent uptake kinetics under moderate operating conditions. With these adsorbents, film diffusion resistance was found to be major governing factor for adsorption (Bi<10 and δ<1). Based on designer objective function, UNOsphere Q was found be best adsorbent for binding of kafirin. The data presented is valuable for designing large scale preparative adsorptive chromatographic kafirin purification systems.

  10. Catalysis using hydrous metal oxide ion exchanges

    Science.gov (United States)

    Dosch, Robert G.; Stephens, Howard P.; Stohl, Frances V.

    1985-01-01

    In a process which is catalyzed by a catalyst comprising an active metal on a carrier, said metal being active as a catalyst for the process, an improvement is provided wherein the catalyst is a hydrous, alkali metal or alkaline earth metal titanate, zirconate, niobate or tantalate wherein alkali or alkaline earth metal cations have been exchanged with a catalytically effective amount of cations of said metal.

  11. Catalysis using hydrous metal oxide ion exchangers

    Science.gov (United States)

    Dosch, R.G.; Stephens, H.P.; Stohl, F.V.

    1983-07-21

    In a process which is catalyzed by a catalyst comprising an active metal on a carrier, said metal being active as a catalyst for the process, an improvement is provided wherein the catalyst is a hydrous, alkali metal or alkaline earth metal titanate, zirconate, niobate or tantalate wherein alkali or alkaline earth metal cations have been exchanged with a catalytically effective amount of cations of said metal.

  12. [Antioxidant activity of cationic whey protein isolate].

    Science.gov (United States)

    titova, M E; Komolov, S A; Tikhomirova, N A

    2012-01-01

    The process of lipid peroxidation (LPO) in biological membranes of cells is carried out by free radical mechanism, a feature of which is the interaction of radicals with other molecules. In this work we investigated the antioxidant activity of cationic whey protein isolate, obtained by the cation-exchange chromatography on KM-cellulose from raw cow's milk, in vitro and in vivo. In biological liquids, which are milk, blood serum, fetal fluids, contains a complex of biologically active substances with a unique multifunctional properties, and which are carrying out a protective, antimicrobial, regenerating, antioxidant, immunomodulatory, regulatory and others functions. Contents of the isolate were determined electrophoretically and by its biological activity. Cationic whey protein isolate included lactoperoxidase, lactoferrin, pancreatic RNase, lysozyme and angeogenin. The given isolate significantly has an antioxidant effect in model experimental systems in vitro and therefore may be considered as a factor that can adjust the intensity of lipid oxidation. In model solutions products of lipid oxidation were obtained by oxidation of phosphatidylcholine by hydrogen peroxide in the presence of a source of iron. The composition of the reaction mixture: 0,4 mM H2O2; 50 mcM of hemin; 2 mg/ml L-alpha-phosphatidylcholine from soybean (Sigma, German). Lipid peroxidation products were formed during the incubation of the reaction mixture for two hours at 37 degrees C. In our studies rats in the adaptation period immediately after isolation from the nest obtained from food given orally native cationic whey protein isolate at the concentration three times higher than in fresh cow's milk. On the manifestation of the antioxidant activity of cationic whey protein isolate in vivo evidence decrease of lipid peroxidation products concentration in the blood of rats from the experimental group receipt whey protein isolate in dos 0,6 mg/g for more than 20% (pwhey protein isolate has an

  13. Synthesis and application of Polymer-encapsulated Zirconia-based cation exchange packing for SPE%聚合物/氧化锆基质阳离子交换固相萃取填料的研制及应用

    Institute of Scientific and Technical Information of China (English)

    江艳; 申书昌; 柳玉辉; 辛建娇

    2012-01-01

    In this paper, zirconia powder synthetized was treated by vinyl-silane coupling agent to get vinyl modified zirconia.The SPE packing of cross-linked polystyrene encapsulated zirconia-base was synthesized by styrene,divinylbenzene and vinyl-modified zirconia in radical polymerization. The polystyrene encapsulated zirconia-based was sulfonated by concentrated sulfuric acid and the cation exchange packing of for solid phase extraction was prepared.The composition and structure of the meterial were characterized by FT- IR, SEM and XRD.The reliability of detection method and adsorption properties of SPE columns were investigated by detecting the content of the sulfamerazine and sulfamethazine in the water on basis of SPE-HPLC, and the results were satisfied.%制备了ZrO2纳米粉体,并使用硅烷偶联剂处理得到乙烯基二氧化锆。通过自由基聚合,苯乙烯、二乙烯基苯与二氧化锆颗粒表面乙烯基反应,将交联聚苯乙烯包覆在锆胶表面上,再经硫酸磺化,制得聚合物/氧化锵阳离子交换同相萃取柱填料。采用Fr-IR和TEM手段表征了合成材料的组成与结构。通过固相萃取与高效液相色谱联用测定了水溶液中磺胺甲基嘧啶和磺胺二甲基嘧啶,考察了该固相萃取小柱的吸附性能及测试方法的可靠性,结果令人满意。

  14. Packed multi-channels for parallel chromatographic separations in microchips.

    Science.gov (United States)

    Nagy, Andrea; Gaspar, Attila

    2013-08-23

    Here we report on a simple method to fabricate microfluidic chip incorporating multi-channel systems packed by conventional chromatographic particles without the use of frits. The retaining effectivities of different bottlenecks created in the channels were studied. For the parallel multi-channel chromatographic separations several channel patterns were designed. The obtained multipackings were applied for parallel separations of dyes. The implementation of several chromatographic separation units in microscopic size makes possible faster and high throughput separations.

  15. PHOTOOXIDATION OF TOLUENE IN CATION-EXCHANGED ZEOLITES. (R825304)

    Science.gov (United States)

    The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

  16. Exploring Alkaline Stable Organic Cations for Polymer Hydroxide Exchange Membranes

    Science.gov (United States)

    2015-04-29

    was stirred at room temperature for 24 h. The solution was added dropwise to 40 mL ethyl ether to precipitate the product . The precipitate was...area of MTPP-(2,6-MeO); A3 is the peak area of ether hydrolysis products . ................................................. 163   Figure C.5...A2 is the peak area of BTPP-(2,6-MeO); A3 is the peak area of ether hydrolysis products . ................................................. 164

  17. Determination of solute descriptors by chromatographic methods

    Energy Technology Data Exchange (ETDEWEB)

    Poole, Colin F., E-mail: cfp@chem.wayne.edu [Department of Chemistry, Wayne State University, Detroit, MI 48202 (United States); Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K. [Department of Chemistry, Wayne State University, Detroit, MI 48202 (United States)

    2009-10-12

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  18. Chromatographic speciation of Cr(III)-species, inter-species equilibrium isotope fractionation and improved chemical purification strategies for high-precision isotope analysis

    DEFF Research Database (Denmark)

    Larsen, Kirsten Kolbjørn; Wielandt, Daniel Kim Peel; Schiller, Martin;

    2016-01-01

    Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of ...

  19. Synthetic cation-selective nanotube: Permeant cations chaperoned by anions

    Science.gov (United States)

    Hilder, Tamsyn A.; Gordon, Dan; Chung, Shin-Ho

    2011-01-01

    The ability to design ion-selective, synthetic nanotubes which mimic biological ion channels may have significant implications for the future treatment of bacteria, diseases, and as ultrasensitive biosensors. We present the design of a synthetic nanotube made from carbon atoms that selectively allows monovalent cations to move across and rejects all anions. The cation-selective nanotube mimics some of the salient properties of biological ion channels. Before practical nanodevices are successfully fabricated it is vital that proof-of-concept computational studies are performed. With this in mind we use molecular and stochastic dynamics simulations to characterize the dynamics of ion permeation across a single-walled (10, 10), 36 Å long, carbon nanotube terminated with carboxylic acid with an effective radius of 5.08 Å. Although cations encounter a high energy barrier of 7 kT, its height is drastically reduced by a chloride ion in the nanotube. The presence of a chloride ion near the pore entrance thus enables a cation to enter the pore and, once in the pore, it is chaperoned by the resident counterion across the narrow pore. The moment the chaperoned cation transits the pore, the counterion moves back to the entrance to ferry another ion. The synthetic nanotube has a high sodium conductance of 124 pS and shows linear current-voltage and current-concentration profiles. The cation-anion selectivity ratio ranges from 8 to 25, depending on the ionic concentrations in the reservoirs.

  20. Synthesis and SMM behaviour of trinuclear versus dinuclear 3d-5f uranyl(v)-cobalt(ii) cation-cation complexes.

    Science.gov (United States)

    Chatelain, Lucile; Tuna, Floriana; Pécaut, Jacques; Mazzanti, Marinella

    2017-01-17

    Trinuclear versus dinuclear heterodimetallic U(V)O2(+)Co(2+) complexes were selectively assembled via a cation-cation interaction by tuning the ligand. The trimeric complex 2, with a linear [Co-O[double bond, length as m-dash]U[double bond, length as m-dash]O-Co] core, exhibits magnetic exchange and slow relaxation with a reversal barrier of 30.5 ± 0.9 K providing the first example of a U-Co exchange-coupled SMM.

  1. Cation binding to 15-TBA quadruplex DNA is a multiple-pathway cation-dependent process.

    Science.gov (United States)

    Reshetnikov, Roman V; Sponer, Jiri; Rassokhina, Olga I; Kopylov, Alexei M; Tsvetkov, Philipp O; Makarov, Alexander A; Golovin, Andrey V

    2011-12-01

    A combination of explicit solvent molecular dynamics simulation (30 simulations reaching 4 µs in total), hybrid quantum mechanics/molecular mechanics approach and isothermal titration calorimetry was used to investigate the atomistic picture of ion binding to 15-mer thrombin-binding quadruplex DNA (G-DNA) aptamer. Binding of ions to G-DNA is complex multiple pathway process, which is strongly affected by the type of the cation. The individual ion-binding events are substantially modulated by the connecting loops of the aptamer, which play several roles. They stabilize the molecule during time periods when the bound ions are not present, they modulate the route of the ion into the stem and they also stabilize the internal ions by closing the gates through which the ions enter the quadruplex. Using our extensive simulations, we for the first time observed full spontaneous exchange of internal cation between quadruplex molecule and bulk solvent at atomistic resolution. The simulation suggests that expulsion of the internally bound ion is correlated with initial binding of the incoming ion. The incoming ion then readily replaces the bound ion while minimizing any destabilization of the solute molecule during the exchange.

  2. Mapping the chromatographic behavior of a cell proteome utilizing orthogonal routines: the influence of feedstock pH

    Directory of Open Access Journals (Sweden)

    Rosa Cabrera

    2008-08-01

    Full Text Available Surface charge, molecular weight, and folding state are known to influence protein chromatographic behavior onto ion-exchangers. Experimentally, information related to such factors can be gathered via two-dimensional electrophoretic (2-DE methods. The separation behavior depicted by the insect cultured-cells proteome, which is an important host for recombinant protein production, was explored in this study. Experimental evidence showed a correlation between apparent isoelectric point distributions and the mobile phase conductivity. It was observed that the information contained in the isoelectric point (pI value(s obtained with a 2-DE routine showed a good correlation with the IEX chromatographic behavior, for a number of commercial adsorbents. This correlation was observed irrespective of the pH of the feedstock within the range 6 to 8. An initial prediction of protein ion-exchange chromatographic behavior could be possible utilizing an experimental approach based on the mentioned orthogonal methods. This technique is providing information that more closely resembles the separation behaviour observed with a complex biotechnological feedstock.Keywords: Insect cells, proteome, chromatography, ion-exchange, bioprocessingReceived: 3 August 2008 / Received in revised form: 15 August 2008, Accepted: 19 August 2008, Published online: 20 August 2008

  3. 萃取色谱法分离实际样品及伴生元素中的铂(Ⅳ)元素%Extraction chromatographic separation of platinum(Ⅳ) from real samples and associated elements

    Institute of Scientific and Technical Information of China (English)

    KOKATE Sudarshan Jagdish; KUCHEKAR Shashikant Raghunath

    2009-01-01

    The extraction behavior of platinum(Ⅳ) was studied with N-n-octylaniline as a function of different parameters,such as pH,concentrations of weak acids,mineral acids,reagents and elution time. A selective method was developed for the extraction chromatographic studies of platinum(Ⅳ) and its separation from several metal ions with N-n-octylaniline (liquid anion exchanger) as a stationary phase on silica gel. The quantitative extraction of platinum(Ⅳ) was observed with 0.067 mol/L N-n-octylaniline and 0.015 mol/L ascorbic acid at pH 1.0. Metal ion was stripped from the column with water and determined spectrophotometrically with stannous chloride method. The proposed method is free from the interference of a large number of cations and anions. Platinum(Ⅳ) was separated from pharmaceutical preparations,alloys and synthetic mixtures. Mutual separation scheme was developed for platinum(Ⅳ),palladium(Ⅱ) and gold(Ⅲ). The log-log plot of N-n-octylaniline concentration versus the distribution ratio indicates that the probable extracted species is [RR~′NH~+_2 ] · Pt(C_6H_7O_6)~-_3.

  4. Water quality monitoring of Jialing-River in Chongqing using advanced ion chromatographic system

    Institute of Scientific and Technical Information of China (English)

    Kazuhiko TANAKA; Chao-Hong SHI; Nobukazu NAKAGOSHI

    2012-01-01

    The water quality monitoring operation to evaluate the water quality of polluted river is an extremely important task for the river-watershed management/control based on the environmental policy.In this study,the novel,simple and convenient water quality monitoring of Jialing-River in Chongqing,China was carried out using an advanced ion chromatography (IC) consisting of ion-exclusion/cation-exchange chromatography (IEC/CEC) with conductivity detection for determining simultaneously the common anions such as SO42 -,Cl -,and NO3- and the cations such as Na+,NH4+,K+,Mg2+,and Ca2+,the ion-exclusion chromatography (IEC) with visible detection for determining simultaneously the nutrient components such as phosphate and silicate ions,and the IEC with the enhanced conductivity detection using a post column of K+ -form cation-exchange resin for determining HCO3- -alkalinity as an inorganic-carbon source for biomass synthesis in biological reaction process under the aerobic conditions.According to the ionic balance theory between the total equivalent con-centrations of anions and cations,the water quality evaluation of the Jialing-River waters taking at different sampling sites in Chongqing metropolitan area was carried out using the advanced IC system.As a result,the effectiveness of this novel water quality monitoring methodology using the IC system was demonstrated on the several practical applications to a typical biological sewage treatment plant on Jialing-River of Chongqing.

  5. Tailoring orthogonal proteomic routines to understand protein separation during ion exchange chromatography.

    Science.gov (United States)

    Cabrera, Rosa; Zhelyazkova, Petya; Galvis, Leonardo; Fernandez-Lahore, Marcelo

    2008-07-01

    Surface charge, molecular weight, and folding state are known to influence protein chromatographic behaviour onto ion exchangers. Experimentally, information related to such factors can be gathered via 2-DE methods. The application of 2-D PAGE under denaturing/reducing conditions was already shown to reveal separation trends within a large protein population from cell extracts. However, ion-exchange chromatography normally runs under native conditions. A tailored protocol consisting in a first separation based on IEF on Immobiline strips under native conditions followed by a second dimension SDS-PAGE run was adopted. The chromatographic versus electrophoretic separation behaviours of two model proteins, thaumatin (TAU) and BSA, were compared to better understand which proteomic routine would be better suited to anticipate IEX chromatographic separations. It was observed that the information contained in the pI value obtained with the adapted 2-DE protocol showed better correlation with the IEX chromatographic behaviour. On the other hand, chromatographic separations performed in the presence of urea as a denaturant have demonstrated the potential influence of hydrodynamic radius/conformation on protein separation. Moreover, the information provided by such 2-D system correlated well with the chromatographic behaviour of an additional set of pure proteins. An initial prediction of protein ion-exchange chromatographic behaviour could be possible utilizing an experimental approach based on 2-DE running under milder chemical conditions. This technique provides information that more closely resembles the separation behaviour observed with a complex biotechnological feedstock.

  6. Asymmetric cation-binding catalysis

    DEFF Research Database (Denmark)

    Oliveira, Maria Teresa; Lee, Jiwoong

    2017-01-01

    and KCN, are selectively bound to the catalyst, providing exceptionally high enantioselectivities for kinetic resolutions, elimination reactions (fluoride base), and Strecker synthesis (cyanide nucleophile). Asymmetric cation-binding catalysis was recently expanded to silicon-based reagents, enabling...... solvents, thus increasing their applicability in synthesis. The expansion of this concept to chiral polyethers led to the emergence of asymmetric cation-binding catalysis, where chiral counter anions are generated from metal salts, particularly using BINOL-based polyethers. Alkali metal salts, namely KF...

  7. Model-based high-throughput design of ion exchange protein chromatography.

    Science.gov (United States)

    Khalaf, Rushd; Heymann, Julia; LeSaout, Xavier; Monard, Florence; Costioli, Matteo; Morbidelli, Massimo

    2016-08-12

    This work describes the development of a model-based high-throughput design (MHD) tool for the operating space determination of a chromatographic cation-exchange protein purification process. Based on a previously developed thermodynamic mechanistic model, the MHD tool generates a large amount of system knowledge and thereby permits minimizing the required experimental workload. In particular, each new experiment is designed to generate information needed to help refine and improve the model. Unnecessary experiments that do not increase system knowledge are avoided. Instead of aspiring to a perfectly parameterized model, the goal of this design tool is to use early model parameter estimates to find interesting experimental spaces, and to refine the model parameter estimates with each new experiment until a satisfactory set of process parameters is found. The MHD tool is split into four sections: (1) prediction, high throughput experimentation using experiments in (2) diluted conditions and (3) robotic automated liquid handling workstations (robotic workstation), and (4) operating space determination and validation. (1) Protein and resin information, in conjunction with the thermodynamic model, is used to predict protein resin capacity. (2) The predicted model parameters are refined based on gradient experiments in diluted conditions. (3) Experiments on the robotic workstation are used to further refine the model parameters. (4) The refined model is used to determine operating parameter space that allows for satisfactory purification of the protein of interest on the HPLC scale. Each section of the MHD tool is used to define the adequate experimental procedures for the next section, thus avoiding any unnecessary experimental work. We used the MHD tool to design a polishing step for two proteins, a monoclonal antibody and a fusion protein, on two chromatographic resins, in order to demonstrate it has the ability to strongly accelerate the early phases of process

  8. Probabilistic peak detection for first-order chromatographic data

    NARCIS (Netherlands)

    Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

    2014-01-01

    We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by suc

  9. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-03

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDTOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet.

  10. Headspace chromatographic determination of water pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Otson, R.; Williams, D.T.

    1982-05-01

    A readily constructed, automated purging assembly, on-column trapping, and simultaneous use of flame ionization and electrolytic conductivity detectors were applied to develop a dynamic headspace gas chromatographic technique which was evaluated for the determination of 42 organic polluants in water. Detection limits of <1 ..mu..g/L and linear plots of peak area against concentration in the range 0.25-16 ..mu..g/L were obtained for 32 compounds. At aqueous concentrations of 4 and 16 ..mu..g/L, peak area precision of <10% relative standard deviation (RSD) for triplicate sample analysis and purging efficiencies of >75% were generally obtained. Storage of aqueous composite standard solutions at 4 and 16 ..mu..g/L for 6 weeks at 4/sup 0/C did not usually affect analytical results by more than +/- 15%.

  11. Functional Polymers for Chromatographic Enantiomer Separation

    Institute of Scientific and Technical Information of China (English)

    S. Allenmark; L. Thunberg

    2005-01-01

    @@ 1Introduction Today, methods to obtain pure enantiomers of organic compounds are of extreme importance, not the least due to the demands imposed on the pharmaceutical industry. Separation of the two enantiomers in a racemate is necessary in order to study possible differences in biological activity. Consequently, research on methods for direct chromatographic resolution by means of columns containing a chiral stationary phase (CSP) has been intense during the last decades and a wide variety of CSPs,many of which commercially available,exist today.Polymeric CSPs have been made from naturally occurring polymers (cellulose, amylose) via suitable derivatization, as well as either by polymerization of chiral monomers or via asymmetric catalysis to yield linear, isotactic polymers of a predominantly single-handed helicity. An excellent review of the field[1], with special emphasis on preparative applications, was published in 1994.

  12. Liquid chromatographic determination of furazolidone in shrimp.

    Science.gov (United States)

    Stehly, G R; Plakas, S M; el Said, K R

    1994-01-01

    A liquid chromatographic (LC) method was developed for the quantitation of furazolidone residues in shrimp muscle. The shrimp homogenate (1.0 g) is extracted with acetonitrile, and the extract is taken to dryness. The residue is dissolved in acetonitrile, and the solution is passed through alumina and C18 cleanup columns. The eluate is taken to dryness and reconstituted in a suitable solvent for reversed-phase (C18) LC with UV detection at 365 nm. Recoveries of furazolidone from shrimp homogenates spiked from 5 to 80 ng/g ranged from 74.3 to 79.7%, and relative standard deviations (RSDs) were 5.0-8.9%. RSDs for incurred furazolidone quantitated at 5.9 and 9.2 ng/g were 6.6 and 7.6%, respectively.

  13. A new chromatographic-method for fast separation of active proteins

    Institute of Scientific and Technical Information of China (English)

    KE CongYu; GENG XinDu

    2008-01-01

    A new method with only a single chromatographic column to accomplish the separation of intact pro-tein molecules by the combination of ion exchange chromatography and hydrophobic interaction chromatography is firstly presented. By selecting twice a suitable stationary phase, mobile phase, buffer exchange condition, and sample injection, some proteins usually required to separate with two-dimensional chromatography can now be accomplished only using the single column in one hour. In addition, the separated proteins can maintain their original three- or four-dimensional molecular structure. It would be expected that this method can also provide a new thought for sample pre-frac-tionation in proteomic investigation, especially, for the limitation of sample source.

  14. Investigations into the chromatographic optimization of combined gas chromatographic/FTIR/MS

    Science.gov (United States)

    Wulff, Ditmar

    1989-12-01

    Even with the explosive growth and acceptance of GC/MS it has some analytical limitations. Several of these deficiencies can be overcome with information provided by GC/FTIR. Combining a GC/MS and a GC/FTIR into one system provides economies of sample, time, space, and money as well as a higher confidence qualitative result. The later results from the ability of the mass spectro -meter to give molecular fragment information with strength in homolog identification while the infrared spectrometer gives class specific-functional group and geometrical isomer data. Several configurations of the combined light pipe GC/FTIR/MS are evaluated looking toward ease of use, information content, and data evaluation. The combined system's sensitivity, chromatographic integrity, and gas chromatographic column choices and their operational parameters are discussed. The series arrangement with the GC column effluent passing through the FTIR light pipe and then serially to the MS is compared to the post column split of the column effluent to the FTIR and MS as well as to the configuration using two GC columns. Operational recommendations are given to maximize chromatographic resolution, detector sensitivity, and sample throughput. Examples are shown illustrating the combined systems operation. All parameters discussed apply to work done on the HP 5890A GC, the HP5965A IRD, and the HP 5970B MSD.

  15. 阳离子交换树脂催化制备纳米纤维素晶体的谱学性能与流变行为%Spectrum and Rheological Properties of Nanocellulose Crystal Prepared with Cation Exchange Resin

    Institute of Scientific and Technical Information of China (English)

    唐丽荣; 黄彪; 戴达松; 欧文; 李涛; 周东东; 陈学榕

    2011-01-01

    采用强酸型阳离子交换树脂在超声波辅助作用下制备了纳米纤维素晶体(NCC).采用场发射环境扫描电子显微镜(ESEM-FEG)、场发射透射电子显微镜(HR-TEM)、X射线粉末衍射仪(XRD)、傅利叶红外光谱仪(FT-IR)和转子式流变仪对所制备NCC的形貌、谱学和流变学行为进行了研究.结果表明,所制备NCC为近球形,颗粒尺寸约为25nm~50nm,样品属于纤维素Ⅰ型,结晶度为84.26%,晶粒平均由6个晶胞组成.由FT-IR分析可知,NCC仍具有纤维素的基本化学结构.NCC胶体为剪切变稀的假塑性流体,随着温度的升高,其黏度逐渐减小,并最终趋于平缓,结果表明NCC胶体具有较好的稳定性.%Nanocellulose crystal (NCC) was prepared by ultrasonic-assisted hydrolysis with strong acidic cation exchange resin. The size and morphology, crystal structure, spectrum properties and rheological behavior of nanocellulose crystal were investigated by field emission gun environment scanning electron microscopes (ESEM-FEG), field emission transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Fourier transform infrared spectrometry(FT-IR) and rotor rheometer. The results indicate that the nanocellulose crystal is spherical and the size is about 25 nm~50 nm. The samples have the crystalline cellulose I structure, the crystallinity is 84.26% , and the grain is composed of 6 unit crystal cell. Moreover, the results of FT-IR show that NCC still has the basic chemical structure of cellulose. NCC is the shear thinned pseudoplastic fluid. Futhermore, as the temperature increases, its viscosity decreases, and gradually tends to flat, the results indicate that the samples enjoy nice stability.

  16. Preparação e propriedades de zeólitas faujasita contendo cátions amônio Preparation and properties of faujasite zeolites containing ammonium cations

    Directory of Open Access Journals (Sweden)

    Karina Arruda Almeida

    2010-01-01

    Full Text Available Sodium faujasite zeolites with Si/Al ratio of 1.4 and 2.5 were exchanged with methylammonium cations. The influence of framework aluminum and ion exchange degree in their basic properties were evaluated. These properties were assessed in the Knoevenagel catalytic condensation. The sodium ion exchange was restricted to the supercavity and the exchange degree depended on the cation volume and on the Si/Al ratio. The higher catalytic activity is achieved for the zeolite with the lower Si/Al ratio exchanged with the monomethylammonium cation. The best performance of this catalyst is attributed to the higher basicity in combination with elevated micropore volume.

  17. A chromatographic estimate of the degree of heterogeneity of RPLC packing materials. 1. Non-endcapped polymeric C30-bonded stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Gritti, Fabrice [University of Tennessee, Knoxville (UTK); Guiochon, Georges A [ORNL

    2006-01-01

    A new chromatographic method estimating the degree of heterogeneity of RPLC packing materials is based on the results of systematic measurements of the adsorption data in a wide concentration range for selected probe compounds. These data are acquired by frontal analysis (FA), modeled, and used for the calculation of the adsorption energy distribution (AED). Four compounds were used, two neutral compounds of different molecular sizes (caffeine and phenol) and two ionizable compounds of opposite charges, 2-naphthalene sulfonate, an anion, and propranololium, a cation. This work was done on a C{sub 30}-bonded silica stationary phase (Prontosil-C{sub 30}), using the same aqueous mobile phase (30% methanol, v/v) for all compounds, except that sodium chloride (25 mM) was added to elute the ionizable compounds. All four adsorption isotherms have Langmuirian behavior. The AEDs are tri-modal for phenol, quadri-modal for caffeine. The total saturation capacity of the stationary phase is four-fold lower for caffeine than for phenol, due in part to its larger molecular size. The equilibrium constants on the low-energy sites of types 1 and 2 are eight-fold larger. These two types of sites characterize the heterogeneity of the bonded layer itself. The density of the high-energy sites of types 3 and 4 is higher for caffeine, suggesting that caffeine molecules can be accommodated in some hydrophobic cages into which smaller molecules like phenol cannot. These high-energy types of sites characterize the heterogeneity of the whole stationary phase (silica support included). The ionizable compounds have larger molecules than the neutral ones and, accordingly, a lower relative density of sites of type 2 to sites of type 1. A tri-modal and a quadri-modal energy distributions were observed for the 2-naphthalene sulfonate anion and the propranololium cation, respectively. The fourth types of sites measured and its unusually high equilibrium constant are most probably due to ion-exchange

  18. Mixed-bed ion exchange chromatography employing a salt-free pH gradient for improved sensitivity and compatibility in MudPIT.

    Science.gov (United States)

    Mommen, Geert P M; Meiring, Hugo D; Heck, Albert J R; de Jong, Ad P J M

    2013-07-16

    In proteomics, comprehensive analysis of peptides mixtures necessitates multiple dimensions of separation prior to mass spectrometry analysis to reduce sample complexity and increase the dynamic range of analysis. The main goal of this work was to improve the performance of (online) multidimensional protein identification technology (MudPIT) in terms of sensitivity, compatibility and recovery. The method employs weak anion and strong cation mixed-bed ion exchange chromatography (ACE) in the first separation dimension and reversed phase chromatography (RP) in the second separation dimension (Motoyama et.al. Anal. Chem 2007, 79, 3623-34.). We demonstrated that the chromatographic behavior of peptides in ACE chromatography depends on both the WAX/SCX mixing ratio as the ionic strength of the mobile phase system. This property allowed us to replace the conventional salt gradient by a (discontinuous) salt-free, pH gradient. First dimensional separation of peptides was accomplished with mixtures of aqueous formic acid and dimethylsulfoxide with increasing concentrations. The overall performance of this mobile phase system was found comparable to ammonium acetate buffers in application to ACE chromatography, but clearly outperformed strong cation exchange for use in first dimensional peptide separation. The dramatically improved compatibility between (salt-free) ion exchange chromatography and reversed phase chromatography-mass spectrometry allowed us to downscale the dimensions of the RP analytical column down to 25 μm i.d. for an additional 2- to 3-fold improvement in performance compared to current technology. The achieved levels of sensitivity, orthogonality, and compatibility demonstrates the potential of salt-free ACE MudPIT for the ultrasensitive, multidimensional analysis of very modest amounts of sample material.

  19. THERMODYNAMICS OF ION-EXCHANGED NATURAL CLINOPTILOLITE

    Science.gov (United States)

    Natural clinoptilolite from Castle Creek, Idaho, and its cation-exchanged variants (Na-Cpt, NaK-Cpt, K-Cpt, and Ca-Cpt) were studied by high-temperature calorimetry. The hydration enthalpy for all clinoptilolites is about -30 kJ/mol H2O (liquid water reference state) at 25 C. T...

  20. A novel silica based click lysine anion exchanger for ion exchange chromatography.

    Science.gov (United States)

    Guo, Hongyue; Chu, Changhu; Li, Yan; Yang, Bingcheng; Liang, Xinmiao

    2011-12-21

    Ion chromatography (IC) is one of the most powerful analysis technologies for the determination of charged compounds. A novel click lysine stationary phase was prepared via Cu(I) catalyzed alkyne-azide 1,3-dipolar cycloaddition (CuAAC) and applied to the analysis of inorganic ions. The chromatographic evaluation demonstrated good performance (e.g. the plate number of thiocyanate is ∼50,000 plates m(-1)) and effective separation ability for the common inorganic anions with aqueous Na(2)SO(4) eluent. The separation mechanism was observed to be mainly dominated by ion exchange interaction. The retention of these analytes is highly dependent on the pH value of eluent. Compared with the lysine stationary phase prepared via the conventional manner, the click lysine exchanger demonstrated shorter retention time and better ion separation characteristics under the same chromatographic conditions, which is a great advantage for rapid separation and analysis of inorganic ions.

  1. Chromatographic analysis of olopatadine in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Maksić, Jelena; Jovanović, Marko; Rakić, Tijana; Popović, Igor; Ivanović, Darko; Jančić-Stojanović, Biljana

    2015-01-01

    In this paper, chromatographic analysis of active substance olopatadine hydrochloride, which is used in eye drops as antihistaminic agent, and its impurity E isomer by hydrophilic interaction liquid chromatography (HILIC) and application of design of experiments (DoE) methodology are presented. In addition, benzalkonium chloride is very often used as a preservative in eye drops. Therefore, the evaluation of its chromatographic behavior in HILIC was carried out as well. In order to estimate chromatographic behavior and set optimal chromatographic conditions, DoE methodology was applied. After the selection of important chromatographic factors, Box-Behnken design was utilized, and on the basis of the obtained models factor effects were examined. Then, multi-objective robust optimization is performed aiming to obtain chromatographic conditions that comply with several quality criteria simultaneously: adequate and robust separation of critical peak pair and maximum retention of the first eluting peak. The optimal conditions are identified by using grid point search methodology. The experimental verification confirmed the adequacy of the defined optimal conditions. Finally, under optimal chromatographic conditions, the method was validated and applicability of the proposed method was confirmed.

  2. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  3. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Ying Liu

    2004-12-19

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  4. Ion-exchange vs reversed-phase chromatography for separation and determination of basic psychotropic drugs.

    Science.gov (United States)

    Petruczynik, Anna; Wróblewski, Karol; Deja, Michał; Waksmundzka-Hajnos, Monika

    2015-11-01

    Ion exchange chromatography, an alternative to reversed-phase (RP) chromatography, is described in this paper. We aimed to obtain optimal conditions for the separation of basic drugs because silica-based RP stationary phases show silanol effect and make the analysis of basic analytes hardly possible. The retention, separation selectivity, symmetry of peaks and system efficiency were examined in different eluent systems containing different types of buffers at acidic pH and with the addition of organic modifiers: methanol and acetonitrile. The obtained results reveal a large influence of the salt cation used for buffer preparation and the type of organic modifier on the retention behavior of the analytes. These results were also compared with those obtained on an XBridge C18 column. The obtained results demonstrated that SCX stationary phases can be successfully used as alternatives to C18 stationary phases in the separation of basic compounds. The most selective and efficient chromatographic systems were applied for the quantification of some psychotropic drugs in fortified human serum samples.

  5. Natural zeolite reactivity towards ozone: the role of compensating cations.

    Science.gov (United States)

    Valdés, Héctor; Alejandro, Serguei; Zaror, Claudio A

    2012-08-15

    Among indoor pollutants, ozone is recognised to pose a threat to human health. Recently, low cost natural zeolites have been applied as alternative materials for ozone abatement. In this work, the effect of compensating cation content of natural zeolite on ozone removal is studied. A Chilean natural zeolite is used here as starting material. The amount of compensating cations in the zeolite framework was modified by ion exchange using an ammonium sulphate solution (0.1 mol L(-1)). Characterisation of natural and modified zeolites were performed by X-ray powder diffraction (XRD), nitrogen adsorption at 77K, elemental analysis, X-ray fluorescence (XRF), thermogravimetric analysis coupled with mass spectroscopy (TGA-MS), and temperature-programmed desorption of ammonia (NH(3)-TPD). Ozone adsorption and/or decomposition on natural and modified zeolites were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Results show that the zeolite compensating cation content affects ozone interaction with zeolite active sites. Ammonium ion-exchange treatments followed by thermal out-gassing at 823 K, reduces ozone diffusion resistance inside the zeolite framework, increasing ozone abatement on zeolite surface active sites. Weak and strong Lewis acid sites of zeolite surface are identified here as the main active sites responsible of ozone removal.

  6. Probing optical band gaps at nanoscale from tetrahedral cation vacancy defects and variation of cation ordering in NiCo2O4 epitaxial thin films

    Science.gov (United States)

    Dileep, K.; Loukya, B.; Silwal, P.; Gupta, A.; Datta, R.

    2014-10-01

    High resolution electron energy loss spectroscopy (HREELS) is utilized to probe the optical band gaps at the nanoscale in epitaxial NiCo2O4 (NCO) thin films with different structural order (cation/charge). The structure of NCO deviates from the ideal inverse spinel (non-magnetic and insulating) for films grown at higher temperatures (>500 °C) towards a mixed cation structure (magnetic with metallic conductivity) at lower deposition temperatures (<450 °C). This significantly modifies the electronic structure as well as the nature of the band gap of the material. Nanoscale regions with unoccupied tetrahedral A site cations are additionally observed in all the samples and direct measurement from such areas reveals considerably lower band gap values as compared to the ideal inverse spinel and mixed cation configurations. Experimental values of band gaps have been found to be in good agreement with the theoretical mBJLDA exchange potential based calculated band gaps for various cation ordering and consideration of A site cation vacancy defects. The origin of rich variation in cation ordering observed in this system is discussed.

  7. Chromatographic Separation of Vitamin E Enantiomers

    Directory of Open Access Journals (Sweden)

    Ju-Yen Fu

    2017-02-01

    Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  8. Cationic Organic/Inorganic Hybrids and Their Swelling Properties

    Institute of Scientific and Technical Information of China (English)

    E. S. Dragan; L. Ghimici; M. Cazacu

    2005-01-01

    @@ 1Introduction Specific properties of poly(dimethylsiloxanes), such as low glass transition temperature, low surface energy, good insulating properties, biological and chemical inertness, high diffusion coefficient of gases, make them very attractive for practical applications in the daily life. However, there is a great interest last time in the preparation of ionic organic/inorganic materials with new properties for new applications. Quaternary ammonium salt(QAS) groups included in siloxane copolymers could induce new interesting properties such as:permanent fungicidal and bactericidal properties, which make them very attractive as materials for sanitary applications, improved selectivity coefficients of the gas-separation membranes, ion-exchange properties and so forth. So far, QAS groups have been located in the side chain[1,2]. Our interest was focused on the preparation of some novel cationic polysiloxane copolymers containing QAS groups of both integral type and pendent type[3,4]. Our objectives for the present study concern the synthesis of some cationic organic/siloxane hybrid materials with swelling properties controlled by both the nature of cationic organic component and the ratio between the organic and inorganic counterparts. Such cationic hybrid materials could be of interest for the preparation of new stimuli-responsive hydrogels[5,6].

  9. Electrically switched ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Lilga, M.A. [Pacific Northwest National Lab., Richland, WA (United States); Schwartz, D.T.; Genders, D.

    1997-10-01

    A variety of waste types containing radioactive {sup 137}Cs are found throughout the DOE complex. These waste types include water in reactor cooling basins, radioactive high-level waste (HLW) in underground storage tanks, and groundwater. Safety and regulatory requirements and economics require the removal of radiocesium before these wastes can be permanently disposed of. Electrically Switched Ion Exchange (ESIX) is an approach for radioactive cesium separation that combines IX and electrochemistry to provide a selective, reversible, and economic separation method that also produces little or no secondary waste. In the ESIX process, an electroactive IX film is deposited electrochemically onto a high-surface area electrode, and ion uptake and elution are controlled directly by modulating the potential of the film. For cesium, the electroactive films under investigation are ferrocyanides, which are well known to have high selectivities for cesium in concentrated sodium solutions. When a cathode potential is applied to the film, Fe{sup +3} is reduced to the Fe{sup +2} state, and a cation must be intercalated into the film to maintain charge neutrality (i.e., Cs{sup +} is loaded). Conversely, if an anodic potential is applied, a cation must be released from the film (i.e., Cs{sup +} is unloaded). Therefore, to load the film with cesium, the film is simply reduced; to unload cesium, the film is oxidized.

  10. Chemical Surface, Thermal and Electrical Characterization of Nafion Membranes Doped with IL-Cations

    Directory of Open Access Journals (Sweden)

    María del Valle Martínez de Yuso

    2014-04-01

    Full Text Available Surface and bulk changes in a Nafion membrane as a result of IL-cation doping (1-butyl-3-methylimidazolium tetrafluoroborate or BMIM+BF4 and phenyltrimethylammonium chloride or TMPA+Cl− were studied by X-ray photoelectron spectroscopy (XPS, contact angle, differential scanning calorimetry (DSC and impedance spectroscopy (IS measurements performed with dry samples after 24 h in contact with the IL-cations BMIM+ and TMPA+. IL-cations were selected due to their similar molecular weight and molar volume but different shape, which could facilitate/obstruct the cation incorporation in the Nafion membrane structure by proton/cation exchange mechanism. The surface coverage of the Nafion membrane by the IL-cations was confirmed by XPS analysis and contact angle, while the results obtained by the other two techniques (DSC and IS seem to indicate differences in thermal and electrical behaviour depending on the doping-cation, being less resistive the Nafion/BMIM+ membrane. For that reason, determination of the ion transport number was obtained for this membrane by measuring the membrane or concentration potential with the samples in contact with HCl solutions at different concentrations. The comparison of these results with those obtained for the original Nafion membrane provides information on the effect of IL-cation BMIM+ on the transport of H+ across wet Nafion/BMIM+ doped membranes.

  11. Research progress in cation-π interactions

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Cation-π interaction is a potent intermolecular interaction between a cation and an aromatic system,which has been viewed as a new kind of binding force,as being compared with the classical interactions(e.g. hydrogen bonding,electrostatic and hydrophobic interactions). Cation-π interactions have been observed in a wide range of biological contexts. In this paper,we present an overview of the typical cation-π interactions in biological systems,the experimental and theoretical investigations on cation-π interactions,as well as the research results on cation-π interactions in our group.

  12. Research progress in cation-π interactions

    Institute of Scientific and Technical Information of China (English)

    CHENG JiaGao; LUO XiaoMin; YAN XiuHua; LI Zhong; TANG Yun; JIANG HuaLiang; ZHU WeiLiang

    2008-01-01

    Cation-π interaction is a potent intermolecular interaction between a cation and an aromatic system, which has been viewed as a new kind of binding force, as being compared with the classical interac-tions (e.g. hydrogen bonding, electrostatic and hydrophobic interactions). Cation-π interactions have been observed in a wide range of biological contexts. In this paper, we present an overview of the typi-cal cation-π interactions in biological systems, the experimental and theoretical investigations on cation-π interactions, as well as the research results on cation-π interactions in our group.

  13. Lack of association between a cationic protein and a cationic fluorosurfactant.

    Science.gov (United States)

    Macakova, Lubica; Nordstierna, Lars; Karlsson, Göran; Blomberg, Eva; Furó, István

    2007-01-16

    Surface tension, 19F and 1H NMR spectroscopy, and cryotransmission electron microscopy are used to characterize the state of association in aqueous solutions of a fluorosurfactant CF3(CF2)nSO2NH(CH2)3-4N(CH3)3+ I- (n = 8, 6) with and without lysozyme added. In the absence of lysozyme, we find monomers, small aggregates, and large vesicles to coexist, with the individual fluorosurfactant molecules exchanging slowly (>1 ms) among those states. When both lysozyme and fluorosurfactant are present in the solution, they have no measurable influence on the physical state of the other. In contrast, a hydrogenated cationic surfactant with the same headgroup, hexadecyltrimethylammonium bromide, is shown to associate to lysozyme.

  14. Heat exchanger

    Energy Technology Data Exchange (ETDEWEB)

    Craig, L.B.; Farma, A.J.

    1987-01-06

    This invention concerns a heat exchanger as used in a space heater, of the type in which hot exhaust gases transfer heat to water or the like flowing through a helical heat exchange coil. A significant improvement to the efficiency of the heat exchange occurring between the air and water is achieved by using a conduit for the water having external helical fluting such that the hot gases circulate along two paths, rather than only one. A preferred embodiment of such a heat exchanger includes a porous combustion element for producing radiant heat from a combustible gas, surrounded by a helical coil for effectively transferring the heat in the exhaust gas, flowing radially from the combustion element, to the water flowing through the coil. 4 figs.

  15. Gas chromatographic separation of hydrogen isotopes using metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Aldridge, F.T.

    1984-05-09

    A study was made of the properties of metal hydrides which may be suitable for use in chromatographic separation of hydrogen isotopes. Sixty-five alloys were measured, with the best having a hydrogen-deuterium separation factor of 1.35 at 60/sup 0/C. Chromatographic columns using these alloys produced deuterium enrichments of up to 3.6 in a single pass, using natural abundance hydrogen as starting material. 25 references, 16 figures, 4 tables.

  16. Gas-chromatographic determination of aluminum in catalytic systems

    Energy Technology Data Exchange (ETDEWEB)

    Astapova, T.I.; Kutepova, A.I.; Frolova, O.D.

    1987-11-10

    The authors studied conditions for the chromatographic determination of aluminum in the form of a complex with pentane-2,4-dione in pilot plant-produced samples of GIAP-16, GIAP-16-2, SPM catalysts, talums and kaolins, aluminum oxides, and hydroxides. The influence of Zn, Mg, Ca, Na, Ni, Ti, and Mn on the extraction and the chromatographic determination of aluminum was studied.

  17. Quantifying process tradeoffs in the operation of chromatographic sequences.

    Science.gov (United States)

    Ngiam, Sheau-Huey; Bracewell, Daniel G; Zhou, Yuhong; Titchener-Hooker, Nigel J

    2003-01-01

    A method for the rapid representation of key process tradeoffs that need to be made during the analysis of chromatographic sequences has been proposed. It involves the construction of fractionation and maximum purification factor versus yield diagrams, which can be completed easily on the basis of chromatographic data. The output of the framework developed reflects the degree of tradeoff between levels of yield and purity and provides a fast and precise prediction of the sample fraction collection strategy needed to meet a desired process specification. The usefulness of this approach for the purposes of product purification and contaminant removal in a single chromatographic step has been successfully demonstrated in an earlier paper and it is now extended by application to a chromatographic sequence: the separation of a hypothetical three-component protein system by hydrophobic interaction chromatography (HIC) followed by size exclusion chromatography (SEC). The HIC operation has a strong impact upon the subsequent SEC step. The studies show how the analysis of performance in such a chromatographic sequence can be carried out easily and in a straightforward fashion using the fractionation diagram approach. The methodology proposed serves as a useful tool for identifying the process tradeoffs that must be made during operation of a sequence of chromatographic steps and indicates the impact on further processing of the cut-point decisions that are made.

  18. 弱阳离子交换纳米磁珠介导的帕金森病血清蛋白质组学的初步研究%Proteomic study for serum biomarkers in Parkinson's disease using weak cation exchange magnetic beads and MALDI-TOF-MS

    Institute of Scientific and Technical Information of China (English)

    王坚; 李尧华; 郑晓立; 张燕莉; 李昕; 于顺; 何欣; 陈彪

    2009-01-01

    Objective To screen for the potential protein biomarkers in serum for the diagnosis of idiopathic Parkinson's disease (PD) using proteomic fingerprint technology. Methods Proteomic fingerprint technology combining weak cation exchange (WCX) magnetic beads with MALDI-TOF-MS was used to identify and compare the serum proteins from 61 patients with idiopathic PD, 29 patients with other neurodegenerative diseases (OND) and 30 healthy blood donors. Model of biomarkers and proteomics patterns associated with PD was analyzed by Biomarker Patterns Software. The model also was validated by 40 newly recruited PD cases. Results A total of 17 discriminating M/Z peaks which were related to PD were identified ( nonparametric test, Z:-4.039--2.633, P<0.01 ). Five biomarkers with M/Z of 6121, 5234, 2961,4309 and 8170 respectively generated an excellent model of distinguishing between PD and healthy groups. The sensitivity was 98.4% and the specificity was 83.1%. Blind testing in 40 newly recruited cases demonstrated a sensitivity of 85.0% (17 of 20 PD) and a specificity of 70. 0% (14 of 20 controls). Conclusions Combination of WCX magnetic beads with MALDI-TOF-MS is a useful method in establishing proteomic patterns associated with PD. It also may be used to construct a diagnostic model with PD Biomarkers. Although this model of biomarkers fails to distinguish between PD and OND controls, it is able to differentiate PD from healthy controls.%目的 探讨帕金森病(PD)患者血清蛋白质组学特征,筛选PD特征性生物标志物.方法 选择原发性PD患者61例、其他神经变性病(OND)患者29例和健康人30名,用弱阳离子交换(WCX)纳米磁珠捕获血清蛋白质组分,用MALDI-TOF-MS(matrix assisted laser desorption/ionization time of flight inass spectrometer)检测各样品的蛋白质质谱,用Biomarker Wizard 3.1和Biomarker Patterns Software Version 5.0软件进行数据分析,筛选差异分子并建立PD诊断模型.用盲法验证此模型.结果

  19. Preparation of strong cation-exchange monolithic column and its application in polypeptide separation by capillary electrochromatography%强阳离子交换整体柱的研制及其在电色谱多肽分离中的应用

    Institute of Scientific and Technical Information of China (English)

    齐楠; 崔瑞红; 尤慧艳

    2011-01-01

    以丙烯酸、2-丙烯酰胺-2-甲基丙磺酸为功能单体,N,N'-亚甲基双丙烯酰胺为交联剂,正十二醇、1,4-丁二醇及二甲基亚砜为致孔剂,偶氮二异丁腈为引发剂,原位聚合制备了丙烯酰胺类强阳离子交换整体柱.考察了驱动电压、有机调节剂、盐浓度、pH值等对电渗流的影响.结果表明,电渗流与驱动电压的线性关系良好,相关系数为0.998 1;有机调节剂乙腈对电渗流的影响除与流动相的黏度有关外,还与同定相的溶胀有关,当浓度低时,电渗流随乙腈浓度的增加有反常的下降趋势;随着磷酸盐浓度逐渐增加,电渗流降低,与理论相符;在pH值为3~9范围内,电渗流基本上保持恒定,体现了整体柱使用酸碱范围宽的优越性.在优化的实验条件下,采用毛细管电色谱法在此整体柱上成功分离了5种多肽,体现了该类整体柱在多肽分离研究中的优势,为进一步将其应用于蛋白质分离研究打下了基础.%A strong cation-exchange monolithic column was prepared by polymerization inside the fused-silica capillary. The solution consisted of acrylic acid and 2-acrylamido-2-methyl-l-propanesulfonic acid as functional monomers, 7V,AT'-methyIenebisacrylamide as a cross-linking agent, dimethyl sulphoxide and dodecanol, 1,4-butanediol as organic porogenic solvents and azobisisobutyronitrile as a suitable initiator. The effects of the applied voltage, concentrations of organic modifier and salt solution, pH value on the electroosmotic flow were investigated. The experimental results showed that there existed a good linear relationship between the applied voltage and electroosmotic flow with a correlation coefficient of 0. 998 1 ; When the concentration of organic modifier (acetonitrile, CAN) was less than 70% , the swelling degree of stationary phase played a main role and the electroosmotic flow was decreased abnormally with the increase of CAN concentration; The electroosmotic flow

  20. Heavy metal cations permeate the TRPV6 epithelial cation channel.

    Science.gov (United States)

    Kovacs, Gergely; Danko, Tamas; Bergeron, Marc J; Balazs, Bernadett; Suzuki, Yoshiro; Zsembery, Akos; Hediger, Matthias A

    2011-01-01

    TRPV6 belongs to the vanilloid family of the transient receptor potential channel (TRP) superfamily. This calcium-selective channel is highly expressed in the duodenum and the placenta, being responsible for calcium absorption in the body and fetus. Previous observations have suggested that TRPV6 is not only permeable to calcium but also to other divalent cations in epithelial tissues. In this study, we tested whether TRPV6 is indeed also permeable to cations such as zinc and cadmium. We found that the basal intracellular calcium concentration was higher in HEK293 cells transfected with hTRPV6 than in non-transfected cells, and that this difference almost disappeared in nominally calcium-free solution. Live cell imaging experiments with Fura-2 and NewPort Green DCF showed that overexpression of human TRPV6 increased the permeability for Ca(2+), Ba(2+), Sr(2+), Mn(2+), Zn(2+), Cd(2+), and interestingly also for La(3+) and Gd(3+). These results were confirmed using the patch clamp technique. (45)Ca uptake experiments showed that cadmium, lanthanum and gadolinium were also highly efficient inhibitors of TRPV6-mediated calcium influx at higher micromolar concentrations. Our results suggest that TRPV6 is not only involved in calcium transport but also in the transport of other divalent cations, including heavy metal ions, which may have toxicological implications.

  1. Natural zeolite reactivity towards ozone: The role of compensating cations

    Energy Technology Data Exchange (ETDEWEB)

    Valdes, Hector, E-mail: hvaldes@ucsc.cl [Laboratorio de Tecnologias Limpias (F. Ingenieria), Universidad Catolica de la Santisima Concepcion, Alonso de Ribera 2850, Concepcion (Chile); Alejandro, Serguei; Zaror, Claudio A. [Departamento de Ingenieria Quimica (F. Ingenieria), Universidad de Concepcion, Concepcion (Chile)

    2012-08-15

    Highlights: Black-Right-Pointing-Pointer Chemical and thermal treatment enhances catalytic activity of natural zeolite. Black-Right-Pointing-Pointer Modified natural zeolite exhibits high stability after thermal treatment. Black-Right-Pointing-Pointer Reducing the compensating cation content leads to an increase on ozone abatement. Black-Right-Pointing-Pointer Surface active atomic oxygen was detected using the DRIFT technique. Black-Right-Pointing-Pointer The highest reactivity toward ozone was performed by NH4Z3 zeolite sample. - Abstract: Among indoor pollutants, ozone is recognised to pose a threat to human health. Recently, low cost natural zeolites have been applied as alternative materials for ozone abatement. In this work, the effect of compensating cation content of natural zeolite on ozone removal is studied. A Chilean natural zeolite is used here as starting material. The amount of compensating cations in the zeolite framework was modified by ion exchange using an ammonium sulphate solution (0.1 mol L{sup -1}). Characterisation of natural and modified zeolites were performed by X-ray powder diffraction (XRD), nitrogen adsorption at 77 K, elemental analysis, X-ray fluorescence (XRF), thermogravimetric analysis coupled with mass spectroscopy (TGA-MS), and temperature-programmed desorption of ammonia (NH{sub 3}-TPD). Ozone adsorption and/or decomposition on natural and modified zeolites were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Results show that the zeolite compensating cation content affects ozone interaction with zeolite active sites. Ammonium ion-exchange treatments followed by thermal out-gassing at 823 K, reduces ozone diffusion resistance inside the zeolite framework, increasing ozone abatement on zeolite surface active sites. Weak and strong Lewis acid sites of zeolite surface are identified here as the main active sites responsible of ozone removal.

  2. The adjuvant mechanism of cationic dimethyldioctadecylammonium liposomes

    DEFF Research Database (Denmark)

    Korsholm, Karen Smith; Agger, Else Marie; Foged, Camilla;

    2007-01-01

    Cationic liposomes are being used increasingly as efficient adjuvants for subunit vaccines but their precise mechanism of action is still unknown. Here, we investigated the adjuvant mechanism of cationic liposomes based on the synthetic amphiphile dimethyldioctadecylammonium (DDA). The liposomes ...

  3. Tripodal Receptors for Cation and Anion Sensors

    NARCIS (Netherlands)

    Kuswandi, Bambang; Nuriman,; Verboom, Willem; Reinhoudt, David N.

    2006-01-01

    This review discusses different types of artificial tripodal receptors for the selectiverecognition and sensing of cations and anions. Examples on the relationship between structure andselectivity towards cations and anions are described. Furthermore, their applications as potentiometricion sensing

  4. Ion exchange properties of humus acids

    Science.gov (United States)

    Shoba, V. N.; Chudnenko, K. V.

    2014-08-01

    Ion exchange equilibriums in a complex of brown humic acids (HAs) and related fulvic acids (FAs) with cations (H+, K+, Na+, Ca2+, Mg2+, Zn2+, Mn2+, Cu2+, Fe3+, and Al3+) have been studied, and the activity coefficients of the acid monoionic forms have been determined. The composition of the stoichiometric cell in the system of black and brown HAs and related FAs in a leached chernozem of the Ob' region has been calculated with consideration for the earlier studies of the ion exchange properties of black HAs and related FAs. It has been shown that hydrogen, calcium, magnesium, aluminum, and iron are the major components in the exchange complex of humus acids in the leached chernozem with the other cations being of subordinate importance. In spite of some differences between the analytical and calculated compositions of the humus acids, the results of the calculations can be considered satisfactory. They indicate that calculations are feasible for such complex objects as soils, and their accuracy will improve with the expansion of the experimental studies. The physicochemical simulation of the transformation of the humus acid composition under different acid-base conditions shows that the contents of most cations decrease under alkalization, and hydroxides or carbonates become the most stable forms of these cations. Under the acidification of solutions, the binding of alkaline and alkaline-earth elements by humus acids decreases and the adsorption of iron and aluminum by humus acids increases.

  5. Diffusion of an organic cation into root cell walls.

    Science.gov (United States)

    Meychik, N R; Yermakov, I P; Prokoptseva, O S

    2003-07-01

    Uptake of a cationic dye (methylene blue) by isolated root cell walls, roots of whole transpiring seedlings, and excised roots was investigated using 7-day-old seedlings of cucumber, maize, and wheat. The number of ionogenic groups per 1 g dry and wet weight of the root cell walls, their swelling capacity (K(cw)), time-dependence of methylene blue (M(cw)) ion exchange capacity, and diffusion coefficients of the cation diffusion in the polymer matrix of the cell walls (D(cw)) were determined. The M(cw) value depended on pH (or carboxyl group dissociation); it changed in accordance with the number of carboxyl groups per 1 g cell wall dry weight. This parameter decreased in the order: cucumber > wheat > maize. For description of experimental kinetic curves and calculation of cation diffusion coefficients, the equation for ion diffusion into a cylinder of infinite length was used. The chosen model adequately described cation diffusion in cell walls and roots. Diffusion coefficient values for cucumber, wheat, and maize were 3.1*10(-8), 1.3*10(-8), and 8.4*10(-8) cm(2)/sec, respectively. There was a statistically significant linear dependence between K(cw) and D(cw) values, which characterize the same property of the polymer matrix, rigidity of its polymer structure or the degree of cross-linkage or permeability. This also confirms the right choice of the model selected for calculation of methylene blue diffusion coefficients, because K(cw) and D(cw) values were obtained in independent experiments. The coefficients determined for methylene blue diffusion in transpiring seedling roots (D(ts)) and excised roots (D(er)) depended on the plant species. The rate of methylene blue diffusion into the excised roots was either 1.5-fold lower (cucumber) or 3-4-times lower (maize, wheat) than in cell walls. The values of diffusion coefficients in roots of whole seedlings were comparable which those for the cell walls. On the basis of the experimental data and results of calculations

  6. Exchangers man the pumps: Functional interplay between proton pumps and proton-coupled Ca(2+) exchangers

    Science.gov (United States)

    Tonoplast-localised proton-coupled Ca(2+) transporters encoded by cation/H(+) exchanger (CAX) genes play a critical role in sequestering Ca(2+) into the vacuole. These transporters may function in coordination with Ca(2+) release channels, to shape stimulus-induced cytosolic Ca(2+) elevations. Recen...

  7. Single column comprehensive analysis of pharmaceutical preparations using dual-injection mixed-mode (ion-exchange and reversed-phase) and hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Kazarian, Artaches A; Taylor, Mark R; Haddad, Paul R; Nesterenko, Pavel N; Paull, Brett

    2013-12-01

    The comprehensive separation and detection of hydrophobic and hydrophilic active pharmaceutical ingredients (APIs), their counter-ions (organic, inorganic) and excipients, using a single mixed-mode chromatographic column, and a dual injection approach is presented. Using a mixed-mode Thermo Fisher Acclaim Trinity P1 column, APIs, their counter-ions and possible degradants were first separated using a combination of anion-exchange, cation-exchange and hydrophobic interactions, using a mobile phase consisting of a dual organic modifier/salt concentration gradient. A complementary method was also developed using the same column for the separation of hydrophilic bulk excipients, using hydrophilic interaction liquid chromatography (HILIC) under high organic solvent mobile phase conditions. These two methods were then combined within a single gradient run using dual sample injection, with the first injection at the start of the applied gradient (mixed-mode retention of solutes), followed by a second sample injection at the end of the gradient (HILIC retention of solutes). Detection using both ultraviolet absorbance and refractive index enabled the sensitive detection of APIs and UV-absorbing counter-ions, together with quantitative determination of bulk excipients. The developed approach was applied successfully to the analysis of a dry powder inhalers (Flixotide(®), Spiriva(®)), enabling comprehensive quantification of all APIs and excipients in the sample.

  8. Microscopic approach for the identification of cationic membrane fouling during cheddar cheese whey electroacidification.

    Science.gov (United States)

    Lin Teng Shee, F; Angers, P; Bazinet, L

    2008-06-15

    This is the first time that fouling of cation-exchange membranes during cheddar cheese whey electroacidification with bipolar membranes is reported. A mineral fouling was observed only on the cationic membrane side in contact with the base. The deposit was identified as magnesium hydroxide and this fouling was more important on the cation-exchange membrane situated close to the cathode. Little deposit was formed after six electroacidification runs, but on long time, the buildup of fouling film would lead after many electroacidifications to an important decrease of the system efficiency. Since, fouling of permselective membranes represents one of the major issues in electrodialytic processes, this result will be the basis for the determination of cleaning conditions allowing the prevention of such a fouling.

  9. Incorporation of Monovalent Cations in Sulfate Green Rust

    DEFF Research Database (Denmark)

    Christiansen, B. C.; Dideriksen, K.; Katz, A.;

    2014-01-01

    Green rust is a naturally occurring layered mixed-valent ferrous-ferric hydroxide, which can react with a range of redox-active compounds. Sulfate-bearing green rust is generally thought to have interlayers composed of sulfate and water. Here, we provide evidence that the interlayers also contain...... with water showed that Na+ and K+ were structurally fixed in the interlayer, whereas Rb+ and Cs+ could be removed, resulting in a decrease in the basal layer spacing. The incorporation of cations in the interlayer opens up new possibilities for the use of sulfate green rust for exchange reactions with both...

  10. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents

    Energy Technology Data Exchange (ETDEWEB)

    Snow, Mathew S.; Finck, Martha R.; Carney, Kevin P.; Morrison, Samuel S.

    2017-02-01

    Ta, Hf, and W analyses from complex matrices (including environmental samples) require high purification of these analytes from each other and major/trace matrix constituents, however, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that suffer from relatively similar distribution coefficient (Kd) values for these analytes. This work reports assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/W,Hf Kd values of up to 106, representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1x4 resin. Variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1x4 resin. Finally, analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils, using a single chromatographic step.

  11. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents.

    Science.gov (United States)

    Snow, Mathew S; Finck, Martha R; Carney, Kevin P; Morrison, Samuel S

    2017-02-10

    Tantalum (Ta), hafnium (Hf), and tungsten (W) analyses from complex matrices require high purification of these analytes from each other and major/trace matrix constituents, however, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that show relatively similar distribution coefficient (Kd) values for each element. This work reports an assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/Hf and Ta/W Kd values of up to 10(6) and 10(4) (respectively), representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1×4 resin. Variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1×4 resin. Analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils using a single chromatographic step.

  12. Single-stage separation and esterification of cation salt carboxylates using electrodeionization

    Science.gov (United States)

    Lin, YuPo J.; Henry, Michael; Hestekin, Jamie; Snyder, Seth W.; St. Martin, Edward J.

    2006-11-28

    A method of and apparatus for continuously making an organic ester from a lower alcohol and an organic acid is disclosed. An organic acid or salt is introduced or produced in an electrode ionization (EDI) stack with a plurality of reaction chambers each formed from a porous solid ion exchange resin wafer interleaved between anion exchange membranes or an anion exchange membrane and a cation exchange membrane or an anion exchange membrane and a bipolar exchange membranes. At least some reaction chambers are esterification chambers and/or bioreactor chambers and/or chambers containing an organic acid or salt. A lower alcohol in the esterification chamber reacts with an anion to form an organic ester and water with at least some of the water splitting with the ions leaving the chamber to drive the reaction.

  13. Preparation and Photochemical Behavior of a Cationic Azobenzene Dye-Montmorillonite Intercalation Compound

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Montmorillonite/cationic azobenzene dye(p-(δ-triethylammoniobutoxy)-p'-methyl-azobenzene bromide) intercalation compounds were prepared by the conventional ion exchange method. As compared with that of pure cationic azo-dye, the thermal stability of the intercalated dye was greatly enhanced, and the absorption band corresponding to azobenzene group in intercalated dye shifted towards longer wave length by 38 nm. This could be ascribed to the strong conjugation of cationic azo-dye supramolecular order structure(J cluster) confined in a nanoscale space of montmorillonite interlayer gallery. UV/vis spectra data show that the intercalated azo dye in the montmorillonite interlayer space exhibited reversible trans-to-cis photoisomerization and daylight cis-to-trans back reaction. FTIR indicates the successful intercalation of cationic azo-dye into the montmorillonite interlayer.

  14. Enthalpy-entropy compensation for n-hexane adsorption on Y zeolite containing transition metal cations

    Directory of Open Access Journals (Sweden)

    Hercigonja R.

    2015-01-01

    Full Text Available In this work, the values of entropy changes related to n-hexane adsorption onto cation exchanged Y zeolite were calculated from differential heats. Various transition metal cations (Co2+, Ni2+, Zn2+ and Cd2+ were introduced into the lattice of the parent NaY, and the existence of enthalpy-entropy compensation effect related to n-hexane adsorption, id. est, the linearity of -ΔH vs. -ΔS plots was examined. The compensation effect was confirmed for all investigated zeolites. The compensation effect can be comprehended as governed by ion-induced dipole interaction between highly polarizing cationic centers in zeolite and nonopolar n-hexane molecules. Finally, the compensation effect and so the compensation temperature were found to depend on the type of charge-balancing cation (charge, size and electronic configuration. [Projekat Ministarstva nauke Republike Srbije, br. 172018

  15. Utilization of a diol-stationary phase column in ion chromatographic separation of inorganic anions.

    Science.gov (United States)

    Arai, Kaori; Mori, Masanobu; Kozaki, Daisuke; Nakatani, Nobutake; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-12-28

    We describe the ion chromatographic separation of inorganic anions using a diol-stationary phase column (-CH(OH)CH(2)OH; diol-column) without charged functional groups. Anions were separated using acidic eluent as in typical anion-exchange chromatography. The retention volumes of anions on the diol-column increased with increasing H(+) concentration in the eluent. The anion-exchange capacities of diol-columns in the acidic eluent (pH 2.8) were larger than that of zwitterionic stationary phase column but smaller than that of an anion-exchange column. The separation of anions using the diol-column was strongly affected by the interaction of H(+) ions with the diol-functional groups and by the types of the eluents. In particular, the selection of the eluent was very important for controlling the retention time and resolution. Good separation was obtained using a diol-column (HILIC-10) with 5 mM phthalic acid as eluent. The limits of detection at a signal-to-noise ratio of 3 ranged from 1.2 to 2.7 μM with relative standard deviations (RSD, n=5) of 0.04-0.07% for the retention time and 0.4-2.0% for the peak areas. This method was successfully applied to the determination of H(2)PO(4)(-), Cl(-), and NO(3)(-) in a liquid fertilizer sample.

  16. Quality by design--thermodynamic modelling of chromatographic separation of proteins.

    Science.gov (United States)

    Mollerup, Jørgen M; Hansen, Thomas Budde; Kidal, Steffen; Staby, Arne

    2008-01-11

    A desired goal of the PAT framework is to design and develop well-understood processes that will consistently ensure a predefined quality at the end of the manufacturing process. Such procedures would be consistent with the basic tenet of quality by design and could reduce risks to quality and regulatory concerns while improving efficiency. To support a more in-depth understanding of the design and development of a chromatographic purification process the paper discusses the general thermodynamic principles of ligand-binding and models of multi-component adsorption in ion-exchange and hydrophobic chromatography. The parameters in the models are easy to determine and have a well-defined physical significance. Examples demonstrate how the model parameters can be determined from experimental data and in order to validate the model, simulated chromatograms are compared to the corresponding experimental chromatograms. Finally it is demonstrated how a simulation can be used to explain an aberration.

  17. International Exchanges

    Institute of Scientific and Technical Information of China (English)

    2014-01-01

    <正>On April 1st,2014,CPAPD Deputy Secretary General Ms.Chen Huaifan met with Mr.Djudjuk Juyoto Suntani,President of the World Peace Committee,Indonesia,who headed the delegation,in the CPAPD office.The two sides exchanged views on issues of common concern including cooperation between the two organizations and the inheritance of Chinese culture.

  18. Exchange Options

    NARCIS (Netherlands)

    Jamshidian, Farshid

    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

  19. A method for the separation of hybrids of chromatographically identical oligomeric proteins. Use of 3,4,5,6-tetrahydrophthaloyl groups as a reversible "chromatographic handle".

    Science.gov (United States)

    Gibbons, I; Schachman, H K

    1976-01-13

    Hybridization experiments with variants of an oligomeric protein often provide important information regarding subunit structure, function, and interactions. In some systems, however, the variants are so similar electrophoretically and chromatographically that purification of individual hybrids is not feasible. Therefore a method was developed for preparing hybrids by using 3,4,5,6-tetrahydrophthalic anhydride as a reversible acylating agent for protein amino groups. The technique involved acylating about 30% of the amino groups at pH 8 to give a derivative with a markedly altered net charge, formation of the hybrid set with unmodified and modified species, separation of the individual components by ion-exchange chromatography, and finally removal of the tetrahydrophthaloyl groups from the desired hybrid by incubation for about 1 day at pH 6 and room temperature. Experiments with model compounds and two enzymes showed that the anhydride was sepcific for amino groups. The extent of modification of proteins was measured by the spectral change at 250 nm, the loss of free amino groups, and the change in electrophoretic mobility of the polypeptide chains in polyacrylamide gels containing 8 M urea. Deacylation of modified, inactive aldolase and the catalytic subunit of aspartate transcarbamylase led to the restoration of the enzyme activity and electrophoretic mobility of the unmodified proteins. Both intra- and inter-subunit hybrids of aspartate transcarbamylase were prepared and isolated by using the tetrahydrophthaloyl groups as a reversible "chromatographic handle". Prior to deacylation the inter-subunit hybrid containing one acylated and one native catalytic subunit (and negative regulatory sub-units) exhibited no homotropic cooperativity and after deacylation the characteristic allosteric properties of the enzyme were regained. Similarly the ligand-promoted conformational changes associated with the allosteric transition were resotred upon deacylation of the intra

  20. Identification of co-existing cationic surfactants with preliminary separation on silica HPTLC plates using mixed aqueous sodium chloride-ethanol as eluent

    Directory of Open Access Journals (Sweden)

    Ali Mohammad

    2015-12-01

    Full Text Available A new high-performance thin-layer chromatographic system comprising of silica gel 60 HPTLC plates as stationary phase and ethanol-5% aqueous sodium chloride (8:2 as mobile phase has been identified as most suitable for separation of quaternary mixture of cationic surfactants. Separation efficacy of developed method has been established by obtaining well-resolved densitogram of separated spots. To check the versatility, effects of presence of metal cations, inorganic anions, amino acids, vitamins and non-ionic surfactants as impurities were also examined. The chromatographic parameters like ΔRF, separation factor (α, resolution (RS and limit of detection were also calculated. The proposed method is applicable for the identification of surfactants in eye drops and Colgate Plax mouthwash.

  1. Physicochemical and chromatographic method of characterization of Matricaria recutita tinctures

    Directory of Open Access Journals (Sweden)

    Jonathan Parra

    2016-02-01

    Full Text Available Context: The pharmacological activity of medicinal products containing plant materials depends on their specific components. However, these components are not characterized in their entirety in all cases. Therefore, manufacturing processes must be duly characterized and validated. Aims: To characterize a chamomile (Matricaria recutita tincture through chemometric analysis of chromatographic data in order to establish quality parameters for its production. Methods: Various chamomile tinctures were manufactured and the precision and robustness of the production process for each was verified. The physicochemical properties of the tinctures were characterized and their chromatographic digital fingerprints analysed through chemometric methods. Results: A good correlation between the physicochemical characterization and the chromatographic analysis was demonstrated. The preparation methodology was proved to be repeatable as long as the source of the plant material is not altered. Conclusions: The principal component multivariate analysis of chromatograms was a helpful and simple tool for the characterization and traceability of the production method.

  2. Mathematical functions for the representation of chromatographic peaks.

    Science.gov (United States)

    Di Marco, V B; Bombi, G G

    2001-10-05

    About ninety empirical functions for the representation of chromatographic peaks have been collected and tabulated. The table, based on almost 200 references, reports for every function: (1) the most used name; (2) the most convenient equation, with the existence intervals for the adjustable parameters and for the independent variable; (3) the applications; (4) the mathematical properties, in relation to the possible applications. The list includes also equations originally proposed to represent peaks obtained in other analytical techniques (e.g. in spectroscopy), which in many instances have proved useful in representing chromatographic peaks as well; the built-in functions employed in some commercial peak-fitting software packages were included, too. Some of the most important chromatographic functions, i.e. the Exponentially Modified Gaussian, the Poisson, the Log-normal, the Edgeworth/Cramér series and the Gram/Charlier series, have been reviewed and commented in more detail.

  3. Transformation of anthracene on various cation-modified clay minerals.

    Science.gov (United States)

    Li, Li; Jia, Hanzhong; Li, Xiyou; Wang, Chuanyi

    2015-01-01

    In this study, anthracene was employed as a probe to explore the potential catalytic effect of clay minerals in soil environment. Clay minerals saturated with various exchangeable cations were tested. The rate of anthracene transformation follows the order: Fe-smectite > Cu-smectite > Al-smectite ≈ Ca-smectite ≈ Mg-smectite ≈ Na-smectite. This suggests that transition-metal ions such as Fe(III) play an important role in anthracene transformation. Among Fe(III)-saturated clays, Fe(III)-smectite exhibits the highest catalytic activity followed by Fe(III)-illite, Fe(III)-pyrophyllite, and Fe(III)-kaolinite, which is in agreement with the interlayer Fe(III) content. Moreover, effects by two common environmental factors, pH and relative humidity (RH), were evaluated. With an increase in pH or RH, the rate of anthracene transformation decreases rapidly at first and then is leveled off. GC-MS analysis identifies that the final product of anthracene transformation is 9,10-anthraquinone, a more bioavailable molecule compared to anthracene. The transformation process mainly involves cation-π bonding, electron transfer leading to cation radical, and further oxidation by chemisorbed O2. The present work provides valuable insights into the abiotic transformation and the fate of PAHs in the soil environment and the development of contaminated land remediation technologies.

  4. The Free Tricoordinated Silyl Cation Problem

    Directory of Open Access Journals (Sweden)

    Čičak, H.

    2010-03-01

    Full Text Available As the importance and abundance of silicon in our environment is large, it has been thought that silicon might take the place of carbon in forming a host of similar compounds and silicon-based life. However, until today there is no experimental evidence for such a hypothesis and carbon is still unique among the elements in the vast number and variety of compounds it can form. Also, the corresponding derivatives of the two elements show considerable differences in their chemical properties.The essential debate concerning organosilicon chemistry relates to the existence of the free planar tricoordinated silyl cations in condensed phase (R3Si+, in analogy to carbocations (R3C+ which have been known and characterized as free species. Although silyl cations are thermodynamically more stable than their carbon analogs, they are very reactive due to their high inherent electrophilicity and the ability of hypervalent coordination. On the other hand, stabilization by inductive and hyperconjugative effects and larger steric effects of carbocations make them less sensitive to solvation or other environmental effects than silyl cations. Hence, observation of free silyl cations in the condensed phase proved extremely difficult and the actual problem is the question of the degree of the (remaining silyl cation character.The first free silyl cation, trimesitylsilyl cation, and in analogy with it tridurylsilyl cation, were synthesized by Lambert et al. Free silyl cations based on analogy to aromatic ions (homocyclopropenylium and tropylium have also been prepared. However, in these silyl cations the cationic character is reduced by internal π -conjugation. Čičak et al. prepared some silyl-cationic intermediates (Me3Si--CH≡CR+in solid state. With the help of quantum-mechanical calculations it was concluded that these adducts have much more silyl cation than carbocation character.

  5. Selective ion exchange recovery of rare earth elements from uranium mining solutions

    Science.gov (United States)

    Rychkov, Vladimir N.; Kirillov, Evgeny V.; Kirillov, Sergey V.; Bunkov, Grigory M.; Mashkovtsev, Maxim A.; Botalov, Maxim S.; Semenishchev, Vladimir S.; Volkovich, Vladimir A.

    2016-09-01

    A comparative study of rare earth, ferric and aluminum ions ion exchange behavior on gel sulfonated p;olystyrene cation exchange resins depending on the degree of the matrix cross-linking and pH of the solution is presented. Selective ion exchange of REEs is possible at the pH range of 1.5-2.0 using strongly acidic cation exchange resins containing more than 8 % of DVB. The preliminary results of testing the efficiency of REEs recovery from the industrial uranium underground leaching solutions are also presented.

  6. Long-term effects of high nitrogen loads on cation and carbon riverine export in agricultural catchments.

    Science.gov (United States)

    Aquilina, Luc; Poszwa, Anne; Walter, Christian; Vergnaud, Virginie; Pierson-Wickmann, Anne-Catherine; Ruiz, Laurent

    2012-09-01

    The intensification of agriculture in recent decades has resulted in extremely high nitrogen inputs to ecosystems. One effect has been H(+) release through NH(4)(+) oxidation in soils, which increases rock weathering and leads to acidification processes such as base-cation leaching from the soil exchange complex. This study investigated the evolution of cation concentrations over the past 50 years in rivers from the Armorican crystalline shield (Brittany, western France). On a regional scale, acidification has resulted in increased base-cation riverine exports (Ca(2+), Mg(2+), Na(+), K(+)) correlated with the increased NO(3)(-) concentration. The estimated cation increase is 0.7 mmol(+)/L for Ca(2+) + Mg(2+) and 0.85 mmol(+)/L for total cations. According to mass balance, cation loss represents >30% of the base-cation exchange capacity of soils. Long-term acidification thus contributes to a decline in soil productivity. Estimates of the total organic nitrogen annually produced worldwide indicate that acidification may also constitute an additional carbon source in crystalline catchments if compensated by liming practices.

  7. Cd/Hg cationic substitution in magic-sized CdSe clusters: Optical characterization and theoretical studies

    Energy Technology Data Exchange (ETDEWEB)

    Antanovich, Artsiom; Prudnikau, Anatol; Gurin, Valerij; Artemyev, Mikhail, E-mail: m_artemyev@yahoo.com

    2015-07-09

    Highlights: • HgSe magic-sized clusters were prepared via Cd/Hg cationic exchange in pyridine. • Upon cationic exchange CdSe clusters behave differently from quantum dots or rods. • Theoretical calculations of magic-sized clusters agree well with experimental data. - Abstract: We examine conversion of magic-sized CdSe clusters (MSCs) into HgSe ones by means of Cd/Hg cation exchange. With this procedure Cd{sub 8}Cd{sub 17}– and Cd{sub 32}–selenide clusters can be converted into corresponding Hg{sub 8}–, Hg{sub 17}– and Hg{sub 32}–selenide ones. Upon cationic exchange MSCs behavior differs from that of bulkier counterparts – larger (2–3 nm) quantum dots. Unlike CdSe colloidal quantum dots, magic-sized clusters are converted in fast and complete manner without a formation of intermediate mixed Cd{sub x}Hg{sub 1−x} compounds that was established on the basis of optical absorption spectroscopy and chemical composition analysis. These assumptions were supported by DFT quantum chemical calculations performed for Cd{sub 8}–, Cd{sub 17}– and Hg{sub 8}–, Hg{sub 17}–selenide model clusters. Energies of experimental and calculated optical transitions were compared in order to prove the isostructural character of cationic substitution in magic-sized clusters.

  8. Anion stripping as a general method to create cationic porous framework with mobile anions.

    Science.gov (United States)

    Mao, Chengyu; Kudla, Ryan A; Zuo, Fan; Zhao, Xiang; Mueller, Leonard J; Bu, Xianhui; Feng, Pingyun

    2014-05-28

    Metal-organic frameworks (MOFs) with cationic frameworks and mobile anions have many applications from sensing, anion exchange and separation, to fast ion conductivity. Despite recent progress, the vast majority of MOFs have neutral frameworks. A common mechanism for the formation of neutral frameworks is the attachment of anionic species such as F(-) or OH(-) to the framework metal sites, neutralizing an otherwise cationic scaffolding. Here, we report a general method capable of converting such neutral frameworks directly into cationic ones with concurrent generation of mobile anions. Our method is based on the differential affinity between distinct metal ions with framework anionic species. Specifically, Al(3+) is used to strip F(-) anions away from framework Cr(3+) sites, leading to cationic frameworks with mobile Cl(-) anions. The subsequent anion exchange with OH(-) further leads to a porous network with mobile OH(-) anions. New materials prepared by anion stripping can undergo ion exchange with anionic organic dyes and also exhibit much improved ionic conductivity compared to the original unmodified MOFs.

  9. Scale-up of chromatographic ion-exchange processes in biotechnology

    DEFF Research Database (Denmark)

    Al-Jibbouri, Sattar

    2006-01-01

    The van Deemter equation has been used to derive a rule of thumb guideline for scaling. The scaling is done by the concept of time scales. The time scales are kept identical for all the columns by scaling the flow rate to the total void volume and the load to the amount of the media. The verifica...

  10. [The gas chromatographic detection of acetylene in cadaveric material].

    Science.gov (United States)

    Iablochkin, V D

    1999-01-01

    Acetylene traces were detected by gas chromatography in the cadaveric right crural muscle of a 30-year-old man dead from an explosion of an acetylene reservoir at a plant. Acetylene was identified using the absolute calibration method on 3 standard gas chromatographic columns, reaction gas chromatography, and acetylene "deduction" by silver sulfate on silicagel.

  11. Chromatographic separation of alkaline phosphatase from dental enamel

    DEFF Research Database (Denmark)

    Moe, D; Kirkeby, S; Salling, E

    1989-01-01

    Alkaline phosphatase (AP) was prepared from partly mineralized bovine enamel by extraction in phosphate buffer, centrifugation and various chromatographic techniques. Chromatofocusing showed that the enamel enzyme possessed five isoelectric points at the acid pH level ranging from pH 5.7 to pH 4....

  12. On the ion chromatographic determination of S(IV)

    Science.gov (United States)

    Dasgupta, Purnendu K.

    Ion Chromatographie determination of S(IV) is described with special reference to the determination of SO 2(g) and/or aerosol S(IV) along with chloride, nitrate and sulfate in particulate matter. A method is presented for the baseline separation of the above species. The Chromatographic behavior of hydroxymethanesulfonate under various eluent conditions is discussed.

  13. Chromatographic fingerprints analysis for evaluation of Ginkgo Biloba products

    Science.gov (United States)

    The leaf extract of Ginkgo biloba has purported value for improving mental capacities in Alzheimer’s patients. The flavonoids and the terpene lactones are considered to be the two main active components that influence human health. This paper compared an LC/UV chromatographic fingerprint method wi...

  14. Chromatographic profiles of Ginkgo biloba leaves and selected products

    Science.gov (United States)

    An LC-DAD-ESI/MS method was developed to obtain chromatographic profiles for the flavonoids and terpene lactones of Ginkgo biloba leaves and selected G. biloba products. The method was used to identify 46 glycosylated flavonols and flavones, 3 free flavonol aglycones, catechin, 10 biflavones, a dihy...

  15. Note on the chromatographic analyses of marine polyunsaturated fatty acids

    Science.gov (United States)

    Schultz, D.M.; Quinn, J.G.

    1977-01-01

    Gas-liquid chromatography was used to study the effects of saponification/methylation and thin-layer chromatographic isolation on the analyses of polyunsaturated fatty acids. Using selected procedures, the qualitative and quantitative distribution of these acids in marine organisms can be determined with a high degree of accuracy. ?? 1977 Springer-Verlag.

  16. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    Science.gov (United States)

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  17. Performance of chromatographic systems to model soil-water sorption.

    Science.gov (United States)

    Hidalgo-Rodríguez, Marta; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

    2012-08-24

    A systematic approach for evaluating the goodness of chromatographic systems to model the sorption of neutral organic compounds by soil from water is presented in this work. It is based on the examination of the three sources of error that determine the overall variance obtained when soil-water partition coefficients are correlated against chromatographic retention factors: the variance of the soil-water sorption data, the variance of the chromatographic data, and the variance attributed to the dissimilarity between the two systems. These contributions of variance are easily predicted through the characterization of the systems by the solvation parameter model. According to this method, several chromatographic systems besides the reference octanol-water partition system have been selected to test their performance in the emulation of soil-water sorption. The results from the experimental correlations agree with the predicted variances. The high-performance liquid chromatography system based on an immobilized artificial membrane and the micellar electrokinetic chromatography systems of sodium dodecylsulfate and sodium taurocholate provide the most precise correlation models. They have shown to predict well soil-water sorption coefficients of several tested herbicides. Octanol-water partitions and high-performance liquid chromatography measurements using C18 columns are less suited for the estimation of soil-water partition coefficients.

  18. Afrikaans Syllabification Patterns

    Directory of Open Access Journals (Sweden)

    Tilla Fick

    2010-01-01

    Full Text Available In contrast to English, automatic hyphenation by computer of Afrikaans words is a problem that still needs to be addressed, since errors are still often encountered in printed text. An initial step in this task is the ability to automatically syllabify words. Since new words are created continuously by joining words, it is necessary to develop an “intelligent” technique for syllabification. As a first phase of the research, we consider only the orthographic information of words, and disregard both syntactic and morphological information. This approach allows us to use machine-learning techniques such as artificial neural networks and decision trees that are known for their pattern recognition abilities. Both these techniques are trained with isolated patterns consisting of input patterns and corresponding outputs (or targets that indicate whether the input pattern should be split at a certain position, or not. In the process of compiling a list of syllabified words from which to generate training data for the  syllabification problem, irregular patterns were identified. The same letter patterns are split differently in different words and complete words that are spelled identically are split differently due to meaning. We also identified irregularities in and between  the different dictionaries that we used. We examined the influence range of letters that are involved in irregularities. For example, for their in agter-ente and vaste-rente we have to consider three letters to the left of r to be certain where the hyphen should be inserted. The influence range of the k in verstek-waarde and kleinste-kwadrate is four to the left and three to the right. In an analysis of letter patterns in Afrikaans words we found that the letter e has the highest frequency overall (16,2% of all letters in the word list. The frequency of words starting with s is the highest, while the frequency of words ending with e is the highest. It is important to

  19. International Exchanges

    Institute of Scientific and Technical Information of China (English)

    2015-01-01

    On October 12,2015,Mr.Zhu Rui,CPAPD Secretary General,chaired informal discussions with U.S.young experts and scholars on arms control and non-proliferation.The two sides exchanged views on international arms control,disarmament,non-proliferation and nuclear security,etc.During October 12 to 16,2015,at the invitation of the CPAPD,a four-member delegation from the Vietnam Peace Committee headed by its Vice-President Ms.Nguyen Thi Hoang Van

  20. High-performance liquid chromatographic determination of the imino acids (opines) meso-alanopine and D-strombine in muscle extract of invertebrates

    NARCIS (Netherlands)

    Sandee, B.; Schipper, C.A.; Eertman, R.H.M.

    1996-01-01

    A sensitive HPLC method is presented for the determination of the imino acids alanopine and strombine, anaerobic metabolites that are formed in muscle tissue of several species of invertebrates. The separation of alanopine and strombine was achieved using the Alltech OA 2000 cation-exchange column.

  1. Cationic Dihydrogen/Dihydride Complexes of Osmium: Structure and Dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Egbert, Jonathan D.; Bullock, R. Morris; Heinekey, D. M.

    2007-03-22

    Reaction of Cp*Os(CO)2Cl with (Et3Si )(BArF4) under hydrogen gas affords the cationic hydrogen complex [Cp*Os(CO)2(H2)][BArF4] (1), (Cp* = C5Me5; ArF = C6F5). When this reaction is carried out with HD gas, complex 1-d1 results, with JHD = 24.5 Hz. When solutions of complex 1 are monitored by 1H NMR spectroscopy over several days, the gradual formation of a trans dihydride species is observed. Similarly, reaction of CpOs(dppm)Br with NaBArF*4 (ArF* = 3,5-(CF3)2C6H3) under hydrogen affords the cationic dihydride complex [CpOs(dppm)H2]BArF*4 (2). At 295 K, complex 2 exists as a 10:1 mixture of cis and trans isomers. The 1H NMR spectrum of the cis form in the hydride region exhibits a triplet with JHP = 6.5 Hz, due to rapid exchange of the hydrogen atoms. At low temperature, static spectra of the HH'PP' spin system can be obtained, revealing quantum mechanical exchange coupling between the two hydride ligands. The observed JHH' is temperature dependent, varying from 133 Hz at 141 K to 176 Hz at 198 K. This is the first report of detectable exchange coupling between pairs of chemically equivalent hydrogen atoms. Research at the University of Washington was supported by the National Science Foundation. Research at Brookhaven National Laboratory was carried out under contract DE-AC02-98CH10886 with the U.S. Department of Energy and was supported by its Division of Chemical Sciences, Office of Basic Energy Sciences. Research at Pacific Northwest National Laboratory (PNNL) was funded by LDRD funds. PNNL is operated by Battelle for the US Department of Energy.

  2. Hydrolyzed Poly(acrylonitrile) Electrospun Ion-Exchange Fibers.

    Science.gov (United States)

    Jassal, Manisha; Bhowmick, Sankha; Sengupta, Sukalyan; Patra, Prabir K; Walker, Douglas I

    2014-06-01

    A potential ion-exchange material was developed from poly(acrylonitrile) fibers that were prepared by electrospinning followed by alkaline hydrolysis (to convert the nitrile group to the carboxylate functional group). Characterization studies performed on this material using X-ray photoelectron spectroscopy, scanning electron microscopy, Fourier-Transform infra-red spectroscopy, and ion chromatography confirmed the presence of ion-exchange functional group (carboxylate). Optimum hydrolysis conditions resulted in an ion-exchange capacity of 2.39 meq/g. Ion-exchange fibers were used in a packed-bed column to selectively remove heavy-metal cation from the background of a benign, competing cation at a much higher concentration. The material can be efficiently regenerated and used for multiple cycles of exhaustion and regeneration.

  3. An improved extraction chromatographic resin for the separation of uranium from acidic nitrate media

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, M.L.; Horwitz, E.P.; Sajdak, L.R.; Chiarizia, R. [Chemistry Division, Argonne National Laboratory, 60439 Argonne, IL (United States)

    2001-07-06

    The preparation and characterization of a new extraction chromatographic resin exhibiting extraordinarily strong retention of hexavalent uranyl ion over a wide range of nitric acid concentrations and very high selectivity for U(VI) over Fe(III) and numerous other cations is described. This new material (designated U/TEVA-2) comprises a novel liquid stationary phase consisting of an equimolar mixture of diamyl amylphosphonate (DA[AP]) and Cyanex 923{sup registered} (a commercially available trialkyl-phosphine oxide, TRPO) sorbed on silanized silica or Amberchrom CG-71. Cyanex 923 is shown to be preferable to a related TRPO, Cyanex 925{sup registered}, due to its lower viscosity and higher selectivity for U(VI) over Fe(III). The retention of uranyl nitrate by the U/TEVA-2 resin, as measured by the k' values (number of free column values to peak maximum) is >5000 from approximately 0.1 to 8 M HNO{sub 3}. The ability of the new resin to strongly and selectively retain U(VI) from such a wide range of acid concentrations, along with its favorable physical properties, make it a good candidate for application in the separation and preconcentration of U(VI) from complex environmental, biological, and nuclear waste samples for subsequent determination.

  4. An improved extraction chromatographic resin for the separation of uranium from acidic nitrate media.

    Science.gov (United States)

    Dietz, M L; Horwitz, E P; Sajdak, L R; Chiarizia, R

    2001-07-01

    The preparation and characterization of a new extraction chromatographic resin exhibiting extraordinarily strong retention of hexavalent uranyl ion over a wide range of nitric acid concentrations and very high selectivity for U(VI) over Fe(III) and numerous other cations is described. This new material (designated U/TEVA-2) comprises a novel liquid stationary phase consisting of an equimolar mixture of diamyl amylphosphonate (DA[AP]) and Cyanex 923((R)) (a commercially available trialkyl-phosphine oxide, TRPO) sorbed on silanized silica or Amberchrom CG-71. Cyanex 923 is shown to be preferable to a related TRPO, Cyanex 925((R)), due to its lower viscosity and higher selectivity for U(VI) over Fe(III). The retention of uranyl nitrate by the U/TEVA-2 resin, as measured by the k' values (number of free column values to peak maximum) is >5000 from approximately 0.1 to 8 M HNO(3). The ability of the new resin to strongly and selectively retain U(VI) from such a wide range of acid concentrations, along with its favorable physical properties, make it a good candidate for application in the separation and preconcentration of U(VI) from complex environmental, biological, and nuclear waste samples for subsequent determination.

  5. High-performance liquid chromatographic assay of free norepinephrine, epinephrine, dopamine, vanillylmandelic acid and homovanillic acid.

    Science.gov (United States)

    Gerlo, E; Malfait, R

    1985-09-13

    A procedure is described for the concurrent assay of free norepinephrine, epinephrine, dopamine, vanillylmandelic acid and homovanillic acid in physiological fluids using high-performance liquid chromatography with electrochemical detection. The column packing is an octadecyl-bonded silica. A single mobile phase containing 1-octanesulphonate is used for the assay of catecholamines and for the assay of the acidic metabolites. An efficient sample preparation scheme is presented for the isolation of the catecholamines and their acidic metabolites from the same sample aliquot. Catecholamines are extracted by ion exchange on small columns and adsorption on alumina, using dihydroxybenzylamine as an internal standard. Vanillylmandelic acid and homovanillic acid are recovered from the combined loading and washing effluents of the ion-exchange column by a solvent extraction procedure. Recovery of catecholamines averages 67%. The limit of detection for individual catecholamines is ca. 30 pg. Recoveries of vanillylmandelic acid and homovanillic acid average 77% and 87%, respectively. The use of the same mobile phase for the concurrent assay of catecholamines and their acidic metabolites considerably increases the throughput of samples in the chromatographic system by eliminating the time-consuming column-equilibration periods.

  6. Changes in the Vibrational Spectra of Zeolites Due to Sorption of Heavy Metal Cations

    Science.gov (United States)

    Król, M.; Mozgawa, W.; Barczyk, K.; Bajda, T.; Kozanecki, M.

    2013-11-01

    This work presents the results of spectroscopic (MIR and Raman) studies of zeolite structures after immobilization of heavy metal cations from aqueous solutions. The sorption of Ag+, Cu2+, Cd2+, Pb2+, Zn2+, and Cr3+ ions has been conducted on zeolites belonging to different structural groups, i.e., sodium forms of natural chabazite, mordenite, ferrierite, and clinoptilolite, as well as on synthetic zeolite Y. Systematic changes in intensities and positions of the bands corresponding to the characteristic ring vibrations have been observed in the measured spectra. The most visible changes are observed in the FT-IR spectra of the samples in the range of 850-450 cm-1, and in the Raman spectra in the range of 600-250 cm-1. Depending on the zeolite structure, the bands, which can be regarded as a kind of indicator of ion exchange, were indentifi ed. For example, in the case of IR spectra, these bands are at 766, 703, 648, 578, and 506 cm-1 for zeolite Y, at 733 and 560 cm-1 for mordenite, at 675 cm-1 for clinoptilolite, etc. The degree of changes depends on both the type of cation and its concentration in the initial solution. This is connected with the way of binding of metal ions to the zeolite aluminosilicate framework, i.e., a proportion of the ion exchange and chemisorption in the process. Cations mainly undergoing ion exchange, such as Cd2+ or Pb2+, have the greatest impact on the character of the spectra. On the other hand, Cr3+ ions practically do not modify the spectra of zeolites. Results of IR and Raman spectroscopic studies have been compared with those obtained by atomic absorption spectroscopy (AAS), from which the proportion of ion exchange to chemisorption in the process and the effective cation exchange capacity of the individual samples have been estimated.

  7. Localization versus delocalization in diamine radical cations

    DEFF Research Database (Denmark)

    Brouwer, A.M.; Wiering, P.G.; Zwier, J.M.;

    1997-01-01

    The optical absorption spectrum of the radical cation of 1,4-diphenylpiperazine 2a shows a strong transition in the near-IR, and only a weak band at 445 nm, in the region where aniline radical cations normally absorb strongly. This indicates that the charge and spin are delocalized over the two...

  8. Ionic liquids as porogens in the microwave-assisted synthesis of methacrylate monoliths for chromatographic application

    Energy Technology Data Exchange (ETDEWEB)

    Singco, Brenda; Lin, Chen-Lan; Cheng, Yi-Jie; Shih, Yung-Han [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China); Huang, Hsi-Ya, E-mail: hyhuang@cycu.edu.tw [Department of Chemistry and Center for Nanotechnology, CYCU (Chung Yuan Christian University), 200 Chung Pei Road, Chung-Li 320, Taiwan (China)

    2012-10-09

    Highlights: Black-Right-Pointing-Pointer An efficient and cleaner monoliths preparation utilizing ionic liquids in conjunction with microwave Black-Right-Pointing-Pointer These ionic liquids with varied cation alkyl chain and anion type successfully tuned the morphology of different alkyl methacrylates Black-Right-Pointing-Pointer Small molecules and peptide digests separated well in these monoliths. - Abstract: Several imidazolium-based ionic liquids (ILs) with varying cation alkyl chain length (C{sub 4}-C{sub 10}) and anion type (tetrafluoroborate ([BF{sub 4}]{sup -}), hexafluorophosphate ([PF{sub 6}]{sup -}) and bis(trifluoromethylsulfonyl)imide ([Tf{sub 2}N]{sup -})) were used as reaction media in the microwave polymerization of methacrylate-based stationary phases. Scanning electron micrographs and backpressures of poly(butyl methacrylate-ethylene dimethacrylate) (poly(BMA-EDMA)) monoliths synthesized in the presence of these ionic liquids demonstrated that porosity and permeability decreased when cation alkyl chain length and anion hydrophobicity were increased. Performance of these monoliths was assessed for their ability to separate parabens by capillary electrochromatography (CEC). Intra-batch precision (n = 3 columns) for retention time and peak area ranged was 0.80-1.13% and 3.71-4.58%, respectively. In addition, a good repeatability of RSD{sub Retentiontime} = <0.30% and {approx}1.0%, RSD{sub Peakarea} = <1.30% and <4.3%, and RSD{sub Efficiency} = <0.6% and <11.5% for intra-day and inter-day, respectively exemplify monolith performance reliability for poly(BMA-EDMA) fabricated using 1-hexyl-3-methylimidazolium tetrafluoroborate ([C{sub 6}mim][BF{sub 4}]) porogen. This monolith was also tested for its potential in nanoLC to separate protein digests in gradient mode. ILs as porogens also fabricated different alkyl methacrylate (AMA) (C4-C18) monoliths. Furthermore, employing binary IL porogen mixture such as 1-butyl-3-methylimidazolium tetrafluoroborate

  9. INTERACTION OF AMINO ACID WITH ION EXCHANGE RESIN Ⅲ.FURTHER INVESTIGA TION OF SUPEREQUIVALENT ADSORPTION MECHANISM OF AMINO ACID ON ION EXCHANGE RESIN

    Institute of Scientific and Technical Information of China (English)

    ZHANGHui; SHAOTong; 等

    1994-01-01

    The adsorption isotherms of glycine,alanine and oxidized glutathion on strong acid cation and strong base anion exchange resins from aqueous solutions were measured and the superequivalent adsorptions of glycine and alanine observed.The infrared spectra of glycine adsorbed on the cation and the anion exchange resins,001×7 and 201×7,were measured.From these results,it is concluded that the amino acid adsorption on the ion exchange resin proceeds not only through ion exchange and proton transfer mechanisms,but also through aminecarboxylate interaction between the adsorbed amino acid molecules,and the formation of second layer of amino acid molecules is the mechanism of superequivalent adsorption of amino acid,the carboxylate or amine groups of the first layer of amino acid molecules on the ion exchange resin act as the exchange sites for the second layer of amino acid molecules.

  10. Segmented heat exchanger

    Science.gov (United States)

    Baldwin, Darryl Dean; Willi, Martin Leo; Fiveland, Scott Byron; Timmons, Kristine Ann

    2010-12-14

    A segmented heat exchanger system for transferring heat energy from an exhaust fluid to a working fluid. The heat exchanger system may include a first heat exchanger for receiving incoming working fluid and the exhaust fluid. The working fluid and exhaust fluid may travel through at least a portion of the first heat exchanger in a parallel flow configuration. In addition, the heat exchanger system may include a second heat exchanger for receiving working fluid from the first heat exchanger and exhaust fluid from a third heat exchanger. The working fluid and exhaust fluid may travel through at least a portion of the second heat exchanger in a counter flow configuration. Furthermore, the heat exchanger system may include a third heat exchanger for receiving working fluid from the second heat exchanger and exhaust fluid from the first heat exchanger. The working fluid and exhaust fluid may travel through at least a portion of the third heat exchanger in a parallel flow configuration.

  11. A study on cations and color removal from thin sugar juice by modified sugar beet pulp.

    Science.gov (United States)

    Arslanoglu, Hasan; Tumen, Fikret

    2012-06-01

    This article describes the use of citric acid modified sugar beet pulp as new ion-exchanger sorbent for the removal of metal cations and colorants from thin juice. The results of batch adsorption runs concerning the effects of contact time, material dosage, temperature and pH drop were presented and discussed. Experimental data on the removal of metal cations showed that the sorption process was rapid and reached equilibrium in 60 min. Modified material in acidic form caused to a significant pH drop in thin juice, which could result with sucrose inversion. Uptake of metal cations increased with temperature whereas that of color decreased. Neutralised type modified product gave more satisfying results. After six successive contacts, 49.7%, 37.5% and 43.7% removals for Ca-Mg, K and color, respectively, were obtained by using neutralised form of modified sugar beet pulp.

  12. Cationic Bolaamphiphiles for Gene Delivery

    Science.gov (United States)

    Tan, Amelia Li Min; Lim, Alisa Xue Ling; Zhu, Yiting; Yang, Yi Yan; Khan, Majad

    2014-05-01

    Advances in medical research have shed light on the genetic cause of many human diseases. Gene therapy is a promising approach which can be used to deliver therapeutic genes to treat genetic diseases at its most fundamental level. In general, nonviral vectors are preferred due to reduced risk of immune response, but they are also commonly associated with low transfection efficiency and high cytotoxicity. In contrast to viral vectors, nonviral vectors do not have a natural mechanism to overcome extra- and intracellular barriers when delivering the therapeutic gene into cell. Hence, its design has been increasingly complex to meet challenges faced in targeting of, penetration of and expression in a specific host cell in achieving more satisfactory transfection efficiency. Flexibility in design of the vector is desirable, to enable a careful and controlled manipulation of its properties and functions. This can be met by the use of bolaamphiphile, a special class of lipid. Unlike conventional lipids, bolaamphiphiles can form asymmetric complexes with the therapeutic gene. The advantage of having an asymmetric complex lies in the different purposes served by the interior and exterior of the complex. More effective gene encapsulation within the interior of the complex can be achieved without triggering greater aggregation of serum proteins with the exterior, potentially overcoming one of the great hurdles faced by conventional single-head cationic lipids. In this review, we will look into the physiochemical considerations as well as the biological aspects of a bolaamphiphile-based gene delivery system.

  13. TLC chromatographic-densitometric assay of ibuprofen and its impurities.

    Science.gov (United States)

    Starek, Małgorzata; Krzek, Jan

    2010-11-01

    A simple and sensitive thin-layer chromatographic (TLC)-densitometric method for the quantitative estimation of S(+)-2-[4-isobutylphenyl]propionic acid (ibuprofen) and its impurities in pharmaceutical preparations has been developed. The chromatographic separation was carried out on silica gel 60 F(254) TLC plates using toluene-ethyl acetate-glacial acetic acid (17:13: 1, v/v/v) as the mobile phase. Detection was carried out densitometrically with a UV detector. The developed method has detection and quantitation limits ranging from 0.13 μg per spot to 0.72 μg per spot. For individual constituents the recovery ranged from 96.8% to 99.0%. In addition, the stability of ibuprofen solutions was investigated, including the effect of pH, temperature, and incubation time. The method is rapid, simple, and suitable for routine quality-control analysis of pharmaceuticals containing ibuprofen.

  14. EVALUATING ION EXCHANGE FOR REMOVING RADIUM FROM GROUNDWATER

    Science.gov (United States)

    This article, the second in a series, focuses on the results of bench- and pilot-scale studies of ion exchange processes for radium removal from groundwater in Lemont, Ill. Batch and column studies indicated a very high resin selectivity for radium compared with common cations. E...

  15. Protein phylogenetic analysis of Ca2+/cation antiporters and insights into their evolution in plants

    Directory of Open Access Journals (Sweden)

    Laura eEmery

    2012-01-01

    Full Text Available Cation transport is a critical process in all organisms and is essential for mineral nutrition, ion stress tolerance, and signal transduction. Transpo