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Sample records for anion exchange chromatography

  1. Test procedure for anion exchange chromatography

    International Nuclear Information System (INIS)

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

  2. Anion-exchange chromatography of phosphopeptides: weak anion exchange versus strong anion exchange and anion-exchange chromatography versus electrostatic repulsion-hydrophilic interaction chromatography.

    Science.gov (United States)

    Alpert, Andrew J; Hudecz, Otto; Mechtler, Karl

    2015-01-01

    Most phosphoproteomics experiments rely on prefractionation of tryptic digests before online liquid chromatography-mass spectrometry. This study compares the potential and limitations of electrostatic repulsion-hydrophilic interaction chromatography (ERLIC) and anion-exchange chromatography (AEX). At a pH higher than 5, phosphopeptides have two negative charges per residue and are well-retained in AEX. However, peptides with one or two phosphate groups are not separated from peptides with multiple Asp or Glu residues, interfering with the identification of phosphopeptides. At a pH of 2, phosphate residues have just a single negative charge but Asp and Glu are uncharged. This facilitates the separation of phosphopeptides from unmodified acidic peptides. Singly phosphorylated peptides are retained weakly under these conditions, due to electrostatic repulsion, unless hydrophilic interaction is superimposed in the ERLIC mode. Weak anion-exchange (WAX) and strong anion-exchange (SAX) columns were compared, with both peptide standards and a HeLa cell tryptic digest. The SAX column exhibited greater retention at pH 6 than did the WAX column. However, only about 60% as many phosphopeptides were identified with SAX at pH 6 than via ERLIC at pH 2. In one ERLIC run, 12 467 phosphopeptides were identified, including 4233 with more than one phosphate. We conclude that chromatography of phosphopeptides is best performed at low pH in the ERLIC mode. Under those conditions, the performances of the SAX and WAX materials were comparable. The data have been deposited with the ProteomeXchange with identifier PXD001333. PMID:25827581

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

    DEFF Research Database (Denmark)

    Andersen, Rikke; Sørensen, A.

    2000-01-01

    Carbohydrates such as alditols (polyols or sugar alcohols), monosaccharides and disaccharides are separated as anions by anion-exchange chromatography with a sodium hydroxide eluent, MA1 CarboPac column and pulsed amperometric detection. We report a high-pH anion-exchange chromatographic...

  4. 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.

  5. Anion exchangers with branched functional ion exchange layers of different hydrophilicity for ion chromatography.

    Science.gov (United States)

    Shchukina, O I; Zatirakha, A V; Smolenkov, A D; Nesterenko, P N; Shpigun, O A

    2015-08-21

    Novel polystyrene-divinylbenzene (PS-DVB) based anion exchangers differing from each other in the structure of the branched functional ion exchange layer are prepared to investigate the role of linker and functional site on ion exchange selectivity. The proposed method of synthesis includes the obtaining of aminated PS-DVB particles by means of their acylation with following reductive amination with methylamine. Further modification of the obtained secondary aminogroups is provided by the alkylation with either 1,4-butanediol diglycidyl ether (1,4-BDDGE) or resorcinol diglycidyl ether (RDGE), which form the linkers of different hydrophobicity, and amination of terminal epoxide rings with trimethylamine (TMA), dimethylethanolamine (DMEA), methyldiethanolamine (MDEA) or triethanolamine (TEA). The variation of the structure and hydrophobicity of the linker and terminal quaternary ammonium sites in the functional layer allows the alteration of selectivity and separation efficiency of the obtained adsorbents. The ion exchange selectivity and separation efficiency of the anion exchangers are evaluated using the model mixtures of anions (F(-), HCOO(-), Cl(-), NO2(-), Br(-), NO3(-), HPO4(2-) and SO4(2-)) in potassium hydroxide eluents. The adsorbents show the decrease of selectivity with increasing the hydrophilicity of the terminal functional site. The anion exchangers having more flexible and hydrophilic 1,4-BDDGE linker provide smaller separation factors for most of the analytes as compared with RDGE-containing adsorbents with the same terminal ion exchange sites, but are characterized with higher column efficiencies and better peak symmetry for polarizable anions. In case of 1,4-BDDGE-modified anion exchangers of the particle size of 3.3μm functionalized with DMEA and MDEA the calculated values of column efficiencies for polarizable NO3(-) and Br(-) are up to 49,000 and 53,000N/m, respectively, which is almost twice higher than the values obtained for the RDGE

  6. Rapid detection of malto-oligosaccharide-forming bacterial amylases by high performance anion-exchange chromatography

    DEFF Research Database (Denmark)

    Duedahl-Olesen, Lene; Larsen, K. L.; Zimmermann, W.

    2000-01-01

    High performance anion-exchange chromatography with pulsed amperometric detection was applied for the rapid analysis of malto-oligosaccharides formed by extracellular enzyme preparations from 49 starch-degrading bacterial strains isolated from soil and compost samples. Malto-oligosaccharide-formi......-oligosaccharide-forming amylases, indicated by a predominant formation of maltohexaose from starch, were produced by enzyme preparations from four of the isolates growing at pH 7.0 and 10....

  7. Determination of petroleum sulfonates in crude oil by column-switching anion-exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    Liang Zhao; Xu Long Cao; Hong Yan Wang; Xia Liu; Sheng Xiang Jiang

    2008-01-01

    A column-switching anion-exchange chromatography method was described for the separation and determination of petroleum monosulfonates (PMS)and petroleum disulfonates (PDS)in crude oil that was simply diluted with the dichloromethane/methanol (60140).The high performance liquid chromatography (HPLC)system consisted of a clean-up column and an analytical column,which were connected with two six-port switching valves.Detection of petroleum sulfonates was available and repeatable.This method has been successfully applied to determine PMS and PDS in crude oil samples from Shengli oil field.

  8. Copper modified platinum electrode for amperometric detection of spectinomycin sulfate by anion-exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    Ling Ling Xi; Pei Min Zhang; Yan Zhu

    2009-01-01

    A La~(3+)-Cu/Pt modified electrode was fabricated by electrodepositing process in CuSO_4 solution by adding a small amount of lanthium compound, and it was employed for direct current (DC) amperometric detection of spectinomycin by anion-exchange chromatography. Without derivatization, this method can simultaneously determine the main component and impurities in spectinomycin pharmaceutical raw material. Ease of preparation, being applied in DC detection mode and good catalytic stability confirmed the interests of this modified electrode as amperometric sensor for the determination of spectinomycin.

  9. Simultaneous determination of NH4+, NO2- and NO3- by ion-exclusion/anion-exchange chromatography on a strongly basic anion-exchange resin with basic eluent%Simultaneous determination of NH4+,NO2- and NO3- by ion-exclusion/anion-exchange chromatography on a strongly basic anion-exchange resin with basic eluent

    Institute of Scientific and Technical Information of China (English)

    Masanobu MORI; Takahiro HIRONAGA; Hideyuki ITABASHI; Nobutake NAKATANI; Daisuke KOZAKI; Kazuhiko TANAKA

    2012-01-01

    Ion-exclusion/anion-exchange chromatography (IEC/AEC) on a combination of a strongly basic anion-exchange resin in the OH--form with basic eluent has been developed.The separation mechanism is based on the ion-exclusion/penetration effect for cations and the anion-exchange effect for anions to anion-exchange resin phase.This system is useful for simultaneous separation and determination of ammonium ion ( NH4+ ),nitrite ion (NO2-),and nitrate ion (NO3-) in water samples.The resolution of analyte ions can be manipulated by changing the concentration of base in eluent on a polystyrene-divinylbenzene based strongly basic anion-exchange resin column.In this study,several separation columns,which consisted of different particle sizes,different functional groups and different anion-exchange capacities,were compared.As the results,the separation column with the smaller anion-exchange capacity (TSKgel Super IC-Anion) showed well-resolved separation of cations and anions,In the optimization of the basic eluent,lithium hydroxide (LiOH) was used as the eluent and the optimal concentration was concluded to be 2 mmol/L,considering the resolution of analyte ions and the whole retention times.In the optimal conditions,the relative standard deviations of the peak areas and the retention times of NH4+,NO2-,and NO3- ranged 1.28% - 3.57% and 0.54% - 1.55%,respectively.The limits of detection at signal-to-noise of 3 were 4.10 μmol/L for NH4+,1.87 μmol/L for NO2- and 2.83 μmol/L for NO3-.

  10. Enhancement of anion-exchange chromatography of DNA using compaction agents

    Science.gov (United States)

    Murphy, Jason C.; Fox, George E.; Willson, Richard C.

    2003-01-01

    The use of adsorptive chromatography for preparative nucleic acid separations is often limited by low capacity. The possibility that the adsorbent surface area sterically accessible to nucleic acid molecules could be increased by reducing their radius of gyration with compaction agents has been investigated. The equilibrium adsorption capacity of Q Sepharose anion-exchange matrix for plasmid DNA at 600 mM NaCl was enhanced by up to ca. 40% in the presence of 2.5 mM spermine. In addition, compaction agent selectivity has been demonstrated. Spermine, for example, enhances the adsorption of both plasmid and genomic DNA, spermidine enhances binding only of plasmid, and hexamine cobalt enhances only the binding of genomic DNA. Compaction may be generally useful for enhancing adsorptive separations of nucleic acids.

  11. Nanostructured cupric oxide electrode: An alternative to amperometric detection of carbohydrates in anion-exchange chromatography.

    Science.gov (United States)

    Barragan, José T C; Kubota, Lauro T

    2016-02-01

    In this paper, a new and low cost copper/cupric oxide nanostructured electrode is presented as an alternative to the amperometric detection of carbohydrates in high-performance anion exchange chromatography. The modified copper electrodes were prepared by a simple and fast method which resulted in the obtainment of homogeneously distributed nanostructures adhered to the surface with controlled chemical nature. The results, when compared to conventional copper electrodes, exhibited considerable improvements in analytical results, including: 1) Better repeatability in consecutive glucose detections, in which the percent relative standard deviation improved from 15.1% to 0.279%. 2) Significant improvements in the stability of the baseline and a decrease of the stabilization time, going from several hours to approximately 15 min. 3) Considerable increase in the sensitivity towards glucose, from 5.02 nA min mg L(-1) to 25.5 nA min mg L(-1). 4) Improvements in the detectability with limits as low as 1.09 pmol. 5) Wide working range of concentrations (1 × 10(-2) to 1 × 10(4) mg L(-1)). 6) Good linearity with correlation coefficients greater than 0.998. 7) Possibility of detecting different molecules of carbohydrates (lactose, maltose, sucrose cellobiose, sorbitol, fructose, glucose, galactose, manose, arabitol, xylose, ribose and arabnose). In comparison to the electrode that is more employed for this type of application (gold electrode), the low cost, the possibility of detection at constant potential and the equivalent detection limits presented by the new electrode material introduced in this work emerge as characteristics that make this material a powerful alternative considering the detection of carbohydrates in anion exchange chromatography.

  12. Anion-exchange high-performance liquid chromatography with conductivity detection for the analysis of phytic acid in food

    OpenAIRE

    Talamond, Pascale; Doulbeau, Sylvie; Rochette, Isabelle; Guyot, Jean-Pierre; Trèche, Serge

    1999-01-01

    A sensitive method for the accurate determination of phytic acid in food samples is described. The proposed procedure involves the anion-exchange liquid chromatography with conductivity detection. Initially, two methods of determination of phytic acid were compared : absorptiometry and high-performance ion chromatography (HPIC) with chemically suppressed conductivity detector. Unlike most conventional methods involving precipitation by FeCl3, the simpler and more reliable HPIC assay avoids th...

  13. Development of a modular virus clearance package for anion exchange chromatography operated in weak partitioning mode.

    Science.gov (United States)

    Iskra, Timothy; Sacramo, Ashley; Gallo, Chris; Godavarti, Ranga; Chen, Shuang; Lute, Scott; Brorson, Kurt

    2015-01-01

    Anion exchange chromatography (AEX) operated under weak partitioning mode has been proven to be a powerful polishing step as well as a robust viral clearance step in Pfizer's monoclonal antibody (mAb) platform purification process. A multivariate design of experiment (DoE) study was conducted to understand the impact of operating parameters and feedstream impurity levels on viral clearance by weak partitioning mode AEX. Bacteriophage was used initially as a surrogate for neutral and acidic isoelectric point mammalian viruses (e.g., retrovirus and parvovirus). Five different mAbs were used in the evaluation of process parameters such as load challenge (both product and impurities), load pH, load conductivity, and contact time (bed height and flow-rate). The operating ranges obtained from phage clearance studies and Pfizer's historical data were used to define an appropriate operating range for a subsequent clearance study with model retrovirus and parvovirus. Both phage and virus clearance evaluations included feedstreams containing different levels of impurities such as high molecular mass species (HMMS), host cell proteins (HCPs), and host cell DNA. For all the conditions tested, over 5 log10 of clearance for both retrovirus and parvovirus was achieved. The results demonstrated that weak partitioning mode AEX chromatography is a robust step for viral clearance and has the potential to be included as part of the modular viral clearance approach.

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

    Science.gov (United States)

    Arfelli, Giuseppe; Sartini, Elisa

    2014-01-01

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

  15. Anion exchange SPE and liquid chromatography-tandem mass spectrometry in GHB analysis.

    Science.gov (United States)

    Elian, Albert A; Hackett, Jeffery

    2011-12-01

    In this study, the extraction of γ-hydroxybutyrate (GHB) from urine using solid-phase extraction (SPE) is described. SPE was performed on anion exchange columns after samples of urine had been diluted with de-ionized water. After application of the diluted samples containing GHB-d(6) as an internal standard, the sorbent was washed with deionized water and methanol and dried. The GHB was eluted from the SPE column with a solvent consisting of methanol containing 6% glacial acetic acid. The eluent was collected, evaporated to dryness, and dissolved in mobile phase (100 μL) for analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative multiple reaction monitoring (MRM) mode. Liquid chromatography was performed in gradient mode employing a biphenyl column and a mobile phase consisting of acetontitrile (containing 0.1% formic acid) and 0.1% aqueous formic acid. The total run time for each analysis was less than 5 min. The limits of detection/quantification for this method were determined to be 50 and 100 ng/mL, respectively. The method was found to be linear from 500 ng/mL to 10,000 ng/mL (r(2)>0.995). The recovery of GHB was found to be greater than 75%. In this report, results of authentic urine samples analyzed for GHB by this method are presented. GHB concentrations in these samples were found to be range from less than 500 ng/mL to 5110 ng/mL.

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

    DEFF Research Database (Denmark)

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

    1998-01-01

    A cleanup method based on anion-exchange solid-phase extraction (SPE) was developed to render biological extracts suitable for the analysis of hexose phosphates with a modified anion-exchange chromatography method and pulsed amperometric detection. The method was applied to cell extracts of Sacch...

  17. 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.

  18. Wheat gluten amino acid analysis by high-performance anion-exchange chromatography with integrated pulsed amperometric detection.

    Science.gov (United States)

    Rombouts, Ine; Lagrain, Bert; Lamberts, Lieve; Celus, Inge; Brijs, Kristof; Delcour, Jan A

    2012-01-01

    This chapter describes an accurate and user-friendly method for determining amino acid composition of wheat gluten proteins and their gliadin and glutenin fractions. The method consists of hydrolysis of the peptide bonds in 6.0 M hydrochloric acid solution at 110°C for 24 h, followed by evaporation of the acid and separation of the free amino acids by high-performance anion-exchange chromatography with integrated pulsed amperometric detection. In contrast to conventional methods, the analysis requires neither pre- or postcolumn derivatization, nor a time-consuming oxidation or derivatization step prior to hydrolysis. Correction factors account for incomplete release of Val and Ile even after hydrolysis for 24 h, and for losses of Ser during evaporation. Gradient conditions including an extra eluent allow multiple sequential sample analyses without risk of Glu accumulation on the anion-exchange column which otherwise would result from high Gln levels in gluten proteins. PMID:22125156

  19. Comparison of displacement versus gradient mode for separation of a complex protein mixture by anion-exchange chromatography.

    Science.gov (United States)

    Ahrends, Robert; Lichtner, Björn; Buck, Friedrich; Hildebrand, Diana; Kotasinska, Marta; Kohlbacher, Oliver; Kwiatkowski, Marcel; Wagner, Moritz; Trusch, Maria; Schlüter, Hartmut

    2012-07-15

    Liquid chromatography is often the method of choice for the analysis of proteins in their native state. Nevertheless compared to two-dimensional electrophoresis, the resolution of common chromatographic techniques is low. Liquid chromatography in the displacement mode has previously been shown to offer higher resolution and to elute proteins in the high concentrations. In this study we compared to what extend displacement mode was a suitable alternative to gradient mode for the separation of a complex protein mixture using anion-exchange displacement chromatography and if it is therefore helpful for proteomic investigations. Hence we analyzed the qualitative protein composition of each fraction by tryptic digestion of the proteins, analysis of the tryptic peptides by liquid chromatography coupled to mass spectrometry followed by data base analysis and by measuring the elution profiles of 22 selected proteins with selected reaction monitoring mass spectrometry. In the fractions of displacement mode a significantly higher number of identified proteins (51 versus 16) was yielded in comparison to gradient mode. The resolution of displacement chromatography was slightly lower than of gradient chromatography for many but not for all proteins. The selectivities of displacement mode and gradient mode are very different. In conclusion displacement chromatography is a well suited alternative for top-down proteomic approaches which start with separating intact proteins first prior to mass spectrometric analysis of intact or digested proteins. The significant orthogonality of both modes may be used in the future for combining them in multidimensional fractionation procedures. PMID:22727752

  20. Refolding with Simultaneous Purification of Recombinant Human Granulocyte Colony-stimulating Factor from Escherichia coli Using Strong Anion Exchange Chromatography

    Institute of Scientific and Technical Information of China (English)

    Chao Zhan WANG; Jiang Feng LIU; Xin Du GENG

    2005-01-01

    The urea denatured recombinant human granulocyte colony-stimulating factor (rhGCSF) which was expressed in Escheriachia coli (E. coli) was refolded with simultaneous purification by strong anion exchange chromatography (SAX) in the presence of low concentration of urea. The effect of urea concentration on this refolding process was investigated. The obtained refolded rhG-CSF has a high specific activity of 2.3×108 U/mg, demonstrating that the proteins were completely refolded during the chromatographic process. With only one step by SAX in 40 min, purity and mass recovery of the refolded and purified rhG-CSF were 97% and43%, respectively.

  1. High performance ion chromatography of haloacetic acids on macrocyclic cryptand anion exchanger.

    Science.gov (United States)

    Bruzzoniti, Maria Concetta; De Carlo, Rosa Maria; Horvath, Krisztian; Perrachon, Daniela; Prelle, Ambra; Tófalvi, Renáta; Sarzanini, Corrado; Hajós, Péter

    2008-04-11

    A new high performance ion chromatographic method has been developed for the separation of the nine chlorinated-brominated haloacetic acids (HAAs) that are the disinfection by-products of chlorination of drinking water, using a macrocycle-based adjustable-capacity anion-exchange separator column (IonPac Cryptand A1). A gradient method based on theoretical and experimental considerations has been optimized in which 10 mM NaOH-LiOH step gradient was performed at the third minute of the analysis. The optimized method allowed us to separate the nine HAAs and seven possibly interfering inorganic anions in less than 25 min with acceptable resolution. The minimum concentrations detectable for HAAs were between 8.0 (MBA) and 210 (TBA) microg L(-1), with linearity included between 0.9947 (TBA) and 0.9998 (MBA). To increase sensitivity, a 25-fold preconcentration step on a reversed phase substrate (LiChrolut EN) has been coupled. Application of this method to the analysis of haloacetic acids in real tap water samples is illustrated.

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

    Science.gov (United States)

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

    2014-09-01

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

  3. Improvement of sugar analysis sensitivity using anion-exchange chromatography-electrospray ionization mass spectrometry with sheath liquid interface.

    Science.gov (United States)

    Xu, Xian-Bing; Liu, Ding-Bo; Guo, Xiao Ming; Yu, Shu-Juan; Yu, Pei

    2014-10-31

    A novel interface that enables high-performance anion-exchange chromatography (HPAEC) to be coupled with electrospray ionization (ESI) mass spectrometry (MS) is reported. A sheath liquid consisting of 50mM NH4Ac in isopropanol with 0.05% acetic acid, infused at a flow rate of 3μL/min at the tip of the electrospray probe, requires less ESI source cleaning and promotes efficient ionization of mono- and di-carbohydrates. The results suggest that use of a sheath liquid interface rather than a T-joint allows volatile ammonium salts to replace non-volatile metal salts as modifiers for improving sugar ESI signals. The efficient ionization of mono- and di-carbohydrates in the ESI source is affected by the sheath liquid properties such as buffer concentration and type of organic solvent. HPAEC-ESI-MS was used for the analysis of monocarbohydrates in pectins, particularly co-eluted sugars, and the performance was evaluated. Addition of a make-up solution through the sheath liquid interface proved to be an efficient tool for enhancing the intensities of sugars analyzed using HPAEC-ESI-MS.

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

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Otero, Natalia; Bermejo-Barrera, Pilar [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela (Spain); Moreda-Pineiro, Antonio, E-mail: antonio.moreda@usc.es [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela (Spain)

    2013-01-14

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

  5. The development of sequential separation methods for the analysis of actinides in sediments and biological materials using anion-exchange resins and extraction chromatography

    International Nuclear Information System (INIS)

    New, quantitative methods for the determination of actinides have been developed for application to marine environmental samples (e.g., sediment and fish). The procedures include aggressive dissolution, separation by anion-exchange resin, separation and purification by extraction chromatography (e.g., TRU, TEVA and UTEVA resins) with measurement of the radionuclides by semiconductor alpha-spectrometry (SAS). Anion-exchange has proved to be a strong tool to treat large volume samples, and extraction chromatography shows an excellent selectivity and reduction of the amounts of acids. The results of the analysis of uranium, thorium, plutonium and americium isotopes by this method in marine samples (IAEA-384, -385 and -414) provided excellent agreement with the recommended values with good chemical recoveries. (author)

  6. Dextrin characterization by high-performance anion-exchange chromatography--pulsed amperometric detection and size-exclusion chromatography--multi-angle light scattering--refractive index detection.

    Science.gov (United States)

    White, D Richard; Hudson, Patricia; Adamson, Julie T

    2003-05-16

    Starch hydrolysis products, or dextrins, are widely used throughout the food industry for their functional properties. Dextrins are saccharide polymers linked primarily by alpha-(1 --> 4) D-glucose units and are prepared by partial hydrolysis of starch. Hydrolysis can be accomplished by the use of acid, enzymes, or by a combination of both. The hydrolysis products are typically characterized by the "dextrose equivalent" (DE), which refers to the total reducing power of all sugars present relative to glucose. While the DE gives the supplier and buyer a rough guide to the bulk properties of the material, the physiochemical properties of dextrins are dependent on the overall oligosaccharide profile. High-performance anion-exchange chromatography (HPAEC) with pulsed amperometric detection and size-exclusion chromatography (SEC) with multi-angle light-scattering and refractive index detection were used to characterize dextrins from commercial sources. HPAEC was used to acquire the oligosaccharide profile, and SEC to obtain an overall molar mass distribution. These methods in combination extended our understanding of the relationship between oligosaccharide profile, DE, and the hydrolysis process. Data from the two techniques enabled a method for estimating the DE that gave results in reasonable agreement with the accepted titration method. PMID:12830879

  7. Determination of Amino Acids in Cell Culture and Fermentation Broth Media Using Anion-Exchange Chromatography with Integrated Pulsed Amperometric Detection

    OpenAIRE

    Hanko, Valoran P.; Heckenberg, Andrea; Rohrer, Jeffrey S.

    2004-01-01

    Anion-exchange chromatography with integrated pulsed amperometric detection (AE-IPAD) separates and directly detects amino acids, carbohydrates, alditols, and glycols in the same injection without pre- or post-column derivatization. These separations use a combination of NaOH and NaOH/sodium acetate eluents. We previously published the successful use of this technique, also known as AAA-Direct, to determine free amino acids in cell culture and fermentation broth media. We showed that retentio...

  8. Survey of inorganic arsenic in marine animals and marine certified reference materials by anion exchange high-performance liquid chromatography-inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

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

    2005-01-01

    A method for the determination of inorganic arsenic in seafood samples using high-performance liquid chromatography-inductively coupled plasma mass spectrometry is described. The principle of the method relied on microwave-assisted alkaline dissolution of the sample, which at the same time oxidized...... arsenite [As(Ill)] to arsenate [As(V)], whereby inorganic arsenic could be determined as the single species As(V). Anion exchange chromatography using isocratic elution with aqueous ammonium carbonate as the mobile phase was used for the separation of As(V) from other coextracted organoarsenic compounds...

  9. Assessing gibberellins oxidase activity by anion exchange/hydrophobic polymer monolithic capillary liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Chen, Ming-Luan; Su, Xin; Xiong, Wei; Liu, Jiu-Feng; Wu, Yan; Feng, Yu-Qi; Yuan, Bi-Feng

    2013-01-01

    Bioactive gibberellins (GAs) play a key regulatory role in plant growth and development. In the biosynthesis of GAs, GA3-oxidase catalyzes the final step to produce bioactive GAs. Thus, the evaluation of GA3-oxidase activity is critical for elucidating the regulation mechanism of plant growth controlled by GAs. However, assessing catalytic activity of endogenous GA3-oxidase remains challenging. In the current study, we developed a capillary liquid chromatography--mass spectrometry (cLC-MS) method for the sensitive assay of in-vitro recombinant or endogenous GA3-oxidase by analyzing the catalytic substrates and products of GA3-oxidase (GA1, GA4, GA9, GA20). An anion exchange/hydrophobic poly([2-(methacryloyloxy)ethyl]trimethylammonium-co-divinylbenzene-co-ethylene glycol dimethacrylate)(META-co-DVB-co-EDMA) monolithic column was successfully prepared for the separation of all target GAs. The limits of detection (LODs, Signal/Noise = 3) of GAs were in the range of 0.62-0.90 fmol. We determined the kinetic parameters (K m) of recombinant GA3-oxidase in Escherichia coli (E. coli) cell lysates, which is consistent with previous reports. Furthermore, by using isotope labeled substrates, we successfully evaluated the activity of endogenous GA3-oxidase that converts GA9 to GA4 in four types of plant samples, which is, to the best of our knowledge, the first report for the quantification of the activity of endogenous GA3-oxidase in plant. Taken together, the method developed here provides a good solution for the evaluation of endogenous GA3-oxidase activity in plant, which may promote the in-depth study of the growth regulation mechanism governed by GAs in plant physiology. PMID:23922762

  10. Assessing gibberellins oxidase activity by anion exchange/hydrophobic polymer monolithic capillary liquid chromatography-mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Ming-Luan Chen

    Full Text Available Bioactive gibberellins (GAs play a key regulatory role in plant growth and development. In the biosynthesis of GAs, GA3-oxidase catalyzes the final step to produce bioactive GAs. Thus, the evaluation of GA3-oxidase activity is critical for elucidating the regulation mechanism of plant growth controlled by GAs. However, assessing catalytic activity of endogenous GA3-oxidase remains challenging. In the current study, we developed a capillary liquid chromatography--mass spectrometry (cLC-MS method for the sensitive assay of in-vitro recombinant or endogenous GA3-oxidase by analyzing the catalytic substrates and products of GA3-oxidase (GA1, GA4, GA9, GA20. An anion exchange/hydrophobic poly([2-(methacryloyloxyethyl]trimethylammonium-co-divinylbenzene-co-ethylene glycol dimethacrylate(META-co-DVB-co-EDMA monolithic column was successfully prepared for the separation of all target GAs. The limits of detection (LODs, Signal/Noise = 3 of GAs were in the range of 0.62-0.90 fmol. We determined the kinetic parameters (K m of recombinant GA3-oxidase in Escherichia coli (E. coli cell lysates, which is consistent with previous reports. Furthermore, by using isotope labeled substrates, we successfully evaluated the activity of endogenous GA3-oxidase that converts GA9 to GA4 in four types of plant samples, which is, to the best of our knowledge, the first report for the quantification of the activity of endogenous GA3-oxidase in plant. Taken together, the method developed here provides a good solution for the evaluation of endogenous GA3-oxidase activity in plant, which may promote the in-depth study of the growth regulation mechanism governed by GAs in plant physiology.

  11. [Determination of fructooligosaccharides in milk powder using high performance anion-exchange chromatography coupled with pulsed amperometric detection].

    Science.gov (United States)

    Geng, Lijuan; Huang, Junrong; Feng, Feng; Jiang, Pingping; Chu, Xiaogang; Zhang, Feng; Ling, Yun

    2014-12-01

    Fructooligosaccharides (FOS) are usually added in milk powder as a kind of prebiotic. Thus, quantitative analysis of the FOS is very important for the quality control of milk powder. In this study, a simple method for the simultaneous determination of three FOS components with degrees of polymerization (DP) 3-5 in milk powder was developed by high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The samples were extracted with 50% (v/v) ethanol aqueous solution and defatted by an On Guard RP pretreatment column. The separation was performed on a CarboPac PA200 column by gradient elution using deionized water, 0. 2 mol/L NaOH solution and 0. 4 mol/L NaAc solution as the mobile phases. The flow rate was 0. 4 mL/min. The column temperature was 30 °C; and the injection volume was 25 µL. Good linear response was observed in the concentration range of 0.05-10 mg/L (r2 >0. 9993). The limits of quantification were 0. 02, 0. 005 and 0. 02 mg/L for 1-kestose, nystose and fructofuranosyl-nystose, respectively. The mean recoveries varied from 86. 0% to 114. 0% at three spiked levels of 0. 5, 1. 0 and 5. 0 mg/L. The short-chain fructooligosaccharides from inulooligosaccharides (IOS) were successfully separated by the developed HPAEC-PAD method. The method is simple, accurate, sensitive, and helpful for the quality control of milk powder. PMID:25902647

  12. Strong anion-exchange fast performance liquid chromatography as a versatile tool for preparation and purification of RNA produced by in vitro transcription.

    Science.gov (United States)

    Koubek, Jiri; Lin, Ku Feng; Chen, Yet Ran; Cheng, Richard Ping; Huang, Joseph Jen Tse

    2013-10-01

    Here we demonstrate the use of strong anion-exchange fast performance liquid chromatography (FPLC) as a simple, fast, and robust method for RNA production by in vitro transcription. With this technique, we have purified different transcription templates from unreacted reagents in large quantities. The same buffer system could be used to readily remove nuclease contamination from the overexpressed pyrophosphatase, the important reagent for in vitro transcription. In addition, the method can be used to monitor in vitro transcription reactions to enable facile optimization of reaction conditions, and we have compared the separation performance between strong and weak anion-exchange FPLC for various transcribed RNAs, including the Diels-Alder ribozyme, the hammerhead ribozyme tRNA, and 4.5S RNA. The functionality of the purified tRNA(Cys) has been confirmed by the aminoacylation assay. Only the purification by strong anion-exchange FPLC has led to the enrichment of the functional tRNA from run-off transcripts as revealed by both enzymatic and electrophoretic analysis. PMID:23929938

  13. 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.

  14. Pu Anion Exchange Process Intensification

    Energy Technology Data Exchange (ETDEWEB)

    Taylor-Pashow, K. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2015-10-08

    This project seeks to improve the efficiency of the plutonium anion-exchange process for purifying Pu through the development of alternate ion-exchange media. The objective of the project in FY15 was to develop and test a porous foam monolith material that could serve as a replacement for the current anion-exchange resin, Reillex® HPQ, used at the Savannah River Site (SRS) for purifying Pu. The new material provides advantages in efficiency over the current resin by the elimination of diffusive mass transport through large granular resin beads. By replacing the large resin beads with a porous foam there is much more efficient contact between the Pu solution and the anion-exchange sites present on the material. Several samples of a polystyrene based foam grafted with poly(4-vinylpyridine) were prepared and the Pu sorption was tested in batch contact tests.

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

    Science.gov (United States)

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

    2015-12-01

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

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

    Science.gov (United States)

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

    2016-01-15

    Recombinant protein-based virus-like particles (VLPs) are steadily gaining in importance as innovative vaccines against cancer and infectious diseases. Multiple VLPs are currently evaluated in clinical phases requiring a straightforward and rational process design. To date, there is no generic platform process available for the purification of VLPs. In order to accelerate and simplify VLP downstream processing, there is a demand for novel development approaches, technologies, and purification tools. Membrane adsorbers have been identified as promising stationary phases for the processing of bionanoparticles due to their large pore sizes. In this work, we present the potential of two strategies for designing VLP processes following the basic tenet of 'quality by design': High-throughput experimentation and process modeling of an anion-exchange membrane capture step. Automated membrane screenings allowed the identification of optimal VLP binding conditions yielding a dynamic binding capacity of 5.7 mg/mL for human B19 parvovirus-like particles derived from Spodoptera frugiperda Sf9 insect cells. A mechanistic approach was implemented for radial ion-exchange membrane chromatography using the lumped-rate model and stoichiometric displacement model for the in silico optimization of a VLP capture step. For the first time, process modeling enabled the in silico design of a selective, robust and scalable process with minimal experimental effort for a complex VLP feedstock. The optimized anion-exchange membrane chromatography process resulted in a protein purity of 81.5%, a DNA clearance of 99.2%, and a VLP recovery of 59%. PMID:26718185

  17. Assay for inorganic pyrophosphate in chondrocyte culture using anion-exchange high-performance liquid chromatography and radioactive orthophosphate labeling

    International Nuclear Information System (INIS)

    A method is described for determination of inorganic pyrophosphate (PPi) in cell culture medium and in rabbit articular chondrocytes grown in the presence of radioactive orthophosphate (32Pi). Intra- and extracellular 32PPi formed was measured using high-performance liquid chromatographic (HPLC) separation of the PPi from orthophosphate (Pi) and other phosphate-containing compounds. The chromatographic separation on a weak anion-exchange column is based on the extent to which various phosphate compounds form complexes with Mg2+ at low pH and the rate at which such formation occurs. These complexes are eluted more readily than the uncomplexed compounds. Best results were obtained using a simultaneous gradient of Mg2+ ions and ionic strength. In this case separation of small amounts of PPi from a large excess of Pi was possible without prior removal of Pi or extraction of the PPi fraction. The assay is also useful for measurement of inorganic pyrophosphatase activity. The sensitivity of the assay depends on the specific activity of the added 32Pi and on the culture conditions, but is comparable with the most sensitive of the enzymatic assays. Sample preparation, particularly deproteinization, proved to be of importance. The losses of PPi which occur during procedures of this sort due to hydrolysis and coprecipitation were quantitated

  18. Determination of neomycin sulfate and impurities using high-performance anion-exchange chromatography with integrated pulsed amperometric detection.

    Science.gov (United States)

    Hanko, Valoran P; Rohrer, Jeffrey S

    2007-01-01

    Neomycin B is one of a class of aminoglycoside antibiotics that lack a good chromophore, and is therefore difficult to determine using reversed-phase HPLC with absorbance detection. This is especially true for determining the quantity of each impurity. We show that neomycin sulfate and its major impurities, including neamine (neomycin A), can be separated on a strong anion-exchange column using a weak potassium hydroxide eluent (2.40 mM) at a column temperature of 30 degrees C, and directly detected by integrated pulsed amperometric detection (IPAD). The resolution (United States Pharmacopeia (USP) definition) between neomycin B and the closest major impurity ranged from 6.56 and 7.45 over 10 days of consecutive analysis (7.24+/-0.10, n=836 injections). Due to the difficulty of producing weak hydroxide eluents of the required purity (i.e. carbonate-free), this method depends on automatic eluent generation to ensure method ruggedness. This method exhibited good long-term (10 days, 822 injections) retention time stability with a R.S.D. of 0.6%. Peak area R.S.D. (10 microM) was 1.3%. Method robustness was evaluated by intentionally varying the flow rate, eluent concentration, column temperature, and column. The spike recoveries of neomycin B from extractions of three different topical ointments and cream formulations ranged from 95 to 100%. The measured concentration of neomycin B in these formulations ranged from 119 to 154% of the label concentration. The R.S.D. for the measured concentration of one of the formulations tested over three separate days, n=11 extracts, was 3.2%. Based on the results of these evaluations, we believe this method can be used for neomycin sulfate identity, assay, and purity.

  19. Characterization of phosphoantigens by high-performance anion-exchange chromatography-electrospray ionization ion trap mass spectrometry and nanoelectrospray ionization ion trap mass spectrometry.

    Science.gov (United States)

    Pont, F; Luciani, B; Belmant, C; Fournié, J J

    2001-08-01

    New phosphorylated microbial metabolites referred to as phosphoantigens activate immune responses in humans. Although these molecules have leading applications in medical research, no direct method allows their rapid and unambiguous structural identification. Here, we interfaced online HPAEC (high performance anion-exchange chromatography) with ESI-ITMS (electrospray ionization ion trap mass spectrometry) to identify such pyrophosphorylated molecules. A self-regenerating anion suppressor located upstream of electrospray ionization enabled the simultaneous detection of pyrophosphoester by conductimetry, UV and MS. By HPAEC-ITMS and HPAEC-ITMS2, a single run permitted characterization of reference phosphoantigens and of related structures. Although all compounds were resolved by HPAEC, MS enabled their detection and identification by [M-H]- and fragment ions. Isobaric phosphoantigen analogues were also separated by HPAEC and distinguished by MS2. The relevance of this device was demonstrated for phosphoantigens analysis in human urine and plasma. Furthermore, identification of natural phosphoantigens by automatically generated 2D mass spectra from nano-ESI-ITMS is presented. This last technique permits the simultaneous performance of molecular screening of natural phosphoantigen extracts and their identification.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-06-01

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

  1. Preparation of quaternary amine monolithic column for strong anion-exchange chromatography and its application to the separation of Enterovirus 71.

    Science.gov (United States)

    Gu, Huimin; Yin, Dezhong; Ren, Jie; Zhang, Baoliang; Zhang, Qiuyu

    2016-10-15

    Large size virion is unable to diffuse into pores of conventional porous chromatography particles. Therefore, separation of virion by conventional column-packing materials is not quite efficient. To solve this problem, a monolithic column with large convective pores and quaternary amine groups was prepared and was applied to separate Enterovirus 71 (EV71, ≈5700-6000kDa). Cross-section, pore structure, hydrodynamic performance, adsorption property and dynamic binding capacity of prepared monolithic column were determined. Double-pore structures, macropore at 2472nm and mesopore at 5-60nm, were formed. The porosity was up to 63.3%, which enable higher permeability and lower back pressure of the monolithic column than commercial UNO™ Q1 column. Based on the breakthrough curves, the loading capacity of bovine serum albumin was calculated to be 42.0mg per column. In addition, prepared quaternary amine monolithic column was proved to be suitable for the separation of protein mixture by strong anion-exchange chromatography. As a practical application, prepared monolith column presents excellent performance to the separation of EV71 from virus-proteins mixture.

  2. Rapid and sensitive quantification of levoglucosan in aerosols by high-performance anion-exchange chromatography with positive electrospray ionization mass spectrometry (HPAEC-positive ESI-MS)

    Science.gov (United States)

    Asakawa, Daichi; Furuichi, Yuko; Yamamoto, Atsushi; Oku, Yuichiro; Funasaka, Kunihiro

    2015-12-01

    A convenient quantification method for underivatized levoglucosan, which is a tracer for biomass burning influenced particulate matter (PM), has been established using high-performance anion-exchange chromatography (HPAEC) coupled to positive electrospray ionization mass spectrometry ((+)ESI-MS). Levoglucosan was chromatographically separated from its isomers (mannosan and galactosan) and detected selectively with positive ESI-MS. Limits of detection and quantification for this method were 0.40 and 1.3 ng mL-1, respectively. A comparison of simultaneous measurements by this method and conventional derivatization gas chromatography/mass spectrometry showed a good linearity with a slope of 1.008 and a determination coefficient of 0.9932. The developed method was applied to ambient suspended particulate matter hourly collected by continuous particulate monitors at 10 stations. The hourly concentration of levoglucosan during August 9-11, 2011, was 1.7-918 ng m-3 and its distribution indicated the transportation of biomass burning aerosols of a forest fire. This is the first report of horizontal distribution of the hourly levoglucosan concentration in Japan.

  3. Rapid simultaneous analysis of oxyhalides and inorganic anions in aqueous media by ion exchange chromatography with indirect UV detection

    Directory of Open Access Journals (Sweden)

    Mohammadine El Haddad

    2015-01-01

    Best separations have also occured between(Cl-/ClO3- and(Br-/BrO3- with good a resolution. Detections limits (S/N = 3 ofBrO3-,ClO3-andNO3- were 2 and 5 ppm for inorganic anions Cl−, Br− andSO42-. The method had a good linearity (r2 > 0.995 and high precision (relative standard deviation <4%. The main reason for the detector choice was that UV detectors are widespread in educational and low level equipment laboratories. Indirect photometric detection is an attractive and inexpensive approach and the system is versatile.

  4. Assessing Gibberellins Oxidase Activity by Anion Exchange/Hydrophobic Polymer Monolithic Capillary Liquid Chromatography-Mass Spectrometry

    OpenAIRE

    Ming-Luan Chen; Xin Su; Wei Xiong; Jiu-Feng Liu; Yan Wu; Yu-Qi Feng; Bi-Feng Yuan

    2013-01-01

    Bioactive gibberellins (GAs) play a key regulatory role in plant growth and development. In the biosynthesis of GAs, GA3-oxidase catalyzes the final step to produce bioactive GAs. Thus, the evaluation of GA3-oxidase activity is critical for elucidating the regulation mechanism of plant growth controlled by GAs. However, assessing catalytic activity of endogenous GA3-oxidase remains challenging. In the current study, we developed a capillary liquid chromatography – mass spectrometry (cLC-MS) m...

  5. Short communication: Quantification of carbohydrates in whey permeate products using high-performance anion-exchange chromatography with pulsed amperometric detection

    Science.gov (United States)

    Lee, Hyeyoung; de MeloSilva, Vitor Luiz; Liu, Yan

    2016-01-01

    A method was developed for the characterization and quantification of the disaccharide lactose and 3 major bovine milk oligosaccharides (BMO) in dairy streams. Based on high-performance anion-exchange chromatography-pulsed amperometric detection (HPAE-PAD), this method is advantageous because it requires minimal sample preparation and achieves good chromatographic separation of oligosaccharide isomers within 30 min. The linear dynamic range and limit of detection were 0.1 to 10 mg/L and 0.03 to 0.22 mg/L, respectively. Mean recoveries of the BMO were excellent and ranged from 98.4 to 100.4%. Without complicated sample preparation procedures, this HPAE-PAD method measured BMO [3′-sialyllactose (3′SL), 6′-sialyllactose (6′SL), and 6′-sialyllactosamine (6′SLN)] and lactose using a single instrument, therefore increasing the accuracy of the measurement and applicability for the dairy industry. In colostrum whey permeate, 3′SL, 6′SL, and 6′SLN were 94, 29, and 46 mg/L, respectively. This work is the first to demonstrate that some commercial products, currently marketed for supporting a healthy immune system, contain significant amounts of bioactive BMO and therefore, carry additional bioactivities. PMID:26364096

  6. Radioimmunoassay of a new angiotensin-converting enzyme inhibitor (perindopril) in human plasma and urine: Advantages of coupling anion-exchange column chromatography with radioimmunoassay

    Energy Technology Data Exchange (ETDEWEB)

    Doucet, L.; De Veyrac, B.; Delaage, M.; Cailla, H.; Bernheim, C.; Devissaguet, M. (Immunotech S. A. Case 915, Marseille (France))

    1990-08-01

    Perindopril (P) is a prodrug whose active metabolite perindoprilat (PT) is an antihypertensive agent which acts by inhibition of angiotensin-converting enzyme (ACE). Anti-PT antiserum was produced in a rabbit immunized against PT that was covalently linked to bovine serum albumin. The radioligand is an iodinated ({sup 125}I) derivative of PT-glycyltyrosinamide. Both the drug (PT) and the prodrug (P) are assayed in the same sample; PT is assayed as is and P is assayed after quantitative alkaline hydrolysis into PT. Certain data obtained from such assays suggest the occurrence in plasma and urine of a third immunoreactive component. A chromatographic fractionation of samples allowed us to isolate a new immunoreactive metabolite which was further identified as a glucuronide of PT (PT-G). Therefore, the whole assay was carried out as follows: biological samples were fractionated by stepwise chromatography on a anion-exchange resin (the first fraction contained P, the second contained PT, and the third contained PT-G); and RIA was performed on fractions 2 and 3 as is, and on fraction 1 after alkaline hydrolysis. Performances and assessments of this method are presented together with an example of a pharmacokinetic profile.

  7. Chiral mobile phase in ligand-exchange chromatography of amino acids: exploring the copper(II) salt anion effect with a computational approach.

    Science.gov (United States)

    Sardella, Roccaldo; Macchiarulo, Antonio; Carotti, Andrea; Ianni, Federica; Rubiño, Maria Eugenia García; Natalini, Benedetto

    2012-12-21

    With the use of a chiral ligand-exchange chromatography (CLEC) system operating with the O-benzyl-(S)-serine [(S)-OBS] [1,2] as the chiral mobile phase (CMP) additive to the eluent, the effect of the copper(II) anion type on retention (k) and separation (α) factors was evaluated, by rationally changing the following experimental conditions: salt concentration and temperature. The CLEC-CMP analysis was carried out on ten amino acidic racemates and with nine different cupric salts. While the group of analytes comprised both aliphatic (leucine, isoleucine, nor-leucine, proline, valine, nor-valine, and α-methyl-valine) and aromatic (1-aminoindan-1,5-dicarboxylic acid, phenylglycine, and tyrosine) species, representative organic (formate, methanesulfonate, and trifluoroacetate) and inorganic (bromide, chloride, fluoride, nitrate, perchlorate, and sulfate) Cu(II) salts were selected as the metal source into the eluent. This route of investigation was pursued with the aim of identifying analogies among the employed Cu(II) salts, by observing the variation profile of the selected chromatographic parameters, upon a change of the above experimental conditions. All the data were collected and analyzed through a statistical approach (PCA and k-means clustering) that revealed the presence of two behavioral classes of cupric salts, sharing the same variation profile for k and α values. Interestingly, this clustering can be explained in terms of ESP (electrostatic surface potential) balance (ESP(bal)) values, obtained by an ab initio calculation operated on the cupric salts. The results of this appraisal could aid the rational choice of the most suitable eluent system, to succeed in the enantioseparation of difficult-to-resolve compounds, along with the eventual scale-up to a semi-preparative level. PMID:22926052

  8. Simultaneous separation and quantitative determination of monosaccharides, uronic acids, and aldonic acids by high performance anion-exchange chromatography coupled with pulsed amperometric detection in corn stover prehydrolysates

    Directory of Open Access Journals (Sweden)

    Xing Wang

    2012-11-01

    Full Text Available A method for simultaneous separation and quantitative determination of arabinose, galactose, glucose, xylose, xylonic acid, gluconic acid, galacturonic acid, and glucuronic acid was developed by using high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD. The separation was performed on a CarboPacTM PA-10 column (250 mm × 2 mm with a various gradient elution of NaOH-NaOAc solution as the mobile phase. The calibration curves showed good linearity (R2 ≥ 0.9993 for the monosaccharides, uronic acids, and aldonic acids in the range of 0.1 to 12.5 mg/L. The detection limits (LODs and the quantification limits (LOQs were 4.91 to 18.75 μg/L and 16.36 to 62.50 μg/L, respectively. Relative standard deviations (RSDs of the retention times and peak areas for the seven consecutive determinations of an unknown amount of mixture were 0.15% to 0.44% and 0.22% to 2.31%, respectively. The established method was used to separate and determine four monosaccharides, two uronic acids, and two aldonic acids in the prehydrolysate from dilute acid steam-exploded corn stover within 21 min. The spiked recoveries of monosaccharides, uronic acids, and aldonic acids ranged from 91.25% to 108.81%, with RSDs (n=3 of 0.04% ~ 6.07%. This method was applied to evaluate the quantitative variation of sugar and sugar acid content in biomass prehydrolysates.

  9. A simple and rapid method for measuring α-D-phosphohexomutases activity by using anion-exchange chromatography coupled with an electrochemical detector.

    Science.gov (United States)

    Jia, Xiaochen; Kang, Jian; Yin, Heng

    2016-01-01

    The interconversion of hexose-6-phosphate and hexose-1-phosphate can be directly analyzed by high-performance anion-exchange chromatography coupled with an electrochemical detector (HPAEC-PAD). Thus, this method can be used to measure the activities of N-acetylglucosamine-phosphate mutase (AGM), glucosamine-phosphate mutase (GlmM) and phosphoglucomutase (PGM), which are the members of α-D-phosphohexomutases superfamily. The detection limits were extremely low as 2.747 pmol, 1.365 pmol, 0.512 pmol, 0.415 pmol, 1.486 pmol and 0.868 pmol for N-acetylglucosamine-1-phosphate (GlcNAc-1-P), N-acetylglucosamine-6-phosphate (GlcNAc-6-P), glucosamine-1-phosphate (GlcN-1-P), glucosamine-6-phosphate (GlcN-6-P), glucose-1-phosphate (Glc-1-P) and glucose-6-phosphate (Glc-6-P), respectively. By employing HPAEC-PAD, activities of AtAGM (AGM from Arabidopsis thaliana) on these six phosphohexoses can be detected. The Km of AtAGM on Glc-1-P determined by HPAEC-PAD was 679.18 ± 156.40 µM, which is comparable with the Km of 707.09 ± 170.36 µM detected by traditional coupled assay. Moreover, the activity of MtGlmM (GlmM from Mycobacterium tuberculosis) on GlcN-6-P tested by HPAEC-PAD was 7493.40 ± 309.12 nmol∕min ⋅ mg, which is much higher than 288.97 ± 35.28 nmol∕min ⋅ mg obtained by the traditional coupled assay. Accordingly, HPAEC-PAD is a more rapid and simple method than the traditional coupled assays given its high specificity and sensitivity, and will certainly bring convenience to further research of α-D-phosphohexomutases. PMID:26788420

  10. Stability study of As(III), As(V), MMA and DMA by anion exchange chromatography and HG-AFS in wastewater samples

    Energy Technology Data Exchange (ETDEWEB)

    Segura, Marta; Munoz, Juan; Madrid, Yolanda; Camara, Carmen [Departamento de Quimica Analitica, Facultad de Ciencias Quimicas, Universidad Complutense, 28040 Madrid (Spain)

    2002-10-01

    The stability of arsenic species {l_brace}arsenate [As(V)], monomethylarsonate [MMA], dimethylarsinate [DMA] and arsenite [As(III)]{r_brace} in two types of urban wastewater samples (raw and treated) was evaluated. Water samples containing a mixture of the different arsenic species were stored in the absence of light at three different temperatures: +4 C, +20 C and +40 C. At regular time intervals, arsenic species were determined by high performance liquid chromatography (HPLC)-hydride generation (HG)-atomic fluorescence spectrometry (AFS). The experimental conditions for the separation of arsenic species by HPLC and their determination by AFS were directly optimised from wastewater samples. As(III), As(V), MMA and DMA were separated on an anion exchange column using phosphate buffer (pH 6.0) as the mobile phase. Under these conditions the four arsenic species were separated in less than 10 min. The detection limits were 0.6, 0.9, 0.9 and 1.8 {mu}g L{sup -1} for As(III), DMA, MMA and As(V), respectively. As(V), MMA and DMA were found stable in the two types of urban wastewater samples over the 4-month period at the three different temperatures tested, while the concentration of As(III) in raw wastewater sample decreased after 2 weeks of storage. A greater stability of As(III) was found in the treated urban wastewater sample. As(III) remained unaltered in this matrix at pH 7.27 over the period studied, while at lower pH (1.6) losses of As(III) were detected after 1 month of storage. The results show that the decrease in As(III) concentration with time was accompanied by an increase in As(V) concentration. (orig.)

  11. Determination of nitric oxide metabolites, nitrate and nitrite, in Anopheles culicifacies mosquito midgut and haemolymph by anion exchange high-performance liquid chromatography: plausible mechanism of refractoriness

    Directory of Open Access Journals (Sweden)

    Adak Tridibesh

    2008-04-01

    Full Text Available Abstract Background The diverse physiological and pathological role of nitric oxide in innate immune defenses against many intra and extracellular pathogens, have led to the development of various methods for determining nitric oxide (NO synthesis. NO metabolites, nitrite (NO2- and nitrate (NO3- are produced by the action of an inducible Anopheles culicifacies NO synthase (AcNOS in mosquito mid-guts and may be central to anti-parasitic arsenal of these mosquitoes. Method While exploring a plausible mechanism of refractoriness based on nitric oxide synthase physiology among the sibling species of An. culicifacies, a sensitive, specific and cost effective high performance liquid chromatography (HPLC method was developed, which is not influenced by the presence of biogenic amines, for the determination of NO2- and NO3- from mosquito mid-guts and haemolymph. Results This method is based on extraction, efficiency, assay reproducibility and contaminant minimization. It entails de-proteinization by centrifugal ultra filtration through ultracel 3 K filter and analysis by high performance anion exchange liquid chromatography (Sphereclone, 5 μ SAX column with UV detection at 214 nm. The lower detection limit of the assay procedure is 50 pmoles in all midgut and haemolymph samples. Retention times for NO2- and NO3- in standards and in mid-gut samples were 3.42 and 4.53 min. respectively. Assay linearity for standards ranged between 50 nM and 1 mM. Recoveries of NO2- and NO3- from spiked samples (1–100 μM and from the extracted standards (1–100 μM were calculated to be 100%. Intra-assay and inter assay variations and relative standard deviations (RSDs for NO2- and NO3- in spiked and un-spiked midgut samples were 5.7% or less. Increased levels NO2- and NO3- in midguts and haemolymph of An. culicifacies sibling species B in comparison to species A reflect towards a mechanism of refractoriness based on AcNOS physiology. Conclusion HPLC is a sensitive

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-31

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

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

    International Nuclear Information System (INIS)

    This paper reports an automated analytical method for rapid determination of plutonium isotopes (239Pu and 240Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-x4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 103 to 104. The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials.

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

    Science.gov (United States)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per; Miró, Manuel

    2011-01-31

    This paper reports an automated analytical method for rapid determination of plutonium isotopes ((239)Pu and (240)Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-×4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 10(3) to 10(4). The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials. PMID:21168558

  15. Anion-exchange high-performance liquid chromatography with post-column detection for the analysis of phytic acid and other inositol phosphates

    Science.gov (United States)

    Rounds, M. A.; Nielsen, S. S.; Mitchell, C. A. (Principal Investigator)

    1993-01-01

    The use of gradient anion-exchange HPLC, with a simple post-column detection system, is described for the separation of myo-inositol phosphates, including "phytic acid" (myo-inositol hexaphosphate). Hexa-, penta-, tetra-, tri- and diphosphate members of this homologous series are clearly resolved within 30 min. This method should facilitate analysis and quantitation of "phytic acid" and other inositol phosphates in plant, food, and soil samples.

  16. Purification of Peanut Allergen Ara h1 with Anion-exchange Chromatography%阴离子交换层析法分离纯化花生主要过敏原Ara h1的研究

    Institute of Scientific and Technical Information of China (English)

    何伟逸; 吴序栎; 刘志刚; 黄海珍; 李瑶; 叶烨; 曹鹤瑶

    2013-01-01

    Protien Ara hi is a major allergen in peanut In order to obtain the natural peanut allergen Ara hi, ammonium sulfate precipitation and anion-exchange chromatography were used for purification. The analysis and identification of peanut allergens was carried out using SDS-PAGE and Western blot The results showed that the purity of Ara hi was more than 90 percent and the recovery accounted 23.1% of total Ara hi with the anion-exchange chromatography. The Ara hi purfied by anion-exchange chromatography had immunocompetence. It can combine to peanut allergy patients serum with high specificity.%Ara h1蛋白是花生的主要过敏原蛋白.本研究从天然的花生提取花生蛋白质,通过硫酸铵分级沉淀及阴离子交换层析法纯化花生主要过敏原Ara h1.通过聚丙烯酰胺凝胶电泳分析蛋白纯度,结合免疫印迹实验对Ara h1免疫活性进行鉴定.结果表明:采用阴离子交换层析法纯化出的Ara h1纯度达到90%以上.得率为23.1%.免疫印迹实验表明,此方法纯化出来的Ara h1仍具有免疫原性,能跟花生过敏病人血清特异结合.

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

    DEFF Research Database (Denmark)

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

    2008-01-01

    A method for determination of mycophenolic acid (MPA) in dry-cured ham, fermented sausage and liver pate is described. MPA was extracted from meat with bicarbonate-acetonitrile, further cleaned-up by mixed mode reversed phase-anion exchange and detected using a LC-MS system with electrospray...... ionisation-time-of-flight detection. The limit of detection was 4 mu g/kg in sausage and 6 mu g/kg in ham and pate. The method was successfully used for quantification of MPA in dry-cured ham and liver pate artificially inoculated with Penicillium brevicompactum. Levels ranged from 190 mu g/kg in centre to I...

  18. Improvement of separation efficiencies of anion-exchange chromatography using monolithic silica capillary columns modified with polyacrylates and polymethacrylates containing tertiary amino or quaternary ammonium groups.

    Science.gov (United States)

    Watanabe, Yuta; Ikegami, Tohru; Horie, Kanta; Hara, Takeshi; Jaafar, Jafariah; Tanaka, Nobuo

    2009-10-30

    Anion-exchange (AEX) columns were prepared by on-column polymerization of acrylates and methacrylates containing tertiary amino or quaternary ammonium groups on monolithic silica in a fused silica capillary modified with anchor groups. The columns provided a plate height (H) of less than 10 microm at optimum linear velocity (u) with keeping their high permeability (K=9-12 x 10(-14) m2). Among seven kinds of AEX columns, a monolithic silica column modified with poly(2-hydroxy-3-(4-methylpiperazin-1-yl)propyl methacrylates) (HMPMA) showed larger retentions and better selectivities for nucleotides and inorganic anions than the others. The HMPMA column of 410 mm length produced 42,000-55,000 theoretical plates (N) at a linear velocity of 0.97 mm/s with a backpressure of 3.8 MPa. The same column could be employed for a fast separation of inorganic anions in 1.8 min at a linear velocity of 5.3 mm/s with a backpressure of 20 MPa. In terms of van Deemter plot and separation impedance, the HMPMA column showed higher performance than a conventional particle-packed AEX column. The HMPMA column showed good recovery of a protein, trypsin inhibitor, and it was applied to the separation of proteins and tryptic digest of bovine serum albumin (BSA) in a gradient elution, to provide better separation compared to a conventional particle-packed AEX column. PMID:19683243

  19. Trace enrichment and characterization of polyphenols in Bistort Rhizoma using weak anion-exchange solid phase extraction and high performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Shao-Teng; Yang, Hua; Gao, Wen; Li, Hui-Jun; Li, Ping

    2016-02-01

    The analysis of trace constituents in herbal medicines has always been a challenge due to complex matrices and structural diversities. In this work, a pH-sensitive solid phase extraction (SPE) procedure capable of enriching trace polyphenols in Bistort Rhizoma (BR) was proposed and preliminary chemical characterization was accomplished by high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS). A weak anion-exchange SPE column packed with divinylbenzene/vinylpyrrolidone bonding quaternary amine group was employed for anionic extraction, and the target fraction was obtained by eluting with acidic methanol (apparent pH 1.9). On the other hand, the MS/MS fragmentation rules of four reference polyphenols in negative ion mode were outlined. Using these rules, a total of 31 polyphenols including 20 benzoyl derivatives and 11 caffeoyl derivatives were screened out from BR extract, of which 26 trace members were found for the first time in this herb. Those findings demonstrated that the anion-exchange SPE could enhance the detection capability and selectivity for plant polyphenols in the LC-MS analysis and the strategy for deducing structures could be applied for analysis of polyphenols in BR and other herbal medicines.

  20. Rapid determination of vitellogenin in fish plasma by anion exchange high performance liquid chromatography using postcolumn fluorescence derivatization with o-phthalaldehyde.

    Science.gov (United States)

    Wu, Cuiqin; Yuan, Dongxing; Liu, Baomin

    2006-12-01

    An analytical method involving anion exchange high performance liquid chromatographic determination of vitellogenin (Vtg) in fish plasma after postcolumn fluorescence derivatization with o-phthalaldehyde (OPA) was developed. The retention time of Vtg was about 11 min. The reagent variables for derivatization were optimized. The fluorophore was excited at 335 nm and detected at 435 nm. A calibration curve was established ranging from 0.13 to 11.28 microg. The determination limit of Vtg was found to be as low as 0.13 microg. The spiked recovery was 93.6% and interassay variability was less than 4%. The method developed was used to determine Vtg in fish plasma obtained from red sea bream (Pagrosomus major), black porgy (Sparus macrocephalus) and skew band grunt (Hapalogenys nitens), without complicated sample pretreatment. The results confirmed that the method showed advantages of being simple, rapid, reproducible and sensitive. PMID:17159322

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

    DEFF Research Database (Denmark)

    Andersen, Rikke; Sørensen, A.

    1999-01-01

    effects than the fructanase reported as normally used. The method is tested on ten standard substances and five fructan products, and nine foods and food products are also analysed. The enzymatic measurement of the released sugars is confirmed by measurements done by high performance anion exchange......We report a new and non-equipment demanding method of measuring the content of fructans as well as the contents of free glucose, free fructose and sucrose in foods and food products enzymatically. This method comprises hydrolysis of fructans into D-glucose and D-fructose enzymatically...... and measurement of the released sugars enzymatically. Sucrose is hydrolysed by alpha-glucosidase instead of beta-fructosidase, which is normally used. In addition, sucrose is measured in the form of D-fructose instead of the typical D-glucose form, and the fructanase used to hydrolyse the fructans has fewer side...

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

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per;

    2011-01-01

    This paper reports an automated analytical method for rapid determination of plutonium isotopes (239Pu and 240Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from...... size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 103 to 104....... The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method...

  3. Short-column anion-exchange chromatography for soil and peat humic substances profiling by step-wise gradient of high pH aqueous sodium ethylenediaminetetraacetate.

    Science.gov (United States)

    Hutta, Milan; Ráczová, Janka; Góra, Róbert; Pessl, Juraj

    2015-08-21

    Novel anion-exchange liquid chromatographic method with step gradient of aqueous EDTA(4-) based mobile phase elution has been developed to profile available Slovak soil humic substances and alkaline extracts of various soils. The method utilize short glass column (30mm×3mm) filled in with hydrolytically stable particles (60μm diameter) Separon HEMA-BIO 1000 having (diethylamino)ethyl functional groups. Step gradient was programmed by mixing mobile phase composed of aqueous solution of sodium EDTA (pH 12.0; 5mmolL(-1)) and mobile phase constituted of aqueous solution of sodium EDTA (pH 12.0, 500mmolL(-1)). The FLD of HSs was set to excitation wavelength 480nm and emission wavelength 530nm (λem). Separation mechanism was studied by use of selected aromatic acids related to humic acids with the aid of UV spectrophotometric detection at 280nm. The proposed method benefits from high ionic strength (I=5molL(-1)) of the end mobile phase buffer and provides high recovery of humic acids (98%). Accurate and reproducible profiling of studied humic substances, alkaline extracts of various types of soils enables straightforward characterization and differentiation of HSs in arable and forest soils. Selected model aromatic acids were used for separation mechanism elucidation.

  4. Short-column anion-exchange chromatography for soil and peat humic substances profiling by step-wise gradient of high pH aqueous sodium ethylenediaminetetraacetate.

    Science.gov (United States)

    Hutta, Milan; Ráczová, Janka; Góra, Róbert; Pessl, Juraj

    2015-08-21

    Novel anion-exchange liquid chromatographic method with step gradient of aqueous EDTA(4-) based mobile phase elution has been developed to profile available Slovak soil humic substances and alkaline extracts of various soils. The method utilize short glass column (30mm×3mm) filled in with hydrolytically stable particles (60μm diameter) Separon HEMA-BIO 1000 having (diethylamino)ethyl functional groups. Step gradient was programmed by mixing mobile phase composed of aqueous solution of sodium EDTA (pH 12.0; 5mmolL(-1)) and mobile phase constituted of aqueous solution of sodium EDTA (pH 12.0, 500mmolL(-1)). The FLD of HSs was set to excitation wavelength 480nm and emission wavelength 530nm (λem). Separation mechanism was studied by use of selected aromatic acids related to humic acids with the aid of UV spectrophotometric detection at 280nm. The proposed method benefits from high ionic strength (I=5molL(-1)) of the end mobile phase buffer and provides high recovery of humic acids (98%). Accurate and reproducible profiling of studied humic substances, alkaline extracts of various types of soils enables straightforward characterization and differentiation of HSs in arable and forest soils. Selected model aromatic acids were used for separation mechanism elucidation. PMID:26143606

  5. 阴离子交换色谱法一步分离牛初乳中的sIgA%Single-step purification of sIgA from bovine colostrums by anion-exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    章飞燕; 叶鹏程; 任其龙

    2011-01-01

    利用强碱3对所获免疫球蛋白A产品纯度的影响,获得从牛初乳中分离免疫球蛋白A的最优条件为pH 7.0,离子强度为0.03mol/L的磷酸盐缓冲液,最终可获得纯度为91.24%的免疫球蛋白A,回收率达到47%.因此,利用以强碱3#树脂为基质的阴离子交换色谱分离牛初乳中的免疫球蛋白A具有很好的发展潜力.%A fraction containing slgA (slgA-rich fraction)was prepared from bovine colostrum by anion exchange chromatography using alkali resin.The effect of changing buffer properties( pH and ionic strength)on purity of slgA was studied.The best result was slgA purity increasing from 16.31% in bovine colostrum solution to 91.24% in the eluting fraction with a recovery of 47% at the condition of pH 7.0,0.03mol/L sodium phosphate.These results suggested that the anion exchange chromatography using alkali resin was a potential process for slgA purification from bovine colostrum.

  6. A tandem laboratory scale protein purification process using Protein A affinity and anion exchange chromatography operated in a weak partitioning mode.

    Science.gov (United States)

    Shamashkin, Michael; Godavarti, Ranga; Iskra, Timothy; Coffman, Jon

    2013-10-01

    A significant consequence of scaling up production of high titer monoclonal antibody (mAb) processes in existing facilities is the generation of in-process pools that exceed the capacity of storage vessels. A semi-continuous downstream process where columns and filters are linked and operated in tandem would eliminate the need for intermediate holding tanks. This study is a bench-scale demonstration of the feasibility of a tandem process for the purification of mAbs employing an affinity Protein A capture step, followed by a flow-through anion-exchange (AEX) step with the possibility of adding an in-line virus filtration step (VF). All three steps were linked sequentially and operated as one continuous process using an ÄKTA FPLC equipped with two pumps and a system of valves and bypasses that allowed the components to be engaged at different stages of the process. The AEX column was operated in a weak partitioning (WP) mode enabled by a precise in-line titration of Protein A effluent. In order to avoid complex control schemes and facilitate validation, quality and robustness were built into the system through selection of buffers based on thermodynamic and empirical models. The tandem system utilized the simplest possible combination of valves, pumps, controls, and automation, so that it could easily be implemented in a clinical or commercial production facility. Linking the purification steps in a tandem process is expected to generate savings in time and production costs and also reduce the size of quality systems due to reduced documentation requirements, microbial sampling, and elimination of hold time validation. PMID:23633385

  7. Online determination of levoglucosan in ambient aerosols with Particle-into-Liquid Sampler – High-Performance Anion-Exchange Chromatography – Mass Spectrometry (PILS–HPAEC–MS

    Directory of Open Access Journals (Sweden)

    K. Saarnio

    2013-06-01

    Full Text Available Biomass burning, such as domestic heating, agricultural, and wild open-land fires, has a significant influence on the atmosphere at the global and, especially, at the local scale. Levoglucosan has been shown to be a good tracer for biomass burning emissions in atmospheric particulate matter and several analytical techniques have been presented for the determination of levoglucosan from filter samples. In this paper, a novel combination of a Particle-into-Liquid Sampler (PILS to a high-performance anion-exchange chromatograph (HPAEC with the detection by a mass spectrometer (MS is presented for the online analysis of levoglucosan in ambient particles. The PILS–HPAEC–MS technique enables a fast online analysis of levoglucosan from the particulate samples. The method was tested at an urban background station in Helsinki, Finland, in winter 2011. A comparison with simultaneous levoglucosan measurements from filter samples by the HPAEC–MS was performed and it showed a good agreement between the online and offline methods. Additionally, the online levoglucosan data were compared with the biomass burning tracer fragments measured by a High-Resolution Time-of-Flight Aerosol Mass Spectrometer (HR-ToF-AMS. As there were no local biomass burning sources close to the measurement station, online levoglucosan measurements revealed that most of the particles from biomass burning were either regionally distributed or long-range transported in the urban background of Helsinki. The average levoglucosan concentrations were relatively low (average 0.083 μg m−3 during the measurement campaign. The highest concentration peak measured for levoglucosan (1.4 μg m−3 seemed to originate from biomass burning in Eastern Europe, likely in Estonia, that was transported to Helsinki.

  8. Online determination of levoglucosan in ambient aerosols with particle-into-liquid sampler – high-performance anion-exchange chromatography – mass spectrometry (PILS–HPAEC–MS

    Directory of Open Access Journals (Sweden)

    K. Saarnio

    2013-10-01

    Full Text Available Biomass burning, such as domestic heating, agricultural, and wild open-land fires, has a significant influence on the atmosphere at the global and, especially, at the local scale. Levoglucosan has been shown to be a good tracer for biomass burning emissions in atmospheric particulate matter, and several analytical techniques have been presented for the determination of levoglucosan from filter samples. In this paper, a novel combination of a particle-into-liquid sampler (PILS to a high-performance anion-exchange chromatograph (HPAEC with the detection by a mass spectrometer (MS is presented for the online analysis of levoglucosan in ambient particles. The PILS–HPAEC–MS technique enables a fast online analysis of levoglucosan from the particulate samples. The method was tested at an urban background station in Helsinki, Finland, in winter 2011. A comparison with simultaneous levoglucosan measurements from filter samples by the HPAEC–MS was performed and it showed a good agreement between the online and offline methods. Additionally, the online levoglucosan data were compared with the biomass burning tracer fragments measured by a high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS. As there were no local biomass burning sources close to the measurement station, online levoglucosan measurements revealed that most of the particles from biomass burning were either regionally distributed or long-range transported in the urban background of Helsinki. The average levoglucosan concentrations were relatively low (average 0.083 μg m−3 during the measurement campaign. The highest concentration peak measured for levoglucosan (1.4 μg m−3 seemed to originate from biomass burning in the Baltic countries, likely in Estonia, that was transported to Helsinki.

  9. Online determination of levoglucosan in ambient aerosols with particle-into-liquid sampler - high-performance anion-exchange chromatography - mass spectrometry (PILS-HPAEC-MS)

    Science.gov (United States)

    Saarnio, K.; Teinilä, K.; Saarikoski, S.; Carbone, S.; Gilardoni, S.; Timonen, H.; Aurela, M.; Hillamo, R.

    2013-10-01

    Biomass burning, such as domestic heating, agricultural, and wild open-land fires, has a significant influence on the atmosphere at the global and, especially, at the local scale. Levoglucosan has been shown to be a good tracer for biomass burning emissions in atmospheric particulate matter, and several analytical techniques have been presented for the determination of levoglucosan from filter samples. In this paper, a novel combination of a particle-into-liquid sampler (PILS) to a high-performance anion-exchange chromatograph (HPAEC) with the detection by a mass spectrometer (MS) is presented for the online analysis of levoglucosan in ambient particles. The PILS-HPAEC-MS technique enables a fast online analysis of levoglucosan from the particulate samples. The method was tested at an urban background station in Helsinki, Finland, in winter 2011. A comparison with simultaneous levoglucosan measurements from filter samples by the HPAEC-MS was performed and it showed a good agreement between the online and offline methods. Additionally, the online levoglucosan data were compared with the biomass burning tracer fragments measured by a high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS). As there were no local biomass burning sources close to the measurement station, online levoglucosan measurements revealed that most of the particles from biomass burning were either regionally distributed or long-range transported in the urban background of Helsinki. The average levoglucosan concentrations were relatively low (average 0.083 μg m-3) during the measurement campaign. The highest concentration peak measured for levoglucosan (1.4 μg m-3) seemed to originate from biomass burning in the Baltic countries, likely in Estonia, that was transported to Helsinki.

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

    Science.gov (United States)

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

    2015-01-01

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

  11. Determination of trace inorganic anions in anionic surfactants by single-pump column-switching ion chromatography

    Institute of Scientific and Technical Information of China (English)

    Jia Jie Zhang; Hai Bao Zhu; Yan Zhu

    2012-01-01

    An ion chromatography method has been proposed for the determination of three common inorganic anions (chloride,nitrate and sulfate) in anionic surfactants using a single pump system.The new system consists of an ion exclusion column,a concentrator column,and an anion exchange column connected in series via two 6-ports valves in a Dionex ICS-2000 ion chromatograph.The valves were switched several times for removing surfactants,concentrating and separating the three anions.The chromatographic conditions were optimized.Detection limits (S/N =3) were in the range of 0.10-0.68 μg/L.The relative standard deviations (RSDs)of peak area were less than 4.6%.The recoveries were in the range of 84.1-112.6%.

  12. A new method for separation and determination of Cr(III) and Cr(VI) in water samples by high-performance liquid chromatography based on anion exchange stationary phase of ionic liquid modified silica.

    Science.gov (United States)

    Sadeghi, Susan; Moghaddam, Ali Zeraatkar

    2015-12-01

    In this work, N-methylimidazolium-chloride ionic liquid functionalized silica was prepared and used as an anion-exchange stationary phase for separation of chromium species by high-performance liquid chromatography (HPLC) with UV detection at 200 nm. The Cr(VI) as HCr2O7(-) and chelated Cr(III) with potassium hydrogen phthalate (PHP) as Cr(PHP)2 (-) was retained on the prepared column and separated using a mobile phase composed of 5% methanol in 25 mM phosphate buffer at pH 6.5. Several variables affecting the chelation/separation steps were modeled by response surface methodology (RSM) using Box-Behnken (BBD) design. The significance of the independent variables and their interactions were tested by the analysis of variances (ANOVA) with 95% confidence limit. Under the optimized conditions, the Cr(III) and Cr(VI) anionic species were well separated with a single peak for each Cr species at retention times of 2.3 and 4.3 min, respectively. The relationship between the peak area and concentration was linear in the range of 0.025-30 for Cr(III) and 0.5-20 mg L(-1) for Cr(VI) with detection limits of 0.010 and 0.210 mg L(-1) for Cr(III) and Cr(VI), respectively. The proposed method was validated by simultaneous separation and determination of the Cr species in tap and underground water samples without impose to any pretreatment. PMID:26526699

  13. Enhanced conductivity detection of common inorganic anions in electrostatic ion chromatography using water eluent

    Institute of Scientific and Technical Information of China (English)

    Daisuke KOZAKI; Chao-Hong SHI; Kazuhiko TANAKA; Nobutake NAKATANI

    2012-01-01

    To enhance the conductivity detection sensitivity of common anions (Na-anions) in electrostatic ion chromatography (EIC) by elution with water,a conductivity enhancement column packed with strong acid cation exchange resin in the H-form was inserted between an octadecyl silane (ODS)-silica separation column modified with zwitterionic surfactant ( CHAPS:3- { ( 3-cholamidopropyl ) -dimethylammonio } propanesulfonate ) and a conductivity detector.Specifically,the Na-anion pairing is converted to H-anion pairing after the EIC separation and then detected sensitively by the conductivity detector.The effects of conductivity enhancement and suppression in the EIC by the enhanced conductivity detection were characterized for the common strong acid anions such as SO42-,Cl-,NO3-,I- and ClO4- and weak acid anions such as F-,NO2-,HCOO-,CH3COO- and HCO3-.For the conductivity enhancement effect in the EIC,it is found that the conductivity of measured for all strong acid anions (Na-anions) was enhanced acording to the theoretical conductivity predicted for H-anions and that of the measured for weak acid anions was suppressed depending on their pKa of H-anions.For the calibration linearity in the EIC,the strong acid anions were linear (r2 =0.99 - 1.00) because the degree of dissociation is almost 1.0 over all the concentration range and that of the weak acid anions was non-linear because the degree of dissociation decreased by increasing the concentration of the weak acid anions.In conclusion,the EIC by enhanced conductivity detection was recognized to be useful only for the strong acid anions in terms of conductivity detection and calibration linearity.

  14. Separation of thorium and uranium in nitric acid solution using silica based anion exchange resin.

    Science.gov (United States)

    Chen, Yanliang; Wei, Yuezhou; He, Linfeng; Tang, Fangdong

    2016-09-30

    To separate thorium and uranium in nitric acid solution using anion exchange process, a strong base silica-based anion exchange resin (SiPyR-N4) was synthesized. Batch experiments were conducted and the separation factor of thorium and uranium in 9M nitric acid was about 10. Ion exchange chromatography was applied to separate thorium and uranium in different ratios. Uranium could be eluted by 9M nitric acid and thorium was eluted by 0.1M nitric acid. It was proved that thorium and uranium can be separated and recovered successfully by this method.

  15. Ion Exchange and Liquid Column Chromatography.

    Science.gov (United States)

    Walton, Harold F.

    1980-01-01

    Emphasizes recent advances in principles and methodology in ion exchange and chromatography. Two tables list representative examples for inorganic ions and organic compounds. Cites 544 references. (CS)

  16. Survey of organic acid eluents for anion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Book, D.E.

    1981-10-01

    Of all the potential eluents surveyed (including aromatic, sulfonic, phosphonic, among other acids), only the carboxylic acids and the nitrophenols are recommended as eluents for anion chromatography. The concentration of the eluent should be in the range 5 x 10/sup -5/ to 1 x 10/sup -3/ M. The eluent should have the same charge as inorganic anions, a higher charge than organic acid samples. Choice of eluents for separation of halides, chloride and sulfate, multivalent inorganic anions, small alkyl acids, and aromatic acids is discussed. (DLC)

  17. Separation of coagulation factor Ⅷ with high activity using gigaporous anion exchange chromatography%超大孔离子交换制备色谱分离纯化高活性凝血因子Ⅷ

    Institute of Scientific and Technical Information of China (English)

    康丽梅; 张焱; 罗坚; 李由; 周月芳; 余蓉; 苏志国

    2012-01-01

    建立了一条从人血浆中分离高活性凝血因子Ⅷ(FⅧ)的纯化工艺.基于FⅧ和介质孔径的尺度比及其对蛋白质活性影响的分析,设计了以超大孔离子交换制备色谱为核心步骤的新型分离纯化工艺.分别进行超大孔离子交换色谱与传统离子交换色谱的条件优化,并对优化工艺所得产品进行了活性检测(底物显色法)和纯度检测(高效凝胶过滤和凝胶电泳).结果表明,超大孔介质结构不但可以有效地保护蛋白质大分子结构,而且能够大幅度地提高制备色谱的传质速率,从而得到具有高凝血活性的FⅧ产品.FⅧ在超大孔制备色谱过程中的回收率(85%)比传统离子交换制备色谱高4~5倍,产品比活高达154 IU/mg.此外,还研究了超大孔介质的再生程序,采用5个柱体积的1mol/L NaOH低流速清洗色谱柱,保证了色谱工艺的稳定性.本纯化工艺步骤简单,重现性好,易于放大生产.%A purification process to obtain coagulation factor Vffl (FVI) with high activity from human plasma was established. Based on the analysis of the size ratio between FVi and matrix porous medium and its effect on the protein activity, a novel purification process designed was superporous ion exchange chromatography (IEC). The operating conditions of gigaporous and traditional anion exchange chromatography were optimized separately. The chromogenic substrate , gel filtration and sodium dodecyl sulfate-polyacrylamide gel electrophoresis ( SDS-PAGE) were used to monitor the bioactivity and purity of the chromatographic products. The results showed that the superporous medium could not only protect structure of macro-protein but also enhance its mass transfer, finally giving FVI product with high activity. The yield of FVM in superporous chromatography was about five times of commercially agarose chromatography and the specific activity was up to 154 IU/mg protein. Furthermore, we studied the regeneration process of

  18. Development and validation of a solid-phase extraction method using anion exchange sorbent for the analysis of cannabinoids in plasma and serum by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gasse, Angela; Pfeiffer, Heidi; Köhler, Helga; Schürenkamp, Jennifer

    2016-07-01

    The aim of this work was to develop and validate a solid-phase extraction (SPE) method for the analysis of cannabinoids with emphasis on a very extensive and effective matrix reduction in order to ensure constant good results in selectivity and sensitivity regardless of the applied measuring technology. This was obtained by the use of an anion exchange sorbent (AXS) and the purposive ionic interaction between matrix components and this sorbent material. In a first step, the neutral cannabinoids ∆9-tetrahydrocannabinol (THC) and 11-hydroxy-∆9-tetrahydrocannabinol (11-OH-THC) were eluted, leaving 11-nor-9-carboxy-∆9-tetrahydrocannabinol (THC-COOH) and the main interfering matrix components bound to the AXS. In a second step, exploiting differences in pH and polarity, it was possible to separate matrix components and THC-COOH, thereby yielding a clean elution of THC-COOH into the same collecting tube as THC and 11-OH-THC. Even when using a simple measuring technology like gas chromatography with single quadrupole mass spectrometry, this two-step elution allows for an obvious decrease in number and intensity of matrix interference in the chromatogram. Hence, in both plasma and serum, the AXS extracts resulted in very good selectivity. Limits of detection and limits of quantification were below 0.25 and 0.35 ng/mL for the neutral cannabinoids in both matrices, 2.0 and 3.0 ng/mL in plasma and 1.6 and 3.3 ng/mL in serum for THC-COOH. The recoveries were ≥79.8 % for all analytes. Interday and intraday imprecisions ranged from 0.8 to 6.1 % relative standard deviation, and accuracy bias ranged from -12.6 to 3.6 %.

  19. Direct determination of glyphosate and its major metabolite, aminomethylphosphonic acid, in fruits and vegetables by mixed-mode hydrophilic interaction/weak anion-exchange liquid chromatography coupled with electrospray tandem mass spectrometry.

    Science.gov (United States)

    Chen, Ming-Xue; Cao, Zhao-Yun; Jiang, Yan; Zhu, Zhi-Wei

    2013-01-11

    A novel method was developed for the direct, sensitive, and rapid determination of glyphosate and its major metabolite, aminomethylphosphonic acid (AMPA), in fruit and vegetable samples by mixed-mode hydrophilic interaction/weak anion-exchange liquid chromatography (HILIC/WAX) coupled with electrospray tandem mass spectrometry (ESI-MS/MS). Homogenized samples were extracted with water, without derivatization or further clean-up, and the extracts were injected directly onto the Asahipak NH2P-50 4E column (250 mm × 4.6 mm i.d., 5 μm). The best results were obtained when the column was operated under mixed-mode HILIC/WAX elution conditions. An initial 10-min washing step with acetonitrile/water (10:90, v/v) in HILIC mode was used to remove potentially interfering compounds, and then the analytes were eluted in WAX mode with acetonitrile and water containing 0.1 molL(-1) ammonium hydroxide under gradient elution for the ESI analysis in negative ion mode. Limits of quantification of glyphosate and AMPA were 5 μgkg(-1) and 50 μgkg(-1), respectively, with limits of detection as low as 1.2 μgkg(-1) for glyphosate and 15 μgkg(-1) for AMPA. The linearity was satisfactory, with correlation coefficients (r)>0.9966. Recovery studies were carried out on spiked matrices (6 vegetables, 3 fruits) with glyphosate at four concentrations and AMPA at three concentrations. The mean recoveries for glyphosate and AMPA were 75.3-110% and 76.1-110%, respectively, with relative standard deviations in the range of 1.1-13.8%. The intra-day precision (n=7) for glyphosate and AMPA in vegetable and fruit samples spiked at an intermediate level between 5.9% and 7.5%, and the inter-day precision over 11 days (n=11) was between 7.0% and 13%.

  20. High-throughput sequential injection method for simultaneous determination of plutonium and neptunium in environmental solids using macroporous anion-exchange chromatography, followed by inductively coupled plasma mass spectrometric detection.

    Science.gov (United States)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per; Miró, Manuel

    2011-01-01

    This paper reports an automated analytical method for rapid and simultaneous determination of plutonium and neptunium in soil, sediment, and seaweed, with detection via inductively coupled plasma mass spectrometry (ICP-MS). A chromatographic column packed with a macroporous anion exchanger (AG MP-1 M) was incorporated in a sequential injection (SI) system for the efficient retrieval of plutonium, along with neptunium, from matrix elements and potential interfering nuclides. The sorption and elution behavior of plutonium and neptunium onto AG MP-1 M resin was compared with a commonly utilized AG 1-gel-type anion exchanger. Experimental results reveal that the pore structure of the anion exchanger plays a pivotal role in ensuring similar separation behavior of plutonium and neptunium along the separation protocol. It is proven that plutonium-242 ((242)Pu) performs well as a tracer for monitoring the chemical yield of neptunium when using AG MP-1 M resin, whereby the difficulties in obtaining a reliable and practicable isotopic neptunium tracer are overcome. An important asset of the SI setup is the feasibility of processing up to 100 g of solid substrates using a small-sized (ca. 2 mL) column with chemical yields of neptunium and plutonium being ≥79%. Analytical results of three certified/standard reference materials and two solid samples from intercomparison exercises are in good agreement with the reference values at the 0.05 significance level. The overall on-column separation can be completed within 3.5 h for 10 g of soil samples. Most importantly, the anion-exchange mini-column suffices to be reused up to 10-fold with satisfactory chemical yields (>70%), as demanded in environmental monitoring and emergency scenarios, making the proposed automated assembly well-suited for unattended and high-throughput analysis.

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

    Science.gov (United States)

    Michalski, Rajmund; Lyko, Aleksandra; Kurzyca, Iwona

    2012-07-01

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

  2. Rejuvenation processes applied to 'poisoned' anion exchangers in uranium processing

    International Nuclear Information System (INIS)

    The removal of 'poisons' from anion exchangers in uranium processing of Canadian radioactive ores is commonly called rejuvenation or regeneration. The cost of the ion exchange recovery of uranium is adversely affected by a decrease in the capacity and efficiency of the anion exchangers, due to their being 'poisoned' by silica, elemental sulphur, molybdenum and tetrathionates. These 'poisons' have a high affinity for the anion exchangers, are adsorbed in preference to the uranyl complex, and do not desorb with the reagents used normally in the uranyl desorption phase. The frequency of rejuvenation and the reagents required for rejuvenation are determined by the severity of the 'poisoning' accumulated by the exchanger in contact with the uranium leach liquor. Caustic soda (NaOH) at approximately equal to 18 cents/lb is commonly used to remove uranium anion exchangers of tetrathionate ((S406)/-/-) 'poisons'. A potential saving in operating cost would be of consequence if other reagents, e.g. sodium carbonate (Na2CO3) at approximately equal to 3.6 cents/lb or calcium hydroxide (Ca(OH)2) at approximately equal to 1.9 cents/lb, were effective in removing (S406)/-/-) from a 'poisoned' exchanger. A rejuvenation process for a test program was adopted after a perusal of the literature

  3. Inorganic anion exchangers for the treatment of radioactive wastes

    International Nuclear Information System (INIS)

    Inorganic anion exchangers are evaluated for Tc, I and S isotope removal from aqueous nuclear waste streams. Chemical, thermal, and radiation stabilities were examined. Selected exchangers were examined in detail for their selectivities, kinetics and mechanism of the sorption process (especially in NO3-, OH- and BO3- environments). Cement encapsulation and leaching experiments were made on the exchangers showing most promise for 'radwaste' treatment. (author)

  4. Anion exchange purification of plasmid DNA using expanded bed adsorption.

    Science.gov (United States)

    Ferreira, G N; Cabral, J M; Prazeres, D M

    2000-01-01

    Recent developments in gene therapy with non-viral vectors and DNA vaccination have increased the demand for large amounts of pharmaceutical-grade plasmid DNA. The high viscosity of process streams is of major concern in the purification of plasmids, since it can cause high back pressures in column operations, thus limiting the throughput. In order to avoid these high back pressures, expanded bed anion exchange chromatography was evaluated as an alternative to fixed bed chromatography. A Streamline 25 column filled with 100 ml of Streamline QXL media, was equilibrated with 0.5 M NaCl in TE (10 mM Tris, 1 mM EDTA, pH = 8.0) buffer at an upward flow of 300 cmh-1, E. coli lysates (obtained from up to 3 liters of fermentation broth) were injected in the column. After washing out the unbound material, the media was allowed to sediment and the plasmid was eluted with 1 M NaCl in TE buffer at a downward flow of 120 cmh-1. Purification factors of 36 +/- 1 fold, 26 +/- 0.4 plasmid purity, and close to 100% yields were obtained when less than one settled column volume of plasmid feed was injected. However, both recovery yield and purity abruptly decreased when larger amounts were processed-values of 35 +/- 2 and 5 +/- 0.7 were obtained for the recovery yield and purity, respectively, when 250 ml of feedstock were processed. In these cases, gel clogging and expansion collapse were observed. The processing of larger volumes, thus larger plasmid quantities, was only possible by performing an isopropanol precipitation step prior to the chromatographic step. This step led to an enhancement of the purification step.

  5. Determination of nitrate by anion exchange with ultraviolet detection

    Energy Technology Data Exchange (ETDEWEB)

    McComas, J.G.

    1976-01-01

    A weak base anion exchange resin is synthesized by surface bonding 3-aminopropyltriethoxysilane to silica gel. This silylated silica gel is used to separate nitrate from interferences. The nitrate is then determined by measuring its absorbance at 220 nm. An interference study was performed and no anions commonly found in potable water interferes. A comparison of this method was made with the brucine method on real samples and satisfactory agreement was obtained between the two methods.

  6. A lanthanide complex for metal encapsulations and anion exchanges.

    Science.gov (United States)

    Sun, Yan-Qiong; Wan, Fang; Li, Xin-Xiong; Lin, Jian; Wu, Tao; Zheng, Shou-Tian; Bu, Xianhui

    2016-08-01

    A cationic lanthanide metalloligand with 3 dangling carboxylate groups on its periphery co-assembles with nitrate into a porous thermochromic solid responsive to both external cations and anions, owing to the presence of exchangeable NO3(-) as well as cation cavities arising from cooperative orientation of free carboxylate groups. An especially interesting feature is the structural memory effect during crystallization exhibited by the metalloligand, even after dissolution and binding to secondary cations (Cu(2+), Cd(2+)…). Moreover, the porous solid can undergo ion-exchange with various anions, leading to tunable thermochromic temperature and color range. PMID:27463609

  7. A new anionic exchange stir bar sorptive extraction coating based on monolithic material for the extraction of inorganic anion.

    Science.gov (United States)

    Huang, Xiaojia; Lin, Jianbing; Yuan, Dongxing

    2010-07-23

    A novel anionic exchange stir bar sorptive extraction (SBSE) coating based on poly(2-(methacryloyloxy)ethyltrimethylammonium chloride-co-divinylbenzene) monolithic material for the extraction of inorganic anion was prepared. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detailed. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to investigate the extraction capacity of the new coating for inorganic anion, the new SBSE was combined with ionic chromatography with conductivity detection, Br-, NO3-, PO4(3-) and SO4(2-) were selected as detected solutes. Several extractive parameters, including pH value and ionic strength in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that strongly ionic strength did not favor the extraction of anlaytes. Under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.92-2.62 and 3.03-9.25 microg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect the two different trademarks of commercial purified water with satisfactory recovery in the range of 70.0-92.6%. To the best of our knowledge, this is the first to use SBSE to enrich inorganic anions. PMID:20576270

  8. Understanding and modeling removal of anionic organic contaminants (AOCs) by anion exchange resins.

    Science.gov (United States)

    Zhang, Huichun; Shields, Anthony J; Jadbabaei, Nastaran; Nelson, Maurice; Pan, Bingjun; Suri, Rominder P S

    2014-07-01

    Ionic organic contaminants (OCs) are a growing concern for water treatment and the environment and are removed inefficiently by many existing technologies. This study examined removal of anionic OCs by anion exchange resins (AXRs) as a promising alternative. Results indicate that two polystyrene AXRs (IRA910 and IRA96) have higher sorption capacities and selectivity than a polyacrylate resin (A860). For the polystyrene resins, selectivity follows: phenolates ≥ aromatic dicarboxylates > aromatic monocarboxylates > benzenesulfonate > aliphatic carboxylates. This trend can be explained based on hydration energy, the number of exchange groups, and aromaticity and hydrophobicity of the nonpolar moiety (NPM) of the anions. For A860, selectivity only varies within a narrow range (0.13-1.64). Despite the importance of the NPM of the anions, neutral solutes were sorbed much less, indicating synergistic combinations of electrostatic and nonelectrostatic interactions in the overall sorption. By conducting multiple linear regression between Abraham's descriptors and nature log of selectivity, induced dipole-related interactions and electrostatic interactions were found to be the most important interaction forces for sorption of the anions, while solute H-bond basicity has a negative effect. A predictive model was then developed for carboxylates and phenolates based on the poly parameter linear free energy relationships established for a diverse range of 16 anions and 5 neutral solutes, and was validated by accurate prediction of sorption of five test solutes within a wide range of equilibrium concentrations and that of benzoate at different pH. PMID:24877792

  9. Magnetic graphitic carbon nitride anion exchanger for specific enrichment of phosphopeptides.

    Science.gov (United States)

    Zhu, Gang-Tian; He, Xiao-Mei; Chen, Xi; Hussain, Dilshad; Ding, Jun; Feng, Yu-Qi

    2016-03-11

    Anion-exchange chromatography (AEX) is one of the chromatography-based methods effectively being used for phosphopeptide enrichment. However, the development of AEX materials with high specificity toward phosphopeptides is still less explored as compared to immobilized metal affinity chromatography (IMAC) or metal oxide affinity chromatography (MOAC). In this work, magnetic graphitic carbon nitride (MCN) was successfully prepared and introduced as a promising AEX candidate for phosphopeptide enrichment. Due to the extremely abundant content of nitrogen with basic functionality on the surface, this material kept excellent retention for phosphopeptides at pH as low as 1.8. Benefiting from the large binding capacity at such low pH, MCN showed remarkable specificity to capture phosphopeptides from tryptic digests of standard protein mixtures as well as nonfat milk and human serum. In addition, MCN was also applied to selective enrichment of phosphopeptides from the tryptic digests of rat brain lysate and 2576 unique phosphopeptides were successfully identified.

  10. Organic resin anion exchangers for the treatment of radioactive wastes

    International Nuclear Information System (INIS)

    Organic anion exchange resins are evaluated for 99-TcO4- (pertechnate) removed from aqueous nuclear waste streams. Chemical, thermal and radiation stabilities were studied. Selected resins were examined in detail for their selectivities in the presence of I-, NO3-, SO4=, CO3=, Cl- and OH-. Ion exchange equilibria and kinetic mechanisms were determined. Preliminary investigations of cement encapsulation in polymer modified form were made and some leach studies carried out. (author)

  11. Reducing nitrogen crossover in microbial reverse-electrodialysis cells by using adjacent anion exchange membranes and anion exchange resin

    KAUST Repository

    Wallack, Maxwell J.

    2015-01-01

    Microbial reverse electrodialysis cells (MRECs) combine power generation from salinity gradient energy using reverse electrodialysis (RED), with power generation from organic matter using a microbial fuel cell. Waste heat can be used to distill ammonium bicarbonate into high (HC) and low salt concentration (LC) solutions for use in the RED stack, but nitrogen crossover into the anode chamber must be minimized to avoid ammonia loses, and foster a healthy microbial community. To reduce nitrogen crossover, an additional low concentration (LC) chamber was inserted before the anode using an additional anion exchange membrane (AEM) next to another AEM, and filled with different amounts of anion or cation ion exchange resins. Addition of the extra AEM increased the ohmic resistance of the test RED stack from 103 Ω cm2 (1 AEM) to 295 Ω cm2 (2 AEMs). However, the use of the anion exchange resin decreased the solution resistance of the LC chamber by 74% (637 Ω cm2, no resin; 166 Ω cm2 with resin). Nitrogen crossover into the anode chamber was reduced by up to 97% using 50% of the chamber filled with an anion exchange resin compared to the control (no additional chamber). The added resistance contributed by the use of the additional LC chamber could be compensated for by using additional LC and HC membrane pairs in the RED stack.

  12. Cholangiocyte anion exchange and biliary bicarbonate excretion

    Institute of Scientific and Technical Information of China (English)

    Jesús M Banales; Jesús Prieto; Juan F Medina

    2006-01-01

    Primary canalicular bile undergoes a process of fluidization and alkalinization along the biliary tract that is influenced by several factors including hormones, innervation/neuropeptides, and biliary constituents. Theexcretion of bicarbonate at both the canaliculi and the bile ducts is an important contributor to the generation of the so-called bile-salt independent flow. Bicarbonate is secreted from hepatocytes and cholangiocytes through parallel mechanisms which involve chloride efflux through activation of Cl- channels, and further bicarbonate secretion via AE2/SLC4A2-mediated Cl-/HCO3-exchange. Glucagon and secretin are two relevant hormones which seem to act very similarly in their target cells (hepatocytes for the former and cholangiocytes for the latter). These hormones interact with their specific G protein-coupled receptors, causing increases in intracellular levels of cAMP and activation of cAMP-dependent Cl- and HCO3- secretory mechanisms. Both hepatocytes and cholangiocytes appear to have cAMP-responsive intracellular vesicles in which AE2/SLC4A2 colocalizes with cell specific Cl- channels (CFTR in cholangiocytes and not yet determined in hepatocytes) and aquaporins (AQP8 in hepatocytes and AQP1 in cholangiocytes). cAMP-induced coordinated trafficking of these vesicles to either canalicular or cholangiocyte lumenal membranes and further exocytosis results in increased osmotic forces and passive movement of water with net bicarbonate-rich hydrocholeresis.

  13. Alkaline Anion-Exchange Membranes Containing Mobile Ion Shuttles.

    Science.gov (United States)

    Ge, Xiaolin; He, Yubin; Guiver, Michael D; Wu, Liang; Ran, Jin; Yang, Zhengjin; Xu, Tongwen

    2016-05-01

    A new class of alkaline anion-exchange membranes containing mobile ion shuttles is developed. It is achieved by threading ionic linear guests into poly(crown ether) hosts via host-guest molecular interaction. The thermal- and pH-triggered shuttling of ionic linear guests remarkably increases the solvation-shell fluctuations in inactive hydrated hydroxide ion complexes (OH(-) (H2 O)4 ) and accelerates the OH(-) transport. PMID:26972938

  14. A Novel Methodology to Synthesize Highly Conductive Anion Exchange Membranes

    OpenAIRE

    Yubin He; Jiefeng Pan; Liang Wu; Yuan Zhu; Xiaolin Ge; Jin Ran; ZhengJin Yang; Tongwen Xu

    2015-01-01

    Alkaline polyelectrolyte fuel cell now receives growing attention as a promising candidate to serve as the next generation energy-generating device by enabling the use of non-precious metal catalysts (silver, cobalt, nickel et al.). However, the development and application of alkaline polyelectrolyte fuel cell is still blocked by the poor hydroxide conductivity of anion exchange membranes. In order to solve this problem, we demonstrate a methodology for the preparation of highly OH− conductiv...

  15. High-performance liquid chromatography - Ultraviolet method for the determination of total specific migration of nine ultraviolet absorbers in food simulants based on 1,1,3,3-Tetramethylguanidine and organic phase anion exchange solid phase extraction to remove glyceride.

    Science.gov (United States)

    Wang, Jianling; Xiao, Xiaofeng; Chen, Tong; Liu, Tingfei; Tao, Huaming; He, Jun

    2016-06-17

    The glyceride in oil food simulant usually causes serious interferences to target analytes and leads to failure of the normal function of the RP-HPLC column. In this work, a convenient HPLC-UV method for the determination of the total specific migration of nine ultraviolet (UV) absorbers in food simulants was developed based on 1,1,3,3-tetramethylguanidine (TMG) and organic phase anion exchange (OPAE) SPE to efficiently remove glyceride in olive oil simulant. In contrast to the normal ion exchange carried out in an aqueous solution or aqueous phase environment, the OPAE SPE was performed in the organic phase environments, and the time-consuming and challenging extraction of the nine UV absorbers from vegetable oil with aqueous solution could be readily omitted. The method was proved to have good linearity (r≥0.99992), precision (intra-day RSD≤3.3%), and accuracy(91.0%≤recoveries≤107%); furthermore, the lower limit of quantifications (0.05-0.2mg/kg) in five types of food simulants(10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol and olive oil) was observed. The method was found to be well suited for quantitative determination of the total specific migration of the nine UV absorbers both in aqueous and vegetable oil simulant according to Commission Regulation (EU) No. 10/2011. Migration levels of the nine UV absorbers were determined in 31 plastic samples, and UV-24, UV-531, HHBP and UV-326 were frequently detected, especially in olive oil simulant for UV-326 in PE samples. In addition, the OPAE SPE procedure was also been applied to efficiently enrich or purify seven antioxidants in olive oil simulant. Results indicate that this procedure will have more extensive applications in the enriching or purification of the extremely weak acidic compounds with phenol hydroxyl group that are relatively stable in TMG n-hexane solution and that can be barely extracted from vegetable oil. PMID:27189432

  16. Multilayer chitosan-based open tubular capillary anion exchange column with integrated monolithic capillary suppressor

    International Nuclear Information System (INIS)

    Highlights: ► Uses a multilayer chitosan–glutaraldehyde coating as anion exchanger. ► Uses a methacrylate-acrylic acid polymer monolith as suppressor. ► Demonstrates first integral suppressor open tubular anion chromatography. - Abstract: We describe a multilayered open tubular anion exchange column fabricated by alternately pumping solutions of chitosan and glutaraldehyde. The column is terminated in an integrally bonded monolithic suppressor cast around a mandrel of a tungsten wire, composed of an acrylic acid (AA)–ethylene dimethacrylate (EDMA) monolith that is made with sufficient porogen for the monolith to function as a membrane. For a 4.5 m long 75 μm bore column coated with 24 successive layers of the condensation polymer (estimated to contain ∼72 molecular layers) and coupled to 1 cm length of a suppressor fabricated with 55–60% AA, effective separation of several common anions (F−, Cl−, NO2−, Br−, NO3−, average number of theoretical plates ∼12,000) and adequate suppression of 1 mM KOH used as eluent was observed at a flow rate of 800 nL min−1 to obtain sub-picomol detection limits at an operating pressure of ∼1 bar. The separation is not time efficient but the system can be meritorious in unique niche applications where a small form factor is desired and liquid volume and power consumption are more important than separation speed.

  17. Optimization of an anion-exchange high performance liquid chromatography-inductively coupled plasma-mass spectrometric method for the speciation analysis of oxyanion-forming metals and metalloids in leachates from cement-based materials.

    Science.gov (United States)

    Mulugeta, Mesay; Wibetoe, Grethe; Engelsen, Christian J; Lund, Walter

    2010-10-01

    A method was developed for the speciation analysis of the oxyanions of As(III), As(V), Cr(VI), Mo(VI), Sb(III), Sb(V), Se(IV), Se(VI) and V(V) in leachates from cement-based materials, based on anion-exchange HPLC coupled with ICP-MS. The method was optimized in a two-step multivariate approach: the effect of sample pH and mobile phase composition on resolution, peak symmetry and analysis time was studied. Optimum conditions were then identified for the significant experimental factors by studying their interdependence. A mobile phase composition of 20 mM ammonium nitrate, 50 mM ammonium tartrate and pH 9.5 was found to be a compromise optimum for the separation of the target analytes using isocratic elution. The optimum condition provided separation of the analytes in less than 6 min, at a mobile phase flow rate of 1.0 mL/min. The signal intensities of the analytes were improved by adding 1% methanol to the mobile phase. The limit of detection of the method was in the range 0.2-2.2 μg/L for the various species. The effect of sample constituents was studied using spiked concrete leachates. The method was used to determine the target oxyanionic species in leachates generated from a concrete material in the pH range 3.5-12.4; CrO(4)(2-), MoO(4)(2-) and VO(4)(3-) were detected in most of the leachates.

  18. Removal of chromium complex dye from aqueous solutions using strongly basic and weakly basic anion exchangers

    OpenAIRE

    Kauspediene, D.; Kazlauskiene E.; Selskiene, A.

    2010-01-01

    Removal of chromium complex dye from aqueous solutions by sorption onto a weakly basic, acrylic matrix anion exchanger Purolite A845 and a strongly basic, polystyrene matrix anion exchanger Purolite A 500P has been investigated under various experimental conditions: the initial dye concentration, pH and temperature. The sorption of chromium complex dye proceeds as a result of miscellaneous interactions between the dye and anion exchanger: ion exchange and physical sorption. The removal effici...

  19. Anion exchange selectivity of surfactant modified clinoptilolite-rich tuff for environmental remediation.

    Science.gov (United States)

    de Gennaro, Bruno; Catalanotti, Lilia; Bowman, Robert S; Mercurio, Mariano

    2014-09-15

    Lately, the functionalization of industrial minerals with high technological properties, such as natural zeolites, is shaping as a promising approach in environmental sphere. In fact, under the specific conditions, the surface functionalization via adsorption of cationic surfactants reverses the surface charge of the mineral, enabling zeolites to simultaneously interact either with organic contaminants or inorganic anions. This aspect allows zeolites to be used in the remediation of contaminated fluids. The present research shed new light on some still not fully understood aspects concerning exchange kinetics such as anion-exchange mechanisms and selectivity of surface modified minerals. For this purpose the mineralogical characterization and the surface properties evaluation (X Ray Powder Diffraction, chemical analysis, thermal analysis, ECEC and AEC) of a clinoptilolite-rich tuff were performed, and the anion exchange isotherms of the sample, modified with hexadecyltrimethylammonium chloride or bromide (HDTMA-Cl/-Br), were determined. Ion-exchange equilibrium data of uni-uni valent reaction were obtained by solutions containing Br(-), Cl(-), NO3(-) or ClO4(-). Liquid phase was analysed via high performance liquid chromatography. Thermodynamic quantities (Ka and ΔG(0)) were determined and compared with the Hofmeister series. The value of the ECEC, calculated in batch conditions, was about 137 mmol/kg, in good agreement with that evaluated in dynamic conditions, while the AEC data were different for the SMNZ-Br and -Cl samples, amounting to 137 and 106 mmol/kg, respectively, thus indicating a different compactness of the bilayer formed in the two cases. Moreover, the anion isotherm results and the mathematical evaluation of the thermodynamic parameters, demonstrated the good affinity of SMNZ-Br towards chloride, nitrate and perchlorate, and of SMNZ-Cl for nitrate and perchlorate, also endorsing the possibility of using the same thermodynamic approach developed to

  20. Anion exchange kinetics of uranium in sulphate media

    International Nuclear Information System (INIS)

    Experiments have shown that the sorption of uranium from acidic sulphate solutions onto strong base-anion exchange resins is particle diffusion controlled in the uranium concentration range 0.0001 to 0.004 M. A simplified diffusion model, based on Fick's Law, fits the kinetic data at each concentration. The rate of sorption falls significantly at lowered solution concentration. This corresponds with a lowered equilibrium loading of uranium and can be predicted with the Nernst-Planck equations using the measured self diffusion coefficient of uranium (1.65 x 10-8 cm2/s) and sulphate ions. The importance of this lowering of uranium sorption on the design of ion exchange equipment is stressed. (author)

  1. Purification of organic acids by chromatography with strong anionic resins: Investigation of uptake mechanisms.

    Science.gov (United States)

    Lemaire, Julien; Blanc, Claire-Line; Lutin, Florence; Théoleyre, Marc-André; Stambouli, Moncef; Pareau, Dominique

    2016-08-01

    Bio-based organic acids are promising renewable carbon sources for the chemical industry. However energy-consuming purification processes are used, like distillation or crystallization, to reach high purities required in some applications. That is why preparative chromatography was studied as an alternative separation technique. In a previous work dealing with the purification of lactic, succinic and citric acids, the Langmuir model was insufficient to explain the elution profiles obtained with a strong anionic resin. Consequently the Langmuir model was coupled with a usual ion-exchange model to take into account the retention of their conjugate bases (acid uptake and ion-exchange selectivity coefficient of conjugate base) and their value were coherent with experimental and resin suppliers' data. These results confirmed that the singular tailing and apparent delay observed with succinic and citric acids can be explained by the high affinity of succinate and citrate for resin cationic sites. The model was implemented in a preparative chromatography simulation program in order to optimize operating parameters of our pilot-scale ISMB unit (Improved Simulated Moving Bed). The comparison with experimental ISMB profiles was conclusive. PMID:27373374

  2. 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.

  3. A Novel Methodology to Synthesize Highly Conductive Anion Exchange Membranes

    Science.gov (United States)

    He, Yubin; Pan, Jiefeng; Wu, Liang; Zhu, Yuan; Ge, Xiaolin; Ran, Jin; Yang, Zhengjin; Xu, Tongwen

    2015-08-01

    Alkaline polyelectrolyte fuel cell now receives growing attention as a promising candidate to serve as the next generation energy-generating device by enabling the use of non-precious metal catalysts (silver, cobalt, nickel et al.). However, the development and application of alkaline polyelectrolyte fuel cell is still blocked by the poor hydroxide conductivity of anion exchange membranes. In order to solve this problem, we demonstrate a methodology for the preparation of highly OH- conductive anion exchange polyelectrolytes with good alkaline tolerance and excellent dimensional stability. Polymer backbones were grafted with flexible aliphatic chains containing two or three quaternized ammonium groups. The highly flexible and hydrophilic multi-functionalized side chains prefer to aggregate together to facilitate the formation of well-defined hydrophilic-hydrophobic microphase separation, which is crucial for the superior OH- conductivity of 69 mS/cm at room temperature. Besides, the as-prepared AEMs also exhibit excellent alkaline tolerance as well as improved dimensional stability due to their carefully designed polymer architecture, which provide new directions to pursue high performance AEMs and are promising to serve as a candidate for fuel cell technology.

  4. Investigation of Polyacrylate Anion-Exchangers for Separation of Rare Earth Element Complexes with EDTA

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The rare earth complexes with EDTA, Ln(edta), show an unusual sequence of affinity for the anion-exchangers. The sorption and chromatographic separation of Y3+ for Nd3+ complexes with EDTA was studied by using the strongly basic gel and macroporous polyacrylate anion-exchangers, Amberlite IRA 458 and Amberlite 958, and the weakly basic gel polyacrylate anion-exchanger, Amberlite IRA-68. The investigations on sorption and separation of rare earth complexes with EDTA on the polyacrylate anion-exchangers applied mainly in the environment protection so far indicate that they can be applied in anionexchange separation of lanthanide complexes with aminopolycarboxylic acids. It was shown that the weakly basic polyacrylate gel anion-exchanger Amberlite IRA-68 is the most effective in purification of Y3+ from Nd3+ in comparison with the strongly basic anion-exchangers of this type.

  5. 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.

  6. Anion-exchangeable inorganic-organic hybrid materials synthesized without using templates

    Institute of Scientific and Technical Information of China (English)

    XU Xianzhu; SONG Jiangwei; LI Defeng; XIAO Fengshou

    2004-01-01

    Inorganic-organic hybrid materials have been obtained at room temperature in aqueous solution without using the templates of surfactants. The materials are care fully characterized by anion-exchange measurement, elements analysis, X-ray diffraction, and infrared spectroscopy. Notably, the anion-exchange capacity of the samples (3.9 Interestingly, both small and large anions could be easily exchanged into the samples due to the plasticity of the sam pies, along with the phase transition.

  7. Optimized anion exchange membranes for vanadium redox flow batteries.

    Science.gov (United States)

    Chen, Dongyang; Hickner, Michael A; Agar, Ertan; Kumbur, E Caglan

    2013-08-14

    In order to understand the properties of low vanadium permeability anion exchange membranes for vanadium redox flow batteries (VRFBs), quaternary ammonium functionalized Radel (QA-Radel) membranes with three ion exchange capacities (IECs) from 1.7 to 2.4 mequiv g(-1) were synthesized and 55-60 μm thick membrane samples were evaluated for their transport properties and in-cell battery performance. The ionic conductivity and vanadium permeability of the membranes were investigated and correlated to the battery performance through measurements of Coulombic efficiency, voltage efficiency and energy efficiency in single cell tests, and capacity fade during cycling. Increasing the IEC of the QA-Radel membranes increased both the ionic conductivity and VO(2+) permeability. The 1.7 mequiv g(-1) IEC QA-Radel had the highest Coulombic efficiency and best cycling capacity maintenance in the VRFB, while the cell's voltage efficiency was limited by the membrane's low ionic conductivity. Increasing the IEC resulted in higher voltage efficiency for the 2.0 and 2.4 mequiv g(-1) samples, but the cells with these membranes displayed reduced Coulombic efficiency and faster capacity fade. The QA-Radel with an IEC of 2.0 mequiv g(-1) had the best balance of ionic conductivity and VO(2+) permeability, achieving a maximum power density of 218 mW cm(-2) which was higher than the maximum power density of a VRFB assembled with a Nafion N212 membrane in our system. While anion exchange membranes are under study for a variety of VRFB applications, this work demonstrates that the material parameters must be optimized to obtain the maximum cell performance. PMID:23799776

  8. Optimized anion exchange membranes for vanadium redox flow batteries.

    Science.gov (United States)

    Chen, Dongyang; Hickner, Michael A; Agar, Ertan; Kumbur, E Caglan

    2013-08-14

    In order to understand the properties of low vanadium permeability anion exchange membranes for vanadium redox flow batteries (VRFBs), quaternary ammonium functionalized Radel (QA-Radel) membranes with three ion exchange capacities (IECs) from 1.7 to 2.4 mequiv g(-1) were synthesized and 55-60 μm thick membrane samples were evaluated for their transport properties and in-cell battery performance. The ionic conductivity and vanadium permeability of the membranes were investigated and correlated to the battery performance through measurements of Coulombic efficiency, voltage efficiency and energy efficiency in single cell tests, and capacity fade during cycling. Increasing the IEC of the QA-Radel membranes increased both the ionic conductivity and VO(2+) permeability. The 1.7 mequiv g(-1) IEC QA-Radel had the highest Coulombic efficiency and best cycling capacity maintenance in the VRFB, while the cell's voltage efficiency was limited by the membrane's low ionic conductivity. Increasing the IEC resulted in higher voltage efficiency for the 2.0 and 2.4 mequiv g(-1) samples, but the cells with these membranes displayed reduced Coulombic efficiency and faster capacity fade. The QA-Radel with an IEC of 2.0 mequiv g(-1) had the best balance of ionic conductivity and VO(2+) permeability, achieving a maximum power density of 218 mW cm(-2) which was higher than the maximum power density of a VRFB assembled with a Nafion N212 membrane in our system. While anion exchange membranes are under study for a variety of VRFB applications, this work demonstrates that the material parameters must be optimized to obtain the maximum cell performance.

  9. Enhanced DOC removal using anion and cation ion exchange resins.

    Science.gov (United States)

    Arias-Paic, Miguel; Cawley, Kaelin M; Byg, Steve; Rosario-Ortiz, Fernando L

    2016-01-01

    Hardness and DOC removal in a single ion exchange unit operation allows for less infrastructure, is advantageous for process operation and depending on the water source, could enhance anion exchange resin removal of dissolved organic carbon (DOC). Simultaneous application of cationic (Plus) and anionic (MIEX) ion exchange resin in a single contact vessel was tested at pilot and bench scales, under multiple regeneration cycles. Hardness removal correlated with theoretical predictions; where measured hardness was between 88 and 98% of the predicted value. Comparing bench scale DOC removal of solely treating water with MIEX compared to Plus and MIEX treated water showed an enhanced DOC removal, where removal was increased from 0.5 to 1.25 mg/L for the simultaneous resin application compared to solely applying MIEX resin. A full scale MIEX treatment plant (14.5 MGD) reduced raw water DOC from 13.7 mg/L to 4.90 mg/L in the treated effluent at a bed volume (BV) treatment rate of 800, where a parallel operation of a simultaneous MIEX and Plus resin pilot (10 gpm) measured effluent DOC concentrations of no greater than 3.4 mg/L, even at bed volumes of treatment 37.5% greater than the full scale plant. MIEX effluent compared to simultaneous Plus and MIEX effluent resulted in differences in fluorescence intensity that correlated to decreases in DOC concentration. The simultaneous treatment of Plus and MIEX resin produced water with predominantly microbial character, indicating the enhanced DOC removal was principally due to increased removal of terrestrially derived organic matter. The addition of Plus resin to a process train with MIEX resin allows for one treatment process to remove both DOC and hardness, where a single brine waste stream can be sent to sewer at a full-scale plant, completely removing lime chemical addition and sludge waste disposal for precipitative softening processes. PMID:26624231

  10. Reillex/trademark/ HPQ: A new, macroporous polyvinylpyridine resin for separating plutonium using nitrate anion exchange

    International Nuclear Information System (INIS)

    Anion exchange in nitric acid is the major aqueous process used to recover and purify plutonium from impure scrap materials. Most strong-base anion exchange resins incorporate a styrene-divinylbenzene copolymer. A newly available, macroporous anion exchange resin based on a copolymer of 1-methyl-4-vinylpyridine and divinylbenzene has been evaluated. Comparative data for Pu(IV) sorption kinetics and capacity are presented for this new resin and two other commonly used anion exchange resins. The new resin offers high capacity and rapid sorption kinetics for Pu(IV) from nitric acid, as well as greater stability to chemical and radiolytic degradation. 8 refs., 12 figs

  11. Performance of selected anion exchange resins for the treatment of a high DOC content surface water.

    Science.gov (United States)

    Humbert, Hugues; Gallard, Hervé; Suty, Hervé; Croué, Jean-Philippe

    2005-05-01

    The objective of this study was first to compare the performance of four strong anion exchange resins (AERs) (MIEX from Orica Pty Ltd, DOWEX-11 and DOWEX-MSA from DOW chemical and IRA-938 from Rohm and Haas) for their application in drinking water treatment (natural organic matter (NOM), mineral anions (nitrate, sulfate and bromide) and pesticide removal) using bench-scale experimental procedures on a high DOC content surface water. The efficiency of MIEX for NOM and mineral anions removal was furthermore evaluated using bench-scale dose-response experiments on raw, clarified and post-ozonated waters. NOM removal was assessed using the measurement of dissolved organic carbon (DOC), UV absorbance at 254 nm (UV254) and the use of high-performance size exclusion chromatography with UV (HPSEC/UV) and fluorescence detection (HPSEC/FLUO). The MIEX and IRA938 anionic resins exhibit a faster removal of NOM and mineral anions compared to the DOWEX11 and MSA AERs. All the resins were found to be very effective with similar performances after 30 to 45 min of contact time. As expected, only limited sorption of atrazine and isoproturon (C0=1 microg/L) occurred with MIEX, DOWEX11 and MSA AERs. MIEX resin proved to be very efficient in eliminating NOM of high-molecular weight but also a large part of the smallest UV absorbing organic compounds which were refractory to coagulation/flocculation treatment. Remaining DOC levels after 30 min of contact with MIEX were found similar in raw water, clarified water and even post-ozonated water implying no DOC benefit can be gained by employing conventional treatment prior to MIEX treatment. Removal of bromide (initial concentration 110 microg/L) was also observed and ranged from 30% to 65% for resin dose increasing from 2 to 8 mL/L. T PMID:15899268

  12. Alkaline direct alcohol fuel cells using an anion exchange membrane

    Energy Technology Data Exchange (ETDEWEB)

    Matsuoka, Koji; Iriyama, Yasutoshi; Abe, Takeshi; Ogumi, Zempachi [Department of Energy and Hydrocarbon Chemistry, Graduate School of Engineering, Kyoto University, Katsura, Nishikyo-ku, Kyoto 615-8510 (Japan); Matsuoka, Masao [Faculty of Science and Engineering, Ritsumeikan University, Kusatsu, Shiga 525-8577 (Japan)

    2005-10-04

    Alkaline direct alcohol fuel cells using an OH-form anion exchange membrane and polyhydric alcohols were studied. A high open circuit voltage of ca. 800mV was obtained for a cell using Pt-Ru/C (anode) and Pt/C (cathode) at 323K, which was about 100-200mV higher than that for a DMFC using Nafion{sup R}. The maximum power densities were in the order of ethylene glycol>glycerol>methanol>erythritol>xylitol. Silver catalysts were used as a cathode catalyst to fabricate alkaline fuel cells, since silver catalyst is almost inactive in the oxidation of polyhydric alcohols. Alkaline direct ethylene glycol fuel cells using silver as a cathode catalyst gave excellent performance because higher concentrations of fuel could be supplied to the anode. (author)

  13. 3D Printing of Micropatterned Anion Exchange Membranes.

    Science.gov (United States)

    Seo, Jiho; Kushner, Douglas I; Hickner, Michael A

    2016-07-01

    Micropatterned anion exchange membranes (AEMs) have been 3D printed via a photoinitiated free radical polymerization and quaternization process. The photocurable formulation, consisting of diurethane dimethacrylate (DUDA), poly(ethylene glycol) diacrylate (PEGDA), dipentaerythritol penta-/hexa- acrylate, and 4-vinylbenzyl chloride (VBC), was directly cured into patterned films using a custom 3D photolithographic printing process similar to stereolithography. Measurements of water uptake, permselectivity, and ionic resistance were conducted on the quaternized poly(DUDA-co-PEGDA-co-VBC) sample series to determine their suitability as ion exchange membranes. The water uptake of the polymers increased as the ion exchange capacity (IEC) increased due to greater quaternized VBC content. Samples with IEC values between 0.98 to 1.63 mequiv/g were synthesized by varying the VBC content from 15 to 25 wt %. The water uptake was sensitive to the PEGDA content in the network resulting in water uptake values ranging from 85 to 410 wt % by varying the PEGDA fractions from 0 to 60 wt %. The permselectivity of the AEM samples decreased from 0.91 (168 wt %, 1.63 mequiv/g) to 0.85 (410 wt %, 1.63 mequiv/g) with increasing water uptake and to 0.88 (162 wt %, 0.98 mequiv/g) with decreasing IEC. Permselectivity results were relatively consistent with the general understanding of the correlation between permselectivity, water uptake, and ion content of the membrane. Lastly, it was revealed that the ionic resistance of patterned membranes was lower than that of flat membranes with the same material volume or equivalent thickness. A parallel resistance model was used to explain the influence of patterning on the overall measured ionic resistance. This model may provide a way to maximize ion exchange membrane performance by optimizing surface patterns without chemical modification to the membrane. PMID:27218137

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

    Science.gov (United States)

    Johnson, Brian J.

    2014-01-01

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

  15. Hydroxide Solvation and Transport in Anion Exchange Membranes

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Chen [Univ. of Chicago, IL (United States); Wuhan Univ. (China); Tse, Ying-Lung Steve [Univ. of Chicago, IL (United States); Lindberg, Gerrick E. [Northern Arizona Univ., Flagstaff, AZ (United States); Knight, Chris [Argonne National Lab. (ANL), Argonne, IL (United States); Voth, Gregory A. [Univ. of Chicago, IL (United States)

    2016-01-27

    Understanding hydroxide solvation and transport in anion exchange membranes (AEMs) can provide important insight into the design principles of these new membranes. To accurately model hydroxide solvation and transport, we developed a new multiscale reactive molecular dynamics model for hydroxide in aqueous solution, which was then subsequently modified for an AEM material. With this model, we investigated the hydroxide solvation structure and transport mechanism in the membrane. We found that a relatively even separation of the rigid side chains produces a continuous overlapping region for hydroxide transport that is made up of the first hydration shell of the tethered cationic groups. Our results show that hydroxide has a significant preference for this overlapping region, transporting through it and between the AEM side chains with substantial contributions from both vehicular (standard diffusion) and Grotthuss (proton hopping) mechanisms. Comparison of the AEM with common proton exchange membranes (PEMs) showed that the excess charge is less delocalized in the AEM than the PEMs, which is correlated with a higher free energy barrier for proton transfer reactions. The vehicular mechanism also contributes considerably more than the Grotthuss mechanism for hydroxide transport in the AEM, while our previous studies of PEM systems showed a larger contribution from the Grotthuss mechanism than the vehicular mechanism for proton transport. The activation energy barrier for hydroxide diffusion in the AEM is greater than that for proton diffusion in PEMs, implying a more significant enhancement of ion transport in the AEM at elevated temperatures.

  16. Gamma radiation effect on gas production in anion exchange resins

    International Nuclear Information System (INIS)

    Radiation-induced decomposition of Amberlite IRA400 anion exchange resin in hydroxide form by gamma radiolysis has been studied at various doses in different atmospheres (anaerobic, anaerobic with liquid water, and aerobic). The effect of these parameters on the degradation of ion exchange resins is rarely investigated in the literature. We focused on the radiolysis gases produced by resin degradation. When the resin was irradiated under anaerobic conditions with liquid water, the liquid phase over the resin was also analyzed to identify any possible water-soluble products released by degradation of the resin. The main products released are trimethylamine (TMA), molecular hydrogen (H2g) and carbon dioxide (CO2g). TMA and H2g are produced in all the irradiation atmospheres. However, TMA was in gaseous form under anaerobic and aerobic conditions and in aqueous form in presence of liquid water. In the latter conditions, TMAaq was associated with aqueous dimethylamine (DMAaq), monomethylamine (MMAaq) and ammonia (NH4+aq). CO2g is formed in the presence of oxygen due to oxidation of organic compounds present in the system, in particular the degradation products such as TMAg

  17. Determination of arsenate in water by anion selective membrane electrode using polyurethane–silica gel fibrous anion exchanger composite

    Energy Technology Data Exchange (ETDEWEB)

    Khan, Asif Ali, E-mail: asifkhan42003@yahoo.com; Shaheen, Shakeeba, E-mail: shakeebashaheen@ymail.com

    2014-01-15

    Highlights: • PU–Si gel is new anion exchanger material synthesized and characterized. • This material used as anion exchange membrane is applied for electroanalytical studies. • The method for detection and determination of AsO{sub 4}{sup 3−} in traces amounts discussed. • The results are also verified from arsenic analyzer. -- Abstract: Polyurethane (PU)–silica (Si gel) based fibrous anion exchanger composites were prepared by solid–gel polymerization of polyurethane in the presence of different amounts of silica gel. The formation of PU–Si gel fibrous anion exchanger composite was characterized by Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTA), scanning electron microscopy (SEM) and elemental analysis. The membrane having a composition of 5:3 (PU:Si gel) shows best results for water content, porosity, thickness and swelling. Our studies show that the present ion selective membrane electrode is selective for arsenic, having detection limit (1 × 10{sup −8} M to 1 × 10{sup −1} M), response time (45 s) and working pH range (5–8). The selectivity coefficient values for interfering ions indicate good selectivity for arsenate (AsO{sub 4}{sup 3−}) over interfering anions. The accuracy of the detection limit results was compared by PCA-Arsenomat.

  18. Analysis of anions in geological brines using ion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Merrill, R.M.

    1985-03-01

    Ion chromatographic procedures for the determination of the anions bromide, sulfate, nitrite, nitrate, phosphate, and iodide in brine samples have been developed and are described. The techniques have been applied to the analysis of natural brines, and geologic evaporites. Sample matrices varied over a range from 15,000 mg/L to 200,000 mg/L total halogens, nearly all of which is chloride. The analyzed anion concentrations ranged from less than 5 mg/L in the cases of nitrite, nitrate, and phosphate, to 20,000 mg/L in the case of sulfate. A technique for suppressing chloride and sulfate ions to facilitate the analysis of lower concentration anions is presented. Analysis times are typically less than 20 minutes for each procedure and the ion chromatographic results compare well with those obtained using more time consuming classical chemical analyses. 10 references, 14 figures.

  19. [Determination of organic acids and inorganic anions by gradient ion chromatography].

    Science.gov (United States)

    Liu, Z; Liu, K; Shen, D; Song, Q; Mou, S; Feng, Y

    1997-07-01

    The chromatographic conditions for separation and detection of organic acids and inorganic anions by gradient ion chromatography with suppressed conductivity detection were studied. The optimized gradient programs were established. Ion chromatography were performed with a DX-100 chromatograph (DIONEX). The separation column is IonPac-AS11. Compared with NaHCO3/Na2CO3 and Na2B4O7, NaOH was the optimal eluent. The effect of organic modifier was also studied. Among methanol, 2-propanol and acetonitrile, methanol can make ion pairs such as malate and succinate, malonate and tartrate gaining baseline resolution. By using ion exchange separation, Cl-, NO3-, malate, succinate, malonate, tartrate, SO4(2-), oxalate were eluted between 5 mmol/L NaOH-16% CH3OH and 10 mmol/L NaOH-16% CH3OH in 25 min. A mobile phase composed of 30 mmol/L NaOH, 50% CH3OH and D.I. water was chosen to elute two groups of organic acids and inorganic anions: (1) quinate, formate, Cl-, malate, malonate, oxalate, citrate, isocitrate, aconitate; (2) lactate, Cl-, SO4(2-), tartrate, PO4(3-), citrate, isocitrate, aconitate. The detection limits (S/N = 3) were 0.1625 (quinate), 0.0691 (formate), 0.0115 (Cl-), 0.0886 (malate), 0.0591 (malonate), 0.0263 (oxalate), 0.1147 (citrate), 0.2017 (isocitrate), 0.3656 (cis-aconitate), 0.1045 (trans-aconitate), 0.1950 (lactate), 0.0729 (tartrate), 0.0224 (SO4(2-)) and 0.0692 (PO4(3-)) mg/L. The relative standard deviations were lower than 11.9% (n = 7) and the correlation coefficients ranged from 0.9212 for Cl- to 0.9999 for formate. The method was applied to determine the organic acids and inorganic anions of beverages and citric acids fermenting-medium. The results were satisfactory.

  20. Preparation of anion exchange membrane using polyvinyl chloride (PVC) for alkaline water electrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, Gab-Jin; Bong, Soo-Yeon; Ryu, Cheol-Hwi [Hoseo University, Asan (Korea, Republic of); Lim, Soo-Gon [Energy and Machinery Korea Co., Ltd., Changwon (Korea, Republic of); Choi, Ho-Sang [Kyungil University, Gyeongsan (Korea, Republic of)

    2015-09-15

    An anion exchange membrane was prepared by the chloromethylation and the amination of polyvinyl chloride (PVC), as the base polymer. The membrane properties of the prepared anion exchange membrane, including ionic conductivity, ion exchange capacity, and water content were measured. The ionic conductivity of the prepared anion exchange membrane was in the range of 0.098x10{sup -2} -7.0x10{sup -2}S cm{sup -1}. The ranges of ion exchange capacity and water content were 1.9-3.7meq./g-dry-membrane and 35.1-63.1%, respectively. The chemical stability of the prepared anion exchange membrane was tested by soaking in 30 wt% KOH solution to determine its availability as a separator in the alkaline water electrolysis. The ionic conductivity during the chemical stability test largely did not change.

  1. Sorption of Pu(IV) from nitric acid by bifunctional anion-exchange resins

    International Nuclear Information System (INIS)

    Anion exchange is attractive for separating plutonium because the Pu(IV) nitrate complex is very strongly sorbed and few other metal ions form competing anionic nitrate complexes. The major disadvantage of this process has been the unusually slow rate at which the Pu(IV) nitrate complex is sorbed by the resin. The paper summarizes the concept of bifunctional anion-exchange resins, proposed mechanism for Pu(IV) sorption, synthesis of the alkylating agent, calculation of Kd values from Pu(IV) sorption results, and conclusions from the study of Pu(IV) sorption from 7M nitric acid by macroporous anion-exchange resins including level of crosslinking, level of alkylation, length of spacer, and bifunctional vs. monofunctional anion-exchange resins

  2. Anion-exchange separations of metal ions in thiocyanate media.

    Science.gov (United States)

    Fritz, J S; Kaminski, E E

    1971-05-01

    The analytical potential of a weak-base macroreticular anion-exchange resin for the quantitative separation of metal ions in thiocyanate media is investigated and demonstrated. Distribution data are given for the sorption of some 25 metal ions from aqueous mixtures of potassium thiocyanate (1.0M or less) and 0.5M hydrochloric acid. The magnitude of the distribution data suggests many possible separations, some of which were quantitatively performed by procedures which are fast, simple and require only mild conditions. Representative separations are removal of traces of iron(III) and copper(II) from water samples prior to the determination of water hardness (calcium and magnesium), separation of nickel(II) from vanadium(IV) and the separation of thorium(IV) from titanium(IV). Some multicomponent separations are the separation of rare earths(III) and thorium(IV) from scandium(III) and the separation of rare earths(III) from iron(III) and uranium(VI). PMID:18960914

  3. Highly conductive side chain block copolymer anion exchange membranes.

    Science.gov (United States)

    Wang, Lizhu; Hickner, Michael A

    2016-06-28

    Block copolymers based on poly(styrene) having pendent trimethyl styrenylbutyl ammonium (with four carbon ring-ionic group alkyl linkers) or benzyltrimethyl ammonium groups with a methylene bridge between the ring and ionic group were synthesized by reversible addition-fragmentation radical (RAFT) polymerization as anion exchange membranes (AEMs). The C4 side chain polymer showed a 17% increase in Cl(-) conductivity of 33.7 mS cm(-1) compared to the benzyltrimethyl ammonium sample (28.9 mS cm(-1)) under the same conditions (IEC = 3.20 meq. g(-1), hydration number, λ = ∼7.0, cast from DMF/1-propanol (v/v = 3 : 1), relative humidity = 95%). As confirmed by small angle X-ray scattering (SAXS), the side chain block copolymers with tethered ammonium cations showed well-defined lamellar morphologies and a significant reduction in interdomain spacing compared to benzyltrimethyl ammonium containing block copolymers. The chemical stabilities of the block copolymers were evaluated under severe, accelerated conditions, and degradation was observed by (1)H NMR. The block copolymer with C4 side chain trimethyl styrenylbutyl ammonium motifs displayed slightly improved stability compared to that of a benzyltrimethyl ammonium-based AEM at 80 °C in 1 M NaOD aqueous solution for 30 days. PMID:27216558

  4. Detection of anionic energetic material residues in enhanced fingermarks on porous and non-porous surfaces using ion chromatography.

    Science.gov (United States)

    Love, Catherine; Gilchrist, Elizabeth; Smith, Norman; Barron, Leon

    2013-09-10

    The ability to link criminal activity and identity using validated analytical approaches can be of great value to forensic scientists. Herein, the factors affecting the recovery and detection of inorganic and organic energetic material residues within chemically or physically enhanced fingermarks on paper and glass substrates are presented using micro-bore anion exchange chromatography with suppressed conductivity detection. Fingermarks on both surfaces were enhanced using aluminium powder or ninhydrin after spiking with model test mixtures or through contact with black-powder substitutes. A quantitative study of the effects of environmental/method interferences, the sweat matrix, the surface and the enhancement technique on the relative anion recovery of forensically relevant species is presented. It is shown that the analytical method could detect target analytes at the nanogram level even within excesses of enhancement reagents and their reaction products when using solid phase extraction and/or microfiltration. To our knowledge, this work demonstrates for the first time that ion chromatography can detect anions in energetic materials within fingermarks on two very different surfaces, after operational enhancement techniques commonly used by forensic scientists and police have been applied.

  5. High throughput determination of cleaning solutions to prevent the fouling of an anion exchange resin.

    Science.gov (United States)

    Elich, Thomas; Iskra, Timothy; Daniels, William; Morrison, Christopher J

    2016-06-01

    Effective cleaning of chromatography resin is required to prevent fouling and maximize the number of processing cycles which can be achieved. Optimization of resin cleaning procedures, however, can lead to prohibitive material, labor, and time requirements, even when using milliliter scale chromatography columns. In this work, high throughput (HT) techniques were used to evaluate cleaning agents for a monoclonal antibody (mAb) polishing step utilizing Fractogel(®) EMD TMAE HiCap (M) anion exchange (AEX) resin. For this particular mAb feed stream, the AEX resin could not be fully restored with traditional NaCl and NaOH cleaning solutions, resulting in a loss of impurity capacity with resin cycling. Miniaturized microliter scale chromatography columns and an automated liquid handling system (LHS) were employed to evaluate various experimental cleaning conditions. Cleaning agents were monitored for their ability to maintain resin impurity capacity over multiple processing cycles by analyzing the flowthrough material for turbidity and high molecular weight (HMW) content. HT experiments indicated that a 167 mM acetic acid strip solution followed by a 0.5 M NaOH, 2 M NaCl sanitization provided approximately 90% cleaning improvement over solutions containing solely NaCl and/or NaOH. Results from the microliter scale HT experiments were confirmed in subsequent evaluations at the milliliter scale. These results identify cleaning agents which may restore resin performance for applications involving fouling species in ion exchange systems. In addition, this work demonstrates the use of miniaturized columns operated with an automated LHS for HT evaluation of chromatographic cleaning procedures, effectively decreasing material requirements while simultaneously increasing throughput. Biotechnol. Bioeng. 2016;113: 1251-1259. © 2015 Wiley Periodicals, Inc. PMID:26552005

  6. Ionic Resistance and Permselectivity Tradeoffs in Anion Exchange Membranes

    KAUST Repository

    Geise, Geoffrey M.

    2013-10-23

    Salinity gradient energy technologies, such as reverse electrodialysis (RED) and capacitive mixing based on Donnan potential (Capmix CDP), could help address the global need for noncarbon-based energy. Anion exchange membranes (AEMs) are a key component in these systems, and improved AEMs are needed in order to optimize and extend salinity gradient energy technologies. We measured ionic resistance and permselectivity properties of quaternary ammonium-functionalized AEMs based on poly(sulfone) and poly(phenylene oxide) polymer backbones and developed structure-property relationships between the transport properties and the water content and fixed charge concentration of the membranes. Ion transport and ion exclusion properties depend on the volume fraction of water in the polymer membrane, and the chemical nature of the polymer itself can influence fine-tuning of the transport properties to obtain membranes with other useful properties, such as chemical and dimensional stability. The ionic resistance of the AEMs considered in this study decreased by more than 3 orders of magnitude (i.e., from 3900 to 1.6 Ω m) and the permselectivity decreased by 6% (i.e., from 0.91 to 0.85) as the volume fraction of water in the polymer was varied by a factor of 3.8 (i.e., from 0.1 to 0.38). Water content was used to rationalize a tradeoff relationship between the permselectivity and ionic resistance of these AEMs whereby polymers with higher water content tend to have lower ionic resistance and lower permselectivity. The correlation of ion transport properties with water volume fraction and fixed charge concentration is discussed with emphasis on the importance of considering water volume fraction when interpreting ion transport data. © 2013 American Chemical Society.

  7. Anion exchange resin as support for invertase immobilization

    Directory of Open Access Journals (Sweden)

    M. Vitolo

    2009-01-01

    Full Text Available

    The invertase (EC 3.2.1.26 from Saccharomyces cerevisiae was employed as a model enzyme in the evaluation of the adsorption capacity of DOWEX-1X8-50®, a basic anion exchange resin, when used as support in enzyme immobilization. By mixing 100mg of resin with 27mg of invertase (pI = 4.0 in buffer solution (pH 4.6, 25°C, stirred at 100rpm, an adsorption of 93% was achieved. The activities (1U = amount of enzyme forming 1mg reducing sugars/min of soluble and insoluble invertase were 0.084 U/mgE and 0.075 U/mgE, respectively, giving an immobilization coefficient of 90.4%. The immobilized invertase had a higher thermal stability than the soluble form. The highest activity was observed at pH 4.5 in both forms of the enzyme, whereas the pH stability ranges for soluble and insoluble invertase were 3.5-5.0 and 4.5-5.5, respectively. The kinetic constants for soluble invertase were KM = 18.3 mM and Vmax = 0.084 U/mgE, and for the insoluble form, KM = 29.1 mM and Vmax = 0.075 U/mgE. The resin tested adsorbed the invertase very well, provided the enzyme molecule had a net negative charge, i.e., the immobilization and reaction procedures had to be carried out at pH > pI. Keywords: Invertase, immobilization, adsorption, anionexchange resin.

  8. Nanostructure-controlled anion exchange membranes for fuel cell applications by high-energy heavy-ion irradiation. Preparation and characterization of anion exchange membranes

    International Nuclear Information System (INIS)

    Heavy ions at kinetic energies typically from several hundreds of MeV to a few GeV passing through a polymer substrate induce a continuous trail of excitations and ionizations called latent tracks. We used a direct ion-track grafting method for preparation of anion exchange membranes for fuel cells. The functional anion exchange groups were introduced inside the latent tracks, thereby achieving OH--conductive channels through the thickness. These straight channels increased conductivities, while the isolated cylindrical structure of tracks restricted the water uptake. (author)

  9. Determination of phytate in high molecular weight, charged organic matrices by two-dimensional size exclusion-ion chromatography

    Science.gov (United States)

    A two-dimensional chromatography method for analyzing anionic targets (specifically phytate) in complex matrices is described. Prior to quantification by anion exchange chromatography, the sample matrix was prepared by size exclusion chromatography, which removed the majority of matrix complexities....

  10. Test procedure for cation exchange chromatography

    International Nuclear Information System (INIS)

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

  11. Ion Exchange Chromatography and Spectrophotometry: An Introductory Undergraduate Laboratory Experiment.

    Science.gov (United States)

    Foster, N.; And Others

    1985-01-01

    Describes an experiment in which students use ion exchange chromatography to separate a mixture of chloro complexes of transition metal ions and then use spectrophotometry to define qualitatively the efficiency of the ion exchange columns. Background information, materials needed, and procedures used are included. (JN)

  12. Separation of whey proteins for chromatography liquid

    OpenAIRE

    Abraham D. Giraldo Zuñiga; Edwin E.García Rojas; Coimbra, Jane S. R.; Wilmer E. Luera Peña

    2010-01-01

    This paper describes and compares three chromatographic methods for the analysis and quantification of most abundant proteins in cheese whey, -lactalbumin and -lactoglobulin. The methods were: Reverse-phase high performance liquid chromatography, anion Exchange chromatography and size-exclusion chromatography. The reverse- phase liquid chromatography led to a better separation of whey proteins than size-exclusion chromatography and anion exchange chromatography, this method offered an ex...

  13. Determination of polysaccharide content in Haemophilus influenzae type b conjugate vaccines by high performance anion exchange chromatography-pulsed amperometric detector%高效阴离子交换色谱-脉冲安培法测定b型流感嗜血杆菌结合疫苗的多糖含量

    Institute of Scientific and Technical Information of China (English)

    贺鹏飞; 唐静; 李亚南; 李茂光; 叶强

    2013-01-01

    Objective To determine the polyribosylribitol phosphate (PRP) content in Haemophilus influenzae type b conjugate vaccine by high performance anion exchange chromatography-pulsed amperometric detector (HPAEC-PAD).Methods The PRP in test samples of Hib conjugate vaccine or isolated free polysaccharide was hydrolyzed with 0.3 mol/L sodium hydroxide at room temperature in oscillation for (16 ± 8) h,then separated by CarboPac(@) PA-10 anion exchange column,eluted by sodium hydroxide/sodium acetate gradient elution,detected by pulsed amperometric detector,and calculated according to the peak area of test samples.The samples were tested for 2 times,and the relative standard deviation (RSD) of test results was calculated.Meanwhile,the PRP content in test sample or free PRP content of the same batch of vaccine were determined by orcinol method in the appendix of Chinese Pharmacopoeia (Volume Ⅲ,2010 edition),and the result was compared with that by HPAEC-PAD.Results The RSD between 2 test results of the same sample was not more than 4.6%.The total PRP contents in samples S01~S03 determined by HPAEC-PAD were 105%,104% and 106%,while the free PRP contents were 126%,109% and 115% of those by orcinol method,respectively.Conclusion HPAEC-PAD method showed high sensitivity,reproducibility and separation effectiveness for PRP content in Hib conjugate vaccine,by which the samples needed no derivation,and multiple components were determined at the same time,therefore may be used as an alternative method of traditional orcinol method for deter-mination of PRP content in Hib conjugate vaccine.%目的 采用高效阴离子交换色谱-脉冲安培检测法(high performance anion exchange chromatography withpulsed amperometric detector,HPAEC-PAD)测定b型流感嗜血杆菌(haemophilus influenzae type b,Hib)结合疫苗的多聚磷酸核糖基核糖醇(polyribosylribitol phosphate,PRP)多糖含量.方法 用终浓度为0.3N的NaOH溶液将待测疫苗中的PRP多糖

  14. Anion-Exchange Properties of Trifluoroacetate and Triflate Salts of N-Alkylammonium Resorcinarenes.

    Science.gov (United States)

    Pan, Fangfang; Beyeh, Ngong Kodiah; Bertella, Stefania; Rissanen, Kari

    2016-03-01

    The synthesis of N-benzyl- and N-cyclohexylammonium resorcinarene trifluoroacetate (TFA) and triflate (OTf) salt receptors was investigated. Solid-state analysis by single-crystal X-ray diffraction revealed that the N-alkylammonium resorcinarene salts (NARSs) with different upper substituents had different cavity sizes and different affinities for anions. Anion-exchange experiments by mixing equimolar amounts of N-benzylammonium resorcinarene trifluoroacetate and N-cyclohexylammonium resorcinarene triflate, as well as N-benzylammonium resorcinarene triflate and N-cyclohexylammonium resorcinarene trifluoroacetate showed that the NARS with flexible benzyl groups preferred the larger OTf anion, whereas the rigid cyclohexyl groups preferred the smaller TFA anions. The anion-exchange processes were confirmed in the solid state by single-crystal and powder X-ray diffraction experiments and in the gas phase by electrospray ionization mass spectrometry. PMID:26749383

  15. Preparation of high-capacity, weak anion-exchange membranes by surface-initiated atom transfer radical polymerization of poly(glycidyl methacrylate) and subsequent derivatization with diethylamine

    Science.gov (United States)

    Qian, Xiaolei; Fan, Hua; Wang, Chaozhan; Wei, Yinmao

    2013-04-01

    Ion-exchange membrane is of importance for the development of membrane chromatography. In this work, a high-capacity anion-exchange membrane was prepared by grafting of glycidyl methacrylate (GMA) onto the surface of regenerated cellulose (RC) membranes via surface-initiated atom transfer radical polymerization (SI-ATRP) and subsequent derivatization with diethylamine. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) were used to characterize changes in the chemical functionality, surface topography and pore morphology of the modified membranes. The static capacity of the prepared anion-exchange membrane was evaluated with bovine serum albumin (BSA) as a model protein. The results indicated that the anion-exchange membrane which could reach a maximum capacity of 96 mg/mL for static adsorption possesses a higher adsorption capacity, and the adsorption capacity increases with the polymerization time. The effect of pH and salt concentration confirmed that the adsorption of BSA followed ion-exchange mechanism. The established method would have potential application in the preparation of anion-exchange membrane.

  16. ZEOLITE PERFORMANCE AS AN ANION EXCHANGER FOR ARSENIC SEQUESTRATION IN WATER

    Science.gov (United States)

    Zeolites are well known for their use in ion exchange and acid catalysis reactions. The use of zeolites in anion or ligand exchange reactions is less studied. The NH4+ form of zeolite Y (NY6, Faujasite) has been tested in this work to evaluate its performance for arsenic removal...

  17. Grafting glycidyl methacrylate to Sepharose gel for fabricating high-capacity protein anion exchangers.

    Science.gov (United States)

    Wang, Qianqian; Yu, Linling; Sun, Yan

    2016-04-22

    To develop ion exchangers of high protein adsorption capacity, we have herein introduced atom transfer radical polymerization (ATRP) method to graft glycidyl methacrylate (GMA) onto Sepharose FF gel. GMA-grafted Sepharose FF resins of four grafting densities and different grafting chain lengths were obtained by adjusting reaction conditions. The epoxy groups on the grafted chains were functionalized by modification with diethylamine (DEA), leading to the fabrication of Sepharose-based anion exchangers of 14 different grafting densities and/or grafting chain lengths. The resins were first characterized for the effects of grafting density, chain length and ionic strength on pore sizes by inverse size exclusion chromatography. Then, the resins were evaluated by adsorption equilibria of bovine serum albumin (BSA) as a function of ionic capacity (IC) (chain length) at individual grafting densities. It was observed that at each grafting density there was a specific IC value (chain length) that offered the maximum equilibrium capacity. Of the resins with maximum values at individual grafting densities, the resin of the second grafting density with an IC value of 330 mmol/L (denoted as FF-Br2-pG-D330) showed the highest capacity, 264 mg/mL, about two times higher than that of the traditional ungrafted resin Q Sepharose FF (137 mg/mL). This resin also showed the most favorable uptake kinetics among the resins of similar IC values but different grafting densities, or of the same grafting density but different IC values. Effects of ionic strength showed that the capacities of FF-Br2-pG-D330 were much higher than Q Sepharose FF at a wide range of NaCl concentrations (0-200 mmol/L), and the uptake rates of the two resins were similar in the ionic strength range. Therefore, the dynamic binding capacity values of BSA on FF-Br2-pG-D330 were much higher than Q Sepharose FF as demonstrated at different residence times and ionic strengths. Taken together, the research has proved the

  18. Rapid exchange between atmospheric CO2 and carbonate anion intercalated within magnesium rich layered double hydroxide.

    Science.gov (United States)

    Sahoo, Pathik; Ishihara, Shinsuke; Yamada, Kazuhiko; Deguchi, Kenzo; Ohki, Shinobu; Tansho, Masataka; Shimizu, Tadashi; Eisaku, Nii; Sasai, Ryo; Labuta, Jan; Ishikawa, Daisuke; Hill, Jonathan P; Ariga, Katsuhiko; Bastakoti, Bishnu Prasad; Yamauchi, Yusuke; Iyi, Nobuo

    2014-10-22

    The carbon cycle, by which carbon atoms circulate between atmosphere, oceans, lithosphere, and the biosphere of Earth, is a current hot research topic. The carbon cycle occurring in the lithosphere (e.g., sedimentary carbonates) is based on weathering and metamorphic events so that its processes are considered to occur on the geological time scale (i.e., over millions of years). In contrast, we have recently reported that carbonate anions intercalated within a hydrotalcite (Mg0.75Al0.25(OH)2(CO3)0.125·yH2O), a class of a layered double hydroxide (LDH), are dynamically exchanging on time scale of hours with atmospheric CO2 under ambient conditions. (Ishihara et al., J. Am. Chem. Soc. 2013, 135, 18040-18043). The use of (13)C-labeling enabled monitoring by infrared spectroscopy of the dynamic exchange between the initially intercalated (13)C-labeled carbonate anions and carbonate anions derived from atmospheric CO2. In this article, we report the significant influence of Mg/Al ratio of LDH on the carbonate anion exchange dynamics. Of three LDHs of various Mg/Al ratios of 2, 3, or 4, magnesium-rich LDH (i.e., Mg/Al ratio = 4) underwent extremely rapid exchange of carbonate anions, and most of the initially intercalated carbonate anions were replaced with carbonate anions derived from atmospheric CO2 within 30 min. Detailed investigations by using infrared spectroscopy, scanning electron microscopy, powder X-ray diffraction, elemental analysis, adsorption, thermogravimetric analysis, and solid-state NMR revealed that magnesium rich LDH has chemical and structural features that promote the exchange of carbonate anions. Our results indicate that the unique interactions between LDH and CO2 can be optimized simply by varying the chemical composition of LDH, implying that LDH is a promising material for CO2 storage and/or separation.

  19. Instrumentation: Ion Chromatography.

    Science.gov (United States)

    Fritz, James S.

    1987-01-01

    Discusses the importance of ion chromatography in separating and measuring anions. The principles of ion exchange are presented, along with some applications of ion chromatography in industry. Ion chromatography systems are described, as well as ion pair and ion exclusion chromatography, column packings, detectors, and programming. (TW)

  20. Significance of anion exchange in pentachlorophenol sorption by variable-charge soils.

    Science.gov (United States)

    Hyun, Seunghun; Lee, Linda S; Rao, P Suresh C

    2003-01-01

    Sorption data and subsequent predictive models for evaluating acidic pesticide behavior on variable-charge soils are needed to improve pesticide management and environmental stewardship. Previous work demonstrated that sorption of pentachlorophenol (PCP), a model organic acid, was adequately modeled by accounting for pH-and pKa-dependent chemical speciation and using two organic carbon-normalized sorption coefficients; one each for the neutral and anionic species. Such models do not account for organic anion interaction to positively charged surface sites, which can be significant for variable-charge minerals present in weathered soils typical of tropical and subtropical regions. The role of anion exchange in sorption of ionizable chemicals by variable-charge soils was assessed by measuring sorption of PCP by several variable-charge soils from aqueous solutions of CaCl2, CaSO4, Ca(H2PO4)2 as a function of pH. Differences in sorption from phosphate and chloride electrolyte solutions were attributed to pentachlorophenolate interactions with anion exchange sites. Suppression of PCP sorption by phosphate ranged from negligible in a soil with essentially no positively charge sites, as measured by negligible anion exchange capacity, to as much as 69% for variable-charge soils. Pentachlorophenolate exchange correlated well with the ratio of pH-dependent anion exchange capacity to net surface charge. Sorption reversibility of PCP by both CaCl2 and Ca(H2PO4)2 solutions was also demonstrated. Results for PCP clearly demonstrate that sorption to anion exchange sites in variable-charge soils should be considered in assessing pesticide mobility and that phosphate fertilizer application may increase the mobility of acidic pesticides.

  1. Significance of anion exchange in pentachlorophenol sorption by variable-charge soils.

    Science.gov (United States)

    Hyun, Seunghun; Lee, Linda S; Rao, P Suresh C

    2003-01-01

    Sorption data and subsequent predictive models for evaluating acidic pesticide behavior on variable-charge soils are needed to improve pesticide management and environmental stewardship. Previous work demonstrated that sorption of pentachlorophenol (PCP), a model organic acid, was adequately modeled by accounting for pH-and pKa-dependent chemical speciation and using two organic carbon-normalized sorption coefficients; one each for the neutral and anionic species. Such models do not account for organic anion interaction to positively charged surface sites, which can be significant for variable-charge minerals present in weathered soils typical of tropical and subtropical regions. The role of anion exchange in sorption of ionizable chemicals by variable-charge soils was assessed by measuring sorption of PCP by several variable-charge soils from aqueous solutions of CaCl2, CaSO4, Ca(H2PO4)2 as a function of pH. Differences in sorption from phosphate and chloride electrolyte solutions were attributed to pentachlorophenolate interactions with anion exchange sites. Suppression of PCP sorption by phosphate ranged from negligible in a soil with essentially no positively charge sites, as measured by negligible anion exchange capacity, to as much as 69% for variable-charge soils. Pentachlorophenolate exchange correlated well with the ratio of pH-dependent anion exchange capacity to net surface charge. Sorption reversibility of PCP by both CaCl2 and Ca(H2PO4)2 solutions was also demonstrated. Results for PCP clearly demonstrate that sorption to anion exchange sites in variable-charge soils should be considered in assessing pesticide mobility and that phosphate fertilizer application may increase the mobility of acidic pesticides. PMID:12809297

  2. Determination of arsenate in water by anion selective membrane electrode using polyurethane-silica gel fibrous anion exchanger composite.

    Science.gov (United States)

    Khan, Asif Ali; Shaheen, Shakeeba

    2014-01-15

    Polyurethane (PU)-silica (Si gel) based fibrous anion exchanger composites were prepared by solid-gel polymerization of polyurethane in the presence of different amounts of silica gel. The formation of PU-Si gel fibrous anion exchanger composite was characterized by Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTA), scanning electron microscopy (SEM) and elemental analysis. The membrane having a composition of 5:3 (PU:Si gel) shows best results for water content, porosity, thickness and swelling. Our studies show that the present ion selective membrane electrode is selective for arsenic, having detection limit (1×10(-8)M to 1×10(-1)M), response time (45s) and working pH range (5-8). The selectivity coefficient values for interfering ions indicate good selectivity for arsenate (AsO4(3-)) over interfering anions. The accuracy of the detection limit results was compared by PCA-Arsenomat.

  3. Simultaneous quantification of sinigrin, sinalbin, and anionic glucosinolate hydrolysis products in Brassica juncea and Sinapis alba seed extracts using ion chromatography.

    Science.gov (United States)

    Popova, Inna E; Morra, Matthew J

    2014-11-01

    Although mustards such as Sinapis alba and Brassica juncea contain glucosinolates (sinalbin and sinigrin, respectively) that hydrolyze to form biopesticidal products, routine quality control methods to measure active ingredients in seed and seed meals are lacking. We present a simple and fast ion chromatography method for the simultaneous quantification of sinigrin, sinalbin, and anionic hydrolysis products in mustard seed to assess biological potency. Optimum conditions include isocratic elution with 100 mM NaOH at a flow rate of 0.9 mL/min on a 4 × 210 mm hydroxide-selective anion-exchange column. All anion analytes including sinigrin, sinalbin, SO4(2-), and SCN(-) yielded recoveries ranging from 83 to 102% and limits of detection ≤0.04 mM, with samples displaying little interference from plant matrix components. Sample preparation is minimized and analysis times are shortened to <90 min as compared with previous methods that took days and multiple instruments.

  4. A simple ion chromatography method for inorganic anion analysis in edible seaweeds.

    Science.gov (United States)

    Gómez-Ordóñez, Eva; Alonso, Esther; Rupérez, Pilar

    2010-09-15

    A new, simple, fast and sensitive ion chromatography (IC) method, for the simultaneous analysis of fluoride, chloride, nitrite, bromide, nitrate, phosphate and sulphate in edible seaweeds was developed and reported for the first time. The validation of the analytical method was studied in terms of linearity, sensitivity, precision and accuracy. All standard calibration curves showed very good correlation between anion peak area and concentration (r>0.999). Limits of detection and quantitation ranged between 0.002-0.05 mg/L and 0.01-0.1mg/L, respectively and indicated the high sensitivity of the method. Relative standard deviation values of repeatability and inter-day precision for standard anions with the same sample were less than 2%. Anion recoveries ranged from 97 to 113% for chloride and from 87 to 105% for sulphate, respectively and showed the fairly good accuracy of the method. The method was applied to the analysis of inorganic anions in brown and red edible seaweeds. Brown seaweeds were characterized by higher chloride content up to 33.7-36.9%, while red seaweeds were characterized by higher sulphate content (45-57%). Sulphate content in seaweeds is related to the presence of sulphated polysaccharides of biological importance. The method developed was well applicable to mineral anion analysis in edible seaweeds and shows suitability and reliability of use in other food samples of nutritional importance. PMID:20801334

  5. Models for the estimation of thermodynamic properties of layered double hydroxides: application to the study of their anion exchange characteristics

    Directory of Open Access Journals (Sweden)

    Bravo-Suárez Juan J.

    2004-01-01

    Full Text Available Several models for the estimation of thermodynamic properties of layered double hydroxides (LDHs are presented. The predicted thermodynamic quantities calculated by the proposed models agree with experimental thermodynamic data. A thermodynamic study of the anion exchange process on LDHs is also made using the described models. Tables for the prediction of monovalent anion exchange selectivities on LDHs are provided. Reasonable agreement is found between the predicted and the experimental monovalent anion exchange selectivities.

  6. Separation of metal ions by anion exchange in mixtures of hydrochloric acid and hydrofluoric acid

    Energy Technology Data Exchange (ETDEWEB)

    Faris, J.P.

    1978-12-01

    Distribution coefficients were determined for the adsorption of more than 40 elements on anion-exchange resins from mixtures of HCl (0.1 to 12M) and HF (0.1-8M). Two resins, Dowex 1 x 10, 200 to 400 mesh and Dowex 1 x 4, 100 to 200 mesh, were used. Distribution coefficients were also determined for the adsorption of many elements on both resins from 0.1 to 12M HCl and 0.1 to 12M HF. Anion exchange in the presence of HF was found useful for separating impurities from various materials for their subsequent determination, and specific procedures used in our spectrochemical laboratory for this purpose are outlined. The results of a literature search on the use of anion exchange in hydrofluoric acid and fluoride-containing media are presented in an extensive bibliography. 404 references, 9 tables.

  7. Anion-exchange Studies of Radioactive Trace Elements in Sulphuric Acid Solutions

    International Nuclear Information System (INIS)

    As part of a chemical group separation procedure used as a pretreatment in gamma spectrometric analysis, a study has been made of the adsorption from sulphuric acid solutions on strongly basic anion exchange resins, prepared in the hydroxide and the sulphate forms, of trace activities of Na, P, K, Ca, Sc, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Rb, Sr, Zr, Nb, Mo, Tc, Ag, Cd, In, Cs, Ba, La, Ce, Hf, Ta, W, Ir, Pa and Np. Besides adsorbing some of the trace elements in the solution, the anion exchange resin in the hydroxide form will neutralize the bulk of the sulphuric acid. This makes possible the subsequent sequential separation of chloride complexes on short anion-exchange columns by a stepwise increasing of the HCl concentration of the solution. On the basis of the results obtained in the present and earlier experiments, a new improved chemical group-separation procedure for mixtures of radioactive trace elements is outlined

  8. [Determination of inorganic anions and gluconate by two-dimensional ion chromatography].

    Science.gov (United States)

    Chen, Ailian; Ding, Hui; Fang, Linmei; Shi, Chaoou

    2015-12-01

    A new two-dimensional ion chromatography method was developed to parallelly analyze two different types of samples with the application of valve switching technology-suppressed conductivity and pulsed amperometric analysis system, for concurrent determination of chloride, nitrite, sulfate, nitrate four inorganic anions and gluconate. The first dimensional chromatography was using Ionpac AG18+Ionpac AS18 anion analysis columns with a suppressed conductivity detector for the separation and detection of Cl-, NO2-, SO4(2-) and NO3-. Respectively, the elution was 5 and 20 mmol/L NaOH at an isocratic flow rate of 1.0 mL/min and sample injection volume of 25 μL. The second dimensional chromatography was utilizing two guard columns, CarboPac PA1 and CarboPac PA20, with 90 mmol/L NaOH solution for the isocratic eluent of 0.8 mL/min. Gluconate was enriched by an AG15 column and switched into the pulsed amperometric detector. The results showed that: each inorganic anion in 0. 1-5.0 mg/L and gluconate in 0.085 6-4.282 5 mg/L had a good linear relationship (R2 ≥ 0.994 5). The RSDs of the peak areas were between 1.05%-1.94%. The limits of detection were 0.61-2.17 μg/L for the anions and 24.24 μg/L for the gluconate. The recoveries were between 90.3% - 102.8%. The two detection modes parallelly have good separation efficiency, detection accuracy and the precision of the separation and are suitable for the analysis of complex samples.

  9. [Determination of inorganic anions and gluconate by two-dimensional ion chromatography].

    Science.gov (United States)

    Chen, Ailian; Ding, Hui; Fang, Linmei; Shi, Chaoou

    2015-12-01

    A new two-dimensional ion chromatography method was developed to parallelly analyze two different types of samples with the application of valve switching technology-suppressed conductivity and pulsed amperometric analysis system, for concurrent determination of chloride, nitrite, sulfate, nitrate four inorganic anions and gluconate. The first dimensional chromatography was using Ionpac AG18+Ionpac AS18 anion analysis columns with a suppressed conductivity detector for the separation and detection of Cl-, NO2-, SO4(2-) and NO3-. Respectively, the elution was 5 and 20 mmol/L NaOH at an isocratic flow rate of 1.0 mL/min and sample injection volume of 25 μL. The second dimensional chromatography was utilizing two guard columns, CarboPac PA1 and CarboPac PA20, with 90 mmol/L NaOH solution for the isocratic eluent of 0.8 mL/min. Gluconate was enriched by an AG15 column and switched into the pulsed amperometric detector. The results showed that: each inorganic anion in 0. 1-5.0 mg/L and gluconate in 0.085 6-4.282 5 mg/L had a good linear relationship (R2 ≥ 0.994 5). The RSDs of the peak areas were between 1.05%-1.94%. The limits of detection were 0.61-2.17 μg/L for the anions and 24.24 μg/L for the gluconate. The recoveries were between 90.3% - 102.8%. The two detection modes parallelly have good separation efficiency, detection accuracy and the precision of the separation and are suitable for the analysis of complex samples. PMID:27097469

  10. 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.

  11. Impact of powdered activated carbon and anion exchange resin on photocatalytic treatment of textile wastewater

    OpenAIRE

    Dhas, Preethi Grace Theva Neethi; Gulyas, Holger; Otterpohl, Ralf

    2015-01-01

    In order to clarify the impact of activated carbon and anion exchange resin on photocatalytic oxidation (PCO) of textile industry wastewater, TiO2-based PCO was investigated with aqueous solutions containing the reactive dye Reactive Blue 4 (RB4) and with a textile dye house effluent in the absence and in the presence of powdered activated carbon (PAC) and the anion exchange resin Lewatit MP 500. Addition of Lewatit improved RB4 removal to a larger extent than PAC addition. Contrasting to chl...

  12. Modified anion-exchange method for determination of thorium in uranium based materials

    International Nuclear Information System (INIS)

    This paper details a modified anion-exchange method for estimation of thorium in uranium based samples like uranium dioxide powders, pellets and uranyl nitrate solutions. The method involves separation of thorium from uranium from 3M commercial grade HCl containing 15% NaCl through an anion-exchange resin. The uranium free effluent containing the analyte(thorium) is determined spectrophotometrically by exploiting absorption of the thorium-arsenazo III complex at 660 nm. The method has a precision of about ±2% at 50 ppm level. (author). 3 refs., 1 tab

  13. Adsorption Mechanisms of Heavy Metal Ions from Drinking Water by Weakly Basic Anion Exchange Resins

    Institute of Scientific and Technical Information of China (English)

    赵璇; 何仕均; 杨磊

    2002-01-01

    Heavy metal micro-contaminants can be removed from water sources technologies. Weakly basic anion exchange resins offer the best ability to remove trace amounts of heavy metals with high selectivity. This paper discusses how weakly basic resins adsorb heavy metals using two different approaches. The removal of mercury, cadmium, and lead ions is based on the fundamental theory of coordination chemistry. The mechanism is not ion exchange but extractive adsorption of heavy metal salts. However, the marked preferential adsorption of chromate by weakly basic anion exchange can be explained using the traditional theory of ion exchange. A lab-scale study produced positive results for the removal of trace amounts of heavy metal ions from drinking water.

  14. Effect of alcohols on separation behavior of rare earth elements using benzimidazole-type anion-exchange resin in nitric acid solutions

    International Nuclear Information System (INIS)

    The mutual separation of rare earth elements based on the ion exchange chromatography has been studied. The effect of alcohols on separation behavior of rare earth elements using the benzimidazole-type anion-exchange resin embedded in high-porous silica beads was investigated in nitric acid/alcohol mixed solvent systems. It was confirmed that the mutual separation of rare earth elements is possible by using our proposed methods. It was found that the distribution coefficients of rare earth elements depend on the corresponding alcoholic relative permittivity and on the steric hindrance due to the hydrophobic interaction among each alcoholic molecule. (author)

  15. Absence of transepithelial anion exchange by rabbit OMCD: Evidence against reversal of cell polarity

    Energy Technology Data Exchange (ETDEWEB)

    Hayashi, Matsuhiko; Schuster, V.L.; Stokes, J.B. (Univ. of Iowa College of Medicine, Iowa City (USA))

    1988-08-01

    In the rabbit cortical collecting duct (CCD), Cl tracer crosses the epithelium predominantly via an anion exchange system that operates in either a Cl-Cl or Cl-HCO{sub 3} exchange mode. In the present study, the authors used the {sup 36}Cl lumen-to-bath rate coefficient (K{sub Cl}, nm/s), a sensitive measurement of CCD transepithelial anion transport, to investigate the nature of Cl transport in the medullary collecting duct dissected from inner stripe, outer medulla (OMCD). The K{sub Cl} in OMCD perfused and bathed in HCO{sub 3}-Ringer solution was low and similar to that value observed in the CCD when anion exchange is inhibited and Cl permeates the epithelium by diffusion. To test the hypothesis that metabolic alkalosis could reverse the polarity of intercalated cells and thus induce an apical Cl-HCO{sub 3} exchanger in H{sup +}-secreting OMCD cells, they measured K{sub Cl} in OMCD from rabbits make alkalotic by deoxycorticosterone and furosemide. Although the base-line K{sub Cl} was slightly higher than in OMCD from control rabbits, the value was still far lower than the K{sub Cl} under comparable conditions in CCD. They conclude (1) Cl transport across the MCD by anion exchange is immeasurably low or nonexistent; (2) unlike the CCD, Cl transport in OMCD is not responsive to cAMP; and (3) metabolic alkalosis does not induce an apical anion exchanger in OMCD, i.e., does not cause epithelial polarity reversal.

  16. Direct determination of seleno-amino acids in biological tissues by anion-exchange separation and electrochemical detection.

    Science.gov (United States)

    Cavalli, S; Cardellicchio, N

    1995-07-01

    Several studies have described the determination of selenium in protein extracts from tissues of marine or terrestrial animals, but have not identified the different chemical forms of selenium that are present. Selenium may be present as seleno-amino acids. Selenocysteine, for example, is a normal component of glutathione peroxidase, an antioxidant enzyme which may behave like other antioxidants, such as vitamin E, protecting tissues against methylmercury toxicity. The present study illustrates a method for the characterization of seleno-amino acids, such as selenocysteine and selenomethionine, in proteins extracted from the liver of marine mammals. The mechanism of detoxification of methylmercury, which involves seleno-compounds, is identified. The analytical determination was carried out using high-performance anion-exchange chromatography coupled with integrated pulsed amperometric detection (HPAEC-IPAD). This method allows the direct determination of underivatized amino acids, eliminating the procedure of pre- or postcolumn derivatization. The chromatographic separation was carried out on an anion-exchange column using a quaternary gradient elution. In order to optimize this method, interferences of amino acids and the influence of pH and ionic strength on the separation and electrochemical detection were studied. The IPAD response for the direct detection of amino acids is optimum at pH > 11. The detection limit (S/N = 3) for selenocysteine was found to be 450 micrograms/l. The application of this method for the identification of seleno-amino acids in protein hydrolysates is also shown. PMID:7640774

  17. Studies concerning the anion ex-change resins catalyzed esterification of epichlorohydrin with organic acids

    Directory of Open Access Journals (Sweden)

    E.I. Muresan

    2009-09-01

    Full Text Available The paper studies the esterification of carboxylic acids with epichlorohydrin over two macroporous strong base anion exchange resins with different polymer matrix. For both resins, the influence of reaction parameters (temperature, catalyst loading, molar ratio on the reaction rate and the yields of the two isomeric esters were investigated.

  18. Separation of the rare earths by anion-exchange in the presence of lactic acid

    Science.gov (United States)

    Faris, J. P.

    1969-01-01

    Investigation of adsorption of rare earths and a few other elements to an anion-exchange resin from mixed solvents containing lactic acid shows that the lanthanides are absorbed more strongly than from the alpha-hydroxyisobutryric acid system, but with less separation between adjacent members of the series.

  19. Tools to discover anionic and nonionic polyfluorinated alkyl surfactants by liquid chromatography electrospray ionisation mass spectrometry

    DEFF Research Database (Denmark)

    Trier, Xenia; Granby, Kit; Christensen, Jan H.

    2011-01-01

    A tiered approach is proposed for the discovery of unknown anionic and nonionic polyfluorinated alkyl surfactants (PFASs) by reversed phase ultra high performance liquid chromatography (UHPLC) – negative electrospray ionisation – quadrupole time of flight mass spectrometry (UHPLC......–ESI−–QTOF–MS). The chromatographic separation, ionisation and detection of PFASs mixtures, was achieved at high pH (pH=9.7) with NH4OH as additive. To distinguish PFASs from other chemicals we used the characteristic negative mass defects of PFASs, their specific losses of 20Da (HF) and the presence of series of chromatographic...

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

    Directory of Open Access Journals (Sweden)

    Glen Andrew D. De Vera

    2011-06-01

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

  1. 高效阴离子交换色谱-脉冲安培法检测低聚异麦芽糖%Determination of Isomaltooligosaccharides by High Performance Anion Exchange Chromatography Coupled with Pulsed Amperometric Detection (HPAEC-PAD)

    Institute of Scientific and Technical Information of China (English)

    张晓萍; 段钢

    2012-01-01

    建立了高效阴离子交换色谱-脉冲安培检测法定量分析低聚异麦芽糖的方法。采用Carbo PakTM PA10色谱柱,配合安培检测器,以NaOH及醋酸钠为洗脱剂。采用此方法不仅一次性实现了低聚异麦芽糖常规组分中葡萄糖、麦芽糖、麦芽三糖、异麦芽糖、异麦芽三糖,潘糖的有效分离,也实现了异麦芽四糖、异麦芽五糖、异麦芽六糖、异麦芽七糖、海藻糖、麦芽酮糖、曲二糖、黑曲霉糖高聚合度糖及二糖同分异构体间的分离及检测。以不同浓度的标准糖混合溶液建立了校正曲线,此方法中,各组分在0.032~25.975mg/L间具有良好的线性关系,各物质的检测限和定量限分别在0.008~0.022mg/L和0.027—0.073mg/L,样品加标回收率为82.02%~116.37%。%A one-step method for quantitatively determination of isomahooligosaccharides (IMO) was developed using high performance anion exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The method was built on a CarboPakTM PAl0 column using NaOH and NaAC as eluents. Using this method, besides conventional components of isomahose, isomaltotriose, panose and some saccharides with higher DP were identified from IMO syrup, other transglycosylation saccharides such as trehalose, kojibiose, nigerose and maltulose were also detected from the syrup. Calibration was carried out by dissolving 15 kinds of standard samples containing glucose, fructose, maltose, maltotriose, isomaltose, isomaltotriose, isomaltotetraose, isomaltopentaose, isomaltohexaose, iso- maltoheptaose, panose, trehalose, maltulose, kojibiose, and nigerose into a mixed solution. The standard solution was diluted to a calibration range from 0. 032 to 25. 975 mg/L. The calibration curves showed good linearity of IMO within this range. The detection limits (LODs) and the quatification limits (LQD) were 0. 008 - 0. 022 mg/L and 0. 027 -0

  2. Simultaneous analysis of trehalose,glucose and maltose in biotransformation samples by high performance anion exchange chromatography with pulsed ampere detection%高效阴离子交换色谱-脉冲安培检测法同时测定生物转化样品中的海藻糖、葡萄糖和麦芽糖

    Institute of Scientific and Technical Information of China (English)

    徐颖; 臧颖; 姜婷; 郑兆娟; 欧阳嘉

    2014-01-01

    An analytical method for the determination of trehalose,maltose,and glucose in biotransformation samples was developed by using high performance anion exchange chroma-tography coupled with pulsed ampere detection( HPAEC-PAD). The analysis was performed on a CarboPacTM 10 column( 250 mm × 2 mm ) with the gradient elution of NaOH-NaAc as the mobile phase. The column temperature was set at 30 ℃,the flow rate was 0. 30 mL/min. The results showed that trehalose,maltose,and glucose in biotransformation system were com-pletely separated and determined in 15 min. The linear ranges and the working curves were determined by using standard samples. The correlation coefficients of three kinds of carbohy-drates were over 0. 999 8 . The detection limits( LODs)were 0. 010-0. 100 mg/L. Under the optimized separation conditions,the recoveries of saccharides in the transformation system at three different spiked levels ranged from 89. 4% to 103. 2%. In biotransformation system,50 IU trehalose synthase were added into 200 g/L maltose for reaction of 8 h at 37 ℃,pH 8. 0. Under the above conditions,the concentration of trehalose in biotransformation sample was 101. 084 g/L,and the conversion rate of trehalose reached 50. 5%. The method can be applied to deter-mine the composition in the transformation system with the advantages of simplicity and con-venience.%建立了高效阴离子交换色谱-脉冲安培电化学检测法同时测定生物转化样品中海藻糖、葡萄糖和麦芽糖的分析方法。选用 CarboPacTM10色谱柱(250 mm×2 mm)对分离条件进行优化,使用标准样品测定了线性范围和工作曲线,柱温为30℃,流速为0.30 mL/min,以氢氧化钠溶液和醋酸钠溶液为流动相进行梯度洗脱,脉冲安培法进行检测。研究结果表明,该方法可在15 min内实现海藻糖生物转化液中3种糖的快速定量分析。海藻糖、葡萄糖和麦芽糖峰面积与质量浓度的线性关系良好,检出限为0

  3. M8L12 cubic cages with all facial Δ or facial Λ configuration: effects of surface anions on the occupancy of the cage and anion exchange.

    Science.gov (United States)

    Yang, Jing; Chang, Xiao-Yong; Sham, Kiu-Chor; Yiu, Shek-Man; Kwong, Hoi-Lun; Che, Chi-Ming

    2016-05-21

    M8L12 cubic cages (M = Mn(II), Zn(II) or Cd(II)), with all eight metal ions having all facial Δ or facial Λ configurations and having an encapsulated anion, were prepared by the self-assembly of m-xylene-bridged imidazolyl-imine ligands and MX2 (X = PF6(-), SbF6(-), TfO(-)) salts; the encapsulated anion exchange with different anions (SbF6(-), Tf2N(-), NO3(-), TsO(-)) was studied and the results with NO3(-) and TsO(-) indicate that anions on the cage surfaces affect the encapsulated anion exchange and the occupancy of the cage. PMID:27064122

  4. Anion-exchange resin-based desulfurization process. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Sheth, A C; Dharmapurikar, R; Strevel, S D

    1994-01-01

    The following investigations were performed: (1) batch mode screening of eleven(11) commercially available resins and selection of three candidate resins for further evaluation in a fixed-bed setup. (2) Process variables study using three candidate resins in the fixed-bed setup and selection of the ``best`` resin for process economics development. (3) Exhaustion efficiency and solution concentration were found to be inversely related necessitating a trade-off between the resin cost versus the cost of evaporation/concentration of ensuing effluents. (4) Higher concentration of the HCO{sub 3}{sup {minus}} form of active sites over less active CO{sub 3}{sup 2{minus}} form of sites in the resin was believed to be the main reason for the observed increase in the equilibrium capacity of the resin at an elevated static CO{sub 2}-pressure. This Increase in capacity was found to level off around 80--120 psig range. The increase in CO{sub 2}-pressure, however, did not appear to affect the overall ion-exchange kinetics. (5) In the fixed-bed mode, the solution concentration was found to affect the equilibrium capacity of candidate resins. Their relationship was well satisfied by the Langmuir type non-linear equilibrium isotherm. Alternatively, the effect of solution concentration on overall ion-exchange kinetics varied from resin to resin. (6) Product inhibition effect on the resin was observed as an initial increase followed by a significant decrease in the resin`s equilibrium capacity for SO{sub 4}{sup 2{minus}} as the HCO{sub 3}{sup {minus}}/SO{sub 4}{sup 2{minus}} molar ratio in the solution was increased from 0 to 1.0. This ratio, however, did not affect the overall ion-exchange kinetics.

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

    Science.gov (United States)

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

    2016-04-01

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

  6. Determination of trace anions in liquefied petroleum gas using liquid absorption and electrokinetic migration for enrichment followed by ion chromatography.

    Science.gov (United States)

    Li, Meilan; Yang, Jianmin; Li, Hai-Fang; Lin, Jin-Ming

    2012-06-01

    A simple sample enrichment technique, electrokinetic migration enrichment in single phase using a designed device, coupled with ion chromatography is presented for the determination of four anions (H(2)PO(4)(-), Cl(-), NO(3)(-), and SO(4)(2-)) in liquefied petroleum gas by liquid adsorption. The electrokinetic migration enrichment is based on the phenomenon of ion electrokinetic migration to the opposite electrode. When the anions migrated to the anode in a smaller volume chamber under the electric field, the concentration was realized. The main parameters affecting enrichment efficiency of applied voltage and enrichment time were investigated. The ion chromatography condition for anions separation was also studied. Under the optimal electrokinetic migration enrichment and ion chromatography conditions, the four anions were detected simultaneously with good linear relationship (r(2) = 0.9908-0.9968) and high precisions (less than 5% of the relative standard deviations of peak areas). The limits of detection of anions (S/N of 3) were in the range of 8-600 μg L(-1). The enrichment factors of the four anions ranged from 3.1 to 5.8. The established method was successfully applied to the analysis of the trace anions in liquefied petroleum gas by liquid adsorption with satisfactory results. The advantages of this method are simple operation and low cost.

  7. THE TESTS AND MECHANISM ABOUT SODIUM IONS FROM AN ANION EXCHANGER

    Institute of Scientific and Technical Information of China (English)

    ZhuXingbao; YuJinchun; 等

    1996-01-01

    There exists a universal phenomena that sodium ions are leaked from the strong basic anion exdchanger in operation,which has been puzzling the researchers working in the field of water treatment for years.It is well known that the leakage of sodium ions will seriously affect the pruity of effluent.On the basis of lots of laboratory and industrial experiments,the mechanism of the sodium ions leaked from an anion exchanger has been preliminarily made out and some new chemical reaction equations as well as some improving measures have been put forward in this article.

  8. Integrating tunable anion exchange with reverse osmosis for enhanced recovery during inland brackish water desalination.

    Science.gov (United States)

    Smith, Ryan C; SenGupta, Arup K

    2015-05-01

    For inland brackish water desalination by reverse osmosis or RO, concentrate or reject disposal poses a major challenge. However, enhanced recovery and consequent reduction in the reject volume using RO processes is limited by the solubility of ions present in the feedwater. One of the most common and stubborn precipitate formed during desalination is calcium sulfate. Reducing or eliminating the presence of sulfate would allow the process to operate at higher recoveries without threat to membrane scaling. In this research, this goal is accomplished by using an appropriate mixture of self-regenerating anion exchange resins that selectively remove and replace sulfate by chloride prior to the RO unit. Most importantly, the mixed bed of anion exchange resins is self-regenerated with the reject brine from the RO process, thus requiring no addition of external chemicals. The current work demonstrates the reversibility of the hybrid ion exchange and RO (HIX-RO) process with 80% recovery for a brackish water composition representative of groundwater in San Joaquin Valley in California containing approximately 5200 mg/L of total dissolved solids or TDS. Consequently, the reject volume can be reduced by 50% without the threat of sulfate scaling and use of antiscaling chemicals can be eliminated altogether. By appropriately designing or tuning the mixed bed of anion exchange resins, the process can be extended to nearly any composition of brackish water for enhanced recovery and consequent reduction in the reject volume.

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

    Science.gov (United States)

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

    2015-05-01

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

  10. Application of monohydric phenols as mobile-phase modifiers in the determination of anions by two-column ion chromatography

    International Nuclear Information System (INIS)

    The effect of monohydric phenols as eluant-modifying additives on the determination of I- and MoO42- anions by ion chromatography was studied. The following phenols were examined: pentafluorophenol, 4-nitrophenol, 2-nitrophenol, 2,4-dinitrophenol, and 4-chlorphenol. It was found that these phenols selectively affect the retention times of weakly and strongly retained anions. A correlation between pKa and the concentration of additive, and the retention times of anions was found. 12 refs., 3 figs., 3 tabs

  11. Effects of Polar Organic Solvent on Separation of Y(edta)-/Nd(edta)- Complexes on Polyacrylic Anion Exchangers

    Institute of Scientific and Technical Information of China (English)

    Halina Hubicka; Dorota Kolodynska

    2005-01-01

    The use of polar organic solvents for the separations of rare earth elements (Ⅲ) is effective especially for their extensive separations despite the solubility limitations. The study shows that polyacrylate anion exchangers, particularly the weakly basic, gel anion exchanger Amberlite IRA 68, can be applied to the separation of rare earth complexes with EDTA in H2O-methanol and H2O-ethanol systems. In most cases the determined distribution coefficients of Ln3+ complexes with EDTA in mixed media like water-methanol on polyacrylate anion exchangers are larger than those in pure water media.

  12. Anion-induced exchange interactions in binuclear complexes of Cu(II) with flexible hexadentate bispicolylamidrazone ligands

    Science.gov (United States)

    Baryshnikov, Gleb V.; Minaev, Boris F.; Baryshnikova, Alina A.; Ågren, Hans

    2016-09-01

    Two recently synthesized copper(II) complexes with spacer-armed bispicolylamidrazone ligands have been theoretically studied at the density functional theory (DFT) level accounting for empirical dispersion correction and intrinsic anionic environment by perchlorate ions. The exchange parameter between the open-shell singlet and triplet states of the studied complexes has been estimated by broken symmetry DFT calculations. The mechanism of spin-spin exchange interaction between the unpaired electrons via the σ-bond aliphatic chain (Gusev et al., 2015) is confirmed. Instead, a anion-induced mechanism is proposed which means that the anionic grid participates in the exchange interaction between the unpaired electrons.

  13. Cross-linked comb-shaped anion exchange membranes with high base stability

    Energy Technology Data Exchange (ETDEWEB)

    Li, NW; Wang, LZ; Hickner, M

    2014-01-01

    A unique one-step cross-linking strategy that connects quaternary ammonium centers using Grubbs II-catalyzed olefin metathesis was developed. The cross-linked anion exchange membranes showed swelling ratios of less than 10% and hydroxide conductivities of 18 to 40 mS cm(- 1). Cross-linking improved the membranes' stability to hydroxide degradation compared to their non-cross-linked analogues.

  14. ELECTROCHEMICAL STABILITY OF STRONG BASIC ANION EXCHANGE MEMBRANES IN CONDITIONS OF HIGH INTENSIVE ELECTRODIALYSIS PROCESS

    OpenAIRE

    Zabolotskiy V. I.; Sharafan M. V.; Chermit R. H.; Vasilieva V. I.

    2014-01-01

    The stability of strongly basic anion-exchange membranes MA-41-2P (JSC "Schekino-Nitrogen", Russia) and AMX (Tokuyama Soda, Japan) under intensive current regimes was investigated in the current study. The process of water molecules dissociation at current densities above the limiting one in 0.01 M sodium chloride solution was studied in detail. The length of the electroconvective instability at the membrane / solution interface at currents exceeding the limiting current was measured by laser...

  15. Development of imidazolium-type alkaline anion exchange membranes for fuel cell application

    OpenAIRE

    Ran, J; Wu, L.; XU, T; Varcoe, JR; Ong, AL; Poynton, SD

    2012-01-01

    This study reports the development of imidazolium-type alkaline anion exchange membranes (Im-AAEMs) based on the functionalization of bromomethylated poly(2,6-dimethyl-1,4-phenylene oxide) (BPPO) using 1-methylimdazole. Aromatic polymers bearing bromomethyl, instead of chloromethyl, functional groups were employed as base materials to avoid complicated chloromethylation which require toxic reagents. H NMR and FT-IR spectroscopic data indicated the synthesis of a series of membranes with contr...

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

    Science.gov (United States)

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

    2015-03-20

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

  17. Determination of neomycin in water samples by high performance anion chromatography with pulsed amperometric detection

    Institute of Scientific and Technical Information of China (English)

    Bin Guan; Dong Xing Yuan

    2007-01-01

    A simple, fast and reliable method, using high performance anion chromatography with pulsed amperometric detection, had been developed for the analysis of neomycin in water samples. The elution and separation were carried out with an isocratic mobile phase, containing 10 mmol/L NaOH. The influence of the concentration and pH of the mobile phase on the separation and detection was investigated. A quadruple-potential waveform used for the detection was optimized. The detection limit of neomycin was down to 0.027 μg/mL. The linearity of neomycin calibration curve ranged from 0.050 to 0.505 μg/mL with correlation coefficient of0.9997. R.S.D. (n= 11) was 4.0%.

  18. Determination of anionic surfactants during wastewater recycling process by ion pair chromatography with suppressed conductivity detection

    Science.gov (United States)

    Levine, L. H.; Judkins, J. E.; Garland, J. L.; Sager, J. C. (Principal Investigator)

    2000-01-01

    A direct approach utilizing ion pairing reversed-phase chromatography coupled with suppressed conductivity detection was developed to monitor biodegradation of anionic surfactants during wastewater recycling through hydroponic plant growth systems and fixed-film bioreactors. Samples of hydroponic nutrient solution and bioreactor effluent with high concentrations (up to 120 mS electrical conductance) of inorganic ions can be analyzed without pretreatment or interference. The presence of non-ionic surfactants did not significantly affect the analysis. Dynamic linear ranges for tested surfactants [Igepon TC-42, ammonium lauryl sulfate, sodium laureth sulfate and sodium alkyl (C10-C16) ether sulfate] were 2 to approximately 500, 1 to approximately 500, 2.5 to approximately 550 and 3.0 to approximately 630 microg/ml, respectively.

  19. Study on the Retention Behavior of Aromatic Carboxylic and Sulfonic acid on a New Anion Exchange Column

    Institute of Scientific and Technical Information of China (English)

    SHI,Ya-Li; CAI,Ya-Qi; MOU,Shi-Fen

    2008-01-01

    Ion chromatography (IC) has gradually developed into a preferred method for the determination of inorganic anions. And in recent years some low molecular aliphatic acid can be also separated in the ion exchange column with the development of stationary phase. But for the determination of aromatic ionic compounds there are some problems. The aromatic anions show enhanced retention due to interaction with the π electrons of the aromatic backbone. Although the addition of an organic modifier can alleviate the difficulty, it is not the ultimate solution.IonPac AS20 column was developed using a unique polymer bonding technology and its substrate coating is aliphatic backbone. The polymer is completely free of any π electron-containing substituents in the AS20 column. In this paper, the retention behavior of aromatic carboxylic and sulfonic acid on two hydroxide-selective columns,IonPac AS11-HC, AS16, and the new column AS20 was also studied. The result showed that the retentions of ten compounds on three columns were different with each other because of their different column characteristics.Among them 4-chlorobenzene sulfonic acid, 3,5-dihydric benzoic acid and salicylic acid obviously exhibited the weakest retention on the IonPac AS20. It was showed that π-π bond function between anion and stationary phases was weakened in AS20 column because its polymer was completely free of any π electron-containing substituents.So in this paper the AS20 was selected as an analytical column to separate ten aromatic ionic compounds, fumaric acid with conjugate bond included. The retention behavior, separation of the ten compounds and effect of temperature on their retention in the anion-exchange column AS20 (2 mm) were studied. The result showed that those compounds could be separated with each other when running in gradient program and the organic modifier was unnecessary during the separation. So it is showed that AS20 column can be used as a separating column because its

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

    Institute of Scientific and Technical Information of China (English)

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

    2007-01-01

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

  1. Sodium-Zinc Exchange Selectivity on Wyoming Montmorillonite in Different Background Anion Solutions

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The effect of background anion on cation exchange reactions, such as Na-Ca and Na-Cu exchange reac-tions, on montmorillonites has been studied, but the results are not always clear and discrepancies exist inthe literature. In this study, the exchange of zinc (Zn2+) for sodium (Na+) on Wyoming montmorillonitewas investigated at 298 .K using Cl-, ClO4-, NO-3, OAc-, and SO42- solution media at a constant totalmetal charge concentration of 0.0200 molc L-1. Results indicated that the clay CEC values were essentialsimilar for Cl-, ClO-4, NO-3 and SO42- solution media with an average CEC of 0.856 ±0.008 molc kg-1; inan OAc- solution the clay CEC was much higher than that in other anion media. The specific adsorption ofZn (SAZn), as defined by the extraction of Zn using 0.05 mol L-1 Na2-EDTA, was different in the variousbackground solutions. The highest value for SAZn was 0.359±0.0350 molc kg-1, which occurred in OAc-solution. There was essentially no difference in the total apparent adsorbed metals (the sum of adsorbedequivalents of Na and Zn per kilogram of clay, Q) among the various background solutions. The average Q forall anion media was 0.807±0.011 mole kg-1 and was independent of exchanger composition. Experimentalresults indicated that there were no significant monovalent cation complexes such as ZnCl+ or ZnNO3+ thatwere adsorbed by montmorillonite. The Na-Zn exchange isotherms indicated that there was an adsorptionpreference for Zn over Na on Wyoming montmorillonite.

  2. New Anion-Exchange Resins for Improved Separations of Nuclear Materials

    International Nuclear Information System (INIS)

    Improved separations of nuclear materials will have a significant impact upon a broad range of DOE activities. DOE-EM Focus Areas and Crosscutting Programs have identified improved methods for the extraction and recovery of radioactive metal ions from process, waste, and environmental waters as critical needs for the coming years. We propose to develop multifunctional anion-exchange resins that facilitate anion uptake by carefully controlling the structure of the anion receptor site. Our new ion-exchange resins interface the field of ion-specific chelating ligands with robust, commercial ion-exchange technology to provide materials which exhibit superior selectivity and kinetics of sorption and desorption. The following Focus Areas and Crosscutting Programs have described needs that would be favorably impacted by the new material: Efficient Separations and Processing - radionuclide removal from aqueous phases; Plutonium - Pu, Am or total alpha removal to meet regulatory requirement s before discharge to the environment; Plumes - U and Tc in groundwater, U, Pu, Am, and Tc in soils; Mixed Waste - radionuclide partitioning; High-Level Tank Waste - actinide and Tc removal from supernatants and/or sludges. The basic scientific issues which need to be addressed are actinide complex speciation along with modeling of metal complex/functional site interactions in order to determine optimal binding-site characteristics. Synthesis of multifunctionalized extractants and ion-exchange materials that implement key features of the optimized binding site, and testing of these materials, will provide feedback to the modeling and design activities. Resin materials which actively facilitate the uptake of actinide complexes from solution should display both improved selectivity and kinetic properties. The long-range implications of this research, however, go far beyond the nuclear complex. This new methodology of ''facilitated uptake'' could revolutionize ion-exchange technology

  3. DEVELOPMENT AND CHARACTERIZATION OF POLYVINYLIDENE FLUORIDE - IMIDAZOLIUM FUNCTIONALIZED POLYSULFONE BLEND ANION EXCHANGE MEMBRANE

    Directory of Open Access Journals (Sweden)

    S. VELU

    2015-09-01

    Full Text Available Anion exchange membrane (AEM is one of the core components of an alkaline fuel cell influencing the fuel cell’s performance, durability and stability. Out of the many anion exchange membranes reported so far, imidazolium functionalized polysulfone (PSf-ImOH membrane has been identified to have high hydroxide ionic conductivity, reaching up to 50 mS cm-1 at 20oC. However, at high levels of ion exchange capacity, the membrane’s water uptake and swelling ratio increases significantly with temperature thus destabilizing it and making it unfit for potential use in high temperature alkaline fuel cells. This limitation of PSf-ImOH membranes has been overcome by blending it with polyvinylidene fluoride (PVDF polymer, which is a thermally stable and highly hydrophobic polymer. PSf-ImOH membrane with a high degree of chloromethylation (180% was synthesized and blended with PVDF at different weight ratios (PVDF / PSf-ImOH: 30/70, 50/50 and 70/30 to create a series of novel anion exchange membranes. The prepared membranes were characterized to study their structure, water uptake, swelling ratio, solubility in low boiling water soluble solvents, thermal stability, ion exchange capacity (IEC and ionic conductivity (IC at different temperatures. The 70% PVDF blend membrane demonstrated the better performance in terms of IEC, IC and water uptake properties compared to other membranes. Comparative studies on the water uptake and IC variation between the 70% PVDF blend membrane and pure PSfImOH membrane (having the same IEC as that of the blend membrane, clearly indicated the superiority and the promising use of the blend membrane in alkaline fuel cell especially for high temperature working condition.

  4. Hydrophilic interaction chromatography-mass spectrometry for anionic metabolic profiling of urine from antibiotic-treated rats

    NARCIS (Netherlands)

    Kok, Miranda G M; Swann, Jonathan R; Wilson, Ian D; Somsen, Govert W; de Jong, Gerhardus J

    2014-01-01

    Hydrophilic interaction chromatography-mass spectrometry (HILIC-MS) was used for anionic metabolic profiling of urine from antibiotic-treated rats to study microbial-host co-metabolism. Rats were treated with the antibiotics penicillin G and streptomycin sulfate for four or eight days and compared t

  5. Ammonium Bicarbonate Transport in Anion Exchange Membranes for Salinity Gradient Energy

    KAUST Repository

    Geise, Geoffrey M.

    2013-09-17

    Many salinity gradient energy technologies such as reverse electrodialysis (RED) rely on highly selective anion transport through polymeric anion exchange membranes. While there is considerable interest in using thermolytic solutions such as ammonium bicarbonate (AmB) in RED processes for closed-loop conversion of heat energy to electricity, little is known about membrane performance in this electrolyte. The resistances of two commercially available cation exchange membranes in AmB were lower than their resistances in NaCl. However, the resistances of commercially available anion exchange membranes (AEMs) were much larger in AmB than in NaCl, which would adversely affect energy recovery. The properties of a series of quaternary ammonium-functionalized poly(phenylene oxide) and Radel-based AEMs were therefore examined to understand the reasons for increased resistance in AmB to overcome this performance penalty due to the lower mobility of bicarbonate, 4.59 × 10-4 cm2/(V s), compared to chloride, 7.90 × 10-4 cm2/(V s) (the dilute aqueous solution mobility ratio of HCO3 - to Cl- is 0.58). Most membrane resistances were generally consistent with the dilute solution mobilities of the anions. For a few key samples, however, increased water uptake in AmB solution reduced the ionic resistance of the polymer compared to its resistance in NaCl solution. This increased water uptake was attributed to the greater hydration of the bicarbonate ion compared to the chloride ion. The increased resistance due to the use of bicarbonate as opposed to chloride ions in AEMs can therefore be mitigated by designing polymers that swell more in AmB compared to NaCl solutions, enabling more efficient energy recovery using AmB thermolytic solutions in RED. © 2013 American Chemical Society.

  6. Synthesis and Characterization of Imidazolium Linear Bisphenol Polycarbonate Hydroxides for Anion Exchange Membrane.

    Science.gov (United States)

    Jang, Hohyoun; Hossain, Md Awlad; Lee, Soonho; Ha, Jaesung; Yoo, Jihoo; Kim, Kyungchul; Kim, Whangi

    2015-11-01

    A novel anion exchange membrane of imidazolium functionalized bisphenol polycarbonate was prepared for application in alkaline fuel cell. Di-imidazolium polycarbonate anionic membrane was synthesized by sequential interfacial polymerization, chloromethylation, substitution with 1-methylimidazole and ion exchange with 1.0 M KOH. Chloromethylation reaction was quantitative to achieve a high content of hydroxide ions. Introduction of conjugated imidazole ring in polymer plays an important role to improve both thermal and chemical stability. Bisphenol polycarbonate is a flexible polymer and shows a good solubility in polar organic solvent. The alkaline imidazolium bisphenol polycarbonate rendered an elevated molecular weight with excellent solubility in polar aprotic solvent. Different levels of substitution and ion exchange were investigated; the resulting membranes showed high ion exchange capacities (IECs) of up to 2.15 mmol g(-1). The imidazolium-functionalized copolymer membranes showed lower water affinity (14.2-42.8% at 30 degrees C) that satisfied an essential criterion for fuel cell application. The chemical structure of the imidazolium functionalized polycarbonate membrane was confirmed by 1H NMR spectroscopy, and also the membrane properties were evaluated by thermogravimetric analysis (TGA) and water uptake (WU), IEC and conductivity assessment. They exhibited hydroxide conductivity above 10(-2) S cm(-1) at room temperature and good chemical stability for up to five days without significant losses of ion conductivity. PMID:26726604

  7. Hydration and sorption characteristics of a polyfunctional weak-base anion exchanger after the sorption of vanillin and ethylvanillin

    Science.gov (United States)

    Rodionova, D. O.; Voronyuk, I. V.; Eliseeva, T. V.

    2016-07-01

    Features of the sorption of substituted aromatic aldehydes by a weak-base anion exchanger under equilibrium conditions are investigated using vanillin and ethylvanillin as examples. Analysis of the sorption isotherms of carbonyl compounds at different temperatures allows us to calculate the equilibrium characteristics of their sorption and assess the entropy and enthalpy contributions to the energy of the process. Hydration characteristics of the macroporous weak-base anion exchanger before and after the sorption of aromatic aldehydes are compared.

  8. Models for the estimation of thermodynamic properties of layered double hydroxides: application to the study of their anion exchange characteristics

    OpenAIRE

    Bravo-Suárez Juan J.; Páez-Mozo Edgar A.; Oyama S. Ted

    2004-01-01

    Several models for the estimation of thermodynamic properties of layered double hydroxides (LDHs) are presented. The predicted thermodynamic quantities calculated by the proposed models agree with experimental thermodynamic data. A thermodynamic study of the anion exchange process on LDHs is also made using the described models. Tables for the prediction of monovalent anion exchange selectivities on LDHs are provided. Reasonable agreement is found between the predicted and the experimental mo...

  9. 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.

  10. Molecular physiology and genetics of Na+-independent SLC4 anion exchangers

    Science.gov (United States)

    Alper, Seth L.

    2009-01-01

    Summary Plasmalemmal Cl–/HCO3– exchangers are encoded by the SLC4 and SLC26 gene superfamilies, and function to regulate intracellular pH, [Cl–] and cell volume. The Cl–/HCO3– exchangers of polarized epithelial cells also contribute to transepithelial secretion and reabsorption of acid–base equivalents and Cl–. This review focuses on Na+-independent electroneutral Cl–/HCO3– exchangers of the SLC4 family. Human SLC4A1/AE1 mutations cause the familial erythroid disorders of spherocytic anemia, stomatocytic anemia and ovalocytosis. A largely discrete set of AE1 mutations causes familial distal renal tubular acidosis. The Slc4a2/Ae2–/– mouse dies before weaning with achlorhydria and osteopetrosis. A hypomorphic Ae2–/– mouse survives to exhibit male infertility with defective spermatogenesis and a syndrome resembling primary biliary cirrhosis. A human SLC4A3/AE3 polymorphism is associated with seizure disorder, and the Ae3–/– mouse has increased seizure susceptibility. The transport mechanism of mammalian SLC4/AE polypeptides is that of electroneutral Cl–/anion exchange, but trout erythroid Ae1 also mediates Cl– conductance. Erythroid Ae1 may mediate the DIDS-sensitive Cl– conductance of mammalian erythrocytes, and, with a single missense mutation, can mediate electrogenic SO42–/Cl– exchange. AE1 trafficking in polarized cells is regulated by phosphorylation and by interaction with other proteins. AE2 exhibits isoform-specific patterns of acute inhibition by acidic intracellular pH and independently by acidic extracellular pH. In contrast, AE2 is activated by hypertonicity and, in a pH-independent manner, by ammonium and by hypertonicity. A growing body of structure–function and interaction data, together with emerging information about physiological function and structure, is advancing our understanding of SLC4 anion exchangers. PMID:19448077

  11. Selective removal of nitrate by using a novel macroporous acrylic anion exchange resin

    Institute of Scientific and Technical Information of China (English)

    Hai Ou Song; Yang Zhou; Ai Min Li; Sandra Mueller

    2012-01-01

    An anion exchange resin NDP-5 has been prepared successfully and applied on the selective removal of nit-ate from SO42-/NO3- binary co-existence system.The composition and morphology of NDP-5 were confirmed by FT-IR and SEM.The NDP-5 resin exhibits the completely different behavior on the adsorption capacity,adsorption kinetic and the effect of the completing anion in the absence or presence of sulfate,compared to D213.And,the resultants of kinetic are well fitted by the pseudo-first-order and pseudo-second-order models.These results are very important to develop novel resins with great features.

  12. Hybrid Anion Exchange Hollow Fiber Membrane for Delivery of Ionic Drugs

    Directory of Open Access Journals (Sweden)

    Na Wang

    2012-01-01

    Full Text Available Hybrid anion exchange hollow fiber membranes (HAEHFMs based on bromomethylated poly(2,6-dimethyl-1,4-phenylene oxide (BPPO are proposed as potential drug carriers for four anionic model drugs, including the sodium salts of benzoate (NaBS, salicylate (NaSA, meta-amino salicylate (NaMAS, and loxoprofen (NaLS. The results of the static loading and release experiments suggest that electrostatic interaction, hydrogen bonding, and hydrophobic interaction are the main interaction patterns between the membrane and the drugs. And they are directly influenced by the external phase conditions and the drug physicochemical characteristics, such as structure, molecular weight, dissociation (pKa, and hydrogen bonding capability. Among the four different drugs, NaSA and NaMAS appear to be the most suitable for controlled release by the HAEHFM due to their excellent adsorption/release behaviors.

  13. Guanidinium based blend anion exchange membranes for direct methanol alkaline fuel cells (DMAFCs)

    Science.gov (United States)

    Sajjad, Syed D.; Liu, Dong; Wei, Zi; Sakri, Shambhavi; Shen, Yi; Hong, Yi; Liu, Fuqiang

    2015-12-01

    Guanidinium based blend anion exchange membranes (AEMs) for direct methanol alkaline fuel cells have been fabricated and studied. The guanidinium prepolymer is first synthesized through a simple polycondensation process with the ion exchange moieties incorporated directly into the polymer backbone, and then is used to make guanidinium - chitosan (Gu-Chi) blend membranes. Besides, a lipophilic guanidinium prepolymer, synthesized by means of a precipitation reaction between sodium stearate and guanidinium salt, is adopted to tune solubility and mechanical properties of the blend AEMs. Results show that both ionic conductivity and methanol permeability of the AEMs can be tuned by blend composition and chemistry of the guanidinium based prepolymer. The selectivity (ratio of ionic conductivity to methanol permeability) of the fabricated membranes is superior to that of commercial membranes. Under fuel cell tests using 3 M methanol, the open circuit voltage (OCV) value for the blend AEM with 72 wt% of the guanidinium polymer (0.69 V) is much higher than that of the commercial Tokuyama A201 (0.47 V) at room temperature, while the blend AEMs with 50 wt% guanidinium content still show comparable values. Overall, the developed membranes demonstrate superior performance and therefore pose great promise for direct methanol anion exchange fuel cell (DMAFC) applications.

  14. The Drosophila Anion Exchanger (DAE lacks a detectable interaction with the spectrin cytoskeleton

    Directory of Open Access Journals (Sweden)

    Base Christine

    2010-06-01

    Full Text Available Abstract Background Current models suggest that the spectrin cytoskeleton stabilizes interacting ion transport proteins at the plasma membrane. The human erythrocyte anion exchanger (AE1 was the first membrane transport protein found to be associated with the spectrin cytoskeleton. Here we evaluated a conserved anion exchanger from Drosophila (DAE as a marker for studies of the downstream effects of spectrin cytoskeleton mutations. Results Sequence comparisons established that DAE belongs to the SLC4A1-3 subfamily of anion exchangers that includes human AE1. Striking sequence conservation was observed in the C-terminal membrane transport domain and parts of the N-terminal cytoplasmic domain, but not in the proposed ankyrin-binding site. Using an antibody raised against DAE and a recombinant transgene expressed in Drosophila S2 cells DAE was shown to be a 136 kd plasma membrane protein. A major site of expression was found in the stomach acid-secreting region of the larval midgut. DAE codistributed with an infolded subcompartment of the basal plasma membrane of interstitial cells. However, spectrin did not codistribute with DAE at this site or in anterior midgut cells that abundantly expressed both spectrin and DAE. Ubiquitous knockdown of DAE with dsRNA eliminated antibody staining and was lethal, indicating that DAE is an essential gene product in Drosophila. Conclusions Based on the lack of colocalization and the lack of sequence conservation at the ankyrin-binding site, it appears that the well-characterized interaction between AE1 and the spectrin cytoskeleton in erythrocytes is not conserved in Drosophila. The results establish a pattern in which most of the known interactions between the spectrin cytoskeleton and the plasma membrane in mammals do not appear to be conserved in Drosophila.

  15. [Development of metal ions analysis by ion chromatography].

    Science.gov (United States)

    Yu, Hong; Wang, Yuxin

    2007-05-01

    Analysis of metal ions by ion chromatography, including cation-exchange ion chromatography, anion-exchange ion chromatography and chelation ion chromatography, is reviewed. The cation-exchange ion chromatography is a main method for the determination of metal ions. Stationary phases in cation-exchange ion chromatography are strong acid cation exchanger (sulfonic) and weak acid cation exchanger (carboxylic). Alkali metal ions, alkaline earth metal ions, transition metal ions, rare earth metal ions, ammonium ions and amines can be analyzed by cation-exchange ion chromatography with a suitable detector. The anion-exchange ion chromatography is suitable for the separation and analysis of alkaline earth metal ions, transition metal ions and rare earth metal ions. The selectivity for analysis of metal ions with anion-exchange ion chromatography is good. Simultaneous determination of metal ions and inorganic anions can be achieved using anion-exchange ion chromatography. Chelation ion chromatography is suitable for the determination of trace metal ions in complex matrices. A total of 125 references are cited.

  16. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

    Science.gov (United States)

    Popov, L

    2016-09-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials.

  17. Alkaline degradation studies of anion exchange polymers to enable new membrane designs

    Science.gov (United States)

    Nunez, Sean Andrew

    Current performance targets for anion-exchange membrane (AEM) fuel cells call for greater than 95% alkaline stability for 5000 hours at temperatures up to 120 °C. Using this target temperature of 120 °C, an incisive 1H NMR-based alkaline degradation method to identify the degradation products of n-alkyl spacer tetraalkylammonium cations in various AEM polymers and small molecule analogs. Herein, the degradation mechanisms and rates of benzyltrimethylammonium-, n-alkyl interstitial spacer- and n-alkyl terminal pendant-cations are studied on several architectures. These findings demonstrate that benzyltrimethylammonium- and n-alkyl terminal pendant cations are more labile than an n-alkyl interstitial spacer cation and conclude that Hofmann elimination is not the predominant mechanism of alkaline degradation. Additionally, the alkaline stability of an n-alkyl interstitial spacer cation is enhanced when combined with an n-alkyl terminal pendant. Interestingly, at 120 °C, an inverse trend was found in the overall alkaline stability of AEM poly(styrene) and AEM poly(phenylene oxide) samples than was previously shown at 80 °C. Successive small molecule studies suggest that at 120 °C, an anion-induced 1,4-elimination degradation mechanism may be activated on styrenic AEM polymers bearing an acidic alpha-hydrogen. In addition, an ATR-FTIR based method was developed to assess the alkaline stability of solid membranes and any added resistance to degradation that may be due to differential solubilities and phase separation. To increase the stability of anion exchange membranes, Oshima magnesate--halogen exchange was demonstrated as a method for the synthesis of new anion exchange membranes that typically fail in the presence of organolithium or Grignard reagents alone. This new chemistry, applied to non-resinous polymers for the first time, proved effective for the n-akyl interstitial spacer functionalization of poly(phenylene oxide) and poly(styrene- co

  18. ELECTROCHEMICAL STABILITY OF STRONG BASIC ANION EXCHANGE MEMBRANES IN CONDITIONS OF HIGH INTENSIVE ELECTRODIALYSIS PROCESS

    Directory of Open Access Journals (Sweden)

    Zabolotskiy V. I.

    2014-12-01

    Full Text Available The stability of strongly basic anion-exchange membranes MA-41-2P (JSC "Schekino-Nitrogen", Russia and AMX (Tokuyama Soda, Japan under intensive current regimes was investigated in the current study. The process of water molecules dissociation at current densities above the limiting one in 0.01 M sodium chloride solution was studied in detail. The length of the electroconvective instability at the membrane / solution interface at currents exceeding the limiting current was measured by laser interferometry

  19. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

    Science.gov (United States)

    Popov, L

    2016-09-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials. PMID:27451111

  20. Synthesis and characterization of quaternized poly(phthalazinone ether sulfone ketone) for anion-exchange membrane

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Chloromethylated poly(phthalazinone ether sulfone ketone) (CMPPESK) was prepared from poly(phthalazinone ether sulfone ketone) (PPESK) using chloromethyl octyl ethers (CMOE) with lower toxicity as chloromethylated regent. CMPPESK was soluble in N-methyl-2-pyrrolidone (NMP), N,N-dimethylacetamide (DMAc) and chloroform. Quatemized poly(phthalazinone ether sulfone ketone) (QAPPESK) was prepared from CMPPESK by quaternization. QAPPESK had excellent solvent resistance,which was only partly soluble in sulfuric acid (98%) and swollen in N,N-dimethylformamide (DMF). The vanadium redox flow battery (V-RFB) using QAPPESK anion-exchange membrane had better performance with 88.3% of overall energy efficiency.

  1. The perchlorate anion is more effective than the trifluoroacetate anion as an ion-pairing reagent for reversed-phase chromatography of peptides

    OpenAIRE

    Shibue, M.; Mant, C.T.; Hodges, R.S.

    2005-01-01

    The addition of salts, specifically sodium perchlorate (NaClO4), to mobile phases at acidic pH as ion-pairing reagents for reversed-phase high-performance liquid chromatography (RP-HPLC) has been generally overlooked. To demonstrate the potential of NaClO4 as an effective anionic ion-pairing reagent, we applied RP-HPLC in the presence of 0–100 mM sodium chloride (NaCl), sodium trifluoroacetate (NaTFA) or NaClO4 to two mixtures of synthetic 18-residue peptides: a mixture of peptides with the s...

  2. Simultaneous quantification of sinigrin, sinalbin, and anionic glucosinolate hydrolysis products in Brassica juncea and Sinapis alba seed extracts using ion chromatography.

    Science.gov (United States)

    Popova, Inna E; Morra, Matthew J

    2014-11-01

    Although mustards such as Sinapis alba and Brassica juncea contain glucosinolates (sinalbin and sinigrin, respectively) that hydrolyze to form biopesticidal products, routine quality control methods to measure active ingredients in seed and seed meals are lacking. We present a simple and fast ion chromatography method for the simultaneous quantification of sinigrin, sinalbin, and anionic hydrolysis products in mustard seed to assess biological potency. Optimum conditions include isocratic elution with 100 mM NaOH at a flow rate of 0.9 mL/min on a 4 × 210 mm hydroxide-selective anion-exchange column. All anion analytes including sinigrin, sinalbin, SO4(2-), and SCN(-) yielded recoveries ranging from 83 to 102% and limits of detection ≤0.04 mM, with samples displaying little interference from plant matrix components. Sample preparation is minimized and analysis times are shortened to <90 min as compared with previous methods that took days and multiple instruments. PMID:25314611

  3. Extracellular Cl(-) regulates human SO4 (2-)/anion exchanger SLC26A1 by altering pH sensitivity of anion transport.

    Science.gov (United States)

    Wu, Meng; Heneghan, John F; Vandorpe, David H; Escobar, Laura I; Wu, Bai-Lin; Alper, Seth L

    2016-08-01

    Genetic deficiency of the SLC26A1 anion exchanger in mice is known to be associated with hyposulfatemia and hyperoxaluria with nephrolithiasis, but many aspects of human SLC26A1 function remain to be explored. We report here the functional characterization of human SLC26A1, a 4,4'-diisothiocyanato-2,2'-stilbenedisulfonic acid (DIDS)-sensitive, electroneutral sodium-independent anion exchanger transporting sulfate, oxalate, bicarbonate, thiosulfate, and (with divergent properties) chloride. Human SLC26A1-mediated anion exchange differs from that of its rodent orthologs in its stimulation by alkaline pHo and inhibition by acidic pHo but not pHi and in its failure to transport glyoxylate. SLC26A1-mediated transport of sulfate and oxalate is highly dependent on allosteric activation by extracellular chloride or non-substrate anions. Extracellular chloride stimulates apparent V max of human SLC26A1-mediated sulfate uptake by conferring a 2-log decrease in sensitivity to inhibition by extracellular protons, without changing transporter affinity for extracellular sulfate. In contrast to SLC26A1-mediated sulfate transport, SLC26A1-associated chloride transport is activated by acid pHo, shows reduced sensitivity to DIDS, and exhibits cation dependence of its DIDS-insensitive component. Human SLC26A1 resembles SLC26 paralogs in its inhibition by phorbol ester activation of protein kinase C (PKC), which differs in its undiminished polypeptide abundance at or near the oocyte surface. Mutation of SLC26A1 residues corresponding to candidate anion binding site-associated residues in avian SLC26A5/prestin altered anion transport in patterns resembling those of prestin. However, rare SLC26A1 polymorphic variants from a patient with renal Fanconi Syndrome and from a patient with nephrolithiasis/calcinosis exhibited no loss-of-function phenotypes consistent with disease pathogenesis. PMID:27125215

  4. Anion Effects on the Ion Exchange Process and the Deformation Property of Ionic Polymer Metal Composite Actuators

    Directory of Open Access Journals (Sweden)

    Wataru Aoyagi

    2016-06-01

    Full Text Available An ionic polymer-metal composite (IPMC actuator composed of a thin perfluorinated ionomer membrane with electrodes plated on both surfaces undergoes a large bending motion when a low electric field is applied across its thickness. Such actuators are soft, lightweight, and able to operate in solutions and thus show promise with regard to a wide range of applications, including MEMS sensors, artificial muscles, biomimetic systems, and medical devices. However, the variations induced by changing the type of anion on the device deformation properties are not well understood; therefore, the present study investigated the effects of different anions on the ion exchange process and the deformation behavior of IPMC actuators with palladium electrodes. Ion exchange was carried out in solutions incorporating various anions and the actuator tip displacement in deionized water was subsequently measured while applying a step voltage. In the step voltage response measurements, larger anions such as nitrate or sulfate led to a more pronounced tip displacement compared to that obtained with smaller anions such as hydroxide or chloride. In AC impedance measurements, larger anions generated greater ion conductivity and a larger double-layer capacitance at the cathode. Based on these mechanical and electrochemical measurements, it is concluded that the presence of larger anions in the ion exchange solution induces a greater degree of double-layer capacitance at the cathode and results in enhanced tip deformation of the IPMC actuators.

  5. Preparation of highly concentrated super-hot (γ-32P)ATP using small-scale ion-exchange chromatography

    International Nuclear Information System (INIS)

    In order to obtain a highly concentrated, pure and super-hot [γ-32P]ATP, we improved the purification method of super-hot [γ-32P]ATP which was synthesized by the method of Johnson and Walseth (1979). The super-hot [γ-32P]ATP was synthesized in a relatively large volume (2 ml) of reaction mixture and purified using semi-micro scale anion exchange chromatography (Dowex 1 x 2, 60 - 70 μl column volume). In combination with washing the reaction product with certain organic solvents, this chromatography technique makes it possible to obtain a highly concentrated and pure super-hot [γ-32P]ATP (approx. 7000 Ci/mmol; 20 - 30 mCi/ml) from [32P]Pi of any commercial source in a good yield. (author)

  6. Adsorption of Monobutyl Phthalate from Aqueous Phase onto Two Macroporous Anion-Exchange Resins

    Directory of Open Access Journals (Sweden)

    Zhengwen Xu

    2014-01-01

    Full Text Available As new emerging pollutants, phthalic acid monoesters (PAMs pose potential ecological and human health risks. In the present study, adsorption performance of monobutyl phthalate (MBP onto two macroporous base anion-exchange resins (D-201 and D-301 was discussed. It was found that the adsorption isotherms were best fitted by the Langmuir equation while the adsorption kinetics were well described by pseudo-first-order model. Analyses of sorption isotherms and thermodynamics proved that the adsorption mechanisms for DBP onto D-201 were ion exchange. However, the obtained enthalpy values indicate that the sorption process of MBP onto D-301 is physical adsorption. The equilibrium adsorption capacities and adsorption rates of DBP on two different resins increased with the increasing temperature of the solution. D-301 exhibited a higher adsorption capacity of MBP than D-201. These results proved that D-301, as an effective sorbent, can be used to remove phthalic acid monoesters from aqueous solution.

  7. Determination of sulfur anions by ion chromatography-postcolumn derivation and UV detection

    Institute of Scientific and Technical Information of China (English)

    Mei Lan Chen; Ming Li Ye; Xue Ling Zeng; Yun Chang Fan; Zhu Yan

    2009-01-01

    A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All species are separated at Dionex IonPac AG22A and AS22Awith mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0 mL/min. The postcolumn derivation solution was 0.24% iodine in 0.2% phosphate acid and the detection wavelength was set at 288 nm. The detection limits (LOD, signal-to-noise ratio of 3) of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 0.004, 0.006, 0.006, and 0.007 mg/L, respectively. Within-day relative standard deviations (RSD, n = 10) of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 3.24%, 3.76%, 2.68%, and 2.07%, respectively. The recoveries of the four anions were in the range of 67.2-116.5%.

  8. Simultaneous determination of three chloroacetic acids, three herbicides, and 12 anions in water by ion chromatography.

    Science.gov (United States)

    Luo, Ximing; Chen, Liang; Zhao, Yanqing

    2015-09-01

    An ion chromatography method was developed for the simultaneous detection of three soluble herbicides (glyphosate, bentazone and picloram), three chlorine disinfection byproducts (monochloroacetic acid, dichloroacetic acid and trichloroacetic acid) and 12 anions in water (Cl(-), Br(-), SO4(2-), CO3(2-), ClO3(-), ClO4(-), BrO3(-), PO4(3-), NO2(-), NO3(-), CH3COO(-) and COO(-)). High linearity (r(2) > 0.996) was observed for all target analytes for each respective concentration range. The limit of detection and limit of quantitation were between 0.21-0.85 and 0.06-25.46 μg/L, respectively. However, the interference effect of Cl(-), NO3(-) , SO4 (2-) and CO3(2-) on some target analytes must be considered during the analysis. Sample pre-treatment by a hydrogen column (H-column) required to reduce the negative effect of CO3(2-). Additionally, sample pre-treatment by a sliver-hydrogen column (Ag-H-column) is required when Cl(-) > 100 mg/L and SO4(2-) 100 mg/L and SO4(2-) > 50 mg/L. When Cl(-) > 100 mg/L, SO4(2-) > 50 mg/L and CO3(2-) > 20 mg/L, the sample pre-treatment by either an Ag-H-Ba-column or an Ag-H-column and Ba-column is required to minimize interference.

  9. Use of Anion Exchange Resins for One-Step Processing of Algae from Harvest to Biofuel

    Directory of Open Access Journals (Sweden)

    Martin Poenie

    2012-07-01

    Full Text Available Some microalgae are particularly attractive as a renewable feedstock for biodiesel production due to their rapid growth, high content of triacylglycerols, and ability to be grown on non-arable land. Unfortunately, obtaining oil from algae is currently cost prohibitive in part due to the need to pump and process large volumes of dilute algal suspensions. In an effort to circumvent this problem, we have explored the use of anion exchange resins for simplifying the processing of algae to biofuel. Anion exchange resins can bind and accumulate the algal cells out of suspension to form a dewatered concentrate. Treatment of the resin-bound algae with sulfuric acid/methanol elutes the algae and regenerates the resin while converting algal lipids to biodiesel. Hydrophobic polymers can remove biodiesel from the sulfuric acid/methanol, allowing the transesterification reagent to be reused. We show that in situ transesterification of algal lipids can efficiently convert algal lipids to fatty acid methyl esters while allowing the resin and transesterification reagent to be recycled numerous times without loss of effectiveness.

  10. A novel self-adaptive microalgae photobioreactor using anion exchange membranes for continuous supply of nutrients.

    Science.gov (United States)

    Fu, Qian; Chang, Hai-Xing; Huang, Yun; Liao, Qiang; Zhu, Xun; Xia, Ao; Sun, Ya-Hui

    2016-08-01

    A novel self-adaptive microalgae photobioreactor using anion exchange membranes (AEM-PBR) for continuous supply of nutrients was proposed to improve microalgae biomass production. The introduction of anion exchange membranes to the PBR can realize continuous supply of nutrients at desired rates, which is beneficial to the growth of microalgae. The results showed that the maximum biomass concentration obtained in the AEM-PBR under continuous supply of nitrogen at an average rate of 19.0mgN/L/d was 2.98g/L, which was 129.2% higher than that (1.30g/L) in a PBR with all the nitrogen supplied in batch at initial. In addition, the feeding rates of nitrogen and phosphorus were optimized in the AEM-PBR to maximize biomass production. The maximum biomass concentration of 4.38g/L was obtained under synergistic regulation of nitrogen and phosphorus feeding rates at 19.0mgN/L/d and 4.2mgP/L/d. The AEM-PBR demonstrates a promising approach for high-density cultivation of microalgae. PMID:27187567

  11. Qualification of Reillex{trademark} HPQ anion exchange resin for use in SRS processes

    Energy Technology Data Exchange (ETDEWEB)

    Crooks, W.J. III

    2000-05-18

    The Phase 2 portion of the HB-Line facility was built in the early 1980's to process plutonium and neptunium from nitric acid solutions into oxide suitable for storage in a vault. Although the other portions of HB-Line were started up in the mid 1980's and have operated since that time, the anion exchange and precipitation processes in Phase 2 were never started up. As part of the material stabilization efforts, Phase 2 is currently being started up. A new anion exchange resin is needed because the resins that were proposed for use 10 years ago are limited by performance characteristics, disposal requirements, or are no longer commercially available. SRTC is responsible for qualifying all resins prior to their use in Nuclear Materials Stabilization and Storage (NMSS) processes. Qualification consists of both process suitability and thermal stability with nitric acid. This report describes the thermal stability qualification of Reillex{trademark} HPQ, the new resin proposed for processing plutonium and neptunium in the HB Line facility.

  12. Analysis of oxyhalide disinfection by-products and other anions of interest in drinking water by ion chromatography.

    Science.gov (United States)

    Hautman, D P; Bolyard, M

    1992-06-01

    The US Environmental Protection Agency is developing regulations for various drinking water disinfection by-products (DBPs). This effort involves developing analytical methods for the DBPs formed as a result of different disinfection treatments and collecting occurrence data for these species. Ion chromatography is one method being used to analyze drinking water samples for the following inorganic DBPs: chlorite, chlorate and bromate. These anions, however, are difficult to separate from common interfering anions of chloride, carbonate and nitrate. A method is therefore presented by which tetraborate/boric acid is used to separate these anions. Method detection limits of the order of 10 micrograms/l, using conductivity and UV detection were obtained. Stability studies of chlorite showing the effectiveness of ethylenediamine as a preservative and summary data for an occurrence of nitrite, nitrate and the DBP precursor bromide are presented.

  13. Strong ion-exchange centrifugal partition chromatography as an efficient method for the large-scale purification of glucosinolates.

    Science.gov (United States)

    Toribio, Alix; Nuzillard, Jean-Marc; Renault, Jean-Hugues

    2007-11-01

    The glucosinolates sinalbin and glucoraphanin were purified by strong ion-exchange displacement centrifugal partition chromatography (SIXCPC). The optimized conditions involved the biphasic solvent system ethyl acetate/n-butanol/water (3:2:5, v/v), the lipophilic anion-exchanger Aliquat 336 (trioctylmethylammonium chloride, 160 and 408 mM) and a sodium iodide solution (80 and 272 mM) as displacer. Amounts as high as 2.4 g of sinalbin and 2.6g of glucoraphanin were obtained in one step in 2.5 and 3.5h respectively, starting from 12 and 25 g of mustard and broccoli seed aqueous extracts, using a laboratory scale CPC column (200 mL inner volume). PMID:17904564

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

    International Nuclear Information System (INIS)

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-20

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

  16. Simultaneous determination of peroxydisulfate and conventional inorganic anions by ion chromatography with the column-switching technique.

    Science.gov (United States)

    Huang, Zhongping; Ni, Chengzhu; Wang, Fengli; Zhu, Zuoyi; Subhani, Qamar; Wang, Muhua; Zhu, Yan

    2014-02-01

    The application of ion chromatography with the column-switching technique for the simultaneous analysis of peroxydisulfate and conventional inorganic anions in a single run is described. With this method, conventional inorganic anions were separated by consecutive elution through both the guard column and separation column, but peroxydisulfate that only passed through the guard column had a good peak shape and short retention time. A series of standard solutions consisting of target anions of various concentrations from 0.01 to 75 mg/L were analyzed, with a correlation coefficient (r) ≥ 0.9990. The limits of detection were in the range of 0.49-9.84 μg/L based on the S/N of 3 and a 25 μL injection volume. RSDs for retention time, peak area, and peak height were all <1.77%. A spiking study was performed with satisfactory recoveries between 97.6 and 103.4% for all anions. The quantitative determination of peroxydisulfate and conventional inorganic anions in surface waters was accomplished within 18 min by this column-switching technique.

  17. Separation of phenolic acids from natural plant extracts using molecularly imprinted anion-exchange polymer confined ionic liquids.

    Science.gov (United States)

    Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2012-04-01

    Polymer-confined ionic liquids were used for the separation of phenolic acids from natural plant extract by utilizing an anion-exchange mechanism. They were synthesized using molecular imprinting technique to reduce non-directional ion-ion interactions during anion-exchange and other interactions with interference substances that could decrease selectivity. A suitable sorbent for phenolic acid separation could be identified based on the adsorption behaviors of phenolic acids on different polymer-confined ionic liquids. Thus, the developed ionic liquid-based molecularly imprinted anion-exchange polymer (IMAP) achieved high recovery rates by solid-phase extraction of phenolic acids from Salicornia herbacea L. extract: 90.1% for protocatechuic acid, 95.5% for ferulic acid and 96.6% for caffeic acid. Moreover, the phenolic acids were separable from each other by repeated solid phase extraction cycles. The proposed method could be used to separate other phenolic acids or organic acids from complex samples. PMID:21903215

  18. Ion-exchange chromatography by dicarboxyl cellulose gel.

    Science.gov (United States)

    Kim, U J; Kuga, S

    2001-06-01

    A new column packing material for ion-exchange chromatography was prepared from cellulose gel by periodate oxidation followed by chlorite oxidation to form spatially paired carboxyl groups (dicarboxyl cellulose, DCC). The carboxyl group was quantitatively introduced to spherical cellulose gel by controlling the extent of oxidation. The DCC gels were examined for their ion-exchange activity for various amines at pH of 2.5-5.5. In this pH range, aromatic amines with acid dissociation constant (pKa) below 2.7 showed no interaction with DCC gels as expected from their lack of protonation. The amines with pKa greater than 3.3, both aromatic and aliphatic, showed strong interaction corresponding to the amount of carboxyl introduced to the gel. However, these amines showed anomalous dependence on pH of the mobile phase, showing a maximum in retention factor at around pH 4. This is in contrast with the nearly constant retention factor of these amines on conventional carboxylated cellulose packing at pH greater than 4.0. The maximum retention factor at pH 4 of DCC gel was 4-5-times greater than that of conventional gel having a similar amount of carboxyls. Since pKa of dicarboxyl groups ranges 3-5 as determined by acid-base titration, the pH giving maximum retention corresponds to the pH at which one of paired carboxyls is dissociated. Possible cause of this anomaly is presented in terms of dissociation state of dicarboxyl groups and its interaction with amines. PMID:11459309

  19. Bifunctional Crosslinking Agents Enhance Anion Exchange Membrane Efficacy for Vanadium Redox Flow Batteries.

    Science.gov (United States)

    Wang, Wenpin; Xu, Min; Wang, Shubo; Xie, Xiaofeng; Lv, Yafei; Ramani, Vijay K

    2014-06-01

    A series of cross-linked fluorinated poly (aryl ether oxadiazole) membranes (FPAEOM) derivatized with imidazolium groups were prepared. Poly (N-vinylimidazole) (PVI) was used as the bifunctional cross-linking agent to: a) lower vanadium permeability, b) enhance dimensional stability, and c) concomitantly provide added ion exchange capacity in the resultant anion exchange membranes. At a molar ratio of PVI to FPAEOM of 1.5, the resultant membrane (FPAEOM-1.5 PVI) had an ion exchange capacity of 2.2 meq g-1, a vanadium permeability of 6.8×10-7 cm2 min-1, a water uptake of 68 wt.%, and an ionic conductivity of 22.0 mS cm-1, all at 25°C. Single cells prepared with the FPAEOM-1.5 PVI membrane exhibited a higher coulombic efficiency (> 92%) and energy efficiency (> 86%) after 40 test cycles in vanadium redox flow battery. The imidazolium cation showed high chemical stability in highly acidic and oxidizing vanadium solution as opposed to poor stability in alkaline solutions. Based on our DFT studies, this was attributed to the lower HOMO energy (-7.265 eV) of the HSO4- ion (compared to the OH- ion; -5.496 eV) and the larger HOMO-LUMO energy gap (6.394 eV) of dimethylimidazolium bisulfate ([DMIM] [HSO4]) as compared to [DMIM] [OH] (5.387 eV).

  20. Bifunctional Crosslinking Agents Enhance Anion Exchange Membrane Efficacy for Vanadium Redox Flow Batteries.

    Science.gov (United States)

    Wang, Wenpin; Xu, Min; Wang, Shubo; Xie, Xiaofeng; Lv, Yafei; Ramani, Vijay K

    2014-06-01

    A series of cross-linked fluorinated poly (aryl ether oxadiazole) membranes (FPAEOM) derivatized with imidazolium groups were prepared. Poly (N-vinylimidazole) (PVI) was used as the bifunctional cross-linking agent to: a) lower vanadium permeability, b) enhance dimensional stability, and c) concomitantly provide added ion exchange capacity in the resultant anion exchange membranes. At a molar ratio of PVI to FPAEOM of 1.5, the resultant membrane (FPAEOM-1.5 PVI) had an ion exchange capacity of 2.2 meq g-1, a vanadium permeability of 6.8×10-7 cm2 min-1, a water uptake of 68 wt.%, and an ionic conductivity of 22.0 mS cm-1, all at 25°C. Single cells prepared with the FPAEOM-1.5 PVI membrane exhibited a higher coulombic efficiency (> 92%) and energy efficiency (> 86%) after 40 test cycles in vanadium redox flow battery. The imidazolium cation showed high chemical stability in highly acidic and oxidizing vanadium solution as opposed to poor stability in alkaline solutions. Based on our DFT studies, this was attributed to the lower HOMO energy (-7.265 eV) of the HSO4- ion (compared to the OH- ion; -5.496 eV) and the larger HOMO-LUMO energy gap (6.394 eV) of dimethylimidazolium bisulfate ([DMIM] [HSO4]) as compared to [DMIM] [OH] (5.387 eV). PMID:24884171

  1. Efficient Separation of Lanthanides Using Poly (Styrene-Divinyl Benzene) Aminated Anion Exchanger

    International Nuclear Information System (INIS)

    New chromatographic method was developed for the determination and separation of lanthanides using AS4A anionic column. The behavior of the column towards lanthanides was studied through many parameters, From the data obtained it is found that, affinity of the column toward investigated ions increase by increasing eluent concentration and it decrease retention factors. With the two investigated eluent (oxalic and citric acids), elution order for lanthanide elements was obtained in their atomic number from La to Lu. Retention times and retention orders obtained at these conditions clearly show that, lanthanides in AS4A are displaced according to anion exchange mechanism. More over separation of lanthanides using AS4A was studied using isocratic and gradient elution programs. Light and the first intermediate lanthanide elements were separated successfully by applying a gradient program containing 70% oxalic acid (100 mM) and 30% water. The problem of separation for heavy and the last intermediate lanthanide elements was solved using 100 mM alpha hydroxy isobutyric acid (α-HIBA)

  2. The direct formate fuel cell with an alkaline anion exchange membrane

    Science.gov (United States)

    Bartrom, Amy M.; Haan, John L.

    2012-09-01

    We demonstrate for the first time an operating Direct Formate Fuel Cell employing formate salts as the anode fuel, air or oxygen as the oxidant, a polymer anion exchange membrane, and metal catalysts at the anode and cathode. Operation of the DFFC at 60 °C using 1 M KOOCH and 2 M KOH as the anode fuel and electrolyte and oxygen gas at the cathode produces 144 mW cm-2 of peak power density, 181 mA cm-2 current density at 0.6 V, and an open circuit voltage of 0.931 V. This performance is competitive with alkaline Direct Liquid Fuel Cells (DLFCs) previously reported in the literature and demonstrates that formate fuel is a legitimate contender with alcohol fuels for alkaline DLFCs. A survey of the literature shows that a formate-oxygen fuel cell has a high theoretical potential, and the safe, renewable formate fuel does not poison the anode catalyst.

  3. An improved, computer-based, on-line gamma monitor for plutonium anion exchange process control

    International Nuclear Information System (INIS)

    An improved, low-cost, computer-based system has replaced a previously developed on-line gamma monitor. Both instruments continuously profile uranium, plutonium, and americium in the nitrate anion exchange process used to recover and purify plutonium at the Los Alamos Plutonium Facility. The latest system incorporates a personal computer that provides full-feature multichannel analyzer (MCA) capabilities by means of a single-slot, plug-in integrated circuit board. In addition to controlling all MCA functions, the computer program continuously corrects for gain shift and performs all other data processing functions. This Plutonium Recovery Operations Gamma Ray Energy Spectrometer System (PROGRESS) provides on-line process operational data essential for efficient operation. By identifying abnormal conditions in real time, it allows operators to take corrective actions promptly. The decision-making capability of the computer will be of increasing value as we implement automated process-control functions in the future. 4 refs., 6 figs

  4. REMOVAL OF GLUCORAPHENIN FROM THE EXTRACT OF RADISH PIGMENT BY ANION EXCHANGE RESIN 201×7

    Institute of Scientific and Technical Information of China (English)

    ZhouXiaohua; ChenQi

    1998-01-01

    A method for removimg glucoraphenin from the extract of Radish pigment by anion exchange resin 201×7 was studied.The adsorption capacity of 201×7 resin for glucoraphenin was 72.8mg/ml resin,the equilibrium time 55 minutes,and the optinum pH5.5.All glucoraphenin that had been adsorbed on 201×7 resin was eluted by 1.5BV.hr-1, eluent in whinc concentration of NaOH was 0.05mol·L-1 at the flow rate of 1.5BV/h.Extracting solution of deglucoraphenin was enriched by vacuum and spray drying.A powder product of Radish pigment was obtained and E1cm1%=4.30.

  5. SORPTION OF PHENOL AND P-NITROPHENOL ONTO A WEAKLY ANION EXCHANGER: XPS ANALYSIS AND MECHANISM

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    X-ray photoelectron spectroscopy (XPS ) was adopted to elucidate sorption mechanism of phenol and p-nitrophenol onto a weakly anion exchanger D301. The distribution of specific forms of tertiary amino group on D301 was obtained and effect of free tertiary amino group on phenol sorption onto D301 was discussed. The result indicated that the percent of the protonated tertiary amine group on polymeric matrix was much lower than the reference compound N,N-dimethylbenzylamine at an identical pH value in solution due to the much lower activity degree of hydrogen ion in inner resin phase than in the external solution. Less free amino group on D301 results in less sorption capacity of phenol and p-nitrophenol in an acidic solution. Under the experimental conditions both phenol sorption onto D301 can be explained as solid extraction and the distribution coefficient varies linearly with the content of free amino group on D301.

  6. Collaborative study of an anion exchange method for the determination of trace plutonium in water

    International Nuclear Information System (INIS)

    A single-laboratory evaluation and an interlaboratory collaborative study were made of a method for determining plutonium in water. The method was written for the analysis of one-liter samples and involves coprecipitation, acid dissolution, anion exchange, electrodeposition, and alpha pulse height analysis. After the single-laboratory evaluation of the selected method, four samples were prepared for the collaborative study: two river-water samples, a substitute ocean water sample, and sample containing sediment. These samples contained plutonium-239 and plutonium-238 at concentrations ranging from 0.42 to 28.9 dis/min/liter. In the collaborative study standard deviations of plutonium concentrations ranged from 5 to 13%. In three cases, standard deviations agreed with those expected from counting statistics. It is believed that hydrolysis occurred in the river water samples resulting in errors greater than those expected from counting statistics

  7. RECOVERY OF URANIURN FROM CARBONATE SOLUTIONS USING STRONGLY BASIC ANION EXCHANGER 3.THE MECHANISMS OF RECOVERY PROCESSES

    Institute of Scientific and Technical Information of China (English)

    SongYinjie; ZhangHui; 等

    1997-01-01

    A moving boundary model under considering the volume change of spherical resin beads during ion exchange processes was employed to recognize the mechanisms of reecovering uranium from carbonate solutions using strongly basic anion exchanger.Two important factors,swelling and ion exchange,which directly affect the violume of ion exchangers were taken into account.An ion exchange mechanism has been found for the forward reaction PCl/[UO2(CO3)3]4-,and is partical diffusion governing at high concentration of the complex anion.The mechanism of RCl/U(VI) at pH 5.5-7.5 is a chemical reaction taking place at the moving boundary of the unreacted nucleus.For the reverse reaction RnU/NaCl,the uranyl tricarbonate complex anion in the resin phase is replaced by Cl- ions with an ion exchange mechanism alway determined by particle diffusion.The other forms of uranium in the solid phase loaded on the resin at pH5.5-7.5 should belong to non-exchangeable uranium.The mechanism of the reverse reaction RnU/HCl is always chemical reaction which is not restricted to the moving boundary of the unreacted core.

  8. Synthesis and Properties of Anion Exchangers Derived from Chloromethyl Styrene Co divinylbenzene and Their Use in Water Treatment

    International Nuclear Information System (INIS)

    Amination of vinylbenzyl chloride-divinylbenzene (VBC-DVB) copolymers is an effective method for preparation of ion-exchange resins. Conventionally, the starting polymer is produced by chloromethylation of a styrene-divinylbenzene copolymer that utilizes chloromethyl methyl ether, a known carcinogen. An alterative approach is to co polymerize vinylbenzyl chloride with divinylbenzene to generate the necessary Vb-Dvb. This method provides precise control over the density of the ion-exchange groups. The regiochemistry of the vinylbenzyl chloride methods was realized using solvent-ion exchange groups. In this investigation, an improved solvent system was found for the preparation of anion exchange resins by the vinylbenzyl chloride route. The effectiveness of amination of the intermediate VBC-DVB polymers with a variety of trimethylamine reagents was investigated, and ethanolic trimethylamine produced the highest degree of amination. These resulting ion-exchange polymers were characterized by a variety of techniques such as analytical titrations, nitrogen analysis, Fourier transform infrared spectroscopy and thermal gravimetric analysis. Testing of these copolymers for breakthrough was performed. The results indicate that these anion exchangers have a meaningful increase in thermal stability over commercial anionic exchange beads

  9. Synthesis and Properties of Anion Exchangers Derived from Chloromethyl Styrene Codivinylbenzene and Their Use in Water Treatment

    Directory of Open Access Journals (Sweden)

    Hesham A. Ezzeldin

    2010-01-01

    Full Text Available Amination of vinylbenzyl chloride-divinylbenzene (VBC-DVB copolymers is an effective method for preparation of ion-exchange resins. Conventionally, the starting polymer is produced by chloromethylation of a styrene-divinylbenzene copolymer that utilizes chloromethyl methyl ether, a known carcinogen. An alterative approach is to copolymerize vinylbenzyl chloride with divinylbenzene to generate the necessary VBC-DVB. This method provides precise control over the density of the ion-exchange groups. The regiochemistry of the vinylbenzyl chloride methods was realized using solvent-ion exchange groups. In this investigation, an improved solvent system was found for the preparation of anion exchange resins by the vinylbenzyl chloride route. The effectiveness of amination of the intermediate VBC-DVB polymers with a variety of trimethylamine reagents was investigated, and ethanolic trimethylamine produced the highest degree of amination. These resulting ion-exchange polymers were characterized by a variety of techniques such as analytical titrations, nitrogen analysis, Fourier transform infrared spectroscopy and thermal gravimetric analysis. Testing of these copolymers for breakthrough was performed. The results indicate that these anion exchangers have a meaningful increase in thermal stability over commercial anionic exchange beads.

  10. Efficient defluoridation of water using reusable nanocrystalline layered double hydroxides impregnated polystyrene anion exchanger.

    Science.gov (United States)

    Cai, Jianguo; Zhang, Yanyang; Pan, Bingcai; Zhang, Weiming; Lv, Lu; Zhang, Quanxing

    2016-10-01

    Water decontamination from fluoride is still a challenging task of global concern. Recently, Al-based layered double hydroxides (LDHs) have been extensively studied for specific fluoride adsorption from water. Unfortunately, they cannot be readily applied in scaled-up application due to their ultrafine particles as well as the regeneration issues caused by their poor stability at alkaline pHs. Here, we developed a novel (LDH)-based hybrid adsorbent, i.e., LALDH-201, by impregnating nanocrystalline Li/Al LDHs (LADLH) inside a commercial polystyrene anion exchanger D201. TEM image and XRD spectra of the resultant nanocomposite confirmed that the LDHs particles were nanosized inside the pores of D201 of highly crystalline nature and well-ordered layer structure. After impregnation, the chemical and mechanical stability of LALDH were significantly improved against pH variation, facilitating its application at a wide pH range (3.5-12). Fluoride adsorption onto LALDH-201 was compared to D201 and activated alumina, evidencing the preferable removal fluoride of LALDH-201. Fluoride adsorption onto LALDH-201 followed pseudo-second-order model, with the maximum capacity (62.5 mg/g from the Sips model) much higher than the other two adsorbents. Fixed-bed adsorption run indicated the qualified treatable volume of the fluoride contaminated groundwater (4.1 mg/L initially) with LALDH-201 was about 11 times as much as with the anion exchanger D201 when the breakthrough point was set as 1.5 mg/L. The capacity of LALDH-201 could be effectively refreshed for continuous column operation without observable loss by using the mixed solution of 0.01 M NaOH + 1 M NaCl. The above results suggested that the hybrid adsorbent LALDH-201 is very promising for water defluoridation in scaled-up application.

  11. Imidazolium-Based Polymeric Materials as Alkaline Anion-Exchange Fuel Cell Membranes

    Science.gov (United States)

    Narayan, Sri R.; Yen, Shiao-Ping S.; Reddy, Prakash V.; Nair, Nanditha

    2012-01-01

    Polymer electrolyte membranes that conduct hydroxide ions have potential use in fuel cells. A variety of polystyrene-based quaternary ammonium hydroxides have been reported as anion exchange fuel cell membranes. However, the hydrolytic stability and conductivity of the commercially available membranes are not adequate to meet the requirements of fuel cell applications. When compared with commercially available membranes, polystyrene-imidazolium alkaline membrane electrolytes are more stable and more highly conducting. At the time of this reporting, this has been the first such usage for imidazolium-based polymeric materials for fuel cells. Imidazolium salts are known to be electrochemically stable over wide potential ranges. By controlling the relative ratio of imidazolium groups in polystyrene-imidazolium salts, their physiochemical properties could be modulated. Alkaline anion exchange membranes based on polystyrene-imidazolium hydroxide materials have been developed. The first step was to synthesize the poly(styrene-co-(1-((4-vinyl)methyl)-3- methylimidazolium) chloride through a free-radical polymerization. Casting of this material followed by in situ treatment of the membranes with sodium hydroxide solutions provided the corresponding hydroxide salts. Various ratios of the monomers 4-chloromoethylvinylbenzine (CMVB) and vinylbenzine (VB) provided various compositions of the polymer. The preferred material, due to the relative ease of casting the film, and its relatively low hygroscopic nature, was a 2:1 ratio of CMVB to VB. Testing confirmed that at room temperature, the new membranes outperformed commercially available membranes by a large margin. With fuel cells now in use at NASA and in transportation, and with defense potential, any improvement to fuel cell efficiency is a significant development.

  12. Efficient defluoridation of water using reusable nanocrystalline layered double hydroxides impregnated polystyrene anion exchanger.

    Science.gov (United States)

    Cai, Jianguo; Zhang, Yanyang; Pan, Bingcai; Zhang, Weiming; Lv, Lu; Zhang, Quanxing

    2016-10-01

    Water decontamination from fluoride is still a challenging task of global concern. Recently, Al-based layered double hydroxides (LDHs) have been extensively studied for specific fluoride adsorption from water. Unfortunately, they cannot be readily applied in scaled-up application due to their ultrafine particles as well as the regeneration issues caused by their poor stability at alkaline pHs. Here, we developed a novel (LDH)-based hybrid adsorbent, i.e., LALDH-201, by impregnating nanocrystalline Li/Al LDHs (LADLH) inside a commercial polystyrene anion exchanger D201. TEM image and XRD spectra of the resultant nanocomposite confirmed that the LDHs particles were nanosized inside the pores of D201 of highly crystalline nature and well-ordered layer structure. After impregnation, the chemical and mechanical stability of LALDH were significantly improved against pH variation, facilitating its application at a wide pH range (3.5-12). Fluoride adsorption onto LALDH-201 was compared to D201 and activated alumina, evidencing the preferable removal fluoride of LALDH-201. Fluoride adsorption onto LALDH-201 followed pseudo-second-order model, with the maximum capacity (62.5 mg/g from the Sips model) much higher than the other two adsorbents. Fixed-bed adsorption run indicated the qualified treatable volume of the fluoride contaminated groundwater (4.1 mg/L initially) with LALDH-201 was about 11 times as much as with the anion exchanger D201 when the breakthrough point was set as 1.5 mg/L. The capacity of LALDH-201 could be effectively refreshed for continuous column operation without observable loss by using the mixed solution of 0.01 M NaOH + 1 M NaCl. The above results suggested that the hybrid adsorbent LALDH-201 is very promising for water defluoridation in scaled-up application. PMID:27337346

  13. Electron exchange between dipole-bound anion and polar molecule and dipole-bound anions dimer formation

    International Nuclear Information System (INIS)

    We consider collision between a dipole-bound molecular anion and a neutral polar molecule and show that the excess electron can bind two neutral molecules into a dimer. Using a variational approach similar to the Heitler-London model of H''+2 ion we obtain the energy terms of such a dimer. Their difference determines the cross-section of electron transfer from the anion to the neutral molecule in quasiclassical near-resonant Born-Oppenheimer approximation. We obtain for the cross-section an analytic expression containing the weak (logarythmic) factor depending on the molecular dipole moment, and collision velocity. Our analytic calculations are in a good accordance with the results of a recent experiment.

  14. Selection of magnetic anion exchange resins for the removal of dissolved organic and inorganic matters

    Institute of Scientific and Technical Information of China (English)

    Qiongjie Wang; Aimin Li; Jinnan Wang; Chengdong Shuang

    2012-01-01

    Four magnetic anion exchange resins (MAERs) were used as adsorbents to purify drinking water.The effect of water quality (pH,temperature,ionic strength,etc.) on the performance of MAER for the removal of dissolved organic matter (DOM) was also investigated.Among the four studied MAERs,the strong base resin named NDMP-1 with high water content and enhanced exchange capacity exhibited the highest removal rate of dissolved organic carbon (DOC) (48.9% removal rate) and UV-absorbing substances (82.4% removal rate) with a resin dose of 10 mL/L after 30 min of contact time.The MAERs could also effectively remove inorganic matter such as sulfate,nitrate and fluoride.Because of the higher specific UV absorbance (SUVA) value,the DOM in the raw water was found to be removed more effectively than that in the clarified water by NDMP resin.The temperature showed a weak influence on the removal of DOC from 6 to 26℃,while a relatively strong one at 36℃.The removal of DOM by NDMP was also affected to some extent by the pH value.Moreover,increasing the sulfate concentration in the raw water could decrease the removal rates of DOC and UV-absorbing substances.

  15. Purification of a recombinant baculovirus of Autographa californica M nucleopolyhedrovirus by ion exchange membrane chromatography.

    Science.gov (United States)

    Grein, Tanja A; Michalsky, Ronald; Vega López, Maria; Czermak, Peter

    2012-08-01

    Significant progress in the application of viral vectors for gene delivery into mammalian cells and the use of viruses as biopesticides requires downstream processing that can satisfy application-specific demands on performance. In the present work the stability and ion exchange membrane chromatography of a recombinant of Autographa californica M nucleopolyhedrovirus is studied. To adjust the degree of purification the effect of ionic conductivity or pH on the viral infectivity was assessed (0.77-78.00mS/cm, pH 3-8). Infectivity decreased rapidly by several orders of magnitude at below 5mS/cm (i.e., 0.49MPa osmotic pressure change) or at below pH 5.5 (rationalized with particle aggregation). The virus was concentrated and purified via adsorption (0.2-1.1×10(16)pfu/m(3) chromatographic bed volume, 0.6-1.1×10(12)pfu/m(2) membrane area facing the incident fluid flow) and elution at pH 6.1 and 6.35mS/cm from three strong anion exchange membranes. Virus recovery and concentration in accord with the volume reduction were obtained using a polyether sulfone-based membrane with quaternary ammonium ligands. The level of host cell protein (down to below the detection limit) and suspended DNA (below 93pg DNA per 10(6)pfu) are reported for each membrane employed, for the purpose of comparability, under equal adsorption or elution conditions respectively.

  16. 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.

  17. High-Capacity and Rapid Removal of Refractory NOM Using Nanoscale Anion Exchange Resin.

    Science.gov (United States)

    Johnson, Billy R; Eldred, Tim B; Nguyen, Andy T; Payne, William M; Schmidt, Emily E; Alansari, Amir Y; Amburgey, James E; Poler, Jordan C

    2016-07-20

    As human health concerns over disinfection byproducts (DBP) in drinking water increase, so does the need to develop new materials that remove them rapidly and at high capacity. Ion exchange (IEX) is an effective method for the removal of natural organic matter (NOM), especially anion exchange resins (AERs) with quaternary ammonium functional groups. However, capacity is limited in existing commercial resin materials because adsorbates can only interact with the outermost surface area, which makes these products inefficient on a mass basis. We have synthesized a novel "NanoResin" exploiting the enhanced NOM removal of the quaternary ammonium resin while utilizing the vast surface area of SWCNTs, which act as scaffolding for the resin. Our nanomaterials show increased adsorption capacity compared to commercially available adsorbents, in a fraction of the time. This NanoResin requires only about 10 s to reach ion-exchange equilibrium. Comparatively, commercial AERs only achieved partial removal after more than 30 min. High capacity adsorption of a low molecular weight (MW) surrogate has been measured. NOM removal was demonstrated in solutions of both low and high specific UV absorbance (SUVA) composition with these nanomaterials. Additionally, the NanoResin showed enhanced removal of a NOM concentrate sample taken from Myrtle Beach, SC, demonstrating NanoResin is an effective method of removal for refractory NOM in a natural aqueous environment. Synthesis and characterization of the polymers and nanomaterials are presented below. Adsorption capacity, adsorption kinetics, and the regeneration and reusability of these new materials for NOM removal are described. The open matrix microstructure precludes any intraparticle diffusion of adsorbates; thus, these nanomaterials act as a "contact resin". PMID:27348616

  18. Anion Exchanger 2 Regulates Dectin-1-Dependent Phagocytosis and Killing of Candida albicans.

    Directory of Open Access Journals (Sweden)

    Katia Urso

    Full Text Available Anion exchanger 2 (Ae2; gene symbol, Slc4a2 is a plasma membrane Cl-/HCO3- exchanger expressed in the gastrointestinal tract, kidney and bone. We have previously shown that Ae2 is required for the function of osteoclasts, bone resorbing cells of the macrophage lineage, to maintain homeostatic cytoplasmic pH and electroneutrality during acid secretion. Macrophages require endosomal acidification for pathogen killing during the process known as phagocytosis. Chloride is thought to be the principal ion responsible for maintaining electroneutrality during organelle acidification, but whether Cl-/HCO3- exchangers such as Ae2 contribute to macrophage function is not known. In this study we investigated the role of Ae2 in primary macrophages during phagocytosis. We find that Ae2 is expressed in macrophages where it regulates intracellular pH and the binding of Zymosan, a fungal cell wall derivative. Surprisingly, the transcription and surface expression of Dectin-1, the major phagocytic receptor for Candida albicans (C. albicans and Zymosan, is reduced in the absence of Ae2. As a consequence, Zymosan-induced Tnfα expression is also impaired in Ae2-deficient macrophages. Similar to Ae2 deficiency, pharmacological alkalinization of lysosomal pH with bafilomycin A decreases both Dectin-1 mRNA and cell surface expression. Finally, Ae2-deficient macrophages demonstrate defective phagocytosis and killing of the human pathogenic fungus C. albicans. Our results strongly suggest that Ae2 is a critical factor in the innate response to C. albicans. This study represents an important contribution to a better understanding of how Dectin-1 expression and fungal clearance is regulated.

  19. Determination of common anions in oxalate by ion chromatography coupled with UV photolysis pretreatment

    Institute of Scientific and Technical Information of China (English)

    Sheng Lin Cao; Ming Li Ye; Wei De Lv; Guang Wen Pan; Ting Ting Zhang; Zhong Yang Hu; Li Na Liang; Yan Zhu

    2012-01-01

    A new and simple method was developed to determine anions in oxalate of analytical reagent grade.After UV photolysis with optimal 1% H2O2 in 10,000 mg/L oxalate in the fabricated photoreactor,sample was directly injected into IC system.Satisfactory linearity,detections limits,good repeatability and spiked recovery were obtained.The method was successfully applied to determine anions in two commercial oxalate samples.

  20. Dowex anion exchanger-loaded-baker's yeast as bi-functionalized biosorbents for selective extraction of anionic and cationic mercury(II) species

    International Nuclear Information System (INIS)

    Dowex anion exchanger-immobilized-baker's yeast [Dae-yeast] were synthesized and potentially applied as environmental friendly biosorbents to evaluate the up-take process of anionic and cationic mercury(II) species as well as other metal ions. Optimization of mass ratio of Dowex anion exchanger versus yeast (1:1-1:10) in presence of various interacting buffer solutions (pH 4.0-9.0) was performed and evaluated. Surface modification of [Dae-yeast] was characterized by scanning electron microscopy (SEM) and infrared spectroscopy. The maximum metal biosorption capacity values of [Dae-yeast] towards mercury(II) were found in the range of 0.800-0.960, 0.840-0.950 and 0.730-0.900 mmol g-1 in presence of buffer solutions pH 2.0, 4.0 and 7.0, respectively. Three possible and different mechanisms are proposed to account for the biosorption of mercury and mercuric species under these three buffering conditions based on ion exchange, ion pair and chelation interaction processes. Factors affecting biosorption of mercury from aqueous medium including the pH effect of aqueous solutions (1.0-7.0), shaking time (1-30 min) and interfering ions were searched. The potential applications of modified biosorbents for selective biosorption and extraction of mercury from different real matrices including dental filling waste materials, industrial waste water samples and mercury lamp waste materials were also explored. The results denote to excellent percentage extraction values, from nitric acid as the dissolution solvent with a pH 2.0, as determined in the range of 90.77-97.91 ± 3.00-5.00%, 90.00-93.40 ± 4.00-5.00% and 92.31-100.00 ± 3.00-4.00% for the three tested samples, respectively.

  1. Model of a vanadium redox flow battery with an anion exchange membrane and a Larminie-correction

    Science.gov (United States)

    Wandschneider, F. T.; Finke, D.; Grosjean, S.; Fischer, P.; Pinkwart, K.; Tübke, J.; Nirschl, H.

    2014-12-01

    Membranes are an important part of vanadium redox flow battery cells. Most cell designs use Nafion®-type membranes which are cation exchange membranes. Anion exchange membranes are reported to improve cell performance. A model for a vanadium redox flow battery with an anion exchange membrane is developed. The model is then used to calculate terminal voltages for open circuit and charge-discharge conditions. The results are compared to measured data from a laboratory test cell with 40 cm2 active membrane area. For higher charge and discharge currents, an empirical correction for the terminal voltage is proposed. The model geometry comprises the porous electrodes and the connected pipes, allowing a study of the flow in the entrance region for different state-of-charges.

  2. Development of an Ion Chromatography Method for Analysis of Organic Anions (Fumarate, Oxalate, Succinate, and Tartrate) in Single Chromatographic Conditions.

    Science.gov (United States)

    Kaviraj, Yarbagi; Srikanth, B; Moses Babu, J; Venkateswara Rao, B; Paul Douglas, S

    2015-01-01

    A single organic counterion analysis method was developed by using an ion chromatography separation technique and conductivity detector. This allows the rapid characterization of an API to support clinical studies and to fulfil the regulatory requirements for the quantitation of fumarate, oxalate, succinate, and tartrate counterions in active pharmaceutical ingredients (quetiapine fumarate, escitalopram oxalate, sumatriptan succinate, and tolterodine tartrate). The method was developed by using the Metrohm Metrosep A Supp 1 (250 × 4.0 mm, 5.0 µm particle size) column with a mobile phase containing an isocratic mixture of solution A: 7.5 mM sodium carbonate and 2.0 mM sodium bicarbonate in Milli-Q water and solution B: acetonitrile. The flow rate was set at 1.0 mL/min and the run time was 25 minutes. The developed method was validated as per ICH guidelines, and the method parameters were chosen to ensure the spontaneous quantitation of all four anions. The method was validated for all four anions to demonstrate the applicability of this method to common anions present in various APIs.

  3. Human kidney anion exchanger 1 interacts with kinesin family member 3B (KIF3B)

    Energy Technology Data Exchange (ETDEWEB)

    Duangtum, Natapol [Medical Molecular Biology Unit, Office for Research and Development Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Department of Anatomy, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Junking, Mutita; Sawasdee, Nunghathai [Medical Molecular Biology Unit, Office for Research and Development Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Cheunsuchon, Boonyarit [Department of Pathology, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Limjindaporn, Thawornchai, E-mail: limjindaporn@yahoo.com [Department of Anatomy, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Yenchitsomanus, Pa-thai, E-mail: grpye@mahidol.ac.th [Medical Molecular Biology Unit, Office for Research and Development Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand)

    2011-09-16

    Highlights: {yields} Impaired trafficking of kAE1 causes distal renal tubular acidosis (dRTA). {yields} The interaction between kAE1 and kinesin family member 3B (KIF3B) is reported. {yields} The co-localization between kAE and KIF3B was detected in human kidney tissues. {yields} A marked reduction of kAE1 on the cell membrane was observed when KIF3B was knockdown. {yields} KFI3B plays an important role in trafficking of kAE1 to the plasma membrane. -- Abstract: Impaired trafficking of human kidney anion exchanger 1 (kAE1) to the basolateral membrane of {alpha}-intercalated cells of the kidney collecting duct leads to the defect of the Cl{sup -}/HCO{sub 3}{sup -} exchange and the failure of proton (H{sup +}) secretion at the apical membrane of these cells, causing distal renal tubular acidosis (dRTA). In the sorting process, kAE1 interacts with AP-1 mu1A, a subunit of AP-1A adaptor complex. However, it is not known whether kAE1 interacts with motor proteins in its trafficking process to the plasma membrane or not. We report here that kAE1 interacts with kinesin family member 3B (KIF3B) in kidney cells and a dileucine motif at the carboxyl terminus of kAE1 contributes to this interaction. We have also demonstrated that kAE1 co-localizes with KIF3B in human kidney tissues and the suppression of endogenous KIF3B in HEK293T cells by small interfering RNA (siRNA) decreases membrane localization of kAE1 but increases its intracellular accumulation. All results suggest that KIF3B is involved in the trafficking of kAE1 to the plasma membrane of human kidney {alpha}-intercalated cells.

  4. Human kidney anion exchanger 1 interacts with kinesin family member 3B (KIF3B)

    International Nuclear Information System (INIS)

    Highlights: → Impaired trafficking of kAE1 causes distal renal tubular acidosis (dRTA). → The interaction between kAE1 and kinesin family member 3B (KIF3B) is reported. → The co-localization between kAE and KIF3B was detected in human kidney tissues. → A marked reduction of kAE1 on the cell membrane was observed when KIF3B was knockdown. → KFI3B plays an important role in trafficking of kAE1 to the plasma membrane. -- Abstract: Impaired trafficking of human kidney anion exchanger 1 (kAE1) to the basolateral membrane of α-intercalated cells of the kidney collecting duct leads to the defect of the Cl-/HCO3- exchange and the failure of proton (H+) secretion at the apical membrane of these cells, causing distal renal tubular acidosis (dRTA). In the sorting process, kAE1 interacts with AP-1 mu1A, a subunit of AP-1A adaptor complex. However, it is not known whether kAE1 interacts with motor proteins in its trafficking process to the plasma membrane or not. We report here that kAE1 interacts with kinesin family member 3B (KIF3B) in kidney cells and a dileucine motif at the carboxyl terminus of kAE1 contributes to this interaction. We have also demonstrated that kAE1 co-localizes with KIF3B in human kidney tissues and the suppression of endogenous KIF3B in HEK293T cells by small interfering RNA (siRNA) decreases membrane localization of kAE1 but increases its intracellular accumulation. All results suggest that KIF3B is involved in the trafficking of kAE1 to the plasma membrane of human kidney α-intercalated cells.

  5. Enhanced performance of anion exchange membranes via crosslinking of ion cluster regions for fuel cells

    Science.gov (United States)

    Lai, Ao Nan; Guo, Dong; Lin, Chen Xiao; Zhang, Qiu Gen; Zhu, Ai Mei; Ye, Mei Ling; Liu, Qing Lin

    2016-09-01

    Development of anion exchange membranes (AEMs) with high hydroxide conductivity, good dimensional and alkaline stabilities is still a challenge for the practical application of AEM fuel cells. In this study, we report a new strategy to prepare high-performance AEMs with crosslinked ionic regions. A series of phenolphthalein-containing poly(arylene ether sulfone)s crosslinked AEMs was synthesized by grafting ion groups selectively and densely on the phenolphthalein units to form ion clusters that are further crosslinked to generate the hydrophilic ionic regions. The crosslinking reaction not only improved the dimensional stability of the AEMs, but also increased the aggregation of the ion clusters leading to the formation of hydrophilic/hydrophobic phase-separated morphology and ion-conducting channels. As a result, enhancements in both ion conductivity and dimensional stability can be achieved. The crosslinked AEMs showed high hydroxide conductivities in the range of 52.2-143.4 mS cm-1 from 30 to 80 °C and a superb ratio of relative conductivity to relative swelling at 80 °C. Furthermore, the crosslinked AEMs also exhibited good mechanical properties, thermal and alkaline stabilities and desirable single cell performance. This work presents a promising strategy for the synthesis of high-performance AEMs for fuel cells.

  6. Water uptake, ionic conductivity and swelling properties of anion-exchange membrane

    Energy Technology Data Exchange (ETDEWEB)

    Duan, QJ; Ge, SH; Wang, CY

    2013-12-01

    Water uptake, ionic conductivity and dimensional change of the anion-exchange membrane made by Tokuyama Corporation (A201 membrane) are investigated at different temperatures and water activities. Specifically, the amount of water taken up by membranes exposed to water vapor and membranes soaked in liquid water is determined. The water uptake of the A201 membrane increases with water content as well as temperature. In addition, water sorption data shows Schroeder's paradox for the AEMs investigated. The swelling properties of the A201 membrane exhibit improved dimensional stability compared with Nafion membrane. Water sorption of the A201 membrane occurs with a substantial negative excess volume of mixing. The threshold value of hydrophilic fraction in the A201 membrane for ionic conductivity is around 0.34, above which, the conductivity begins to rise quickly. This indicates that a change in the connectivity of the hydrophilic domains occurs when hydrophilic fraction approaches 0.34. (C) 2013 Elsevier B.V. All rights reserved.

  7. Adsorption of Zinc and Cyanide from Cyanide Effluents on Anionic Ion-exchange Resin

    Institute of Scientific and Technical Information of China (English)

    ZHANG Ya-li; FANG Tao; YU Xian-jin

    2013-01-01

    The adsorption of zinc and cyanide from cyanide effluents onto strong and weak basic anion exchange resins was studied in a batch adsorption system.Factors influencing the adsorption rates such as resin selection,resin amounts,contact time and temperature were studied and scanning electron microscopy-energy disperse spectroscopy(SEM-EDS) was used in the analysis.The present study shows that the adsorption capacity of resin 201 ×7 is better than that of resin 301.The adsorption process was relatively fast and came to equilibrium after 60 min.The kinetic data were analyzed with three models and the pseudo-second-order kinetic model was found to agree with the experimental data well.The equilibrium data could also be described well by Langmuir isotherm model.Thermodynamic parameters such as enthalpy change(△H0),free energy change(△G0) and entropy change(△S0) were calculated and the adsorption process was spontaneous and endothermic.

  8. Polyphenylene sulfide based anion exchange fiber: Synthesis, characterization and adsorption of Cr(Ⅵ)

    Institute of Scientific and Technical Information of China (English)

    Jiajia Huang; Xin Zhang; Lingling Bai; Siguo Yuan

    2012-01-01

    A fibrous strong base anion exchanger(QAPPS)was prepared for the first time via chloromethylation and quaternary amination reaction of polyphenylene sulfide fiber(PPS),and its physical-chemical structure and adsorption behavior for Cr(Ⅵ)were characterized by FTIR,Energy Dispersive Spectrometry,TG-DTG,elemental analysis and batch adsorptive technique,respectively.The novel fibrous adsorbent could effectively adsorb Cr(Ⅵ)over the pH range 1-12,the maximum adsorption capacity was 166.39 mg/g at pH 3.5,and the adsorption behavior could be described well by Langrnuir isotherm equation model.The adsorption kinetics was studied using pseudo first-order and pseudo second-order models,and the t1/2 and equilibrium adsorption time were 5 and 20 rain respectively when initial Cr(Ⅵ)concentration was 100 mg/L.The saturated fibers could be regenerated rapidly by a mixed solution of 0.5 mol/L NaOH and 0.5 mol/L NaCl,and the adsorption capacity was well maintained after six adsorption-desorption cycles.

  9. A new method for antimony speciation in plant biomass and nutrient media using anion exchange cartridge.

    Science.gov (United States)

    Tisarum, Rujira; Ren, Jing-Hua; Dong, Xiaoling; Chen, Hao; Lessl, Jason T; Ma, Lena Q

    2015-11-01

    A selective separation method based on anion exchange cartridge was developed to determine antimony (Sb) speciation in biological matrices by graphite furnace atomic absorption spectrophotometry (GFAAS). The selectivity of the cartridge towards antimonite [Sb(III)] and antimonate [Sb(V)] reversed in the presence of deionized (DI) water and 2mM citric acid. While Sb(V) was retained by the cartridge in DI water, Sb(III) was retained in citric acid media. At pH 6, Sb(III) and Sb(V) formed Sb(III)- and Sb(V)-citrate complexes, but the cartridge had higher affinity towards the Sb(III)-citrate complex. Separation of Sb(III) was tested at various concentrations in fresh and spent growth media and plant tissues. Our results showed that cartridge-based Sb speciation was successful in plant tissues, which was confirmed by HPLC-ICP-MS. The cartridge retained Sb(III) and showed 92-104% Sb(V) recovery from arsenic hyperaccumulator Pteris vittata roots treated with Sb(III) and Sb(V). The cartridge procedure is an effective alternative for Sb speciation, offering low cost, reproducible results, and simple Sb analysis using GFAAS.

  10. Separation of Fluoride Ions in an Electrolytic Cell by Using an AnionExchange Membrane

    International Nuclear Information System (INIS)

    Separation of fluoride ions in an electrolytic cell with an anionexchange membrane which is so-called an electrodialysis process has beenperformed. The experiment have been taken place in room temperature in anelectrolytic cell made by plexiglas consisted on anode and cathode chambersseparated by an anion exchange membrane in dimension of 4 x 4 cm. The carbonand stainless steel are applied as an anode and platinum as s' cathode. Theanolyte is a HNO3 0.3 M solution, while a solution of NaF 0.3 M, and amixture of NaF 0.3 M containing uranyl nitrate solution for separating offluoride ions and uranium are used as a catholyte. The distance between theelectrode and the membrane is 1.5 cm and this distance is kept constant. Theparameters observed are the current voltage, cathode applied, and uraniumconcentration. For the solution without uranium, the results show that thefluoride ions transferred are around 50 % using carbon as a cathode for 3hours and the voltage of 10 volts, while for SS as a cathode are around 93 %.For the solution containing uranium, the fluoride ions transferred are around78 % for 3.5 hours and the uranium ions remain in the catholyte in which mostof them are as 8 yellow deposit of Na2U2O7 on the cathode surface andothers are as a white precipitate of NaUF5 on the bottom of the cathodechamber. (author)

  11. Concentration and separation of vanadium from alkaline media by strong alkaline anion-exchange resin 717

    Institute of Scientific and Technical Information of China (English)

    HUANG Jinwen; SU Peng; WU Wenwei; LIAO Sen; QIN Huiquan; WU Xuehang; HE Xiaohu; TAO Liujia; FAN Yanjin

    2010-01-01

    With strong alkaline anion-exchange resin 717 as the sorbent and NaOH solution as the eluent, a study on the sorption from alkaline solution and elution of vanadium(Ⅴ), silicon(Ⅳ), and aluminium(Ⅲ) was carried out. Different parameters affecting the sorption and elution process,including temperature, pH values as well as the ratio of resin to solution, were investigated. The results show that sorption degree of vanadium(Ⅴ) increases with a decrease of pH values, and V(Ⅴ) ions are easier sorbed than Si(Ⅳ) and Al(Ⅲ) ions under the same conditions. The sorption degree of V(Ⅴ), Si(Ⅳ), and Al(Ⅲ) at pH 9.14 for 15 min are 90.6%, 33.5%, and 21.6%, respectively. Si(Ⅳ), Al(Ⅲ), and V(Ⅴ) ions sorbed on 717 resin were eluted by use of 2 mol.L-1 NaOH solution; the desorption degree of V(Ⅴ), Si(Ⅳ), and Al(Ⅲ) for 5 min are 81.7 %,99.1%, and 99.3%, respectively.

  12. PLUTONIUM LOADING CAPACITY OF REILLEX HPQ ANION EXCHANGE COLUMN - AFS-2 PLUTONIUM FLOWSHEET FOR MOX

    Energy Technology Data Exchange (ETDEWEB)

    Kyser, E.; King, W.; O' Rourke, P.

    2012-07-26

    Radioactive plutonium (Pu) anion exchange column experiments using scaled HB-Line designs were performed to investigate the dependence of column loading performance on the feed composition in the H-Canyon dissolution process for plutonium oxide (PuO{sub 2}) product shipped to the Mixed Oxide (MOX) Fuel Fabrication Facility (MFFF). These loading experiments show that a representative feed solution containing {approx}5 g Pu/L can be loaded onto Reillex{trademark} HPQ resin from solutions containing 8 M total nitrate and 0.1 M KF provided that the F is complexed with Al to an [Al]/[F] molar ratio range of 1.5-2.0. Lower concentrations of total nitrate and [Al]/[F] molar ratios may still have acceptable performance but were not tested in this study. Loading and washing Pu losses should be relatively low (<1%) for resin loading of up to 60 g Pu/L. Loading above 60 g Pu/L resin is possible, but Pu wash losses will increase such that 10-20% of the additional Pu fed may not be retained by the resin as the resin loading approaches 80 g Pu/L resin.

  13. Poly(phenyl sulfone) anion exchange membranes with pyridinium groups for vanadium redox flow battery applications

    Science.gov (United States)

    Zhang, Bengui; Zhang, Enlei; Wang, Guosheng; Yu, Ping; Zhao, Qiuxia; Yao, Fangbo

    2015-05-01

    To develop high performance and cost-effective membranes with low permeability of vanadium ions for vanadium redox flow battery (VRFB) application, poly(phenyl sulfone) anion exchange membranes with pyridinium groups (PyPPSU) are prepared and first investigated for VRFB application. PyPPSU membranes show much lower vanadium ions permeability (0.07 × 10-7-0.15 × 10-7 cm2 min-1) than that of Nafion 117 membrane (31.3 × 10-7 cm2 min-1). As a result, the self-discharge duration of the VRFB cell with PyPPSU membrane (418 h) is about four times longer than that of VRFB cell with Nafion 117 membrane (110 h). Furthermore, the VRFB cell with PyPPSU membrane exhibits higher battery efficiency (coulombic efficiency of 97.8% and energy efficiency of 80.2%) compare with that of VRFB cell with Nafion 117 membrane (coulombic efficiency of 96.1% and energy efficiency of 77.2%) at a high current density of 100 mA cm-2. In addition, PyPPSU membrane exhibits stable performance in 100-cycle test. The results indicate that PyPPSU membrane is high performance and low-cost alternative membrane for VRFB application.

  14. Methods development for separation of inorganic anions, organic acids and bases, and neutral organic compounds by ion chromatography and capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Li, J.

    1999-04-01

    A novel anion-exchange resin containing three amine groups was prepared by reaction of a chloromethylated polystyrene-divinylbenzene (PS-DVB) resin with diethylenetriamine. After being protonated by contact with an aqueous acid, this resin can be used for ion chromatographic separation of anions. The charge on the resins can be varied from +1 to +3 by changing the mobile phase pH. The selectivity of the new ion exchangers for various inorganic anions was quite different from that of conventional anion exchangers. The performance of this new anion exchanger was studied by changing the pH and the concentration of the eluent, and several different eluents were used with some common anions as testing analytes. Conductivity detection and UV-visible detection were applied to detect the anions after separation. The new resin can also be used for HPLC separation of neutral organic compounds. Alkylphenols and alkylbenzenes were separated with this new polymeric resin, and excellent separations were obtained under simple conditions. This report contains Chapter 1: General introduction and Chapter 6: General conclusions.

  15. Intercalation chemistry in a LDH system: anion exchange process and staging phenomenon investigated by means of time-resolved, in situ X-ray diffraction.

    Science.gov (United States)

    Taviot-Guého, Christine; Feng, Yongjun; Faour, Azzam; Leroux, Fabrice

    2010-07-14

    Using time-resolved, in situ energy-dispersive X-ray diffraction (EDXRD), the formation of interstratified LDH structures, with alternate interlayer spaces occupied by different anions, have been demonstrated during anion exchange reactions. Novel hybrid LDH nanostructures can thus be prepared, combining the physicochemical properties of two intercalated anions plus those of the LDH host. A general trend is that inorganic-inorganic anion exchange reactions occur in a one-step process while inorganic-organic exchanges may proceed via a second-stage intermediate, suggesting that staging occurs partly as a result of organic-inorganic separation. Yet, other influencing parameters must be considered such as LDH host composition, LDH affinity for different anions and LDH particle size as well as extrinsic parameters like the reaction temperature. Hence, a correlation between the occurrence of staging phenomenon and the difficulty of the exchange of the initial anion is observed, suggesting that staging is needed to overcome the energy barrier in the case of the exchange by organic anions. Notwithstanding the LiAl(2) system, staging has mainly been observed with Zn(2)Cr LDH host so far, a peculiar LDH composition with a unique Zn/Cr ratio of two and a local order of the cations within the hydroxide layers. The formation of a higher order-staged intermediate than stage two, observed during the exchange reaction of CO(3)(2-) or SO(4)(2-) anions with Zn(2)Cr-tartrate, is in favour of a Daumas-Herold model although this model implies a bending of LDH layers. The analysis of the X-ray powder diffraction pattern of Zn(2)Cr-Cl/tartrate second-stage intermediate, isolated almost as a pure phase during the exchange of Cl(-) with tartrate anions in Zn(2)Cr LDH, indicates a disorder in the stacking sequence and a relative proportion of the two kinds of interlayers slightly different from 50/50. Besides, the microstructural analysis of the XRD pattern reveals a great reduction of the

  16. An Anion-Exchange Method for the Separation of P-32 Activity in Neutron-Irradiated Biological Material

    International Nuclear Information System (INIS)

    Strong hydrochloric-acid solutions containing small amounts of orthophosphoric and citric acid and radioactive tracers of the elements Na, P, K, Ca, Se, Cr, Mn, Ni, Rb, Sr, Cs, Ba, La, and Ce were titrated with a water suspension of strongly basic anion-exchange resin in the hydroxide form. The titration was carried out to pH = 3.0. It was followed by filtration of the mixture on the top of a small anion-exchange column in the chloride form and a final washing with water. Phosphorus was quantitatively adsorbed by the resin and the scandium retention was better than 96 per cent. The remaining elements passed quantitatively into the effluent, with the exception of nickel, which was adsorbed to a very small extent

  17. THERMODYNAMIC STUDY ON ADSORPTION OF AROMATIC SULFONIC ACIDS ONTO MACROPOROUS WEAK BASE ANION EXCHANGER FROM AQUEOUS SOLUTIONS

    Institute of Scientific and Technical Information of China (English)

    Chao Long; Quan-xing Zhang; Ai-min Li; Jin-long Chen

    2004-01-01

    The adsorption equilibrium isotherms of three aromatic sulfonic acid compounds, 2-naphthalenesulfonic acid, ptoluenesulfonic acid and p-chlorobenzenesulfonic acid, from aqueous solutions by macroporous weak base anion exchanger within the temperature range of 293 K-313 K were obtained. Several isotherm equations were correlated with the equilibrium data, and the experimental data was found to fit the three-parameter Redlich-Peterson equation best within the entire range of concentrations. The study showed that the hydrophobicity of solute has distinct influence on adsorption capacity of the anion exchanger for the aromatic sulfonic acid. Moreover, estimations of the isosteric enthalpy, free energy,and entropy change of adsorption were also reported. The positive isosteric enthalpy and entropy change for adsorption indicate an endothermic and entropy driven process in the present study.

  18. Gluconic acid production in bioreactor with immobilized glucose oxidase plus catalase on polymer membrane adjacent to anion-exchange membrane.

    Science.gov (United States)

    Godjevargova, Tzonka; Dayal, Rajeshwar; Turmanova, Sevdalina

    2004-10-20

    Gluconic acid was obtained in the permeate side of the bioreactor with glucose oxidase (GOD) immobilized onto anion-exchange membrane (AEM) of low-density polyethylene grafted with 4-vinylpiridine. The electric resistance of the anion-exchange membranes was increased after the enzyme immobilization on the membrane. The gluconic acid productions were relatively low with the GOD immobilized by any method on the AEM. To increase the enzyme reaction efficiency, GOD was immobilized on membrane of AN copolymer (PAN) adjacent to an anion-exchange membrane in bioreactor. Uses of anion-exchange membrane led to selective removal of the gluconic acid from the glucose solution and reduce the gluconic acid inhibition. The amount of gluconic acid obtained in the permeate side of the bioreactor with the GOD immobilized on the PAN membrane adjacent to the AEM under electrodialysis was about 30 times higher than that obtained with enzyme directly bound to the AEM. The optimal substrate concentration in the feed side was found to be about 1 g/l. Further experiments were carried out with the co-immobilized GOD plus Catalase (CAT) on the PAN membrane adjacent to the AEM to improve the efficiency of the immobilize system. The yield of this process was at least 95%. The storage stability of the co-immobilized GOD and CAT was studied (lost 20% of initial activity for 90 d). The results obtained clearly showed the higher potential of the dual membrane bioreactor with GOD plus CAT bound to ultrafiltration polymer membrane adjacent to the AEM. Storage stability of GOD activity in GOD plus CAT immobilized on PAN//AEM membranes and on AEM.

  19. Nondestructive radio isotopic technique for performance evaluation of industrial grade anion exchange resins Amberlite IRN78 and Indion NSSR

    Energy Technology Data Exchange (ETDEWEB)

    Singare, Pravin U. [Bhavan' s College, Mumbai (India). Dept. of Chemistry

    2016-01-15

    The present study deals with the application of radiotracers 131I and 82Br as a non-destructive tool to evaluate the performance of Amberlite IRN78 (nuclear grade) and Indion NSSR (non-nuclear grade) anion exchange resins. In general based on radiotracer applications it was observed that Amberlite IRN78 resins show superior performance over Indion NSSR resins under identical operational parameters.

  20. THE EFFECT OF IONIC STRENGTH ON THE UPTAKE OF TAURINE ON A STRONG-BASIC ANION EXCHANGE RESIN

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Studied the effect of ionic strength on the uptake of taurine on a strong-basic anionexchange resin. The batch phase equilibrium experiments of ta urine on the anion exchange resin D290 were conducted at different ionic strength, and then the amounts of uptake of taurine on the resin at different pH were determined. The ion exchange mechanisms of taurine on the anion exchange resin at different pH were discussed. Experimental results showed that with increase of the ionic strength of solution, the adsorbed amount of taurine on the resin D290 decreased; Adding small amounts of NaOH or HCl into the system of taurine aqueous solution/D290 anionresin would make the amount of taurine taken up on the resin to decrease due to the competition uptakes of hydroxyl ion with taurine or the decrease in the amount of absorbable zwitterions of taurine in the solution and excluding the cations of taurine from the anion resin.

  1. Deletion of the anion exchanger Slc26a4 (pendrin) decreases apical Cl−/HCO3− exchanger activity and impairs bicarbonate secretion in kidney collecting duct

    OpenAIRE

    Amlal, Hassane; Petrovic, Snezana; Xu, Jie; Wang, Zhaohui; Sun, Xuming; Barone, Sharon; Soleimani, Manoocher

    2010-01-01

    The anion exchanger Pendrin, which is encoded by SLC26A4 (human)/Slc26a4 (mouse) gene, is localized on the apical membrane of non-acid-secreting intercalated (IC) cells in the kidney cortical collecting duct (CCD). To examine its role in the mediation of bicarbonate secretion in vivo and the apical Cl−/HCO3− exchanger in the kidney CCD, mice with genetic deletion of pendrin were generated. The mutant mice show the complete absence of pendrin expression in their kidneys as assessed by Northern...

  2. HB-LINE ANION EXCHANGE PURIFICATION OF AFS-2 PLUTONIUM FOR MOX

    Energy Technology Data Exchange (ETDEWEB)

    Kyser, E.; King, W.

    2012-04-25

    Non-radioactive cerium (Ce) and radioactive plutonium (Pu) anion exchange column experiments using scaled HB-Line designs were performed to investigate the feasibility of using either gadolinium nitrate (Gd) or boric acid (B as H{sub 3}BO{sub 3}) as a neutron poison in the H-Canyon dissolution process. Expected typical concentrations of probable impurities were tested and the removal of these impurities by a decontamination wash was measured. Impurity concentrations are compared to two specifications - designated as Column A or Column B (most restrictive) - proposed for plutonium oxide (PuO{sub 2}) product shipped to the Mixed Oxide (MOX) Fuel Fabrication Facility (MFFF). Use of Gd as a neutron poison requires a larger volume of wash for the proposed Column A specification. Since boron (B) has a higher proposed specification and is more easily removed by washing, it appears to be the better candidate for use in the H-Canyon dissolution process. Some difficulty was observed in achieving the Column A specification due to the limited effectiveness that the wash step has in removing the residual B after {approx}4 BV's wash. However a combination of the experimental 10 BV's wash results and a calculated DF from the oxalate precipitation process yields an overall DF sufficient to meet the Column A specification. For those impurities (other than B) not removed by 10 BV's of wash, the impurity is either not expected to be present in the feedstock or process, or recommendations have been provided for improvement in the analytical detection/method or validation of calculated results. In summary, boron is recommended as the appropriate neutron poison for H-Canyon dissolution and impurities are expected to meet the Column A specification limits for oxide production in HB-Line.

  3. HB-LINE ANION EXCHANGE PURIFICATION OF AFS-2 PLUTONIUM FOR MOX

    Energy Technology Data Exchange (ETDEWEB)

    Kyser, E. A.; King, W. D.

    2012-07-31

    Non-radioactive cerium (Ce) and radioactive plutonium (Pu) anion exchange column experiments using scaled HB-Line designs were performed to investigate the feasibility of using either gadolinium nitrate (Gd) or boric acid (B as H{sub 3}BO{sub 3}) as a neutron poison in the H-Canyon dissolution process. Expected typical concentrations of probable impurities were tested and the removal of these impurities by a decontamination wash was measured. Impurity concentrations are compared to two specifications - designated as Column A or Column B (most restrictive) - proposed for plutonium oxide (PuO{sub 2}) product shipped to the Mixed Oxide (MOX) Fuel Fabrication Facility (MFFF). Use of Gd as a neutron poison requires a larger volume of wash for the proposed Column A specification. Since boron (B) has a higher proposed specification and is more easily removed by washing, it appears to be the better candidate for use in the H-Canyon dissolution process. Some difficulty was observed in achieving the Column A specification due to the limited effectiveness that the wash step has in removing the residual B after ~4 BV's wash. However a combination of the experimental 10 BV's wash results and a calculated DF from the oxalate precipitation process yields an overall DF sufficient to meet the Column A specification. For those impurities (other than B) not removed by 10 BV's of wash, the impurity is either not expected to be present in the feedstock or process, or recommendations have been provided for improvement in the analytical detection/method or validation of calculated results. In summary, boron is recommended as the appropriate neutron poison for H-Canyon dissolution and impurities are expected to meet the Column A specification limits for oxide production in HB-Line.

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

    International Nuclear Information System (INIS)

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

  5. Radiotracer application for characterization of nuclear grade anion exchange resins Tulsion A-23 and Dowex SBR LC

    Energy Technology Data Exchange (ETDEWEB)

    Singare, P.U. [Bhavan' s College, Mumbai (India). Dept. of Chemistry

    2015-12-15

    Radio isotopic tracer technique as one of the versatile nondestructive technique is employed to evaluate the performance of nuclear grade anion exchange resins Tulsion A-23 and Dowex SBR LC. The evaluation was made on the basis of ion-isotopic exchange reaction kinetics by using {sup 131}I and {sup 82}Br radioactive tracer isotopes. It was observed that for both the resins, the values of specific reaction rate (min{sup -1}), amount of ion exchanged (mmol) and initial rate of ion exchange (mmol/min) were calculated to be lower for bromide ion-isotopic exchange reaction than that for iodide ion-isotopic exchange reaction. It was observed that for iodide ion-isotopic exchange reaction under identical experimental conditions of 30.0 C, 1.000 g of ion exchange resins and 0.001 mol/L labeled iodide ion solution, the values of specific reaction rate (min{sup -1}), amount of iodide ion exchanged (mmol), initial rate of iodide ion exchange (mmol/min) and log K{sub d} were calculated as 0.377, 0.212, 0.080 and 15.5 respectively for Dowex SBR LC resin, which was higher than 0.215, 0.144, 0.031 and 14.1 respectively as that obtained for Tulsion A23 resins. Also at a constant temperature of 30.0 C, as the concentration of labeled iodide ion solution increases from 0.001 mol/L to 0.004 mol/L, the percentage of iodide ions exchanged increases from 84.75 % to 90.20 % for Dowex SBR LC resins which was higher than increases from 57.66 % to 62.38 % obtained for Tulsion A23 resins. The identical trend was observed for the two resins during bromide ion-isotopic exchange reaction. The overall results indicate superior performance of Dowex SBR LC over Tulsion A23 resins under identical experimental conditions.

  6. Effect of alcohols on separation behavior of rare earth elements using benzimidazole-type anion-exchange resin in nitric acid solutions

    International Nuclear Information System (INIS)

    Chromatographic separation experiments of trivalent rare earth elements were performed using benzimidazole type anion-exchange resin in nitric/alcohol mixed solvent systems at room temperature. As a result, it was found those trivalent rare earth elements are able to be separated mutually in a 20% HNO3 and 80% MeOH mixed solvent. Based on these results, we systematically examined using various alcohols to make clear the role of alcohols in anion-exchange reactions at various temperatures. (author)

  7. Understanding ion and solvent transport in anion exchange membranes under humidified conditions

    Science.gov (United States)

    Sarode, Himanshu

    Anion exchange membranes (AEM) have been studied for more than a decade for potential applications in low temperature fuel cells and other electrochemical devices. They offer the advantage of faster reaction kinetics under alkaline conditions and ability to perform without costly platinum catalyst. Inherently slow diffusion of hydroxide ions compared to protons is a primary reason for synthesizing and studying the ion transport properties in AEMs. The aim of this thesis is to understand ion transport in novel AEMs using Pulse Gradient stimulated Spin Echo Nuclear Magnetic Resonance technique (PGSE NMR), water uptake, ionic conductivity, Small Angle X-ray Scattering (SAXS) etc. All experiments were performed under humidified conditions (80--95% relative humidity) and fuel cell operating temperatures of 30--90°C. In this work, the NMR tube design was modified for humidifying the entire NMR tube evenly from our previous design. We have developed a new protocol for replacing caustic hydroxide with harmless fluoride or bicarbonate ions for 19F and 13 C NMR diffusion experiments. After performing these NMR experiments, we have obtained in-depth understanding of the morphology linked ion transport in AEMs. We have obtained the highest fluoride self-diffusion coefficient of > 1 x 10-5 cm2/sec ( 55°C) for ETFE-g-PVBTMA membrane which is a result of low tortuosity of 1 obtained for the membrane. This faster fluoride transport combined with low tortuosity of the membrane resulted in > 100mS/cm hydroxide conductivity for the membrane. Polycyclooctene (PCOE) based triblock copolymers are also studied for in-depth understanding of molecular weight, IEC, mechanical and transport properties. Effect of melting temperature of PCOE has favorable effect on increasing ion conductivity and lowering activation energy. Mechanical properties of these types of membranes were studied showing detrimental effect of water plasticization which results in unsuitable mechanical properties

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

    DEFF Research Database (Denmark)

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

    2001-01-01

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

  9. Behavior of cationic, anionic and colloidal species of titanium, zirconium and thorium in presence of ion exchange resins

    International Nuclear Information System (INIS)

    The distribution of titanium, zirconium and thorium is aqueous and resin phases has been studied using strong cationic resin in the R-NH4 form. Solutions of the above elements in perchloric, nitric, hydrochloric and suphuric media were used. Each set of experiments was made by separately varying one of the five parameters - type of anion present, acidity of solution, temperature of percolation, age of solution and concentration of the element. It was found that, depending on the particular balance of these parameters, the elements investigated may be found in acidic solutions either as cationic, anionic or colloidal species. It is emphasized that the colloidal species of titanium, zirconium or thorium are not retained by the ion exchangers, and from this property a method for the separation and purification of the above elements has been outlined

  10. Anion exchange removal of Al3+ from Li+-Al3+ aqueous solution (originating from lithium recovery from brine

    Directory of Open Access Journals (Sweden)

    Anissa Somrani

    2014-06-01

    Full Text Available The purpose of this study is to separate aluminum(III ion from an aqueous solution containing Li+ at 25°C. Al3+ was transferred into [Al(C2O43]3- by means of complexation and removed by an anion exchange resin. This resin was anionic type Amberlite IRA 402 regenerated by sodium chloride. Hence, a theoretical study based on speciation diagrams was carried out to determine the best pH domain for separation. The complexation of aluminum ions by ammonium oxalate was studied. The motar ratio of Ox/Al and pH was investigated. Optimum values of these factors were found to be 3 and 4 respectively. In this case, the remaining lithium is 98.5%.

  11. Purification of drinking water from radioactive contamination by final consumers by means of combined cation and anion exchangers

    International Nuclear Information System (INIS)

    It should be tried to develop an apparatus which makes it possible for the final consumer to purify the drinking water himself in the case of a radioactive contamination of the water. After thorough preliminary studies the most suitable kinds of exchange resins and the best arrangement for a combined cation and anion exchange resins and the best arrangement for a combined cation and anion exchange equipment were determined in inactive preliminary tests. Subsequent the useful capacity (NK) and the purifying factor (RF) were determined for the fission products 90Sr, 131I and 137Cs. The results were for 90Sr: NK = 30 1/2 x 0.5 l resin, RF >= 4.102, for 131I: NK = 32 1/2 x 0.5 l resin, RF = 3.7.102 and for 137Cs: NK > 35 1/2 x 0.5 l resin, RF >= 103. With 2 x 1 l resin the concentration of possible fission products in water can be reduced by 2 orders of magnitude ore more. A proposal for the construction of a household decontamination equipment for drinking water is made. The cost of production will be about A.S. 400,-- to 600,--. (author)

  12. Ra/Ca separation by ion exchange chromatography

    International Nuclear Information System (INIS)

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

  13. Evidence for F-/SiO- anion exchange in the framework of As-synthesized all-silica zeolites

    KAUST Repository

    Liu, Xiaolong

    2011-05-12

    Not everything changes: Charge-compensating anions can be exchanged in as-synthesized zeolite frameworks with changes in both the density of defect sites and of the hydrophobic character of the zeolite. The reversible transformation occurs without dissolution/recrystallization of the zeolite and preserves the size and shape of the crystals (see picture). Fluoride removal is not possible in all-silica D4R units, for which fluoride ions play a structure-directing role. © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Dynamic separation of Szilard-Chalmers reaction products applied to the trioxalatochromium ion adsorbed on anionic exchange resin

    International Nuclear Information System (INIS)

    A method of dynamic elution of recoiled 51Cr+3, formed by the Szilard-Chalmers reaction during the irradiation of trioxalatochromium ion adsorbed on anionic exchange resin is presented. The influence of some factors on the separation yield of chromium-51, such as: composition, concentration and flow rate of eluent, mesh size of the resin and irradiation time are studied. The results are compardd with those obtained by the static method, in which the recoiled atom is separated from the target after irradiation. Because of the high separation yield of chromium-51, the method of dynamic separation is proposed for routine production of this elemnt, with high specific activities. (author)

  15. Ion-Isotopic Exchange Reaction Kinetics using Anion Exchange Resins Dowex 550A LC and Indion-930A

    Directory of Open Access Journals (Sweden)

    P.U. Singare

    2014-06-01

    Full Text Available The present paper deals with the characterization of ion exchange resins Dowex 550A LC and Indion-930A based on kinetics of ion-isotopic exchange reactions for which the short lived radioactive isotopes 131I and 82Br were used as a tracers. The study was performed for different concentration of ionic solution varying from 0.001 mol/L to 0.004 mol/L and temperature in the range of 30.0 °C to 45.0 °C. The results indicate that as compared to bromide ion-isotopic exchange reaction, iodide exchange reaction take place at the faster rate. For both the ion-isotopic exchange reactions, under identical experimental conditions, the values of specific reaction rate increases with increase in the ionic concentration and decreases with rise in temperature. It was observed that at 35.00C, 1.000 g of ion exchange resins and 0.002 mol/L labeled iodide ion solution for iodide ion-isotopic exchange reaction, the values of specific reaction rate (min-1, amount of ion exchanged (mmol, initial rate of ion exchange (mmol/min and log Kd were 0.270, 0.342, 0.092 and 11.8 respectively for Dowex 550A LC resin, which was higher than the respective values of 0.156, 0.241, 0.038 and 7.4 as that obtained for Indion-930A resins. From the results, it appears that Dowex 550A LC resins show superior performance over Indion-930A resins under identical experimental conditions.

  16. Increased selectivity for planar chromatography by ion exchange : cation chromatography on papers impregnated with titanium (IV) based inorganic ion exchangers in DMSO-HNO3 mobile phases

    International Nuclear Information System (INIS)

    Planar chromatography of thirty six metal ions on titanium(IV) phosphate, titanium(IV) tungstate and titanium(IV) molybdate impregnated papers in DMSO-HNO3 mobile phases has been carried out. The ion-exchange capacity of papers is determined and the effects of solvent composition, impregnation and pH on RF values are studied. For K+, Rb+ and Cs+, RF = KC1/2, where C is the nitric acid concentration. The movement of ions is explained on the basis of ion-exchange, adsorption and precipitation. Alberti and Torracca's view for the prediction of elution sequence from RF values has been checked. The sequence of adsorption of ions follows the order : titanium(IV) molybdate > titanium(IV) tungstate > titanium(IV) phosphate. Some of the analytically important separations are reported. (author)

  17. Design of expanded bed supports for the recovery of plasmid DNA by anion exchange adsorption

    DEFF Research Database (Denmark)

    Theodossiou, Irini; Søndergaard, M.; Thomas, Owen R. T.

    2001-01-01

    In this study we detail the rational design of new chromatographic adsorbents tailored for the capture of plasmid DNA. Features present on current chromatographic supports that can significantly enhance plasmid binding capacity have been identified in packed bed chromatography experiments...

  18. Highly efficient platinum group metal free based membrane-electrode assembly for anion exchange membrane water electrolysis.

    Science.gov (United States)

    Pavel, Claudiu C; Cecconi, Franco; Emiliani, Chiara; Santiccioli, Serena; Scaffidi, Adriana; Catanorchi, Stefano; Comotti, Massimiliano

    2014-01-27

    Low-temperature electricity-driven water splitting is an established technology for hydrogen production. However, the two main types, namely proton exchange membrane (PEM) and liquid alkaline electrolysis, have limitations. For instance, PEM electrolysis requires a high amount of costly platinum-group-metal (PGM) catalysts, and liquid alkaline electrolysis is not well suited for intermittent operation. Herein we report a highly efficient alkaline polymer electrolysis design, which uses a membrane-electrode assembly (MEA) based on low-cost transition-metal catalysts and an anion exchange membrane (AEM). This system exhibited similar performance to the one achievable with PGM catalysts. Moreover, it is very suitable for intermittent power operation, durable, and able to efficiently operate at differential pressure up to 3 MPa. This system combines the benefits of PEM and liquid alkaline technologies allowing the scalable production of low-cost hydrogen from renewable sources. PMID:24339230

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

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Hansen, Sven Hedegaard

    1992-01-01

    Arsenite, arsenate, monomethylarsonate, dimethylarsinate, arsenobetaine, arsenocholine and the tetramethylarsonium ion were subjected to ion-exchange and ion-pair reversed phase HPLC. The ion exchange method was superior in selectivity and time of analysis for the arsenic anions. The ammonium ion...

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

    Science.gov (United States)

    Pirok, Bob W J; Knip, Jitske; van Bommel, Maarten R; Schoenmakers, Peter J

    2016-03-01

    In the late 19th century, newly invented synthetic dyes rapidly replaced the natural dyes on the market. The characterization of mixtures of these so-called early synthetic dyes is complicated through the occurrence of many impurities and degradation products. Conventional one-dimensional liquid chromatography does not suffice to obtain fingerprints with sufficient resolution and baseline integrity. Comprehensive two-dimensional liquid chromatography (LC×LC) is employed in this study, with ion-exchange chromatography in the first dimension and fast ion-pair liquid chromatography in the second. Retention in the first dimension is largely determined by the number of charges, while the selection of a small ion-pair reagent (tetramethylammonium hydroxide) in the second dimension causes retention to be largely determined by the molecular structure of the dye. As a result, there is a high degree of orthogonality of the two dimensions, similar to the values typically encountered in GC×GC. The proposed LC×LC method shows a theroretical peak capacity of about 2000 in an analysis time of about three hours. Clear, informative fingerprints are obtained that open a way to a more efficient characterization of dyes used in objects of cultural heritage. PMID:26868445

  1. Recovery of uranium from UCF liquid waste by anion exchange resin CG-400: Breakthrough curves, elution behavior and modeling studies

    International Nuclear Information System (INIS)

    Highlights: ► Amberlite CG-400 anion exchange resin has been used for the recovery of uranium. ► The breakthrough curves and elution behaviors of CG-400 resin have been studied in detailed. ► The mathematical models have been used to analyze the experimental data. ► The CG-400 resin has been applied successfully for uranium recovery from UCF liquid waste. - Abstract: Continuous fixed-bed column studies were carried out by using Amberlite CG-400 anion exchange resin for the recovery of uranium from aqueous solutions (synthetic solutions and uranium conversion facility (UCF) liquid waste). Effects of operating parameters such as flow rate and bed height were studied. The breakthrough capacity decreases with increasing flow rate, but this dependence was not significant with a long column. The maximum breakthrough capacity of uranium ions were achieved by CG-400 resin at a flow rate of 0.2 mL min−1 and bed height 9.1 cm (4 g resin). The elution behavior of uranium from CG-400 resin by various eluents have been investigated and the results show that 0.5 mol L−1 HNO3 is a good eluent for uranium recovery. The Adams–Bohart, Thomas, Yoon–Nelson and Dose–Response models were applied to the experimental data to determine the characteristic parameters of the column for process design using linear regression. The breakthrough curve calculated from the Dose–Response model was in best agreement with the experimental data

  2. Production of {sup 61}Cu using natural cobalt target and its separation using ascorbic acid and common anion exchange resin

    Energy Technology Data Exchange (ETDEWEB)

    Das, Sujata Saha; Chattopadhyay, Sankha; Barua, Luna [Radiopharmaceuticals Laboratory, Board of Radiation and Isotope Technology (BRIT), Variable Energy Cyclotron Centre (VECC), Kolkata 700064 (India); Das, Malay Kanti, E-mail: mkdas@vecc.gov.in [Radiopharmaceuticals Laboratory, Board of Radiation and Isotope Technology (BRIT), Variable Energy Cyclotron Centre (VECC), Kolkata 700064 (India)

    2012-02-15

    {sup 61}Cu was produced by {sup nat}Co({alpha}, xn){sup 61}Cu reaction. {sup 61}Cu production yield was 89.5 MBq/{mu}Ah (2.42 mCi/{mu}Ah) at the end of irradiation (EOI). A simple radiochemical separation method using anion exchange resin and ascorbic acid has been employed to separate the product radionuclide from inactive target material and co-produced non-isotopic impurities. The radiochemical separation yield was about 90%. Radiochemical purity of {sup 61}Cu was >99% 1 h after EOI. Final product was suitable for making complex with N{sub 2}S{sub 2} type of ligands. - Highlights: Black-Right-Pointing-Pointer High purity, no-carrier added {sup 61}Cu produced from natural cobalt target. Black-Right-Pointing-Pointer {sup 61}Cu separated from impurities using anion exchange resin and ascorbic acid. Black-Right-Pointing-Pointer {sup 61}Cu preparation was successfully used to label N{sub 2}S{sub 2}-type of ligand.

  3. Determination of plutonium isotopes in urine samples from radiation workers using 236Pu tracer, anion exchange resin and alpha spectrometry

    International Nuclear Information System (INIS)

    Bioassay technique is used for the estimation of actinides present in the body based on their excretion rate through body fluids. For occupational radiation workers urine assay is the preferred method for monitoring of chronic internal exposure. Determination of low concentrations of actinides such as plutonium, americium and uranium at low level of mBq in urine by alpha spectrometry requires pre-concentration of large volumes of urine. This paper deals with standardization of analytical method for the determination of Pu-isotopes in urine samples using anion exchange resin and 236Pu tracer for radiochemical recovery. The method involves oxidation of urine followed by co-precipitation of plutonium along with calcium phosphate. Separation of Pu was carried out by Amberlite, IRA-400, anion exchange resin. Pu-fraction was electrodeposited and activity estimated using tracer recovery by alpha spectrometer. Twenty routine urine samples of radiation workers were analyzed and consistent radiochemical tracer recovery was obtained in the range 74-96% with a mean and standard deviation of 85 and 6% respectively. (author)

  4. Determination of thorium and uranium in activated concrete by inductively coupled plasma mass spectrometry after anion-exchange separation

    International Nuclear Information System (INIS)

    A sensitive analytical method was established for the determination of Th and U in activated concrete samples. The method combines an anion-exchange separation step with an ICP-MS determination technique. In the ICP-MS measurement, a few μg mL-1 of Al and Ca, a few ng mL-1 of Mn, La, Ce, Nd and Pb and pg mL-1amounts of Li, Zr, Nb and Ba coexisting in the anion-exchange fraction of Th and U did not interfere. No adverse interference effects were observed in real sample analyses. The obtained detection limits (3 σ, n = 10) of Th and U were 2.3 and 1.8 pg mL -1, respectively. The analytical precisions for ca. 5 μg g -1 Th and ca. 1 μg g -1 U in real activated concrete samples were equally less than 7% RSD. The accuracies obtained by the analysis of GSJ rock standard samples were -18.1 to 0.4% for the Th determination and -14.0 to -5.7% for the U determination. The method uses the conventional absolute calibration curve. The internal standard calibration is unnecessary. (orig.)

  5. Chromatography.

    Science.gov (United States)

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

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

  6. Properties of solvated electrons, alkali anions and other species in metal solutions and kinetics of cation and electron exchange reactions. Final report

    International Nuclear Information System (INIS)

    The properties of solutions of alkali metals in amine solvents were studied by optical, ETR, NMR and electrochemical methods. Complexation of the alkali cations by crown ethers and cryptands permitted the preparation of concentrated solutions of alkali metals in amine and ether solvents. Extensive alkali metal NMR studies of the exchange of M+ with crown-ethers and cryptands and of the alkali metal anion, M-, were made. The first crystalline salt of an alkali metal anion, Na+ Cryptand [2.2.2]Na- was synthesized and characterized and led to the preparation of other alkali metal anion salts. This research provided the foundation for continuing studies of crystalline alkalide salts

  7. Molecular physiology and genetics of Na+-independent SLC4 anion exchangers

    OpenAIRE

    Alper, Seth L.

    2009-01-01

    Plasmalemmal Cl–/HCO3– exchangers are encoded by the SLC4 and SLC26 gene superfamilies, and function to regulate intracellular pH, [Cl–] and cell volume. The Cl–/HCO3– exchangers of polarized epithelial cells also contribute to transepithelial secretion and reabsorption of acid–base equivalents and Cl–. This review focuses on Na+-independent electroneutral Cl–/HCO3– exchangers of the SLC4 family. Human SLC4A1/AE1 mutations cause the familial erythroid disor...

  8. Ion Mobility Spectrometry-Hydrogen Deuterium Exchange Mass Spectrometry of Anions: Part 1. Peptides to Proteins

    Science.gov (United States)

    Donohoe, Gregory C.; Khakinejad, Mahdiar; Valentine, Stephen J.

    2015-04-01

    Ion mobility spectrometry (IMS) coupled with hydrogen deuterium exchange (HDX)-mass spectrometry (MS) has been used to study the conformations of negatively-charged peptide and protein ions. Results are presented for ion conformers of angiotensin 1, a synthetic peptide (SP), bovine insulin, ubiquitin, and equine cytochrome c. In general, the SP ion conformers demonstrate a greater level of HDX efficiency as a greater proportion of the sites undergo HDX. Additionally, these ions exhibit the fastest rates of exchange. Comparatively, the angiotensin 1 ions exhibit a lower rate of exchange and HDX level presumably because of decreased accessibility of exchange sites by charge sites. The latter are likely confined to the peptide termini. Insulin ions show dramatically reduced HDX levels and exchange rates, which can be attributed to decreased conformational flexibility resulting from the disulfide bonds. For the larger ubiquitin and protein ions, increased HDX is observed for larger ions of higher charge state. For ubiquitin, a conformational transition from compact to more elongated species (from lower to higher charge states) is reflected by an increase in HDX levels. These results can be explained by a combination of interior site protection by compact conformers as well as decreased access by charge sites. The elongated cytochrome c ions provide the largest HDX levels where higher values correlate with charge state. These results are consistent with increased exchange site accessibility by additional charge sites. The data from these enhanced IMS-HDX experiments are described in terms of charge site location, conformer rigidity, and interior site protection.

  9. The Role of Anion Exchanger on Pulmonary Vascular Response to Sustained Alveolar Hypoxia in the Isolated Perfused Rabbit Lung

    Directory of Open Access Journals (Sweden)

    Farzaneh Ketabchi

    2015-05-01

    Full Text Available Background: Some respiratory diseases may induce alveolar hypoxia thereby hypoxic pulmonary vasoconstriction (HPV. However, the mechanisms of this physiologic phenomenon are not fully understood. This study was the first to investigate the role of anion exchanger in sustained HPV. Methods: Experiments were performed in the isolated perfused rabbit lung. After preparation, the lungs were divided into six groups: two DIDS (4,4-diisothiocyanostilbene 2,2-disulfonic acid, anion exchanger inhibitor-treated [200 µM (n=5 or 400 µM (n=3] hypoxic groups, two HCO3- free hypoxic groups, one control hypoxic group (n=7 and one control normoxic group (n=4. DIDS were added to the perfusate at 10 minutes before starting the experiments. In the HCO3- free groups, HEPES (4-(2-Hydroxyethylpiperazine-1-ethanesulfonic acid were added to the perfusate instead of bicarbonate. Furthermore, in the HEPES1 (n=4 and HEPES2 (n=4 groups, the lungs were ventilated with hypoxic gas with or without CO2, respectively. Results: Ventilation of the lungs with hypoxic gas resulted in biphasic HPV, the acute (0-20 minutes and sustained (20-60 minutes phases. No alteration in both phases of HPV was detected by DIDS (200 µM. However, DIDS (400 µM, extended the ascending part of acute HPV until min 24. Both phases of HPV were decreased in the HEPES1 group. However, in the HEPES 2 group, HPV tended to increase during the rising part of the acute phase of HPV. Conclusions: Since DIDS (400 µM extended acute phase of HPV, and HCO3- free perfusate buffer enhanced rising phase of it, therefore it can be suggested that anion exchanger may modulate HPV especially during the acute phase. The abstract of this article was presented as a poster in the congress of European Respiratory Society (ERS on Monday, 08 September 2014, Munich, Germany and was published in the ERJ September 1, 2014 vol. 44 no. Suppl 58 P2343.

  10. Enantioseparation of Dencichine and D-Isomer on L-Cysteine Derivative Phase by Ligand-exchange Chromatography

    Institute of Scientific and Technical Information of China (English)

    Yan Shun MA; Qing Hua MENG; Hong Yu SHI; Yuan De LONG; Tian Bao HUANG

    2006-01-01

    The enantioseparation of dencichine and its D-isomer was achieved on a novel chiral stationary phase via coating N-(2-hydroxyl-3-octoxyl) propyl-S-benzyl-(L)-cysteine on YWG-C18phase by ligand exchange chromatography.

  11. Determination of {sup 129}I in environmental samples by AMS and NAA using an anion exchange resin disk

    Energy Technology Data Exchange (ETDEWEB)

    Suzuki, Takashi [AMS Management Section, Mutsu Establishment, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan)]. E-mail: suzuki.takashi58@jaea.go.jp; Banba, Shigeru [Natural Radioactivity Analysis Group, Japan Chemical Analysis Center, 295-3, Sanno-cho, Inage-ku, Chiba-shi, Chiba 263-0002 (Japan); Kitamura, Toshikatsu [AMS Management Section, Mutsu Establishment, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan); Kabuto, Shoji [AMS Management Section, Mutsu Establishment, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan); Isogai, Keisuke [Natural Radioactivity Analysis Group, Japan Chemical Analysis Center, 295-3, Sanno-cho, Inage-ku, Chiba-shi, Chiba 263-0002 (Japan); Amano, Hikaru [AMS Management Section, Mutsu Establishment, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan)

    2007-06-15

    We have developed a new extraction method for the measurement of {sup 129}I by accelerator mass spectrometry (AMS) utilizing an anion exchange resin disk. In comparison to traditional methods such as solvent extraction and ion exchange, this method provides for simple and quick sample handling. This extraction method was tested on soil, seaweed and milk samples, but because of disk clogging, the milk samples and some of the seaweed could not be applied successfully. Using this new extraction method to prepare samples for AMS analysis produced isotope ratios of iodine in good agreement with neutron activation analysis (NAA). The disk extraction method which take half an hour is faster than previous techniques, such as solvent extraction or ion exchange which take a few hours. The combination of the disk method and the AMS measurement is a powerful tool for the determination of {sup 129}I. Furthermore, these data will be available for the environmental monitoring before and during the operation of a new nuclear fuel reprocessing plant in Japan.

  12. 1,2,3-Triazolium-Based Poly(2,6-Dimethyl Phenylene Oxide) Copolymers as Anion Exchange Membranes.

    Science.gov (United States)

    Liu, Lei; He, Shuqing; Zhang, Shufang; Zhang, Min; Guiver, Michael D; Li, Nanwen

    2016-02-01

    Anion exchange membranes (AEMs) based on 1,2,3-triazolium (TAM) were prepared from commercial poly(2,6-dimethyl phenylene oxide) (PPO) via "click chemistry" and subsequent N-alkylation. Flexible and tough membranes with various ion exchange capacities (IECs) were obtained by casting the polymers from NMP solutions. Although the resulting TAM-functionalized PPOs (PPO-TAM) membranes exhibited incomplete ion exchange in 1 M NaOH or NaHCO3 for 24 h even at elevated temperature, the highest hydroxide conductivities of the membranes were above 20 mS/cm at room temperature, which is comparable to many reported AEMs. Alkaline stability tests indicate that the PPO-TAM membranes showed a better alkaline stability than that of membranes containing imidazolium groups in 1 M NaOH at 80 °C, but still require further improvements in long-term stability for alkaline fuel cell application. An investigation of alkaline stability of model compounds demonstrated the instability of TAM cations under alkaline conditions could contribute to the deprotonation of benzylic methylene, C4 and C5 position on the triazolium ring. These results suggests that the alkaline stability of 1,2,3-triazolium cation could be improved by the introduction of substituents at the C4, C5 positions and benzylic methylene, and also provide insight and directions for organic cation designs for AEM application by the facile synthetic strategy of "click chemistry". PMID:26820176

  13. Anion exchange polymer coated graphite granule electrodes for improving the performance of anodes in unbuffered microbial fuel cells

    Science.gov (United States)

    Wang, Xu; Li, Dengfeng; Mao, Xuhui; Yu, Eileen Hao; Scott, Keith; Zhang, Enren; Wang, Dihua

    2016-10-01

    In this paper, graphite granule composite electrodes are prepared for microbial fuel cells (MFCs) by coating commercial graphite granules with the mixture of quaternary DABCO polysulfone or Nafion ion exchange polymer and carbon black. The results of electrochemical impedance spectroscopy (EIS) suggest that the addition of carbon black could significantly improve the electrical conductivity of graphite granule anodes. When phosphate buffer solution (PBS) is replaced by NaCl solution, the current densities of the pristine anode, 0.08 g Nafion coated anode and 0.16 g QDPSU coated anode decrease by 52.6%, 20.6% and 10.3% at -0.2 V (vs. Ag/AgCl), respectively. The solution resistance of ion exchange polymer coated anodes is more stable in comparison with that of pristine anode. After 40 operational days, the performance drop of 0.16 g QDPSU coated anode when switching the solution from PBS to NaCl is still smaller than that of pristine anode. However, 0.08 g Nafion coated anode shows the similar performance in NaCl solution to the pristine anode after long term operation. This study reveals that QDPSU anion exchange polymer is more suitable for the anode modification. The QDPSU coated anode promises a great potential for three-dimensional anode based MFCs to treat domestic wastewater.

  14. Determination of 129I in environmental samples by AMS and NAA using an anion exchange resin disk

    Science.gov (United States)

    Suzuki, Takashi; Banba, Shigeru; Kitamura, Toshikatsu; Kabuto, Shoji; Isogai, Keisuke; Amano, Hikaru

    2007-06-01

    We have developed a new extraction method for the measurement of 129I by accelerator mass spectrometry (AMS) utilizing an anion exchange resin disk. In comparison to traditional methods such as solvent extraction and ion exchange, this method provides for simple and quick sample handling. This extraction method was tested on soil, seaweed and milk samples, but because of disk clogging, the milk samples and some of the seaweed could not be applied successfully. Using this new extraction method to prepare samples for AMS analysis produced isotope ratios of iodine in good agreement with neutron activation analysis (NAA). The disk extraction method which take half an hour is faster than previous techniques, such as solvent extraction or ion exchange which take a few hours. The combination of the disk method and the AMS measurement is a powerful tool for the determination of 129I. Furthermore, these data will be available for the environmental monitoring before and during the operation of a new nuclear fuel reprocessing plant in Japan.

  15. Mathematical modeling of salt-gradient ion-exchange simulated moving bed chromatography for protein separations

    Institute of Scientific and Technical Information of China (English)

    卢建刚

    2004-01-01

    The salt-gradient operation mode used in ion-exchange simulated moving bed chromatography (SMBC) can improve the efficiency of protein separations. A detailed model that takes into account any kind of adsorption/ion-exchange equilibrium, salt gradient, size exclusion, mass transfer resistance, and port periodic switching mechanism, was developed to simulate the complex dynamics. The model predictions were verified by the experimental data on upward and downward gradients for protein separations reported in the literature. All design and operating parameters (number, configuration, length and diameter of columns, particle size, switching period, flow rates of feed, raffinate, desorbent and extract, protein concentrations in feed, different salt concentrations in desorbent and feed) can be chosen correctly by numerical simulation. This model can facilitate the design, operation, optimization, control and scale-up of salt-gradient ion-exchange SMBC for protein separations.

  16. Liquid–liquid anion exchange extraction studies of samarium(III from salicylate media using high molecular weight amine

    Directory of Open Access Journals (Sweden)

    Aniruddha M. Mandhare

    2015-07-01

    Full Text Available Liquid–liquid extraction and separation of samarium(III were carried out by using 0.025 mol dm−3 2-octylaminopyridine(2-OAP in xylene at 298 K. The extraction behavior of samarium was studied as a function of pH, weak acid concentration, extractant concentration, diluent, and equilibration time. Samarium was quantitatively extracted at pH 7.5 to 10.0 from 0.01 mol dm−3 sodium salicylate solution with 0.025 mol dm−3 2-OAP. The possible composition of the extracted species in organic phase has been determined by using model of slope analysis method and extraction mechanism was found to proceed via an anion exchange mechanism. The stripping efficiency was found to be quantitative in HNO3, HCl and CH3COOH. The robustness of the procedure was demonstrated by the average recoveries obtained (>99.6% for samarium(III extraction in the presence of several cations and anions which are commonly associated with it. The proposed method facilitates the separation and determination of samarium(III from binary and synthetic mixtures. The various thermodynamic functions like free energy (ΔG, enthalpy (ΔH and entropy (ΔS of extraction mechanism were discussed.

  17. A SIM-MOF: three-dimensional organisation of single-ion magnets with anion-exchange capabilities.

    Science.gov (United States)

    Baldoví, José J; Coronado, Eugenio; Gaita-Ariño, Alejandro; Gamer, Christoph; Giménez-Marqués, Mónica; Mínguez Espallargas, Guillermo

    2014-08-18

    The formation of a metal-organic framework (MOF) with nodes that have single-molecule magnet (SMM) behaviour has been achieved by using mononuclear lanthanoid analogues, also known as single-ion magnets (SIMs), which enormously simplifies the challenging issue of making SMM-MOFs. Here we present a rational design of a family of MOFs, [Ln(bipyNO)4](TfO)3⋅x solvent (Ln=Tb (1); Dy (2); Ho (3); Er (4); TfO=triflate), in which the lanthanoid centres have an square-antiprismatic coordination environment suitable for SIM behaviour. Magnetic measurements confirm the existence of slow magnetic relaxation typical of SMMs, which has been rationalised by means of a radial effective charge model. In addition, we have explored the incorporation of bulky polyoxometalates (POMs) into the cavities of the SIM-MOF by anion exchange, finding that they do not interfere with the slow magnetic relaxation. This demonstrates the robustness of the frameworks and opens the possibility of incorporating non-innocent anions. PMID:24804629

  18. Illustrating Chromatography with Colorful Proteins

    Science.gov (United States)

    Lefebvre, Brian G.; Farrell, Stephanie; Dominiak, Richard S.

    2007-01-01

    Advances in biology are prompting new discoveries in the biotechnology, pharmaceutical, medical technology, and chemical industries. This paper presents a detailed description of an anion exchange chromatography experiment using a pair of colorful proteins and summarizes the effect of operating parameters on protein separation. This experiment…

  19. INTERACTION MECHANISM OF ORGANIC MATTER WITH GEL TYPE POLYSTYRENE STROUGLY BASIC ANION EXCHANGE RESIN AND REGENERATION OF THE ORGANISM FOULED RESIN I.The interreaction mechanism be

    Institute of Scientific and Technical Information of China (English)

    ZhuXingbao; WangZhansen; 等

    1995-01-01

    It was generally considered that contamination of the gel type polystyrene strong basic anion exchange resin by or ganic matter in natural water is the result of ion exchange and Van der waal′s adsorption on it.On the basis of laboratory and industrial experiments,this paper confirmed that the interreaction between organic matter and resin polymer matrix is primarily controled by a Van der waal′s adsorption.

  20. 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.

  1. Investigation on the Use of the Weakly Basic Polyacrylate Anion-Exchanger Amberlite IRA-68 for Sorption and Separation of Iminodiacetate Complexes of Rare Earth Elements

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Based on the determined affinity series of rare earth element complexes with IMDA for the anion-exchangers, purification of macroquantities of Nd3+ from Y3+, Sm3+ from Ho3+, La3+ from Nd3+ and La3+ from Pr3+ on the weakly basic gel anion-exchanger Amberlite IRA-68 was studied. Using the presented method on 1 L of Amberlite IRA-68 in the acetate form, it is possible to obtain about 240 g Nd2O3 purified from Y2O3. Great difference in affinity of La3+ and Nd3+ as well as Pr3+ complexes for this anion-exchanger in the acetate form indicates the possibility of applying this process for purification of lanthanum on the increased scale. On 1 L of Amberilte IRA-68 in the acetate form it is possible to obtain about 1125 g La2O3 purified from Nd2O3. On the basis of these results it can be assumed that unique properties of polyacrylate anion-exchangers enable their application for separation of rare earth elements.

  2. Application of the two-film theory to the determination of mass transfer coefficients for bovine serum albumin on anion-exchange columns

    DEFF Research Database (Denmark)

    Hansen, Ernst; Mollerup, Jørgen

    1999-01-01

    -all driving force models fail to describe the flux correctly and this is substantiated by the theory. Results obtained with BSA on the anion exchange media Q HyperD, Source, and Poros show that the external film resistance is significant for Reynolds numbers less than one. The experimental Sherwood numbers...

  3. Synthesis and performance of novel anion exchange membranes based on imidazolium ionic liquids for alkaline fuel cell applications

    Science.gov (United States)

    Fang, Jun; Lyu, Ming; Wang, Xin; Wu, Yongbin; Zhao, Jinbao

    2015-06-01

    Novel anion exchange membranes (AEMs) based on two types of imidazolium ionic liquids, 1-vinyl-3-methylimidazolium iodide [VMI]I and 1-vinyl-3-butylimidazolium bromide [VBI]Br, have been synthesized by copolymerization. The obtained membranes are characterized in terms of water uptake, ion exchange capacity (IEC), ionic conductivity as well as thermal and chemical stability. The conductivity reaches 0.0226 Scm-1 at 30 °C. All the membranes show excellent thermostability. The membranes are stable in 10 mol L-1 NaOH solution at 60 °C for 120 h without obvious changes in ion conductivity. Fuel cell performance using the resulting membrane has been investigated. The open circuit voltage (OCV) of the H2/O2 fuel cell is 1.07 V. A peek power density of 116 mW cm-2 is obtained at a current density of 230 mA cm-2 at 60 °C. The results demonstrate the brilliant prospect of the developed membranes for alkaline fuel cell applications.

  4. Comparison in the extraction properties of Pu(IV) in piperidinium and pyrrolidinium nitrate anchored anion exchange resins

    Energy Technology Data Exchange (ETDEWEB)

    Selvan, B. Robert; Suneesh, A.S.; Venkatesan, K.A.; Antony, M.P.; Vasudeva Rao, P.R. [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Fuel Chemistry Div.

    2016-07-01

    Piperidinium nitrate (Pip-NO{sub 3}) and pyrrolidinium nitrate (Pyr-NO{sub 3}) functional groups were anchored on a poly(styrene-divinylbenzene) matrix and evaluated the resultant anion exchange resin for the extraction of plutonium from nitric acid medium. The distribution coefficient (K{sub d}, mL/g) of Pu(IV) in these resins increased with the concentration of nitric acid, reaching a maximum K{sub d} at 7 M nitric acid, followed by decrease. The extraction of Pu(IV) increased with the duration of equilibration followed by the establishment of equilibrium, occurred within four hours of equilibration. The kinetic data were fitted with pseudo-first order and pseudo-second order rate equations. The apparent plutonium exchange capacity was determined to be ∝256 mg/g for Pip-NO{sub 3} resin and 285 mg/g for Pyr-NO{sub 3} resin at 7 M nitric acid. The radiolytic degradation of Pip-NO{sub 3} and Pyr-NO{sub 3} in presence of nitric acid (7 M) was studied upto a dose of 200 KGy and the results are reported in this paper.

  5. Characterization of an anionic-exchange membranes for direct methanol alkaline fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Abuin, Graciela C. [Centro de Procesos Superficiales, Instituto Nacional de Tecnologia Industrial (INTI), Av. Gral. Paz 5445, B1650KNA, San Martin, Buenos Aires (Argentina); Nonjola, Patrick; Mathe, Mkhulu K. [Council for Scientific and Industrial Research (CSIR), Material Science and Manufacturing, PO Box 395, Brumeria, Pretoria 0001 (South Africa); Franceschini, Esteban A.; Izraelevitch, Federico H.; Corti, Horacio R. [Departamento de Fisica de la Materia Condensada, Comision Nacional de Energia Atomica (CNEA), Av. Gral. Paz 1499, B1650KNA, San Martin, Buenos Aires (Argentina)

    2010-06-15

    Ammonium quaternized polymers such as poly (arylene ether sulfones) are being developed and studied as candidates of ionomeric materials for application in alkaline fuel cells, due to their low cost and promising electrochemical properties. In this work, a quaternary ammonium polymer was synthesized by chloromethylation of a commercial polysulfone followed by amination process. Quaternized polysulfone membrane properties such us water and water-methanol uptake, electrical conductivity and Young's modulus were evaluated and compared to Nafion 117, commonly employed in direct methanol fuel cells. The anionic polysulfone membrane sorbs more water than Nafion all over the whole range of water activities, but it uptakes much less methanol as compared to Nafion. The specific conductivity of the fully hydrated polysulfone membrane equilibrated with KOH solutions at ambient temperature increases with the KOH concentration, reaching a maximum of 0.083 S cm{sup -1} for 2 M KOH, slightly less conductive than Nafion 117. The elastic modulus of the polysulfone membranes inmersed in water is similar to that reported for Nafion membranes under the same conditions. We concluded that quaternized polysulfone membrane are good candidates as electrolytes in alkaline direct methanol fuel cells. (author)

  6. Chromium (VI removal from aqueous solutions by purolite base anion-exchange resins with gel structure

    Directory of Open Access Journals (Sweden)

    Balan Catalin

    2013-01-01

    Full Text Available The removal of Cr (VI from aqueous solution using two strong base anionic resins with gel structure, Purolite A-400 (styrene-divinylbenzene matrix and Purolite A-850 (acrylic matrix was investigated in batch technique. The sorption efficiency was determined as a function of phases contact time, solution pH, resin dose, temperature and initial Cr (VI concentration. The percentage of Cr (VI removed reaches maximum values (up to 99 % in the pH range 4 - 5.3 under a resin dose of 6 g/L and of Cr (VI concentration up to 100 mg/L. An increase in temperature has a positive effect on the Cr (VI sorption process. The equilibrium sorption data were fitted with the Freundlich, Langmuir and Dubinin-Radushkevich isotherm models, using both linear and nonlinear regression method. The Langmuir model very well verifies the experimental data and gives the maximum sorption capacity of 120.55 mg Cr (VI/g and 95.82 mg Cr (VI/g for A-400 and A-850 resins, respectively. The thermodynamic study and mean free energy of sorption values calculated using Dubinin-Radushkevich equation indicated the sorption is a chemical endothermic process. The kinetic data were well described by pseudo-second order kinetic equation and the sorption process is controlled by external (film diffusion and intraparticle diffusion.

  7. Determination of plutonium in environmental samples by controlled valence in anion exchange

    DEFF Research Database (Denmark)

    Chen, Q.J.; Aarkrog, A.; Nielsen, S.P.;

    1993-01-01

    The title method was successfully used for collecting Pu-239, Pu-249 from 200 litres of seawater by coprecipitation with 16 g FeSO4 . 7H2O under reducing conditions without filtering. The plutonium is leached by concentrated HNO3 + HCI from the coprecipitate and the solid particles. The precipitate...... is heated at 400-degrees-C and digested in aqua regia. Na2SO3 and NaNO2 have been applied to obtain the Pu4+ valence state in 0.571 N HN03 for different samples. Plutonium and thorium are coadsorbed on anionic resin from 8N HN03. The column is eluted with 8N HN03 containing fresh NaNO2 to keep the Pu4......+ state for uranium decontamination. The system of the column is changed from 8N HNO3 to concentrated HCl with 50 ml concentrated HCI containing a few milligrams of NaNO2. Further decontamination of thorium was achieved by elution with concentrated HCI instead of 9N HCl. The plutonium is successfully...

  8. Determination of plutonium in environmental samples by controlled valence in anion exchange

    International Nuclear Information System (INIS)

    The method was successfully used for collecting 239,240Pu from 200 litres seawater by coprecipitation with 16 g FeSO4.7H2O under reducing conditions without filtering. The plutonium is leached by concentrated HNO3 + HCl from the coprecipitate and the solid particles. The precipitate is heated at 400 deg. C and digested in aqua regia. Na2SO3 and NaNO2 have been applied to obtain Pu+4 valence in 0.5-1 N HNO3 for different samples. Plutonium and thorium are coabsorbed on anionic resin from 8 N HNO3. The column is eluated with 8 N HNO3 containing fresh NaNO2 to keep Pu+4 valence for uranium decontamination. The system of the column is changed from 8 N HNO3 to concentrated HCl with 50 ml conc. HCl containing a few milligram NaNO2. Further decontamination of thorium was achieved by eluation with concentrated HCl instead of 9 N HCl. The plutonium is successfully stripped by H2O, NaOH, 2 N HNO3 and 0.5 N HNO3 containing 0.01 M NaNO3. The chemical yield of plutonium for a 200 litres-seawater sample is 60-80%. The resolution of the electroplated thin source is very good. (author)

  9. Measuring various anions content in water with ion chromatography method%离子色谱法测定水中多种阴离子的含量

    Institute of Scientific and Technical Information of China (English)

    徐胜

    2014-01-01

    介绍了离子色谱仪的工作原理与工作流程,对离子色谱法测定水中多种阴离子含量的试验方法进行了论述,通过试验得到了水中各离子的标准物质色谱图、标准曲线及标准溶液度的偏差等,指出运用离子色谱法测定水中阴离子含量操作方便,效率高。%The paper introduces the working principles and working procedures of ion chromatography, discusses various anions content testing method with ion chromatography method, and achieves their standard chromatogram, standard curve and standard solution errors and so on, and finally points out advantages of applying ion chromatography method to test anions content, such as convenient operation and high efficiency.

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

    Science.gov (United States)

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

    2015-08-28

    Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with <1mL of sample. This new approach provides a reliable and robust analytical method for the simultaneous determination of organic and inorganic anions, including fluoride, methanesulfonate, chloride, sulfate and nitrate anions. Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak.

  11. 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.

  12. 离子色谱法测定炸药FOX7中3种阴离子%Determination of Three Anions in FOX7 by Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    张勇; 何乃珍; 郭蓉; 索志荣

    2014-01-01

    建立了测定炸药FOX7中3种阴离子的离子色谱分析方法,并用该方法测定了炸药FOX7。采用离子色谱检测法,以Metrosep A Supp5-250型阴离子柱为色谱柱;3.2 mmol/L Na2 CO3+1.0 mmol/L NaHCO3为流动相,流速为0.7 mL/min。结果表明:测定SO2-4、 NO3-、 Cl-三种离子的精密度试验、重复性试验、加样回收率试验的RSD均小于3.0%,平均回收率( n=6)分别为99.1%,98.4%和99.0%。方法快速,准确,可用于炸药FOX7的质量控制。%An ion chromatography method was established for determining of three kinds of anions in FOX7 simultaneously. Ion chromatography was used. The anions were analyzed on Metrosep A Supp5 -250 anion exchange column and the mobile phase consisted of 3. 2 mmol/L Na2 CO3 +1. 0 mmol/L NaHCO3. The flow rate was 0. 7 mL/min. The RSD of precision test, reproducibility test and recovery test were all less than 3%. The average recoveries ( n=6 ) were 99. 1% for SO2-4 , 98. 4% for NO3- and 99. 0% for Cl-, respectively. A rapid, sensitive and accurate method for the determination of three kinds of anions was founded. This study may provide a scientific basis for the quality control of FOX7.

  13. Formation of Semimetallic Cobalt Telluride Nanotube Film via Anion Exchange Tellurization Strategy in Aqueous Solution for Electrocatalytic Applications.

    Science.gov (United States)

    Patil, Supriya A; Kim, Eun-Kyung; Shrestha, Nabeen K; Chang, Jinho; Lee, Joong Kee; Han, Sung-Hwan

    2015-11-25

    Metal telluride nanostructures have demonstrated several potential applications particularly in harvesting and storing green energy. Metal tellurides are synthesized by tellurization process performed basically at high temperature in reducing gas atmosphere, which makes the process expensive and complicated. The development of a facile and economical process for desirable metal telluride nanostructures without complicated manipulation is still a challenge. In an effort to develop an alternative strategy of tellurization, herein we report a thin film formation of self-standing cobalt telluride nanotubes on various conducting and nonconducting substrates using a simple binder-free synthetic strategy based on anion exchange transformation from a thin film of cobalt hydroxycarbonate nanostructures in aqueous solution at room temperature. The nanostructured films before and after ion exchange transformation reaction are characterized using field emission scanning electron microscope, energy dispersive X-ray analyzer, X-ray photoelectron spectroscopy, thin film X-ray diffraction technique, high resolution transmission electron microscope, and selected area electron diffraction analysis technique. After the ion exchange transformation of nanostructures, the film shows conversion from insulator to highly electrical conductive semimetallic characteristic. When used as a counter electrode in I3(-)/I(-) redox electrolyte based dye-sensitized solar cells, the telluride film exhibits an electrocatalytic reduction activity for I3(-) with a demonstration of solar-light to electrical power conversion efficiency of 8.10%, which is highly competitive to the efficiency of 8.20% exhibited by a benchmarked Pt-film counter electrode. On the other hand, the telluride film electrode also demonstrates electrocatalytic activity for oxygen evolution reaction from oxidation of water.

  14. Arsenate Adsorption by Hydrous Ferric Oxide Nanoparticles Embedded in Cross-linked Anion Exchanger: Effect of the Host Pore Structure.

    Science.gov (United States)

    Li, Hongchao; Shan, Chao; Zhang, Yanyang; Cai, Jianguo; Zhang, Weiming; Pan, Bingcai

    2016-02-10

    Three composite adsorbents were fabricated via confined growth of hydrous ferric oxide (HFO) nanoparticles within cross-linked anion exchangers (NS) of different pore size distributions to investigate the effect of host pore structure on the adsorption of As(V). With the decrease in the average pore size of the NS hosts from 38.7 to 9.2 nm, the mean diameter of the confined HFO nanoparticles was lessened from 31.4 to 11.6 nm as observed by transmission electron microscopy (TEM), while the density of active surface sites was increased due to size-dependent effect proved by potentiometric titration. The adsorption capacity of As(V) yielded by Sips model was elevated from 24.2 to 31.6 mg/g via tailoring the pore size of the NS hosts, and the adsorption kinetics was slightly accelerated with the decrease of pore size in background solution containing 500 mg/L of Cl(-). Furthermore, the enhanced adsorption of As(V) was achieved over a wide pH range from 3 to 10, as well as in the presence of competing anions including Cl(-), SO4(2-), HCO3(-), NO3(-) (up to 800 mg/L), and PO4(3-) (up to 10 mg P/L). In addition, the fixed-bed working capacity increased from 2200 to 2950 bed volumes (BV) owing to the size confinement effect, which did not have adverse effect on the desorption of As(V) as the cumulative desorption efficiency reached 94% with 10 BV of binary solution (5% NaOH + 5% NaCl) for all the three adsorbents. Therefore, this study provided a promising strategy to regulate the reactivity of the nanoparticles via the size confinement effect of the host pore structure. PMID:26765396

  15. New inorganic (an)ion exchangers with a higher affinity for arsenate and a competitive removal capacity towards fluoride, bromate, bromide, selenate, selenite, arsenite and borate

    KAUST Repository

    Chubar, Natalia

    2011-12-01

    Highly selective materials and effective technologies are needed to meet the increasingly stronger drinking water standards for targeted ionic species. Inorganic ion exchangers based on individual and mixed-metal hydrous oxides (or mixed adsorbents that contain inorganic ion exchangers in their composition) are adsorptive materials that are capable of lowering the concentrations of anionic contaminants, such as H 2AsO 4 -, H 3AsO 3, F -, Br -, BrO 3 -, HSeO 4 -, HSeO 3 - and H 3BO 3, to 10 μg/L or less. To achieve a higher selectivity towards arsenate, a new ion exchanger based on Mg-Al hydrous oxides was developed by a novel, cost-effective and environmentally friendly synthesis method via a non-traditional (alkoxide-free) sol-gel approach. The exceptional adsorptive capacity of the Mg-Al hydrous oxides towards H 2AsO 4 - (up to 200 mg[As]/gdw) is due to the high affinity of this sorbent towards arsenate (steep equilibrium isotherms) and its fast adsorption kinetics. Because of the mesoporous (as determined by N 2 adsorption and SEM) and layered (as determined by XRD and FTIR) structure of the ion-exchange material as well as the abundance of anion exchange sites (as determined by XPS and potentiometric titration) on its surface the material demonstrated very competitive (or very high) removal capacity towards other targeted anions, including fluoride, bromide, bromate, selenate, selenite, and borate. © 2011 IWA Publishing.

  16. 3-Methyltrimethylammonium poly(2,6-dimethyl-1,4-phenylene oxide) based anion exchange membrane for alkaline polymer electrolyte fuel cells

    Indian Academy of Sciences (India)

    K Hari Gopi; S Gouse Peera; S D Bhat; P Sridhar; S Pitchumani

    2014-06-01

    Hydroxyl ion (OH–) conducting anion exchange membranes based on modified poly (phenylene oxide) are fabricated for their application in alkaline polymer electrolyte fuel cells (APEFCs). In the present study, chloromethylation of poly(phenylene oxide) (PPO) is performed by aryl substitution rather than benzyl substitution and homogeneously quaternized to form an anion exchange membrane (AEM). 1H NMR and FT–IR studies reveal successful incorporation of the above groups in the polymer backbone. The membrane is characterized for its ion exchange capacity and water uptake. The membrane formed by these processes show good ionic conductivity and when used in fuel cell exhibited an enhanced performance in comparison with the state-of-the-art commercial AHA membrane. A peak power density of 111 mW/cm2 at a load current density of 250 mA/cm2 is obtained for PPO based membrane in APEFCs at 30 °C.

  17. Efficiencies and Optimization of Weak Base Anion Ion-Exchange Resin for Groundwater Hexavalent Chromium Removal at Hanford

    Energy Technology Data Exchange (ETDEWEB)

    Nesham, Dean O.; Ivarson, Kristine A.; Hanson, James P.; Miller, Charles W.; Meyers, P.; Jaschke, Naomi M.

    2014-02-03

    The U.S. Department of Energy’s (DOE’s) contractor, CH2M HILL Plateau Remediation Company, has successfully converted a series of groundwater treatment facilities to use a new treatment resin that is delivering more than $3 million in annual cost savings and efficiency in treating groundwater contamination at the DOE Hanford Site in southeastern Washington State. During the production era, the nuclear reactors at the Hanford Site required a continuous supply of high-quality cooling water during operations. Cooling water consumption ranged from about 151,417 to 378,541 L/min (40,000 to 100,000 gal/min) per reactor, depending on specific operating conditions. Water from the Columbia River was filtered and treated chemically prior to use as cooling water, including the addition of sodium dichromate as a corrosion inhibitor. Hexavalent chromium was the primary component of the sodium dichromate and was introduced into the groundwater at the Hanford Site as a result of planned and unplanned discharges from the reactors starting in 1944. Groundwater contamination by hexavalent chromium and other contaminants related to nuclear reactor operations resulted in the need for groundwater remedial actions within the Hanford Site reactor areas. Beginning in 1995, groundwater treatment methods were evaluated, leading to the use of pump-and-treat facilities with ion exchange using Dowex™ 21K, a regenerable, strong-base anion exchange resin. This required regeneration of the resin, which was performed offsite. In 2008, DOE recognized that regulatory agreements would require significant expansion for the groundwater chromium treatment capacity. As a result, CH2M HILL performed testing at the Hanford Site in 2009 and 2010 to demonstrate resin performance in the specific groundwater chemistry at different waste sites. The testing demonstrated that a weak-base anion, single-use resin, specifically ResinTech SIR-700 ®, was effective at removing chromium, had a significantly

  18. Sequential determination system for anionic detergents by complexation with methylene blue by dual high-speed counter-current chromatography

    OpenAIRE

    Kitazume, Eiich; Koikawa, Saki; Hui, Lu; Sannohe, Syou; Yang, Yanjun; Yonosuke, Maki; Ito, Yoichiro

    2012-01-01

    A new dual high-speed counter-current chromatographic system using organic extraction phase and aqueous mobile phase containing methylene blue was applied to the analysis of anionic-type detergents. After selecting appropriate conditions such as flow rate of each mobile phase, sample volume, etc., the new system was successfully applied to the analysis of anionic detergent in river water. As all the analytical procedure can be made in a closed system, the method has no health hazard. The pres...

  19. Single-Crystal-to-Single-Crystal Anion Exchange in a Gadolinium MOF: Incorporation of POMs and [AuCl4]−

    Directory of Open Access Journals (Sweden)

    Javier López-Cabrelles

    2016-04-01

    Full Text Available The encapsulation of functional molecules inside porous coordination polymers (also known as metal-organic frameworks, MOFs has become of great interest in recent years at the field of multifunctional materials. In this article, we present a study of the effects of size and charge in the anion exchange process of a Gd based MOF, involving molecular species like polyoxometalates (POMs, and [AuCl4]−. This post-synthetic modification has been characterized by IR, EDAX, and single crystal diffraction, which have provided unequivocal evidence of the location of the anion molecules in the framework.

  20. Recovery of lactic acid from simultaneous saccharification and fermentation media using anion exchange resins.

    Science.gov (United States)

    Moldes, A B; Alonso, J L; Parajó, J C

    2003-07-01

    The physicochemical properties (capacity, kinetics and selectivity) of the ion exchange resins Amberlite IRA900, IRA400, IRA96 and IRA67 were determined to evaluate their comparative suitability for lactic acid recovery. Both the kinetics of lactic acid sorption from aqueous solutions and the equilibrium were assessed using mathematical models, which provided a close interpretation of the experimental results. The best resins (Amberlite IRA96 and IRA67) were employed in further fixed-bed operation using aqueous lactic acid solutions as feed. In this set of experiments, parameters such as capacity, regenerant consumption, percentage of lactic acid recovery and product concentration were measured. Amberlite IRA67, a weak base resin, was selected for lactic acid recovery from SSF (simultaneous saccharification and fermentation) broths. Owing to the presence of nutrients and ions other than lactate, a slightly decreased capacity was determined when using SSF media instead aqueous lactic acid solutions, but quantitative lactic acid recoveries at constant capacities were obtained in four sequential load/regeneration cycles.

  1. Ion Mobility Spectrometry-Hydrogen Deuterium Exchange Mass Spectrometry of Anions: Part 3. Estimating Surface Area Exposure by Deuterium Uptake.

    Science.gov (United States)

    Khakinejad, Mahdiar; Kondalaji, Samaneh Ghassabi; Donohoe, Gregory C; Valentine, Stephen J

    2016-03-01

    Gas-phase hydrogen deuterium exchange (HDX), collision cross section (CCS) measurement, and molecular dynamics simulation (MDS) techniques were utilized to develop and compare three methods for estimating the relative surface area exposure of separate peptide chains within bovine insulin ions. Electrosprayed [M - 3H](3-) and [M - 5H](5-) insulin ions produced a single conformer type with respective collision cross sections of 528 ± 5 Å(2) and 808 ± 2 Å(2). [M - 4H](4-) ions were comprised of more compact (Ω = 676 ± 3 Å(2)) and diffuse (i.e., more elongated, Ω = 779 ± 3 Å(2)) ion conformer types. Ions were subjected to HDX in the drift tube using D2O as the reagent gas. Collision-induced dissociation was used to fragment mobility-selected, isotopically labeled [M - 4H](4-) and [M - 5H](5-) ions into the protein subchains. Deuterium uptake levels of each chain can be explained by limited inter-chain isotopic scrambling upon collisional activation. Using nominal ion structures from MDS and a hydrogen accessibility model, the deuterium uptake for each chain was correlated to its exposed surface area. In separate experiments, the per-residue deuterium content for the protonated and deprotonated ions of the synthetic peptide KKDDDDDIIKIIK were compared. The differences in deuterium content indicated the regional HDX accessibility for cations versus anions. Using ions of similar conformational type, this comparison highlights the complementary nature of HDX data obtained from positive- and negative-ion analysis. PMID:26620531

  2. The oxidative degradation of polystyrene resins on the removal of Cr(VI) from wastewater by anion exchange.

    Science.gov (United States)

    Xiao, Ke; Xu, Fuyuan; Jiang, Linhua; Dan, Zhigang; Duan, Ning

    2016-08-01

    Cr(VI) is a powerful oxidant and is capable of oxidizing most of the organic materials. Therefore, it is possible for Cr(VI) to oxidize the polymeric resins and change the sorption properties of the resins on the removal of Cr(VI) from wastewater by anion exchange. In this study, three polystyrene resins (D201, D202, and D301) with different functional groups (-N(+)(CH3)3, -N(+)(CH3)2(C2H4OH), and N(CH3)2) were assessed on oxidation stability for Cr(VI) removal from wastewater in fixed-bed column experiments. After a 10-cycle operation, due to the oxidation of the resin, the sorption capacity of D201, D202, and D301 resins decreased by 23.5, 29.3, and 17.3%, when approximately 20-34%, 31-50%, and 18-30% of Cr(VI) was reduced to Cr(III) during each cycle respectively. The results of the Fourier transform infrared spectroscopy (FT-IR) showed that both the cleavage of CN and the formation of CO bonds occurred on the polystyrene resins during the Cr(VI) removal process. The resin simulation experiments further validated the oxidation of CC and CN bonds connected with phenethyl groups. Based upon the results from column operations and the resin simulated experiments, the oxidation mechanism of the polystyrene resin was proposed.

  3. Novel carbamoyl type quinine and quinidine based chiral anion exchangers implementing alkyne-azide cycloaddition immobilization chemistry.

    Science.gov (United States)

    Hettegger, Hubert; Kohout, Michal; Mimini, Vebi; Lindner, Wolfgang

    2014-04-11

    The synthesis and chromatographic evaluation of a series of new Cinchona derived chiral weak anion exchangers is presented. Huisgen Cu(I) mediated alkyne-azide cycloaddition, so-called click chemistry, was used as an immobilization strategy. In this way it was possible to immobilize about 90% of offered selector via 1,2,3-triazole linker, which displays a more efficient way of binding the selector to modified silica compared to common radical mediated thiol-ene addition. Problems associated with potential radical scavenging properties of chiral selectors thereby could be circumvented. The evaluation of the synthesized chiral stationary phases regarding chromatographic behavior was carried out using polar organic mode mobile phase composition and a set of representative chiral organic acids. Different loading densities revealed an optimum selector density of about 310μmol/g chiral stationary phase with respect to resolution and selectivity. A decrease of performance was observed for higher loading, indicating mutual spatial influence of selector units leading to sterical hindrance. In addition, we observed that the effect of free azide groups on retention is negligible and the overall chromatographic behavior is comparable to other Cinchona derived chiral stationary phases.

  4. Ion Mobility Spectrometry-Hydrogen Deuterium Exchange Mass Spectrometry of Anions: Part 2. Assessing Charge Site Location and Isotope Scrambling

    Science.gov (United States)

    Khakinejad, Mahdiar; Ghassabi Kondalaji, Samaneh; Donohoe, Gregory C.; Valentine, Stephen J.

    2016-03-01

    Ion mobility spectrometry (IMS) coupled with gas-phase hydrogen deuterium exchange (HDX)-mass spectrometry (MS) and molecular dynamic simulations (MDS) has been used for structural investigation of anions produced by electrospraying a sample containing a synthetic peptide having the sequence KKDDDDDIIKIIK. In these experiments the potential of the analytical method for locating charge sites on ions as well as for utilizing collision-induced dissociation (CID) to reveal the degree of deuterium uptake within specific amino acid residues has been assessed. For diffuse (i.e., more elongated) [M - 2H]2- ions, decreased deuterium content along with MDS data suggest that the D4 and D6 residues are charge sites, whereas for the more diffuse [M - 3H]3- ions, the data suggest that the D4, D7, and the C-terminus are deprotonated. Fragmentation of mobility-selected, diffuse [M - 2H]2- ions to determine deuterium uptake at individual amino acid residues reveals a degree of deuterium retention at incorporation sites. Although the diffuse [M - 3H]3- ions may show more HD scrambling, it is not possible to clearly distinguish HD scrambling from the expected deuterium uptake based on a hydrogen accessibility model. The capability of the IMS-HDX-MS/MS approach to provide relevant details about ion structure is discussed. Additionally, the ability to extend the approach for locating protonation sites on positively-charged ions is presented.

  5. Oxygen evolution reaction characteristics of synthetic nickel-cobalt-oxide electrodes for alkaline anion-exchange membrane water electrolysis

    Science.gov (United States)

    Koo, Tae Woo; Park, ChanSu; Kim, Yang Do; Lee, Dooyong; Park, Sungkyun; Lee, Jae Ho; Choi, Sung Mook; Choi, Chul Young

    2015-11-01

    A polymer electrolyte membrane water electrolysis system can produce high-purity hydrogen gases in a highly efficient manner. However, the level of hydrogen gas production is still small. In addition, noble-metal catalysts for the reaction in acidic environments, as well as an additional drying step to remove water contained in the hydrogen, are required. Therefore, water electrolysis system with high efficiency and lower cost, an alkaline anion-exchange membrane system that can produce high-purity hydrogen without a noble-metal catalyst, is needed. Nano-size NiCo2O4 powders were prepared by using a sol-gel method to achieve an efficient and economical water electrolysis system. When the powder was calcined at 450 °C, the crystallinity and the cyclic voltammogram measurement showed the best values. In addition, the 15-wt.% polytetrafluoroethylene mixed NiCo2O4 powders exhibited the largest cyclic voltammetry active area and the highest oxygen evolution reaction activity with the appropriate stability.

  6. Quaternized adamantane-containing poly(aryl ether ketone) anion exchange membranes for vanadium redox flow battery applications

    Science.gov (United States)

    Zhang, Bengui; Zhang, Shouhai; Weng, Zhihuan; Wang, Guosheng; Zhang, Enlei; Yu, Ping; Chen, Xiaomeng; Wang, Xinwei

    2016-09-01

    Quaternized adamantane-containing poly(aryl ether ketone) anion exchange membranes (QADMPEK) are prepared and investigated for vanadium redox flow batteries (VRFB) application. The bulky, rigid and highly hydrophobic adamantane segment incorporated into the backbone of membrane material makes QADMPEK membranes have low water uptake and swelling ratio, and the as-prepared membranes display significantly lower permeability of vanadium ions than that of Nafion117 membrane. As a consequence, the VRFB cell with QADMPEK-3 membrane shows higher coulombic efficiency (99.4%) and energy efficiency (84.0%) than those for Nafion117 membrane (95.2% and 80.5%, respectively) at the current density of 80 mA cm-2. Furthermore, at a much higher current density of 140 mA cm-2, QADMPEK membrane still exhibits better coulombic efficiency and energy efficiency than Nafion117 membrane (coulombic efficiency 99.2% vs 96.5% and energy efficiency 76.0% vs 74.0%). Moreover, QADMPEK membranes show high stability in in-situ VRFB cycle test and ex-situ oxidation stability test. These results indicate that QADMPEK membranes are good candidates for VRFB applications.

  7. Ion Mobility Spectrometry-Hydrogen Deuterium Exchange Mass Spectrometry of Anions: Part 3. Estimating Surface Area Exposure by Deuterium Uptake

    Science.gov (United States)

    Khakinejad, Mahdiar; Ghassabi Kondalaji, Samaneh; Donohoe, Gregory C.; Valentine, Stephen J.

    2016-03-01

    Gas-phase hydrogen deuterium exchange (HDX), collision cross section (CCS) measurement, and molecular dynamics simulation (MDS) techniques were utilized to develop and compare three methods for estimating the relative surface area exposure of separate peptide chains within bovine insulin ions. Electrosprayed [M - 3H]3- and [M - 5H]5- insulin ions produced a single conformer type with respective collision cross sections of 528 ± 5 Å2 and 808 ± 2 Å2. [M - 4H]4- ions were comprised of more compact (Ω = 676 ± 3 Å2) and diffuse (i.e., more elongated, Ω = 779 ± 3 Å2) ion conformer types. Ions were subjected to HDX in the drift tube using D2O as the reagent gas. Collision-induced dissociation was used to fragment mobility-selected, isotopically labeled [M - 4H]4- and [M - 5H]5- ions into the protein subchains. Deuterium uptake levels of each chain can be explained by limited inter-chain isotopic scrambling upon collisional activation. Using nominal ion structures from MDS and a hydrogen accessibility model, the deuterium uptake for each chain was correlated to its exposed surface area. In separate experiments, the per-residue deuterium content for the protonated and deprotonated ions of the synthetic peptide KKDDDDDIIKIIK were compared. The differences in deuterium content indicated the regional HDX accessibility for cations versus anions. Using ions of similar conformational type, this comparison highlights the complementary nature of HDX data obtained from positive- and negative-ion analysis.

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

    Directory of Open Access Journals (Sweden)

    Rukowicz Beata

    2014-06-01

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

  9. Recent Advances in Solid Catalysts Obtained by Metalloporphyrins Immobilization on Layered Anionic Exchangers: A Short Review and Some New Catalytic Results

    Directory of Open Access Journals (Sweden)

    Shirley Nakagaki

    2016-02-01

    Full Text Available Layered materials are a very interesting class of compounds obtained by stacking of two-dimensional layers along the basal axis. A remarkable property of these materials is their capacity to interact with a variety of chemical species, irrespective of their charge (neutral, cationic or anionic. These species can be grafted onto the surface of the layered materials or intercalated between the layers, to expand or contract the interlayer distance. Metalloporphyrins, which are typically soluble oxidation catalysts, are examples of molecules that can interact with layered materials. This work presents a short review of the studies involving metalloporphyrin immobilization on two different anionic exchangers, Layered Double Hydroxides (LDHs and Layered Hydroxide Salts (LHSs, published over the past year. After immobilization of anionic porphyrins, the resulting solids behave as reusable catalysts for heterogeneous oxidation processes. Although a large number of publications involving metalloporphyrin immobilization on LDHs exist, only a few papers have dealt with LHSs as supports, so metalloporphyrins immobilized on LHSs represent a new and promising research field. This work also describes new results on an anionic manganese porphyrin (MnP immobilized on Mg/Al-LDH solids with different nominal Mg/Al molar ratios (2:1, 3:1 and 4:1 and intercalated with different anions (CO32− or NO3−. The influence of the support composition on the MnP immobilization rates and the catalytic performance of the resulting solid in cyclooctene oxidation reactions will be reported.

  10. Recent Advances in Solid Catalysts Obtained by Metalloporphyrins Immobilization on Layered Anionic Exchangers: A Short Review and Some New Catalytic Results.

    Science.gov (United States)

    Nakagaki, Shirley; Mantovani, Karen Mary; Machado, Guilherme Sippel; Castro, Kelly Aparecida Dias de Freitas; Wypych, Fernando

    2016-01-01

    Layered materials are a very interesting class of compounds obtained by stacking of two-dimensional layers along the basal axis. A remarkable property of these materials is their capacity to interact with a variety of chemical species, irrespective of their charge (neutral, cationic or anionic). These species can be grafted onto the surface of the layered materials or intercalated between the layers, to expand or contract the interlayer distance. Metalloporphyrins, which are typically soluble oxidation catalysts, are examples of molecules that can interact with layered materials. This work presents a short review of the studies involving metalloporphyrin immobilization on two different anionic exchangers, Layered Double Hydroxides (LDHs) and Layered Hydroxide Salts (LHSs), published over the past year. After immobilization of anionic porphyrins, the resulting solids behave as reusable catalysts for heterogeneous oxidation processes. Although a large number of publications involving metalloporphyrin immobilization on LDHs exist, only a few papers have dealt with LHSs as supports, so metalloporphyrins immobilized on LHSs represent a new and promising research field. This work also describes new results on an anionic manganese porphyrin (MnP) immobilized on Mg/Al-LDH solids with different nominal Mg/Al molar ratios (2:1, 3:1 and 4:1) and intercalated with different anions (CO₃(2-) or NO₃(-)). The influence of the support composition on the MnP immobilization rates and the catalytic performance of the resulting solid in cyclooctene oxidation reactions will be reported. PMID:26938518

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

    Directory of Open Access Journals (Sweden)

    Sérgio Freire de Carvalhaes

    2002-01-01

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

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

    International Nuclear Information System (INIS)

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-06-01

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

  14. Anion- or Cation-Exchange Membranes for NaBH4/H2O2 Fuel Cells?

    Directory of Open Access Journals (Sweden)

    César A. C. Sequeira

    2012-07-01

    Full Text Available Direct borohydride fuel cells (DBFC, which operate on sodium borohydride (NaBH4 as the fuel, and hydrogen peroxide (H2O2 as the oxidant, are receiving increasing attention. This is due to their promising use as power sources for space and underwater applications, where air is not available and gas storage poses obvious problems. One key factor to improve the performance of DBFCs concerns the type of separator used. Both anion- and cation-exchange membranes may be considered as potential separators for DBFC. In the present paper, the effect of the membrane type on the performance of laboratory NaBH4/H2O2 fuel cells using Pt electrodes is studied at room temperature. Two commercial ion-exchange membranes from Membranes International Inc., an anion-exchange membrane (AMI-7001S and a cation-exchange membrane (CMI-7000S, are tested as ionic separators for the DBFC. The membranes are compared directly by the observation and analysis of the corresponding DBFC’s performance. Cell polarization, power density, stability, and durability tests are used in the membranes’ evaluation. Energy densities and specific capacities are estimated. Most tests conducted, clearly indicate a superior performance of the cation-exchange membranes over the anion-exchange membrane. The two membranes are also compared with several other previously tested commercial membranes. For long term cell operation, these membranes seem to outperform the stability of the benchmark Nafion membranes but further studies are still required to improve their instantaneous power load.

  15. Differential inhibition of AE1 and AE2 anion exchangers by oxonol dyes and by novel polyaminosterol analogs of the shark antibiotic squalamine.

    Science.gov (United States)

    Alper, S L; Chernova, M N; Williams, J; Zasloff, M; Law, F Y; Knauf, P A

    1998-01-01

    Oxonol and polyaminosterol drugs were examined as inhibitors of recombinant mouse AE1 and AE2 anion exchangers expressed in Xenopus laevis oocytes and were compared as inhibitors of AE1-mediated anion flux in red cells and in HL-60 cells that express AE2. The oxonols WW-781, diBA(5)C4, and diBA(3)C4 inhibited HL-60 cell Cl-/Cl- exchange with IC50 values from 1 to 7 microM, 100-1000 times less potent than their IC50 values for red cell Cl-/anion exchange. In Xenopus oocytes, diBA(5)C4 inhibited AE1-mediated Cl- efflux several hundred times more potently than that mediated by AE2. Several novel squalamine-related polyaminosterols were also evaluated as anion exchange inhibitors. In contrast to diBA(5)C4, polyaminosterol 1361 inhibited oocyte-expressed AE2 8-fold more potently than AE1 (IC50 0.6 versus 5.2 microM). The 3-fold less potent desulfo-analog, 1360, showed similar preference for AE2. It was found that 1361 also partially inhibited Cl- efflux from red cells, whereas neither polyaminosterol inhibited Cl efflux from HL60 cells. Thus, the oxonol diBA(5)C4 is >100-fold more potent as an inhibitor of AE1 than of AE2, whereas the polyaminosterols 1360 and 1361 are 8-fold more potent as inhibitors of AE2 than of AE1. Assay conditions and cell type influenced IC50 values for both classes of compounds. PMID:10353714

  16. Characterization of Anion Exchange Membrane Containing Epoxy Ring and C–Cl Bond Quaternized by Various Amine Groups for Application in Fuel Cells

    OpenAIRE

    Sung Kuk Jeong; Ju Sung Lee; Sahng Hyuck Woo; Jin Ah Seo; Byoung Ryul Min

    2015-01-01

    Anion exchange membranes were synthesized from different compositions of glycidyl methacrylate (GMA) and vinylbenzyl chloride (VBC), with constant content of divinyl benzene (DVB) by radical polymerization using benzoyl peroxide (BPO) on non-woven polyethylene terephthalate (PET) substrate. Polymerized membranes were then quaternized by soaking in trimethylamine (TMA), triethylamine (TEA), tripropylamine (TPA), and 1,4-diazabicyclo [2.2.2] octane (DABCO). Characteristics of membranes were con...

  17. Characterization of Anion Exchange Membrane Containing Epoxy Ring and C–Cl Bond Quaternized by Various Amine Groups for Application in Fuel Cells

    OpenAIRE

    Sung Kuk Jeong; Ju Sung Lee; Sahng Hyuck Woo; Jin Ah Seo; Byoung Ryul Min

    2015-01-01

    Anion exchange membranes were synthesized from different compositions of glycidyl methacrylate (GMA) and vinylbenzyl chloride (VBC), with constant content of divinyl benzene (DVB) by radical polymerization using benzoyl peroxide (BPO) on non-woven polyethylene terephthalate (PET) substrate. Polymerized membranes were then quaternized by soaking in trimethylamine (TMA), triethylamine (TEA), tripropylamine (TPA), and 1,4-diazabicyclo [2.2.2] octane (DABCO). Characteristics of membranes were co...

  18. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides: an in situ X-ray powder diffraction study

    DEFF Research Database (Denmark)

    Johnsen, Rune; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO3 CoAl-Cl CoAl-CO3, CoAl-Cl CoAl-NO3 and CoAl-CO3 CoAl-SO4. The XRPD data show that the CoAl-CO3 CoAl-Cl process...

  19. Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

    OpenAIRE

    Ball James W; Nordstrom D Kirk; Schoonen Martin AA; Druschel Greg K; Xu Yong; Cohn Corey A

    2003-01-01

    A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad™ AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted w...

  20. Understanding the Adsorption of PFOA on MIL-101(Cr)-Based Anionic-Exchange Metal-Organic Frameworks: Comparing DFT Calculations with Aqueous Sorption Experiments.

    Science.gov (United States)

    Liu, Kai; Zhang, Siyu; Hu, Xiyue; Zhang, Kunyang; Roy, Ajay; Yu, Gang

    2015-07-21

    To examine the effects of different functionalization methods on adsorption behavior, anionic-exchange MIL-101(Cr) metal-organic frameworks (MOFs) were synthesized using preassembled modification (PAM) and postsynthetic modification (PSM) methods. Perfluorooctanoic acid (PFOA) adsorption results indicated that the maximum PFOA adsorption capacity was 1.19 and 1.89 mmol g(-1) for anionic-exchange MIL-101(Cr) prepared by PAM and PSM, respectively. The sorption equilibrium was rapidly reached within 60 min. Our results indicated that PSM is a better modification technique for introducing functional groups onto MOFs for adsorptive removal because PAM places functional groups onto the aperture of the nanopore, which hinders the entrance of organic contaminants. Our experimental results and the results of complementary density functional theory calculations revealed that in addition to the anion-exchange mechanism, the major PFOA adsorption mechanism is a combination of Lewis acid/base complexation between PFOA and Cr(III) and electrostatic interaction between PFOA and the protonated carboxyl groups of the bdc (terephthalic acid) linker.

  1. Chlorine isotope enrichment on a strong alkaline anion exchanger in dependence of type and concentration of the strange electrolytic solution

    International Nuclear Information System (INIS)

    Chlorine isotope enrichment for heterogenous ionexchange equilibria was studied. The dependence of element separation effects on the anion of the strange electrolyte (for same cation), on the cation of the strange electrolyte (for same anion), on the concentration of the strange electrolyte and also on the acetone: water ratio of the solvent was investigated. (orig./HBR)

  2. Compensatory role of inducible annexin A2 for impaired biliary epithelial anion-exchange activity of inflammatory cholangiopathy.

    Science.gov (United States)

    Kido, Osamu; Fukushima, Koji; Ueno, Yoshiyuki; Inoue, Jun; Jefferson, Douglas M; Shimosegawa, Tooru

    2009-12-01

    The peribiliary inflammation of cholangiopathy affects the physiological properties of biliary epithelial cells (cholangiocyte), including bicarbonate-rich ductular secretion. We revealed the upregulation of annexin A2 (ANXA2) in cholangiocytes in primary biliary cirrhosis (PBC) by a proteomics approach and evaluated its physiological significance. Global protein expression profiles of a normal human cholangiocyte line (H69) in response to interferon-gamma (IFNgamma) were obtained by two-dimensional electrophoresis followed by MALDI-TOF-MS. Histological expression patterns of the identified molecules in PBC liver were confirmed by immunostaining. H69 cells stably transfected with doxycyclin-inducible ANXA2 were subjected to physiological evaluation. Recovery of the intracellular pH after acute alkalinization was measured consecutively by a pH indicator with a specific inhibitor of anion exchanger (AE), 4,4'-diisothiocyanatostilbene-2,2'-disulfonic acid (DIDS). Protein kinase-C (PKC) activation was measured by PepTag Assay and immunoblotting. Twenty spots that included ANXA2 were identified as IFNgamma-responsive molecules. Cholangiocytes of PBC liver were decorated by the unique membranous overexpression of ANXA2. Apical ANXA2 of small ducts of PBC was directly correlated with the clinical cholestatic markers and transaminases. Controlled induction of ANXA2 resulted in significant increase of the DIDS-inhibitory fraction of AE activity of H69, which was accompanied by modulation of PKC activity. We, therefore, identified ANXA2 as an IFNgamma-inducible gene in cholangiocytes that could serve as a potential histological marker of inflammatory cholangiopathy, including PBC. We conclude that inducible ANXA2 expression in cholangiocytes may play a compensatory role for the impaired AE activity of cholangiocytes in PBC in terms of bicarbonate-rich ductular secretion and bile formation through modulation of the PKC activity. PMID:19823170

  3. Effect of dissolved organic matter on nitrate-nitrogen removal by anion exchange resin and kinetics studies

    Institute of Scientific and Technical Information of China (English)

    Haiou Song; Zhijian Yao; Mengqiao Wang; Jinnan Wang; Zhaolian Zhu; Aimin Li

    2013-01-01

    The effects of dissolved organic matter (DOM) on the removal of nitrate-nitrogen from the model contaminated water have been investigated utilizing the strong base anion exchange resins.With the increase of gallic acid concentration from 0 to 400 mg/L,the adsorption amount of nitrate-nitrogen on the commercial resins,including D201,Purolite A 300 (A300) and Purolite A 520E (A520E),would significantly decrease.However,the presence of tannin acid has little impact on nitrate-nitrogen adsorption on them.Compared to D201 and A300 resins,A520E resin exhibited more preferable adsorption ability toward nitrate-nitrogen in the presence of competing organic molecules,such as gallic acid and tannin acid at greater levels in aqueous solution.Attractively,the equilibrium data showed that the adsorption isotherm of nitrate-nitrogen on A520E resin was in good agreement with Langmuir and Freundlich equations.The rate parameters for the intra particle diffusion have been estimated for the different initial concentrations.In batch adsorption processes,nitrate-nitrogen diffuse in porous adsorbent and rate process usually depends on t1/2 rather than the contact time.The pseudo first-and the second-order kinetic models fit better for nitrate-nitrogen adsorption onto A520E resin.The observations reported herein illustrated that A520E resin will be an excellent adsorbent for enhanced removal of nitrate-nitrogen from contaminated groundwater.

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

    DEFF Research Database (Denmark)

    Al-Jibbouri, Sattar

    2007-01-01

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

  5. The use of ion exchange chromatography in the cyclotron production of the radioisotopes 85Sr, 54Mn, 57Co and 109Cd

    International Nuclear Information System (INIS)

    This dissertation shows the successful application of ion exchange chromatography to the isolation of carrier free cyclotron produced radioisotopes. A simple method is presented for the isolation of 85Sr from a 10 g rubidium chloride target. Cation exchange with AG50-X12 is used to retain 85Sr from a bombarded target dissolved in 0.1 mol/dm3 hydrochloric acid. Rubidium is effectively eluted with 0.5 mol/dm3 hydrochloric acid and trace impurities such as copper, iron and 65Zn are eluted with 0.5 mol/dm3 hydrochloric acid/φ=0.95 acetone (where φ is the volume fraction of acetone). Strontium-85 is eluted in nearly 100% yield with 3.0 mol/dm3 nitric acid. The isolation of 54Mn, 57Co and 109Cd from a composite iron-silver target is performed with AG50-X4 cation exchange resin in a hydrochloric acid-acetone medium subsequent to the removal of silver by reduction with hydrazine hydrate. Cadmium-109 is eluted with 0.1 mol/dm3 hydrochloric acid/φ=0.80 acetone and is further refined by absorption onto a AG1-X8 anion exchange column and subsequent washing with 0.25 mol/dm3 nitric acid/0.1 mol/dm3 hydrobromic acid. The elution of copper, iron, 65Zn and other impurities from the cation exhanger is performed with 0.5 mol/dm3 hydrochloric acid/φ=0.83 acetone. Cobalt-57 is quantitively eluted with 0.35 mol/dm3 hydrochloric acid/φ=0.90 acetone, and 54Mn, the remaining element on the column, is recovered with 3.0 mol/dm3 hydrochloric acid

  6. Pilot-scale ion-exchange centrifugal partition chromatography: purification of sinalbin from white mustard seeds.

    Science.gov (United States)

    Toribio, Alix; Nuzillard, Jean-Marc; Pinel, Benoît; Boudesocque, Leslie; Lafosse, Michel; De La Poype, François; Renault, Jean-Hugues

    2009-06-01

    The purification of p-hydroxybenzylglucosinolate (sinalbin) on a multigram scale from a crude aqueous extract of white mustard seeds (Sinapis alba var. concerta) was successfully achieved by scaling up a strong ion-exchange centrifugal partition chromatography (SIXCPC) laboratory procedure. Thus, the one-step sinalbin purification was performed with 2.35 g of crude extract in approximately 170 min (830 mg/h) up to 70.3 g in approximately 160 min (26.3 g/h) by switching from a 200 mL laboratory scale column to a 5.7 L pilot-scale column. The required biphasic solvent system contained ethyl acetate, n-butanol, and water in 3:2:5 v/v/v proportions, Aliquat 336 (trioctylmethyl ammonium chloride) was added to the organic stationary phase (80 mM) and acted as ion-exchanger. Potassium iodide in the aqueous mobile phase (80 mM) was used as sinalbin displacer. The 28.5 mass scale factor arose from the increase in mobile phase flow-rate (from 2 to 50 mL/min), from the higher mass of injected white mustard seed extract (from 12 to 350 g), and from the calculated productivity (from 830 mg to 26.3 g). These results demonstrate that industry scale production of glucosinolates is easily performed by SIXCPC, thus providing pure reference standards for pharmacology studies. PMID:19479767

  7. Resolution of Enantiomers of (RS)-Baclofen by Ligand-Exchange Thin-Layer Chromatography.

    Science.gov (United States)

    Singh, Manisha; Malik, Poonam; Bhushan, Ravi

    2016-05-01

    A new chromatographic method has been developed for direct enantioresolution of (RS)-baclofen by ligand-exchange thin-layer chromatography (TLC) adopting two different approaches; (A) TLC plates were prepared by mixing the ligand exchange reagents (LER) with silica gel slurry and the chromatograms were developed with different achiral solvents or solvents having no chiral additive, and (B) the LER consisting of Cu(II)-l-amino acid complex was used as chiral mobile phase additive and the plain plates of silica gel having no chiral selector were used. Cu(II) acetate and fourl-amino acids (namely,l-tryptophan,l-histidine,l-proline andl-phenylalanine) were used for the preparation of LERs. Spots were located by the use of iodine vapor. Effect of temperature and the mole ratio of Cu(II)-to-amino acid on enantioresolution were also studied. The results for the two methods have been compared, and the issue of involvement of the Cu(II) cation for the best performance of the two methods has been discussed with respect to the same mobile phase.l-Trp proved to be a good ligand using a common mobile phase in each case. PMID:26896346

  8. Tandem anion and cation exchange solid phase extraction for the enrichment of micropollutants and their transformation products from ozonation in a wastewater treatment plant.

    Science.gov (United States)

    Deeb, Ahmad A; Schmidt, Torsten C

    2016-06-01

    The presence of organic micropollutants and their transformation products (TPs) from biotic and abiotic processes in aquatic environments is receiving intense public and scientific attention. Yet a suitable sample preparation method that would enable extraction and enrichment of a wide range of such compounds from water is missing. The focus of this paper was to develop an enhanced solid phase extraction (SPE) protocol which enabled isolation of parent compounds and low molecular weight transformation products (that are produced after treatment of water with ozone) from different water matrices. Ten SPE sorbents were evaluated with regard to their ability to extract acidic, neutral, and basic compounds from water at several pH values. Highest recoveries (91-99 %) for all analytes in pure water were obtained by combining strong anion and cation exchangers of two manufacturers in a tandem mode without pH adjustment. Tandem Oasis (MAX+MCX) was finally applied to extract the spiked analytes from tap water, surface water, and several wastewater samples. The efficiency of the used SPE procedure was examined using an optimized liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method using multiple reaction monitoring (MRM) mode. The occurrence of some of the investigated TPs in environmental water matrices was proven for the first time in this study. Method quantification limits (MQLs) for all compounds ranged from 3.7 to 15.3 ng/L in all matrices. Recoveries (%RE) were between 90 and 110 %. Intraday and interday precision, expressed as relative standard deviation, varied from 0.7 to 5.9 % and 1.8 to 10.3 %, respectively. Matrix effect (%ME) evaluation demonstrated that even complex sample matrices did not show significant ion suppression or enhancement. The applicability of the method was shown during two sampling campaigns at Ruhr river and a wastewater treatment plant (WWTP) equipped with an ozonation step after regular

  9. Sodium citrate-assisted anion exchange strategy for construction of Bi{sub 2}O{sub 2}CO{sub 3}/BiOI photocatalysts

    Energy Technology Data Exchange (ETDEWEB)

    Song, Peng-Yuan; Xu, Ming; Zhang, Wei-De, E-mail: zhangwd@scut.edu.cn

    2015-02-15

    Highlights: • Heterostructured Bi{sub 2}O{sub 2}CO{sub 3}/BiOI microspheres were prepared via anion exchange. • Sodium citrate-assisted anion exchange for construction of composite photocatalysts. • Bi{sub 2}O{sub 2}CO{sub 3}/BiOI composites show high visible light photocatalytic activity. - Abstract: Bi{sub 2}O{sub 2}CO{sub 3}/BiOI heterojuncted photocatalysts were constructed through a facile partial anion exchange strategy starting from BiOI microspheres and urea with the assistance of sodium citrate. The content of Bi{sub 2}O{sub 2}CO{sub 3} in the catalysts was regulated by modulating the amount of urea as a precursor, which was decomposed to generate CO{sub 3}{sup 2−} in the hydrothermal process. Citrate anion plays a key role in controlling the morphology and composition of the products. The Bi{sub 2}O{sub 2}CO{sub 3}/BiOI catalysts display much higher photocatalytic activity than pure BiOI and Bi{sub 2}O{sub 2}CO{sub 3} towards the degradation of rhodamine B (RhB) and bisphenol A (BPA). The enhancement of photocatalytic activity of the heterojuncted catalysts is attributed to the formation of p–n junction between p-BiOI and n-Bi{sub 2}O{sub 2}CO{sub 3}, which is favorable for retarding the recombination of photoinduced electron-hole pairs. Moreover, the holes are demonstrated to be the main active species for the degradation of RhB and BPA.

  10. Trace analysis of anions in organic matrices by ion chromatography coupled with a novel reversed-phase column for on-line sample pretreatment

    Institute of Scientific and Technical Information of China (English)

    Ying Ying Zhong; Wen Fang Zhou; Xue Ling Zeng; Ming Li Ye; Yan Zhu

    2011-01-01

    An ion chromatography (IC) system coupled with on-line column-switching technique was used to determine anions of μg/g levels in organic chemicals of analytical reagent grade. A novel polystyrene-divinylbenzene-carbon nanotube (PS-DVB-CNT) stationary phase was utilized for matrix elimination. A calibration study was conducted by preparing and analyzing eight concentrations (between 10 and 5000 μg/L) of eight standards in deionized water. The linearity was between 0.9978 and 1. And the detection limits ranged from 1.54 μg/L to 10.02 μg/L. A spiking study was performed on two representative organic chemicals. The recoveries were between 84.3% and 119.6%.

  11. 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.

  12. Separation of Ofloxacin and Its Six Related Substances Enantiomers by Chiral Ligand-Exchange Chromatography.

    Science.gov (United States)

    Liang, Xinlei; Zhao, Longshan; Deng, Miaoduo; Liu, Lijie; Ma, Yongfu; Guo, Xingjie

    2015-11-01

    A chiral ligand-exchange high-performance liquid chromatography method was developed for the enantioseparation of ofloxacin and its six related substances termed impurities A, B, C, D, E, and F. The separation was performed on a conventional C18 column. Different organic modifiers, copper salts, amino acids, the ratio of Cu(2+) to amino acid, pH of aqueous phase, and column temperature were optimized. The optimal mobile phase conditions were methanol-water systems consisting of 5 mmol/L copper sulfate and 10 mmol/L L-isoleucine (L-Ile). Under such conditions, good enantioseparation of ofloxacin and impurities A, C, E, and F could be observed with resolutions (RS ) of 3.54, 1.97, 3.21, 3.50, and 2.12, respectively. On the relationship between the thermodynamic parameters and structures of analytes, the mechanism of chiral recognition was investigated. It was concluded that ofloxacin and impurities A, C, E, and F were all enthalpically driven enantioseparation and that low column temperature was beneficial to enantioseparation. Furthermore, the structure-separation relationship of these analytes is also discussed.

  13. Oxidation-labile subfraction of human plasma low density lipoprotein isolated by ion-exchange chromatography.

    Science.gov (United States)

    Shimano, H; Yamada, N; Ishibashi, S; Mokuno, H; Mori, N; Gotoda, T; Harada, K; Akanuma, Y; Murase, T; Yazaki, Y

    1991-05-01

    We isolated subfractions of human plasma low density lipoprotein (LDL) using ion-exchange chromatography. Plasma LDL from normolipidemic subjects were applied to a DEAE Sepharose 6B column. After elution of the bulk of LDL at 150 mM NaCl (the major fraction), the residual LDL was eluted at 500 mM NaCl and designated as the minor fraction. The minor fraction, only less than 1% of total LDL, tended to be somewhat similar in certain properties to oxidized LDL, e.g., an increased negative charge, higher protein/cholesterol ratio, and a higher flotation density than native LDL. These results were consistent with data reported by Avogaro et al. (1988. Arteriosclerosis. 8: 79-87). However, assays of 125I-labeled LDL binding activity for LDL receptors equal to that of the major fraction. Incorporation of [14C]oleate into cholesteryl ester [acyl-CoA:cholesterol acyltransferase (ACAT) activity] in mouse peritoneal macrophages incubated with the minor fraction was only slightly greater than that with the major fraction. Incubation of the minor fraction with 0.5 microM Cu2+ caused a remarkable stimulation of ACAT activity, while stimulation by the major fraction required incubation with 5 microM Cu2+, suggesting that the minor fraction was relatively labile to oxidation. The minor but definite presence of a plasma LDL subfraction more negative and susceptible to oxidation implicates the possibility of its association with atherogenesis. PMID:2072039

  14. Transcellular oxalate and Cl- absorption in mouse intestine is mediated by the DRA anion exchanger Slc26a3, and DRA deletion decreases urinary oxalate.

    Science.gov (United States)

    Freel, Robert W; Whittamore, Jonathan M; Hatch, Marguerite

    2013-10-01

    Active transcellular oxalate transport in the mammalian intestine contributes to the homeostasis of this important lithogenic anion. Several members of the Slc26a gene family of anion exchangers have a measurable oxalate affinity and are expressed along the gut, apically and basolaterally. Mouse Slc26a6 (PAT1) targets to the apical membrane of enterocytes in the small intestine, and its deletion results in net oxalate absorption and hyperoxaluria. Apical exchangers of the Slc26a family that mediate oxalate absorption have not been established, yet the Slc26a3 [downregulated in adenoma (DRA)] protein is a candidate mediator of oxalate uptake. We evaluated the role of DRA in intestinal oxalate and Cl(-) transport by comparing unidirectional and net ion fluxes across short-circuited segments of small (ileum) and large (cecum and distal colon) intestine from wild-type (WT) and DRA knockout (KO) mice. In WT mice, all segments demonstrated net oxalate and Cl(-) absorption to varying degrees. In KO mice, however, all segments exhibited net anion secretion, which was consistently, and solely, due to a significant reduction in the absorptive unidirectional fluxes. In KO mice, daily urinary oxalate excretion was reduced 66% compared with that in WT mice, while urinary creatinine excretion was unchanged. We conclude that DRA mediates a predominance of the apical uptake of oxalate and Cl(-) absorbed in the small and large intestine of mice under short-circuit conditions. The large reductions in urinary oxalate excretion underscore the importance of transcellular intestinal oxalate absorption, in general, and, more specifically, the importance of the DRA exchanger in oxalate homeostasis.

  15. Cell wall bound anionic peroxidases from asparagus byproducts.

    Science.gov (United States)

    Jaramillo-Carmona, Sara; López, Sergio; Vazquez-Castilla, Sara; Jimenez-Araujo, Ana; Rodriguez-Arcos, Rocio; Guillen-Bejarano, Rafael

    2014-10-01

    Asparagus byproducts are a good source of cationic soluble peroxidases (CAP) useful for the bioremediation of phenol-contaminated wastewaters. In this study, cell wall bound peroxidases (POD) from the same byproducts have been purified and characterized. The covalent forms of POD represent >90% of the total cell wall bound POD. Isoelectric focusing showed that whereas the covalent fraction is constituted primarily by anionic isoenzymes, the ionic fraction is a mixture of anionic, neutral, and cationic isoenzymes. Covalently bound peroxidases were purified by means of ion exchange chromatography and affinity chromatography. In vitro detoxification studies showed that although CAP are more effective for the removal of 4-CP and 2,4-DCP, anionic asparagus peroxidase (AAP) is a better option for the removal of hydroxytyrosol (HT), the main phenol present in olive mill wastewaters.

  16. Heterodimers formed through a partial anionic exchange process: scanning tunneling spectroscopy to monitor bands across the junction vis-à-vis photoinduced charge separation

    Science.gov (United States)

    Bera, Abhijit; Saha, Sudip K.; Pal, Amlan J.

    2015-10-01

    We report controlled formation of heterodimers and their charge separation properties. CdS|CdTe heterodimers were formed through an anionic exchange process of CdS nanostructures. With control over the duration of the anionic exchange process, bulk|dot, bulk|bulk, and then dot|bulk phases of the semiconductors could be observed to have formed. A mapping of density of states as derived from scanning tunneling spectroscopy (STS) brought out conduction and valence band-edges along the nanostructures and heterodimers. The CdS|CdTe heterodimers evidenced a type-II band-alignment between the semiconductors along with the formation of a depletion region at the interface. The width (of the depletion region) and the energy-offset at the interface depended on the size of the semiconductors. We report that the width that is instrumental for photoinduced charge separation in the heterodimers has a direct correlation with the performance of hybrid bulk-heterojunction solar cells based on the nanostructures in a polymer matrix.We report controlled formation of heterodimers and their charge separation properties. CdS|CdTe heterodimers were formed through an anionic exchange process of CdS nanostructures. With control over the duration of the anionic exchange process, bulk|dot, bulk|bulk, and then dot|bulk phases of the semiconductors could be observed to have formed. A mapping of density of states as derived from scanning tunneling spectroscopy (STS) brought out conduction and valence band-edges along the nanostructures and heterodimers. The CdS|CdTe heterodimers evidenced a type-II band-alignment between the semiconductors along with the formation of a depletion region at the interface. The width (of the depletion region) and the energy-offset at the interface depended on the size of the semiconductors. We report that the width that is instrumental for photoinduced charge separation in the heterodimers has a direct correlation with the performance of hybrid bulk

  17. Retention model of protein for mixed-mode interaction mechanism in ion exchange and hydrophobic interaction chromatography

    Institute of Scientific and Technical Information of China (English)

    WEI, Yin-Mao; LUO, Quan-Zhou; LIU,Tong; GENG, Xin-Du

    2000-01-01

    A unified retention equation of proteins was proved to be valid for a mixed-mode interaction mechanism in ion exchange chromatography (IEC) and hydrophobic interaction chromatography (HIC). The reason to form a “U” shape retention curve of proteins in both HIC and IEC was explained and the concentration range of the strongest elution ability for the mobile phase was determined with this equation. The parameters in this equation could be used to characterize the difference for either HIC or IEC adsorbents and the changes in the molecular conformation of proteins. With the parameters in this equation, the contributions of salt and water in the mobile phase to the protein retention in HIC and IEC were discussed,respectively. In addition, the comparison between the unified equation and Melander's three-parameter equation for mixedmode interaction chromatography was also investigated and better results were obtained in former equation.

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

    OpenAIRE

    Storm, Ida Drejer; Have Rasmussen, Peter; Strobel, Bjarne W.; Hansen, Hans Christian Bruun

    2008-01-01

    Abstract Ergot alkaloids (EAs) are mycotoxins which are unavoidable contaminants of cereal products, particularly rye. A method was compiled employing clean-up by cation-exchange solid phase extraction, separation by high-pressure liquid chromatography under alkaline conditions and fluorescence detection. It is capable of separating and quantifying both C8-isomers of ergocornine, a-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61?10 % with limits ...

  19. Mechanistic modeling of ion-exchange process chromatography of charge variants of monoclonal antibody products.

    Science.gov (United States)

    Kumar, Vijesh; Leweke, Samuel; von Lieres, Eric; Rathore, Anurag S

    2015-12-24

    Ion-exchange chromatography (IEX) is universally accepted as the optimal method for achieving process scale separation of charge variants of a monoclonal antibody (mAb) therapeutic. These variants are closely related to the product and a baseline separation is rarely achieved. The general practice is to fractionate the eluate from the IEX column, analyze the fractions and then pool the desired fractions to obtain the targeted composition of variants. This is, however, a very cumbersome and time consuming exercise. A mechanistic model that is capable of simulating the peak profile will be a much more elegant and effective way to make a decision on the pooling strategy. This paper proposes a mechanistic model, based on the general rate model, to predict elution peak profile for separation of the main product from its variants. The proposed approach uses inverse fit of process scale chromatogram for estimation of model parameters using the initial values that are obtained from theoretical correlations. The packed bed column has been modeled along with the chromatographic system consisting of the mixer, tubing and detectors as a series of dispersed plug flow and continuous stirred tank reactors. The model uses loading ranges starting at 25% to a maximum of 70% of the loading capacity and hence is applicable to process scale separations. Langmuir model has been extended to include the effects of salt concentration and temperature on the model parameters. The extended Langmuir model that has been proposed uses one less parameter than the SMA model and this results in a significant ease of estimating the model parameters from inverse fitting. The proposed model has been validated with experimental data and has been shown to successfully predict peak profile for a range of load capacities (15-28mg/mL), gradient lengths (10-30CV), bed heights (6-20cm), and for three different resins with good accuracy (as measured by estimation of residuals). The model has been also

  20. Flow-injection Chemiluminescence Sensor for the Determination of Gallic Acid by Immobilizing Luminol and Periodate on Anion-exchange Resin

    Institute of Scientific and Technical Information of China (English)

    ZHANG,Si-Chun(张四纯); ZHOU,Guo-Jun(周国俊); JU,Huang-Xian(鞠熀先)

    2002-01-01

    A novel chemihuminescence (CL) sensor for the determination of gallic acid combined with flow injection analysis was developed by electrostatically immobilizing luminol and periodate on anion-exchange resins respectively. Gallic acid was sensed by its enhancing effect on the weak CL reaction between luminol and periodate, which were eluted from the ion exchang ecolumn.The possible reaction mechanism of the CL system was suggested and discussed. The response of the sensor to gallic acid concentration was linear over the range of 8.0 × 10-9-1.0 × 10-6 mol/L with a detection limit of 6.5 × 10-9 mol/L (3σσ). The relative standard deviation (RSD) for 7 repetitive determinations of gallic acid (1.0 × 10-7 moL/L) was 1.8%. The sensor could be used for over 400 times determination with a good reproducibility.

  1. Separation of proteins by cation-exchange sequential injection chromatography using a polymeric monolithic column.

    Science.gov (United States)

    Masini, Jorge Cesar

    2016-02-01

    Since sequential injection chromatography (SIC) emerged in 2003, it has been used for separation of small molecules in diverse samples, but separations of high molar mass compounds such as proteins have not yet been described. In the present work a poly(glycidyl methacrylate-co-ethylene dimethacrylate) (GMA-co-EDMA) monolithic column was prepared by free radical polymerization inside a 2.1-mm-i.d. activated fused silica-lined stainless steel tubing and modified with iminodiacetic acid (IDA). The column was prepared from a mixture of 24% GMA, 16% EDMA, 20% cyclohexanol, and 40% 1-dodecanol (all% as w/w) containing 1% of azobisisobutyronitrile (AIBN) (in relation to monomers). Polymerization was done at 60 °C for 24 h. The polymer was modified with 1.0 M IDA (in 2 M Na2CO3, pH 10.5) at 80 °C for 16 h. Separation of myoglobin, ribonuclease A, cytochrome C, and lysozyme was achieved at pH 7.0 (20 mM KH2PO4/K2HPO4) using a salt gradient (NaCl). Myoglobin was not retained, and the other proteins were separated by a gradient of NaCl created inside the holding coil (4 m of 0.8-mm-i.d. PTFE tubing) by sequential aspiration of 750 and 700 μL of 0.2 and 0.1 M NaCl, respectively. As the flow was reversed toward the column (5 μL s(-1)) the interdispersion of these solutions created a reproducible gradient which separated the proteins in 10 min, with the following order of retention: ribonuclease A < cytochrome C < lysozyme. The elution order was consistent with a cation-exchange mechanism as the retention increased with the isoelectric points.

  2. Rapid chiral separation and impurity determination of levofloxacin by ligand-exchange chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Hongyuan [Center for Advanced Bioseparation Technology, Department of Chemical Engineering, Inha University, Incheon 402-751 (Korea, Republic of); Row, Kyung Ho [Center for Advanced Bioseparation Technology, Department of Chemical Engineering, Inha University, Incheon 402-751 (Korea, Republic of)]. E-mail: rowkho@inha.ac.kr

    2007-02-12

    A sensitive, simple, and accurate method for determination of levofloxacin and its (R)-enantiomer was developed to determine the chiral impurity of levofloxacin in Cravit Tablets material by ligand-exchange high performance liquid chromatography. The effects of different kinds of ligands, concentration of ligands in mobile phase, organic modifier, pH of mobile phase, and temperature on enantioseparation were investigated and evaluated. Chiral separation was performed on a conventional C{sub 18} column, where the mobile phase consisted of a methanol-water solution (containing10 mmol L{sup -1} L-leucine and 5 mmol L{sup -1} copper sulfate) (88:12, v/v) and its flow-rate was set at 1.0 mL min{sup -1}. The conventional C{sub 18} column offers baseline separation of two enantiomers with a resolution of 2.4 in less than 20 min. Thermodynamic data ({delta}{delta}H and {delta}{delta}S) obtained by Van't Hoff plots revealed the chiral separation is an enthalpy-controlled process. The standard curves showed excellent linearity over the concentration range from 0.5 to 400 mg L{sup -1} for levofloxacin and its (R)-enantiomer. The linear correlation equations are: y = 1.33 x 10{sup 5} x + 6297 (r = 0.9991) and y = 1.34 x 10{sup 5} x + 3565 (r = 0.9997), respectively. The relative standard deviation (RSD) of the method was below 2.3% (n = 3)

  3. Molecular rheology of branched polymers: Decoding and exploring the role of architectural dispersity through a synergy of anionic synthesis, interaction chromatography, rheometry and modeling

    KAUST Repository

    Van Ruymbeke, Evelyne

    2014-01-01

    An emerging challenge in polymer physics is the quantitative understanding of the influence of a macromolecular architecture (i.e., branching) on the rheological response of entangled complex polymers. Recent investigations of the rheology of well-defined architecturally complex polymers have determined the composition in the molecular structure and identified the role of side-products in the measured samples. The combination of different characterization techniques, experimental and/or theoretical, represents the current state-of-the-art. Here we review this interdisciplinary approach to molecular rheology of complex polymers, and show the importance of confronting these different tools for ensuring an accurate characterization of a given polymeric sample. We use statistical tools in order to relate the information available from the synthesis protocols of a sample and its experimental molar mass distribution (typically obtained from size exclusion chromatography), and hence obtain precise information about its structural composition, i.e. enhance the existing sensitivity limit. We critically discuss the use of linear rheology as a reliable quantitative characterization tool, along with the recently developed temperature gradient interaction chromatography. The latter, which has emerged as an indispensable characterization tool for branched architectures, offers unprecedented sensitivity in detecting the presence of different molecular structures in a sample. Combining these techniques is imperative in order to quantify the molecular composition of a polymer and its consequences on the macroscopic properties. We validate this approach by means of a new model asymmetric comb polymer which was synthesized anionically. It was thoroughly characterized and its rheology was carefully analyzed. The main result is that the rheological signal reveals fine molecular details, which must be taken into account to fully elucidate the viscoelastic response of entangled branched

  4. Ion distribution in quaternary-ammonium-functionalized aromatic polymers: effects on the ionic clustering and conductivity of anion-exchange membranes.

    Science.gov (United States)

    Weiber, E Annika; Jannasch, Patric

    2014-09-01

    A series of copoly(arylene ether sulfone)s that have precisely two, three, or four quaternary ammonium (QA) groups clustered directly on single phenylene rings along the backbone are studied as anion-exchange membranes. The copolymers are synthesized by condensation polymerizations that involve either di-, tri-, or tetramethylhydroquinone followed by virtually complete benzylic bromination using N-bromosuccinimide and quaternization with trimethylamine. This synthetic strategy allows excellent control and systematic variation of the local density and distribution of QA groups along the backbone. Small-angle X-ray scattering of these copolymers shows extensive ionic clustering, promoted by an increasing density of QA on the single phenylene rings. At an ion-exchange capacity (IEC) of 2.1 meq g(-1), the water uptake decreases with the increasing local density of QA groups. Moreover, at moderate IECs at 20 °C, the Br(-) conductivity of the densely functionalized copolymers is higher than a corresponding randomly functionalized polymer, despite the significantly higher water uptake of the latter. Thus, the location of multiple cations on single aromatic rings in the polymers facilitates the formation of a distinct percolating hydrophilic phase domain with a high ionic concentration to promote efficient anion transport, despite probable limitations by reduced ion dissociation. These findings imply a viable strategy to improve the performance of alkaline membrane fuel cells. PMID:25044778

  5. Accelerated Analyte Uptake on Single Beads in Microliter-scale Batch Separations using Acoustic Streaming: Plutonium Uptake by Anion Exchange for Analysis by Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Paxton, Walter F.; O' Hara, Matthew J.; Peper, Shane M.; Petersen, Steven L.; Grate, Jay W.

    2008-06-01

    The use of acoustic streaming as a non-contact mixing platform to accelerate mass transport-limited diffusion processes in small volume heterogeneous reactions has been investigated. Single bead anion exchange of plutonium at nanomolar and sub-picomolar concentrations in 20 microliter liquid volumes was used to demonstrate the effect of acoustic mixing. Pu uptake rates on individual ~760 micrometer diameter AG 1x4 anion exchange resin beads were determined using acoustic mixing and compared with Pu uptake rates achieved by static diffusion alone. An 82 MHz surface acoustic wave (SAW) device was placed in contact with the underside of a 384-well microplate containing flat-bottomed semiconical wells. Acoustic energy was coupled into the solution in the well, inducing acoustic streaming. Pu uptake rates were determined by the plutonium remaining in solution after specific elapsed time intervals, using liquid scintillation counting (LSC) for nanomolar concentrations and thermal ionization mass spectrometry (TIMS) analysis for the sub-picomolar concentration experiments. It was found that this small batch uptake reaction could be accelerated by a factor of about five-fold or more, depending on the acoustic power applied.

  6. Adsorption properties of Ag(I), Au(III), Pd(II) and Pt(IV) ions on commercial 717 anion-exchange resin

    Institute of Scientific and Technical Information of China (English)

    LIU Peng; LIU Guang-feng; CHEN Da-lin; CHENG Shao-yi; TANG Ning

    2009-01-01

    The adsorption properties of the four precious metal ions (Ag(Ⅰ),Au(Ⅲ),Pd(Ⅱ) and Pt(Ⅳ)) on the commercial Cl--form 717 strongly basic anion-exchange resin were studied in detail.The effects of the contact time,solution acidity,and concentrations of Cl~- and Pb~(2+) ions on the adsorption properties were studied by the batch method.Then,the column method was conducted under the optimized adsorption conditions (pH=3.0).The effects of the sample loading flow rate and the length-to-diameter ratios of the columns were investigated.The precious metal ions adsorbed could not be eluted completely after the saturated adsorption because the precious metal ions were found to be reduced to their metallic states during the adsorption process.So,it is recommended that the commercial Cl~--form 717 strongly basic anion-exchange resin should be decomposed directly to recovery the precious metals after the saturated adsorption.

  7. Determination of uranium isotopes in urine samples from radiation workers using 232U tracer, anion-exchange resin and alpha-spectrometry

    International Nuclear Information System (INIS)

    Bioassay technique is used for the estimation of actinides present in the body based on the excretion rate of body fluids. For occupational radiation workers urine assay is the preferred method for monitoring of chronic internal exposure. Determination of low concentrations of actinides such as plutonium, americium and uranium at low level of mBq in urine by alpha-spectrometry requires pre-concentration of large volumes of urine. This paper deals with standardization of analytical method for the determination of U-isotopes in urine samples using anion-exchange resin and 232U tracer for radiochemical recovery. The method involves oxidation of urine followed by co-precipitation of uranium along with calcium phosphate. Separation of U was carried out by Amberlite, IRA-400, anion-exchange resin. U-fraction was electrodeposited and activity estimated using tracer recovery by alpha-spectrometer. Eight routine urine samples of radiation workers were analyzed and consistent radiochemical tracer recovery was obtained in the range of 51% to 67% with a mean and standard deviation of 60% and 5.4%, respectively. (author)

  8. Tuned synthesis of two coordination polymers of Cd(II) using substituted bent 3-pyridyl linker and succinate: structures and their applications in anion exchange and sorption properties.

    Science.gov (United States)

    Maity, Dilip Kumar; Bhattacharya, Biswajit; Halder, Arijit; Ghoshal, Debajyoti

    2015-12-28

    Two new Cd(II) coordination polymers, namely [Cd(3-bpdh)2(ClO4)2]n (1) and {[Cd(3-bpdh)(suc)(H2O)]·3(H2O)}n (2), have been synthesized using a substituted bent N,N'-donor ligand 2,5-bis-(3-pyridyl)-3,4-diaza-2,4-hexadiene (3-bpdh) and aliphatic dicarboxylate disodium succinate (suc) with Cd(II) perchlorate salts at room temperature by a slow diffusion technique for the exploration of our previous reported work. Both the structures were determined by single-crystal X-ray diffraction analysis and also by other physicochemical methods. Structure analysis revealed that complex 1 is a 1D chain structure containing coordinated perchlorate with a metal centre, and complex 2 shows a porous 3D framework with encapsulation of lattice water molecules into the void along the crystallographic a-axis. The PXRD study shows the bulk purity of both the complexes and TGA analysis of 2 exhibits that the structure is thermally stable up to 250 °C. Complex 1 shows a nice anion exchange property with replacement of weakly coordinated perchlorate with the inclusion of new anions; and the anion exchanged solids were characterised by FT-IR, PXRD and photoluminescence properties. The desolvated framework of 2 exhibits sorption of CO2 and water vapor and surface adsorption of N2 corroborating with the nature of the pore environment present in 2. The photoluminescence study has been also done for both complexes in the solid state which exhibits ligand based emissions at room temperature. PMID:26586233

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

    International Nuclear Information System (INIS)

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

  10. tRNA separation by high-performance liquid chromatography using an aggregate of ODS-Hypersil and trioctylmethylammonium chloride

    NARCIS (Netherlands)

    Bischoff, Rainer; Graeser, E.; Mclaughlin, L.W.

    1983-01-01

    High-performance liquid chromatography on a reversed-phase support treated with a tetraalkylammonium salt was used to separate tRNAs from baker's yeast. While resolution by this column appears to result from both anion-exchange and reversed-phase chromatography, it is the hydrophobic interactions wh

  11. Ae4 (Slc4a9) Anion Exchanger Drives Cl- Uptake-dependent Fluid Secretion by Mouse Submandibular Gland Acinar Cells.

    Science.gov (United States)

    Peña-Münzenmayer, Gaspar; Catalán, Marcelo A; Kondo, Yusuke; Jaramillo, Yasna; Liu, Frances; Shull, Gary E; Melvin, James E

    2015-04-24

    Transcellular Cl(-) movement across acinar cells is the rate-limiting step for salivary gland fluid secretion. Basolateral Nkcc1 Na(+)-K(+)-2Cl(-) cotransporters play a critical role in fluid secretion by promoting the intracellular accumulation of Cl(-) above its equilibrium potential. However, salivation is only partially abolished in the absence of Nkcc1 cotransporter activity, suggesting that another Cl(-) uptake pathway concentrates Cl(-) ions in acinar cells. To identify alternative molecular mechanisms, we studied mice lacking Ae2 and Ae4 Cl(-)/HCO3 (-) exchangers. We found that salivation stimulated by muscarinic and β-adrenergic receptor agonists was normal in the submandibular glands of Ae2(-/-) mice. In contrast, saliva secretion was reduced by 35% in Ae4(-/-) mice. The decrease in salivation was not related to loss of Na(+)-K(+)-2Cl(-) cotransporter or Na(+)/H(+) exchanger activity in Ae4(-/-) mice but correlated with reduced Cl(-) uptake during β-adrenergic receptor activation of cAMP signaling. Direct measurements of Cl(-)/HCO3 (-) exchanger activity revealed that HCO3 (-)-dependent Cl(-) uptake was reduced in the acinar cells of Ae2(-/-) and Ae4(-/-) mice. Moreover, Cl(-)/HCO3 (-) exchanger activity was nearly abolished in double Ae4/Ae2 knock-out mice, suggesting that most of the Cl(-)/HCO3 (-) exchanger activity in submandibular acinar cells depends on Ae2 and Ae4 expression. In conclusion, both Ae2 and Ae4 anion exchangers are functionally expressed in submandibular acinar cells; however, only Ae4 expression appears to be important for cAMP-dependent regulation of fluid secretion.

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

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    Human Milk Oligosaccharides (HMOs) are composed of 5 different monosaccharides: D-glucose, D-galactose, L-fucose, N-acetylneuraminic acid and N-acetylglucosamine. Approximately 200 unique structures have been identified, ranging in the degree of polymerization from 3 to 22. The diversity among...

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

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    Human Milk Oligosaccharides (HMOs) are composed of 5 different monosaccharides: D-glucose, D galactose, L-fucose, N-acetylneuraminic acid and N-acetylglucosamine. Approximately 200 unique structures have been identified, ranging in degree of polymerization from 3 to 22. The diversity among...

  14. Synthesis and anion exchange reactions of a layered copper-zinc hydroxy double salt, Cu1×6Zn0×4(OH)3(OAc)×H2O

    Indian Academy of Sciences (India)

    Jacqueline Therese Rajamathi; Sylvia Britto; Michael Rajamathi

    2005-11-01

    A mixed-metal hydroxysalt of formula Cu1.6Zn0.4(OH)3(OAc)$\\cdot$H2O has been synthesized by an acetate hydrolysis route. Acetate ions can be exchanged with simple inorganic anions such as chloride and nitrate, and organic anions such as benzoate and large surfactant anions such as dodecyl sulphate. Structures of these hydroxysalts are derived from that of Cu2(OH)3NO3$\\cdot$H2O with some of the Cu2+ ions being replaced by Zn2+.

  15. Study on the identification of organic and common anions in the pyrohydrolysis distillate of mixed uranium-plutonium carbide for the interference free determination of chlorine and fluorine by ion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Jeyakumar, Subbiah; Mishra, Vivekchandra Guruprasad; Das, Mrinal Kanti; Raut, Vaibhavi Vishwajeet; Sawant, Ramesh Mahadeo [Bhabha Atomic Research Centre, Mumbai (India). Radioanalytical Chemistry Div.; Ramakumar, Karanam Lakshminarayana [Bhabha Atomic Research Centre, Mumbai (India). Radiochemistry and Isotope Group

    2014-07-01

    Identification of various soluble organic acids formed during the pyrohydrolysis of uranium-plutonium mixed carbide [(U,Pu)C] was carried out using ion chromatography. This has significant importance as the soluble organic acids can cause severe interferences during the ion chromatography separation and determination of Cl{sup -} and F{sup -} in the pyrohydrolysis distillate of (U,Pu)C. Determination of Cl and F is important in the chemical quality control of nuclear materials as these two elements can cause corrosion and hence, their concentrations in all nuclear materials are restricted to certain specified values. Since the pyrohydrolysis distillates contain both inorganic and organic acid anions, for the sake of separating and identifying organic acid anions from the common inorganic anions, three independent isocratic elutions using varying concentrations of NaOH eluent were employed for the separation of weakly, moderately and strongly retained anions. It was observed that pyrohydrolysis of (U,Pu)C also produced soluble organic acids as in the case of nitric acid dissolution of UC. The present investigation revealed the presence of formic, acetic, propionic, butyric, oxalic acid anions in the pyrohydrolysis distillate of (U,Pu)C in trace or ultra-trace concentrations. The presence of each organic acid identified in the chromatogram was confirmed with spike addition as well as by separating them by capillary electrophoresis method. The presence of lower aliphatic acids viz. formic and acetic acids was reconfirmed by carrying out an independent separation with tetraborate eluent. It is suggested that nitric acid being formed during pyrohydrolysis could be responsible for the formation of organic acids. Based on the findings, an ion chromatography separation method has been proposed for the interference-free determination of chloride and fluoride in pyrohydrolysis distillate of (U,Pu)C. (orig.)

  16. 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...... 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...

  17. LAB-SCALE DEMONSTRATION OF PLUTONIUM PURIFICATION BY ANION EXCHANGE, PLUTONIUM (IV) OXALATE PRECIPITATION, AND CALCINATION TO PLUTONIUM OXIDE TO SUPPORT THE MOX FEED MISSION

    Energy Technology Data Exchange (ETDEWEB)

    Crowder, M.; Pierce, R.

    2012-08-22

    H-Canyon and HB-Line are tasked with the production of PuO{sub 2} from a feed of plutonium metal. The PuO{sub 2} will provide feed material for the MOX Fuel Fabrication Facility. After dissolution of the Pu metal in H-Canyon, the solution will be transferred to HB-Line for purification by anion exchange. Subsequent unit operations include Pu(IV) oxalate precipitation, filtration and calcination to form PuO{sub 2}. This report details the results from SRNL anion exchange, precipitation, filtration, calcination, and characterization tests, as requested by HB-Line1 and described in the task plan. This study involved an 80-g batch of Pu and employed test conditions prototypical of HB-Line conditions, wherever feasible. In addition, this study integrated lessons learned from earlier anion exchange and precipitation and calcination studies. H-Area Engineering selected direct strike Pu(IV) oxalate precipitation to produce a more dense PuO{sub 2} product than expected from Pu(III) oxalate precipitation. One benefit of the Pu(IV) approach is that it eliminates the need for reduction by ascorbic acid. The proposed HB-Line precipitation process involves a digestion time of 5 minutes after the time (44 min) required for oxalic acid addition. These were the conditions during HB-line production of neptunium oxide (NpO{sub 2}). In addition, a series of small Pu(IV) oxalate precipitation tests with different digestion times were conducted to better understand the effect of digestion time on particle size, filtration efficiency and other factors. To test the recommended process conditions, researchers performed two nearly-identical larger-scale precipitation and calcination tests. The calcined batches of PuO{sub 2} were characterized for density, specific surface area (SSA), particle size, moisture content, and impurities. Because the 3013 Standard requires that the calcination (or stabilization) process eliminate organics, characterization of PuO{sub 2} batches monitored the

  18. Anion exchange membrane prepared from simultaneous polymerization and quaternization of 4-vinyl pyridine for non-aqueous vanadium redox flow battery applications

    Science.gov (United States)

    Maurya, Sandip; Shin, Sung-Hee; Sung, Ki-Won; Moon, Seung-Hyeon

    2014-06-01

    A simple, single step and environmentally friendly process is developed for the synthesis of anion exchange membrane (AEM) by simultaneous polymerization and quaternization, unlike the conventional membrane synthesis which consists of separate polymerization and quaternization step. The membrane synthesis is carried out by dissolving polyvinyl chloride (PVC) in cyclohexanone along with 4-vinyl pyridine (4VP) and 1,4-dibromobutane (DBB) in the presence of thermal initiator benzoyl peroxide, followed by film casting to get thin and flexible AEMs. The membrane properties such as ion exchange capacity, ionic conductivity and swelling behaviour are tuned by varying the degree of crosslinking. These AEMs exhibit low vanadium permeability, while retaining good dimensional and chemical stability in an electrolyte solution, making them appropriate candidates for non-aqueous vanadium acetylacetonate redox flow battery (VRFB) applications. The optimized membrane displays ion exchange capacity and ionic conductivity of 2.0 mequiv g-1 and 0.105 mS cm-1, respectively, whereas the efficiency of 91.7%, 95.7% and 87.7% for coulombic, voltage and energy parameter in non-aqueous VRFB, respectively. This study reveals that the non-aqueous VRFB performance is greatly influenced by membrane properties; therefore the optimal control over the membrane properties is advantageous for the improved performance.

  19. Kinetics of fast ligand exchange in excited lanthanide complexes with anions of salicylic and 5-sulfosalisylic acids

    International Nuclear Information System (INIS)

    The luminescent-kinetic spectroscopic method with a flash selective photoexcitation has been used for studying the reaction of ligand substitution with solvent molecules in complexes of electron-excited ions Tb3+(5D4) and Dysup(3+)(sup(4)Fsub(9/2) with anions of salicylic and 5-sulphosalicylic acids in water and methanol. The acidic-catalytic mechanism of this reaction in water has been established, the limiting stage of complex dissociation being the stage of proton addition to the -COO- group of the ligand proceeding at a rate of 1x1010 mol-1s-1 and 0.77x1010 mol-1xs-1 for complexes of Tb3+(5D4) in H2O and D2O. It has been shown that in an aqueous medium anions of salicylic and 5-sulphosalicylic acids behave with respect to r.e.e. ions as bidentate ligands coordinating these ions with the oxygen of the -COO- group and oxygroup whereas in methanol an additional coordination with oxygen of the oxygroup is absent

  20. [Effects and mechanism on removing organics and reduction of membrane fouling using granular macro-porous anion exchange resin in drinking water treatment].

    Science.gov (United States)

    He, Huan; Dong, Bing-Zhi; Xu, Guang-Hong; Yan, Zhao-Hui

    2014-05-01

    A granular macro-porous anion exchange resin combined with coagulation was used as pretreatment of microfiltration membrane, and their effects and mechanism on removing organics and reduction of membrane fouling were evaluated. The results showed that resin could be effective in removing organics with medium and small molecular weight ( Mr) but ineffective in removing organics with large Mr, while couagulation could significantly remove organics with large Mr, with a limited removal for organics with medium and small Mr. Using resin alone as pretreatment could be effective in removal of organics but limited in reduction of membrane fouling. With combination of coagulation and resin as pretreatment of microfiltration, not only organics could be removed effectively, but also membrane fouling could be reduced.

  1. Dialysis is superior to anion exchange for removal of dissolved inorganic nitrogen from freshwater samples prior to dissolved organic nitrogen determination

    DEFF Research Database (Denmark)

    Graeber, Daniel; Gücker, Björn; Zwirnmann, Elke;

    2012-01-01

    Dissolved organic nitrogen (DON) is usually determined as the difference between total dissolved nitrogen (TDN) and dissolved inorganic nitrogen (DIN). When applying this approach to samples with high DIN concentrations, there is a risk, that small relative errors in TDN and DIN measurements may...... of AEP and DP for DIN removal in order to increase DON determination accuracy of freshwater samples. The AEP pretreatment performed well for standard compounds, yielding high dissolved organic carbon (DOC) recovery rates and > 99% removal of nitrate, whereas DON recovery rates varied and no removal...... propagate into high absolute errors of the determined DON concentration. To reduce such errors, two pretreatment methods have been suggested for the removal of DIN prior to the determination of DON: anion-exchange pretreatment (AEP) and dialysis pretreatment (DP). In this study, we tested the suitability...

  2. Optimization of SHINE Process: Design and Verification of Plant-Scale AG 1 Anion-Exchange Concentration Column and Titania Sorbent Pretreatment

    Energy Technology Data Exchange (ETDEWEB)

    Stepinski, Dominique C. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Abdul, Momen [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Youker, Amanda J. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Rotsch, David A. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Tkac, Peter [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Chemerisov, Sergey [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Vandegrift, George F. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2016-06-01

    Argonne National Laboratory has developed a Mo-recovery and -purification system for the SHINE medical technologies process, which uses a uranyl sulfate solution for the accelerator-driven production of Mo-99. The objective of this effort is to reduce the processing time for the acidification of the Mo-99 product prior to loading onto a concentration column and concentration of the Mo-99 product solution. Two methods were investigated: (1) the replacement of the titania concentration column by an anion-exchange column to decrease processing time and increase the radioiodine-decontamination efficiency and (2) pretreatment of the titania sorbent to improve its effectiveness for the Mo-recovery and -concentration columns. Promising results are reported for both methods.

  3. Optimization of SHINE Process: Design and Verification of Plant-Scale AG 1 Anion-Exchange Concentration Column and Titania Sorbent Pretreatment

    Energy Technology Data Exchange (ETDEWEB)

    Stepinski, Dominique C. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Abdul, Momen [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Youker, Amanda J. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Rotsch, David A. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Tkac, Peter [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Chemerisov, Sergey [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Vandegrift, George F. [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2016-06-01

    Argonne National Laboratory has developed a Mo-recovery and -purification system for the shine medical technologies process, which uses a uranyl sulfate solution for the accelerator-driven production of Mo-99. The objective of this effort is to reduce the processing time for the acidification of the Mo-99 product prior to loading onto a concentration column and concentration of the Mo-99 product solution. Two methods were investigated: (1) the replacement of the titania concentration column by an anion-exchange column to decrease processing time and increase the radioiodine-decontamination efficiency and (2) pretreatment of the titania sorbent to improve its effectiveness for the Mo-recovery and -concentration columns. Promising results are reported for both methods.

  4. In situ redox speciation analysis of chromium in water by diffusive gradients in thin films using a DE81 anion exchange membrane.

    Science.gov (United States)

    Suárez, Carlos A; de Simone, Thays V; Menegário, Amauri A; Rolisola, Ana M C M; Luko, Karen S; Gastmans, Didier; da Conceição, Fabiano T; Kiang, Chang H

    2016-07-01

    A method for the in situ redox speciation analysis of chromium in water by the diffusive gradients in thin films (DGT) technique using a DE81 anion exchange membrane was successfully developed. For the selective uptake of Cr(VI), a DGT device containing an anion exchange membrane DE81 (cellulose acetate chromatographic paper) was used (DE81-DGT), while selective uptake of Cr(III) was carried out using DGT devices containing the Chelex-100 resin (Chelex-100-DGT). A correlation coefficient of 0.993 was obtained for the linearity of the immersion curves (mass versus time) using DE81-DGT. The diffusion coefficient values for Cr(VI) through the agarose diffusive layer were equal to 4.89±0.5×10(-6)cm(2)s(-1) and 3.95±0.02×10(-6)cm(2)s(-1) (T=23±1°C, I=0.03molL(-1) NaNO3) were obtained by using diffusion cell and immersion curves, respectively. The retention of Cr(VI) by the DE81 membrane in a synthetic sample and river water was not affected by the pH over a wide range 4-9). Recoveries of Cr(VI) between 90% and 120% from solutions of ionic strength ranging from 0.01 to 0. 5molL(-1) NaNO3 were achieved. Finally, the redox speciation analysis of Cr(III) and Cr(VI) in spiked river water and synthetic samples was performed with recoveries greater than 80% and 87% by using Chelex-100-DGT and DE81-DGT devices, respectively. Those results were in excellent agreement with the diphenylcarbazide spectrophotometric method. PMID:27154678

  5. Rapid and simultaneous determination of neptunium and plutonium in environmental samples using anion exchange chromatographic and sequential injection setup combined with inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Full text: This paper presents an automated analytical method for the rapid and simultaneous determination of Pu and Np in the environmental samples. Anion exchange chromatographic column was incorporated in a sequential injection system to actualize the automated separation of Pu isotpes along with 237Np from the matrix elements and interfering radionuclides. K2S2O5-conc. HNO3 was applied as redox reagents for the valence adjustment and stabilization of Pu(IV) and Np(IV). 242Pu preformed well as a tracer for both Pu isotopes and 237Np. It was observed that the cross-link and particle size of the resins had significant effluence on the separation efficiency and anion exchange resin Bio-Rad AG 1 x 4 with the particle size of 100-200 mesh was chosen as the optimum. The investigation on the capacity showed small-sized column packed with 2mL resin sufficed up to 50g of soil sample, which provides an advantage of low consumption of the resin and low generation of acid waste after the column washing. The analytical results for Pu and Np in three reference materials showed good agreement with the certified or reference values at the 0.05 significance level. Chemical yields of Pu and Np equally range from 80% to 100%, and the decontamination factors for uranium, thorium and lead were in the range of 103 to 104. The total time of separation for a single sample was < 2.5 hours, which extremely improve the analysis efficiency and reduces the labor intensity, as well as enables a rapid determination of Pu and Np in emergency situations. (author)

  6. Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

    Directory of Open Access Journals (Sweden)

    Ball James W

    2003-06-01

    Full Text Available A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad™ AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan. Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad™ AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns.

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

    Science.gov (United States)

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

    2016-04-29

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

  8. Isolation and purification of uremic middle molecules by multi-step liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    储结根; 何炳林; 刘晓航; 袁直

    2002-01-01

    Isolation and comparison of uremic sera and urine and normal sera and urine were performed by gel permeation chromatography, anion exchange chromatography and re-versed-phase high performance liquid chromatography. Two uremic middle molecular fractions (A and B) were obtained from uremic sera and urine and normal urine by gel permeation chromatography, but not from normal sera. The anion exchange chromatographic results of fraction A from different origins demonstrate that subfraction A-3 could be excreted in urine by healthy subject, but accumulated in uremic serum for renal failure of patient with uremia. After desalinization subfraction A-3 was analyzed by MALDI-TOF-MS. The results show that subfraction A-3 consists of six compounds with molecular weight 839, 873, 1007.94, 1106, 1680 and 2015 respectively. Finally, by reversed-phase high performance liquid chromatography, subfraction A-3 was further resolved into six independent fractions. Thus, the isolation and purification of six middle molecular c

  9. Liquid chromatography tandem mass spectrometry for measuring ¹³C-labeling in intermediates of the glycolysis and pentose phosphate pathway.

    Science.gov (United States)

    Cocuron, Jean-Christophe; Alonso, Ana Paula

    2014-01-01

    This chapter describes a procedure to analyze (13)C-labeled phosphorylated compounds by liquid chromatography tandem mass spectrometry. Phosphorylated compounds, intermediaries of the glycolysis and pentose phosphate pathway, are separated by anion exchange chromatography and their isotopic labeling is determined by mass spectrometry. A sensitivity in the fmole range is achieved using scheduled multiple reaction monitoring mode.

  10. The rapid identification of elution conditions for therapeutic antibodies from cation-exchange chromatography resins using high-throughput screening.

    Science.gov (United States)

    McDonald, Paul; Tran, Benjamin; Williams, Christopher R; Wong, Marc; Zhao, Ti; Kelley, Brian D; Lester, Philip

    2016-02-12

    Cation-exchange chromatography is widely used in the purification of therapeutic antibodies, wherein parameters such as elution pH and counterion concentration require optimization for individual antibodies across different chromatography resins. With a growing number of antibodies in clinical trials and the pressure to expedite process development, we developed and automated a high-throughput batch-binding screen to more efficiently optimize elution conditions for cation-exchange chromatography resins. The screen maps the binding behavior of antibodies and impurities as a function of pH and counterion concentration in terms of a partition coefficient (Kp). Using this approach, the binding behavior of a library of antibodies was assessed on Poros 50HS and SP Sepharose Fast Flow resins. The diversity in binding behavior between antibodies and across resins translated to the requirement of a variable counterion concentration to elute each antibody. This requirement can be met through the use of a gradient elution. However, a gradient of increasing counterion concentration spans the transition from binding to non-binding for impurities as well as the antibody, resulting in the elution of impurities within the antibody elution peak. Step elution conditions that selectively elute the antibody while retaining impurities on the resin can now be rapidly identified using our high-throughput approach. We demonstrate that by correlating antibody Kp to elution pool volume and yield on packed-bed columns and through the calculation of a separation factor, we can efficiently optimize step elution conditions that maximize impurity clearance and yield for each antibody. PMID:26803905

  11. 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)

  12. Imidazolium-Functionalized Poly(arylene ether sulfone) Anion-Exchange Membranes Densely Grafted with Flexible Side Chains for Fuel Cells.

    Science.gov (United States)

    Guo, Dong; Lai, Ao Nan; Lin, Chen Xiao; Zhang, Qiu Gen; Zhu, Ai Mei; Liu, Qing Lin

    2016-09-28

    With the intention of optimizing the performance of anion-exchange membranes (AEMs), a set of imidazolium-functionalized poly(arylene ether sulfone)s with densely distributed long flexible aliphatic side chains were synthesized. The membranes made from the as-synthesized polymers are robust, transparent, and endowed with microphase segregation capability. The ionic exchange capacity (IEC), hydroxide conductivity, water uptake, thermal stability, and alkaline resistance of the AEMs were evaluated in detail for fuel cell applications. Morphological observation with the use of atomic force microscopy and small-angle X-ray scattering reveals that the combination of high-local-density-type and side-chain-type architectures induces distinguished nanophase separation in the AEMs. The as-prepared membranes have advantages in effective water management and ionic conductivity over traditional main-chain polymers. Typically, the conductivity and IEC were in the ranges of 57.3-112.5 mS cm(-1) and 1.35-1.84 mequiv g(-1) at 80 °C, respectively. Furthermore, the membranes exhibit good thermal and alkaline stability and achieve a peak power density of 114.5 mW cm(-2) at a current density of 250.1 mA cm(-2). Therefore, the present polymers containing clustered flexible pendent aliphatic imidazolium promise to be attractive AEM materials for fuel cells.

  13. A Pd/C-CeO2 Anode Catalyst for High-Performance Platinum-Free Anion Exchange Membrane Fuel Cells.

    Science.gov (United States)

    Miller, Hamish A; Lavacchi, Alessandro; Vizza, Francesco; Marelli, Marcello; Di Benedetto, Francesco; D'Acapito, Francesco; Paska, Yair; Page, Miles; Dekel, Dario R

    2016-05-10

    One of the biggest obstacles to the dissemination of fuel cells is their cost, a large part of which is due to platinum (Pt) electrocatalysts. Complete removal of Pt is a difficult if not impossible task for proton exchange membrane fuel cells (PEM-FCs). The anion exchange membrane fuel cell (AEM-FC) has long been proposed as a solution as non-Pt metals may be employed. Despite this, few examples of Pt-free AEM-FCs have been demonstrated with modest power output. The main obstacle preventing the realization of a high power density Pt-free AEM-FC is sluggish hydrogen oxidation (HOR) kinetics of the anode catalyst. Here we describe a Pt-free AEM-FC that employs a mixed carbon-CeO2 supported palladium (Pd) anode catalyst that exhibits enhanced kinetics for the HOR. AEM-FC tests run on dry H2 and pure air show peak power densities of more than 500 mW cm(-2) .

  14. Characterization of Anion Exchange Membrane Containing Epoxy Ring and C–Cl Bond Quaternized by Various Amine Groups for Application in Fuel Cells

    Directory of Open Access Journals (Sweden)

    Sung Kuk Jeong

    2015-07-01

    Full Text Available Anion exchange membranes were synthesized from different compositions of glycidyl methacrylate (GMA and vinylbenzyl chloride (VBC, with constant content of divinyl benzene (DVB by radical polymerization using benzoyl peroxide (BPO on non-woven polyethylene terephthalate (PET substrate. Polymerized membranes were then quaternized by soaking in trimethylamine (TMA, triethylamine (TEA, tripropylamine (TPA, and 1,4-diazabicyclo [2.2.2] octane (DABCO. Characteristics of membranes were confirmed by Fourier transform infrared spectroscopy, water uptake, ion exchange capacity, ion conductivity, thermal, and alkaline stability. The results revealed that membranes quaternized by TPA and DABCO showed high affinity when GMA content was 15 wt% and 75 wt%, respectively. IEC and ion conductivity of membranes quaternized by TPA were 1.34 meq·g−1 and 0.022 S·cm−1 (at 60 °C, respectively. IEC and ion conductivity of membranes were quaternized by DABCO were 1.34 meq·g−1 and 0.021 S·cm−1 (at 60 °C, respectively. The results indicate that the membrane containing GMA 15 wt% quaternized by TPA showed the highest thermal stability among membranes and exhibited high ion conductivity compared to existing researches using GMA, VBC, and DVB monomers.

  15. New inorganic (an)ion exchangers based on Mg–Al hydrous oxides: (Alkoxide-free) sol–gel synthesis and characterisation

    KAUST Repository

    Chubar, Natalia

    2011-05-01

    New inorganic ion exchangers based on double Mg-Al hydrous oxides were generated via the new non-traditional sol-gel synthesis method which avoids using metal alkoxides as raw materials. Surface chemical and adsorptive properties of the final products were controlled by several ways of hydrogels and xerogels treatments which produced the materials of the layered structure, mixed hydrous oxides or amorphous adsorbents. The final adsorptive materials obtained via thermal treatment of xerogels were the layered mesoporous materials with carbonate in the interlayer space, surface abundance with hydroxylic groups and maximum adsorptive capacity to arsenate. Higher affinity of Mg-Al hydrous oxides towards H2AsO4- is confirmed by steep adsorption isotherms having plateau (removal capacity) at 220. mg[As]. gdw-1 for the best sample at pH = 7, fast adsorption kinetics and little pH effect. Adsorption of arsenite, fluoride, bromate, bromide, selenate, borate by Mg-Al hydrous oxides was few times high either competitive (depending on the anion) as compare with the conventional inorganic ion exchange adsorbents. © 2011 Elsevier Inc.

  16. Single particle electron microscopy analysis of the bovine anion exchanger 1 reveals a flexible linker connecting the cytoplasmic and membrane domains.

    Directory of Open Access Journals (Sweden)

    Jiansen Jiang

    Full Text Available Anion exchanger 1 (AE1 is the major erythrocyte membrane protein that mediates chloride/bicarbonate exchange across the erythrocyte membrane facilitating CO₂ transport by the blood, and anchors the plasma membrane to the spectrin-based cytoskeleton. This multi-protein cytoskeletal complex plays an important role in erythrocyte elasticity and membrane stability. An in-frame AE1 deletion of nine amino acids in the cytoplasmic domain in a proximity to the membrane domain results in a marked increase in membrane rigidity and ovalocytic red cells in the disease Southeast Asian Ovalocytosis (SAO. We hypothesized that AE1 has a flexible region connecting the cytoplasmic and membrane domains, which is partially deleted in SAO, thus causing the loss of erythrocyte elasticity. To explore this hypothesis, we developed a new non-denaturing method of AE1 purification from bovine erythrocyte membranes. A three-dimensional (3D structure of bovine AE1 at 2.4 nm resolution was obtained by negative staining electron microscopy, orthogonal tilt reconstruction and single particle analysis. The cytoplasmic and membrane domains are connected by two parallel linkers. Image classification demonstrated substantial flexibility in the linker region. We propose a mechanism whereby flexibility of the linker region plays a critical role in regulating red cell elasticity.

  17. Imidazolium-Functionalized Poly(arylene ether sulfone) Anion-Exchange Membranes Densely Grafted with Flexible Side Chains for Fuel Cells.

    Science.gov (United States)

    Guo, Dong; Lai, Ao Nan; Lin, Chen Xiao; Zhang, Qiu Gen; Zhu, Ai Mei; Liu, Qing Lin

    2016-09-28

    With the intention of optimizing the performance of anion-exchange membranes (AEMs), a set of imidazolium-functionalized poly(arylene ether sulfone)s with densely distributed long flexible aliphatic side chains were synthesized. The membranes made from the as-synthesized polymers are robust, transparent, and endowed with microphase segregation capability. The ionic exchange capacity (IEC), hydroxide conductivity, water uptake, thermal stability, and alkaline resistance of the AEMs were evaluated in detail for fuel cell applications. Morphological observation with the use of atomic force microscopy and small-angle X-ray scattering reveals that the combination of high-local-density-type and side-chain-type architectures induces distinguished nanophase separation in the AEMs. The as-prepared membranes have advantages in effective water management and ionic conductivity over traditional main-chain polymers. Typically, the conductivity and IEC were in the ranges of 57.3-112.5 mS cm(-1) and 1.35-1.84 mequiv g(-1) at 80 °C, respectively. Furthermore, the membranes exhibit good thermal and alkaline stability and achieve a peak power density of 114.5 mW cm(-2) at a current density of 250.1 mA cm(-2). Therefore, the present polymers containing clustered flexible pendent aliphatic imidazolium promise to be attractive AEM materials for fuel cells. PMID:27579786

  18. Sequential injection analysis of lead using time-based colorimetric detection and preconcentration on an anionic-exchange resin.

    Science.gov (United States)

    Aracama, Nestor Zárate; Araújo, Alberto N; Perez-Olmos, Ricardo

    2004-04-01

    The development of a sequential injection analysis manifold for the colorimetric determination of lead in water samples is described The concentration of lead was assessed from its catalytic effect on the reaction of resazurine reduction caused by sulfide in an alkali medium. To that effect, the reaction zone was stopped at the detector, and the time interval required for the attainment of an absorbance decrease of 0.800 at the wavelength of 610 nm was estimated. Interference of other transition metals of the samples was minimized by adding potassium iodide to the sample and retaining the iodocomplexes formed in an on-line anionic resin (AGI X8). Elution was made with a 2 mol/L sodium hydroxide solution. The relationship [SIA] microg/L = 0.99 (+/- 0.11) x [ETAAS] microg/L + 0 (+/- 4) was obtained upon comparing the results given by the proposed system and by electrothermal atomization atomic absorption spectrometry (ETAAS) after the analysis of ten water samples. PMID:15116968

  19. Simultaneous determination of iodide and iodate in povidone iodine solution by ion chromatography with homemade and exchange capacity controllable columns and column-switching technique.

    Science.gov (United States)

    Huang, Zhongping; Zhu, Zuoyi; Subhani, Qamar; Yan, Wenwu; Guo, Weiqiang; Zhu, Yan

    2012-08-17

    A simple ion chromatographic method for simultaneous detection of iodide and iodate in a single running was proposed, with columns packed with homemade functionalized polystyrene-divinylbenzene (PS-DVB) resins and column-switching technique. Homemade resins were functionalized with controllable amounts of quaternary ammonium groups. The low-capacity anion-exchange column and high-capacity anion-exchange column were prepared, due to the resins having different exchange capacities. With this method, iodide and iodate in povidone iodine solution were detected simultaneously in a short time with iodide being eluted off first. A series of standard solutions consisting of target anions of various concentrations from 0.01 mg/L to 100 mg/L were analyzed. Each anion exhibited satisfactory linearity, with correlation coefficient r ≥ 0.9990. The detection limits (LODs) for iodide and iodate obtained by injecting 100 μL of sample were 5.66 and 14.83 μg/L (S/N=3), respectively. A spiking study was performed with satisfactory recoveries between 101.2% and 100.6% for iodide and iodate. PMID:22771256

  20. Use of strong anion exchange resins for the removal of perfluoroalkylated substances from contaminated drinking water in batch and continuous pilot plants.

    Science.gov (United States)

    Zaggia, Alessandro; Conte, Lino; Falletti, Luigi; Fant, Massimo; Chiorboli, Andrea

    2016-03-15

    In recent years abnormally high levels of perfluoroalkylated substances (PFAS) have been detected both in surface and underground water sampled in an area covering approximately 150 square kilometers in the Veneto region (Italy) indicating the presence of a pollution point source (fluorochemicals production plant). Adsorption on granular activated carbon is an emergency measure which is poorly effective requiring frequent replacement. This work focuses on the application of three strong anion exchange resins (Purolite® A520E, A600E and A532E) for the removal of traces of PFOA, PFOS, PFBA and PFBS (concentration of hundreds of ng L(-1)) from drinking water. This technology is attractive for the possibility of reusing resins after an in-situ regeneration step. A strong relationship between the hydrophobicity of the exchange functional group of the resin and its capacity in removing PFAS exists. A600E (non hydrophobic) and A520E (fairly hydrophobic) show a reduced sorption capacity compared to A532E (highly hydrophobic). While A600E and A520E can be regenerated with solvent-less dilute solutions of non-toxic NH4Cl and NH4OH, A532E requires concentrated solutions of methanol or ethanol and 1% NH4Cl and for the sake of this work it was regarded as non-regenerable. The volume of regeneration effluents requiring incineration can be efficiently reduced by more than 96.5% by using reverse osmosis coupled with under-vacuum evaporation. Transmission electron analysis on saturated resins showed that large molecular macro-aggregates of PFAS can form in the intraparticle pores of resin indicating that ion exchange is not the only mechanism involved in PFAS removal. PMID:26774262

  1. Mutations associated with Dent’s disease affect gating and voltage dependence of the human anion/proton exchanger ClC-5

    Directory of Open Access Journals (Sweden)

    Alexi eAlekov

    2015-05-01

    Full Text Available Dent’s disease is associated with impaired renal endocytosis and endosomal acidification. It is linked to mutations in the membrane chloride/proton exchanger ClC-5, however, a direct link between localization in the protein and functional phenotype of the mutants has not been established until now. Here, two Dent’s disease mutations, G212A and E267A, were investigated using heterologous expression in HEK293T cells, patch-clamp measurements and confocal imaging. WT and, mutant ClC-5 exhibited mixed cell membrane and vesicular distribution. Reduced ion currents were measured for both mutants and both exhibited reduced capability to support endosomal acidification. Functionally, mutation G212A was capable of mediating anion/proton antiport but dramatically shifted the activation of ClC-5 towards more depolarized potentials. The shift can be explained by impeded movements of the neighboring gating glutamate Gluext, a residue that confers major part of the voltage dependence of ClC-5 and serves as a gate at the extracellular entrance of the anion transport pathway. Cell surface abundance of E267A was reduced by ~50% but also dramatically increased gating currents were detected for this mutant and accordingly reduced probability to undergoing cycles associated with electrogenic ion transport. Structurally, the gating alternations correlate to the proximity of E267A to the proton glutamate Gluin that serves as intracellular gate in the proton transport pathway and regulates the open probability of ClC-5. Remarkably, two other mammalian isoforms, ClC-3 and ClC-4, also differ from ClC-5 in gating characteristics affected by the here investigated disease-causing mutations. This evolutionary specialization, together with the functional defects arising from mutations G212A and E267A, demonstrate that the complex gating behavior exhibited by most of the mammalian CLC transporters is an important determinant of their cellular function.

  2. Purification of Staphylococcus aureus beta-lactamases by using sequential cation-exchange and affinity chromatography.

    OpenAIRE

    Kernodle, D S; Zygmunt, D J; McGraw, P A; Chipley, J R

    1990-01-01

    Boronic acids are active-site inhibitors of serine beta-lactamases, and a phenylboronic acid-agarose affinity column has been used to purify beta-lactamase from crude cell extracts of several bacterial species. We applied phenylboronic acid-agarose chromatography to the purification of Staphylococcus aureus beta-lactamase. Two factors interfered with the success of the previously described single-step chromatographic protocol. First, staphylococcal beta-lactamase exhibited non-active-site-med...

  3. Discovery and early development of non-suppressed ion chromatography.

    Science.gov (United States)

    Fritz, James S; Gjerde, Douglas T

    2010-08-01

    This year marks the 30th anniversary of the publication of Non-Suppressed Ion Chromatography, which is a method for the rapid separation of anions with on-line conductimetric detection. In this method, the separation column is connected directly to the conductimetric detector. This single-column method is a simpler technique than the original suppressed ion chromatography method, which requires a large suppressor column to reduce the background conductance. In the new method, the background signal is reduced to a manageable level simply by using an ion-exchange separation column of low exchange capacity that lowers the eluent concentration needed for separation. The eluent ion used for separation is chosen based on having large, bulky structure, which lowers the equivalent conductance and facilitates detection of the sample anions. This is a personal account of the initial discovery and early development of non-suppressed ion chromatography. The circumstances for the discovery are recounted by the two authors. Methods are described for determination of anions, cations with indirect detection, and techniques for increasing detection sensitivity. A fundamental equation for the prediction of ion chromatography detector response is given, and the development of several types of detection schemes for ion chromatography is discussed. Finally, the impact of non-suppressed ion chromatography is discussed together with comments on the discovery process.

  4. AMP18 interacts with the anion exchanger SLC26A3 and enhances its expression in gastric cancer cells.

    Science.gov (United States)

    Di Stadio, Chiara Stella; Altieri, Filomena; Miselli, Giuseppina; Elce, Ausilia; Severino, Valeria; Chambery, Angela; Quagliariello, Vincenzo; Villano, Valentina; de Dominicis, Gianfranco; Rippa, Emilia; Arcari, Paolo

    2016-02-01

    AMP18 is a stomach-specific secreted protein expressed in normal gastric mucosa but absent in gastric cancer. AMP18 plays a major role in maintaining gastric mucosa integrity and is characterized by the presence of a BRICHOS domain consisting of about 100 amino acids, present also in several unrelated proteins, and probably endowed with a chaperon-like activity. In this work, we exploited a functional proteomic strategy to identify potential AMP18 interactors with the aim to add knowledge on its functional role within gastric cell lines and tissues. To this purpose, recombinant biotinylated AMP18 was purified and incubated with protein extract from human normal gastric mucosa by applying an affinity chromatography strategy. The interacting proteins were identified by peptide mass fingerprinting using MALDI-TOF mass spectrometry. The pool of interacting proteins contained SLC26A3, a protein expressed in the apical membrane of intestinal epithelial cells, supposed to play a critical role in Cl(-) absorption and fluid homeostasis. The interaction was also confirmed by Western blot with anti-SLC26A3 on transfected AGS cell extract following AMP18 pull-down. Furthermore, the interaction between AMP18 and SLC26A3 was also validated by confocal microscopy that showed a co-localization of both proteins at plasma membrane level. More importantly, for the first time, we showed that SLC26A3 is down-regulated in gastric cancer and that the overexpression of AMP18 in AMP-transfected gastric cancer cells up-regulated the expression of SLC26A3 both at transcriptional and translational level, the latter probably through the activation of the MAP kinases pathway. These findings strongly suggest that AMP18 might play an anti-inflammatory role in maintaining mucosal integrity also by regulating SLC26A3 level. PMID:26700142

  5. 超声提取-离子色谱法测定蜂蜜柚子茶中的可溶性糖%Determination of Soluble Sugars in Honey Pomelo Tea by Anion Chromatography with Ultrasonic Extraction

    Institute of Scientific and Technical Information of China (English)

    许丽; 周光明; 余娜; 张丽贤

    2011-01-01

    建立超声提取-高效阴离子交换-脉冲安培检测(HPAE-PAD)同时分离并测定蜂蜜柚子茶中可溶性糖的分析方法.采用METROSEP CARB 1(150mm×4.0mm)分离柱,对分离条件进行了优化,确定淋洗液为5.0mmol/L的NaOH溶液,流速为1.0mL/min.蔗糖、葡萄糖、果糖的检出限分别为0.2,0.1,1.0μg/mL.混合标准溶液连续6次进样,峰高相对标准偏差为1.56%3.40%,回收率为86.80%98.80%.该方法样品前处理简单,灵敏度高,为蜂蜜柚子茶的质量检测提供了一个简单有效的方法.%A method for the determination of soluble sugars in honey pomelo tea by high performance anion exchange chromatography with ultrasonic extraction and pulsed amperometric detection(HPAE-PAD) is described in this paper.The separation conditions were investigated on METROSEP CARB 1(150 mm×4.0 mm) column.The optimal separations were achieved with 5.0 mmol/L NaOH as the eluent at a rate of 1.0 mL/min.The detection limits of sucrose,glucose and fructose were 0.2 μg/mL,0.1 μg/mL and 1.0 μg/mL,respectively.The RSDs(relative standard deviation) of peak height for six consecutive determinations varied from 1.56% to 3.40%,with a recovery of 86.80%-98.80%.The above method proved to be simple and highly sensitive for sample pretreatment and is,therefore,recommended for quality inspection of honey pomelo tea.

  6. Treatment of Perchlorate-Contaminated Groundwater Using Highly-Selective, Regenerable Anion-Exchange Resins at Edwards Air Force Base

    Energy Technology Data Exchange (ETDEWEB)

    Gu, B.

    2003-05-30

    Selective ion exchange is one of the most effective treatment technologies for removing low levels of perchlorate (ClO{sub 4}{sup -}) from contaminated water because of its high efficiency without adverse impacts on the water quality caused by adding or removing any chemicals or nutrients. This report summarizes both the laboratory and a field pilot-scale studies to determine the ability and efficiency of the bifunctional synthetic resins to remove ClO{sub 4}{sup -} from the contaminated groundwater at the Edwards Air Force Base in California. Regeneration of the resins after groundwater treatment was also evaluated using the FeCl{sub 3}-HCl regeneration technique recently developed at Oak Ridge National Laboratory. On the basis of this study, the bifunctional resin, D-3696 was found to be highly selective toward ClO{sub 4}{sup -} and performed much better than one of the best commercial nitrate-selective resins (Purolite A-520E) and more than an order of magnitude better than the Purolite A-500 resin (with a relatively low selectivity). At an influent concentration of {approx} 450 {micro}g/L ClO{sub 4}{sup -} in groundwater, the bifunctional resin bed treated {approx} 40,000 empty bed volumes of groundwater before a significant breakthrough of ClO{sub 4}{sup -} occurred. The presence of relatively high concentrations of chloride and sulfate in site groundwater did not appear to affect the ability of the bifunctional resin to remove ClO{sub 4}{sup -}. However, the presence of high iron or iron oxyhydroxides and/or biomass in groundwater caused a significant fouling of the resin beds and greatly influenced the effectiveness in regenerating the resins sorbed with ClO{sub 4}{sup -}. Under such circumstances, a prefilter ({approx} 0.5-1 {micro}m) was found to be necessary to remove these particulates and to reduce the risk of fouling of the resin beds. Without significant fouling, the resin bed could be effectively regenerated by the FeCl{sub 3} displacement technique

  7. Determination of Inorganic Anions in Water by Ion Chromatography Method to Explore the Minimum Detectable Concentration%水中无机阴离子最低检出浓度的计算--离子色谱法

    Institute of Scientific and Technical Information of China (English)

    金梓谦

    2014-01-01

    The method for determination of the minimum detectable concentration of the inorganic anions in water by ion chromatography method was explored, and the calculation results are given to meet the relevant requirements of environmental standards.%对离子色谱法测定水中无机阴离子的最低检出浓度的方法进行了探究,并给出计算结果,满足环境标准相关要求。

  8. Multivariate analysis of the transport in an ion exchange membrane bioreactor for removal of anionic micropollutants from drinking water.

    Science.gov (United States)

    Ricardo, A R; Velizarov, S; Crespo, J G; Reis, M A M

    2011-01-01

    The present study focuses on investigating the effects of biological compartment conditions on the transport of nitrate and perchlorate in an Ion Exchange Membrane Bioreactor (IEMB). In this hybrid process, the transport depends not only on the membrane properties but also on the biological compartment conditions. The experiments were planned according to the Plackett-Burman statistical design in order to cover a broader range of experimental conditions, under which a previously developed mechanistic transport model was not able to predict correctly the transport fluxes of the target pollutants. Using Principal Component Analysis, it was possible to identify not only the concentrations of target (nitrate and perchlorate) and of major driving counter-ion (chloride) but also those of some biomedium components (e.g. ammonia, ethanol and sulphate) as variables that affect the transport rate of micropollutants across the membrane. These conclusions are based on the loadings of the two first principal components that describe 84% of the data variance. The present study also revealed that the hydraulic retention time and the hydrodynamic conditions in the biocompartment have a minor contribution to the micropollutants transport. The results obtained are important for process optimization purposes. PMID:21977639

  9. Cation Exchange Strategy for the Encapsulation of a Photoactive CO-Releasing Organometallic Molecule into Anionic Porous Frameworks.

    Science.gov (United States)

    Carmona, Francisco J; Rojas, Sara; Sánchez, Purificación; Jeremias, Hélia; Marques, Ana R; Romão, Carlos C; Choquesillo-Lazarte, Duane; Navarro, Jorge A R; Maldonado, Carmen R; Barea, Elisa

    2016-07-01

    The encapsulation of the photoactive, nontoxic, water-soluble, and air-stable cationic CORM [Mn(tacn)(CO)3]Br (tacn = 1,4,7-triazacyclononane) in different inorganic porous matrixes, namely, the metalorganic framework bio-MOF-1, (NH2(CH3)2)2[Zn8(adeninate)4(BPDC)6]·8DMF·11H2O (BPDC = 4,4'-biphenyldicarboxylate), and the functionalized mesoporous silicas MCM-41-SO3H and SBA-15-SO3H, is achieved by a cation exchange strategy. The CO release from these loaded materials, under simulated physiological conditions, is triggered by visible light. The results show that the silica matrixes, which are unaltered under physiological conditions, slow the kinetics of CO release, allowing a more controlled CO supply. In contrast, bio-MOF-1 instability leads to the complete leaching of the CORM. Nevertheless, the degradation of the MOF matrix gives rise to an enhanced CO release rate, which is related to the presence of free adenine in the solution. PMID:27291890

  10. A single nucleotide polymorphism in kidney anion exchanger 1 gene is associated with incomplete type 1 renal tubular acidosis

    Science.gov (United States)

    Takeuchi, Takumi; Hattori-Kato, Mami; Okuno, Yumiko; Kanatani, Atsushi; Zaitsu, Masayoshi; Mikami, Koji

    2016-01-01

    Various conditions including distal renal tubular acidosis (dRTA) can induce stone formation in the kidney. dRTA is characterized by an impairment of urine acidification in the distal nephron. dRTA is caused by variations in genes functioning in intercalated cells including SLC4A1/AE1/Band3 transcribing two kinds of mRNAs encoding the Cl−/HCO3− exchanger in erythrocytes and that expressed in α-intercalated cells (kAE1). With the acid-loading test, 25% of urolithiasis patients were diagnosed with incomplete dRTA. In erythroid intron 3 containing the promoter region of kAE1, rs999716 SNP showed a significantly higher minor allele A frequency in incomplete dRTA compared with non-dRTA patients. The promoter regions of the kAE1 gene with the minor allele A at rs999716 downstream of the TATA box showed reduced promoter activities compared that with the major allele G. Patients with the A allele at rs999716 may express less kAE1 mRNA and protein in the intercalated cells, developing incomplete dRTA. PMID:27767102

  11. Adsorption and Desorption Properties of Phytic Acid from Rice Bran on Anion Exchange Resin%阴离子交换树脂对米糠植酸的吸附解吸性能

    Institute of Scientific and Technical Information of China (English)

    王琳; 罗建平; 查学强; 张海林; 潘利华

    2011-01-01

    通过静态和动态试验研究了6种阴离子交换树脂对植酸的吸附与解吸性能.结果表明,D201树脂对植酸的吸附交换作用较好,且在pH值为2.2时吸附能力最强,静态吸附量达到94.54 mg/g,1.5 mol/L的NaOH溶液利于植酸解吸;Freundlich吸附等温方程可以较好地描述D201树脂对植酸的等温吸附,表明吸附在常温下进行即可;D201树脂对植酸的吸附过程符合Lagergren一级速率方程,表观吸附速率常数k与植酸起始植酸浓度呈负相关关系,与温度呈正相关关系.在D201树脂对植酸的动态吸附与解吸过程中,层析柱管径、上样液浓度、上样液流速和洗脱剂流速对吸附与解吸效果影响较大.%The absorption and desorption properties of phytic acid on anion exchange resin were investigated through static and dynamic experiments. The results showed that D201 resin had the best exchange adsorption performance among all tested resins. The static absorption capacity of D201 resin reached 94. 54 mg/g when the pH value of phytic acid solution was adjusted to 2. 2, and sodium hydroxide solution of 1. 5 mol/L was beneficial to desorption. The absorption behavior of D201 resin for phytic acid obeyed the Freundlich adsorption isotherm equation, indicating that the absorption can be performed under normal temperature. The absorption kinetic data complied with Lagergren pseudo-first-order rate equation. The apparent adsorption rate k has a negative correlation with the initial concentration of phytic acid and has a positive correlation with temperature. As far as the dynamic absorption and desorption of phytic acid on D201 resin was concerned, the effects of chromatography column diameter, sample concentration, sample flowing velocity and eluant flowing velocity were notably observed.

  12. Role of adaptor proteins and clathrin in the trafficking of human kidney anion exchanger 1 (kAE1) to the cell surface.

    Science.gov (United States)

    Junking, Mutita; Sawasdee, Nunghathai; Duangtum, Natapol; Cheunsuchon, Boonyarit; Limjindaporn, Thawornchai; Yenchitsomanus, Pa-thai

    2014-07-01

    Kidney anion exchanger 1 (kAE1) plays an important role in acid-base homeostasis by mediating chloride/bicarbornate (Cl-/HCO3-) exchange at the basolateral membrane of α-intercalated cells in the distal nephron. Impaired intracellular trafficking of kAE1 caused by mutations of SLC4A1 encoding kAE1 results in kidney disease - distal renal tubular acidosis (dRTA). However, it is not known how the intracellular sorting and trafficking of kAE1 from trans-Golgi network (TGN) to the basolateral membrane occurs. Here, we studied the role of basolateral-related sorting proteins, including the mu1 subunit of adaptor protein (AP) complexes, clathrin and protein kinase D, on kAE1 trafficking in polarized and non-polarized kidney cells. By using RNA interference, co-immunoprecipitation, yellow fluorescent protein-based protein fragment complementation assays and immunofluorescence staining, we demonstrated that AP-1 mu1A, AP-3 mu1, AP-4 mu1 and clathrin (but not AP-1 mu1B, PKD1 or PKD2) play crucial roles in intracellular sorting and trafficking of kAE1. We also demonstrated colocalization of kAE1 and basolateral-related sorting proteins in human kidney tissues by double immunofluorescence staining. These findings indicate that AP-1 mu1A, AP-3 mu1, AP-4 mu1 and clathrin are required for kAE1 sorting and trafficking from TGN to the basolateral membrane of acid-secreting α-intercalated cells.

  13. Durability and performance of polystyrene- b -poly(vinylbenzyl trimethylammonium) diblock copolymer and equivalent blend anion exchange membranes

    Energy Technology Data Exchange (ETDEWEB)

    Vandiver, Melissa A. [Department of Chemical and Biological Engineering, Colorado School of Mines, Golden Colorado 80401; Caire, Benjamin R. [Department of Chemical and Biological Engineering, Colorado School of Mines, Golden Colorado 80401; Poskin, Zach [Department of Chemical and Biological Engineering, Colorado School of Mines, Golden Colorado 80401; Li, Yifan [Department of Chemistry and Geochemistry, Colorado School of Mines, Golden Colorado 80401; Seifert, Sönke [X-Ray Science Division, Argonne National Laboratory, Argonne Illinois 60439; Knauss, Daniel M. [Department of Chemistry and Geochemistry, Colorado School of Mines, Golden Colorado 80401; Herring, Andrew M. [Department of Chemical and Biological Engineering, Colorado School of Mines, Golden Colorado 80401; Liberatore, Matthew W. [Department of Chemical and Biological Engineering, Colorado School of Mines, Golden Colorado 80401

    2014-11-01

    Anion exchange membranes (AEM) are solid polymer electrolytes that facilitate ion transport in fuel cells. In this study, a polystyrene-b-poly(vinylbenzyl trimethylammonium) diblock copolymer was evaluated as potential AEM and compared with the equivalent homopolymer blend. The diblock had a 92% conversion of reactive sites with an IEC of 1.72 ± 0.05 mmol g-1, while the blend had a 43% conversion for an IEC of 0.80 ± 0.03 mmol g-1. At 50°C and 95% relative humidity, the chloride conductivity of the diblock was higher, 24–33 mS cm-1, compared with the blend, 1–6 mS cm-1. The diblock displayed phase separation on the length scale of 100 nm, while the blend displayed microphase separation (~10 μm). Mechanical characterization of films from 40 to 90 microns thick found that elasticity and elongation decreased with the addition of cations to the films. At humidified conditions, water acted as a plasticizer to increase film elasticity and elongation. While the polystyrene-based diblock displayed sufficient ionic conductivity, the films' mechanical properties require improvement, i.e., greater elasticity and strength, before use in fuel cells. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41596.

  14. Using an Anion Exchange Membrane to Predict Soil Available N and S Supplies and the Impact of N and S Fertilization on Canola and Wheat Growth

    Institute of Scientific and Technical Information of China (English)

    P. QIAN; J. J. SCHOENAU

    2007-01-01

    A growth chamber study was conducted to determine the relationships between the supply of soil available nitrogen (N) and sulfur (S) and canola (Brassica napus) and wheat (Triticum aestivum L. 'Biggar') N and S uptake and yield in three Western Canadian soils. The suitability of one-hour burial with an anion exchange membrane (AEM) was assessed for its utility as a quick test of the available N:S balance in the soil. Canola and wheat were grown on a Luvisolic soil low in available S and on Brown and Black Chernozemic soils low in both available N and S, with different rates and combinations of N and S fertilizers applied. AEM burial was used to assess soil available nitrate and sulfate supply rates after fertilization. Dry matter yield and N and S concentrations in plant tissues were determined after 6 weeks of growth.The soil available N:S ratio determined by AEM burial closely reflected the relative supplies of available N and S as revealed in the N:S ratios of plant tissue dry matter. The highest yields were achieved where the available N:S ratio in soil and plant tissue ranged from 5 to 13. Thus, a one-hour burial of an AEM probe in the field may be a useful tool to quickly test if a balanced N and S supply is present in the soil for optimum crop yield.

  15. An efficient method for decoloration of polysaccharides from the sprouts of Toona sinensis (A. Juss.) Roem by anion exchange macroporous resins.

    Science.gov (United States)

    Shi, Yingying; Liu, Tingting; Han, Yun; Zhu, Xiufang; Zhao, Xiaojuan; Ma, Xijun; Jiang, Dingyun; Zhang, Qianghua

    2017-02-15

    An efficient decoloration method for polysaccharides from the sprouts of Toona sinensis (A. Juss.) Roem (PSTS) by anion exchange macroporous resins (AEMR) was investigated in the present paper. The results suggested that D941 resin offered better decoloration efficiency than other tested resins. Based on single-factor experiments, the optimal decoloration parameters of D941 resin were obtained as follows: temperature of 45°C, sample initial concentration of 30mg/ml, pH value of 8.5, static decoloration time of 90min, dynamic decoloration processing volume of 5.5BV with the flow rate of 2BV/h. Decoloration ratio, PSTS recovery ratio and selectivity coefficient were 91.94±1.23%, 90.05±2.35% and 10.92±0.63, respectively. Most of pigment impurities were successfully removed from PSTS solutions after treated by D941 resin, and there was no significant difference in carbohydrate concentration, characteristic groups and molecular weight. Compared with H2O2 oxidation and activated carbon adsorption, this developed method is superior. PMID:27664659

  16. Mulliken Hush elucidation of the encounter (precursor) complex in intermolecular electron transfer via self-exchange of tetracyanoethylene anion-radical

    Science.gov (United States)

    Rosokha, S. V.; Newton, M. D.; Head-Gordon, M.; Kochi, J. K.

    2006-05-01

    The paramagnetic [1:1] encounter complex (TCNE)2-rad is established as the important precursor in the kinetics and mechanism of electron-transfer for the self-exchange between tetracyanoethylene acceptor ( TCNE) and its radical-anion as the donor. Spectroscopic observation of the dimeric complex (TCNE)2-rad by its intervalence absorption band at the solvent-dependent wavelength of λIV ˜ 1500 nm facilitates the application of Mulliken-Hush theory which reveals the significant electronic interaction extant between the pair of cofacial TCNE moieties with the sizable coupling of HDA = 1000 cm -1. The transient existence of such an encounter complex provides the critical link in the electron-transfer kinetics by lowering the classical Marcus reorganization barrier by the amount of HDA in this strongly adiabatic system. Ab initio quantum-mechanical methods as applied to independent theoretical computations of both the reorganization energy ( λ) and the electronic coupling element ( HDA) confirm the essential correctness of the Mulliken-Hush formalism for fast electron transfer via strongly coupled donor/acceptor encounter complexes.

  17. Cross-Linked Quaternized Poly(styrene-b-(ethylene-co-butylene)-b-styrene) for Anion Exchange Membrane: Synthesis, Characterization and Properties.

    Science.gov (United States)

    Dai, Pei; Mo, Zhao-Hua; Xu, Ri-Wei; Zhang, Shu; Wu, Yi-Xian

    2016-08-10

    Poly(styrene-b-(ethylene-co-butylene)-b-styrene) triblock copolymer (SEBS) was selected for functionalization and cross-linking reaction to prepare the anion exchange membrane. The cross-linked quaternized SEBS (QSEBS-Cn) membranes were synthesized by simultaneous of quaternization and cross-linking of chloromethylated SEBS with α,ω-difunctional tertiary amines. The spacer groups of (-CH2-)n in diamines did affect the functionalization, micromorphology and properties of the resulting QSEBS-Cn membranes. The ionic conductivity of QSEBS-Cn membranes greatly increased and methanol resistance slightly decreased with increasing the length of spacer groups in the cross-linked structures from -(CH2)- to -(CH2)6-. Compared to the un-cross-linked QSEBS, the QSEBS-Cn membranes behaved much higher mechanical property, service temperature, chemical stability and thermal stability. Moreover, the hybrid composite membrane of QSEBS-C6 with 0.5% of graphene oxide could also be in situ prepared. This hybrid membrane had both relatively high ionic conductivity of 2.0 × 10(-2) S·cm(-1) and high selectivity of 7.6 × 10(4) S·s·cm(-3) at 60 °C due to its low methanol permeability. PMID:27459593

  18. 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...

  19. [Determination of succinic acid in desvenlafaxine succinate by high performance ion-exclusion chromatography and high performance ion-exchange chromatography].

    Science.gov (United States)

    Zong, Yanping; Li, Jinghua; Sun, Wei; Liu, Guixia; Lu, Jinghua; Shan, Guangzhi

    2016-02-01

    New methods were developed for the determination of succinic acid in desvenlafaxine succinate (DVS) by high performance ion-exclusion chromatography (HPIEC) and high performance ion-exchange chromatography (HPIC). HPIEC and HPIC methods were used separately to determinate the succinic acid in DVS. With HPIEC, the sample was diluted with 2. 50 x 10(-3) mol/L sulfuric acid solution and filtrated by 0. 22 µm polyether sulfone filter membrane, and then analyzed by HPIEC directly without any further pretreatment. The analytical column was Phenomenex Rezex ROA-organic Acid H+(8%) (300 mmx7. 8 mm). The mobile phase was 2. 50x10(-3) mol/L sulfuric acid solution at the flow rate of 0. 5 mL/min. The column temperature was set at 40 °C, and the detection wavelength was 210 nm. The injection volume was 10 KL. The assay was quantified by external standard method. With HPIC, the sample was diluted with ultrapure water and filtrated by 0. 22 µm polyether sulfone filter membrane, and then analyzed by HPIC directly without any further pretreatment. The analytical column was Dionex IonPac AS11-HC (250 mm x 4 mm) with a guard column IonPacAG11-HC (50 mm x 4 mm). Isocratic KOH elute generator was used at the flow rate of 1. 0 mL/min. The detection was performed by a Dionex suppressed (DIONEX AERS 500 4-mm) conductivity detector. The injection volume was 10 µL. The content computation was performed with peak area external reference method. The results of HPIEC method for succinic acid were 28. 8%, 28. 9% and 28. 9%, while the results of HPIEC method were 28. 2%, 28. 6% and 28. 6%. The results of HPIEC and HPIC methods were not significantly different. The two methods can both be used to determine the contents of succinic acid in DVS. The surveillance analytical method should be chosen according to the situation. PMID:27382725

  20. 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.

  1. 离子色谱法与传统方法测定水体中阴离子的比较%A Comparison between Ion Chromatography and Traditional Method for Determining the Water.Body Anion

    Institute of Scientific and Technical Information of China (English)

    陈舰; 吴亚榕

    2011-01-01

    采用美国戴安ICS-900型离子色谱仪,一次进样同时分析了湖水中F-、Cl-、NO3-、SO4^2-等离子,并与其常规的检测方法进行了比较。结果表明离子色谱法测定相关性指标良好.方法比对结果基本一致.无显著性差异。离子色谱仪的发展为离子色谱在各行业的应用带来了更加广阔的空间,尤其是快速检验测能力对于环境监测有着重要的意义。%The Dionex ICS- 900 ion chromatography was used to analyze the F- , Cl , NO3- ,SO4^2- Anion in the water of the lake in once sample injection instead of conventional detection methods, and the results show that the ion chromatography deter- mination has good correlation index, the results are basically the same way as the conventional methods with no significant differ- ences. Ion chromatography development for the application of ion chromatography in industries has brought more extensive space, especially fast inspection abilities for environmental monitoring has important significance.

  2. Human kidney anion exchanger 1 interacts with adaptor-related protein complex 1 {mu}1A (AP-1 mu1A)

    Energy Technology Data Exchange (ETDEWEB)

    Sawasdee, Nunghathai; Junking, Mutita [Division of Medical Molecular Biology and BIOTEC-Medical Biotechnology Unit, Department of Research and Development, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Ngaojanlar, Piengpaga [Division of Medical Molecular Biology and BIOTEC-Medical Biotechnology Unit, Department of Research and Development, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Department of Immunology and Graduate Program in Immunology, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Sukomon, Nattakan; Ungsupravate, Duangporn [Division of Medical Molecular Biology and BIOTEC-Medical Biotechnology Unit, Department of Research and Development, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Limjindaporn, Thawornchai [Division of Medical Molecular Biology and BIOTEC-Medical Biotechnology Unit, Department of Research and Development, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Department of Anatomy, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Akkarapatumwong, Varaporn [Institute of Molecular Biosciences, Mahidol University at Salaya Campus, Nakorn Pathom 73170 (Thailand); Noisakran, Sansanee [Division of Medical Molecular Biology and BIOTEC-Medical Biotechnology Unit, Department of Research and Development, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand); Yenchitsomanus, Pa-thai, E-mail: grpye@mahidol.ac.th [Division of Medical Molecular Biology and BIOTEC-Medical Biotechnology Unit, Department of Research and Development, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700 (Thailand)

    2010-10-08

    Research highlights: {yields} Trafficking defect of kAE1 is a cause of dRTA but trafficking pathway of kAE1 has not been clearly described. {yields} Adaptor-related protein complex 1 {mu}1A (AP-1 mu1A) was firstly reported to interact with kAE1. {yields} The interacting site for AP-1 mu1A on Ct-kAE1 was found to be Y904DEV907, a subset of YXXO motif. {yields} AP-1 mu1A knockdown showed a marked reduction of kAE1 on the cell membrane and its accumulation in endoplasmic reticulum. {yields} AP-1 mu1A has a critical role in kAE1 trafficking to the plasma membrane. -- Abstract: Kidney anion exchanger 1 (kAE1) mediates chloride (Cl{sup -}) and bicarbonate (HCO{sub 3}{sup -}) exchange at the basolateral membrane of kidney {alpha}-intercalated cells. Impaired trafficking of kAE1 leads to defect of the Cl{sup -}/HCO{sub 3}{sup -} exchange at the basolateral membrane and failure of proton (H{sup +}) secretion at the apical membrane, causing a kidney disease - distal renal tubular acidosis (dRTA). To gain a better insight into kAE1 trafficking, we searched for proteins physically interacting with the C-terminal region of kAE1 (Ct-kAE1), which contains motifs crucial for intracellular trafficking, by a yeast two-hybrid (Y2H) system. An adaptor-related protein complex 1 {mu}1A (AP-1 mu1A) subunit was found to interact with Ct-kAE1. The interaction between either Ct-kAE1 or full-length kAE1 and AP-1 mu1A were confirmed in human embryonic kidney (HEK) 293T by co-immunoprecipitation, affinity co-purification, co-localization, yellow fluorescent protein (YFP)-based protein fragment complementation assay (PCA) and GST pull-down assay. The interacting site for AP-1 mu1A on Ct-kAE1 was found to be Y904DEV907, a subset of YXXO motif. Interestingly, suppression of endogenous AP-1 mu1A in HEK 293T by small interfering RNA (siRNA) decreased membrane localization of kAE1 and increased its intracellular accumulation, suggesting for the first time that AP-1 mu1A is involved in the kAE1

  3. Human kidney anion exchanger 1 interacts with adaptor-related protein complex 1 μ1A (AP-1 mu1A)

    International Nuclear Information System (INIS)

    Research highlights: → Trafficking defect of kAE1 is a cause of dRTA but trafficking pathway of kAE1 has not been clearly described. → Adaptor-related protein complex 1 μ1A (AP-1 mu1A) was firstly reported to interact with kAE1. → The interacting site for AP-1 mu1A on Ct-kAE1 was found to be Y904DEV907, a subset of YXXO motif. → AP-1 mu1A knockdown showed a marked reduction of kAE1 on the cell membrane and its accumulation in endoplasmic reticulum. → AP-1 mu1A has a critical role in kAE1 trafficking to the plasma membrane. -- Abstract: Kidney anion exchanger 1 (kAE1) mediates chloride (Cl-) and bicarbonate (HCO3-) exchange at the basolateral membrane of kidney α-intercalated cells. Impaired trafficking of kAE1 leads to defect of the Cl-/HCO3- exchange at the basolateral membrane and failure of proton (H+) secretion at the apical membrane, causing a kidney disease - distal renal tubular acidosis (dRTA). To gain a better insight into kAE1 trafficking, we searched for proteins physically interacting with the C-terminal region of kAE1 (Ct-kAE1), which contains motifs crucial for intracellular trafficking, by a yeast two-hybrid (Y2H) system. An adaptor-related protein complex 1 μ1A (AP-1 mu1A) subunit was found to interact with Ct-kAE1. The interaction between either Ct-kAE1 or full-length kAE1 and AP-1 mu1A were confirmed in human embryonic kidney (HEK) 293T by co-immunoprecipitation, affinity co-purification, co-localization, yellow fluorescent protein (YFP)-based protein fragment complementation assay (PCA) and GST pull-down assay. The interacting site for AP-1 mu1A on Ct-kAE1 was found to be Y904DEV907, a subset of YXXO motif. Interestingly, suppression of endogenous AP-1 mu1A in HEK 293T by small interfering RNA (siRNA) decreased membrane localization of kAE1 and increased its intracellular accumulation, suggesting for the first time that AP-1 mu1A is involved in the kAE1 trafficking of kidney α-intercalated cells.

  4. Adsorption and desorption kinetics of bovine serum albumin in ion exchange and hydrophobic interaction chromatography on silica matrices.

    Science.gov (United States)

    Conder; Hayek

    2000-12-01

    Large scale chromatographic separation of proteins can be carried out more rapidly on rigid adsorbents than on soft gel media. The kinetics of adsorption of bovine serum albumin (BSA) have been studied on rigid adsorbents based on a wide-pore, hydrophilically-coated silica gel matrix in a packed bed (chromatographic column). Process parameters have been varied comprehensively. The effects of surface chemistry (weak anion exchanger and hydrophobic interaction), particle size and liquid flow velocity have been studied on both the adsorption and desorption processes. The relative influences of the adsorption kinetics and equilibrium isotherm on the shape of the breakthrough curve are found to vary with the process parameters in an interpretable and therefore, predictable manner. Pore diffusion resistance is dominant over the external liquid film resistance in controlling the adsorption kinetics, with Biot numbers in the range 170-2600. A two-step model based on these two resistances simulates the breakthrough curves with only limited quantitative accuracy, but gives good predictions of the effect of changes in process parameters. PMID:11080653

  5. Preparation of new hybrid organic/inorganic polymeric chiral stationary phases for ligand-exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Three new hybrid organic/inorganic polymeric ligand-exchange chiral stationary phases were developed by radical chain transfer reaction and surface grafting on silica gel, and successfully used for the enantioseparations of DL-amino acids and DL-hydroxyl acids. The resolutions were achieved by using water containing 2.0 × 10-4 mol/L of CuAc2 as a mobile phase, column temperature of 40 ℃, flow rate of 1.0 mL/min and detection at UV 254 mn. The elution order of D-isomer before L-isomer was observed for all DL-amino acids resolved except DL-Pro.

  6. Classification of the geographical origin of Italian donkey milk based on differences in inorganic anions

    OpenAIRE

    Di Bella, Giuseppa; Lo Turco, Vincenzo; Potortì, Angela Giorgia; Luppino, Rosario Rocco; Fotia, Vincenzo; Conte, Francesca; Dugo, Giacomo

    2012-01-01

    Abstract In this work the content of chlorides, nitrites, nitrates, phosphates and sulphates were used to classify 45 donkey milk samples collected from different Italian regions. An ion exchange chromatography with conductivity detector and chemical suppression method was used. The quantitative results indicate phosphates (569.39-1304.40 mg kg-1) and chlorides (545.93-1757.89 mg kg-1) that as the most abundant anions, followed by and sulphates (109.52-200.69 mg kg-1). The concentr...

  7. Adsorption properties of glyphosate onto 330 anion exchange resin%330阴离子交换树脂对草甘膦的吸附性能

    Institute of Scientific and Technical Information of China (English)

    肖谷清; 龙立平; 何露; 余婷; 钟桐生

    2011-01-01

    采用静态吸附法研究了330阴离子交换树脂对水中草甘膦的吸附性能,并研究了吸附动力学;测定了溶液的pH值、温度、NaCl含量等因素对330树脂吸附草甘膦的影响.结果表明:330树脂对水中草甘膦的吸附速率快;在pH=2.69时对草甘膦的吸附性能最好;330树脂对草甘膦的吸附是放热、自发的过程,吸附等温线符合Freundlich方程;NaCl含量对330树脂吸附草甘膦有显著影响.%The objective of this work was to study the adsorption properties of glyphosate onto 330 anion exchange resin by static adsorption.The adsorption kinetics of glyphosate onto 330 resin was measured.The study focused on the effects of the solution pH, temperature and NaCl on the adsorption of glyphosate onto 330 resin.The results showed that adsorption rate of glyphosate onto 330 resin was fast.The adsorption at the solution pH of 2.69 was the most efficient for 330 resin.Heat was discharged during the adsorption and the adsorption occurred automatically.It was found that the adsorption isotherms were ? tted to Freundlich models.NaCl is one of the most important factors influencing the adsorption of glyphosate onto 330 resin.

  8. 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.

  9. Quantification of melamine in human urine using cation-exchange based high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Panuwet, Parinya; Nguyen, Johnny V; Wade, Erin L; D'Souza, Priya E; Ryan, P Barry; Barr, Dana Boyd

    2012-03-01

    Melamine and cyanuric acid have been implicated as adulterants in baby formula in China and pet foods in North America. In China, the effect of melamine or melamine-cyanuric acid adulteration lead to kidney stone development and acute renal failure in thousands of Chinese infants. A selective and sensitive analytical method was developed to measure melamine in human urine in order to evaluate the extent of potential health implications resulting from the consumption of these types of adulterated products in the general US population. This method involves extracting melamine from human urine using cation-exchange solid-phase extraction, chromatographically separating it from its urinary matrix co-extractants on a silica-based, strong-cation exchange analytical column using high performance liquid chromatography, and analysis using positive mode electrospray ionization tandem mass spectrometry. Quantification was performed using modified, matrix-based isotope dilution calibration covering the concentration range of 0.50-100 ng/mL. The limit of detection, calculated using replicates of blank and low level spiked samples, was 0.66 ng/mL and the relative standard deviations were between 6.89 and 14.9%. The relative recovery of melamine was 101-106%. This method was tested for viability by analyzing samples collected from the general US population. Melamine was detected in 76% of the samples tested, with a geometric mean of 2.37 ng/mL, indicating that this method is suitable for reliably detecting background exposures to melamine or other chemicals from which it can be derived. PMID:22309774

  10. Advance chromatin extraction enhances performance and productivity of cation exchange chromatography-based capture of Immunoglobulin G monoclonal antibodies.

    Science.gov (United States)

    Nian, Rui; Gagnon, Pete

    2016-07-01

    The impact of host cell-derived chromatin was investigated on the performance and productivity of cation exchange chromatography as a method for capture-purification of an IgG monoclonal antibody. Cell culture supernatant was prepared for loading by titration to pH 6.0, dilution with water to a conductivity of 4mS/cm, then microfiltration to remove solids. DNA content was reduced 99% to 30ppm, histone host cell protein content by 76% to 6300ppm, non-histone host cell protein content by 15% to 321,000ppm, and aggregates from 33% to 15%. IgG recovery was 83%. An alternative preparation was performed, adding octanoic acid, allantoin, and electropositive particles to the harvest at pH 5.3, then removing solids. DNA content was reduced to<1 ppb, histones became undetectable, non-histones were reduced to 24,000ppm, and aggregates were reduced to 2.4%. IgG recovery was 95%. This treatment increased dynamic capacity (DBC) of cation exchange capture to 173g/L and enabled the column to reduce non-histone host proteins to 671ppm. Step recovery was 99%. A single multimodal polishing step further reduced them to 15ppm and aggregates to <0.1%. Overall process recovery was 89%. Productivity at feed stream IgG concentrations of 5-10g/L was roughly double the productivity of a same-size protein A column with a DBC of 55g/L. PMID:27247214

  11. 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

  12. The many ways of making anionic clays

    Indian Academy of Sciences (India)

    Michael Rajamathi; Grace S Thomas; P Vishnu Kamath

    2001-10-01

    Together with hydrotalcite-like layered double hydroxides, bivalent and trivalent metal hydroxides and their hydroxy salts are actually anionic clays consisting of positively charged hydroxide layers with anions intercalated in the interlayer region. The anionic clays exhibit anion sorption, anion diffusion and exchange properties together with surface basicity making them materials of importance for many modern applications. In this article, we discuss many different ways of making anionic clays and compare and contrast the rich diversity of this class of materials with the better-known cationic clays.

  13. 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. PMID:22748375

  14. 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.

  15. Quantitation of sulfate and thiosulfate in clinical samples by ion chromatography.

    Science.gov (United States)

    Cole, D E; Evrovski, J

    1997-11-21

    For assay of serum sulfate, quantitation by ion conductimetry after separation by anion-exchange chromatography is the method of choice. In comparison to classical barium precipitation methods, chromatographic methods demonstrate increased precision, specificity and sensitivity, and they may be superior to spectrophotometric methods that rely on organic cation precipitation of sulfate. The increased sensitivity and specificity, as well as the inherent capacity of chromatographic methods for simultaneous determination of other anions, has led to its increasing use in the determination of excreted sulfate in clinical profiles of urinary anion composition. Ion chromatography can also be used to quantitate free sulfate in other clinical samples, including cerebrospinal fluid, sweat, saliva, breast milk and human tissues. Finally, ion chromatography shows promise as a more precise and sensitive method for measurement of total acid-labile sulfoesters and thiosulfate.

  16. In situ modification of chromatography adsorbents using cold atmospheric pressure plasmas

    Science.gov (United States)

    Olszewski, P.; Willett, T. C.; Theodosiou, E.; Thomas, O. R. T.; Walsh, J. L.

    2013-05-01

    Efficient manufacturing of increasingly sophisticated biopharmaceuticals requires the development of new breeds of chromatographic materials featuring two or more layers, with each layer affording different functions. This letter reports the in situ modification of a commercial beaded anion exchange adsorbent using atmospheric pressure plasma generated within gas bubbles. The results show that exposure to He-O2 plasma in this way yields significant reductions in the surface binding of plasmid DNA to the adsorbent exterior, with minimal loss of core protein binding capacity; thus, a bi-layered chromatography material exhibiting both size excluding and anion exchange functionalities within the same bead is produced.

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

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    2000-01-01

    The selenium species selenite, selenate and selenomethionine were separated in aqueous solution by ion chromatography. The separation was performed on an IonPac AG11 in series with an AS11 anion exchange column by elution with 25 mM sodium hydroxide in 2% methanol. The Se-78 and Se-82 isotopes were...

  18. 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

  19. Determination of Fructooligosaccharides in Milk and Milk Products by High Performance Ion Exchange Chromatography%高效离子色谱法测定乳及乳制品中低聚果糖含量

    Institute of Scientific and Technical Information of China (English)

    刘玉峰; 李东; 唐华澄; 张绩觅

    2012-01-01

    An analytical method was established to determine fructooligosaccharides (FOS) in milk and milk products by high performance ion exchange chromatography method with pulsed amperometric detection. The column was a CarboPac PAl (4 mm x 250 mm) anion exchange column. Fructooligosaccharides were separated under gradient elution mode. The mobile phase A was 150 mmol/L NaOH and the mobile phased B was composed of 150 mmol/L NaOH and 100 mmol/L sodium acetate. The relative standard derivations for 6 replicate determinations of four fructooligosaccharides in liquid milk were less than 9%. The average spike recovery rates for three fructooligosaccharides in liquid milk varied between 94.8% and 103.6%. The method was simple, fast and suitable for determining FOS in milk and milk products.%建立离子色谱法定量测定乳及乳制品中低聚果糖的方法,应用CarboPacTMPA1(4mm×250mm)阴离子交换柱、氢氧化钠和醋酸钠淋洗液梯度淋洗、脉冲安培检测器检测。6次测定液态奶中低聚果糖的含量,相对标准偏差小于9%,3种糖的加标回收率在94.8%~103.6%之间。本方法简单快捷,适用于乳及乳制品中低聚果糖含量的检测。

  20. 电去离子过程中的阴膜降解及其对水解离的影响%Degradation of anion exchange membrane and its influences on water decomposition in electrodeionization process

    Institute of Scientific and Technical Information of China (English)

    费兆辉; 王建友; 陈维利; 樊改肖

    2012-01-01

    电去离子(EDI)及其衍生过程近年来在脱盐、离子浓缩和化工产品的新颖制备等领域日渐重要,但在离子交换膜“膜-液”界面的水解离这一核心机理研究方面仍有诸多不足.对EDI过程中阴离子交换膜的降解及其对水解离的影响进行了实验研究和总结分析.首先通过对阴离子交换膜的选择透过率、交换容量和电导率的测定,以及红外光谱分析确认了EDI过程中存在季铵型强碱性阴离子膜的部分叔胺化降解行为.进一步通过对EDI过程特征曲线等过程宏观特性的对比研究,证明了季铵型阴离子交换膜的降解对阴离子交换膜“膜-液”界面层的水解离具有催化效应.为EDI过程的进一步优化设计,实现具有可控水解离的电驱动膜过程奠定了良好基础.%In recent years, the electrodeionization (EDI) and some integrated processes derived from EDI play important roles in some fields such as desalination, ion concentrating and chemical synthesis, but it is still needed to explore the mechanism of water decomposition at the membrane-liquid interface of ion-exchange membranes. In this study, the degradation of anion exchange membrane in EDI process and its effects on water decomposition were examined and analyzed through experiments. The phenomenon of partial degradation of the anion exchange membrane from quarternary ammonium to tertiary amine is confirmed through the tests for permselectivity, exchange capacity, conductivity and infrared spectroscopy analysis. Furthermore, based on the investigation on the characteristic curves of the EDI process, it is validated that the weakly basic tertiary amine group has a catalytic effect on the water decomposition at the membrane-solution interface of the anion exchange membrane. The results are helpful for the design and improvement of the EDI and EDI-based electro-membrane processes, so that the water decomposition can be well controlled to achieve some

  1. The poisoning effect of mercury complexes with an anionic exchange membrane used in an electrodialysis process: a Raman study; Etude par spectrometrie Raman de l`empoisonnement d`une membrane echangeuse d`anions, par des complexes mercuriques, au cours d`un procede d`electrodialyse

    Energy Technology Data Exchange (ETDEWEB)

    Chaouki, M.; Huguet, P.; Persin, F.; Bribes, J.L. [Montpellier-2 Univ., 34 (France). Laboratoire des Materiaux et des Pocedes Membrnaires, CNRS UMR 5635

    1998-03-01

    Electrodialysis is a powerful technique for the treatment of many waste acids. However, some important problems can be encountered if poisoning of the ionic exchange membrane occurs. This is the case in the purification and concentration process of hydrochloric acid solutions containing zinc, cadmium or mercury chlorides, because metallic complexes formation gives rise to an important poisoning effect of the membranes used. In this work, the poisoning of an anion exchange membrane, used in an electrodialysis process to purify and reconcentrate an hydrochloric acid solution containing mercury chloride, has been investigated. Raman spectroscopic analysis of the contaminated material, combined with electrodialysis results, are presented and discussed. The stoichiometry of the poisoning mercury complex and its action as a counter ion inside the membrane are determined. Moreover, a strong interaction between the membrane fixed sites and the mercury complex is pointed out. (authors) 11 refs.

  2. 离子色谱法测定标准物质DIANP中的无机阴离子%Determination of Inorganic Anion in Standard Substance DIANP by Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    梁忆; 温晓燕; 张新智; 汪伟; 刘宁; 赵娟

    2011-01-01

    采用离子色谱法对DIANP中无机阴离子NO2-,N3-,N03-,C03-2,SO4-2进行测定.乙腈溶解DI-ANP后,加水萃取无机离子,通过On Guard Ⅱ RP柱,去除DIANP或其分解的有机产物,用氢氧化钾溶液为淋洗液梯度洗脱,流速为1.OmL/min,采用IonPac AS11-HC阴离子色谱柱进行分析.测定结果,5种阴离子相关系数达到0.999以上,相对标准偏差为1.57%~4.30%,N02-,N3-,N03-,SO4-2加标平均回收率为89.3%~98.6%.该方法简便、快速,且结果满意.%A method to determine the content of fifths inorganic anions in DIANP by ion chromatography was established. After added acetonitnle and water, the sample was passed though the On Guard Ⅱ RP column to wipe off DIANP and other organic compound then was determined directly. The separation was performed with KOH as isocratic mobile phase at a flow rate of 1.0mL/min and accomplished with a Dionex IonPac AS11 - HC column. The calibration curve of DIANP was linear, results showed that correlation of frfths anions were higher than 0. 999. The relation standard deviation were 1. 57%~4. 30% , NO2- , N3- , NO3- , SO24- the recoveries were 89. 3% ~ 98. 6% . The method was simple, rapid and satisfaction.

  3. Determination of Sweeteners, Preservatives and Anions in Integrated Alcoholic Beverages by Ion Chromatography%离子色谱法测定配制酒中甜味剂、防腐剂和阴离子

    Institute of Scientific and Technical Information of China (English)

    马国军; 张玲芳

    2013-01-01

    A method was developed for the simultaneous determination of Sodium cyclamate,Acesulfame,saccharin sodium,benzoic acid,sorbic acid,nitrate,sulfate and chloride in integrated alcoholic beverages by ion chromatography (IC).The analytical column was ThermoFisher IonPac AS17-C,Gradient KOH was used as the eluent at a flow rate of 1.0 mL/min.The detection was performed by a suppressed conductive detector.The linear range of the method for Sweeteners,preservatives and anions were 0.1~50 mg/L,the average recoveries were 94.0% ~104.l%.The method has been applied to determine trace Sweeteners,preservatives and anions in integrated alcoholic beverages with satisfactory results.%本文建立了一种用离子色谱-电导检测器测定配制酒中甜蜜素、安赛蜜、糖精钠、山梨酸、苯甲酸、硝酸根、硫酸根和氯离子的方法.以IonPac AS1 7-C色谱柱为分离柱,用KOH梯度洗脱方式使待测组分分离,流速为1 mL/min,抑制电导检测.该方法线性范围0.1~50 mg/L,方法回收率在94.0%到104.1%之间,适合于配制酒中甜味剂、防腐剂和常见无机阴离子的检测.

  4. Determination of rare-earth elements in geological materials by ion-exchange chromatography separation and induction coupled plasma emission spectroscopy

    International Nuclear Information System (INIS)

    A methodology for the analysis of Rare-Earth elements in geological samples has been developed. Ion exchange chromatography for the separation and induction coupled plasma emission spectroscopy for the analysis have been used. The columns with cationic resin were calibrated with radioactive elements. With complexes matrices, the instrument's data must be corrected for the presence of majors elements (CEM) and for the interferences of the Rare-earth elements (CETR). The accuracy and precision are evaluated critically with respect to the convenience and efficiency of this methodology in the analysis of rare-Earth elements i geological samples. (author)

  5. 离子色谱法同时测定湖光岩玛珥湖水中5种阴离子%Simultaneous Determination of Five Kinds of Anions in Huguangyan Maar Lake Water by Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    张兆霞; 李泳

    2016-01-01

    Simultaneous determination of five kinds of anions in Huguangyan Maar Lake water by ion chro-matography was established in this paper.Water samples were filtered by 0.22 μm microporous membrane fil-ter,then five kinds of anions including F- ,Cl- ,NO-2 ,NO-3 ,and SO2 -4 in Huguangyan Maar Lake water were determined quickly and accurately with 1.8 mmol·L-1 Na2 CO3-1.7 mmol·L-1 NaHCO3 mixed solution as a mobile phase,and the flow rate was 1.0 mL·min-1 .Detection results had wide linear range and good linear correlation(R =0.9990 ~0.9995 ),the relative standard deviation(RSD)was below 5%,the average recovery rate was 95.2%~106.5%,and the minimum detection limit was 0.01 ~0.28 μg·mL-1 .This method is sim-ple,rapid,accurate and reliable,and it can be used for simultaneous determination of anions in water.%建立了一种同时测定湖光岩玛珥湖水中5种阴离子的离子色谱分析法。水样经0.22μm 微孔滤膜过滤后直接进样,以1.8 mmol·L-1碳酸钠-1.7 mmol·L-1碳酸氢钠混合溶液为流动相,流速为1.0 mL·min-1,快速准确地同时测定湖光岩玛珥湖水中 F-、Cl-、NO-2、NO-3、SO2-4等5种阴离子。检测结果线性范围广,线性相关性好(R=0.9990~0.9995),相对标准偏差(RSD)均低于5%,平均加标回收率为95.2%~106.5%,最低检测限为0.01~0.28μg·mL-1。该法简便、快速、准确、可靠,可用于水中阴离子的同时测定。

  6. 原料奶中5种阴离子的离子色谱分析%Determination of five kinds of anion in raw milk by ion chromatography

    Institute of Scientific and Technical Information of China (English)

    王庭欣; 张晓瑜; 刘叶婷; 李晓晖

    2012-01-01

    为了建立原料奶中5种阴离子(C1-,NO3 -,H PO42-,SO42-,SCN-)的离子色谱检测方法,将原料奶经乙腈沉淀蛋白质后离心过滤处理进行离子色谱检测.色谱条件,淋洗液:NaHCO3(1.0 mmol/L),Na2CO3 (3.2 mmol/L),体积分数为15%的丙酮超纯水混合液.流速为1.0 mL/min,检测嚣为电导检测器.该方法对5种离子的电导检出限均为0.02 mg/L.在线性范围内r=0.997 6及以上.5种离子的精密度RSD为0.08%~9.58%,各阴离子的回收率均为80%~120%,变异系数在10%以内.该方法具有方便、准确、成本低的优点.%A new method was established for determination of five kinds of anion(Cl ,NQ3- ,HPO42- ,SO42-, SCN- )in raw milk by ion chromatography. The method was adopted with sodium bicarbonate (1.0 mmol/L ) .so dium carbonate(3. 2 mmol/Dand 15% acetone aqueous (volume fraction) as the eluent. The flow rate was 1. 0 mL/min. The detection was performed by a conductivity detection mode. The lowest detection limit of five kinds of anion in raw milk was 0. 02 mg/L. In linear range r-0. 997 6 or above. Precision test RSD was 0. 08% -9. 58%. The recovery rate was in 80% -120% range. The coefficient of variation was in less than 10%. This method is simple, accurate and suitable for the determination of five kinds of anion in raw milk.

  7. Ion chromatography in the manufacture of multilayer circuit boards

    Science.gov (United States)

    Smith, Robert E.

    1990-09-01

    Ion chromatography (IC) has proven useful in analyzing chemical solutions used in the manufacture of multilayer circuit boards. The manufacturing process is described briefly and previously published IC methods are reviewed. Then, methods are described for determining chlorate and chlorite in a brown oxide solution; salicylic acid in an epoxy cure agent; formate, sulfate, and tartrate in an electroless copper bath; anionic detergents in a tin-lead brightener and in a cleaning solution; and aqueous photoresist and nonionic brightener in a tin-lead bath. Anion exchange, reverse phase HPLC on a poly(styrene/divinylbenzene), PS/DVB, column and 2-D liquid chromatography also are described. Chemically suppressed conductivity and photometric detection are used.

  8. Ion Chromatography.

    Science.gov (United States)

    Mulik, James D.; Sawicki, Eugene

    1979-01-01

    Accurate for the analysis of ions in solution, this form of analysis enables the analyst to directly assay many compounds that previously were difficult or impossible to analyze. The method is a combination of the methodologies of ion exchange, liquid chromatography, and conductimetric determination with eluant suppression. (Author/RE)

  9. 离子色谱法测定水中阴离子的质量控制%Quality Control of Determination of Anions in Water by Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    蔡芹

    2011-01-01

    目的 为消除和减小离子色谱法测定水中阴离子(Cl-)的实验误差,保证测量结果的准确性和可比性.方法 选用Metrosep A SUPP 4(4.0mm×250 mm)阴离子色谱柱,1.7 mmol/L Na2HCO3和1.8 mmol/L Na2CO3淋洗液为流动相,流速为1.0 ml/min,抑制型电导检测器,经0.45.μm滤膜过滤后,进样检测.结果 测得Cl-在5.0 ~100 mg/L范围内线性关系好,相关系数r=0.9997,加标回收率为98.4%~101.0%,RSD在0.000 9% ~0.002 9%间,对水中4种阴离子F-、Cl-、NO3 -、SO42-同时分析,相关系数均大于0.9990;具有良好的准确度和精密度.结论 经过实施全面有效的质量控制措施,Cl获得满意结果,在实际工作应用中,能较好地监控农村饮用水中阴离子的分布动态.%[ Objective ] To eliminate and reduce the error of the ion chromatography method for determination of anion, and guarantee the accuracy of the measurement results and comparability. [ Methods ] The methods was based on the detection through the inhibited type electric conductivity detector under the condition of eluent with 1.7 mmol/L NaHCO3 and 1.8 mmol/L Na2CO3 as mobile phase and flow rate 1. 0ml/min, filtering through the 0. 45 μm membrane filter by using of the Metrosep A SUPP 4(4. 0x 250 mm) Anionic chromatography column. [Results]This method had a good relativity (r = 0.999 7), and the Cl"curve showed good linearity in the range of 5.0 - 100 mg/L. The recoveries was between 98.4% ~ 101% .RSDwas between 0. 000 9% -0. 002 9% , and the correlation coefficient was greater than 0.999 by analyzing the F- , Cl- , NO3-, and SO42- in water, and the detection method had good accuracy and precision. [ Conclusion ] After the implementation of the comprehensive and effective quality control measures, Cl shows satisfactory results, during the actual work application, the distribution of anion dynamic in rural drinking water can be monitored well.

  10. Speciation of selenoamino acids, selenonium ions and inorganic selenium by ion exchange HPLC with mass spectrometric detection and its application to yeast and algae

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Hansen, M.; Fan, T.;

    2001-01-01

    Cation and anion exchange HPLC were used to separate a mixture of 12 selenium species comprising selenoamino acids, selenonium ions and inorganic selenium. The cationic species were separated from each other and from the co-injected anions using a cation exchange column with gradient elution...... by aqueous pyridinium formate at pH similar to 3 as the mobile phase. The anionic species were separated using an anion exchange column with isocratic elution by an aqueous salicylate-TRIS mobile phase at pH 8.5. The separated selenium species were detected as Se-80 by ICP-dynamic reaction cell (DRC...... acid extract of Chlorella algae contained dimethylselenonium propionate (DMSeP), which was verified by HPLC-ES-MS. Se-allylselenocysteine and selenoethionine was detected at the low ng g(-1) concentration level based on co-chromatography with the standard substances spiked to the algal extract....

  11. 离子色谱法同时测定蔬菜中6种阴离子的含量%Simultaneous determination of six anions in vegetables by ion chromatography

    Institute of Scientific and Technical Information of China (English)

    贾宏新; 李文杰; 王树诚

    2011-01-01

    Objective:To develop a method with ion chromatography to simultaneously determine six anions in vegetables.Methods: The six anions in samples were extracted by ultrasound and separated by an lonpac AS 23 column (250 mm × 4 mm i.d. ) with lonpac AG23 and 3.5 mM Na2CO3/1.0 mM NaHCO3 as eluent. The flow rate was 1.0 ml/min. Anions were detected by suppressed conductivity detection. Results: The linearity of F-, Cl-, NO2- , NO3- , PO34- , SO42- were good in the range of 0.1 mg/L ~ 10.0 mg/L, 1.0 mg/L ~ 20.0 mg/L,O. 1 mg/L ~ 10.0 mg/L, 1.0 mg/L ~ 50.0 mg/L, 1.0 mg/L ~ 50.0 mg/L,1.0 mg/L ~ 50.0 mg/L. The recovery of the method was 92.0% ~ 107.2% and relative standard deviation (RSD) was < 5%.The detection limit were F- :0.6 mg/kg;Cl- :7.0 mg/kg; NO2-: 0.6 mg/kg; NO3-: 7.0 mg/kg; PO43-: 7.0 mg/kg; SO42-:7.0 mg/kg. Conclusion: The method was accurate, sensitive, simple and it can be applied for inspection of F- ,Cl-, NO2-,NO3-, PO43-, SO42- in vegetable, which simultaneously and completely separated all anions in 30 minutes.%目的:建立蔬菜中6种无机阴离子含量的测定方法.方法:样品用超声提取,离子色谱法同时测定氟、氯、亚硝酸盐、硝酸盐、磷酸盐、硫酸盐.色谱柱为:Ionpac AS23阴离子交换色谱柱(250 mm x4 mm i.d.)和lonpac AG23保护柱;淋洗液为:3.5 mM NaCO/1.0 mM NaHCO;流速为:1.0 ml/min;检测方式为:抑制型电导检测.结果:F、NO在0.1 mg/L~10.0 mg/L,CI在1.0 mg/L~20.0 mg/L,NO、PO、SO在1.0 mg/L~50.0 mg/L范围内线性良好,回收率在92.0%~107.2%之间,相对标准偏差均小于5%,检出限分别为F:0.6 mg/kg;Cl:7.0 mg/kg;NO:0.6 mg/kg;NO:7.0 mg/kg;PO:7.0 mg/kg;SO:7.0 mg/kg.结论:本方法准确、灵敏、操作简便,一次进样30 min内完全分离,适用于蔬菜中6种无机阴离子含量的日常监测工作.

  12. Determination of nitric oxide metabolites, nitrate and nitrite, in Anopheles culicifacies mosquito midgut and haemolymph by anion exchange high-performance liquid chromatography: plausible mechanism of refractoriness

    OpenAIRE

    Adak Tridibesh; Raghavendra Kamaraju; Sharma Arun; Dash Aditya P

    2008-01-01

    Abstract Background The diverse physiological and pathological role of nitric oxide in innate immune defenses against many intra and extracellular pathogens, have led to the development of various methods for determining nitric oxide (NO) synthesis. NO metabolites, nitrite (NO2-) and nitrate (NO3-) are produced by the action of an inducible Anopheles culicifacies NO synthase (AcNOS) in mosquito mid-guts and may be central to anti-parasitic arsenal of these mosquitoes. Method While exploring a...

  13. Mitigation of chromatography adsorbent lot performance variability through control of buffer solution design space.

    Science.gov (United States)

    Aono, Hiromasa; Iliescu, Ionela; Cecchini, Doug; Wood, Susanne; McCue, Justin T

    2013-11-29

    The separation of undesired product-related impurities often poses a challenge in the purification of protein therapeutic species. Product-related impurity species, which may consist of undesirable isoforms, aggregated, or misfolded variants of the desired monomeric form of the product, can be challenging to remove using preparatory scale chromatographic techniques. When using anion exchange chromatography to remove undesirable product-related impurities, the separation can be highly sensitive to relatively small changes in the chromatography operating conditions, including changes to buffer solution pH, buffer solution conductivity protein loading, and operating temperature. When performing difficult separations, slight changes to the chemical and physical properties of the anion exchange adsorbent lot may also impact the separation profile. Such lot-to-lot variability may not be readily measurable by the adsorbent manufacturer, since variability can be highly dependent on a specific protein separation. Consequently, manufacturers of chromatographic adsorbents may not be able to control adsorbent lot to lot variability tightly enough to prevent differences from occurring when performing difficult product-related separations at the preparatory scale. In such cases, it is desirable to design a chromatography step with a control strategy which accounts for adsorbent lot to lot variability in the separation performance. In order to avoid the undesired changes to process consistency and product quality, a proper adjustment of the column operating conditions can be implemented, based on the performance of each adsorbent lot or lot mixture. In this work, we describe how the adjustment of the column buffer solution composition can be used as a design space based-control strategy used to ensure consistent process performance and product quality are achieved for an anion exchange chromatography step susceptible to adsorbent lot to lot performance variability. In addition, a

  14. New inorganic (an)ion exchangers based on Mg–Al hydrous oxides: (Alkoxide-free) sol–gel synthesis and characterisation

    NARCIS (Netherlands)

    Chubar, N.

    2011-01-01

    New inorganic ion exchangers based on double Mg–Al hydrous oxides were generated via the new non-traditional sol–gel synthesis method which avoids using metal alkoxides as raw materials. Surface chemical and adsorptive properties of the final products were controlled by several ways of hydrogels and

  15. 离子色谱法同时测定感冒清热颗粒中9种无机阴离子%Determination of 9 Inorganic Anions in Ganmao Qingre Granules by Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    周伟娥; 杨立佼; 谢巍; 蒋受军

    2015-01-01

    OBJECTIVE:To establish the ion chromatography for the mass fractions of 9 inorganic anions (fluoride ion,for-mate radical,chloride ion,nitrite radical,bromide ion,nitrate radical,sulfate radical,oxalate radical and phosphate radical) in Ganmao qingre granules. METHODS:Ion chromatograph was used. The column was Ion Pac AS11-HC with the mobile phase of po-tassium hydroxide solution by gradient elution(concentration:30 mmol/L,time:15 min),the column temperature was room tem-perature,the volume was 25 μl. RESULTS:The 9 inorganic anions were basically achieved separation and had good linear relation-ship with r of 0.999 2-0.999 9,respectively;RSDs of precision,stability and reproducibility tests were less than 3.50%. Average re-covery was 92.47%-103.51%(RSD=0.42%-3.41%,n=6),respectively. CONCLUSIONS:The established method is fast,accu-rate,sensitive and repeatable and can be used for the determination of 9 inorganic anions in Ganmao qingre granules.%目的:建立同时测定感冒清热颗粒中9种无机阴离子(氟离子、甲酸根、氯离子、亚硝酸根、溴离子、硝酸根、硫酸根、草酸根和磷酸根)含量的方法。方法:采用离子色谱法。色谱柱为Ion Pac AS11-HC,流动相为氢氧化钾溶液,等度洗脱(洗脱浓度30 mmol/L,洗脱时间15 min),柱温为室温,进样量为25μl。结果:9种无机阴离子基本达到分离,线性关系良好,相关系数分别在0.9992~0.9999范围内;精密度、稳定性、重复性试验的RSD<3.50%;平均加样回收率分别在92.47%~103.51%范围内,RSD分别在0.42%~3.41%范围内(n=6)。结论:本方法快速、准确、灵敏、重复性好,可用于感冒清热颗粒中9种无机阴离子的测定。

  16. High Performance of Alkaline Anion-Exchange Membranes Based on Chitosan/Poly (vinyl) Alcohol Doped with Graphene Oxide for the Electrooxidation of Primary Alcohols

    OpenAIRE

    García Cruz, Leticia; Casado-Coterillo, Clara; Irabien, Ángel; Montiel Leguey, Vicente; Iniesta Valcárcel, Jesús

    2016-01-01

    Mixed matrix membranes (MMM) based on chitosan (CS) and poly (vinyl) alcohol (PVA) with a 50:50 w/w ratio doped with graphene oxide (GO) are prepared by solution casting and characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), water uptake, alcohol permeability, ion exchange capacity (IEC) and OH− conductivity measurements. The SEM analysis revealed a dense MMM where the GO nanosheets were well dispersed over the entire polymer matrix...

  17. Non-ionic surfactant modified ligand exchange chromatography using copper (II) complex of N,N-dimethyl-L-phenylalanine as the chiral additive for enantioselective amino acids separation.

    Science.gov (United States)

    Dimitrova, Pepa; Bart, Hans-Jörg

    2010-03-17

    The influence of non-ionic surfactants on the selectivity and retention in the ligand exchange chromatography for the enantioselective separation of racemic mixtures of the amino acids dl-methionine, dl-leucine, dl-valine and dl-tyrosine applying chiral mobile phases was investigated, whereas five different surfactants were tested as modifiers. The experiments were carried out using a commercially available non-chiral RP-C8 column and the copper (II) complex of N,N-dimethyl-l-phenylalanine as the chiral additive. Varying the surfactant concentrations the retention factors and the selectivity could be controlled and in general no negative influence on the separation (due to surfactant adsorption on the non-chiral stationary phase) occurred. Changing the temperature the van't Hoff plots were obtained and the thermodynamic parameters calculated. Temperature had influence on the selectivity for each surfactant and lowered the retention times as expected.

  18. Non-ionic surfactant modified ligand exchange chromatography using copper (II) complex of N,N-dimethyl-L-phenylalanine as the chiral additive for enantioselective amino acids separation

    Energy Technology Data Exchange (ETDEWEB)

    Dimitrova, Pepa [TU Kaiserslautern, Institut fuer Thermische Verfahrenstechnik, P.O. Box 3049, Gottlieb-Daimler-Str. 44, 67653 Kaiserslautern (Germany); Bart, Hans-Joerg, E-mail: bart@mv.uni-kl.de [TU Kaiserslautern, Institut fuer Thermische Verfahrenstechnik, P.O. Box 3049, Gottlieb-Daimler-Str. 44, 67653 Kaiserslautern (Germany)

    2010-03-17

    The influence of non-ionic surfactants on the selectivity and retention in the ligand exchange chromatography for the enantioselective separation of racemic mixtures of the amino acids DL-methionine, DL-leucine, DL-valine and DL-tyrosine applying chiral mobile phases was investigated, whereas five different surfactants were tested as modifiers. The experiments were carried out using a commercially available non-chiral RP-C8 column and the copper (II) complex of N,N-dimethyl-L-phenylalanine as the chiral additive. Varying the surfactant concentrations the retention factors and the selectivity could be controlled and in general no negative influence on the separation (due to surfactant adsorption on the non-chiral stationary phase) occurred. Changing the temperature the van't Hoff plots were obtained and the thermodynamic parameters calculated. Temperature had influence on the selectivity for each surfactant and lowered the retention times as expected.

  19. Ultrafiltration Membrane Fouling and the Effect of Ion Exchange Resins

    KAUST Repository

    Jamaly, Sanaa

    2011-12-01

    Membrane fouling is a challenging process for the ultrafiltration membrane during wastewater treatment. This research paper determines the organic character of foulants of different kinds of wastewater before and after adding some ion exchange resins. Two advanced organic characterization methods are compared in terms of concentration of dissolved organic carbons: The liquid chromatography with organic carbon (LC-OCD) and Shimadzu total organic carbon (TOC). In this study, two secondary wastewater effluents were treated using ultrafiltration membrane. To reduce fouling, pretreatment using some adsorbents were used in the study. Six ion exchange resins out of twenty were chosen to compare the effect of adsorbents on fouling membrane. Based on the percent of dissolved organic carbon’s removal, three adsorbents were determined to be the most efficient (DOWEX Marathon 11 anion exchange resin, DOWEX Optipore SD2 polymeric adsorbent, and DOWEX PSR2 anion exchange), and three other ones were determined to the least efficient (DOWEX Marathon A2 anion exchange resin, DOWEX SAR anion exchange resin, and DOWEX Optipore L493 polymeric adsorbent). Organic characterization for feed, permeate, and backwash samples were tested using LC-OCD and TOC to better understand the characteristics of foulants to prevent ultrafiltration membrane fouling. The results suggested that the polymeric ion exchange resin, DOWEX SD2, reduced fouling potential for both treated wastewaters. All the six ion exchange resins removed more humic fraction than other organic fractions in different percent, so this fraction is not the main for cause for UF membrane fouling. The fouling of colloids was tested before and after adding calcium. There is a severe fouling after adding Ca2+ to effluent colloids.

  20. Removal of Evans Blue and Yellow thiazole dyes from aqueous solution by Mg-Al-CO3 Layered Double Hydroxides as anion-exchanger

    Directory of Open Access Journals (Sweden)

    Mohamed Bouraada

    2014-06-01

    Full Text Available Mg-Al-CO3 Layered double hydroxide (LDH was prepared by co-precipitation method at constant pH, and subsequently used to remove Evans Blue (EB and Yellow thiazole (YT dyes from aqueous solutions. The obtained material was characterized by powder X-ray diffraction (PXRD, Fourier transform infrared spectroscopy (FTIR, thermal analysis and BET. The kinetic and equilibrium aspects of sorption of the anionic dyes from aqueous solution by Mg-Al-CO3 were investigated in batch mode. The sorption kinetic data were found to be consistent with the pseudo-second-order model. Data for YT and EB sorption by Mg-Al-CO3 were fitted better by the Langmuir equation than by the Freundlich equation based on the determination coefficient values R2 . The maximum adsorption capacities of 222.2 mgg-1 for Yellow thiazole and 107.5 mgg-1 for Evans blue. The thermodynamic parameters including Gibbs free energy (G°, standard enthalpy change (H°, and standard entropy change (S° for the process were calculated. The negative G° value indicates the spontaneity of the removal process.

  1. 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.

  2. Isolation and purification of uremic middle molecules by multi-step liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    储结根; 刘晓航; 袁直; 何炳林

    2002-01-01

    Isolation and comparison of uremic sera and urine and normal sera and urine were performed by gel permeation chromatography, anion exchange chromatography and reversed-phase high performance liquid chromatography. Two uremic middle molecular fractions (A and B) were obtained from uremic sera and urine and normal urine by gel permeation chromatography, but not from normal sera. The anion exchange chromatographic results of fraction A from different origins demonstrate that subfraction A-3 could be excreted in urine by healthy subject, but accumulated in uremic serum for renal failure of patient with uremia. After desalinization subfraction A-3 was analyzed by MALDI-TOF-MS. The results show that subfraction A-3 consists of six compounds with molecular weight 839, 873, 1007.94, 1106, 1680 and 2015 respectively. Finally, by reversed-phase high performance liquid chromatography, subfraction A-3 was further resolved into six independent fractions. Thus, the isolation and purification of six middle molecular compounds in subfraction A-3 came true by our method.

  3. 布洛芬在阴离子交换树脂上的负载及其缓释%LOADING AND SUSTAINED RELEASE OF IBUPROFEN IN ANION EXCHANGE RESINS

    Institute of Scientific and Technical Information of China (English)

    张月恒; 阙茝璐; 张更辉; 阎虎生

    2012-01-01

    将布洛芬通过静电和疏水作用的共同作用负载于聚苯乙烯型大孔弱碱性阴离子交换树脂D301R和D301T上,最佳负载条件为:布洛芬悬浮于5~10%的乙醇水溶液中,加入树脂后在60℃下搅拌12h,负载量可达到0.49g/g树脂.研究了负载的布洛芬在模拟胃肠道的条件下(pH2下2h、pH 7.4下4h和pH 6.7下18h)的释放动力学,在前12h的释放接近于线性释放,释放率为58~60%.后12h的释放量较小,释放率为13~17%.如果每12h服药1次,第2次服药后的24h的累加释放率接近于线性释放.与聚苯乙烯骨架的大孔弱碱性阴离子交换树脂相比,聚甲基丙烯酸酯骨架的弱碱性阴离子交换树脂(甲基丙烯酸正丁酯/甲基丙烯酸N,N-二甲胺基乙酯/双甲基丙烯酸乙二醇酯共聚物)负载的布洛芬在相同释放条件下突释明显,表明布洛芬与苯乙烯型弱碱性阴离子交换树脂之间的π-π作用在布洛芬的缓释中起关键的作用.%Ibuprofen was loaded into polystyrene-based macroporous weakly basic anion exchange resins, D301R and D301T. The loading was driven by electrostatic and hydrophobic interactions. The optimized loading condition was: a suspension of the resin in 5~10% ethanol aqueous solution with dispersed ibuprofen was stirred for 12h at 60℃. The loading capacity could be up to 0.49g/g resin. The release of the loaded ibuprofen in buffer mimicking gastrointestinal Ph environments (2h, 4h and 18h at Ph 2, 7.4 and 6.7, respectively) was studied. The loaded ibuprofen was released almost linearly against time in the first 12h with release percentage of 58~60%. The release percentage in the followed 12h was quite low, being 13-17%. In simulated administrations taken at 12h interval, the loaded ibuprofen in D301R was released almost linearly against time during a 24h period after the second administration. In contrast, an initial burst release of the loaded ibuprofen in a polymethacrylate-based weakly basic anion

  4. Device to generate high purity hydroxide solution in-line for ion chromatography.

    Science.gov (United States)

    Masunaga, Hiroto; Higo, Yuji; Ishii, Mizuo; Maruyama, Noboru; Yamazaki, Shigeo

    2016-05-01

    Herein, we report a new device that generates a high-purity hydroxide solution in line. The device's container has three compartments that are isolated from each other by two cation exchange (CE) membranes. In each end of the container, an electrode is installed. The three compartments are filled with ion exchange resins. A bipolar boundary is a composite boundary comprising anion- and cation-exchangers. This device has two bipolar boundaries, which are used to separate the location of hydroxide solution generation from the location where water is electrolyzed. Therefore, it can produce high-purity hydroxide solutions that are free from gases and anionic impurities. The hydroxide solution is generated on the basis of an electrokinetic phenomenon at the surfaces of ion-exchange resins and membranes in an electric field; NaOH concentration can be controlled at rates from 0.01 to 100mM per 1mL/min by adjusting the electrical current (0-200mA) applied to the device. As the generated solution is used as an eluent for a suppressed anion chromatography, the electrical conductivity of the effluent from the suppressor is as low as that of ultra-pure water. Thus, the noise of the base-line electrical conductivity is improved, and so the detection limit of anions on the sub-ng/mL order can be achieved. PMID:27063368

  5. Device to generate high purity hydroxide solution in-line for ion chromatography.

    Science.gov (United States)

    Masunaga, Hiroto; Higo, Yuji; Ishii, Mizuo; Maruyama, Noboru; Yamazaki, Shigeo

    2016-05-01

    Herein, we report a new device that generates a high-purity hydroxide solution in line. The device's container has three compartments that are isolated from each other by two cation exchange (CE) membranes. In each end of the container, an electrode is installed. The three compartments are filled with ion exchange resins. A bipolar boundary is a composite boundary comprising anion- and cation-exchangers. This device has two bipolar boundaries, which are used to separate the location of hydroxide solution generation from the location where water is electrolyzed. Therefore, it can produce high-purity hydroxide solutions that are free from gases and anionic impurities. The hydroxide solution is generated on the basis of an electrokinetic phenomenon at the surfaces of ion-exchange resins and membranes in an electric field; NaOH concentration can be controlled at rates from 0.01 to 100mM per 1mL/min by adjusting the electrical current (0-200mA) applied to the device. As the generated solution is used as an eluent for a suppressed anion chromatography, the electrical conductivity of the effluent from the suppressor is as low as that of ultra-pure water. Thus, the noise of the base-line electrical conductivity is improved, and so the detection limit of anions on the sub-ng/mL order can be achieved.

  6. Analysis of moniliformin in maize plants using hydrophilic interaction chromatography

    DEFF Research Database (Denmark)

    Sørensen, Jens Laurids; Nielsen, Kristian Fog; Thrane, Ulf

    2007-01-01

    A novel HPLC method was developed for detection of the Fusarium mycotoxin, moniliformin in whole maize plants. The method is based on hydrophilic interaction chromatography (HILIC) on a ZIC zwitterion column combined with diode array detection and negative electrospray mass spectrometry (ESI......−-MS). Samples were extracted using acetonitrile–water (85:15), and the extracts were cleaned up on strong anion exchange columns. By this procedure we obtained a recovery rate of 57–74% moniliformin with a limit of detection at 48 ng/g and a limit of quantification at 96 ng/g using UV detection at 229 nm, which...

  7. High-Pressure Liquid Chromatography of Irradiated Nuclear Fue - Separation of Neodymium for Burn-up Determination

    DEFF Research Database (Denmark)

    Larsen, N. R.

    1979-01-01

    Neodymium is separated from solutions of spent nuclear fuel by high-pressure liquid chromatography in methanol-nitric acid-water media using an anion-exchange column. Chromatograms obtained by monitoring at 280 nm, illustrate the difficulties especially with the fission product ruthenium in nuclear...... chemistry. Preseparation of the rare earths and trivalent actinides using a di(2-ethylhexyl)phosphoric acid/kieselguhr column is described....

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-07-01

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

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

    International Nuclear Information System (INIS)

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

  10. Enzymatic and toxinological activities of Hypnale hypnale (hump-nosed pit viper venom and its fractionation by ion exchange high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    CH Tan

    2011-01-01

    Full Text Available Hypnale hypnale (hump-nosed pit viper has been recently identified as one of the medically important venomous snakes in Sri Lanka and on the southwestern coast of India. The characterization of its venom is essential for understanding the pathophysiology of envenomation and for optimizing its management. In the present study, the biological properties of Hypnale hypnale venom and venom fractions obtained using Resource Q ion exchange chromatography were determined. The venom exhibited toxic activities typical of pit viper venom, comparable to that of its sister taxon, the Malayan pit viper (Calloselasma rhodostoma. Particularly noteworthy were its high activities of thrombin-like enzyme, proteases, phospholipase A2, L-amino acid oxidase and hyaluronidase. The thrombin-like enzyme was mainly acidic and distributed over several chromatography fractions, indicating its existence in multiple isoforms. The hemorrhagic and necrotic activities of the venom were likely associated with the proteolytic enzyme found mainly in the basic fraction. Phospholipase A2 and phosphomonoesterase exist in both acidic and basic isoforms, while L-amino acid oxidase and hyaluronidase are highly acidic. The venom clotting activity on fibrinogens showed distinct species specificity in the following increasing order for clotting time: bovine < rabbit < goat < human < horse < < dog, and was comparable to that of C. rhodostoma venom. Its clot formation on human fibrinogen is gradual and prolonged, a phenomenon suggestive of consumptive coagulopathy as a complication observed clinically. At an intramuscular sublethal dose, the venom did not cause acute kidney injury in a rodent model, contrary to the positive control group treated with Daboia russelii venom. Nephrotoxicity may result from higher venom doses in the context of coagulopathy, as a complication provoked by venom hematoxicity.

  11. 离子交换-反相色谱纯化育亨宾%Purification of crude yohimbine by ion-exchange and reversed-phase chromatography

    Institute of Scientific and Technical Information of China (English)

    陶蕾; 赵明珠; 赵凤生; 徐伟; 王芝祥

    2011-01-01

    目的 从育亨宾树皮中提取的育亨宾粗品,一般纯度较低(10%左右).本文研究纯化育亨宾粗品的方法.方法 结合离子交换与反相色谱两种方法,考察了洗脱条件对纯化效果的影响.结果 采用1 ×2型阳离子交换树脂,以乙醇-水-氨水(40:55:5)为洗脱液,洗脱的育亨宾纯度最高;然后用C18反相色谱进一步纯化,流动相为甲醇-水(含0.01%三氟乙酸),甲醇浓度按3%,30%,40%,95%分阶段增加,洗脱液中的育亨宾纯度提高至71.2%.结论 这项工艺具有成本低、收率高、纯度好、步骤少的特点,在天然产物的分离纯化方面具有潜在的应用价值.%Purpose Crude yohimbine separated from Corynanthe yohimbe is only with low purity (a-bout 10% ). A method to purify crude yohimbine should be studied. Methods Ion-exchange and reversed-phase chromatography were combined in this study. The influence of elution conditions on purifying effects was investigated. Results By adsorption with 1×2 cation exchange resin and elution with mixture of etha-nol,water and ammonia(40:55 = 5) .highest purity of yohimbine was obtained. Next separation with C,g re-versed-phase chromatography was eluted with the mixture of methanol and water( containing 0. 01% triflu-oroacetic acid). When the concentration of methanol increased progressively based on 3%-30%-40%-95% ,the purity of yohimbine in eluent could increase to 71. 2% . Conclusion This technique has advantages of low cost, high yield, good purity and fewer procedures and has potential application value in the separation and purification of natural products.

  12. Separation of mono- and di-PEGylate of exenatide and resolution of positional isomers of mono-PEGylates by preparative ion exchange chromatography.

    Science.gov (United States)

    Nguyen, Ngoc-Thanh Thi; Lee, Jae Sun; Yun, Soi; Lee, E K

    2016-07-29

    Exenatide is a synthetic version of the 39-mer peptide of Exendin-4, which is an FDA-approved therapeutic against Type II diabetes mellitus. However, exenatide has a very short in-serum half-life and PEGylation have been performed to improve its in-serum stability. PEGylation often yields multivalent binding to non-specific residues, and the desired species should be carefully separated by chromatographies. In this study, we first devised an aqueous-phase, two-step PEGylation process. This consists of thiolation of Lys 12 and 27 residues followed by attachment of PEG-maleimide (10kD) to thiol groups. This process yields various species: mono-PEGylates with positional isomers, di-PEGylate, and other higher MW substances. A prep-grade cationic exchange chromatography (HiTrap SP) at pH 3.0 partially separated mono- and di-PEGylates based on the molar ratio of conjugated PEG and peptide and thus molecular weight of the conjugates. To further investigate the chromatographic separation of positional isomers of mono-PEGylates, we prepared two kinds of exenatide analogs by point mutation; K12C and K27C. Each analog was mono-PEGylated with very high yield (>95%). When a mixture of the two positional isomers of mono-PEGylates was applied to HiTrap SP chromatography, K12C-PEGylate and K27C-PEGylate eluted separately at 0.22M and 0.33M NaCl, respectively. When the proportions of acid and its conjugate base of the amino acid residues adjacent to the PEGylation site at pH 3.0 were analyzed, K27C-PEGylate shows stronger positive charge than K12C-PEGylate, and we propose the residence time difference between the two mono-PEGylates could be due to the charge difference. ELISA result shows that the immuno-binding activity of both analogs and their mono-PEGylates are well maintained. Furthermore, both mono-PEGylates of the analogs show higher than 50-fold improved anti-trypsin stability. We expect that mono-PEGylates of the exenatide analogs are alternatives to the conventional C40

  13. Method for immobilizing invertase by adsorption on Dowex® anionic exchange resin Método para a imobilização da invertase por adsorção em resinas trocadoras de ânions (DOWEX

    Directory of Open Access Journals (Sweden)

    Ester Junko Tomotani

    2006-06-01

    Full Text Available This communication describes a method for adsorbing the invertase (EC.3.2.1.26 on DOWEX® anion exchange resin. Among the types of DOWEX® resins studied (1x8:50-400; 1x4:50-400 and 1x2:100-400, 1X4-200 was the most suitable, because it adsorbed the invertase molecules completely and the complex 1X4-200/invertase retained 100% of the catalytic activity. Moreover, no leakage of enzyme from the support was noted at the end of the sucrose hydrolysis.O presente trabalho descreve um método de adsorção da invertase (EC. 3.2.1.26 na resina de troca aniônica do tipo Dowex®. Entre os tipos de resinas Dowex® estudados (1x8:50-400; 1x4:50-400 e 1x2:100-400, 1x4-200 foi a mais apropriada devido à completa adsorção das moléculas de invertase e a sua retenção de atividade catalítica de 100% do complexo 1x4-200/invertase. Salienta-se ainda a ausência do desprendimento da enzima do suporte após o término da hidrólise da sacarose.

  14. Uranium separations using extraction chromatography

    International Nuclear Information System (INIS)

    In the analysis of environmental samples for uranium and thorium pollutants and at natural levels for the dating of geological samples there was felt a need to develop better uranium and thorium, separation procedures to replace the established anion exchange method used at AEA Technology plc. This was the first aim of the PhD research. Separation of uranium from thorium prior to measurement of the isotopes by alpha spectrometry was necessary due to the similar alpha energies of 234U and 230Th. TRU and UTEVA extraction chromatography resins (EIChroM Industries) were investigated as potential replacements to the anion exchange separation method. The resins are claimed by EIChroM to offer the advantage of providing an actinide specific separation while reducing the separation time from 2 to 0.5 days; the volume of acidic waste produced by a factor of 3, therefore, the cost of analysis was reduced. A uranium and thorium separation procedure using the UTEVA extraction chromatography resin was developed. The uranium and thorium were sorbed by the UTEVA resin from 2M nitric acid. The thorium was then eluted from the resin with 5M hydrochloric acid and the uranium with 0.02M hydrochloric acid. The separation procedure was then evaluated using uraninite ore, coral, granite and lake sediment reference materials. The uranium and thorium concentrations and the 234U/238U and 230Th/234U activity ratio values determined for the reference material were in good agreement with certified values. The presence of plutonium was found to interfere with the measurement of uranium and thorium by alpha spectrometry. This was due to the similar alpha energies of uranium, thorium and plutonium. The co-elution of plutonium with uranium and thorium from the UTEVA resin was prevented by the inclusion of a reduction step using iron (II) sulphamate. The resulting plutonium (III) was not retained by the UTEVA column. The chemical recoveries for the procedure were similar to those for anion-exchange

  15. 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

    2011-11-01

    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 (Pmethod, 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. PMID:21968344

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

    Science.gov (United States)

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

    2014-11-01

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

  17. Measurement of gas-phase ammonia and amines in air by collection onto an ion exchange resin and analysis by ion chromatography

    Directory of Open Access Journals (Sweden)

    M. L. Dawson

    2014-02-01

    Full Text Available Ammonia and amines are common trace gases in the atmosphere and have a variety of both biogenic and anthropogenic sources, with a major contribution coming from agricultural sites. In addition to their malodorous nature, both ammonia and amines have been shown to enhance particle formation from acids such as nitric, sulfuric and methanesulfonic acids, which has implications for visibility, human health and climate. A key component of quantifying the effects of these species on particle formation is accurate gas-phase measurements in both laboratory and field studies. However, these species are notoriously difficult to measure as they are readily taken up on surfaces, including onto glass surfaces from aqueous solution as established in the present studies. We describe here a novel technique for measuring gas-phase ammonia and amines that involves uptake onto a weak cation exchange resin followed by extraction and analysis using ion chromatography. Two variants, one for ppb concentrations in air and the second with lower (ppt detection limits, are described. The latter involves the use of a custom-designed high-pressure cartridge to hold the resin for in-line extraction. These methods avoid the use of sampling lines, which can lead to significant inlet losses of these compounds. They also have the advantages of being relatively simple and inexpensive. The applicability of this technique to ambient air is demonstrated in measurements made near a cattle farm in Chino, CA.

  18. Simultaneous detection of perchlorate and bromate using rapid high-performance ion exchange chromatography-tandem mass spectrometry and perchlorate removal in drinking water.

    Science.gov (United States)

    West, Danielle M; Mu, Ruipu; Gamagedara, Sanjeewa; Ma, Yinfa; Adams, Craig; Eichholz, Todd; Burken, Joel G; Shi, Honglan

    2015-06-01

    Perchlorate and bromate occurrence in drinking water causes health concerns due to their effects on thyroid function and carcinogenicity, respectively. The purpose of this study was threefold: (1) to advance a sensitive method for simultaneous rapid detection of perchlorate and bromate in drinking water system, (2) to systematically study the occurrence of these two contaminants in Missouri drinking water treatment systems, and (3) to examine effective sorbents for minimizing perchlorate in drinking water. A rapid high-performance ion exchange chromatography-tandem mass spectrometry (HPIC-MS/MS) method was advanced for simultaneous detection of perchlorate and bromate in drinking water. The HPIC-MS/MS method was rapid, required no preconcentration of the water samples, and had detection limits for perchlorate and bromate of 0.04 and 0.01 μg/L, respectively. The method was applied to determine perchlorate and bromate concentrations in total of 23 selected Missouri drinking water treatment systems during differing seasons. The water systems selected include different source waters: groundwater, lake water, river water, and groundwater influenced by surface water. The concentrations of perchlorate and bromate were lower than or near to method detection limits in most of the drinking water samples monitored. The removal of perchlorate by various adsorbents was studied. A cationic organoclay (TC-99) exhibited effective removal of perchlorate from drinking water matrices.

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

    Science.gov (United States)

    Cernei, Natalia; Lackova, Zuzana; Guran, Roman; Hynek, David; Skladanka, Jiri; Horky, Pavel; Zitka, Ondrej; Adam, Vojtech

    2016-01-01

    The presence of biogenic amines is a hallmark of degraded food and its products. Herein, we focused on the utilization of magnetic nanoparticles off-line coupled with ion exchange chromatography with post-column ninhydrin derivatization and Vis detection for histamine (Him) separation and detection. Primarily, we described the synthesis of magnetic nanoparticles with nanomaghemite core (γ-Fe2O3) functionalized with titanium dioxide and, then, applied these particles to specific isolation of Him. To obtain further insight into interactions between paramagnetic particles’ (PMP) surface and Him, a scanning electron microscope was employed. It was shown that binding of histamine causes an increase of relative current response of deprotonated PMPs, which confirmed formation of Him-PMPs clusters. The recovery of the isolation showed that titanium dioxide-based particles were able to bind and preconcentrate Him with recovery exceeding 90%. Finally, we successfully carried out the analyses of real samples obtained from silage. We can conclude that our modified particles are suitable for Him isolation, and thus may serve as the first isolation step of Him from biological samples, as it is demonstrated on alfalfa seed variety Tereza silage. PMID:27626434

  20. Speciation of heavy metals in environmental water by ion chromatography coupled to ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Ammann, A.A. [Swiss Federal Institute for Environmental Science and Technology (EAWAG), Duebendorf (Switzerland)

    2002-02-01

    Biogenic (e.g. phytochelatins, porphyrins, DOM) as well as anthropogenic (e.g. NTA, EDTA, phosphonates) chelators affect the mobility and cycling of heavy metals in environmental waters. Since such chelators can form strongly bound anionic heavy metal complexes that are stable and highly mobile, anion-exchange chromatography coupled to ICP-MS was investigated. A narrow bore HPLC system was connected to a micro concentric nebuliser for in-line sample introduction. A new chromatographic procedure based on a synthetic hydrophilic quaternary ammonium anion exchanger in combination with nitrate as a strong eluent anion, and gradient elution, provided high separation selectivity and a large analytical window. Low detection limits (nmol L{sup -1}) were achieved by on-column matrix removal and sample preconcentration. This allowed the method to be successfully applied to different environmental research areas. In ecotoxicological studies of heavy metal effects on algae low concentrations of metal EDTA complexes were determined in nutrient solutions without interference from high (buffer) salt concentrations. In groundwater, infiltrated by a polluted river, mobile metal EDTA species were observed. In river water of different pollution levels beside CuEDTA other anionic Cu-complexes were found in nmol L{sup -1} concentrations. (orig.)

  1. 离子色谱法测定冰川雪冰样品中阴离子含量不确定度评定%Analysis of Uncertainty in Detecting Anion from Ice and Snow by Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    崔晓庆; 任贾文; 王晓香; 秦翔

    2011-01-01

    The research of the climate and the environmental information in snow and ice can reveal the climate and environmental characteristics of modem times to contemporary, and even reveal that over the last hundreds thousand years, but also through a combination of modem meteorological records, to improve the capacity of predicting the future climate change. Snow and ice plays an important role in the studies of the past global changes; the ice core research is also an extremely important area in studying the past global changes. The record of chemical composition in snow and ice provide a direct or indirect basis for global change research, such as climate change, biogeochemical cycle. Human activities, geological and cosmic events and many other scientific proposition's study. These records include the stable isotopes, heavy metals, particulates, aerosols, black carbon, ion.The ion chemical study of snow and ice has an important position. To analyze the uncertainty in detecting the anion in snow and ice by ion chromatography, find out the factors which influence the uncertainty , evaluate the uncertainty and give out the uncertainty of evaluation which faithfully reflects metrical credibility and accuracy.%雪冰内化学成分的记录为全球变化的各个方面,如气候变化、生物地球化学循环、人类活动、地质和宇宙事件等诸多科学命题的研究提供了直接或间接依据,这些化学成分记录主要包括雪冰内的稳定氢氧同位素、重金属、微粒、气溶胶、黑炭、离子等.雪冰内的离子化学成分的研究在冰川雪冰化学研究中具有重要的地位.为了更为准确地反映冰川雪冰内的记录信息,对离子的分析测试技术的要求就更高.采用离子色谱法测定冰川雪冰中阴离子的含量,并对测定的不确定度进行了分析,找出了影响冰川雪冰样品中阴离子不确定度的因素,并对不确定度进行了评佑.应用不确定度评定理论,计算得出

  2. ESTIMATION OF UNCERTAINTY AND VALIDATION OF ANALYTICAL PROCEDURES AS A QUALITY CONTROL TOOL THE EVALUATION OF UNCERTAINTY FOR AMINO ACID ANALYSIS WITH ION-EXCHANGE CHROMATOGRAPHY – CASE STUDY

    OpenAIRE

    Barbara Mickowska; Anna Sadowska-Rociek; Ewa Cieślik

    2013-01-01

    The aim of this study was to assess the importance of validation and uncertainty estimation related to the results of amino acid analysis using the ion-exchange chromatography with post-column derivatization technique. The method was validated and the components of standard uncertainty were identified and quantified to recognize the major contributions to uncertainty of analysis. Estimated relative extended uncertainty (k=2, P=95%) varied in range from 9.03% to 12.68%. Quantification of the u...

  3. Anions in Cometary Comae

    Science.gov (United States)

    Charnley, Steven B.

    2011-01-01

    The presence of negative ions (anions) in cometary comae is known from Giotto mass spectrometry of IP/Halley. The anions 0-, OH-, C-, CH- and CN- have been detected, as well as unidentified anions with masses 22-65 and 85-110 amu (Chaizy et al. 1991). Organic molecular anions are known to have a significant impact on the charge balance of interstellar clouds and circumstellar envelopes and have been shown to act as catalysts for the gas-phase synthesis of larger hydrocarbon molecules in the ISM, but their importance in cometary comae has not yet been explored. We present details of the first attempt to model the chemistry of anions in cometary comae. Based on the combined chemical and hydro dynamical model of Rodgers & Charnley (2002), we investigate the role of large carbon-chain anions in cometary coma chemistry. We calculate the effects of these anions on coma thermodynamics, charge balance and examine their impact on molecule formation.

  4. Separation and determination of the difficult-to-measure radionuclide 99Tc in radioactive wastes from nuclear power plants by using extraction chromatography and radiometric techniques

    International Nuclear Information System (INIS)

    A radiochemical separation and purification of 99Tc is proposed for radioactive wastes from Brazilian nuclear power plants. The method uses anion exchange and extraction chromatography employing a TEVA resin. The radiometric determination was performed by liquid scintillation counting using a Quantulus 1220 spectrometer. Rhenium is used as a yield monitor and the chemical recovery was in the range of 70-90 %. The limit of detection, Ld, obtained was 3.15 Bq L-1. (author)

  5. Performance comparison of suspended bed and batch contactor chromatography.

    Science.gov (United States)

    Quiñones-García, I; Rayner, I; Levison, P R; Dickson, N; Purdom, G

    2001-01-26

    In some applications, the purification and recovery of biomolecules is performed via a cascade of batch adsorption and desorption stages using agitated contactors and related filtration devices. Suspended bed chromatography is a recent process-scale innovation that is applicable to these separations. This hybrid technique exploits the benefits of combining batch adsorption in an agitated contactor with elution in an enclosed column system. To some extent, the process is similar to batch contactor chromatography but can be fully contained and significantly quicker. The process has two steps; first the fluid containing the sample is mixed with the adsorbent in a stirred tank. Second, the slurry suspension is transferred directly into a specialized column, such as an IsoPak column. The media with the adsorbed product is formed as a packed bed, whilst the suspension liquid is passed out of the column. The product is then eluted from the packed bed utilizing standard column-chromatography techniques. The performance of the suspended bed and the agitated contactor operations are demonstrated both by full-scale experimental results and process simulations. The purification of ovalbumin from a hen-egg white feedstock by anion-exchange chromatography was used as a case study in order to prove the concept. With the availability of both pump-packed systems and shear-resistant media, suspended bed chromatography is a better alternative for a range of applications than the traditional batch separations using agitated contactors. PMID:11218119

  6. Ion chromatography for the separation of heparin and structurally related glycoaminoglycans: A review.

    Science.gov (United States)

    Fasciano, Jennifer M; Danielson, Neil D

    2016-03-01

    The global crisis resulting from adulterated heparin in late 2007 and early 2008 revived the importance of analytical techniques for the purity analysis of heparin products. The utilization of ion chromatography techniques for the separation, detection, and structural determination of heparin and structurally related glycoaminoglycans, including their corresponding oligosaccharides, has become increasingly important. This review summarizes the primary HPLC approaches, particularly strong anion exchange, weak ion exchange, and reversed-phase ion-pair, used for heparin purity analysis as well as structural characterization. Strong anion exchange HPLC has been studied most extensively and currently offers the best separation of crude heparin and heparin-like compounds. Weak anion exchange HPLC has been shown to provide shorter analysis times with lower salt concentrations in the mobile phase but is not as widely developed for the separation of all glycoaminoglycans of interest. Reversed-phase ion-pair HPLC offers fast and effective separations of oligosaccharides derived from glycoaminoglycans that can be coupled to mass spectrometry for structural analysis. However, this method generally does not provide sufficient retention of intact glycoaminoglycans.

  7. Development of Radiochemical Analysis of Uranium Isotopes in Soil Samples with Extraction Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Myung Ho; Choi, Guk Sik; Cho, Young Hyun; Lee, Chang Woo [KAERI, Daejeon (Korea, Republic of); Lee, Soo Yong [Hanyang Univ., Seoul (Korea, Republic of)

    2001-03-15

    An accurate and rapid analytical technique of uranium isotopes in highly contaminated soil samples was developed and validated by application to the IAEA-Reference samples. For overcoming the demerits of the TBP extraction method, sample materials were decomposited with HNO{sub 3} and HF, and uranium isotopes were purified by an anion exchange resin and a TRU Spec resin. With the extraction chromatography method, the hindrance elements were completely removed from the uranium fraction. The chemical yields with the extraction chromatography method were more 10% higher than those with the TBP extraction method. The concentrations of uranium isotopes in soil samples using the extraction chromatography method were consistent with the reference values reported by the IAEA.

  8. Detection of Perchlorate Anion on Functionalized Silver Colloids Using Surface-Enhanced Raman Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Tio, J.; Wang, W.; Gu, B.

    2005-01-01

    Perchlorate anion interferes with the uptake of iodide by the human thyroid gland and consequently disrupts the regulation of metabolism. Chronic exposure to high levels of perchlorate may lead to the formation of thyroid gland tumors. Although the Environmental Protection Agency (EPA) has not set a maximum contaminant level (MCL) for perchlorate, a draft drinking water range of 4-18 ppb based on 2 liter daily consumption of water has been established. The current EPA approved method for detecting perchlorate uses ion chromatography which has a detection limit of ~1ppb and involves lengthy analytical time in the laboratory. A unique combination of the surface-enhanced Raman scattering (SERS) effect and the bifunctional anion exchange resin’s high selectivity may provide an alternative way to detect perchlorate at such low concentrations and with high specificity. SERS, which uses laser excitation of adsorbed perchlorate anions on silver nanoparticles, has been shown to detect perchlorate anions at concentrations as low as 50 ppb. Normal micro-Raman analysis of perchlorate sorbed onto the resin beads has detected an even lower concentration of 10 ppb. In an effort to integrate these two effects, silver nanoparticles were coated with N-trimethoxysilylpropyl-N,N,N-trimethylammonium chloride, a functional group similar to that found on the resin bead, and subsequently inserted into different perchlorate concentration environments. This method has resulted in perchlorate detection down to ~10 ppb and a more consistent detection of perchlorate anion at ~50 ppb than that of earlier methods. As suggested by the direct insertion of functionalized silver colloids into perchlorate samples, this technique may potentially allow for the development of a probe using on-site Raman spectrometry to detect significantly low concentrations of perchlorate in situ rather than in the laboratory.

  9. Highly active carbon supported palladium-rhodium PdXRh/C catalysts for methanol electrooxidation in alkaline media and their performance in anion exchange direct methanol fuel cells (AEM-DMFCs)

    International Nuclear Information System (INIS)

    Highlights: • Synthesis and physical evaluation of carbon supported, Rh containing Pd electrocatalysts. • Electroactivity towards methanol oxidation strongly enhanced in alkaline media. • Bimetallic catalyst show low CO oxidation and OH adsorption potentials. • CO2 current efficiency higher for bimetallic catalysts than for Pt/C or Pd/C. • Power density of 105 mW cm−2 for platinum-free alkaline direct methanol fuel cell. - Abstract: In this study carbon supported PdXRh electrocatalysts synthesized by wet chemical reduction process were tested for the potential use in anion-exchange membrane direct methanol fuel cells (AEM-DMFC) and compared to Pd/C and commercially available Pt/C. A metal loading of 20wt% on carbon was confirmed by thermogravimetric analysis (TGA) and catalyst compositions of PdRh3/C, PdRh/C and Pd3Rh/C were found via inductively coupled plasma optical emission spectroscopy (ICP-OES). Transmission electron microscopy (TEM) and x-ray diffraction (XRD) studies showed that the average particle and crystallite sizes of the PdXRh/C catalysts are in the range of 3.1 to 4.3 nm. It was also found that these catalysts are not alloyed. Cyclic voltammetry (CV) data reveals a 85–140 mV lower CH3OH oxidation onset potential and higher mass current densities for PdXRh/C catalysts compared with Pd/C. Steady-state measurements via chronoamperometry (CA) showed a good stability against poisoning during methanol oxidation and higher mass activities for PdRh/C and Pd3Rh/C compared to Pt/C. By using differential electrochemical mass spectrometry (DEMS) it was successfully shown that adding Rh to Pd results in an enhanced CO2 current efficiency (CCE) compared to Pd/C or Pt/C. AEM-DMFCs free from platinum were fabricated and single cell tests at 60 °C showed a significant increase of power density at 0.5 V cell potential from 4.8 mW cm−2 for Pd/C to 16.5 mW cm−2 for PdRh/C with the anode and cathode fed with 1 M methanol + 2 M KOH and synthetic air

  10. Studies of anions sorption on natural zeolites.

    Science.gov (United States)

    Barczyk, K; Mozgawa, W; Król, M

    2014-12-10

    This work presents results of FT-IR spectroscopic studies of anions-chromate, phosphate and arsenate - sorbed from aqueous solutions (different concentrations of anions) on zeolites. The sorption has been conducted on natural zeolites from different structural groups, i.e. chabazite, mordenite, ferrierite and clinoptilolite. The Na-forms of sorbents were exchanged with hexadecyltrimethylammonium cations (HDTMA(+)) and organo-zeolites were obtained. External cation exchange capacities (ECEC) of organo-zeolites were measured. Their values are 17mmol/100g for chabazite, 4mmol/100g for mordenite and ferrierite and 10mmol/100g for clinoptilolite. The used initial inputs of HDTMA correspond to 100% and 200% ECEC of the minerals. Organo-modificated sorbents were subsequently used for immobilization of mentioned anions. It was proven that aforementioned anions' sorption causes changes in IR spectra of the HDTMA-zeolites. These alterations are dependent on the kind of anions that were sorbed. In all cases, variations are due to bands corresponding to the characteristic Si-O(Si,Al) vibrations (occurring in alumino- and silicooxygen tetrahedra building spatial framework of zeolites). Alkylammonium surfactant vibrations have also been observed. Systematic changes in the spectra connected with the anion concentration in the initial solution have been revealed. The amounts of sorbed CrO4(2-), AsO4(3-) and PO4(3-) ions were calculated from the difference between their concentrations in solutions before (initial concentration) and after (equilibrium concentration) sorption experiments. Concentrations of anions were determined by spectrophotometric method. PMID:25002191

  11. Study of surface-bonded dicationic ionic liquids as stationary phases for hydrophilic interaction chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Li, Hua; Shan, Yuanhong; Wang, Shuangyuan; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2014-02-21

    In the present study, several geminal dicationic ionic liquids based on 1,4-bis(3-allylimidazolium)butane and 1,8-bis(3-allylimidazolium)octane in combination with different anions bromide and bis(trifluoromethanesulphonyl)imide were prepared and then bonded to the surface of 3-mercaptopropyl modified silica materials through the "thiol-ene" click chemistry as stationary phases for hydrophilic interaction chromatography (HILIC). Compared with their monocationic analogues, the dicationic ionic liquids stationary phases presented effective retention and good selectivity for typical hydrophilic compounds under HILIC mode with the column efficiency as high as 130,000 plates/m. Moreover, the influence of different alkyl chain spacer between dications and combined anions on the retention behavior and selectivity of the dicationic ionic liquids stationary phases under HILIC mode was displayed. The results indicated that the longer linkage chain would decrease the hydrophilicity and retention on the dicationic ionic liquid stationary phase, and while differently combined anions had no difference due to the exchangeability under the common HILIC mobile phase with buffer salt. Finally, the retention mechanism was investigated by evaluating the effect of chromatographic factors on retention, including the water content in the mobile phase, the mobile phase pH and buffer salt concentration. The results showed that the dicationic ionic liquids stationary phases presented a mixed-mode retention behavior with HILIC mechanism and anion exchange.

  12. Studies on rapid ion-exchange separation of the transplutonium elements with mineral acid-methanol mixed media

    International Nuclear Information System (INIS)

    In order to study properties of short-lived transplutonium nuclides synthesized by heavy-ion bombardment, three methods for rapid separation of tri-valent transplutonium elements by ion-exchange chromatography with mineral acid-methanol mixed media at elevated temperature were investigated. The first separation method was anion-exchange chromatography with nitric acid-methanol mixed media. The second method was anion-exchange choromatography with dilute hydrochloric acid-methanol mixed media. The third method was improved cation-exchange chromatography with single-column operation using the mixed media of hydrochloric acid and methanol. The separation methods developed were found applicable to studies on synthesis of the trans-plutonium nuclides, 250Fm (T1/2:30 min), 244,245,246Cf (T1/2:20 min, 46 min and 35.7 h, respectively) from the 16O + 238U and12C + 242Pu reactions, and on the decay property of 245Cf. Attempts to search for new actinide nuclides, such as 240U and neutron deficient nuclides of Am, Cm and Bk, were made by a quick purification. The separation system was also applied to the rapid and effective separation of Nd, Am and Cm from spent nuclear fuel samples, for burn-up determination. (J.P.N.) 242 refs

  13. Selective isolation of β-glucan from corn pericarp hemicelluloses by affinity chromatography on cellulose column.

    Science.gov (United States)

    Yoshida, Tomoki; Honda, Yoichi; Tsujimoto, Takashi; Uyama, Hiroshi; Azuma, Jun-ichi

    2014-10-13

    A combination of anion-exchange chromatography and affinity chromatography on a cellulose column was found to be effective for the isolation of β-(1,3;1,4)-glucan (BG) from corn pericarp hemicelluloses (CPHs). CPHs containing 6.6% BG were extracted from corn pericarp with 6M urea-2 wt% NaOH solution and initially fractionated into neutral and acidic parts by anion exchange chromatography to remove acidic arabinoxylan consisting of arabinose (35.6%) and xylose (50.9%). The neutral fraction (yield; 10.1% on the basis of CPHs) consisting of 1.0% arabinose, 10.1% xylose and 80.3% glucose containing 28.4% BG was then applied to a cellulose column of Whatman CF-11. BG could be recovered from the adsorbed fraction on the cellulose column by elution with 2% NaOH in a yield of 2.6% on the basis of CPHs with a purity of 84.7%. The chemical structure of the isolated corn pericarp BG was confirmed by (13)C NMR spectroscopic, methylation and lichenase treatment analyses. The results indicate that the ratios of (1,4)/(1,3) linkage and cellotriosyl/cellotetraosyl segments of the BG were 2.60 and 2.5, respectively.

  14. 不纯流动相对离子色谱法分析无机阴离子的影响%Investigation of Interferences Caused by Extraneous Chloride in the Analysis of Inorganic Anions with Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    刘勇建; HEBERLINGShawn; 等

    2002-01-01

    采用离子色谱模拟研究了流动相不纯对样品中无机阴离子测定造成的干扰.结果表明,在流动相中加入Cl-,使得其他6种阴离子响应值增加.这主要是由于Cl-加入的同时也带来了相应的阳离子,在通过抑制器时可带来等量的H+,H+伴随着各个阴离子样品一起通过检测器,使总的样品离子响应值增加.在6种阴离子中,F-和NO-2对AS14色谱柱的亲和力和Cl-相近,其响应值随Cl-加入量的变化趋势相似;Br-,NO-3,PO3-4及SO2-4因其对色谱柱的亲和力大于Cl-,它们的响应值随Cl-加入量的变化趋势也相同.对Cl-本身,当流动相中Cl-加入浓度不大于样品中Cl-的浓度(3 mgL-1)时,由流动相中Cl-造成的负系统峰小于样品中Cl-产生的正峰,其响应值基本没有变化.当流动相中Cl-浓度大于样品中Cl-浓度时,流动相中Cl-的负系统峰大于样品中Cl-的正峰,Cl-样品峰被系统峰覆盖.%A series of experiments were conducted by adding Cl- to the eluent to simulate the contaminated eluent. It was found that the added Cl- would cause the peak response of the anions increase largely. Because of the introduction of the superfluous H+, the total conductivity of each anion band was enhanced, and it was regarded as the increase of the sample anion. In the anions except Cl-, for the low affinities of F- and NO-2 for an AS14 column that were close to Cl-, they had the similar variation trends according to the amount of Cl- added to the eluent, and the two anions had the maximal responses when the concentration of Cl- in the eluent was 3 mg*L-1 that was just equal to the content in the sample. As to Br-, NO-3, PO3-4 and SO2-4 whose variation trends were the same, all of the peak responses of the anions reached the maximum when the concentration of Cl- in the eluent was 6 mg*L-1. For Cl-, the peak response hardly changed when the amount of Cl- added was less than or equal to the concentration of 3 mg*L-1 in the sample. When

  15. Controlled Release Kinetics in Hydroxy Double Salts: Effect of Host Anion Structure

    OpenAIRE

    Stephen Majoni; Jeanne M. Hossenlopp

    2014-01-01

    Nanodimensional layered metal hydroxides such as layered double hydroxides (LDHs) and hydroxy double salts (HDSs) can undergo anion exchange reactions releasing intercalated anions. Because of this, these metal hydroxides have found applications in controlled release delivery of bioactive species such as drugs and pesticides. In this work, isomers of hydroxycinnamate were used as model compounds to systematically explore the effects of anion structure on the rate and extent of anion release i...

  16. A procedure for reducing the concentration of hydrogen ions in acid anionic eluate and equipment therefore

    International Nuclear Information System (INIS)

    The method is described of reducing the concentration of hydrogen ions in acid anionic eluate produced in the separation of uranium or other metals, in which anion exchanger elution, precipitation, filtration and precipitate and anion exchanger washing are used. The technological line for such elution comprises at least one ion exchange column and at least one container. They together form the first and the second stages of preparation of the acid anion elution solution, the sorption-elution separation of hydrogen ions on an cation exchanger being inserted between them. The preparation of the solution is divide into two stages. In the first stage, the acid and part of the solution for the preparation of the acid anion elution solution are supplied. The resulting enriched acid elution solution is fe onto the cation exchanger where the hydrogen ion concentration i reduced. It is then carried into the second stage where it is mixed with the remaining part of the solution. (B.S.)

  17. Intrinsic anion oxidation potentials.

    Science.gov (United States)

    Johansson, Patrik

    2006-11-01

    Anions of lithium battery salts have been investigated by electronic structure calculations with the objective to find a computational measure to correlate with the observed (in)stability of nonaqueous lithium battery electrolytes vs oxidation often encountered in practice. Accurate prediction of intrinsic anion oxidation potentials is here made possible by computing the vertical free energy difference between anion and neutral radical (Delta Gv) and further strengthened by an empirical correction using only the anion volume as a parameter. The 6-311+G(2df,p) basis set, the VSXC functional, and the C-PCM SCRF algorithm were used. The Delta Gv calculations can be performed using any standard computational chemistry software. PMID:17078600

  18. Separation and characterization of anti-benzylpenicilloyl (BPO) antibodies. I. Biochemical and biophysical properties of anti-BPO-IgG obtained by affinity and subsequent ion-exchange chromatography.

    Science.gov (United States)

    Scheiner, O; Stemberger, H; Kraft, D; Wiedermann, G

    1978-01-01

    Anti-BPO antibodies were purified by means of affinity chromatography using AH-Sepharose 4B coated with covalently bound BPO groups. Specific elution was achieved by the hapten analogue BPO-epsilon-aminocaproic acid (BPO-EACA); desorption of the remaining antibody was performed thereafter by 0.1 M acetic acid. The resulting antibody fractions--hapten-eluted antibody (H-Ab) and acid eluted antibody (A-Ab), respectively--were further separated by ion-exchange chromatography which led to the appearance of 3 subfractions in the case of H-Ab (H1, H2, H3) and 2 subfractions in the case of A-Ab (A1 and A2). In liquid isoelectrofocusing an inhomogeneous pattern resulted. The bulk of antibodies focused between pH 6.5 and 7.0. The average avidity of H-Ab was found to be higher than that of A-Ab suggesting that avidity may influence the elution pattern in affinity chromatography. The hydrophobic influence of the "spacer" and/or interactions of antibodies directed against the hydrophobic regions of the BPO group may explain why a considerable part of the antibodies could be recovered from the immunosorbent only by acid elution.

  19. Determination of phytate in high molecular weight, charged organic matrices by two-dimensional size exclusion-ion chromatography.

    Science.gov (United States)

    Elkin, Kyle R; Slingsby, Rosanne; Bryant, Ray B

    2016-08-15

    A two-dimensional chromatography method for analyzing phytate or other ionic targets in matrices containing high molecular weight, charged organic species is described. Prior to quantification by anion exchange chromatography, the sample matrix was prepared by size exclusion chromatography, which removed the majority of the matrix. Quantification of phytate on the AS11-HC was sensitive (0.25µM, 0.17mg/l) and reproducible (4.6% RSD) allowing this method to provide baseline separation of phytate from a manure extract within 14min. The method is simple, requiring only sample filtering, reproducible (between-run variation 5% RSD) and linear from 0.38 to 76µM (0.25-50mg/l). The method is suitable for routine determination of phytate in high organic matrices such as manure extracts.

  20. Determination of heat stable salt anions in alkanolamine desulphurization solution by ion chromatography%离子色谱法测定醇胺脱硫溶液中热稳定盐

    Institute of Scientific and Technical Information of China (English)

    唐飞; 汪玉洁; 罗勤; 唐蒙; 陈赓良

    2012-01-01

    为了控制热稳定盐(HSS)对天然气净化装置造成的危害,建立了一种同时检测醇胺脱硫溶液中的乙酸根离子、甲酸根离子、氯离子、硫酸根离子、草酸根离子、硫代硫酸根离子和硫氰酸根离子的离子色谱方法.该方法利用膜过滤、反相固相萃取和稀释3个步骤对工业样品进行前处理,采用氢氧化钾梯度淋洗和电导检测的方式,实现了7种离子的分离与检测.方法的线性范围为0.01~0.5mmol/L,检出限(以信噪比(S/N)为3计)小于0.1 mg/L,回收率为80.0%~100.3%.在5个不同添加浓度下分别测定了上述7个离子,色谱峰面积的重复性良好(相对标准偏差(RSD,n=10)为0.94%~3.99%.通过3个实验室比对试验,表明该方法再现性良好,色谱峰面积的RSD小于5%.应用该方法成功地检测了8家天然气净化厂、3家石油炼厂和1家煤制油工厂的脱硫溶液样品中的HSS,并连续监测某天然气净化装置15 d.该方法具有良好的可靠性和实用性.%To control the potential risk of natural gas purification plants, an Ion chromato-graphic method has been developed to determine the heat stable salts (HSS) in alkanolamine desulphurization solution. Seven HSS anions, including CH3COO-, HCOO-, Cl-, SO2-4, C2O2-4, S2O2-3, SCN-, were determined in a single injection. Before the chromatographic analysis , these industrial samples were pie treated by three steps, i. e. filtration, solid phase extraction and dilution. Using the gradient elution with KOH solution, all of the seven anions have been separated and determined by a conductivity detector. As the calibration results, the linear range of this method was 0. 01 - 0. 5 mmol/L for the 7 anions. The limit of detection ( LOD, S/ N =3) was 0.1 mg/L for each anion. By spiked standard solutions in the samples, the recoveries were in the range of 80. 0% - 100. 3%. The repeatability of this method was evaluated at five different concentrations. The relative