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Sample records for automated anion-exchange purification

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

    PubMed

    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.

  2. Purification of Simulated Neptunium Filtrate Solution by Anion Exchange

    SciTech Connect

    Crowder, Mark L.; Kyser, Edward A. III

    2007-07-01

    Full text of publication follows: Anion exchange was investigated as a means to recover and purify neptunium (Np) from solutions containing significant plutonium (Pu), sodium (Na), and manganese (Mn) impurities and a high nitrate concentration. The solution being evaluated resulted from lean filtrate and precipitator clean-out solutions which were generated during Np processing at the Savannah River Site. Prior to anion exchange, valence adjustment of the Np using ferrous sulfamate (i.e., Fe{sub 2}(SO{sub 3}NH{sub 2}){sub 2} or FS) was evaluated. For testing, a simulated filtrate solution was made with {approx}1.5 g Np/L and slightly elevated levels of impurities. Two anion exchange column runs were performed. In both runs, Np was loaded onto Reillex HPQ resin in high nitric acid (HNO{sub 3}) solution, typical for Np processing. The resin wash step differed in the two runs, but the elution step was the same. In the first column run, 12 column bed volumes (BV) of reductive or partition wash with 6.4 M nitric acid / 0.05 M FS were used. In the second run, six BV of 5 M HNO{sub 3} / 0.05 M FS were used as the reductive wash. Reported results will include Pu rejection, Np losses and decontamination factors for Na and Mn. (authors)

  3. Purification Or Organic Acids Using Anion Exchange Chromatography.

    DOEpatents

    Ponnampalam; Elankovan

    2001-09-04

    Disclosed is a cost-effective method for purifying and acidifying carboxylic acids, including organic acids and amino acids. The method involves removing impurities by allowing the anionic form of the carboxylic acid to bind to an anion exchange column and washing the column. The carboxylic anion is displaced as carboxylic acid by washing the resin with a strong inorganic anion. This method is effective in removing organic carboxylic acids and amino acids from a variety of industrial sources, including fermentation broths, hydrolysates, and waste streams.

  4. Improved recovery and purification of plutonium at Los Alamos using macroporous anion exchange resin

    SciTech Connect

    Marsh, S.F.; Mann, M.J.

    1987-05-01

    For almost 30 years, Los Alamos National Laboratory has used anion exchange in nitric acid as the major aqueous process or the recovery and purification of plutonium. One of the few disadvantages of this system is the particularly slow rate at which the anionic nitrato complex of Pu(IV) equilibrates with the resin. The Nuclear Materials Process Technology Group at Los Alamos recently completed an ion exchange development program that focused on improving the slow sorption kinetics that limits this process. A comprehensive investigation of modern anion exchange resins identified porosity and bead size as the properties that most influence plutonium sorption kinetics. Our study found that small beads of macroporous resin produced a dramatic increase in plutonium process efficiency. The Rocky Flats Plant has already adopted this improved ion exchange technology, and it currently is being evaluated for use in other DOE plutonium-processing facilities.

  5. Purification of small interfering RNA using nondenaturing anion-exchange chromatography.

    PubMed

    Noll, Bernhard; Seiffert, Stephan; Hertel, Frank; Debelak, Harald; Hadwiger, Philipp; Vornlocher, Hans-Peter; Roehl, Ingo

    2011-12-01

    A manufacturing and purification process for duplex oligonucleotides was established, which shortens and simplifies currently used procedures, yielding a product of higher purity. The reported procedure is based on nondenaturing anion-exchange (AEX) chromatography, which is performed on the annealed duplex rather than the individual single strands. The duplex is formed early in the process by annealing of the crude single strands directly after solid-phase synthesis. Two 30 μmol manufacturing runs using duplex purification were performed on 2 different AEX resins and compared with a manufacturing run of the same scale using conventional single-strand chromatography. The same pooling strategy was employed for all purifications. Content of optimal duplex (duplex exclusively comprising full-length single strands) was 90.5% and 90.2% for the batches obtained by duplex purification and 86.1% for the batch obtained by single-strand purification. Maximum chromatographic recoveries were 67% for the duplex purification and 68% for the single-strand purification. Hence, the manufacture of small interfering RNA (siRNA) using duplex purification was simpler and faster than conventional single-strand purification and provided better purity and similar yield of final siRNA.

  6. Cored anion-exchange chromatography media for antibody flow-through purification.

    PubMed

    Wang, Chen; Soice, Neil P; Ramaswamy, Senthilkumar; Gagnon, Brian A; Umana, Joaquin; Cotoni, Kristen A; Bian, Nanying; Cheng, Kwok-Shun C

    2007-06-29

    Agarose-based anion-exchangers (e.g. quaternary amine, Q) have been widely used in monoclonal antibody flow-through purification to remove trace levels of impurities. Such media are often packed in a large column and the operation is usually robust but with limited throughput due to the compressibility of agarose and consequentially low bed permeability. In order to address this limitation, cored Q beads consisting of a rigid core and a thin agarose gel coating were developed and evaluated for protein flow-through chromatography. Using laboratory-scale columns it was found that, the cored beads indeed provide significantly enhanced rigidity and flow permeability relative to conventional homogeneous agarose resins. Depending on the structure and size of the cored beads, the permeability was 2-4-fold higher than that of a commonly used commercial agarose resin. Good virus and host cell protein clearance was achieved with the cored Q beads even at increased flow velocities. In addition, the impermeable core allows for more efficient use of buffers without loss of useful capacity in polishing applications. Process analyses based upon the experimental data demonstrated that the enhanced permeability achieved with the cored beads can significantly improve process throughput and economics.

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

    PubMed

    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

  8. High-throughput purification of double-stranded RNA molecules using convective interaction media monolithic anion exchange columns.

    PubMed

    Romanovskaya, Alesia; Sarin, L Peter; Bamford, Dennis H; Poranen, Minna M

    2013-02-22

    Recent advances in the field of RNA interference and new cost-effective approaches for large-scale double-stranded RNA (dsRNA) synthesis have fuelled the demand for robust high-performance purification techniques suitable for dsRNA molecules of various lengths. To address this issue, we developed an improved dsRNA purification method based on anion exchange chromatography utilizing convective interaction media (CIM) monolithic columns. To evaluate column performance we synthesized a selection of dsRNA molecules (58-1810 bp) in a one-step enzymatic reaction involving bacteriophage T7 DNA-dependent RNA polymerase and phi6 RNA-dependent RNA polymerase. In addition, small interfering RNAs (siRNAs) of 25-27 bp were generated by Dicer digestion of the genomic dsRNA of bacteriophage phi6. We demonstrated that linearly scalable CIM monolithic quaternary amine (QA) columns can be used as a fast and superior alternative to standard purification methods (e.g. LiCl precipitation) to obtain highly pure dsRNA preparations. The impurities following Dicer treatment were quickly and efficiently removed with the QA CIM monolithic column, yielding siRNA molecules of high purity suitable for potential therapeutic applications. Moreover, baseline separation of dsRNA molecules up to 1 kb in non-denaturing conditions was achieved.

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

    SciTech Connect

    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.

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

    SciTech Connect

    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.

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

    PubMed

    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

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

    PubMed

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

    PubMed

    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.

  14. A simple and efficient purification platform for monoclonal antibody production based on chromatin-directed cell culture clarification integrated with precipitation and void-exclusion anion exchange chromatography.

    PubMed

    Chen, Quan; Abdul Latiff, Sarah Maria; Toh, Phyllicia; Peng, Xinying; Hoi, Aina; Xian, Mo; Zhang, Haibo; Nian, Rui; Zhang, Wei; Gagnon, Pete

    2016-10-20

    Protein A affinity chromatography, featured by its robustness and high-specificity, is still dominant as a first capture step for the purification of immunoglobulin G monoclonal antibodies (IgG mAbs). However, the material and operational costs of protein A are universally recognized as high, and its productivity is also limited as column mode. In order to overcome these limitations, industry is increasingly considering the use of non-protein A-based processes for IgG purification. In this study, sodium citrate precipitation (SCP) was developed as the primary purification step, and chromatin-directed cell culture clarification was demonstrated to significantly elevate the purification capability. Additional 0.05% (w/v) of Tween 20 was shown to effectively reduce the residual free antibody light chain (LC) during precipitation. The resuspended IgG was further polished by void-exclusion anion exchange chromatography (VEAX), which supported protein loading without buffer adjustment. The non-histone host cell protein (nh-HCP) content in the final product was about 5ppm and histone HCP below limit of detection (LOD). DNA was reduced to less than 1ppb, and aggregates/free LC less than 0.1%. The overall IgG recovery was 87.2%. A simple and efficient purification platform with only one-column step was therefore established, providing a more promising alternative to the current prevailing protein A-based purification platforms. PMID:27568167

  15. Anion exchange membrane

    DOEpatents

    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.

  16. Anion exchange polymer electrolytes

    SciTech Connect

    Kim, Yu Seung; Kim, Dae Sik

    2015-06-02

    Anion exchange polymer electrolytes that include guanidinium functionalized polymers may be used as membranes and binders for electrocatalysts in preparation of anodes for electrochemical cells such as solid alkaline fuel cells.

  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

    SciTech Connect

    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 polymer electrolytes

    DOEpatents

    Kim, Yu Seung; Kim, Dae Sik; Lee, Kwan-Soo

    2013-07-23

    Solid anion exchange polymer electrolytes and compositions comprising chemical compounds comprising a polymeric core, a spacer A, and a guanidine base, wherein said chemical compound is uniformly dispersed in a suitable solvent and has the structure: ##STR00001## wherein: i) A is a spacer having the structure O, S, SO.sub.2, --NH--, --N(CH.sub.2).sub.n, wherein n=1-10, --(CH.sub.2).sub.n--CH.sub.3--, wherein n=1-10, SO.sub.2-Ph, CO-Ph, ##STR00002## wherein R.sub.5, R.sub.6, R.sub.7 and R.sub.8 each are independently --H, --NH.sub.2, F, Cl, Br, CN, or a C.sub.1-C.sub.6 alkyl group, or any combination of thereof; ii) R.sub.9, R.sub.10, R.sub.11, R.sub.12, or R.sub.13 each independently are --H, --CH.sub.3, --NH.sub.2, --NO, --CH.sub.nCH.sub.3 where n=1-6, HC.dbd.O--, NH.sub.2C.dbd.O--, --CH.sub.nCOOH where n=1-6, --(CH.sub.2).sub.n--C(NH.sub.2)--COOH where n=1-6, --CH--(COOH)--CH.sub.2--COOH, --CH.sub.2--CH(O--CH.sub.2CH.sub.3).sub.2, --(C.dbd.S)--NH.sub.2, --(C.dbd.NH)--N--(CH.sub.2).sub.nCH.sub.3, where n=0-6, --NH--(C.dbd.S)--SH, --CH.sub.2--(C.dbd.O)--O--C(CH.sub.3).sub.3, --O--(CH.sub.2).sub.n--CH--(NH.sub.2)--COOH, where n=1-6, --(CH.sub.2).sub.n--CH.dbd.CH wherein n=1-6, --(CH.sub.2).sub.n--CH--CN wherein n=1-6, an aromatic group such as a phenyl, benzyl, phenoxy, methylbenzyl, nitrogen-substituted benzyl or phenyl groups, a halide, or halide-substituted methyl groups; and iii) wherein the composition is suitable for use in a membrane electrode assembly.

  19. Pu Anion Exchange Process Intensification

    SciTech Connect

    Taylor-Pashow, K.

    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.

  20. Anion exchange resins: Structure, formulation, and applications. (Latest citations from the Rubber and Plastics Research Association database). Published Search

    SciTech Connect

    Not Available

    1994-07-01

    The bibliography contains citations concerning the formulation and synthesis of anion exchange resins based on such resins as amides, polyethylenes, and styrenes. Osmotic, sorption, and electrical properties; exchange kinetics behavior; structure studies; and temperature related performance effects on anion exchange resins are considered. Anion exchange chromatography of liquids, and applications in water purification, pollution control, and protein and metallic ion separation are included. (Contains a minimum of 222 citations and includes a subject term index and title list.)

  1. [Chromatographic separation of plasmid DNA by anion-exchange cryogel].

    PubMed

    Guo, Yantao; Shen, Shaochuan; Yun, Junxian; Yao, Kejian

    2012-08-01

    Plasmid DNA (pDNA) is used as an important vector for gene therapy, and its wide application is restricted by the purity and yield. To obtain high-purity pDNA, a chromatographic method based on anion-exchange supermacroporous cryogel was explored. The anion-exchange cryogel was prepared by grafting diethylaminoethyl-dextran to the epoxide groups of polyacrylamide-based matrix and pUC19 plasmid was used as a target to test the method. The plasmid was transferred into Escherichia coli DH5alpha, cultivated, harvested and lysed. The obtained culture was centrifuged and the supernatant was used as the plasmid feedstock, which was loaded into the anion-exchange cryogel bed for chromatographic separation. By optimizing the pH of running buffer and the elution conditions, high-purity pDNA was obtained by elution with 0.5 mol/L sodium chloride solution at pH 6.6. Compared to the traditional methods for purification of pDNA, animal source enzymes and toxic reagents were not involved in the present separation process, ensuring the safety of both the purification operations and the obtained pDNA.

  2. [Chromatographic separation of plasmid DNA by anion-exchange cryogel].

    PubMed

    Guo, Yantao; Shen, Shaochuan; Yun, Junxian; Yao, Kejian

    2012-08-01

    Plasmid DNA (pDNA) is used as an important vector for gene therapy, and its wide application is restricted by the purity and yield. To obtain high-purity pDNA, a chromatographic method based on anion-exchange supermacroporous cryogel was explored. The anion-exchange cryogel was prepared by grafting diethylaminoethyl-dextran to the epoxide groups of polyacrylamide-based matrix and pUC19 plasmid was used as a target to test the method. The plasmid was transferred into Escherichia coli DH5alpha, cultivated, harvested and lysed. The obtained culture was centrifuged and the supernatant was used as the plasmid feedstock, which was loaded into the anion-exchange cryogel bed for chromatographic separation. By optimizing the pH of running buffer and the elution conditions, high-purity pDNA was obtained by elution with 0.5 mol/L sodium chloride solution at pH 6.6. Compared to the traditional methods for purification of pDNA, animal source enzymes and toxic reagents were not involved in the present separation process, ensuring the safety of both the purification operations and the obtained pDNA. PMID:23185899

  3. Automated multi-step purification protocol for Angiotensin-I-Converting-Enzyme (ACE).

    PubMed

    Eisele, Thomas; Stressler, Timo; Kranz, Bertolt; Fischer, Lutz

    2012-12-12

    Highly purified proteins are essential for the investigation of the functional and biochemical properties of proteins. The purification of a protein requires several steps, which are often time-consuming. In our study, the Angiotensin-I-Converting-Enzyme (ACE; EC 3.4.15.1) was solubilised from pig lung without additional detergents, which are commonly used, under mild alkaline conditions in a Tris-HCl buffer (50mM, pH 9.0) for 48h. An automation of the ACE purification was performed using a multi-step protocol in less than 8h, resulting in a purified protein with a specific activity of 37Umg(-1) (purification factor 308) and a yield of 23.6%. The automated ACE purification used an ordinary fast-protein-liquid-chromatography (FPLC) system equipped with two additional switching valves. These switching valves were needed for the buffer stream inversion and for the connection of the Superloop™ used for the protein parking. Automated ACE purification was performed using four combined chromatography steps, including two desalting procedures. The purification methods contained two hydrophobic interaction chromatography steps, a Cibacron 3FG-A chromatography step and a strong anion exchange chromatography step. The purified ACE was characterised by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE) and native-PAGE. The estimated monomer size of the purified glycosylated ACE was determined to be ∼175kDa by SDS-PAGE, with the dimeric form at ∼330kDa as characterised by a native PAGE using a novel activity staining protocol. For the activity staining, the tripeptide l-Phe-Gly-Gly was used as the substrate. The ACE cleaved the dipeptide Gly-Gly, releasing the l-Phe to be oxidised with l-amino acid oxidase. Combined with peroxidase and o-dianisidine, the generated H(2)O(2) stained a brown coloured band. This automated purification protocol can be easily adapted to be used with other protein purification tasks. PMID:23217308

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

    PubMed

    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

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

    PubMed

    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.

  6. Advancements in Anion Exchange Membrane Cations

    SciTech Connect

    Sturgeon, Matthew R.; Long, Hai; Park, Andrew M.; Pivovar, Bryan S.

    2015-10-15

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

  7. Poly(phenylene)-based anion exchange membrane

    DOEpatents

    Hibbs, Michael; Cornelius, Christopher J.; Fujimoto, Cy H.

    2011-02-15

    A poly(phenylene) compound of copolymers that can be prepared with either random or multiblock structures where a first polymer has a repeat unit with a structure of four sequentially connected phenyl rings with a total of 2 pendant phenyl groups and 4 pendant tolyl groups and the second polymer has a repeat unit with a structure of four sequentially connected phenyl rings with a total of 6 pendant phenyl groups. The second polymer has chemical groups attached to some of the pendant phenyl groups selected from CH.sub.3, CH.sub.2Br, and CH.sub.2N(CH.sub.3).sub.3Br groups. When at least one group is CH.sub.2N(CH.sub.3).sub.3Br, the material functions as an anion exchange membrane.

  8. Superporous agarose anion exchangers for plasmid isolation.

    PubMed

    Tiainen, Peter; Gustavsson, Per-Erik; Ljunglöf, Anders; Larsson, Per-Olof

    2007-01-01

    Superporous agarose beads have wide, connecting flow pores allowing large molecules such as plasmids to be transported into the interior of the beads by convective flow. The pore walls provide additional surface for plasmid binding thus increasing the binding capacity of the adsorbent. Novel superporous agarose anion exchangers have been prepared, differing with respect to bead diameter, superpore diameter and type of anion-exchange functional group (poly(ethyleneimine) and quaternary amine). The plasmid binding capacities were obtained from breakthrough curves and compared with the binding capacity of homogeneous agarose beads of the same particle size. Significantly, the smaller diameter superporous agarose beads were found to have four to five times higher plasmid binding capacity than the corresponding homogeneous agarose beads. The experimentally determined plasmid binding capacity was compared with the theoretically calculated surface area for each adsorbent and fair agreement was found. Confocal microscopy studies of beads with adsorbed, fluorescently labelled plasmids aided in the interpretation of the results. Superporous poly(ethyleneimine)-substituted beads with a high ion capacity (230 micromol/ml) showed a plasmid binding of 3-4 mg/ml adsorbent. Superporous quaternary amine-substituted beads had a lower ion capacity (81 micromol/ml) and showed a correspondingly lower plasmid binding capacity (1-2 mg/ml adsorbent). In spite of the lower capacity, the beads with quaternary amine ligand were preferred, due to their much better plasmid recovery (70-100% recovery). Interestingly, both capacity and recovery was improved when the plasmid adsorption step was carried out in the presence of a moderate salt concentration. The most suitable superporous bead type (45-75 microm diameter beads; 4 microm superpores; quaternary amine ligand) was chosen for the capture of plasmid DNA from a clarified alkaline lysate. Two strategies were evaluated, one with and one

  9. 8. VIEW OF GLOVE BOXES USED IN THE ANION EXCHANGE ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    8. VIEW OF GLOVE BOXES USED IN THE ANION EXCHANGE PROCESS. THE ANION EXCHANGE PROCESS PURIFIED AND CONCENTRATED PLUTONIUM-BEARING NITRIC ACID SOLUTIONS TO MAKE THEM ACCEPTABLE AS FEED FOR CONVERSION TO METAL. (6/20/60) - Rocky Flats Plant, Plutonium Recovery & Fabrication Facility, North-central section of plant, Golden, Jefferson County, CO

  10. Neutron activation analysis of nickel purified by floating zone-refining and anion exchange.

    PubMed

    Isshiki, M; Yakushiji, K; Kikuchi, T; Sato, M; Yanagisawa, E; Igaki, K; Mizohata, A; Mamuro, T; Tsujimoto, T

    1981-04-01

    Nondestructive neutron activation analysis was performed on the nickel purified by floating zone-refining and anion exchange. It is found that floating zone-refining in vacuum is effective to remove Na, Sc, Cr, Zn, As, Ag, Sb and Hg through vaporization in addition to elimination of Se, Sb, Ta, Sm and Tb through segregation. Anion exchange method is also effective to separate Fe, Co, Zn, Mo, Hg, Th and U usually contained in the commercial nickel sources. It is concluded that combination of these two purification methods is required to obtain high purity nickel, since floating zone-refining is known ineffective to eliminate Fe and Co, main impurities in commercial nickel sources. PMID:7291628

  11. Anion-exchange sorption of molybdate and germanate

    SciTech Connect

    Kislinskaya, G.E.; Denisova, T.I.; Sheka, I.A.

    1983-07-20

    Interest in sorption of molybdenum and germanium from salt solutions is prompted by industrial requirements related to purification of such solutions and also to extraction of these elements from various industrial liquors.In order to identify the ionic forms of molybdenum and germanium having the highest sorption activity and to determine the optimal conditions for extraction of these elements from solutions with high electrolyte contents, we studied the states of molybdenum(VI) and germanium(IV) in solutions of sodium chloride in various concentrations, and sorption of these elements by strongly basic macroporous anion-exchange resins and by iron and aluminum hydroxides in relation to the pH, concentrations of the elements, and time of contact between the solution and the sorbent. Examination of literature data shows that the molecular and ionic states of these elements in the presence of high salt concentrations have been studied mainly in acidic solutions and at higher molybdenum and germanium concentrations. However, for selection of a method of removal of molybdenum and germanium from production liquors it is also necessary to have analogous information on their states when present in microconcentrations over wide ranges of pH.

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

    PubMed

    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

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

    PubMed

    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.

  14. Anion-exchange resin-based desulfurization process

    SciTech Connect

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

    1992-01-01

    Under DOE Grant No. FG22-90PC90309, the University of Tennessee Space Institute (UTSI) is contracted to further develop its anion-exchange, resin-based desulfurization concept to desulfurize alkali metal sulfates. From environmental as well as economic viewpoints, it is necessary to remove soluble sulfates from the wastes created by flue gas desulfurization systems. In order to do this economically, a low-cost desulfurization process for spent sorbents is necessary. UTSI's anion-exchange resin-based desulfurization concept is believed to satisfy these requirements.

  15. Automated RNA Extraction and Purification for Multiplexed Pathogen Detection

    SciTech Connect

    Bruzek, Amy K.; Bruckner-Lea, Cindy J.

    2005-01-01

    Pathogen detection has become an extremely important part of our nation?s defense in this post 9/11 world where the threat of bioterrorist attacks are a grim reality. When a biological attack takes place, response time is critical. The faster the biothreat is assessed, the faster countermeasures can be put in place to protect the health of the general public. Today some of the most widely used methods for detecting pathogens are either time consuming or not reliable [1]. Therefore, a method that can detect multiple pathogens that is inherently reliable, rapid, automated and field portable is needed. To that end, we are developing automated fluidics systems for the recovery, cleanup, and direct labeling of community RNA from suspect environmental samples. The advantage of using RNA for detection is that there are multiple copies of mRNA in a cell, whereas there are normally only one or two copies of DNA [2]. Because there are multiple copies of mRNA in a cell for highly expressed genes, no amplification of the genetic material may be necessary, and thus rapid and direct detection of only a few cells may be possible [3]. This report outlines the development of both manual and automated methods for the extraction and purification of mRNA. The methods were evaluated using cell lysates from Escherichia coli 25922 (nonpathogenic), Salmonella typhimurium (pathogenic), and Shigella spp (pathogenic). Automated RNA purification was achieved using a custom sequential injection fluidics system consisting of a syringe pump, a multi-port valve and a magnetic capture cell. mRNA was captured using silica coated superparamagnetic beads that were trapped in the tubing by a rare earth magnet. RNA was detected by gel electrophoresis and/or by hybridization of the RNA to microarrays. The versatility of the fluidics systems and the ability to automate these systems allows for quick and easy processing of samples and eliminates the need for an experienced operator.

  16. Highly Water Resistant Anion Exchange Membrane for Fuel Cells.

    PubMed

    Yang, Zhengjin; Hou, Jianqiu; Wang, Xinyu; Wu, Liang; Xu, Tongwen

    2015-07-01

    For anion exchange membranes (AEMs), achieving efficient hydroxide conductivity without excessive hydrophilicity presents a challenge. Hence, new strategies for constructing mechanically strengthened and hydroxide conductive (especially at controlled humidity) membranes are critical for developing better AEMs. Macromolecular modification involving ylide chemistry (Wittig reaction) for the fabrication of novel AEMs with an interpenetrating polymer network structure is reported. The macromolecular modification is cost effective, facile, and based on a one-pot synthesis. AEM water uptake is reduced to 3.6 wt% and a high hydroxide conductivity (69.7 mS cm(-1) , 90 °C) is achieved simultaneously. More importantly, the membrane exhibits similar tensile strength (>35 MPa) and comparable flexibility in both dry and wet states. These AEMs could find further applications within anion exchange membrane fuel cells with low humidity or photoelectric assemblies.

  17. Highly Water Resistant Anion Exchange Membrane for Fuel Cells.

    PubMed

    Yang, Zhengjin; Hou, Jianqiu; Wang, Xinyu; Wu, Liang; Xu, Tongwen

    2015-07-01

    For anion exchange membranes (AEMs), achieving efficient hydroxide conductivity without excessive hydrophilicity presents a challenge. Hence, new strategies for constructing mechanically strengthened and hydroxide conductive (especially at controlled humidity) membranes are critical for developing better AEMs. Macromolecular modification involving ylide chemistry (Wittig reaction) for the fabrication of novel AEMs with an interpenetrating polymer network structure is reported. The macromolecular modification is cost effective, facile, and based on a one-pot synthesis. AEM water uptake is reduced to 3.6 wt% and a high hydroxide conductivity (69.7 mS cm(-1) , 90 °C) is achieved simultaneously. More importantly, the membrane exhibits similar tensile strength (>35 MPa) and comparable flexibility in both dry and wet states. These AEMs could find further applications within anion exchange membrane fuel cells with low humidity or photoelectric assemblies. PMID:25962480

  18. Thermodynamic study of the interaction between linear plasmid DNA and an anion exchange support under linear and overloaded conditions.

    PubMed

    Aguilar, P A; Twarda, A; Sousa, F; Dias-Cabral, A C

    2014-11-01

    Anion-exchange chromatography has been successfully used in plasmid DNA (pDNA) purification. However, pDNA adsorption mechanism using this method is still not completely understood, and the prediction of the separation behavior is generally unreliable. Flow microcalorimetry (FMC) has proven its ability to provide an improved understanding of the driving forces and mechanisms involved in the adsorption process of biomolecules onto several chromatographic systems. Thus, using FMC, this study aims to understand the adsorption mechanism of linear pDNA (pVAX1-LacZ) onto the anion-exchange support Fast Flow (FF) Q-Sepharose. Static binding capacity studies have shown that the mechanism of pDNA adsorption onto Q-Sepharose follows a Langmuir isotherm. FMC experiments resulted in thermograms that comprised endothermic and exothermic heats. Endothermic heat major contributor was suggested to be the desolvation process. Exothermic heats were related to the interaction between pDNA and Q-Sepharose primary and secondary adsorption. Furthermore, FMC revealed that the overall adsorption process is exothermic, as expected for an anion-exchange interaction. Nevertheless, there are evidences of the presence of nonspecific effects, such as reorientation and electrostatic repulsive forces. PMID:25465014

  19. Sorption of heavy metal metatartrate complexes on polystyrene anion exchangers.

    PubMed

    Hubicki, Zbigniew; Geca, Marzena; Kołodyńska, Dorota

    2011-04-01

    The performance of polystyrene anion exchangers in purifying wastewaters containing metatartaric acid and heavy metal ions (especially those from electroless plating processes) was investigated. The following anion exchangers were selected: Lewatit MonoPlus M 500, Lewatit MonoPlus MP 64, Lewatit MP 62 and Amberlite IRA 402. A batch method was used to study the influence of: phase contact time (1-120 min); solution pH (2-9); concentration of initial heavy metal Cu(II), Zn(II), Co(II) and Ni(II) complexes (1.25 x 10(-4) M to 8.0 x 10(-3) M); temperature (303-333K); and interfering ions (Cl-, NO3-, SO4(2-), Ca2+, Mg2+). The amounts of Cu(II), Zn(II), Co(II) and Ni(II) complexes with metatartaric acid sorbed at equilibrium using the strongly basic anion exchanger Lewatit MonoPlus M 500 were equal to 7.25 mg/g, 3.21 mg/g, 3.78 mg/g and 3.98 mg/g, respectively. The equilibrium sorption capacity increased slightly with increasing temperature. The optimal pH sorption was found to be 6.5. The experimental data were analysed using the Langmuir and Freundlich models. The maximum adsorption capacities q(0) determined from the Langmuir adsorption equation equal to 7.53 mg/g, 3.75 mg/g, 3.55 mg/g and 4.60 mg/g were in good agreement with the experimental values for Lewatit MonoPlus M 500. The kinetic data obtained at different concentrations were modelled using pseudo first order, pseudo second order and intraparticle diffusion equations. The experimental data were well described by the pseudo second order kinetic model.

  20. Anion Exchange Membranes: Current Status and Moving Forward

    SciTech Connect

    Hickner, MA; Herring, AM; Coughlin, EB

    2013-10-29

    This short review is meant to provide the reader with highlights in anion exchange membrane research, describe current needs in the field, and point out promising directions for future work. Anion exchange membranes (AEMs) provide one possible route to low platinum or platinum-free fuel cells with the potential for facile oxidation of complex fuels beyond hydrogen and methanol. AEMs and related stable cationic polymers also have applications in energy storage and other electrochemical technologies such as water electrolyzers and redox flow batteries. While anion exchange membranes have been known for a long time in water treatment applications, materials for electrochemical technology with robust mechanical properties in thin film format have only recently become more widely available. High hydroxide and bicarbonate anion conductivity have been demonstrated in a range of AEM formats, but intrinsic stability of the polymers and demonstration of long device lifetime remain major roadblocks. Novel approaches to stable materials have focused on new types of cations that employ delocalization and steric shielding of the positive center to mitigate nucleophilic attack by hydroxide. A number of promising polymer backbones and membrane architectures have been identified, but limited device testing and a lack of understanding of the degradation mechanisms in operating devices is slowing progress on engineered systems with alkaline fuel cell technology. Our objective is to spur more research in this area to develop fuel cell systems that approach the costs of inexpensive batteries for large-scale applications. (c) 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2013, 51, 1727-1735, 2013

  1. Anion-exchange nanospheres as titration reagents for anionic analytes.

    PubMed

    Zhai, Jingying; Xie, Xiaojiang; Bakker, Eric

    2015-08-18

    We present here anion-exchange nanospheres as novel titration reagents for anions. The nanospheres contain a lipophilic cation for which the counterion is initially Cl(-). Ion exchange takes place between Cl(-) in the nanospheres and a more lipophilic anion in the sample, such as ClO4(-) and NO3(-). Consecutive titration in the same sample solution for ClO4(-) and NO3(-) were demonstrated. As an application, the concentration of NO3(-) in spinach was successfully determined using this method.

  2. Regeneration of anion exchange resins by catalyzed electrochemical reduction

    DOEpatents

    Gu, Baohua; Brown, Gilbert M.

    2002-01-01

    Anion exchange resins sorbed with perchlorate may be regenerated by a combination of chemical reduction of perchlorate to chloride using a reducing agent and an electrochemical reduction of the oxidized reducing agent. Transitional metals including Ti, Re, and V are preferred chemical reagents for the reduction of perchlorate to chloride. Complexing agents such as oxalate are used to prevent the precipitation of the oxidized Ti(IV) species, and ethyl alcohol may be added to accelerate the reduction kinetics of perchlorate. The regeneration may be performed by continuously recycling the regenerating solution through the resin bed and an electrochemical cell so that the secondary waste generation is minimized.

  3. Determining gold in water by anion-exchange batch extraction

    USGS Publications Warehouse

    McHugh, J.B.

    1986-01-01

    This paper describes a batch procedure for determining gold in natural waters. It is completely adaptable to field operations. The water samples are filtered and acidified before they are equilibrated with an anion-exchange resin by shaking. The gold is then eluted with acetone-nitric acid solution, and the eluate evaporated to dryness. The residue is taken up in hydrobromic acid-bromine solution and the gold is extracted with methyl isobutyl ketone. The extract is electrothermally atomized in an atomic-absorption spectrophotometer. The limit of determination is 1 ng 1. ?? 1986.

  4. ANION EXCHANGE METHOD FOR SEPARATION OF METAL VALUES

    DOEpatents

    Hyde, E.K.; Raby, B.A.

    1959-02-10

    A method is described for selectively separating radium, bismuth, poloniums and lead values from a metallic mixture of thc same. The mixture is dissolved in aqueous hydrochloric acid and the acidity is adjusted to between 1 to 2M in hydrochloric acid to form the anionic polychloro complexes of polonium and bismuth. The solution is contacted with a first anion exchange resin such as strong base quaternary ammonia type to selectively absorb the polonium and bismuth leaving the radium and lead in the effluent. The effluent, after treatment in hydrochloric acid to increase the hydrochloric acid concentration to 6M is contacted with a second anion exchange iesin of the same type as the above to selectively adsorb the lead leaving the radium in the effluent. Radium is separately recovered from the effluent from the second exchange column. Lead is stripped from the loaded resin of the second column by treatment with 3M hydrochloric acid solution. The loaded resin of the first column is washed with 8M hydrochloric acid solution to recover bismuth and then treated with strong nitric acid solution to recover polonium.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. Trace adsorption of positively charged proteins onto Sepharose FF and Sepharose FF-based anion exchangers.

    PubMed

    Yu, Lin-Ling; Sun, Yan

    2012-08-31

    Agarose-based matrices have been widely used in ion exchange chromatography (IEC). We have herein observed that positively charged proteins (lysozyme and cytochrome c) are adsorbed on the agarose-based anion-exchangers (Q and DEAE Sepharose FF gels) in a capacity of 10-40 μg/mL. In contrast, negatively charged protein (bovine serum albumin) is not adsorbed to Sepharose FF and SP Sepharose FF gels. Elemental analysis of the gel indicated that the residual anionic sulfate groups in agarose would have worked as the cation exchange groups for the positively charged proteins. The trace adsorption behavior of lysozyme onto Sepharose FF and Sepharose FF-based anion exchangers was studied and the effects of NaCl concentration and cation group density on the adsorption were examined for better understanding of the trace adsorption in chromatographic processes. At NaCl concentrations less than 0.05 mol/L, which is the normal adsorption condition in IEC, the trace adsorption kept at a high level, so this trace adsorption cannot be avoided in the ionic strength range of routine IEC operations. Grafting poly(ethylenimine) (PEI) chain of 60 kDa to a cation group density of 700 mmol/L could reduce the adsorption capacity to about 20 μg/mL, but further reduction was not possible by increasing the cation group density to 1200 mmol/L. Therefore, attentions need to be paid to the phenomenon in protein purification practice using agarose-based matrices. The research is expected to call attentions to the trace adsorption on agarose-based matrices and to the importance in the selection of the suitable solid matrices in the production of high-purity protein products in large-scale bioprocesses.

  7. Evaluation of a new, macroporous polyvinylpyridine resin for processing plutonium using nitrate anion exchange

    SciTech Connect

    Marsh, S.F.

    1989-04-01

    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 greatly stability to chemical and radiolytic degradation. 8 refs., 14 figs.

  8. Development of an automated mid-scale parallel protein purification system for antibody purification and affinity chromatography.

    PubMed

    Zhang, Chi; Long, Alexander M; Swalm, Brooke; Charest, Ken; Wang, Yan; Hu, Jiali; Schulz, Craig; Goetzinger, Wolfgang; Hall, Brian E

    2016-12-01

    Protein purification is often a bottleneck during protein generation for large molecule drug discovery. Therapeutic antibody campaigns typically require the purification of hundreds of monoclonal antibodies (mAbs) during the hybridoma process and lead optimization. With the increase in high-throughput cloning, faster DNA sequencing, and the use of parallel protein expression systems, a need for high-throughput purification approaches has evolved, particularly in the midsize range between 20 ml and 100 ml. To address this we modified a four channel Gilson solid phase extraction system (referred to as MG-SPE) with switching valves and sample holding loops to be able to perform standard affinity purification using commercially available columns and micro-titer format deep well blocks. By running 4 samples in parallel, the MG-SPE has the capacity to purify up to 24 samples of greater than 50 ml each using a single-step affinity purification protocol or a two-step protocol consisting of affinity chromatography followed by desalting/buffer exchange overnight (∼12 h run time). Our evaluation of affinity purification using mAbs and Fc-fusion proteins from mammalian cell supernatants demonstrates that the MG-SPE compared favorably with industry standard systems for both protein quality and yield. Overall the system is simple to operate and fills a void in purification processes where a simple, efficient, automated system is needed for affinity purification of midsize research samples. PMID:27498022

  9. Development of an automated mid-scale parallel protein purification system for antibody purification and affinity chromatography.

    PubMed

    Zhang, Chi; Long, Alexander M; Swalm, Brooke; Charest, Ken; Wang, Yan; Hu, Jiali; Schulz, Craig; Goetzinger, Wolfgang; Hall, Brian E

    2016-12-01

    Protein purification is often a bottleneck during protein generation for large molecule drug discovery. Therapeutic antibody campaigns typically require the purification of hundreds of monoclonal antibodies (mAbs) during the hybridoma process and lead optimization. With the increase in high-throughput cloning, faster DNA sequencing, and the use of parallel protein expression systems, a need for high-throughput purification approaches has evolved, particularly in the midsize range between 20 ml and 100 ml. To address this we modified a four channel Gilson solid phase extraction system (referred to as MG-SPE) with switching valves and sample holding loops to be able to perform standard affinity purification using commercially available columns and micro-titer format deep well blocks. By running 4 samples in parallel, the MG-SPE has the capacity to purify up to 24 samples of greater than 50 ml each using a single-step affinity purification protocol or a two-step protocol consisting of affinity chromatography followed by desalting/buffer exchange overnight (∼12 h run time). Our evaluation of affinity purification using mAbs and Fc-fusion proteins from mammalian cell supernatants demonstrates that the MG-SPE compared favorably with industry standard systems for both protein quality and yield. Overall the system is simple to operate and fills a void in purification processes where a simple, efficient, automated system is needed for affinity purification of midsize research samples.

  10. Using solvent extraction to process nitrate anion exchange column effluents

    SciTech Connect

    Yarbro, S.L.

    1987-10-01

    Octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO), a new organophosphorous extractant, and a new centrifugal mixer-settler both recently developed at Argonne were evaluated for their potential use in the recovery of actinides from nitrate anion exchange column effluents. The performance of the extractant was evaluated by measuring the extraction coefficient values as a function of acid and salt concentration. Additional performance parameters include extraction coefficient behavior as a function of the total metal concentration in the organic phase, and comparison of different stripping and organic scrubbing techniques. A simulated effluent stream was used to evaluate the performance of the centrifugal mixer-settlers by comparing experimental and calculated interstage concentration profiles. Both the CMPO extractant and the centrifugal mixer-settlers have potential for processing nitrate column effluents, particularly if the stripping behavior can be improved. Details of the proposed process are presented in the flowsheet and contactor design analyses.

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

    NASA Astrophysics Data System (ADS)

    Matsuoka, Koji; Iriyama, Yasutoshi; Abe, Takeshi; Matsuoka, Masao; Ogumi, Zempachi

    Alkaline direct alcohol fuel cells using an OH-form anion exchange membrane and polyhydric alcohols were studied. A high open circuit voltage of ca. 800 mV was obtained for a cell using Pt-Ru/C (anode) and Pt/C (cathode) at 323 K, which was about 100-200 mV higher than that for a DMFC using Nafion ®. 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.

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

    PubMed

    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.

  13. Characterization of a biopharmaceutical protein and evaluation of its purification process using automated capillary Western blot.

    PubMed

    Xu, Dong; Mane, Sarthak; Sosic, Zoran

    2015-01-01

    This paper describes the application of an automated size-based capillary Western blot system (Sally instrument) from ProteinSimple, Inc., for biopharmaceutical fusion-Fc protein characterization and evaluation of its purification process. The fusion-Fc protein column purification from an excess of single chain Fc polypeptide and removal of an enzyme coexpressed for protein maturation have been demonstrated using an automated capillary Western system. The clearance of a selected host cell protein (HCP) present in cell culture of fusion-Fc protein was also quantitatively monitored throughout the protein purification process. Additionally, the low levels of fusion-Fc product-related impurities detected by traditional slab gel Western blot were confirmed by the automated capillary Western system. Compared to the manual approach, the automated capillary Western blot provides the advantages of ease of operation, higher sample throughput, greater linearity range, and higher precision for protein quantitation.

  14. Human anion exchanger1 mutations and distal renal tubular acidosis.

    PubMed

    Yenchitsomanus, Pa-thai

    2003-09-01

    The human anion exchanger 1 (AE1 or SLC4A1) gene encodes anion exchanger 1 (or band 3) protein in erythrocytes and in alpha-intercalated cells of the kidney. Thus, AE1 mutations show pleiotrophic effects resulting in two distinct and seemingly unrelated defects, an erythrocyte abnormality and distal renal tubular acidosis (dRTA). Southeast Asian ovalocytosis (SAO), a well-known red blood cell (RBC) defect, which is widespread in Southeast Asian regions, is caused by AE1 mutation due to a deletion of 27 base pairs in codons 400-408 (delta400-408) leading to an in-frame 9 amino-acid loss in the protein. Co-existence of SAO and dRTA is usually not seen in the same individual. However, the two conditions can co-exist as the result of compound heterozygosities between delta400-408 and other mutations. The reported genotypes include delta400-408/G701D, delta400-408/R602H, delta400-408/deltaV850, and delta400-408/A858D. The presence of dRTA, with or without RBC abnormalities, may occur from homozygous or compound heterozygous conditions of recessive AE1 mutations (eg G701D/G701D, V488M/V488M, deltaV850/deltaV850, deltaV850/A858D, G701D/S773P) or heterozygous dominant AE1 mutations (eg R598H, R589C, R589S, S613F, R901X). Codon 589 of this gene seems to be a 'mutational hot-spot' since repeated mutations at this codon occurring in different ethnic groups and at least two de novo (R589H and R589C) mutations have been observed. Therefore, AE1 mutations can result in both recessive and dominant dRTA, possibly depending on the position of the amino acid change in the protein. As several mutant AE1 proteins still maintain a significant anion transport function but are defective in targeting to the cell surface, impaired intracellular trafficking of the mutant AE1 is an important molecular mechanism involved in the pathogenesis of dRTA associated with AE1 mutations. PMID:15115146

  15. Modeling of protein-anion exchange resin interaction for the human growth hormone charge variants.

    PubMed

    Lapelosa, Mauro; Patapoff, Thomas W; Zarraga, Isidro E

    2015-12-01

    Modeling ion exchange chromatography (IEC) behavior has generated significant interest because of the wide use of IEC as an analytical technique as well as a preparative protein purification process; indeed there is a need for better understanding of what drives the unique behavior of protein charge variants. We hypothesize that a complex protein molecule, which contains both hydrophobic and charged moieties, would interact strongly with an in silico designed resin through charged electrostatic patches on the surface of the protein. In the present work, variants of recombinant human growth hormone that mimic naturally-occurring deamidation products were produced and characterized in silico. The study included these four variants: rhGH, N149D, N152D, and N149D/N152D. Poisson-Boltzmann calculations were used to determine surface electrostatic potential. Metropolis Monte Carlo simulations were carried out with the resulting variants to simulate IEC systems, examining the free energy of the interaction of the protein with an in silico anion exchange column represented by polylysine polypeptide. The results show that the charge variants have different average binding energies and the free energy of interaction can be used to predict the retention time for the different variants.

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

    PubMed

    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.

  17. Ion-exchange equilibrium of N-acetyl-D-neuraminic acid on a strong anionic exchanger.

    PubMed

    Wu, Jinglan; Ke, Xu; Zhang, Xudong; Zhuang, Wei; Zhou, Jingwei; Ying, Hanjie

    2015-09-15

    N-acetyl-D-neuraminic acid (Neu5Ac) is a high value-added product widely applied in the food industry. A suitable equilibrium model is required for purification of Neu5Ac based on ion-exchange chromatography. Hence, the equilibrium uptake of Neu5Ac on a strong anion exchanger, AD-1 was investigated experimentally and theoretically. The uptake of Neu5Ac by the hydroxyl form of the resin occurred primarily by a stoichiometric exchange of Neu5Ac(-) and OH(-). The experimental data showed that the selectivity coefficient for the exchange of Neu5Ac(-) with OH(-) was a non-constant quantity. Subsequently, the Saunders' model, which took into account the dissociation reactions of Neu5Ac and the condition of electroneutrality, was used to correlate the Neu5Ac sorption isotherms at various solution pHs and Neu5Ac concentrations. The model provided an excellent fit to the binary exchange data for Cl(-)/OH(-) and Neu5Ac(-)/OH(-), and an approximate prediction of equilibrium in the ternary system Cl(-)/Neu5Ac(-)/OH(-). This basic information combined with the general mass transfer model could lay the foundation for the prediction of dynamic behavior of fixed bed separation process afterwards.

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

    PubMed

    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

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

    NASA Astrophysics Data System (ADS)

    Traboulsi, A.; Labed, V.; Dauvois, V.; Dupuy, N.; Rebufa, C.

    2013-10-01

    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 (NH). 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.

  20. Removal of bromide and natural organic matter by anion exchange.

    PubMed

    Hsu, Susan; Singer, Philip C

    2010-04-01

    Bromide removal by anion exchange was explored for various water qualities, process configurations, and resin characteristics. Simulated natural waters containing different amounts of natural organic matter (NOM), bicarbonate, chloride, and bromide were treated with a polyacrylate-based magnetic ion exchange (MIEX) resin on a batch basis to evaluate the effectiveness of the resin for removal of bromide. While bromide removal was achieved to some degree, alkalinity (bicarbonate), dissolved organic carbon (DOC), and chloride were shown to inhibit bromide removal in waters with bromide concentrations of 100 and 300 microg/L. Water was also treated using a two-stage batch MIEX process. Two-stage treatment resulted in only a slight improvement in bromide removal compared to single-stage treatment, presumably due to competition with the high concentration of chloride which is present along with bromide in natural waters. In view of the relatively poor bromide removal results for the MIEX resin, a limited set of experiments was performed using polystyrene resins. DOC and bromide removal were compared by treating model waters with MIEX and two polystyrene resins, Ionac A-641 and Amberlite IRA910. The two polystyrene resins were seen to be more effective for bromide removal, while the MIEX resin was more effective at removing DOC.

  1. Fouling mitigation of anion exchange membrane by zeta potential control.

    PubMed

    Park, Jin-Soo; Lee, Hong-Joo; Choi, Seok-Ju; Geckeler, Kurt E; Cho, Jaeweon; Moon, Seung-Hyeon

    2003-03-15

    The feasibility of fouling mitigation of anion exchange membranes (AEMs) in the presence of humate was studied by adding three different types of water-soluble polymers, i.e., poly(acrylic acid) (PAA), poly(vinyl alcohol) (PVA), and poly(ethylene imine) (PEI), during electrodialysis (ED) desalination. Measurement of zeta potential of the humate used in this study showed highly negative potential (about -30 mV), implying that the humate had a strong fouling potential on the AEMs in ED. Of the three water-soluble polymers, PEI showed a positive zeta potential (about +14 mV) and is able to form an interpolymer complex with the humate. PAA and PVA hardly formed interpolymer complexes with humate due to electrostatic repulsion. The PEI-humate mixture with a volume ratio of 1:20 (PEI:humate) showed zero zeta potential, and a complexed humate with zero surface charge was formed, resulting in no fouling effects on the AEMs. Accordingly, the desalting ED experiments with PEI showed improved ED performance. Further, black colloids formed in the mixture did not cause the cell resistance to increase. PMID:16256509

  2. Fouling mitigation of anion exchange membrane by zeta potential control.

    PubMed

    Park, Jin-Soo; Lee, Hong-Joo; Choi, Seok-Ju; Geckeler, Kurt E; Cho, Jaeweon; Moon, Seung-Hyeon

    2003-03-15

    The feasibility of fouling mitigation of anion exchange membranes (AEMs) in the presence of humate was studied by adding three different types of water-soluble polymers, i.e., poly(acrylic acid) (PAA), poly(vinyl alcohol) (PVA), and poly(ethylene imine) (PEI), during electrodialysis (ED) desalination. Measurement of zeta potential of the humate used in this study showed highly negative potential (about -30 mV), implying that the humate had a strong fouling potential on the AEMs in ED. Of the three water-soluble polymers, PEI showed a positive zeta potential (about +14 mV) and is able to form an interpolymer complex with the humate. PAA and PVA hardly formed interpolymer complexes with humate due to electrostatic repulsion. The PEI-humate mixture with a volume ratio of 1:20 (PEI:humate) showed zero zeta potential, and a complexed humate with zero surface charge was formed, resulting in no fouling effects on the AEMs. Accordingly, the desalting ED experiments with PEI showed improved ED performance. Further, black colloids formed in the mixture did not cause the cell resistance to increase.

  3. Slc26A9 - anion exchanger, channel and Na+ transporter

    PubMed Central

    Chang, Min-Hwang; Plata, Consuelo; Zandi-Nejad, Kambiz; Sinđić, Aleksandra; Sussman, Caroline R.; Mercado, Adriana; Broumand, Vadjista; Raghuram, Viswanathan; Mount, David B.; Romero, Michael F.

    2009-01-01

    The SLC26 gene family encodes anion transporters with diverse functional attributes: (a) anion exchanger, (b) anion sensor and (c) anion conductance (likely channel). We have cloned and studied Slc26a9, a paralog expressed mostly in lung and stomach. Immunohistochemistry shows that Slc26a9 is present at apical and intracellular membranes of lung and stomach epithelia. Using expression in Xenopus laevis oocytes and ion-sensitive microelectrodes, we discovered that Slc26a9 has a novel function not found in any other Slc26 proteins – cation coupling. Intracellular pH and voltage measurements show that Slc26a9 is a nCl--HCO3- exchanger, suggesting roles in gastric HCl secretion or pulmonary HCO3- secretion; Na+ electrodes and uptakes reveal that Slc26a9 has a cation-dependence. Single channel measurements indicate that Slc26a9 displays discrete open and close states. These experiments show that Slc26a9 has three discrete physiological modes: nCl--HCO3- exchanger, Cl- channel, and Na+-anion cotransporter. Thus, the Slc26a9 transporter-channel is uniquely suited for dynamic and tissue-specific physiology or regulation in epithelial tissues. PMID:19365592

  4. Anion-exchange resin-based desulfurization process

    SciTech Connect

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

    1992-01-01

    Under the current grant, the University of Tennessee Space Institute (UTSI) will carry out the bench scale evaluation and further development of the anion-exchange resin-based desulfurization concept to desulfurize alkali metal sulfates. This concept has been developed and patented by UTSI under US Patent No. 4,917,874. The developmental program proposed under this DOE grant includes screening of commercially available resins to select three candidate resins for further study. These three resins will undergo a series of experiments designed to test the resins' performance under different process conditions (including the use of spent MHD seed material). The best of these resins will be used in optimizing the regeneration step and in testing the effects of performance enhancers. The process schematic developed from the results will be used to estimate the related economics. During this reporting period, October 1, 1991 to September 30, 1992, analysis of batch mode screening experiments was completed to select three candidate resins for process variables study in the fixed-bed set-up. This setup was modified and the experiments were carded out to evaluate effects of major process variables. The analysis of fixed-bed experiments is going on and we have also started simple batch mode experiments to identify desirable conditions for resin regeneration step. We have also started simple process engineering type calculations to determine the trade-off between the solution concentration and the resulting evaporation/concentration load.

  5. High-capacity anion exchangers based on poly (glycidylmethacrylate-divinylbenzene) microspheres for ion chromatography.

    PubMed

    Liu, Junwei; Wang, Yong; Cheng, Heli; Wang, Nani; Wu, Shuchao; Zhang, Peimin; Zhu, Yan

    2016-10-01

    Poly (glycidylmethacrylate-divinylbenzene) microspheres were prepared by the two-staged swelling and polymerization method and applied to prepare anion exchange stationary phases. Methylamine, dimethylamine, trimethylamine, diethylamine and triethylamine were selected to prepare the quaternary ammonium groups of anion exchangers, respectively. The diameters and surface characteristics of microspheres were measured by scanning electron microscope and nitrogen adsorption-desorption measurements. The anion exchangers were characterized by Fourier transform infrared spectrum, elemental analysis and breakthrough curve methods. The chromatographic performances of anion exchangers were illustrated by separating conventional anions, organic weak acids and carbohydrates. The results indicated that the anion exchange capacities were controllable by changing either the content of glycidylmethacrylate in microspheres or the number of bonded quaternary ammonium layer. Meanwhile, the substituents of quaternary ammonium groups greatly influenced the separation properties of anion exchangers. Finally, the three-layer methylamine-quaternized anion exchanger was successfully applied for the determination of fluoride in tea sample. The content of fluoride was detected to be 0.13mgg(-1) without the interference of acetate and formate. PMID:27474308

  6. Diffusional transport of ions in plasticized anion-exchange membranes.

    PubMed

    Kumar, Rakesh; Pandey, Ashok K; Sharma, Manoj K; Panicker, L V; Sodaye, Suparna; Suresh, G; Ramagiri, Shobha V; Bellare, Jayesh R; Goswami, A

    2011-05-19

    Diffusional transport properties of hydrophobic anion-exchange membranes were studied using the polymer inclusion membrane (PIM). This class of membranes is extensively used in the chemical sensor and membrane based separation processes. The samples of PIM were prepared by physical containment of the trioctylmethylammonium chloride (Aliquat-336) in the plasticized matrix of cellulose triacetate (CTA). The plasticizers 2-nitrophenyl octyl ether, dioctyl phthalate, and tris(2-ethylhexyl)phosphate having different dielectric constant and viscosity were used to vary local environment of the membrane matrix. The morphological structure of the PIM was obtained by atomic force microscopy and transmission electron microscopy (TEM). For TEM, platinum nanoparticles (Pt nps) were formed in the PIM sample. The formation of Pt nps involved in situ reduction of PtCl(6)(2-) ions with BH(4)(-) ions in the membrane matrix. Since both the species are anions, Pt nps thus formed can provide information on spatial distribution of anion-exchanging molecules (Aliquat-336) in the membrane. The glass transitions in the membrane samples were measured to study the effects of plasticizer on physical structure of the membrane. The self-diffusion coefficients (D) of the I(-) ions and water in these membranes were obtained by analyzing the experimentally measured exchange rate profiles of (131)I(-) with (nat)I(-) and tritiated water with H(2)O, respectively, between the membrane and equilibrating solution using an analytical solution of Fick's second law. The values of D(I(-)) in membrane samples with a fixed proportion of CTA, plasticizer, and Aliquat-336 were found to vary significantly depending upon the nature of the plasticizer used. The comparison of values of D with properties of the plasticizers indicated that both dielectric constant and viscosity of the plasticizer affect the self-diffusion mobility of I(-) ions in the membrane. The value of D(I(-)) in the PIM samples did not vary

  7. Anion exchanger 1 interacts with nephrin in podocytes.

    PubMed

    Wu, Fiona; Saleem, Moin A; Kampik, Nicole B; Satchwell, Timothy J; Williamson, Rosalind C; Blattner, Simone M; Ni, Lan; Toth, Tibor; White, Graham; Young, Mark T; Parker, Mark D; Alper, Seth L; Wagner, Carsten A; Toye, Ashley M

    2010-09-01

    The central role of the multifunctional protein nephrin within the macromolecular complex forming the glomerular slit diaphragm is well established, but the mechanisms linking the slit diaphragm to the cytoskeleton and to the signaling pathways involved in maintaining the integrity of the glomerular filter remain incompletely understood. Here, we report that nephrin interacts with the bicarbonate/chloride transporter kidney anion exchanger 1 (kAE1), detected by yeast two-hybrid assay and confirmed by immunoprecipitation and co-localization studies. We confirmed low-level glomerular expression of kAE1 in human and mouse kidneys by immunoblotting and immunofluorescence microscopy. We observed less kAE1 in human glomeruli homozygous for the NPHS1(FinMaj) nephrin mutation, whereas kAE1 expression remained unchanged in the collecting duct. We could not detect endogenous kAE1 expression in NPHS1(FinMaj) podocytes in primary culture, but heterologous re-introduction of wild-type nephrin into these podocytes rescued kAE1 expression. In kidneys of Ae1(-/-) mice, nephrin abundance was normal but its distribution was altered along with the reported kAE1-binding protein integrin-linked kinase (ILK). Ae1(-/-) mice had increased albuminuria with glomerular enlargement, mesangial expansion, mesangiosclerosis, and expansion of the glomerular basement membrane. Glomeruli with ILK-deficient podocytes also demonstrated altered AE1 and nephrin expression, further supporting the functional interdependence of these proteins. These data suggest that the podocyte protein kAE1 interacts with nephrin and ILK to maintain the structure and function of the glomerular basement membrane.

  8. Removal of Pu238 from Neptunium Solution by Anion Exchange

    SciTech Connect

    KYSER, EDWARD

    2003-12-01

    A new anion flowsheet for use in HB-Line was tested in the lab with Reillex{trademark} HPQ for removal of Pu{sup 238} contamination from Np. Significant rejection of Pu{sup 238} was observed by washing with 6 to 12 bed volumes (BV) of reductive wash containing reduced nitric acid concentration along with both ferrous sulfamate (FS) and hydrazine. A shortened-height column was utilized in these tests to match changes in the plant equipment. Lab experiments scaled to plant batch sizes of 1500 to 2200 g Np were observed with modest losses for up-flow washing. Down-flow washing was observed to have high losses. The following are recommended conditions for removing Pu{sup 238} from Np solutions by anion exchange in HB-Line: (1) Feed conditions: Up-flow 6.4-8 M HNO{sub 3}, 0.02 M hydrazine, 0.05 M excess FS, less than 5 days storage of solution after FS addition. (2) Reductive Wash conditions: Up-flow 6-12 BV of 6.4 M HNO{sub 3}, 0.05 M FS, 0.05 M hydrazine. 1.8 mL/min/cm{sup 2} flowrate. (3) Decontamination Wash conditions: Up-flow 1-2 BV of 6.4-8 M HNO{sub 3}, no FS, no hydrazine. (4) Elution conditions: Down-flow 0.17 M HNO{sub 3}, 0.05 M hydrazine, no FS.

  9. 3D Printing of Micropatterned Anion Exchange Membranes.

    PubMed

    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

  10. Analysis of carbohydrates by anion exchange chromatography and mass spectrometry.

    PubMed

    Bruggink, Cees; Maurer, Rolf; Herrmann, Heiko; Cavalli, Silvano; Hoefler, Frank

    2005-08-26

    A versatile liquid chromatographic platform has been developed for analysing underivatized carbohydrates using high performance anion exchange chromatography (HPAEC) followed by an inert PEEK splitter that splits the effluent to the integrated pulsed amperometric detector (IPAD) and to an on-line single quadrupole mass spectrometer (MS). Common eluents for HPAEC such as sodium hydroxide and sodium acetate are beneficial for the amperometric detection but not compatible with electrospray ionisation (ESI). Therefore a membrane-desalting device was installed after the splitter and prior to the ESI interface converting sodium hydroxide into water and sodium acetate into acetic acid. To enhance the sensitivity for the MS detection, 0.5 mmol/l lithium chloride was added after the membrane desalter to form lithium adducts of the carbohydrates. To compare sensitivity of IPAD and MS detection glucose, fructose, and sucrose were used as analytes. A calibration with external standards from 2.5 to 1000 pmole was performed showing a linear range over three orders of magnitude. Minimum detection limits (MDL) with IPAD were determined at 5 pmole levels for glucose to be 0.12 pmole, fructose 0.22 pmole and sucrose 0.11 pmole. With MS detection in the selected ion mode (SIM) the lithium adducts of the carbohydrates were detected obtaining MDL's for glucose of 1.49 pmole, fructose 1.19 pmole, and sucrose 0.36 pmole showing that under these conditions IPAD is 3-10 times more sensitive for those carbohydrates. The applicability of the method was demonstrated analysing carbohydrates in real world samples such as chicory inulin where polyfructans up to a molecular mass of 7000 g/mol were detected as quadrupoly charged lithium adducts. Furthermore mono-, di-, tri-, and oligosaccharides were detected in chicory coffee, honey and beer samples. PMID:16106855

  11. Controlled optical properties of water-soluble CdTe nanocrystals via anion exchange.

    PubMed

    Li, Jing; Jia, Jianguang; Lin, Yuan; Zhou, Xiaowen

    2016-02-01

    We report a study on anion exchange reaction of CdTe nanocrystals with S(2-) in aqueous solution under ambient condition. We found that the optical properties of CdTe nanocrystals can be well tuned by controlling the reaction conditions, in which the reaction temperature is crucially important. At low reaction temperature, the product nanocrystals showed blue-shifts in both absorption and PL spectra, while the photoluminescence quantum yield (PLQY) was significantly enhanced. When anion exchanges were carried out at higher reaction temperature, on the other hand, obvious red shifts in absorption and PL spectra accompanied by a fast increase followed by gradual decrease in PLQY were observed. On variation of S(2-) concentration, it was found that the overall kinetics of Te(2-) for S(2-) exchanges depends also on [S(2-)] when anion exchanges were performed at higher temperature. A possible mechanism for anion exchanges in CdTe NCs was proposed. PMID:26520812

  12. Impact of multiple re-use of anion-exchange chromatography media on virus removal.

    PubMed

    Norling, Lenore; Lute, Scott; Emery, Rachel; Khuu, Wynn; Voisard, Mark; Xu, Yuan; Chen, Qi; Blank, Greg; Brorson, Kurt

    2005-03-25

    We evaluated viral clearance in multiply-cycled anion-exchange media run in flow-through mode. We found that anion-exchange columns do not lose viral clearance capacity after extensive re-use, if they are cleaned with recommended buffers that do not chemically degrade the media. In contrast, anion-exchange (AEX) columns that are not cleaned or are cleaned with buffers that chemically degrade the media lost viral clearance capacity after extended use. In these cases, other performance attributes that changed at the same time were increased band spreading, decreased DNA clearance and accumulating backpressure that prevented re-use past 80-120 cycles. Thus, our data suggests that flow through mode anion-exchange columns that are cleaned with recommended cleaning buffers, and periodically monitored for band spreading, DNA clearance and/or backpressure need not be re-evaluated for viral clearance at the end of the validated media lifetime.

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

    PubMed

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

    2016-09-30

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

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

    PubMed

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

    2016-09-30

    Reactive chromatography using an anion exchange resin is proposed for a transesterification reaction of propylene glycol methyl ether (DOWANOL™ PM) with ethyl acetate to produce propylene glycol methyl ether acetate (DOWANOL™ PMA). This reaction is studied in batch and chromatographic reactors catalyzed by an anion exchange resin. Several anion exchange resins are tested and compared based on the performance of resin as an adsorbent and a catalyst. A chromatographic column is packed with a selected catalyst, AMBERLITE™ IRA904, and both reaction and chromatographic elution are studied at different temperatures and feed concentrations. The resulting chromatograms are fitted to a mathematical model to obtain adsorption equilibrium and reaction kinetic parameters by the inverse method. Compared to esterification investigated in a previous study, transesterification has advantages such as a higher conversion at lower temperature and easy removal of the byproduct which may lead to higher productivity. Deactivation of anion exchange resins is observed and potential solutions are suggested. PMID:27623064

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

    SciTech Connect

    Bartsch, R.A.; Zhang, Z.Y.; Elshani, S.; Zhao, W.; Jarvinen, G.D.; Barr, M.E.; Marsh, S.F.; Chamberlin, R.M.

    1999-06-01

    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 K{sub d} 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.

  16. Controlled optical properties of water-soluble CdTe nanocrystals via anion exchange.

    PubMed

    Li, Jing; Jia, Jianguang; Lin, Yuan; Zhou, Xiaowen

    2016-02-01

    We report a study on anion exchange reaction of CdTe nanocrystals with S(2-) in aqueous solution under ambient condition. We found that the optical properties of CdTe nanocrystals can be well tuned by controlling the reaction conditions, in which the reaction temperature is crucially important. At low reaction temperature, the product nanocrystals showed blue-shifts in both absorption and PL spectra, while the photoluminescence quantum yield (PLQY) was significantly enhanced. When anion exchanges were carried out at higher reaction temperature, on the other hand, obvious red shifts in absorption and PL spectra accompanied by a fast increase followed by gradual decrease in PLQY were observed. On variation of S(2-) concentration, it was found that the overall kinetics of Te(2-) for S(2-) exchanges depends also on [S(2-)] when anion exchanges were performed at higher temperature. A possible mechanism for anion exchanges in CdTe NCs was proposed.

  17. CATALYTIC PROMOTION OF THE ADSORPTION OF VANADIUM ON AN ANIONIC EXCHANGE RESIN

    DOEpatents

    Bailes, R.H.; Ellis, D.A.

    1958-08-26

    An improvement in the process for the recovery of vanadium from acidic phosphatic solutions is presented. In this process the vanadium is first oxidized to the pentavaleat state, and is then separated by contacting such solutions with an anion exchange resin whereby adsorption of the complexed pentavalent vanadium is effected. The improvement lies in the fact that adsorp tion of the vanadium complex by the anion exchange resin is promoted and improved by providing fiuoride ions in solution to be contacted.

  18. Automated small‐scale protein purification and analysis for accelerated development of protein therapeutics

    PubMed Central

    LeSaout, Xavier; Costioli, Matteo; Jordan, Lynn; Lambert, Jeremy; Beighley, Ross; Provencher, Laurel; McGuire, Kevin; Verlinden, Nico; Barry, Andrew

    2015-01-01

    Small‐scale protein purification presents opportunities for accelerated process development of biotherapeutic molecules. Miniaturization of purification conditions reduces time and allows for parallel processing of samples, thus offering increased statistical significance and greater breadth of variables. The ability of the miniaturized platform to be predictive of larger scale purification schemes is of critical importance. The PerkinElmer JANUS BioTx Pro and Pro‐Plus workstations were developed as intuitive, flexible, and automated devices capable of performing parallel small‐scale analytical protein purification. Preprogrammed methods automate a variety of commercially available ion exchange and affinity chromatography solutions, including miniaturized chromatography columns, resin‐packed pipette tips, and resin‐filled microtiter vacuum filtration plates. Here, we present a comparison of microscale chromatography versus standard fast protein LC (FPLC) methods for process optimization. In this study, we evaluated the capabilities of the JANUS BioTx Pro‐Plus robotic platform for miniaturized chromatographic purification of proteins with the GE ӒKTA Express system. We were able to demonstrate predictive analysis similar to that of larger scale purification platforms, while offering advantages in speed and number of samples processed. This approach is predictive of scale‐up conditions, resulting in shorter biotherapeutic development cycles and less consumed material than traditional FPLC methods, thus reducing time‐to‐market from discovery to manufacturing.

  19. Automated genomic DNA purification options in agricultural applications using MagneSil paramagnetic particles

    NASA Astrophysics Data System (ADS)

    Bitner, Rex M.; Koller, Susan C.

    2002-06-01

    The automated high throughput purification of genomic DNA form plant materials can be performed using MagneSil paramagnetic particles on the Beckman-Coulter FX, BioMek 2000, and the Tecan Genesis robot. Similar automated methods are available for DNA purifications from animal blood. These methods eliminate organic extractions, lengthy incubations and cumbersome filter plates. The DNA is suitable for applications such as PCR and RAPD analysis. Methods are described for processing traditionally difficult samples such as those containing large amounts of polyphenolics or oils, while still maintaining a high level of DNA purity. The robotic protocols have ben optimized for agricultural applications such as marker assisted breeding, seed-quality testing, and SNP discovery and scoring. In addition to high yield purification of DNA from plant samples or animal blood, the use of Promega's DNA-IQ purification system is also described. This method allows for the purification of a narrow range of DNA regardless of the amount of additional DNA that is present in the initial sample. This simultaneous Isolation and Quantification of DNA allows the DNA to be used directly in applications such as PCR, SNP analysis, and RAPD, without the need for separate quantitation of the DNA.

  20. Removal of dissolved organic matter by anion exchange: Effect of dissolved organic matter properties

    USGS Publications Warehouse

    Boyer, T.H.; Singer, P.C.; Aiken, G.R.

    2008-01-01

    Ten isolates of aquatic dissolved organic matter (DOM) were evaluated to determine the effect that chemical properties of the DOM, such as charge density, aromaticity, and molecular weight, have on DOM removal by anion exchange. The DOM isolates were characterized asterrestrial, microbial, or intermediate humic substances or transphilic acids. All anion exchange experiments were conducted using a magnetic ion exchange (MIEX) resin. The charge density of the DOM isolates, determined by direct potentiometric titration, was fundamental to quantifying the stoichiometry of the anion exchange mechanism. The results clearly show that all DOM isolates were removed by anion exchange; however, differences among the DOM isolates did influence their removal by MIEX resin. In particular, MIEX resin had the greatest affinity for DOM with high charge density and the least affinity for DOM with low charge density and low aromaticity. This work illustrates that the chemical characteristics of DOM and solution conditions must be considered when evaluating anion exchange treatment for the removal of DOM. ?? 2008 American Chemical Society.

  1. Quaternized poly (styrene-co-vinylbenzyl chloride) anion exchange membranes for alkaline water electrolysers

    NASA Astrophysics Data System (ADS)

    Vengatesan, S.; Santhi, S.; Jeevanantham, S.; Sozhan, G.

    2015-06-01

    In this study, poly (ST-co-VBC) based anion exchange membranes with different styrene to VBC ratios (1: 0.16, 1: 0.33 and 1: 1) have been prepared via chloromethylation-free synthetic route using aromatic vinyl monomers. The synthesized co-polymers are identified by FTIR and 1H-NMR analysis. Hydroxide (OH-) ion conductivity of the anion exchange membrane with styrene to VBC ratio of 1: 0.33 is as high as 6.8 × 10-3 S cm-1 in de-ionised water at 25 °C. The membrane also acquires the ion-exchange capacity of 2.14 meq. g-1, and the water uptake of 127%. Membrane-electrode-assembly (MEA) using the anion exchange membrane and Ni - foam catalyst demonstrate the current density of 40 mA cm-2 at 2.3 V in a water electrolyser cell.

  2. Preparation of High-Purity Cobalt by Anion-Exchange Separation and Plasma Arc Melting

    NASA Astrophysics Data System (ADS)

    Uchikoshi, Masahito; Shibuya, Hideka; Imaizumi, Junichi; Kékesi, Tamás; Mimura, Kouji; Isshiki, Minoru

    2010-04-01

    High-purity Co was prepared with valence-controlled anion-exchange separation, oxidation refining using plasma arc melting, and H2-Ar plasma arc melting on a pilot scale. The result of a laboratory-scale experiment indicated that the slower flow rate is more effective to remove the impurities by anion-exchange separation. However, the separation efficiency is reduced by scaling up the column from the laboratory to pilot scale. The discussion of the decrease in the separation efficiency implies that the distribution coefficient increases as the concentration of the adsorbate is lowered, but a reduced slower flow rate might increase the final purity of Co. In addition to anion-exchange separation, Co oxidation refining using plasma arc melting was useful. Consequently, a high-purity Co of 99.9998 pct by mass excluding gaseous elements was prepared, which represents the highest purity reported.

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

    PubMed

    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.

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

    PubMed

    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. PMID:27614730

  5. Hyper-branched anion exchange membranes with high conductivity and chemical stability.

    PubMed

    Ge, Qianqian; Liu, Yazhi; Yang, Zhengjin; Wu, Bin; Hu, Min; Liu, Xiaohe; Hou, Jianqiu; Xu, Tongwen

    2016-08-01

    In the manuscript, we report the design and preparation of hyper-branched polymer electrolytes intended for alkaline anion exchange membrane fuel cells. The resulting membrane exhibits high conductivity, lower water swelling and shows prolonged chemical stability under alkaline conditions. PMID:27456659

  6. DEMINERALIZER BUILDING, TRA608. CATION AND ANION EXCHANGERS LINE UP ALONG ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    DEMINERALIZER BUILDING, TRA-608. CATION AND ANION EXCHANGERS LINE UP ALONG NORTH WALL ON CONCRETE PLATFORMS. INL NEGATIVE NO. 2527. Unknown Photographer, 6/12/1951 - Idaho National Engineering Laboratory, Test Reactor Area, Materials & Engineering Test Reactors, Scoville, Butte County, ID

  7. Relationship of net chloride flow across the human erythrocyte membrane to the anion exchange mechanism

    SciTech Connect

    Knauf, P.A.; Law, F.Y.; Marchant, P.J.

    1983-01-01

    The parallel effects of the anion transport inhibitor DIDS (4,4'-diisothiocyanostilbene-2,2'disulfonate) on net chloride flow and on chloride exchange suggest that a major portion of net chloride flow takes place through the anion exchange system. The ''slippage'' model postulates that the rate of net anion flow is determined by the movement of the unloaded anion transport site across the membrane. Both the halide selectivity of net anion flow and the dependence of net chloride flux on chloride concentration over the range of 75 to 300 mM are inconsistent with the slippage model. Models in which the divalent form of the anion exchange carrier or water pores mediate net anion flow are also inconsistent with the data. The observations that net chloride flux increases with chloride concentration and that the DIDS-sensitive component tends to saturate suggest a model in which net anion flow involves ''transit'' of anions through the diffusion barriers in series with the transport site, without any change in transport site conformation such as normally occurs during the anion exchange process. This model is successful in predicting that the anion exchange inhibitor NAP-taurine, which binds to the modifier site and inhibits the conformational change, has less effect on net chloride flow than on chloride exchange.

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

    PubMed

    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.

  9. Properties of ionic liquids on Au surfaces: non-conventional anion exchange reactions with carbonate.

    PubMed

    Ratel, Mathieu; Branca, Mathieu; Breault-Turcot, Julien; Zhao, Sandy Shuo; Chaurand, Pierre; Schmitzer, Andreea R; Masson, Jean-Francois

    2011-10-14

    A simple anion metathesis in diluted aqueous carbonate at room temperature affords 1-(12-mercaptododecyl)-3-methyl-imidazolium carbonate (MDMI-HCO(3)) from MDMI salts self-assembled on gold films and nanoparticles. The properties of MDMI-SAM differ from MDMI in solution, for which the anion exchange reaction does not proceed. PMID:21879044

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

    NASA Technical Reports Server (NTRS)

    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.

  11. OXIDATIVE STRESS ACTIVATES ANION EXCHANGE PROTEIN 2 AND AP-1 IN AIRWAY EPITHELIAL CELLS

    EPA Science Inventory

    Anion exchange protein 2 (AE2) is a membrane-bound protein that mediates chloride-bicarbonate exchange. In addition to regulating intracellular pH and cell volume, AE2 exports superoxide (O.) to the extracellular matrix in an HCO-dependent process. Given this ability to export O....

  12. Comparison of automated and manual purification of total RNA for mRNA-based identification of body fluids.

    PubMed

    Akutsu, Tomoko; Kitayama, Tetsushi; Watanabe, Ken; Sakurada, Koichi

    2015-01-01

    Silica column-based RNA purification procedures have widespread use in mRNA profiling for body fluid identification in forensic samples. Also, automated RNA purification systems employing magnetic bead technology have recently become available. In this preliminary study, to ascertain which RNA purification technology is more suitable for the identification of body fluids by real-time reverse transcription polymerase chain reaction (RT-PCR), comparative analyses of the yield and quality of total RNA were performed between automated purification using an EZ1 Advanced Instrument and manual purification using an RNeasy Mini Kit. The yield and size distribution of total RNA were compared by gene expression analysis of two different sized fragments of the β-actin gene. In addition, the relative amounts of several target genes were compared between the purification methods, and the integrity of total RNA was determined by chip-based electrophoresis. The results of this study suggest that RNeasy can purify higher-quality RNA as compared with automated purification using EZ1. The sensitivity of the RT-PCR analysis, however, was higher in the EZ1-purified samples, likely due to the relative efficiency of EZ1 in extracting short-length RNA from degraded samples. We also show that the quantification of relative levels of body fluid-specific genes could be influenced by the purification procedure. Our results indicate that although use of high-quality RNA is generally required for reproducible results in gene expression analysis, the forensic relevance of short RNA fragments in highly degraded samples cannot be ruled out. Furthermore, our results suggest that automated purification procedures as well as silica column-based manual purification procedures can be used for mRNA-based body fluid identification in forensic samples.

  13. Comparison of automated and manual purification of total RNA for mRNA-based identification of body fluids.

    PubMed

    Akutsu, Tomoko; Kitayama, Tetsushi; Watanabe, Ken; Sakurada, Koichi

    2015-01-01

    Silica column-based RNA purification procedures have widespread use in mRNA profiling for body fluid identification in forensic samples. Also, automated RNA purification systems employing magnetic bead technology have recently become available. In this preliminary study, to ascertain which RNA purification technology is more suitable for the identification of body fluids by real-time reverse transcription polymerase chain reaction (RT-PCR), comparative analyses of the yield and quality of total RNA were performed between automated purification using an EZ1 Advanced Instrument and manual purification using an RNeasy Mini Kit. The yield and size distribution of total RNA were compared by gene expression analysis of two different sized fragments of the β-actin gene. In addition, the relative amounts of several target genes were compared between the purification methods, and the integrity of total RNA was determined by chip-based electrophoresis. The results of this study suggest that RNeasy can purify higher-quality RNA as compared with automated purification using EZ1. The sensitivity of the RT-PCR analysis, however, was higher in the EZ1-purified samples, likely due to the relative efficiency of EZ1 in extracting short-length RNA from degraded samples. We also show that the quantification of relative levels of body fluid-specific genes could be influenced by the purification procedure. Our results indicate that although use of high-quality RNA is generally required for reproducible results in gene expression analysis, the forensic relevance of short RNA fragments in highly degraded samples cannot be ruled out. Furthermore, our results suggest that automated purification procedures as well as silica column-based manual purification procedures can be used for mRNA-based body fluid identification in forensic samples. PMID:25270217

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

    PubMed

    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

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

    PubMed

    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.

  16. Automated modular preparative HPLC-MS purification laboratory with enhanced efficiency.

    PubMed

    Guth, Oliver; Krewer, Dietmar; Freudenberg, Björn; Paulitz, Christian; Hauser, Manfred; Ilg, Kerstin

    2008-01-01

    Automated parallel synthesis as tool to increase productivity in chemical synthesis is well-established. However, even more time-consuming than the synthesis process is the following purification of the resulting crude products. To enhance efficiency of the lead optimization process at Bayer CropScience, a high-throughput HPLC/MS-laboratory for the purification of up to 48 crude products per day in the range of 200-400 mg each in one injection per sample has been set up. The use of Covaris technology for HPLC sample preparation, automated aliquotation during fractionation, and a novel evaporation process by combination with freeze-drying are new key technologies applied successfully for the first time in this purification unit facilitating to achieve the targeted efficiency. The whole process is supported by a specially designed IT-landscape covering each step of the workflow. Both the technical instruments used within the laboratory and the workflow and IT platform are described in this article.

  17. Automated centrifugal-microfluidic platform for DNA purification using laser burst valve and coriolis effect.

    PubMed

    Choi, Min-Seong; Yoo, Jae-Chern

    2015-04-01

    We report a fully automated DNA purification platform with a micropored membrane in the channel utilizing centrifugal microfluidics on a lab-on-a-disc (LOD). The microfluidic flow in the LOD, into which the reagents are injected for DNA purification, is controlled by a single motor and laser burst valve. The sample and reagents pass successively through the micropored membrane in the channel when each laser burst valve is opened. The Coriolis effect is used by rotating the LOD bi-directionally to increase the purity of the DNA, thereby preventing the mixing of the waste and elution solutions. The total process from the lysed sample injection into the LOD to obtaining the purified DNA was finished within 7 min with only one manual step. The experimental result for Salmonella shows that the proposed microfluidic platform is comparable to the existing devices in terms of the purity and yield of DNA.

  18. Transmembrane protein 139 (TMEM139) interacts with human kidney isoform of anion exchanger 1 (kAE1).

    PubMed

    Nuiplot, Nalin-On; Junking, Mutita; Duangtum, Natapol; Khunchai, Sasiprapa; Sawasdee, Nunghathai; Yenchitsomanus, Pa-Thai; Akkarapatumwong, Varaporn

    2015-08-01

    Human kidney anion exchanger 1 (kAE1) mediates Cl(-)/HCO3(-) exchanges at the basolateral membrane of the acid-secreting α-intercalated cells. Mutations in SLC4A1 gene encoding kAE1 are associated with distal renal tubular acidosis (dRTA). Several studies have shown that impaired trafficking of the mutant kAE1 is an important molecular mechanism underlying the pathogenesis of dRTA. Proteins involved in kAE1 trafficking were identified but the mechanism resulting in dRTA remained unclear. Thus, this study attempted to search for additional proteins interacting with C-terminal of kAE1 (Ct-kAE1) and involved in kAE1 trafficking to cell membrane. Transmembrane protein 139 (TMEM139) was identified as a protein interacting with Ct-kAE1 by yeast two-hybrid screening. The interaction between kAE1 and TMEM139 was confirmed by affinity co-purification, co-immunoprecipitation (co-IP) and yellow fluorescent protein (YFP)-based protein fragment complementation assay (PCA). In addition, flow cytometry results showed that suppression of endogenous TMEM139 by small interfering RNA (siRNA) and over-expression of TMEM139 in HEK293T cells could reduce and increase membrane localization of kAE1, respectively. The presented data demonstrate that TMEM139 interacts with kAE1 and promotes its intracellular trafficking. PMID:26049106

  19. Evaluation of automated and manual DNA purification methods for detecting Ricinus communis DNA during ricin investigations.

    PubMed

    Hutchins, Anne S; Astwood, Michael J; Saah, J Royden; Michel, Pierre A; Newton, Bruce R; Dauphin, Leslie A

    2014-03-01

    In April of 2013, letters addressed to the President of United States and other government officials were intercepted and found to be contaminated with ricin, heightening awareness about the need to evaluate laboratory methods for detecting ricin. This study evaluated commercial DNA purification methods for isolating Ricinus communis DNA as measured by real-time polymerase chain reaction (PCR). Four commercially available DNA purification methods (two automated, MagNA Pure compact and MagNA Pure LC, and two manual, MasterPure complete DNA and RNA purification kit and QIAamp DNA blood mini kit) were evaluated. We compared their ability to purify detectable levels of R. communis DNA from four different sample types, including crude preparations of ricin that could be used for biological crimes or acts of bioterrorism. Castor beans, spiked swabs, and spiked powders were included to simulate sample types typically tested during criminal and public health investigations. Real-time PCR analysis indicated that the QIAamp kit resulted in the greatest sensitivity for ricin preparations; the MasterPure kit performed best with spiked powders. The four methods detected equivalent levels by real-time PCR when castor beans and spiked swabs were used. All four methods yielded DNA free of PCR inhibitors as determined by the use of a PCR inhibition control assay. This study demonstrated that DNA purification methods differ in their ability to purify R. communis DNA; therefore, the purification method used for a given sample type can influence the sensitivity of real-time PCR assays for R. communis.

  20. Role of urea on recombinant Apo A-I stability and its utilization in anion exchange chromatography.

    PubMed

    Angarita, Monica; Arosio, Paolo; Müller-Späth, Thomas; Baur, Daniel; Falkenstein, Roberto; Kuhne, Wolfgang; Morbidelli, Massimo

    2014-08-01

    Apolipoprotein A-I (Apo A-I) is an important lipid-binding protein involved in the transport and metabolism of cholesterol. High protein purity, in particular with respect to endotoxins is required for therapeutic applications. The use of urea during the purification process of recombinant Apo A-I produced in Escherichia coli has been suggested so as to provide high endotoxin clearance. In this work, we show that urea can be used as a sole modifier during the ion exchange chromatographic purification of Apo A-I and we investigate the molecular mechanism of elution by correlating the effect of urea on self-association, conformation and adsorption equilibrium properties of a modified model Apo A-I. In the absence of urea the protein was found to be present as a population of oligomers represented mainly by trimers, hexamers and nonamers. The addition of urea induced oligomer dissociation and protein structure unfolding. We correlated the changes in protein association and conformation with variations of the adsorption equilibrium of the protein on a strong anion exchanger. It was confirmed that the adsorption isotherms, described by a Langmuir model, were dependent on both protein and urea concentrations. Monomers, observed at low urea concentration (0.5M), were characterized by larger binding affinity and adsorption capacity compared to both protein oligomers (0M) and unfolded monomers (2-8M). The reduction of both the binding strength and maximum adsorption capacity at urea concentrations larger than 0.5M explains the ability of urea of inducing elution of the protein from the ion exchange resin. The dissociation of the protein complexes occurring during the elution could likely be the origin of the effective clearance of endotoxins originally trapped inside the oligomers.

  1. Formation of pseudomorphic nanocages from Cu2O nanocrystals through anion exchange reactions.

    PubMed

    Wu, Hsin-Lun; Sato, Ryota; Yamaguchi, Atsushi; Kimura, Masato; Haruta, Mitsutaka; Kurata, Hiroki; Teranishi, Toshiharu

    2016-03-18

    The crystal structure of ionic nanocrystals (NCs) is usually controlled through reaction temperature, according to their phase diagram. We show that when ionic NCs with different shapes, but identical crystal structures, were subjected to anion exchange reactions under ambient conditions, pseudomorphic products with different crystal systems were obtained. The shape-dependent anionic framework (surface anion sublattice and stacking pattern) of Cu2O NCs determined the crystal system of anion-exchanged products of CuxS nanocages. This method enabled us to convert a body-centered cubic lattice into either a face-centered cubic or a hexagonally close-packed lattice to form crystallographically unusual, multiply twinned structures. Subsequent cation exchange reactions produced CdS nanocages while preserving the multiply-twinned structures. A high-temperature stable phase such as wurtzite ZnS was also obtained with this method at ambient conditions. PMID:26989249

  2. Mechanism of Polysulfone-Based Anion Exchange Membranes Degradation in Vanadium Flow Battery.

    PubMed

    Yuan, Zhizhang; Li, Xianfeng; Zhao, Yuyue; Zhang, Huamin

    2015-09-01

    The stability of hydrocarbon ion exchange membranes is one of the critical issues for a flow battery. However, the degradation mechanism of ion exchange membranes has been rarely investigated especially for anion exchange membranes. Here, the degradation mechanism of polysulfone based anion exchange membranes, carrying pyridine ion exchange groups, under vanadium flow battery (VFB) medium was investigated in detail. We find that sp(2) hybrid orbital interactions between pyridinic-nitrogen in 4,4'-bipyridine and benzylic carbon disrupt the charge state balance of pristine chloromethylated polysulfone. This difference in electronegativity inversely induces an electrophilic carbon center in the benzene ring, which can be attacked by the lone pair electron on the vanadium(V) oxygen species, further leading to the degradation of polymer backbone, while leaving the 4,4'-bipyridine ion exchange groups stable. This work represents a step toward design and construction of alternative type of chemically stable hydrocarbon ion exchange membranes for VFB. PMID:26284752

  3. Tuning the Optical Properties of Cesium Lead Halide Perovskite Nanocrystals by Anion Exchange Reactions

    PubMed Central

    2015-01-01

    We demonstrate that, via controlled anion exchange reactions using a range of different halide precursors, we can finely tune the chemical composition and the optical properties of presynthesized colloidal cesium lead halide perovskite nanocrystals (NCs), from green emitting CsPbBr3 to bright emitters in any other region of the visible spectrum, and back, by displacement of Cl– or I– ions and reinsertion of Br– ions. This approach gives access to perovskite semiconductor NCs with both structural and optical qualities comparable to those of directly synthesized NCs. We also show that anion exchange is a dynamic process that takes place in solution between NCs. Therefore, by mixing solutions containing perovskite NCs emitting in different spectral ranges (due to different halide compositions) their mutual fast exchange dynamics leads to homogenization in their composition, resulting in NCs emitting in a narrow spectral region that is intermediate between those of the parent nanoparticles. PMID:26214734

  4. TGR5 potentiates GLP-1 secretion in response to anionic exchange resins.

    PubMed

    Harach, Taoufiq; Pols, Thijs W H; Nomura, Mitsunori; Maida, Adriano; Watanabe, Mitsuhiro; Auwerx, Johan; Schoonjans, Kristina

    2012-01-01

    Anionic exchange resins are bona fide cholesterol-lowering agents with glycemia lowering actions in diabetic patients. Potentiation of intestinal GLP-1 secretion has been proposed to contribute to the glycemia lowering effect of these non-systemic drugs. Here, we show that resin exposure enhances GLP-1 secretion and improves glycemic control in diet-induced animal models of "diabesity", effects which are critically dependent on TGR5, a G protein-coupled receptor that is activated by bile acids. We identified the colon as a major source of GLP-1 secretion after resin treatment. Furthermore, we demonstrate that the boost in GLP-1 release by resins is due to both enhanced TGR5-dependent production of the precursor transcript of GLP-1 as well as to the local enrichment of TGR5 agonists in the colon. Thus, TGR5 represents an essential component in the pathway mediating the enhanced GLP-1 release in response to anionic exchange resins. PMID:22666533

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

    PubMed

    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. The dynamics of sorption of sulfuric acid by weakly basic polyacrylic anion exchangers

    NASA Astrophysics Data System (ADS)

    Mamchenko, A. V.; Kushnir, T. V.

    2009-05-01

    The nonequilibrium dynamics of sorption of sulfuric acid by free base forms of Amberlite IRA-67 and Lewatite VP.OC.1072 weakly basic anion exchangers is studied. It is established that, in hydrodynamic regimes of filtration, which are typical of OH filters of the first stage of water-desalting plants, the limiting stage of sorption kinetics is inside diffusion. It is concluded that the process is correctly described by an asymptotic solution to the inside-diffusion model of sorption dynamics.

  7. Test procedure for anion exchange testing with Argonne 10-L solutions

    SciTech Connect

    Compton, J.A.

    1995-05-17

    Four anion exchange resins will be tested to confirm that they will sorb and release plutonium from/to the appropriate solutions in the presence of other cations. Certain cations need to be removed from the test solutions to minimize adverse behavior in other processing equipment. The ion exchange resins will be tested using old laboratory solutions from Argonne National Laboratory; results will be compared to results from other similar processes for application to all plutonium solutions stored in the Plutonium Finishing Plant.

  8. Sorption and binary exchange of nitrate, sulfate, and uranium on an anion-exchange resin.

    PubMed

    Gu, Baohua; Ku, Yee-Kyoung; Jardine, Philip M

    2004-06-01

    Competitive ion-exchange reactions were studied on a strong-base anion-exchange resin to remove NO3- and uranium from a contaminated groundwater containing high levels of NO3- (approximately 140 mM), SO4(2-) (approximately 10 mM), and U(VI) (approximately 0.2 mM). Results indicate that although SO4(2-) carries divalent negative charges, it showed the least selectivity for sorption by the Purolite A-520E resin, which is functionalized with triethylamine exchange sites. Nitrate was the most strongly sorbed. Sorption selectivity followed the order of NO3- > Cl- > SO4(2-) under the experimental conditions. Nitrate competitively sorbed and displaced previously sorbed SO4(2-) in a column flow-through experiment and resulted in a high elution front of SO4(2-) in the effluent. Although the concentration of uranium in groundwater is orders of magnitude lower than that of NO3- or SO4(2-), it was found to be strongly sorbed by the anion-exchange resin. Because the most stable uranium species in oxic and suboxic environments is the UO2(2+) cation, its strong sorption by anion-exchange resins is hypothesized to be the result of the co-ion effect of NO3- by forming anionic UO2(NO3)3- complexes in the resin matrix. These observations point out a potential alternative remediation strategy that uses strong-base anion-exchange resins to remove uranium from this site-specific groundwater, which has a low pH and a relatively high NO3- concentration.

  9. Preparation, Characterization and Anion Exchange Properties of Polypyrrole/Carbon Nanotube Nanocomposite

    SciTech Connect

    Cui, Xiaoli; Engelhard, Mark H.; Lin, Yuehe

    2006-02-01

    In this study, polypyrrole (PPy) thin film was electrodeposited on carbon nanotube (CNT) backbones by applying a constant deposition potential in solution with 0.1 M pyrrole with different electrolytes such as NaCl, NaNO3, or NaClO4. The hybrid films were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, and cyclic voltammetry. SEM images revealed the nanostructrure of PPy film generated on CNTs surface. The electrochemical and anion exchange properties of PPy-CNT composite film have been investigated. Nanostructured composite thin films of polypyrrole/CNTs were studied by cyclic voltammetry between 0.4 and -0.8 V in aqueous solution to evaluate their cycling stability and capacity for electrically switched anion exchange. It is found that the PPy/CNTs nanocomposites can improve the anion exchange capacity and stability of the PPy-CNTs composite film, which may be attributed to the nanostructure of the polypyrrole film, which offer the high aspect ratio of the film and ease of diffusion of anions in the nanostructured film, and the interaction between CNTs and PPy.

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

    PubMed

    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.

  11. Renewable Microcolumns for Automated DNA Purification and Flow-through Amplification: From Sediment Samples through Polymerase Chain Reaction

    SciTech Connect

    Bruckner-Lea, Cindy J. ); Tsukuda, Toyoko ); Dockendorff, Brian P. ); Follansbee, James C. ); Kingsley, Mark T. ); Ocampo, Catherine O.; Stults, Jennie R.; Chandler, Darrell P.

    2001-12-01

    There is an increasing need for field-portable systems for the detection and characterization of microorganisms in the environment. Nucleic acids analysis is frequently the method of choice for discriminating between bacteria in complex systems, but standard protocols are difficult to automate and current microfluidic devices are not configured specifically for environmental sample analysis. In this report, we describe the development of an integrated DNA purification and PCR amplification system and demonstrate its use for the automated purification and amplification of Geobacter chapelli DNA (genomic DNA or plasmid targets) from sediments. The system includes renewable separation columns for the automated capture and release of microparticle purification matrices, and can be easily reprogrammed for new separation chemistries and sample types. The DNA extraction efficiency for the automated system ranged from 3 to 25 percent, depending on the length and concentration of the DNA target . The system was more efficient than batch capture methods for the recovery of dilute genomic DNA even though the reagen volumes were smaller than required for the batch procedure. The automated DNA concentration and purification module was coupled to a flow-through, Peltier-controlled DNA amplification chamber, and used to successfully purify and amplify genomic and plasmid DNA from sediment extracts. Cleaning protocols were also developed to allow reuse of the integrated sample preparation system, including the flow-through PCR tube.

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

    NASA Astrophysics Data System (ADS)

    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.

  13. 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.

    PubMed

    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.

  14. Removal of fluorescent dissolved organic matter in biologically treated textile effluents by NDMP anion exchange process: efficiency and mechanism.

    PubMed

    Li, Wen-Tao; Xu, Zi-Xiao; Shuang, Chen-Dong; Zhou, Qing; Li, Hai-Bo; Li, Ai-Min

    2016-03-01

    The efficiency and mechanism of anion exchange resin Nanda Magnetic Polymer (NDMP) for removal of fluorescent dissolved organic matter in biologically treated textile effluents were studied. The bench-scale experiments showed that as well as activated carbon, anion exchange resin could efficiently remove both aniline-like and humic-like fluorescent components, which can be up to 40 % of dissolved organic matter. The humic-like fluorescent component HS-Em460-Ex3 was more hydrophilic than HS-Em430-Ex2 and contained fewer alkyl chains but more acid groups. As a result, HS-Em460-Ex3 was eliminated more preferentially by NDMP anion exchange. However, compared with adsorption resins, the polarity of fluorescent components had a relatively small effect on the performance of anion exchange resin. The long-term pilot-scale experiments showed that the NDMP anion exchange process could remove approximately 30 % of the chemical oxygen demand and about 90 % of color from the biologically treated textile effluents. Once the issue of waste brine from resin desorption is solved, the NDMP anion exchange process could be a promising alternative for the advanced treatment of textile effluents. PMID:26578375

  15. Mono- and polyprotic buffer systems in anion exchange chromatography of influenza virus particles.

    PubMed

    Vajda, Judith; Weber, Dennis; Stefaniak, Sabine; Hundt, Boris; Rathfelder, Tanja; Müller, Egbert

    2016-05-27

    Different ions typically used in downstream processing of biologicals are evaluated for their potential in anion exchange chromatography of an industrially produced, pandemic influenza H1N1 virus. Capacity, selectivity and recovery are investigated based on single step elution parallel chromatography experiments. The inactivated H1N1 feedstream is produced in Madin-Darby Bovine Kidney cells. Interesting effects are found for sodium phosphate and sodium citrate. Both anions are triprotic kosmotropes. Anion exchange chromatography generally offers high scalability to satisfy sudden demands for vaccines, which may occur in case of an emerging influenza outbreak. Appropriate pH conditions for H1N1 adsorption are determined by Zeta potential measurements. The dynamic binding capacity of a salt tolerant polyamine-type resin is up to 6.4 times greater than the capacity of a grafted Q-type resin. Pseudo-affinity interactions of polyamines with the M2 protein of influenza may contribute to the obtained capacity increase. Both resins achieve greater capacity in sodium phosphate buffer compared to Tris/HCl. A recovery of 67% and DNA clearance close to 100% without DNAse treatment are achieved for the Q-type resin. Recovery of the virus from the salt tolerant resin requires the use of polyprotic acids in the elution buffer. 85% of the DNA and 60% of the proteins can be removed by the salt tolerant resin. The presence of sodium phosphate during anion exchange chromatography seems to support stability of the H1N1 particles in presence of hydrophobic cations. PMID:27130581

  16. An instrument for automated purification of nucleic acids from contaminated forensic samples.

    PubMed

    Broemeling, David J; Pel, Joel; Gunn, Dylan C; Mai, Laura; Thompson, Jason D; Poon, Hiron; Marziali, Andre

    2008-02-01

    Forensic crime scene sample analysis, by its nature, often deals with samples in which there are low amounts of nucleic acids, on substrates that often lead to inhibition of subsequent enzymatic reactions such as PCR amplification for STR profiling. Common substrates include denim from blue jeans, which yields indigo dye as a PCR inhibitor, and soil, which yields humic substances as inhibitors. These inhibitors frequently co-extract with nucleic acids in standard column or bead-based preps, leading to frequent failure of STR profiling. We present a novel instrument for DNA purification of forensic samples that is capable of highly effective concentration of nucleic acids from soil particulates, fabric, and other complex samples including solid components. The novel concentration process, known as SCODA, is inherently selective for long charged polymers such as DNA, and therefore is able to effectively reject known contaminants. We present an automated sample preparation instrument based on this process, and preliminary results based on mock forensic samples.

  17. Reactive oxygen species accelerate degradation of anion exchange membranes based on polyphenylene oxide in alkaline environments.

    PubMed

    Parrondo, Javier; Wang, Zhongyang; Jung, Min-Suk J; Ramani, Vijay

    2016-07-20

    Anion exchange membranes (AEM) based on polyphenylene oxide (PPO) suffered quaternary-ammonium-cation-site degradation in alkaline environments. Surprisingly, the degradation rate was considerably faster in the presence of molecular oxygen. We postulated that the AEM cation-site catalyzes the reduction of dioxygen by hydroxide ions to yield the superoxide anion radical and the highly reactive hydroxyl free radical. We substantiated our hypothesis by using a phosphorous-containing spin trap (5-diisopropoxy-phosphoryl-5-methyl-1-pyrroline-N-oxide) to detect the adducts for both free radicals in situ using (31)P-NMR spectroscopy. PMID:27381009

  18. Relationships of anion-exchange sorption of boron from natural thermal-spring water

    SciTech Connect

    Meichik, N.R.; Leikin, Yu.A.; Antipov, M.A.; Goryacheva, N.V.; Klimenko, I.S.; Medvedev, S.A.; Galitskaya, N.B.

    1988-02-20

    Boric acid is one of the characteristic components of Kamchatka waters. Extraction of boron from thermal waters for production of potable water is closely linked with current problems of multiproduct utilization of resources and protection of the environment. The authors have investigated the possibilities of using ion exchange for extraction of boron from natural waters, and studied the sorption relationships by a dynamic method. They synthesized a macroporous anion-exchanger based on a copolymer of styrene with divinylbenzene, containing N-methylglucamine groups (ANB-11 resin). ANB-11 resin had high sorption capacity for boron anions during sorption from thermal-spring water. The experimental data were described by Elkins equation.

  19. Bifunctional anion-exchange resins with improved selectivity and exchange kinetics

    DOEpatents

    Alexandratos, Spiro D.; Brown, Gilbert M.; Bonnesen, Peter V.; Moyer, Bruce A.

    2000-01-01

    Disclosed herein are a class of anion exchange resins containing two different exchange sites with improved selectivity and sorptive capability for chemical species in solution, such as heptavalent technetium (as pertechnetate anion, TcO.sub.4.sup.-). The resins are prepared by first reacting haloalkylated crosslinked copolymer beads with a large tertiary amine in a solvent in which the resin beads can swell, followed by reaction with a second, smaller, tertiary amine to more fully complete the functionalization of the resin. The resins have enhanced selectivity, capacity, and exchange kinetics.

  20. Donnan dialysis of transition metal ions using anion exchange membrane modified with Xylenol Orange

    SciTech Connect

    Sawicka, B.; Brajter, K.; Trojanowicz, M.; Kado, B. )

    1991-01-01

    A chelating ion-exchange membrane was obtained by modification of a PTFE-based anion-exchange membrane with Xylenol Orange. Its utility for dialysis of Cu(II), Ni(II), Mn(II), and Zn(II) was investigated by using receiver solutions without and with iminodiacetate. 1,2-diaminocyclohexanetetraacetic acid, and tetraethylenepentamine. In comparison to commercial PTFE cation-exchange membranes, modified chelating membranes exhibit for the metal ions investigated a larger differentiation of retention in the membrane phase and transport-to-receiver solution depending on the modifier used and the composition of the receiver solution.

  1. Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

    USGS Publications Warehouse

    Chao, T.T.; Fishman, M. J.; Ball, J.W.

    1969-01-01

    A method has been developed for the accurate determination of 0.1-1 ??g of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1-10 ??g 1 range can be determined by extraction without pre-concentration on an ion-exchange resin. ?? 1969.

  2. Test plan for anion exchange testing with Argonne 10-L solutions

    SciTech Connect

    Compton, J.A.

    1995-05-10

    The purpose of this test plan is to determine the performance characteristics of four anion exchange resins. This information is required to scale up an ion exchange process for removing undesirable chemicals from calciner feed at PFP. The performance characteristics will be judged by comparing the total exchange capacity, the sorption and desorption of plutonium, the distribution coefficient, and other operating information in the presence of various complexing anions. The results will be compared to a similar process using organic extractants to determine the best way of removing the undesirable chemicals from the plutonium solutions.

  3. Preparative isolation of the lectin jacalin by anion-exchange high-performance liquid chromatography.

    PubMed

    De Simone, S G; Santos, R; Araujo, M F; Pinho, R T

    1994-12-30

    The lectin jacalin from Artocarpus integrifolia was purified to homogeneity in a single step by preparative anion-exchange high-performance liquid chromatography (HPLC). Selection of the optimum chromatographic parameters in gradient elution allowed a rapid procedure to be obtained for the qualitative and quantitative isolation of the most important alpha- and alpha'-jacalin components. A recovery of 27-33% was obtained from a total soluble extract using a polyacrylate-DEAE HPLC column. The identities of the two isolated polypeptides were established by N-terminal amino acid sequence analysis and from the IgA1 binding lectin activity.

  4. TREATMENT FOR IMPROVING THE OPERATION OF STRONG BASE ANION EXCHANGE RESINS

    DOEpatents

    Stevenson, P.C.

    1960-11-29

    A process is offered for improving quaternary ammonium type strongly basic anion exchange resins so that centain zinc and cadmium residues, which normally stick to and "poison" this type of resin, can be removed by elution. Specifically, the resin as obtained commercially is treated with an aqueous solution of sodium hydroxide of about 1 to 4 M concentration by heating therein and periodically adding small amounts of oxidizing agent selected from hydrogen peroxide, sodium peroxide and hypochlorite. Zinc and cadmium values may then be adsorbed onto the resin from a 0.1 to 3 M HCl and thereafter eluted therefrom with very dilute HCl solutions.

  5. Solvent Processable Tetraalkylammonium-Functionalized Polyethylene for Use as an Alkaline Anion Exchange Membrane

    SciTech Connect

    Kostalik, IV, Henry A.; Clark, Timothy J.; Robertson, Nicholas J.; Mutolo, Paul F.; Longo, Julie M.; Abruña, Héctor D.; Coates, Geoffrey W.

    2010-08-02

    We report the synthesis of a solvent processable, tetraalkylammonium-functionalized polyethylene for use as an alkaline anion exchange membrane (AAEM). The membranes are insoluble in both pure water and aqueous methanol (50 vol % water) at 50 °C but exhibit excellent solubility in a variety of other aqueous alcohols (e.g., 5 wt % AAEM in aqueous n-propanol, 50 vol % water). These solubility characteristics extend the potential utility of this system for use as both an AAEM and ionomer electrode material from a single polymer composition. The AAEMs generated are mechanically strong and exhibit high hydroxide and carbonate conductivities.

  6. Automated hydrophobic interaction chromatography column selection for use in protein purification.

    PubMed

    Murphy, Patrick J M; Stone, Orrin J; Anderson, Michelle E

    2011-01-01

    In contrast to other chromatographic methods for purifying proteins (e.g. gel filtration, affinity, and ion exchange), hydrophobic interaction chromatography (HIC) commonly requires experimental determination (referred to as screening or "scouting") in order to select the most suitable chromatographic medium for purifying a given protein (1). The method presented here describes an automated approach to scouting for an optimal HIC media to be used in protein purification. HIC separates proteins and other biomolecules from a crude lysate based on differences in hydrophobicity. Similar to affinity chromatography (AC) and ion exchange chromatography (IEX), HIC is capable of concentrating the protein of interest as it progresses through the chromatographic process. Proteins best suited for purification by HIC include those with hydrophobic surface regions and able to withstand exposure to salt concentrations in excess of 2 M ammonium sulfate ((NH(4;))(2;)SO(4;)). HIC is often chosen as a purification method for proteins lacking an affinity tag, and thus unsuitable for AC, and when IEX fails to provide adequate purification. Hydrophobic moieties on the protein surface temporarily bind to a nonpolar ligand coupled to an inert, immobile matrix. The interaction between protein and ligand are highly dependent on the salt concentration of the buffer flowing through the chromatography column, with high ionic concentrations strengthening the protein-ligand interaction and making the protein immobile (i.e. bound inside the column) (2). As salt concentrations decrease, the protein-ligand interaction dissipates, the protein again becomes mobile and elutes from the column. Several HIC media are commercially available in pre-packed columns, each containing one of several hydrophobic ligands (e.g. S-butyl, butyl, octyl, and phenyl) cross-linked at varying densities to agarose beads of a specific diameter (3). Automated column scouting allows for an efficient approach for determining

  7. Controlling Disorder and Superconductivity in Titanium Oxynitride Nanoribbons with Anion Exchange.

    PubMed

    Sluban, Melita; Umek, Polona; Jagličić, Zvonko; Buh, Jože; Šmitek, Petra; Mrzel, Aleš; Bittencourt, Carla; Guttmann, Peter; Delville, Marie-Helene; Mihailović, Dragan; Arčon, Denis

    2015-10-27

    In recent years, conversion chemical reactions, which are driven by ion diffusion, emerged as an important concept for formation of nanoparticles. Here we demonstrate that the slow anion diffusion in anion exchange reactions can be efficiently used to tune the disorder strength and the related electronic properties of nanoparticles. This paradigm is applied to high-temperature formation of titanium oxynitride nanoribbons, Ti(O,N), transformed from hydrogen titanate nanoribbons in an ammonia atmosphere. The nitrogen content, which determines the chemical disorder through random O/N occupancy and ion vacancies in the Ti(O,N) composition, increases with the reaction time. The presence of disorder has paramount effects on resistivity of Ti(O,N) nanoribbons. Atypically for metals, the resistivity increases with decreasing temperature due to the weak localization effects. From this state, superconductivity develops below considerably or completely suppressed critical temperatures, depending on the disorder strength. Our results thus establish the remarkable versatility of anion exchange for tuning of the electronic properties of Ti(O,N) nanoribbons and suggest that similar strategies may be applied to a vast number of nanostructures.

  8. A green approach for preparing anion exchange membrane based on cardo polyetherketone powders

    NASA Astrophysics Data System (ADS)

    Hu, Jue; Zhang, Chengxu; Zhang, Xiaodong; Chen, Longwei; Jiang, Lin; Meng, Yuedong; Wang, Xiangke

    2014-12-01

    Anion exchange membranes (AEMs) have attracted great attention due to their irreplaceable role in platinum-free fuel cell applications. The majority of AEM preparations have been performed in two steps: the grafting of functional groups and quaternization. Here, we adopted a simpler, more eco-friendly approach for the first time to prepare AEMs by atmospheric-pressure plasma-grafting. This approach enables the direct introduction of anion exchange groups (benzyltrimethylammonium groups) into the polymer matrix, overcoming the need for toxic chloromethyl ether and quaternization reagents. Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and 1H NMR spectroscopy results demonstrate that benzyltrimethylammonium groups have been successfully grafted into the cardo polyetherketone (PEK-C) matrix. Thermogravimetric analysis reveals that the plasma-grafting technique is a facile and non-destructive method able to improve the thermal stability of the polymer matrix due to the strong preservation of the PEK-C backbone structure and the cross-linking of the grafted side chains. The plasma-grafted PG-NOH membrane, which shows satisfactory alcohol resistance (ethanol permeability of 6.3 × 10-7 cm2 s-1), selectivity (1.2 × 104 S s cm-3), thermal stability (safely used below 130 °C), chemical stability, anion conductivity (7.7 mS cm-1 at 20 °C in deionized water) and mechanical properties is promising for the construction of high-performance fuel cells.

  9. Isotope Fractionation of chlorine in Aqueous System: One Study on Anion-Exchange Chromatography.

    NASA Astrophysics Data System (ADS)

    Musashi, M.; Oi, T.; Eggenkamp, H.; Van Cappellen, P.

    2001-05-01

    Stable chlorine isotopes such as 37Cl and 35Cl have been paid attention as useful tool identifying the source, and monitoring the transport process and natural fate of chlorinated organic pollutants in air and groundwater. However, it is not established yet whether any isotope effects accompany biodegradation or reductive dehalogenation of the pollutants (Clark and Fritz, 1997). Here we first present an experimental determination of isotope fractionation factor of chlorine in aqueous system by using anion-exchange chromatographic technique. Into the Cl-free anion exchange resin (Muromac, OH- form) packed in a 30 cm long pyrex glass column and controlled temperature at 25 oC, hydrochloric solution was fed with controlling the flow rate constant. Effluent from the column was recovered by an automatic fraction collector and prepared for Cl isotope analysis. The Cl isotope ratio (δ 37Cl vs. SMOC) was measured by IR-MS at the Utrecht University with precision of 0.06 per-mil. Magnitude of the factor obtained was 1.00035 at 25 oC. The result indicates that the lighter isotope (35Cl) was preferably fractionated into the resin phase, while the heavier one (37Cl) was enriched into the aqueous phase. This trend suggests that molecular structure of hydrolysis with Cl in aqueous phase may be more stable than that of Cl ionically bonding with the resin. This result may offer physico-chemical insights into behavior and fate of the pollutants.

  10. Quantitative H-1 NMR Analysis of Chemical Stabilities in Anion-Exchange Membranes

    SciTech Connect

    Nunez, SA; Hickner, MA

    2013-01-01

    We compared the alkaline stability of three classes of anion exchange membranes that are leading candidates for applications in platinum-free fuel cells. A methodology is presented for the study of chemical stability of anion-exchange polymers in alkaline media that provides clear and quantitative H-1 NMR spectroscopic data of dissolved polymers containing benzyltrimethylammonium functionalities. Recent studies have investigated the stabilities of benzimidazolium- and alkylimidazolium-bearing polymers using periodic H-1 NMR sampling. These studies included varying alkaline concentrations, external heating sources, and excessive processing and contained no internal standard for absolute measurements. Key aspects of our time-resolved H-1 NMR method include in situ heating and sampling within the spectrometer, fixed Stoichiometric relationships between the benzyltrimethylammonium functionalities of each polymer and potassium deuteroxide (KOD), and the incorporation of an internal standard for the absolute measurement of the polymer degradation. In addition, our method permits the identification of the degradation products to find the underlying cause of chemical lability. Our results demonstrate that a styrene-based polymer containing benzyltrimethylammonium functional groups is remarkably stable when exposed to 20 equivalents per cation of KOD at 80 degrees C with a half-life (t(1/2)) of 231 h. Under these standard conditions, functionalized poly(phenylene oxide) and poly(arylene ether sulfone) copolymers, both bearing benzyltrimethylammonium functionalities were found to degrade with a half-lives of 57.8 and 2.7 h, respectively.

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

    PubMed

    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.

  12. The recovery of zinc from hot galvanizing slag in an anion-exchange membrane electrolysis reactor.

    PubMed

    Ren, Xiulian; Wei, Qifeng; Hu, Surong; Wei, Sijie

    2010-09-15

    This paper reports the optimization of the process parameters for recovery of zinc from hot galvanizing slag in an anion-exchange membrane electrolysis reactor. The experiments were carried out in an ammoniacal ammonium chloride system. The influence of composition of electrolytes, pH, stirring rate, current density and temperature, on cathodic current efficiency, specific power consumption and anodic dissolution of Zn were investigated. The results indicate that the cathode current efficiency increases and the hydrogen evolution decreased with increasing the cathode current density. The partial current for electrodeposition of Zn has liner relationship with omega(1/2) (omega: rotation rate). The highest current efficiency for dissolving zinc was obtained when NH(4)Cl concentration was 53.46 g L(-1) and the anodic dissolution of zinc was determined by mass transfer rate at stirring rate 0-300 r min(-1). Increase in temperature benefits to improve CE and dissolution of Zn, and reduce cell voltage. Initial pH of electrolytes plays an important role in the deposition and anodic dissolution of Zn. The results of single factor experiment show that about 50% energy consumption was saved for electrodeposition of Zn in the anion-exchange membrane electrolysis reactor.

  13. Enhanced removal of fluoride by polystyrene anion exchanger supported hydrous zirconium oxide nanoparticles.

    PubMed

    Pan, Bingcai; Xu, Jingsheng; Wu, Bing; Li, Zhigang; Liu, Xitong

    2013-08-20

    Here we fabricated a novel nanocomposite HZO-201, an encapsulated nanosized hydrous zirconium oxide (HZO) within a commercial porous polystyrene anion exchanger D201, for highly efficient defluoridation of water. HZO-201 exhibited much higher preference than activated alumina and D201 toward fluoride removal when competing anions (chloride, sulfate, nitrate, and bicarbonate) coexisted at relatively high levels. Fixed column adsorption indicated that the effective treatable volume of water with HZO-201 was about 7-14 times as much as with D201 irrespective of whether synthetic solution or groundwater was the feeding solution. In addition, HZO-201 could treat >3000 BV of the acidic effluent (around 3.5 mg F(-)/L) per run at pH 3.5, compared to only ∼4 BV with D201. The exhausted HZO-201 could be regenerated by NaOH solution for repeated use without any significant capacity loss. Such attractive performance of HZO-201 resulted from its specific hybrid structure, that is, the host anion exchanger D201 favors the preconcentration of fluoride ions inside the polymer based on the Donnan principle, and the encapsulated nanosized HZO exhibits preferable sequestration of fluoride through specific interaction, as further demonstrated by XPS spectra. The influence of solution pH, competitive anions, and contact time was also examined. The results suggested that HZO-201 has a great potential in efficient defluoridation of groundwater and acidic mine drainage.

  14. Enhanced removal of fluoride by polystyrene anion exchanger supported hydrous zirconium oxide nanoparticles.

    PubMed

    Pan, Bingcai; Xu, Jingsheng; Wu, Bing; Li, Zhigang; Liu, Xitong

    2013-08-20

    Here we fabricated a novel nanocomposite HZO-201, an encapsulated nanosized hydrous zirconium oxide (HZO) within a commercial porous polystyrene anion exchanger D201, for highly efficient defluoridation of water. HZO-201 exhibited much higher preference than activated alumina and D201 toward fluoride removal when competing anions (chloride, sulfate, nitrate, and bicarbonate) coexisted at relatively high levels. Fixed column adsorption indicated that the effective treatable volume of water with HZO-201 was about 7-14 times as much as with D201 irrespective of whether synthetic solution or groundwater was the feeding solution. In addition, HZO-201 could treat >3000 BV of the acidic effluent (around 3.5 mg F(-)/L) per run at pH 3.5, compared to only ∼4 BV with D201. The exhausted HZO-201 could be regenerated by NaOH solution for repeated use without any significant capacity loss. Such attractive performance of HZO-201 resulted from its specific hybrid structure, that is, the host anion exchanger D201 favors the preconcentration of fluoride ions inside the polymer based on the Donnan principle, and the encapsulated nanosized HZO exhibits preferable sequestration of fluoride through specific interaction, as further demonstrated by XPS spectra. The influence of solution pH, competitive anions, and contact time was also examined. The results suggested that HZO-201 has a great potential in efficient defluoridation of groundwater and acidic mine drainage. PMID:23909842

  15. Sorption of uranium(VI) ions from hydrochloric acid and ammonium chloride solutions by anion exchangers

    SciTech Connect

    Pakholkov, V.S.; Denisova, L.A.; Rychkov, V.N.; Kurnosenko, N.A.

    1988-01-01

    The sorption of macroscopic quantities of uranium from solutions of UO/sub 2/Cl/sub 2/ containing HCl and NH/sub 4/Cl in concentrations from 0.0 to 6.0 M by the AV-17 x 8, AV-16G, EDE-10P, AN-31, AN-2F, AN22, and AN-251 anion exchangers has been investigated under static conditions. The sorption isotherms are described by an equation similar to Freundlich's equation: K/sub d/ = K tilde x C/sub eq/sup 1/z/ or log K/sub d/ = log K tilde + 1/z x log C/sub eq/. Equations describing the dependence of the sorbability (or K/sub d/) on the equilibrium concentration of uranium in the solution have been obtained with the aid of the least-squares method. Conclusions regarding the chemistry of the exchange of uranium ions on anion exchangers in chloride solutions have been drawn on the basis of the UV spectra of the original solutions and the IR spectra of the ion exchangers obtained in this work, as well as the established general laws governing sorption.

  16. Phosphorus recovery from microbial biofuel residual using microwave peroxide digestion and anion exchange.

    PubMed

    Gifford, McKay; Liu, Jianyong; Rittmann, Bruce E; Vannela, Raveender; Westerhoff, Paul

    2015-03-01

    Sustainable production of microalgae for biofuel requires efficient phosphorus (P) utilization, which is a limited resource and vital for global food security. This research tracks the fate of P through biofuel production and investigates P recovery from the biomass using the cyanobacterium Synechocystis sp. PCC 6803. Our results show that Synechocystis contained 1.4% P dry weight. After crude lipids were extracted (e.g., for biofuel processing), 92% of the intracellular P remained in the residual biomass, indicating phospholipids comprised only a small percentage of cellular P. We estimate a majority of the P is primarily associated with nucleic acids. Advanced oxidation using hydrogen peroxide and microwave heating released 92% of the cellular P into orthophosphate. We then recovered the orthophosphate from the digestion matrix using two different types of anion exchange resins. One resin impregnated with iron nanoparticles adsorbed 98% of the influent P through 20 bed volumes, but only released 23% during regeneration. A strong-base anion exchange resin adsorbed 87% of the influent P through 20 bed volumes and released 50% of it upon regeneration. This recovered P subsequently supported growth of Synechocystis. This proof-of-concept recovery process reduced P demand of biofuel microalgae by 54%. PMID:25528543

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

    SciTech Connect

    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.

  18. Russian studies of the safety of anion exchange in nitric acid

    SciTech Connect

    Hyder, M.L.; Bartenev, S.A.; Lazarev, L.N.

    1997-07-01

    Synthetic ion exchange resins came into use in the Soviet Union in the 1950`s, and domestic anion exchange resins based on quaternary amine groups have long been used in the Russian nuclear industry. These resins are similar to resins used in the West, and include pyridine-based resins, as well as the more conventional aryl polymers with substituted methyl amines. (Slide 1) The sensitivity of these amines to reaction with nitric acid and other oxidants has been a concern in Russia as in the West, and numerous laboratory studies have been conducted on the reactions involved. Several incidents involving pressure or temperature excursions have provided incentives for such studies. (Slide 2) This report briefly summarizes this work. A report by the Russian authors of this paper providing greater detail is to be issued as a U.S. Dept. of Energy document. Additionally, a second report by these authors, describing new studies on anion exchange resin safety, will also be issued as a DOE report. The separation of plutonium, neptunium, etc. from other materials by ion exchange requires rather strong nitric acid (6-8 M). In some systems, such as the processing of {sup 238}Pu, intense ionizing radiation may also be present during ion exchange separation. As a result, it is necessary to consider not only thermal hydrolysis and oxidation and their effects on the resin, but also radiolysis. All of these were investigated in the Russian studies.

  19. Anion exchange pathways for Cl sup minus transport in rabbit renal microvillus membranes

    SciTech Connect

    Karniski, L.P.; Aronson, P.S. Yale School of Medicine, New Haven, CT )

    1987-09-01

    The authors evaluated the mechanisms of chloride transport in microvillus membrane vesicles isolated from the rabbit renal cortex. The presence of Cl-formate exchange was confirmed. Outward gradients of oxaloacetate, HCO{sub 3}, acetate, lactate, succinate, sulfate, and p-aminohippurate (PAH) stimulated the rate of Cl uptake minimally or not at all. However, an outward gradient of oxalate stimulated Cl uptake by 70%, and an outward Cl gradient induced uphill oxalate uptake, indicting Cl-oxalate exchange. Moreover, an outward formate gradient induced uphill oxalate uptake, indicating formate-oxalate exchange. Studies of inhibitor and substrate specificity indicated the probably operation of at least two separate anion exchangers in mediating Cl transport. The Cl-formate exchanger accepted Cl and formate as substrates, had little or no affinity for oxalate, was sensitive to inhibition by furosemide, and was less sensitive to inhibition by 4,4{prime}-diisothiocyanostilbene-2,2{prime}-disulfonic acid (DIDS). The Cl (formate)-oxalate exchanger also accepted Cl and formate as substrates but had high affinity for oxalate, was highly sensitive to inhibition by DIDS, and was less sensitive to inhibition by furosemide. The Cl-formate exchanger was electroneutral, whereas the Cl (formate)-oxalate exchanger was electrogenic. They conclude that at least separate anion exchangers mediating Cl transport are present on the luminal membrane of the rabbit proximal tubule cell. These exchangers may play important roles in mediating transtubular Cl and oxalate transport in this nephron segment.

  20. Automated sample preparation facilitated by PhyNexus MEA purification system for oligosaccharide mapping of glycoproteins.

    PubMed

    Prater, Bradley D; Anumula, Kalyan R; Hutchins, Jeff T

    2007-10-15

    A reproducible high-throughput sample cleanup method for fluorescent oligosaccharide mapping of glycoproteins is described. Oligosaccharides are released from glycoproteins using PNGase F and labeled with 2-aminobenzoic acid (anthranilic acid, AA). A PhyNexus MEA system was adapted for automated isolation of the fluorescently labeled oligosaccharides from the reaction mixture prior to mapping by HPLC. The oligosaccharide purification uses a normal-phase polyamide resin (DPA-6S) in custom-made pipette tips. The resin volume, wash, and elution steps involved were optimized to obtain high recovery of oligosaccharides with the least amount of contaminating free fluorescent dye in the shortest amount of time. The automated protocol for sample cleanup eliminated all manual manipulations with a recycle time of 23 min. We have reduced the amount of excess AA by 150-fold, allowing quantitative oligosaccharide mapping from as little as 500 ng digested recombinant immunoglobulin G (rIgG). This low sample requirement allows early selection of a cell line with desired characteristics (e.g., oligosaccharide profile and high specific productivity) for the production of glycoprotein drugs. In addition, the use of Tecan or another robotic platform in conjunction with this method should allow the cleanup of 96 samples in 23 min, a significant decrease in the amount of time currently required to process such a large number of samples.

  1. Incorporation of multi-walled carbon nanotubes in microspheres used as anion exchange resin via suspension polymerization

    NASA Astrophysics Data System (ADS)

    Fathy, Mahmoud; Abdel Moghny, Th.; Awadallah, Ahmed E.; El-Bellihi, Abdel-Hameed A.-A.

    2014-06-01

    Amination of vinylbenzyl chloride-divinylbenzene (VBC-DVB) copolymers is an effective method for preparation of anion-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. These resulting anion-exchange polymers were characterized by a variety of techniques such as analytical titrations, 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. Resins containing MWCNTs achieved anion exchange capacity value of 323.6 meq/100 g over than that of copolymer resins and that useful in water desalination or treatment.

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

    PubMed

    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

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

    NASA Astrophysics Data System (ADS)

    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

  4. Equilibrium distribution of SO/sub 2/ between anion-exchange resins and aqueous solutions

    SciTech Connect

    Vulikh, A.I.; Alovyainikov, A.A.

    1983-05-20

    The results are published of a systematic study of SO/sub 2/ adsorption by ion-exchange resins in the presence of moisture. The swelling water in an ion-exchange resin is the medium for transfer of SO/sub 2/ (and of other gases which dissolve in water) from the gas phase to the functional groups of the resin. An external solution of SO/sub 2/ in water is also formed at 100% relative humidity of the gas mixture, and an equilibrium distribution of SO/sub 2/ over the chain of contacting media is established: SO/sub 2/ (gas) ..-->..0 SO/sub 2/ (external solution) ..-->..0 SO/sub 2/ (solution in resin) ..-->..0 SO/sub 2/ (resin runctional groups). If the swollen ion-exchange resin is considered a single phase, then the SO/sub 2/ distribution between it and the water-saturated gas phase may be calculated using data for the individual gas phase-aqueous SO/sub 2/ solution and SO/sub 2/ solution-swollen resin systems. Exhaustive handbook data are available for gas phase-aqueous SO/sub 2/ solution systems. The SO/sub 2/ solution-swollen resin system was studied for a number of resin in the present work. The distribution of SO/sub 2/ between anion-exchange resins in basic forms and aqueous solutons (and the equilibrium gas phase) is described by equations for the neutralization of the resins by sulfurous acid and ion exchange in the system. Anion-exchange resin AV-17 takes up form 1 mole SO/sub 2//g-eq exchange capacity for C/sub SO/sub 2/(g)/ > 1 g/m/sub 3/ to approx.0.5 m/g-eq for C/sub SO/sub 2/(g)/ < 1 mg/m/sup 3/ from the moisture-saturated gas phase. Weekly basic anion-exchange resins (pK/sub B/ > 7) absorb approx.1 mole/g-eq for C/sub SO/sub 2/(g)/ > 50 g/m/sup 3/, but their volume decreases sharply for C/sub SO/sub 2/(g)/ < 10 g/m/sup 3/, and there is virtually no adsorption at C/sub SO/sub 2/(g)/ approx.1 mg/m/sup 3/.

  5. Anion-exchange resin-based desulfurization process. Quarterly technical progress report, Januray 1, 1992--March 31, 1992

    SciTech Connect

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

    1992-07-01

    Under DOE Grant No. FG22-90PC90309, the University of Tennessee Space Institute (UTSI) is contracted to further develop its anion-exchange, resin-based desulfurization concept to desulfurize alkali metal sulfates. From environmental as well as economic viewpoints, it is necessary to remove soluble sulfates from the wastes created by flue gas desulfurization systems. In order to do this economically, a low-cost desulfurization process for spent sorbents is necessary. UTSI`s anion-exchange resin-based desulfurization concept is believed to satisfy these requirements.

  6. Effect of Surface Ion Conductivity of Anion Exchange Membranes on Fuel Cell Performance.

    PubMed

    Hara, Masanori; Kimura, Taro; Nakamura, Takuya; Shimada, Manai; Ono, Hideaki; Shimada, Shigefumi; Miyatake, Kenji; Uchida, Makoto; Inukai, Junji; Watanabe, Masahiro

    2016-09-20

    Anion conductivity at the surfaces of two anion-exchange membranes (AEMs), quaternized ammonium poly(arylene ether) multiblock copolymer (QPE-bl-3) and quaternized ammonium poly(arylene perfluoro-alkylene) copolymer (QPAF-1), synthesized by our group was investigated using current-sensing atomic force microscopy under purified air at various relative humidities. The anion-conducting spots were distributed inhomogeneously on the surface of QPE-bl-3, and the total areas of the anion-conducting spots and the current at each spot increased with humidity. The anion-conductive areas on QPAF-1 were found on the entire surface even at a low humidity. Distribution of the anion-conducting spots on the membrane was found to directly affect the performance of an AEM fuel cell. PMID:27556745

  7. Mesoporous platinum electrodes for amperometric determination of sugars with anion exchange chromatography.

    PubMed

    Han, Jee Hoon; Choi, Han Nim; Park, Sejin; Chung, Taek Dong; Lee, Won-Yong

    2010-01-01

    A simple amperometric detection (AD) method based on mesoporous platinum (Pt) electrodes has been developed for the determination of sugars (glucose, fructose, and sucrose) with high-performance anion-exchange chromatography (HPAEC). The amperometric detection is based on the direct oxidation of sugars on mesoporous Pt films formed on a gold electrode. The mesoporous Pt electrode (roughness factor of 243) sensitively responded to glucose, fructose, and sucrose in 80 mM sodium hydroxide solution as an alkaline mobile-phase for HPAEC. Under the optimum conditions, the limits of detection (S/N = 3) in these sugars were 0.24, 0.29, and 1.8 mM, for glucose, fructose, and sucrose, respectively. The reproducibility (relative standard deviation) of the measurements was less than 3.5%. The present method was applied to the determination of sugars in apple juice. The recoveries for all sugars ranged from 97 to 99%.

  8. Highly Conductive Anion-Exchange Membranes from Microporous Tröger's Base Polymers.

    PubMed

    Yang, Zhengjin; Guo, Rui; Malpass-Evans, Richard; Carta, Mariolino; McKeown, Neil B; Guiver, Michael D; Wu, Liang; Xu, Tongwen

    2016-09-12

    The development of polymeric anion-exchange membranes (AEMs) combining high ion conductivity and long-term stability is a major challenge for materials chemistry. AEMs with regularly distributed fixed cationic groups, based on the formation of microporous polymers containing the V-shape rigid Tröger's base units, are reported for the first time. Despite their simple preparation, which involves only two synthetic steps using commercially available precursors, the polymers provide AEMs with exceptional hydroxide conductivity at relatively low ion-exchange capacity, as well as a high swelling resistance and chemical stability. An unprecedented hydroxide conductivity of 164.4 mS cm(-1) is obtained at a relatively a low ion-exchange capacity of 0.82 mmol g(-1) under optimal operating conditions. The exceptional anion conductivity appears related to the intrinsic microporosity of the charged polymer matrix, which facilitates rapid anion transport. PMID:27505421

  9. NASA Li/CF(x) cell problem analysis: Anion exchange chromatography analysis

    NASA Technical Reports Server (NTRS)

    Bytella, Joseph

    1991-01-01

    An analysis was made of wiper samples used to wipe down lithium/chlorine fluorine battery components and production equipment. These components and equipment were potentially exposed to thionyl chloride vapors. In the presence of moisture, thionyl chloride decomposes to sulfur dioxide and hydrogen chloride. The wiper samples were analyzed for soluble chlorides and fluorides by anion exchange chromatography. During the examination of the test chromatographs, fluoride contamination was discovered in wiper samples from the test equipment. An analytical method to determine fluoride was developed. The first 3 extracts from the potentially exposed and clean wiper samples were tested, and the total fluoride from both groups determined. A comparison of the results from both groups was made to determine the extent of fluoride contamination.

  10. Regeneration of strong-base anion-exchange resins by sequential chemical displacement

    DOEpatents

    Brown, Gilbert M.; Gu, Baohua; Moyer, Bruce A.; Bonnesen, Peter V.

    2002-01-01

    A method for regenerating strong-base anion exchange resins utilizing a sequential chemical displacement technique with new regenerant formulation. The new first regenerant solution is composed of a mixture of ferric chloride, a water-miscible organic solvent, hydrochloric acid, and water in which tetrachloroferrate anion is formed and used to displace the target anions on the resin. The second regenerant is composed of a dilute hydrochloric acid and is used to decompose tetrachloroferrate and elute ferric ions, thereby regenerating the resin. Alternative chemical displacement methods include: (1) displacement of target anions with fluoroborate followed by nitrate or salicylate and (2) displacement of target anions with salicylate followed by dilute hydrochloric acid. The methodology offers an improved regeneration efficiency, recovery, and waste minimization over the conventional displacement technique using sodium chloride (or a brine) or alkali metal hydroxide.

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

    NASA Technical Reports Server (NTRS)

    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.

  12. Thermally Cross-Linked Anion Exchange Membranes from Solvent Processable Isoprene Containing Ionomers

    SciTech Connect

    Tsai, Tsung-Han; Ertem, S. Piril; Maes, Ashley M.; Seifert, Soenke; Herring, Andrew M; Coughlin, E. Bryan

    2015-01-28

    Random copolymers of isoprene and 4-vinylbenzyl chloride (VBCl) with varying compositions were synthesized via nitroxide-mediated polymerization. Subsequent quaternization afforded solvent processable and cross-linkable ionomers with a wide range of ion exchange capacities (IECs). Solution cast membranes were thermally cross-linked to form anion exchange membranes. Cross-linking was achieved by taking advantage of the unsaturations on the polyisoprene backbone, without added cross-linkers. A strong correlation was found between water uptake and ion conductivity of the membranes: conductivities of the membranes with IECs beyond a critical value were found to be constant related to their high water absorption. Environmentally controlled small-angle X-ray scattering experiments revealed a correlation between the average distance between ionic clusters and the ion conductivity, indicating that a well-connected network of ion clusters is necessary for efficient ion conduction and high ion conductivity.

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

    NASA Astrophysics Data System (ADS)

    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.

  14. Anion-exchange separation of Pt and Pd using perchloric and hydrochloric acid solutions

    USGS Publications Warehouse

    Petrie, R.K.; Morgan, J.W.

    1982-01-01

    On Biorad Ag-1X8 anion-exchange resin (200-400 mesh), Pd and Pt may be separated from one another by elution with 0.2M HClO4, and 5M HClO4, respectively. If present, Au may be retained by making the elutriants 0.003M in HCl. Alternatively, reduction by H2SO3 enables elution of Pt2+ with 6M HCl before recovery of Pd2+ with 0.2M HClO4??Ir4+ is reduced to Ir3+ by H2SO3 and may be eluted ahead of Pt2+ by 2M HCl. ?? 1982 Akade??miai Kiado??.

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

    PubMed

    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.

  16. Simultaneous enhancements of conductivity and stability for anion exchange membranes (AEMs) through precise structure design.

    PubMed

    Ran, Jin; Wu, Liang; Wei, Bing; Chen, Yaoyao; Xu, Tongwen

    2014-09-26

    Polymeric materials as anion exchange membranes (AEMs) play an essential role in the field of energy and environment. The achievement of high performance AEMs by the precise manipulation of macromolecular architecture remains a daunting challenge. Herein, we firstly report a novel rod-coil graft copolymer AEM, possessing rigid hydrophobic main chains and soft hydrophilic graft chains. The low graft density, which can alleviate the adverse influences of ionic graft chains on the main chains, was obtained by using the living polymerization technique. Consequently, the grafted ionic groups which result in the degradation of polymer backbone was decreased to a small degree. Moreover, the relatively long graft chains induced the nanophase separation between the hydrophobic polymer chains and hydrophilic graft chains, which creates a convenient pathway for high hydroxide ion mobility. Such an accurate molecular design simultaneously improves the hydroxide ion conductivity and alkaline stability as well as dimensional stability.

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

    PubMed

    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. PMID:26772128

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

    PubMed

    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.

  19. The anion exchanger Ae2 is required for enamel maturation in mouse teeth

    PubMed Central

    Lyaruu, DM; Bronckers, ALJJ; Mulder, L; Mardones, P; Medina, JF; Kellokumpu, S; Elferink, RPJ Oude; Everts, V

    2008-01-01

    One of the mechanisms by which epithelial cells regulate intracellular pH is exchanging bicarbonate for Cl−. We tested the hypothesis that in ameloblasts the anion exchanger-2 (Ae2) is involved in pH regulation during maturation stage amelogenesis. Quantitative X-ray microprobe mineral content analysis, scanning electron microscopy, histology, micro-computed tomography and Ae2 immuno-localisation analyses were applied to Ae2-deficient and wild-type mouse mandibles. Immuno-localisation of Ae2 in wild-type mouse incisors showed a very strong expression of Ae2 in the basolateral membranes of the maturation stage ameloblasts. Strikingly, zones of contiguous ameloblasts were found within the maturation stage in which Ae2 expression was extremely low as opposed to neighbouring cells. Maturation stage ameloblasts of the Ae2a,b−/− mice failed to stain for Ae2 and showed progressive disorganisation as enamel development advanced. Maturation stage enamel of the Ae2a,b−/− mice contained substantially less mineral and more protein than wild-type enamel as determined by quantitative X-ray microanalysis. Incisor enamel was more severely affected than molar enamel. Scanning electron microscopy revealed that the rod-inter-rod structures of the Ae2a,b−/− mice incisor enamel were absent. Mineral content of dentine and bone of Ae2a,b−/− mice was not significantly different from wild-type mice. The enamel from knockout mouse teeth wore down much faster than that from wild-type litter mates. Basolateral bicarbonate secretion via the anionic exchanger Ae2 is essential for mineral growth in the maturation stage enamel. The observed zonal expression of Ae2 in the maturation stage ameloblasts is in line with a model for cyclic proton secretion during maturation stage amelogenesis. PMID:18042363

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

    PubMed

    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

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

    PubMed

    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.

  2. Defluoridation of water via electrically controlled anion exchange by polyaniline modified electrode reactor.

    PubMed

    Cui, Hao; Li, Qin; Qian, Yan; Tang, Rong; An, Hao; Zhai, Jianping

    2011-11-01

    A polyaniline (PANI) modified electrode reactor was designed for fluoride removal from aqueous solutions. The innovative concept behind the reactor design is that the uptake and elute of fluoride could be well controlled by modulating the potential of the PANI film. The maximum fluoride removal capacity of PANI is more than 20 mg/g at a positive voltage based on the electrically controlled anion-exchange mechanism. The results of batch tests showed that terminal potential values had a major impact on fluoride removal by this PANI, with optimal removal occurring at 1.5 V. The fluoride removal capacity (q(e)) increased rapidly within 5 min and reached equilibrium within 10 min, which indicated a rapid removal velocity of fluoride by PANI under this condition. The applicability of defluoridation using the PANI reactor to treat fluoride-contaminated tap water was also tested through flow cell breakthrough studies. At initial fluoride concentrations of 5 mg/L and 10 mg/L, the breakthrough capacities were 20.08 mg/g and 19.24 mg/g, respectively. Moreover, during the first half of the period before the breakthrough point, the fluoride concentration of the treated solution was below the WHO's recommended levels (1.5 mg/L). The results of the five consecutive treatment-regeneration studies also showed that the PANI films could be reused. Taken together, these results implied that the electrically controlled anion exchange by the PANI-modified electrode reactor may be an effective technique for the removal of fluoride from water. PMID:21907382

  3. Evaluating of arsenic(V) removal from water by weak-base anion exchange adsorbents.

    PubMed

    Awual, M Rabiul; Hossain, M Amran; Shenashen, M A; Yaita, Tsuyoshi; Suzuki, Shinichi; Jyo, Akinori

    2013-01-01

    Arsenic contamination of groundwater has been called the largest mass poisoning calamity in human history and creates severe health problems. The effective adsorbents are imperative in response to the widespread removal of toxic arsenic exposure through drinking water. Evaluation of arsenic(V) removal from water by weak-base anion exchange adsorbents was studied in this paper, aiming at the determination of the effects of pH, competing anions, and feed flow rates to improvement on remediation. Two types of weak-base adsorbents were used to evaluate arsenic(V) removal efficiency both in batch and column approaches. Anion selectivity was determined by both adsorbents in batch method as equilibrium As(V) adsorption capacities. Column studies were performed in fixed-bed experiments using both adsorbent packed columns, and kinetic performance was dependent on the feed flow rate and competing anions. The weak-base adsorbents clarified that these are selective to arsenic(V) over competition of chloride, nitrate, and sulfate anions. The solution pH played an important role in arsenic(V) removal, and a higher pH can cause lower adsorption capacities. A low concentration level of arsenic(V) was also removed by these adsorbents even at a high flow rate of 250-350 h(-1). Adsorbed arsenic(V) was quantitatively eluted with 1 M HCl acid and regenerated into hydrochloride form simultaneously for the next adsorption operation after rinsing with water. The weak-base anion exchange adsorbents are to be an effective means to remove arsenic(V) from drinking water. The fast adsorption rate and the excellent adsorption capacity in the neutral pH range will render this removal technique attractive in practical use in chemical industry.

  4. Defluoridation of water via electrically controlled anion exchange by polyaniline modified electrode reactor.

    PubMed

    Cui, Hao; Li, Qin; Qian, Yan; Tang, Rong; An, Hao; Zhai, Jianping

    2011-11-01

    A polyaniline (PANI) modified electrode reactor was designed for fluoride removal from aqueous solutions. The innovative concept behind the reactor design is that the uptake and elute of fluoride could be well controlled by modulating the potential of the PANI film. The maximum fluoride removal capacity of PANI is more than 20 mg/g at a positive voltage based on the electrically controlled anion-exchange mechanism. The results of batch tests showed that terminal potential values had a major impact on fluoride removal by this PANI, with optimal removal occurring at 1.5 V. The fluoride removal capacity (q(e)) increased rapidly within 5 min and reached equilibrium within 10 min, which indicated a rapid removal velocity of fluoride by PANI under this condition. The applicability of defluoridation using the PANI reactor to treat fluoride-contaminated tap water was also tested through flow cell breakthrough studies. At initial fluoride concentrations of 5 mg/L and 10 mg/L, the breakthrough capacities were 20.08 mg/g and 19.24 mg/g, respectively. Moreover, during the first half of the period before the breakthrough point, the fluoride concentration of the treated solution was below the WHO's recommended levels (1.5 mg/L). The results of the five consecutive treatment-regeneration studies also showed that the PANI films could be reused. Taken together, these results implied that the electrically controlled anion exchange by the PANI-modified electrode reactor may be an effective technique for the removal of fluoride from water.

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

    NASA Technical Reports Server (NTRS)

    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.

  6. Mechanism of sorption sulpho-derivative organic chelating agents on strong base anion exchanger Amberlite IRA-402 by FT-IR/PAS and DRS methods

    NASA Astrophysics Data System (ADS)

    Wronski, G.; Pasieczna-Patkowska, S.; Hubicki, Z.

    2008-02-01

    In the paper, strong base anion exchanger Amberlite IRA-402 was modified by using sulpho-derivative organic chelating agents as: Brilliant Yellow, Xylenol Orange, Bromophenyl Blue. The investigations exhibited, that anion exchanger Amberlite IRA-402 is modified very simply by organic chelating agents (working capacity 0.25 0.5 g/cm3).

  7. ANIONIC EXCHANGE PROCESS FOR THE RECOVERY OF URANIUM AND VANADIUM FROM CARBONATE SOLUTIONS

    DOEpatents

    Bailes, R.H.; Ellis, D.A.; Long, R.S.

    1958-12-16

    Uranium and vanadium can be economically purified and recovered from non- salt roast carbonate leach liquors by adsorption on a strongly basic anionic exchange resin and subsequent selective elution by one of three alternative methods. Method 1 comprises selectively eluting uranium from the resin with an ammonium sulfate solution followed by eluting vanadium from the resin with either 5 M NaCl, saturated (NH/sub 4/)/sub 2/CO/sub 3/, saturated NaHCO/sub 3/, 1 M NaOH, or saturated S0/sub 2/ solutions. Method II comprises selectively eluting vanadium from the resin with either concentrated NaCl or S0/sub 2/ solutions subsequent to pretreatment of the column with either S0/sub 2/ gas, 1 N HCl, or 0.1 N H/sub 2/8O/sub 4/ followed by eluting uranium from the resin with solutions containing 0.9 M NH/sub 4/Cl or NaCl and 0.1 Cl. Method III comprises flowing the carbonate leac solutlon through a first column of a strongly basic anlonlc exchange resin untll vanadium breakthrough occurs, so that the effluent solution is enriched ln uranium content and the vanadium is chiefly retalned by the resln, absorbing the uranlum from the enriched effluent solution on a second column of a strongly basic anionic exchange resin, pretreating the first column with either 0.1 N HCl, 0.1 H/sub 2/SO/sub 4/, C0/sub 2/ gas, or ammonium sulfate, selectively eluting the vanadlum from the column with saturated S0/sub 2/ solution, pretreatlng the second column with either 0.1 N HCl or S0/sub 2/ gas, selectively eluting residual vanadium from the column with saturated S0/sub 2/ solution, and then eluting the uranium from the column with either 0.1 N HCl and 1 N NaCl orO.l N HCl and 1 N NH/sub 4/Cl.

  8. Effect of Oxalate on the Recycle of Neptunium Filtrate Solution by Anion Exchange

    SciTech Connect

    Kyser, E

    2004-11-18

    A series of laboratory column runs has been performed that demonstrates the recovery of neptunium (Np) containing up to 0.05 M oxalate. Np losses were generally less than one percent to the raffinate for feed solutions that contained 2 to 10 g Np/L. Up to 16 percent Np losses were observed with lower Np feed concentrations, but those losses were attributed to the shortened residence times rather than the higher oxalate to Np ratios. Losses in the plant are expected to be significantly less due to the lower cross-section flowrate possible with existing plant pumps. Elimination of the permanganate treatment of filtrates appears to be reasonable since the amount of Np in those filtrates does not appear to be practical to recover. Combination of untreated filtrates with other actinide rich solutions is not advisable as precipitation problems are likely. If untreated filtrates are kept segregated from other actinide rich streams, the recovery of the remaining Np is probably still possible, but could be limited due to the excessively high oxalate to Np ratio. The persistence of hydrazine/hydrazoic acid in filtrate solutions dictates that the nitrite treatment be retained to eliminate those species from the filtrates prior to transfer to the canyon. Elimination of the permanganate treatment of precipitator flushes and recovery by anion exchange does not appear to be limited by the oxalate effect on anion exchange. Np from solutions with higher oxalate to Np molar ratios than expected in precipitator flushes was recovered with low to modest losses. Solubility problems appear to be unlikely when the moles of oxalate involved are less than the total number of moles of Np due to complexation effects. The presence of significant concentrations of iron (Fe) in the solutions will further decrease the probability of Np oxalate precipitation due the formation of Fe oxalate complexes. Np oxalate solubility data in 8 M HNO{sub 3} with from one to six times as much oxalate as Np have

  9. Large Scale Solid Phase Synthesis of Peptide Drugs: Use of Commercial Anion Exchange Resin as Quenching Agent for Removal of Iodine during Disulphide Bond Formation

    PubMed Central

    Reddy, K. M. Bhaskara; Kumari, Y. Bharathi; Mallikharjunasarma, Dokka; Bulliraju, Kamana; Sreelatha, Vanjivaka; Ananda, Kuppanna

    2012-01-01

    The S-acetamidomethyl (Acm) or trityl (Trt) protecting groups are widely used in the chemical synthesis of peptides that contain one or more disulfide bonds. Treatment of peptides containing S-Acm protecting group with iodine results in simultaneous removal of the sulfhydryl protecting group and disulfide formation. However, the excess iodine needs to be quenched or adsorbed as quickly as possible after completion of the disulfide bond formation in order to minimize side reactions that are often associated with the iodination step. We report here a simple method for simultaneous quenching and removal of iodine and isolation of disulphide bridge peptides. The use of excess inexpensive anion exchange resin to the oxidized peptide from the aqueous acetic acid/methanol solution affords quantitative removal of iodine and other color impurities. This improves the resin life time of expensive chromatography media that is used in preparative HPLC column during the purification of peptide using preparative HPLC. Further, it is very useful for the conversion of TFA salt to acetate in situ. It was successfully applied commercially, to the large scale synthesis of various peptides including Desmopressin, Oxytocin, and Octreotide. This new approach offers significant advantages such as more simple utility, minimal side reactions, large scale synthesis of peptide drugs, and greater cost effectiveness. PMID:23118772

  10. Carminic acid modified anion exchanger for the removal and preconcentration of Mo(VI) from wastewater.

    PubMed

    El-Moselhy, Medhat Mohamed; Sengupta, Arup K; Smith, Ryan

    2011-01-15

    Removal and preconcentration of Mo(VI) from water and wastewater solutions was investigated using carminic acid modified anion exchanger (IRA743). Various factors influencing the adsorption of Mo(VI), e.g. pH, initial concentration, and coexisting oxyanions were studied. Adsorption reached equilibrium within <10 min and was independent of initial concentration of Mo(VI). Studies were performed at different pH values to find the pH at which maximum adsorption occurred and was determined to be at a pH between 4.0 and 6.0. The Langmuir adsorption capacity (q(max)) was found to be 13.5mg Mo(VI)/g of the adsorbent. The results showed that modification of IRA743 with carminic acid is suitable for the removal of Mo(VI), as molybdate, from water and wastewater samples. The concentration of Mo(VI) was determined spectrophotometrically using bromopyrogallol red as a complexation reagent. This allows the determination of Mo(VI) in the range 1.0-100.0 μg/mL. The obtained material was subjected to efficient regeneration. PMID:20943315

  11. Diels Alder polyphenylene anion exchange membrane for nonaqueous redox flow batteries

    DOE PAGES

    Small, Leo J.; Pratt, III, Harry D.; Fujimoto, Cy H.; Anderson, Travis M.

    2015-10-23

    Here highly conductive, solvent-resistant anionic Diels Alder polyphenylene (DAPP) membranes were synthesized with three different ionic contents and tested in an ionic liquid-based nonaqueous redox flow battery (RFB). These membranes display 3–10× increase in conductivity in propylene carbonate compared to some commercially available (aqueous) anion exchange membranes. The membrane with an ion content of 1.5 meq/g (DAPP1.5) proved too brittle for operation in a RFB, while the membrane with an ion content of 2.5 meq/g (DAPP2.5) allowed excessive movement of solvent and poor electrochemical yields (capacity fade). Despite having lower voltage efficiencies compared to DAPP2.5, the membrane with an intermediatemore » ion content of 2.0 meq/g (DAPP2.0) exhibited higher coulombic efficiencies (96.4% vs. 89.1%) and electrochemical yields (21.6% vs. 10.9%) after 50 cycles. Crossover of the electroactive species was the primary reason for decreased electrochemical yields. Analysis of the anolyte and catholyte revealed degradation of the electroactive species and formation of a film at the membrane-solution interface. Increases in membrane resistance were attributed to mechanical and thermal aging of the membrane; no chemical change was observed. As a result, improvements in the ionic selectivity and ionic conductivity of the membrane will increase the electrochemical yield and voltage efficiency of future nonaqueous redox flow batteries.« less

  12. Diels Alder polyphenylene anion exchange membrane for nonaqueous redox flow batteries

    SciTech Connect

    Small, Leo J.; Pratt, III, Harry D.; Fujimoto, Cy H.; Anderson, Travis M.

    2015-10-23

    Here highly conductive, solvent-resistant anionic Diels Alder polyphenylene (DAPP) membranes were synthesized with three different ionic contents and tested in an ionic liquid-based nonaqueous redox flow battery (RFB). These membranes display 3–10× increase in conductivity in propylene carbonate compared to some commercially available (aqueous) anion exchange membranes. The membrane with an ion content of 1.5 meq/g (DAPP1.5) proved too brittle for operation in a RFB, while the membrane with an ion content of 2.5 meq/g (DAPP2.5) allowed excessive movement of solvent and poor electrochemical yields (capacity fade). Despite having lower voltage efficiencies compared to DAPP2.5, the membrane with an intermediate ion content of 2.0 meq/g (DAPP2.0) exhibited higher coulombic efficiencies (96.4% vs. 89.1%) and electrochemical yields (21.6% vs. 10.9%) after 50 cycles. Crossover of the electroactive species was the primary reason for decreased electrochemical yields. Analysis of the anolyte and catholyte revealed degradation of the electroactive species and formation of a film at the membrane-solution interface. Increases in membrane resistance were attributed to mechanical and thermal aging of the membrane; no chemical change was observed. As a result, improvements in the ionic selectivity and ionic conductivity of the membrane will increase the electrochemical yield and voltage efficiency of future nonaqueous redox flow batteries.

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

    PubMed

    Wang, Qiongjie; Li, Aimin; Wang, Jinnan; Shuang, Chengdong

    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 degrees C, while a relatively strong one at 36 degrees C. 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.

  14. Tunable high performance cross-linked alkaline anion exchange membranes for fuel cell applications.

    PubMed

    Robertson, Nicholas J; Kostalik, Henry A; Clark, Timothy J; Mutolo, Paul F; Abruña, Héctor D; Coates, Geoffrey W

    2010-03-17

    Fuel cells are energy conversion devices that show great potential in numerous applications ranging from automobiles to portable electronics. However, further development of fuel cell components is necessary for them to become commercially viable. One component critical to their performance is the polymer electrolyte membrane, which is an ion conductive medium separating the two electrodes. While proton conducting membranes are well established (e.g., Nafion), hydroxide conducting membranes (alkaline anion exchange membranes, AAEMs) have been relatively unexplored by comparison. Operating under alkaline conditions offers significant efficiency benefits, especially for the oxygen reduction reaction; therefore, effective AAEMs could significantly advance fuel cell technologies. Here we demonstrate the use of ring-opening metathesis polymerization to generate new cross-linked membrane materials exhibiting high hydroxide ion conductivity and good mechanical properties. Cross-linking allows for increased ion incorporation, which, in turn supports high conductivities. This facile synthetic approach enables the preparation of cross-linked materials with the potential to meet the demands of hydrogen-powered fuel cells as well as direct methanol fuel cells. PMID:20178312

  15. Functional rescue of a kidney anion exchanger 1 trafficking mutant in renal epithelial cells.

    PubMed

    Chu, Carmen Y S; King, Jennifer C; Berrini, Mattia; Alexander, R Todd; Cordat, Emmanuelle

    2013-01-01

    Mutations in the SLC4A1 gene encoding the anion exchanger 1 (AE1) can cause distal renal tubular acidosis (dRTA), a disease often due to mis-trafficking of the mutant protein. In this study, we investigated whether trafficking of a Golgi-retained dRTA mutant, G701D kAE1, or two dRTA mutants retained in the endoplasmic reticulum, C479W and R589H kAE1, could be functionally rescued to the plasma membrane of Madin-Darby Canine Kidney (MDCK) cells. Treatments with DMSO, glycerol, the corrector VX-809, or low temperature incubations restored the basolateral trafficking of G701D kAE1 mutant. These treatments had no significant rescuing effect on trafficking of the mis-folded C479W or R589H kAE1 mutants. DMSO was the only treatment that partially restored G701D kAE1 function in the plasma membrane of MDCK cells. Our experiments show that trafficking of intracellularly retained dRTA kAE1 mutants can be partially restored, and that one chemical treatment rescued both trafficking and function of a dRTA mutant. These studies provide an opportunity to develop alternative therapeutic solutions for dRTA patients. PMID:23460825

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

    PubMed

    Duangtum, Natapol; Junking, Mutita; Sawasdee, Nunghathai; Cheunsuchon, Boonyarit; Limjindaporn, Thawornchai; Yenchitsomanus, Pa-thai

    2011-09-16

    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(-)/HCO(3)(-) 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. PMID:21871436

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

    PubMed

    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.

  18. Phosphate removal from wastewaters using a weak anion exchanger prepared from a lignocellulosic residue.

    PubMed

    Anirudhan, T S; Noeline, B F; Manohar, D M

    2006-04-15

    Surface modifications of lignocellulosic residues has become increasingly important for improving their applications as adsorbents. In this study a new adsorbent system (BS-DMAHP) containing dimethylaminohydroxypropyl (DMAHP) weak base groups was prepared by the reaction of banana stem (BS), a lignocellulosic residue with epichlorohydrin and dimethylamine followed by treatment of hydrochloric acid. The original BS and BS-DMAHP were characterized with the help of surface area analyzer, infrared spectroscopy (IR) and scanning electron microscopy (SEM). Surface charge density of the samples as a function of pH was investigated using potentiometric titrations. Adsorbent exhibits very high adsorption potential for phosphate and more than 99.0% removal was achieved in the pH range of 5.0-7.0. Adsorption has been found to be concentration dependent and endothermic and follows a reversible second-order kinetics. The Langmuir and Freundlich isotherm models were applied to describe the equilibrium data. Equilibrium data agreed very well with the Langmuir model. Adsorption experiments were conducted using a commercial chloride form Duolite A-7, a weak base anion exchanger. The removal efficiency was tested using fertilizer industry wastewater. Adsorbed phosphate on BS-DMAHP can be recovered by treating with 0.1 M NaOH solution. A stability test operated for four cycles indicate a capacity loss of < 12.0%.

  19. Synthesis and Structure-Property Relationships of Poly(sulfone)s for Anion Exchange Membranes

    SciTech Connect

    Yan, JL; Moore, HD; Hibbs, MR; Hickner, MA

    2013-10-05

    Membranes based on cationic polymers that conduct anions are important for enabling alkaline membrane fuel cells and other solid-state electrochemical devices that operate at high pH. Anion exchange membranes with poly(arylene ether sulfone) backbones are demonstrated by two routes: chloromethylation of commercially available poly(sulfone)s or radical bromination of benzylmethyl moieties in poly(sulfone)s containing tetramethylbisphenol A monomer residues. Polymers with tethered trimethylbenzyl ammonium moieties resulted from conversion of the halomethyl groups by quaternization with trimethyl amine. The water uptake of the chloromethylated polymers was dependent on the type of poly(sulfone) backbone for a given IEC. Bisphenol A-based Udel (R) poly(sulfone) membranes swelled in water to a large extent while membranes from biphenol-based Radel (R) poly(sulfone), a stiffer backbone than Udel, only showed moderate water uptake. The water uptake of cationic poly(sulfone)s was further reduced by synthesizing tetramethylbisphenol A and 4,4-biphenol-containing poly(sulfone) copolymers where the ionic groups were clustered on the tetramethylbisphenol A residues. The conductivity of all samples scaled with the bulk water uptake. The hydration number of the membranes could be increased by casting membranes from the ionic form polymers versus converting the halomethyl form cast polymers to ionic form in the solid state. (c) 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2013, 51, 1790-1798, 2013

  20. Kinetics of adsorption of sulphonated azo dyes on strong basic anion exchangers.

    PubMed

    Wawrzkiewicz, Monika; Hubicki, Zbigniew

    2009-09-01

    The macroporous polystyrene anion exchangers Amberlite IRA-900 and Amberlite IRA-910 were used in order to remove sulphonated azo dyes (Allura Red and Sunset Yellow) from aqueous solutions of 100-500 mg/L concentrations. The experimental data obtained at 100, 200, 300 and 500 mg/L initial concentrations at 20 degrees C were applied to the pseudo-first-order, pseudo-second-order and Weber-Morris kinetic models. The calculated sorption capacities (qe,cal) and the rate constant of the first-order adsorption (k1) were determined. The pseudo-second-order kinetic constants (k2) and capacities were calculated from the plots of t/qt vs t, 1/qt vs 1/t, 1/t vs 1/qt, qt/t vs qt and 1/qe-qt vs t for type 1, type 2, type 3, type 4 and type 5 of the pseudo-second-order expression, respectively. The influence of phase contact time, initial dye concentration, solution pH and temperature on Allura Red and Sunset Yellow removal was also discussed.

  1. Influence of Hydration Level on Polymer and Water Dynamics in Alkaline Anion Exchange Fuel Cell Membranes

    NASA Astrophysics Data System (ADS)

    Tarver, Jacob; Kim, Jenny; Tyagi, Madhu; Soles, Christopher; Tsai, Tsung-Han; Coughlin, Bryan

    2015-03-01

    Triblock copolymers based on poly(chloromethylstyrene)-b-poly(ethylene)-b-poly(chloromethylstyrene) can be quaternized to different extents to yield anion exchange membranes for alkaline fuel cells. In the absence of moisture, these membranes demonstrate bilayer lamellar morphology. Upon high levels of hydration, however, in-situ small angle neutron scattering reveals the emergence of higher-order diffraction peaks. This phenomena has previously been observed in analogous diblock copolymer-based membranes and has been attributed to the induction of a multilayer lamellar morphology in which selective striping of water occurs in the center of the ion-rich domain. By conducting humidity-resolved quasielastic neutron scattering (QENS) measurements using deuterated water, we are able to isolate differences in the pico- to nanosecond timescale dynamics of the hydrogenated membrane upon hydration. QENS measurements in the presence of a hydrogenated water source subsequently permit deconvolution and isolation of the translational and rotational dynamics of water as a function of relative humidity, revealing spatial and temporal changes in polymer and water motion at high levels of hydration.

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

    SciTech Connect

    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.

  3. Weak anion exchange chromatographic profiling of glycoprotein isoforms on a polymer monolithic capillary.

    PubMed

    Liu, Jing; Ren, Lianbing; Liu, Yunchun; Li, Hengye; Liu, Zhen

    2012-03-01

    High resolution separation of intact glycoproteins, which is essential for many aspects such as finger-print profiling, represents a great challenge because one glycoprotein can exhibit many isoforms with close physicochemical properties. Monolithic columns are important separation media for the separation of intact proteins due to its significant advantages such as easy preparation, high column efficiency and high permeability. However, there are few reports on high resolution profiling of intact glycoproteins. Herein, we presented a polymeric weak anion exchange (WAX) monolithic capillary for high resolution separation of glycoprotein isoforms. A base monolith was first prepared through ring-opening polymerization between tris(2,3-epoxypropyl)isocyanurate and tri(2-aminoethyl), and then modified through reacting with ammonia aqueous solution to convert the unreacted epoxide moieties into primary amino groups. The prepared monolithic capillary was characterized in terms of morphology, pore size, hydrophilicity and reproducibility. The obtained WAX monolithic capillary exhibited desired through-pores and mesopore size, stable skeleton and hydrophilic nature. The performance of the capillary was evaluated using several typical glycoproteins such as α(1)-acid glycoprotein (AGP) as mode analytes. Effects of the experimental parameters on the glycoform resolution were investigated. Under the optimized separation conditions, the tested glycoproteins were all resolved into distinct glycoforms. A comparative investigation with capillary zone electrophoresis (CZE) revealed that this WAX column provided better selectivity as more isoforms were observed, although the resolution of some glycoprotein isoforms decreased.

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

    PubMed

    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. PMID:26452943

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

    PubMed

    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

  6. Quaternized dimethylaminoethyl methacrylate strong base anion exchange fibers for As(V) adsorption

    NASA Astrophysics Data System (ADS)

    Kavaklı, Cengiz; Akkaş Kavaklı, Pınar; Turan, Burcu Dila; Hamurcu, Aslı; Güven, Olgun

    2014-09-01

    N,N-Dimethylaminoethyl methacrylate (DMAEMA) grafted polyethylene/polypropylene (PE/PP) nonwoven fibers (DMAEMA-g-PE/PP) was prepared by radiation-induced graft polymerization. DMAEMA graft chains on nonwoven fibers were quaternized with dimethyl sulfate solution for the preparation of strong base anion exchange fibers (QDMAEMA-g-PE/PP). Fiber structures were characterized by FTIR, XPS and SEM techniques. The effect of solution pH, contact time, initial As(V) ion concentration and coexisting ions on the As(V) adsorption capacity of the QDMAEMA-g-PE/PP fibers were investigated by performing batch adsorption experiments. The adsorption of As(V) by QDMAEMA-g-PE/PP fibers was found to be independent on solution pH in the range 4.00-10.00. Kinetic experiments show that the As(V) adsorption rate was rapid and As(V) adsorption follows pseudo second-order kinetic model. As(V) adsorption equilibrium data were analyzed using Langmuir and Freundlich adsorption isotherm model equations. Langmuir and Freundlich adsorption isotherm models fitted the experimental data well. The maximum adsorption capacity (qmax) calculated from Langmuir isotherm was found to be 83.33 mg As(V)/g polymer at pH 7.00. The adsorbent was used for three cycles without significant loss of adsorption capacity. The adsorbed As(V) ions were desorbed effectively by a 0.1 M NaOH solution.

  7. Performance testing of grout-based waste forms for the solidification of anion exchange resins

    SciTech Connect

    Morgan, I.L.; Bostick, W.D.

    1990-10-01

    The solidification of spent ion exchanges resins in a grout matrix as a means of disposing of spent organic resins produced in the nuclear fuel cycle has many advantages in terms of process simplicity and economy, but associated with the process is the potential for water/cement/resins to interact and degrade the integrity of the waste form solidified. Described in this paper is one possible solution to preserving the integrity of these solidified waste forms: the encapsulation of beaded anion exchange resins in grout formulations containing ground granulated blast furnace slag, Type I-II (mixed) portland cement, and additives (clays, amorphous silica, silica fume, and fly ash). The results of the study reported herein show the cured waste form tested has a low leach rate for nitrate ion from the resin (and a low leach rate is inferred for Tc-99) and acceptable durability as assessed by the water immersion and freezing/thawing test protocols. The results also suggest a tested surrogate waste form prepared in vinyl ester styrene binder performs satisfactorily against the wetting/drying criterion, and it should offer additional insight into future work on the solidification of spent organic resins. 26 refs., 4 figs., 5 tabs.

  8. [Determination of sulfide in gourmet powder by anion exchange chromatography with pulsed amperometric detection].

    PubMed

    Li, Renyong; Liang, Lina; Li, Jing

    2010-12-01

    A chromatographic method was developed for the determination of sulfide in gourmet powder. The samples were dissolved in 2 g/L sodium hydroxide solution directly, and filtrated with a 0.22 microm nylon membrane. The sulfide and other anions such as high concentration of glutamate were separated well in 6 min by an IonPac AS7 Anion Exchange column (250 mm x4 mm). A mixed solution of 100 mmol/L sodium hydroxide, 500 mmol/L sodium acetate and 0.5% ethylenediamine was used isocratically as the mobile phase. The detection limit of the sulfide was 0.3 microg/L at 25 microL injection (S/N = 3). Moreover, the method had a wide linear range (0.001-1 mg/L) and satisfactory recovery (94.2%-99.0%). The method was applied in the determinations of the sulfide in 99% monosodium glutamate, special delicious monosodium glutamate and salted monosodium glutamate samples. The method is simple, fast and good in separation performance, and has high selectivity and sensitivity.

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

    PubMed

    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. Tunable High Performance Cross-Linked Alkaline Anion Exchange Membranes for Fuel Cell Applications

    SciTech Connect

    Robertson, Nicholas J.; Kostalik, IV, Henry A.; Clark, Timothy J.; Mutolo, Paul F.; Abruña, Héctor D.; Coates, Geoffrey W.

    2010-02-23

    Fuel cells are energy conversion devices that show great potential in numerous applications ranging from automobiles to portable electronics. However, further development of fuel cell components is necessary for them to become commercially viable. One component critical to their performance is the polymer electrolyte membrane, which is an ion conductive medium separating the two electrodes. While proton conducting membranes are well established (e.g., Nafion), hydroxide conducting membranes (alkaline anion exchange membranes, AAEMs) have been relatively unexplored by comparison. Operating under alkaline conditions offers significant efficiency benefits, especially for the oxygen reduction reaction; therefore, effective AAEMs could significantly advance fuel cell technologies. Here we demonstrate the use of ring-opening metathesis polymerization to generate new cross-linked membrane materials exhibiting high hydroxide ion conductivity and good mechanical properties. Cross-linking allows for increased ion incorporation, which, in turn supports high conductivities. This facile synthetic approach enables the preparation of cross-linked materials with the potential to meet the demands of hydrogen-powered fuel cells as well as direct methanol fuel cells.

  11. Adsorption of uranium (VI) from mixed chloride-fluoride solutions by anion-exchange resins

    SciTech Connect

    Pakholkov, V.S.; Denisova, L.A.; Rychkov, V.N.; Kurnosenko, N.A.

    1988-03-01

    Experimental data are reported and discussed concerning the adsorption of uranium from 0.025 M solutions of UO/sub 2/Cl/sub 2/, containing HCl, HF, and NH/sub 4/Cl over a wide concentration range, using anion-exchange resins of varying basicities. UV and IR spectroscopic studies were conducted in order to clarify the chemical mechanism of uranium adsorption. Adsorption isotherms for all of the ion-exchange resins studied are convex in shape and can be described by the following equations: log K/sub d/ = a + b (-log C/sub e/), and log A = a + (b + 1) log C/sub e/, where A is the adsorptivity in mmole U/g; K/sub d/ is the distribution coefficient in mg/liter; and C/sub e/ is the equilibrium concentration of U in mmole/ml. General mathematical models have been obtained to describe the adsorption process; these consist of a system of regression equations derived from the results of a complete 2/sup 3/ factorial study.

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

    PubMed

    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.

  13. Synthesis of Composition Tunable and Highly Luminescent Cesium Lead Halide Nanowires through Anion-Exchange Reactions.

    PubMed

    Zhang, Dandan; Yang, Yiming; Bekenstein, Yehonadav; Yu, Yi; Gibson, Natalie A; Wong, Andrew B; Eaton, Samuel W; Kornienko, Nikolay; Kong, Qiao; Lai, Minliang; Alivisatos, A Paul; Leone, Stephen R; Yang, Peidong

    2016-06-15

    Here, we demonstrate the successful synthesis of brightly emitting colloidal cesium lead halide (CsPbX3, X = Cl, Br, I) nanowires (NWs) with uniform diameters and tunable compositions. By using highly monodisperse CsPbBr3 NWs as templates, the NW composition can be independently controlled through anion-exchange reactions. CsPbX3 alloy NWs with a wide range of alloy compositions can be achieved with well-preserved morphology and crystal structure. The NWs are highly luminescent with photoluminescence quantum yields (PLQY) ranging from 20% to 80%. The bright photoluminescence can be tuned over nearly the entire visible spectrum. The high PLQYs together with charge transport measurements exemplify the efficient alloying of the anionic sublattice in a one-dimensional CsPbX3 system. The wires increased functionality in the form of fast photoresponse rates and the low defect density suggest CsPbX3 NWs as prospective materials for optoelectronic applications. PMID:27213511

  14. Experimental study on the adsorption of excess heparin with anion exchange resin fiber.

    PubMed

    Matsuda, K; Oka, T; Tani, T; Hanasawa, K; Yoshioka, T; Aoki, H; Endo, Y; Ishii, Y; Numa, K; Kodama, M

    1989-12-01

    Anion exchange resin fiber (Ionex) was used as a heparin adsorbent. Ionex has the adsorption capacity of 70 mg/g (weight by desiccation) for heparin, and was used in an attempt to remove the heparin from blood-perfused artificial organs, before the blood was transfused back into the patients. In the ex vivo study, the 5 systemically heparinized dogs (500 U/kg) were treated with a 35-40 g column of Ionex, by direct hemoperfusion (DHP). The concentration of heparin was significantly reduced, within 15 to 60 minutes, using the Ionex. This suggested the possibility of removing excess heparin from the living body. In in vitro, the relationship between the amount of heparin by Ionex and the blood-flow volume were evaluated. Whole blood taken from dogs was added to 5 U/ml of heparin. This was then introduced into a small column containing 0.9 g Ionex, at blood-flow rates of 0.8, 1.6, and 3.2 ml/min. A good adsorption capacity was shown at the blood-flow rate of 0.8 ml/min. One possible explanation for this is that the heparin dispersed in the blood cells gradually was passed on into the plasma and, so, did not have time to be adsorbed at the faster flow rates. PMID:2604592

  15. Removal of chromium (VI) from electroplating wastewater using an anion exchanger derived from rice straw.

    PubMed

    Cao, Wei; Dang, Zhi; Yia, Xiao-Yun; Yang, Chen; Lu, Gui-Ning; Liu, Yun-Feng; Huang, Se-Yan; Zheng, Liu-Chun

    2013-01-01

    An anion exchanger from rice straw was used to remove Cr (VI) from synthetic wastewater and electroplating effluent. The exchanger was characterized using Fourier transform infrared (FTIR) spectrum and scanning electron microscopy (SEM), and it was found that the quaternary amino group and hydroxyl group are the main functional groups on the fibrous surface of the exchanger. The effect of contact time, initial concentration and pH on the removal of Cr (VI), and adsorption isotherms at different temperature, was investigated. The results showed that the removal of Cr (VI) was very rapid and was significantly affected by the initial pH of the solution. Although acidic conditions (pH = 2-6) facilitated Cr (VI) adsorption, the exchanger was effective in neutral solution and even under weak base conditions. The equilibrium data fitted well with Langmuir adsorption model, and the maximum Cr (VI) adsorption capacities at pH 6.4 were 0.35, 0.36 and 0.38 mmol/g for 15, 25 and 35 degrees C, respectively. The exchanger was finally tested with real electroplating wastewater, and at sorbent dosage of 10 g/L, the removal efficiencies for Cr (VI) and total Cr were 99.4% and 97.8%, respectively. In addition, the positive relationship between adsorbed Cr (VI) and desorbed Cl- suggested that Cr (VI) was mainly removed by ion exchange with chlorine. PMID:23530310

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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).

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

    NASA Astrophysics Data System (ADS)

    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.

  19. Phosphate recovery using hybrid anion exchange: applications to source-separated urine and combined wastewater streams.

    PubMed

    O'Neal, Jeremy A; Boyer, Treavor H

    2013-09-15

    There is increasing interest in recovering phosphorus (P) from various wastewater streams for beneficial use as fertilizer and to minimize environmental impacts of excess P on receiving waters. One such example is P recovery from human urine, which has a high concentration of phosphate (200-800 mg P/L) and accounts for a small volume (≈ 1%) of total wastewater flow. Accordingly, the goal of this study was to evaluate the potential to recover P from source-separated and combined wastewater streams that included undiluted human urine, urine diluted with tap water, greywater, mixture of urine and greywater, anaerobic digester supernatant, and secondary wastewater effluent. A hybrid anion exchange (HAIX) resin containing hydrous ferric oxide was used to recover P because of its selectivity for phosphate and the option to precipitate P minerals in the waste regeneration solution. The P recovery potential was fresh urine > hydrolyzed urine > greywater > biological wastewater effluent > anaerobic digester supernatant. The maximum loading of P on HAIX resin was fresh urine > hydrolyzed urine > anaerobic digester supernatant ≈ greywater > biological wastewater effluent. Results indicated that the sorption capacity of HAIX resin for phosphate and the total P recovery potential were greater for source-separated urine than the combined wastewater streams of secondary wastewater effluent and anaerobic digester supernatant. Dilution of urine with tap water decreased the phosphate loading on HAIX resin. The results of this work advance the current understanding of nutrient recovery from complex wastewater streams by sorption processes.

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

    SciTech Connect

    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.

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

    PubMed

    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.

  2. Onboard determination of submicromolar nitrate in seawater by anion-exchange chromatography with lithium chloride eluent.

    PubMed

    Maruo, Masahiro; Doi, Takashi; Obata, Hajime

    2006-09-01

    Ion-exchange chromatography using a high-capacity anion exchanger with UV detection was applied to the determination of nitrate in seawater. Major ions in seawater samples did not affect the peak shape and the retention time of the nitrate when an alkaline metal cation-chloride solution was used as an eluent at high concentrations (0.5-2 mol/l). At a wavelength of 220 nm, the peak of bromide was very small because of low absorption, while its separation from the nitrate peak was good at high concentrations. Among the eluents tested, lithium chloride gave the best separation of nitrate from bromide. It was estimated that the lithium ion had the least potential for ion-pair formation with nitrate, and its retention time was prolonged compared with the retention times when using other cations; with bromide and nitrite, such an effect was not observed. The results of shipboard seawater nitrate determination by our method in the South Pacific Ocean and Antarctic Sea showed good agreement with those by the conventional photometric method using continuous flow.

  3. Enhanced sensitivity of an antibody competitive blocking enzyme-linked immunosorbent assay using Equine arteritis virus purified by anion-exchange membrane chromatography.

    PubMed

    Chung, Chungwon J; Grimm, Amanda L; Wilson, Carey L; Balasuriya, Udeni B R; Chung, Grace; Timoney, Peter J; Bandaranayaka-Mudiyanselage, Chandima-Bandara; Lee, Stephen S; McGuire, Travis C

    2015-11-01

    In an effort to improve a competitive blocking enzyme-linked immunosorbent assay (cELISA) for antibody detection to Equine arteritis virus (EAV), antigen purified by anion-exchange membrane chromatography capsule (AEC) was evaluated. Virus purification by the AEC method was rapid and easily scalable. A comparison was made between virus purified by the AEC method with that obtained by differential centrifugation based on the following: 1) the relative purity and quality of EAV glycoprotein 5 (GP5) containing the epitope defined by monoclonal antibody 17B7, and 2) the relative sensitivity of a commercial antibody cELISA with the only change being the 2 purified antigens. On evaluation by Western blot using GP5-specific monoclonal antibody 17B7, the AEC-purified EAV contained 86% GP5 monomer whereas the differentially centrifuged EAV contained <29% of the monomer. Improvement of analytical sensitivity without sacrifice of analytical specificity was clearly evident when cELISAs prepared with EAV antigen by each purification method were evaluated using 7 sensitivity and specificity check sets. Furthermore, the AEC-purified EAV-based cELISA had 30-40% higher agreement with the virus neutralization (VN) test than the cELISA prepared with differentially centrifuged EAV based on testing 40 borderline EAV-seropositive samples as defined by the VN test. In addition, the AEC-purified cELISA had highly significant (P = 0.001) robustness indicated by intra-laboratory repeatability and interlaboratory reproducibility when evaluated with the sensitivity check sets. Thus, use of AEC-purified EAV in the cELISA should lead to closer harmonization of the cELISA with the World Organization for Animal Health-prescribed VN test.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

  7. Synthesis of blue-photoluminescent graphene quantum dots/polystyrenic anion-exchange resin for Fe(III) detection

    NASA Astrophysics Data System (ADS)

    Zhang, Wenjun; Gan, Jie

    2016-05-01

    A novel solid fluorescent sensor with millimeter size, based on graphene quantum dots/polystyrenic anion-exchange resin (GQDs/PS-AER) was obtained for the detection of Fe3+. The linear response range of Fe3+ was obtained from 1 μM to 7 μM and the detection limit was as low as 0.65 μM. In addition, the sensor could be regenerated by adding complexing agent EDTA and be separated by using simple filtration.

  8. Nanoporous hollow transition metal chalcogenide nanosheets synthesized via the anion-exchange reaction of metal hydroxides with chalcogenide ions.

    PubMed

    Zhao, Weiwei; Zhang, Chao; Geng, Feiyang; Zhuo, Sifei; Zhang, Bin

    2014-10-28

    Nanoporous hollow transition metal chalcogenides are of special interest for a variety of promising applications. Although some advanced synthetic methods have been reported, the development of a facile and general strategy to fabricate porous hollow nanostructures of transition metal chalcogenides, especially with enhanced electrocatalytic performance, still remains highly challenged. Herein, we report a facile chemical transformation strategy to prepare nanoporous hollow Co3S4 nanosheets via the anion exchange reaction of Co(OH)2 with sulfide ions. The chemical transformation mechanism involves the as-formed layer of nanoporous cobalt sulfide on Co(OH)2 driven by the anion-exchange-reaction and lattice mismatch induced quick strain release, a following diffusion-effect-dominated core-shell hollow intermediate with hollow interiors, and subsequent Ostwald ripening growth of hollow nanosheets at elevated temperatures. This anion-exchange strategy of transition metal hydroxides with chalcogenide ions is also suitable for fabricating nanoporous hollow nanosheets of other metal chalcogenides (e.g., CoSe2, CoTe2, CdS, and NiS). The as-prepared nanoporous hollow Co3S4 nanosheets are found to be highly active and stable for electrocatalytic oxygen evolution reaction.

  9. Overlapping expression of anion exchangers in the cochlea of a non-human primate suggests functional compensation.

    PubMed

    Hosoya, Makoto; Fujioka, Masato; Kobayashi, Reona; Okano, Hideyuki; Ogawa, Kaoru

    2016-09-01

    Ion homeostasis in the inner ear is essential for proper hearing. Anion exchangers are one of the transporters responsible for the maintenance of homeostasis, but their expression profile in the primate cochlea has not been fully characterized. However, species-specific overlapping expression patterns and functional compensation in other organs, such as the kidney, pancreas and small intestine, have been reported. Here, we determined the expression patterns of the anion exchangers SLC26A4, SLC26A5, SLC26A6, SLC26A7, SLC26A11, SLC4A2 and SLC4A3 in the cochlea of a non-human primate, the common marmoset (Callithrix jacchus). Although the pattern of expression of SLC26A4 and SLC26A5 was similar to that in rodents, SLC26A7, SLC4A2, SLC4A3 exhibited different distributions. Notably, five transporters, SLC26A4, SLC26A6, SLC26A11 SLC4A2 and SLC4A3, were expressed in the cells of the outer sulcus. Our results reveal a species-specific distribution pattern of anion exchangers in the cochlea, particularly in the outer sulcus cells, suggesting functional compensation among these exchangers. This "primate-specific" pattern may be related to the human-specific hearing loss phenotypes of channelopathy disorders, including the SLC26A4-related diseases Pendred syndrome/DFNB4. PMID:27091614

  10. Functional characterization of three novel tissue-specific anion exchangers SLC26A7, -A8, and -A9.

    PubMed

    Lohi, Hannes; Kujala, Minna; Makela, Siru; Lehtonen, Eero; Kestila, Marjo; Saarialho-Kere, Ulpu; Markovich, Daniel; Kere, Juha

    2002-04-19

    A second distinct family of anion exchangers, SLC26, in addition to the classical SLC4 (or anion exchanger) family, has recently been delineated. Particular interest in this gene family is stimulated by the fact that the SLC26A2, SLC26A3, and SLC26A4 genes have been recognized as the disease genes mutated in diastrophic dysplasia, congenital chloride diarrhea, and Pendred syndrome, respectively. We report the expansion of the SLC26 gene family by characterizing three novel tissue-specific members, named SLC26A7, SLC26A8, and SLC26A9, on chromosomes 8, 6, and 1, respectively. The SLC26A7-A9 proteins are structurally very similar at the amino acid level to the previous family members and show tissue-specific expression in kidney, testis, and lung, respectively. More detailed characterization by immunohistochemistry and/or in situ hybridization localized SLC26A7 to distal segments of nephrons, SLC26A8 to developing spermatocytes, and SLC26A9 to the lumenal side of the bronchiolar and alveolar epithelium of lung. Expression of SLC26A7-A9 proteins in Xenopus oocytes demonstrated chloride, sulfate, and oxalate transport activity, suggesting that they encode functional anion exchangers. The functional characterization of the novel tissue-specific members may provide new insights to anion transport physiology in different parts of body. PMID:11834742

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

    PubMed

    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.

  12. Click Chemistry Finds Its Way in Constructing an Ionic Highway in Anion-Exchange Membrane.

    PubMed

    Ge, Qianqian; Ran, Jin; Miao, Jibin; Yang, Zhengjin; Xu, Tongwen

    2015-12-30

    To find the way to construct an ionic highway in anion-exchange membranes (AEMs), a series of side-chain-type alkaline polymer electrolytes (APEs) based on poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) polymer backbones were synthesized via Cu(I)-catalyzed click chemistry. The resulting triazole groups and quaternary ammonium (QA) groups facilitate the formation of a continuous hydrogen bond network, which will lead to high hydroxide conductivity according to Grotthuss-type mechanism. Microphase separation induced by long alkyl side chains contributes at the same time to further improving the hydroxide conductivity of the resultant AEMs. Hydroxide conductivity as high as 52.8 mS/cm is obtained for membrane TA-14C-1.21 (IEC = 1.21 mmol/g) with the longest pendant chain at 30 °C, and the conductivity can be increased to 140 mS/cm when the temperature was increased to 80 °C. Moreover, the corresponding water uptake is only 8.6 wt % at 30 °C. In the meantime, the membrane properties can be tuned by precisely regulating the hydrophilic/hydrophobic ratio in the cationic head groups. Compared with AEMs containing triazole and quaternized trimethylammonium head groups, enhanced dimensional stability and mechanical properties are obtained by tuning side-chain chemistry. However, the alkaline stability of the membrane is not as stable as anticipated, probably because of the existence of the triazole ring. Further study will be focused on increasing the alkali stability of the membrane. We envisage that the side-chain-type APEs meditated by click chemistry bearing long hydrophobic side chains pendant to the cationic head groups hold promise as a novel AEMs material. PMID:26645427

  13. Towards high conductivity in anion-exchange membranes for alkaline fuel cells.

    PubMed

    Li, Nanwen; Guiver, Michael D; Binder, Wolfgang H

    2013-08-01

    Quaternized poly(2,6-dimethylphenylene oxide) materials (PPOs) containing clicked 1,2,3-triazoles were first prepared through Cu(I) -catalyzed "click chemistry" to improve the anion transport in anion-exchange membranes (AEMs). Clicked 1,2,3-triazoles incorporated into AEMs provided more sites to form efficient and continuous hydrogen-bond networks between the water/hydroxide and the triazole for anion transport. Higher water uptake was observed for these triazole membranes. Thus, the membranes showed an impressive enhancement of the hydroxide diffusion coefficient and, therefore, the anion conductivities. The recorded hydroxide conductivity was 27.8-62 mS cm(-1) at 20 °C in water, which was several times higher than that of a typical PPO-based AEM (TMA-20) derived from trimethylamine (5 mS cm(-1) ). Even at reduced relative humidity, the clicked membrane showed superior conductivity to a trimethylamine-based membrane. Moreover, similar alkaline stabilities at 80 °C in 1 M NaOH were observed for the clicked and non-clicked membranes. The performance of a H2 /O2 single cell assembled with a clicked AEM was much improved compared to that of a non-clicked TMA-20 membrane. The peak power density achieved for an alkaline fuel cell with the synthesized membrane 1a(20) was 188.7 mW cm(-2) at 50 °C. These results indicated that clicked AEM could be a viable strategy for improving the performance of alkaline fuel cells.

  14. Protonation and ion exchange equilibria of weak base anion-exchange resins.

    PubMed

    Miyazaki, Yoshinobu; Nakai, Mariko

    2011-09-30

    Protonation and ion exchange equilibria of weak base anion-exchange resins, in which tertiary amine moieties were introduced as a functional group, were investigated by applying NMR spectroscopy to species adsorbed into the resins. (31)P NMR signals of the phosphinate ion in the resin phases shifted to a lower field due to the influence of protonation of the tertiary amine groups of the resins in the pH range of 4-10. Protonation constants of the tertiary amine groups in styrene-divinylbenzene (DVB)-based resins were estimated to be K(H)=10(6.4) for Amberlite IRA96 and 10(6.5) for DIAION WA30 by the (31)P NMR method using the phosphinate ion as a probe species. In addition to the low field shift caused by the protonation of the tertiary amine moieties, another low field shift was observed for the phosphinate ion in acrylic acid-DVB-based resins at a rather high pH. This shift should be due to an unexpected deprotonation in the acrylic resin: a tautomerism accompanying the proton release from the amide form to the imide one in the functional group, thus, the resin could exhibit a cation exchange property at the high pH. Protonation constants of the tertiary amine moieties in the acrylic resins were estimated to be 10(8.8) for DIAION WA10, 10(9.0) for Amberlite IRA67 and 10(9.3) for Bio-Rad AG 4-X4 on the basis of the Henderson-Hasselbalch equation using the resin phase pH estimated by the (133)Cs and (1)H NMR signal intensities.

  15. Chemical separation of Mo and W from terrestrial and extraterrestrial samples via anion exchange chromatography.

    PubMed

    Nagai, Yuichiro; Yokoyama, Tetsuya

    2014-05-20

    A new two-stage chemical separation method was established using an anion exchange resin, Eichrom 1 × 8, to separate Mo and W from four natural rock samples. First, the distribution coefficients of nine elements (Ti, Fe, Zn, Zr, Nb, Mo, Hf, Ta, and W) under various chemical conditions were determined using HCl, HNO3, and HF. On the basis of the obtained distribution coefficients, a new technique for the two-stage chemical separation of Mo and W, along with the group separation of Ti-Zr-Hf, was developed as follows: 0.4 M HCl-0.5 M HF (major elements), 9 M HCl-0.05 M HF (Ti-Zr-Hf), 9 M HCl-1 M HF (W), and 6 M HNO3-3 M HF (Mo). After the chemical procedure, Nb remaining in the W fraction was separated using 9 M HCl-3 M HF. On the other hand, Nb and Zn remaining in the Mo fraction were removed using 2 M HF and 6 M HCl-0.1 M HF. The performance of this technique was evaluated by separating these elements from two terrestrial and two extraterrestrial samples. The recovery yields for Mo, W, Zr, and Hf were nearly 100% for all of the examined samples. The total contents of the Zr, Hf, W, and Mo in the blanks used for the chemical separation procedure were 582, 9, 29, and 396 pg, respectively. Therefore, our new separation technique can be widely used in various fields of geochemistry, cosmochemistry, and environmental sciences and particularly for multi-isotope analysis of these elements from a single sample with significant internal isotope heterogeneities.

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

    SciTech Connect

    Duangtum, Natapol; Junking, Mutita; Sawasdee, Nunghathai; Cheunsuchon, Boonyarit; Limjindaporn, Thawornchai; Yenchitsomanus, Pa-thai

    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.

  17. Anion exchanger immunoreactivity in human salivary glands in health and Sjögren's syndrome.

    PubMed Central

    Vázquez, J. J.; Vázquez, M.; Idoate, M. A.; Montuenga, L.; Martínez-Ansó, E.; Castillo, J. E.; García, N.; Medina, J. F.; Prieto, J.

    1995-01-01

    Salivary gland ducts play a relevant role in saliva secretion through transport processes. Na(+)-independent chloride-bicarbonate anion exchangers (AE) may be involved in these processes by generating ion fluxes into the salivary secretion. In Sjögren's syndrome, a disorder with gland dysfunction, there might be an impaired expression of AE proteins. Here we study AE immunoreactivities in human salivary glands, both in health and in Sjögren's syndrome. Immunohistochemistry was carried out on salivary glands from normal subjects and patients with Sjögren's syndrome, using two monoclonal antibodies against AE1 and AE2. Normal salivary glands showed AE2 immunoreactivity, which was restricted to the epithelium of the ducts, with no staining at the acini. A strong positivity was seen in the basolateral portion of the striated ducts, while interlobular duct cells showed a discrete positivity at their apical pole. In salivary glands from most of the patients with Sjögren's syndrome, AE2 immunoreactivity was absent in the ducts as well as in the acini. In both normal and diseased salivary glands, AE1 immunoreactivity was only located at the erythrocyte membrane. The recently reported AE0 was discarded because no AE0 message was found in salivary glands by reverse transcription polymerase chain reaction. In conclusion, AE2 immunoreactivity is observed in the ducts of normal salivary glands, particularly in the striated ducts. AE2 immunoreactivity is virtually absent in salivary glands from patients with Sjögren's syndrome, which may reflect either a loss of AE2 after inflammatory atrophy, or a primary defect occurring in the disease. Images Figure 2 Figure 3 Figure 4 Figure 5 PMID:7778681

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

    PubMed

    Urso, Katia; Charles, Julia F; Shull, Gary E; Aliprantis, Antonios O; Balestrieri, Barbara

    2016-01-01

    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. PMID:27391897

  19. Separation of boric acid in liquid waste with anion exchange membrane contactor

    SciTech Connect

    Park, J.K.; Lee, K.J.

    1995-12-31

    In order to separate boric acid in liquid waste, some possible technologies were investigated and the membrane contactor without dispersion and density differences was selected. The separation experiments on a Celgard 3401{reg_sign} hydrophilic microporous membrane contactor were first performed to obtain the basic data and to determine the properties of the contactor. The experimental conditions were as follows: boric acid concentrations up to 2.0 M, pH 7.0, temperatures of 25 and 55 C, and flow rates of 100, 300, 500, and 800 cm{sup 3}/min. Secondly, an AFN{reg_sign} anion exchange membrane contactor was tested at temperatures of 40 and 55 C and flow rate 400 cm{sup 3}/min. Boric acid solutions were prepared by the same method as that for Celgard 3401{reg_sign} but contained 5.0{times}10{sup {minus}4} M cobalt chloride (CoCl{sub 2}). To simulate membrane contractors, parameters such as the differential diffusion coefficients of boric acid and the mass transfer coefficients in the AFN membrane were measured, and regression models estimating the diffusion coefficient at several conditions were developed. The Celgard 3401{reg_sign} membrane contactor was simulated and compared with experimental data. Simulation results agreed with the experimental data well when a proper correction factor was utilized. The correction factor was independent of the solution temperature and was 8.75 at the flow rates of 300--800 cm{sup 3}/min. This correction factor was also applied to simulate the AFN{reg_sign} resulted in a good agreement with experiment at 40 C, but not 55 C. The retention on cobalt was also better at 40 c than 55 C. The simulating computer program was also applied to a life size contactor designed conceptually.

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

    PubMed Central

    Urso, Katia; Charles, Julia F.; Shull, Gary E.; Aliprantis, Antonios O.; Balestrieri, Barbara

    2016-01-01

    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. PMID:27391897

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

    PubMed

    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

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

    SciTech Connect

    Bartsch, Richard A.; Barr, Mary E.

    2001-04-30

    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. A Robust and Fully-Automated Chromatographic Method for the Quantitative Purification of Ca and Sr for Isotopic Analysis

    NASA Astrophysics Data System (ADS)

    Smith, H. B.; Kim, H.; Romaniello, S. J.; Field, P.; Anbar, A. D.

    2014-12-01

    High throughput methods for sample purification are required to effectively exploit new opportunities in the study of non-traditional stable isotopes. Many geochemical isotopic studies would benefit from larger data sets, but these are often impractical with manual drip chromatography techniques, which can be time-consuming and demand the attention of skilled laboratory staff. Here we present a new, fully-automated single-column method suitable for the purification of both Ca and Sr for stable and radiogenic isotopic analysis. The method can accommodate a wide variety of sample types, including carbonates, bones, and teeth; silicate rocks and sediments; fresh and marine waters; and biological samples such as blood and urine. Protocols for these isotopic analyses are being developed for use on the new prepFAST-MCTM system from Elemental Scientific (ESI). The system is highly adaptable and processes up to 24-60 samples per day by reusing a single chromatographic column. Efficient column cleaning between samples and an all Teflon flow path ensures that sample carryover is maintained at the level of background laboratory blanks typical for manual drip chromatography. This method is part of a family of new fully-automated chromatographic methods being developed to address many different isotopic systems including B, Ca, Fe, Cu, Zn, Sr, Cd, Pb, and U. These methods are designed to be rugged and transferrable, and to allow the preparation of large, diverse sample sets via a highly repeatable process with minimal effort.

  4. Automated high-throughput purification of genomic DNA from whole blood using Promega's MagneSilTM paramagnetic particles with either the Max Yield or MagneSilTM ONE normalized purification methods

    NASA Astrophysics Data System (ADS)

    Bitner, Rex M.; Koller, Susan C.; Sankbeil, Jacqui

    2003-07-01

    Two different methods of automated high throughput purification of genomic DNA from human whole blood in 96 well plates are described. One method uses MagneSilTM paramagnetic particles to purify a maximal amount of the DNA present in the sample. Another method, the MagnesilTM ONE system, allows for the purification of a predetermined amount of DNA from human whole blood. Protocols for the purification of 100 ng or, alternatively 1 ug, of human genomic DNA from whole blood using MagneSilTM paramagnetic particles and a Beckman BioMekTM FX robot are described. With the maximal yield purification system, typical DNA yields fall in the range of 4-9 ug of DNA from 200ul of human whole blood, depending upon the white cell content of donor sample. For situations where DNA achiving is desired, or when the number of downstream sample applications is not clearly defined (e.g. multiple SNP analyses) the maximal yield method is usually preferred. However, in situations with a defined downstream application (e.g. criminal databasing or use of a defined set of amplifications) where purifying DNA in a narrow concentrate range streamlines the high throughput purification and analysis process, the automated MagneSilTM ONE purification system is the method of choice. DNA from either method is suitable for applications such as PCR, STR, READITTM SNP analysis, and multiplexed PCR systems such as Promega's Y-chromosome deletion detection system.

  5. Rapid sequential determination of Pu, 90Sr and 241Am nuclides in environmental samples using an anion exchange and Sr-Spec resins.

    PubMed

    Lee, M H; Ahn, H J; Park, J H; Park, Y J; Song, K

    2011-02-01

    This paper presents a quantitative and rapid method of sequential separation of Pu, (90)Sr and (241)Am nuclides in environmental soil samples with an anion exchange resin and Sr Spec resin. After the sample solution was passed through an anion exchange column connected to a Sr Spec column, Pu isotopes were purified from the anion exchange column. Strontium-90 was separated from other interfering elements by the Sr Spec column. Americium-241 was purified from lanthanides by the anion exchange resin after oxalate co-precipitation. Measurement of Pu and Am isotopes was carried out using an α-spectrometer. Strontium-90 was measured by a low-level liquid scintillation counter. The radiochemical procedure of Pu, (90)Sr and (241)Am nuclides investigated in this study validated by application to IAEA reference materials and environmental soil samples.

  6. SLC26 anion exchangers of guinea pig pancreatic duct: molecular cloning and functional characterization

    PubMed Central

    Stewart, Andrew K.; Shmukler, Boris E.; Vandorpe, David H.; Reimold, Fabian; Heneghan, John F.; Nakakuki, M.; Akhavein, Arash; Ko, Shigeru; Ishiguro, Hiroshi

    2011-01-01

    The secretin-stimulated human pancreatic duct secretes HCO3−-rich fluid essential for normal digestion. Optimal stimulation of pancreatic HCO3− secretion likely requires coupled activities of the cystic fibrosis transmembrane regulator (CFTR) anion channel and apical SLC26 Cl−/HCO3− exchangers. However, whereas stimulated human and guinea pig pancreatic ducts secrete ∼140 mM HCO3− or more, mouse and rat ducts secrete ∼40–70 mM HCO3−. Moreover, the axial distribution and physiological roles of SLC26 anion exchangers in pancreatic duct secretory processes remain controversial and may vary among mammalian species. Thus the property of high HCO3− secretion shared by human and guinea pig pancreatic ducts prompted us to clone from guinea pig pancreatic duct cDNAs encoding Slc26a3, Slc26a6, and Slc26a11 polypeptides. We then functionally characterized these anion transporters in Xenopus oocytes and human embryonic kidney (HEK) 293 cells. In Xenopus oocytes, gpSlc26a3 mediated only Cl−/Cl− exchange and electroneutral Cl−/HCO3− exchange. gpSlc26a6 in Xenopus oocytes mediated Cl−/Cl− exchange and bidirectional exchange of Cl− for oxalate and sulfate, but Cl−/HCO3− exchange was detected only in HEK 293 cells. gpSlc26a11 in Xenopus oocytes exhibited pH-dependent Cl−, oxalate, and sulfate transport but no detectable Cl−/HCO3− exchange. The three gpSlc26 anion transporters exhibited distinct pharmacological profiles of 36Cl− influx, including partial sensitivity to CFTR inhibitors Inh-172 and GlyH101, but only Slc26a11 was inhibited by PPQ-102. This first molecular and functional assessment of recombinant SLC26 anion transporters from guinea pig pancreatic duct enhances our understanding of pancreatic HCO3− secretion in species that share a high HCO3− secretory output. PMID:21593449

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

    NASA Astrophysics Data System (ADS)

    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. Selective Anion Exchange Resins for the Removal of Perchlorate [(CIO{sub 4}{sup -})] from Groundwater

    SciTech Connect

    Gu, B.

    1999-05-20

    The primary objective of this project was to evaluate a novel bifunctional anion exchange resin for the cost-effective, in situ treatment of groundwater contaminated with perchlorate (ClO{sub 4}{sup -}). Both laboratory and field studies were performed to determine the selectivity and capacity of the bifunctional synthetic resins to sorb ClO{sub 4}{sup -} from simulated or actual contaminated groundwater. A number of synthetic bifunctional resins, including two commercial versions made by Purolite International and three commercially available, mono-functional resins, were tested. Initial laboratory batch and column breakthrough studies determined the best synthetic resins and the optimal conditions for the field experiment. Laboratory results indicated that the bifunctional synthetic resins, D-3696 and RO-02-119 were highly selective toward ClO{sub 4}{sup -} and performed {approx}5 times better than the best commercial nitrate resin (Purolite{reg_sign} A-520E) and more than an order of magnitude better than some nonselective commercial resins (e.g. Amberlite{reg_sign} IRA-900). The bifunctional resins were particularly effective in removing trace quantities of ClO{sub 4}{sup -} in groundwater to below the detection limit ({approx} 3 {micro}g/L). A field trial demonstrated that the bifunctional resin (D-3696) was able to treat {approx} 110,000 bed volumes of groundwater before a 10% breakthrough of ClO{sub 4}{sup -} occurred under the column flow-through conditions (running at {approx} 2 bed volumes per minute). On the other hand, the Purolite{reg_sign} A-520E resin was able to treat {approx} 23,000 bed volumes of groundwater under the same experimental conditions. No pretreatment was needed to remove either dissolved organic matter or other competing anions (such as SO{sub 4}{sup 2-} or NO{sub 3}{sup -}) in the groundwater, and the treatment process did not alter the water quality by removing or adding secondary by-products because of the high selectivity of the

  9. Strategies for automated sample preparation, nucleic acid purification, and concentration of low-target-number nucleic acids in environmental and food processing samples

    NASA Astrophysics Data System (ADS)

    Bruckner-Lea, Cynthia J.; Holman, David A.; Schuck, Beatrice L.; Brockman, Fred J.; Chandler, Darrell P.

    1999-01-01

    The purpose of this work is to develop a rapid, automated system for nucleic acid purification and concentration from environmental and food processing samples. Our current approach involves off-line filtration and cell lysis (ballistic disintegration) functions in appropriate buffers followed by automated nucleic acid capture and purification on renewable affinity matrix microcolumns. Physical cell lysis and renewable affinity microcolumns eliminate the need for toxic organic solvents, enzyme digestions or other time- consuming sample manipulations. Within the renewable affinity microcolumn, we have examined nucleic acid capture and purification efficiency with various microbead matrices (glass, polymer, paramagnetic), surface derivitization (sequence-specific capture oligonucleotides or peptide nucleic acids), and DNA target size and concentration under variable solution conditions and temperatures. Results will be presented comparing automated system performance relative to benchtop procedures for both clean (pure DNA from a laboratory culture) and environmental (soil extract) samples, including results which demonstrate 8 minute purification and elution of low-copy nucleic acid targets from a crude soil extract in a form suitable for PCR or microarray-based detectors. Future research will involve the development of improved affinity reagents and complete system integration, including upstream cell concentration and cell lysis functions and downstream, gene-based detectors. Results of this research will ultimately lead to improved processes and instrumentation for on-line, automated monitors for pathogenic micro-organisms in food, water, air, and soil samples.

  10. Human kidney anion exchanger 1 interacts with adaptor-related protein complex 1 μ1A (AP-1 mu1A).

    PubMed

    Sawasdee, Nunghathai; Junking, Mutita; Ngaojanlar, Piengpaga; Sukomon, Nattakan; Ungsupravate, Duangporn; Limjindaporn, Thawornchai; Akkarapatumwong, Varaporn; Noisakran, Sansanee; Yenchitsomanus, Pa-Thai

    2010-10-01

    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 YXXØ 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. PMID:20833140

  11. Electrostatic potentials and electrostatic interaction energies of rat cytochrome b5 and a simulated anion-exchange adsorbent surface.

    PubMed Central

    Roush, D J; Gill, D S; Willson, R C

    1994-01-01

    Electrostatic potentials were determined for the soluble tryptic core of rat cytochrome b5 (using a structure derived from homology modeling) and a simulated anion-exchange surface through application of the linearized finite-difference Poisson-Boltzmann equation with the simulation code UHBD. Objectives of this work included determination of the contributions of the various charged groups on the protein surface to electrostatic interactions with a simulated anion-exchange surface as a function of orientation, separation distance, and ionic strength, as well as examining the potential existence of a preferred contact orientation. Electrostatic interaction free energies for the complex of the model protein and the simulated surface were computed using the electrostatics section of UHBD employing a 110(3) grid. An initial coarse grid spacing of 2.0 A was required to obtain correct boundary conditions. The boundary conditions of the coarse grid were used in subsequent focusing steps until the electrostatic interaction free energies were relatively independent of grid spacing (at approximately 0.5 A). Explicit error analyses were performed to determine the effects of grid spacing and other model assumptions on the electrostatic interaction free energies. The computational results reveal the presence of a preferred interaction orientation; the interaction energy between these two entities, of opposite net charge, is repulsive over a range of orientations. The electrostatic interaction free energies appear to be the summation of multiple fractional interactions between the protein and the anion-exchange surface. The simulation results are compared with those of ion-exchange adsorption experiments with site-directed mutants of the recombinant protein. Comparisons of the results from the computational and experimental studies should lead to a better understanding of electrostatic interactions of proteins and charged surfaces. Images FIGURE 4 FIGURE 5 FIGURE 6 PMID:8061185

  12. Role of anion exchangers in Cl- and HCO3- secretion by the human airway epithelial cell line Calu-3.

    PubMed

    Kim, Dusik; Kim, Juyeon; Burghardt, Beáta; Best, Len; Steward, Martin C

    2014-07-15

    Despite the importance of airway surface liquid pH in the lung's defenses against infection, the mechanism of airway HCO3- secretion remains unclear. Our aim was to assess the contribution of apical and basolateral Cl-/HCO3- exchangers to Cl- and HCO3- transport in the Calu-3 cell line, derived from human airway submucosal glands. Changes in intracellular pH (pHi) were measured following substitution of Cl- with gluconate. Apical Cl- substitution led to an alkalinization in forskolin-stimulated cells, indicative of Cl-/HCO3- exchange. This was unaffected by the anion exchange inhibitor DIDS but inhibited by the CFTR blocker CFTRinh-172, suggesting that the HCO3- influx might occur via CFTR, rather than a solute carrier family 26 (SLC26) exchanger, as recently proposed. The anion selectivity of the recovery process more closely resembled that of CFTR than an SLC26 exchanger, and quantitative RT-PCR showed only low levels of SLC26 exchanger transcripts relative to CFTR and anion exchanger 2 (AE2). For pHi to rise to observed values (∼7.8) through HCO3- entry via CFTR, the apical membrane potential must reverse to at least +20 mV following Cl- substitution; this was confirmed by perforated-patch recordings. Substitution of basolateral Cl- evoked a DIDS-sensitive alkalinization, attributed to Cl-/HCO3- exchange via AE2. This appeared to be abolished in forskolin-stimulated cells but was unmasked by blocking apical efflux of HCO3- via CFTR. We conclude that Calu-3 cells secrete HCO3- predominantly via CFTR, and, contrary to previous reports, the basolateral anion exchanger AE2 remains active during stimulation, providing an important pathway for basolateral Cl- uptake.

  13. Flavourzyme, an Enzyme Preparation with Industrial Relevance: Automated Nine-Step Purification and Partial Characterization of Eight Enzymes.

    PubMed

    Merz, Michael; Eisele, Thomas; Berends, Pieter; Appel, Daniel; Rabe, Swen; Blank, Imre; Stressler, Timo; Fischer, Lutz

    2015-06-17

    Flavourzyme is sold as a peptidase preparation from Aspergillus oryzae. The enzyme preparation is widely and diversely used for protein hydrolysis in industrial and research applications. However, detailed information about the composition of this mixture is still missing due to the complexity. The present study identified eight key enzymes by mass spectrometry and partially by activity staining on native polyacrylamide gels or gel zymography. The eight enzymes identified were two aminopeptidases, two dipeptidyl peptidases, three endopeptidases, and one α-amylase from the A. oryzae strain ATCC 42149/RIB 40 (yellow koji mold). Various specific marker substrates for these Flavourzyme enzymes were ascertained. An automated, time-saving nine-step protocol for the purification of all eight enzymes within 7 h was designed. Finally, the purified Flavourzyme enzymes were biochemically characterized with regard to pH and temperature profiles and molecular sizes.

  14. Separation of alditols of interest in food products by high-performance anion-exchange chromatography with pulsed amperometric detection.

    PubMed

    Corradini, C; Canali, G; Cogliandro, E; Nicoletti, I

    1997-12-12

    High-performance anion-exchange chromatography (HPAEC)-pulsed amperometric detection (PAD) employing a CarboPac MA 1 column was investigated with respect to mobile phase composition, linear response characteristics, repeatability, reproducibility and sensitivity with different alditols used as sugar substitutes in food and confectionery products. The energy-reduced bulk sweeteners isomalt and maltitol were well resolved in less than 25 min by isocratic elution with 600 mM sodium hydroxide solution. HPAEC-PAD was also successfully applied to the determination of alditols in sugar-free products and a low-calorie sweetener containing sorbitol, mannitol and fructose at different levels.

  15. Ion-exchange selectivity of tertiary pyridine-type anion-exchange resin for treatment of spent nuclear fuels

    SciTech Connect

    Nogami, Masanobu; Aida, Masao; Fujii, Yasuhiko; Maekawa, Akira; Ohe, Shinobu; Kawai, Hiroomi; Yoneda, Morihiro

    1996-09-01

    The tertiary pyridine-type anion-exchange resin has been synthesized for the treatment of spent nuclear fuels and high-level radioactive waste. This resin, with a uniform diameter of 60 {micro}m, is mechanically strong enough and shows no swelling or shrinking regardless of its chemical forms. Systematic analysis was made of the adsorption selectivities of the resin in HCl solutions for a number of cations that exist in spent fuels, such as uranium and fission product elements. The results indicate that the resin is suitable to be used for the treatment of spent fuels and high-level radioactive waste.

  16. Disposable and removable nucleic acid extraction and purification cartridges for automated flow-through systems

    SciTech Connect

    Regan, John Frederick

    2014-09-09

    Removable cartridges are used on automated flow-through systems for the purpose of extracting and purifying genetic material from complex matrices. Different types of cartridges are paired with specific automated protocols to concentrate, extract, and purifying pathogenic or human genetic material. Their flow-through nature allows large quantities sample to be processed. Matrices may be filtered using size exclusion and/or affinity filters to concentrate the pathogen of interest. Lysed material is ultimately passed through a filter to remove the insoluble material before the soluble genetic material is delivered past a silica-like membrane that binds the genetic material, where it is washed, dried, and eluted. Cartridges are inserted into the housing areas of flow-through automated instruments, which are equipped with sensors to ensure proper placement and usage of the cartridges. Properly inserted cartridges create fluid- and air-tight seals with the flow lines of an automated instrument.

  17. Degradation of Imidazolium- and Quaternary Ammonium-Functionalized Poly(fluorenyl ether ketone sulfone) Anion Exchange Membranes

    SciTech Connect

    Chen, DY; Hickner, MA

    2012-11-01

    Imidazolium and quaternary ammonium-functionalized poly(fluorenyl ether ketone sulfone)s were synthesized successfully with the same degree of cationic functionalization and identical polymer backbones for a comparative study of anion exchange membranes (AEMs) for solid-state alkaline membrane fuel cells (AMFCs). Both anion exchange membranes were synthesized using a new methyl-containing monomer that avoided the use of toxic chloromethylation reagents. The polymer chemical structures were confirmed by H-1 NMR and FTIR. The derived AEMs were fully characterized by water uptake, anion conductivity, stability under aqueous basic conditions, and thermal stability. Interestingly, both the cationic groups and the polymer backbone were found to be degraded in 1 M NaOH solution at 60 degrees C over 48 h as measured by changes of ion exchange capacity and intrinsic viscosity. Imidazolium-functionalized poly(fluorenyl ether ketone sulfone)s had similar aqueous alkaline stability to quaternary ammonium-functionalized materials at 60 degrees C but much lower stability at 80 degrees C. This work demonstrates that quaternary ammonium and imidazolium cationic groups are not stable on poly(arylene ether sulfone) backbones under relatively mild conditions. Additionally, the poly(arylene ether sulfone) backbone, which is one of the most common polymers used in ion exchange membrane applications, is not stable in the types of molecular configurations analyzed.

  18. Alkaline stable C2-substituted imidazolium-based cross-linked anion exchange membranes for alkaline fuel cell applications

    NASA Astrophysics Data System (ADS)

    Lin, Bencai; Chu, Fuqiang; Ren, Yurong; Jia, Baoping; Yuan, Ningyi; Shang, Hui; Feng, Tianying; Zhu, Yuanyuan; Ding, Jianning

    2014-11-01

    Novel C2-substituted imidazolium-based cross-linked anion exchange membranes (AEMs) are prepared via irradiation with ultraviolet light cross-linking of styrene, acrylonitrile and 1,3-diallyl-2-methyl imidazolium bromine ([DAMIm][Br]), and followed by anion exchange with hydroxide ions. [DAMIm][Br] is synthesized and used both as crosslinker and hydrophilic phase. The ionic conductivity of the AEMs increases with increasing [DAMIm][Br] content due to the hydrophilic regions and the continuous hydrophilic polymeric networks formed in the membranes. The imidazolium-based cross-linked AEMs show excellent thermal stabilities, and the membrane which containing 30% mass fraction of [DAMIm][Br] shows ionic conductivity up to 2.0 × 10-2 S cm-1 and good long-term chemical stability in 1 M KOH solution. The results of this study suggest that the C2-substituted imidazolium-based cross-linked AEMs have good perspectives for alkaline fuel cell applications.

  19. Anion-exchange resin-based desulfurization process. Quarterly technical progress report, January 1, 1993--March 31, 1993

    SciTech Connect

    Sheth, A.C.; Dharmapurikar, R.

    1993-06-01

    Under DOE Grant No. FG22-90PC90309, the University of Tennessee Space Institute (UTSI) is contracted to further develop its anion-exchange, resin-based desulfurization concept to desulfurize alkali metal sulfates. From environmental as well as economic viewpoints, it is necessary to remove soluble sulfates from the wastes created by flue gas desulfurization systems. In order to do this economically, a low-cost desulfurization process for spent sorbents is necessary. UTSI`s anion-exchange resin-based desulfurization concept is believed to satisfy these requirements. UTSI has completed the batch mode experiments to locate the position of the CO{sub 3}{sup 2} and SO{sub 4}{sup 2} ions in the affinity chart. Also, the reviews of the ASPEN Code`s capabilities and EPRI-TAG document`s methodology are in progress for developing the Best Process Schematic and related economics. The fixed-bed experiments are also in progress to evaluate the cycle efficiency of the candidate resins. So far we have completed ten consecutive cycles of exhaustion/carbonation and regeneration for IRA-35 resin. Because of the past problems (now resolved) with the fixed-bed system, the addition of batch mode screening experiments, Christmas holidays and spring break, and the moving of UTSI`s Chemistry Laboratory to a new location, the program is about 6--8 weeks behind schedule, but well within the budget.

  20. Investigation of Anion-Exchange and Immunoaffinity Particle-Loaded Membranes for the Isolation of Charged Organic Analytes from Water

    USGS Publications Warehouse

    Dombrowski, T.R.; Wilson, G.S.; Thurman, E.M.

    1998-01-01

    Anion-exchange and immunoaffinity particle loaded membranes (PLMs) were investigated as a mechanism for the isolation of charged organic analytes from water. Kinetic properties determined theoretically included dynamic capacity, pressure drop (??P), residence and diffusion times (Tr, Td), and total membrane porosity (???T). These properties were confirmed through experimental evaluation, and the PLM method showed significant improvement over conventional solid-phase extraction (SPE) and ion-exchange formats. Recoveries of more than 90% were observed for a variety of test compounds at flow rates up to 70 mL/min (equipment-limited maximum flow rate). A fast-flow immunoaffinity column was developed using antibodies (Abs) attached to the PLMs. Reproducible recoveries (88% ?? 4%) were observed at flow rates up to 70 mL/min for the antibody (Ab)-loaded PLMs. Findings indicate increased selectivity over anion-exchange PLMs and conventional SPE or ion-exchange methods and rapid Ab-antigen binding rates given the excellent mass-transfer characteristics of the PLMs.

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

    PubMed

    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. PMID:24275475

  2. Anion-exchange resin-based desulfurization process. Annual technical progress report, October 1, 1992--September 30, 1993

    SciTech Connect

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

    1993-11-01

    Under the DOE Grant No. DE-FG22-90PC90309, the University of Tennessee Space Institute (UTSI) has been directed to further develop an anion-exchange, resin-based desulfurization concept that has been developed and tested on a limited scope for feasibility. From environmental as well as the economic viewpoints, it is necessary that the soluble sulfates of alkali metal sorbents be desulfurized (regenerated) and recycled to make regenerative flue gas desulfurization and MHD spent seed regeneration options more attractive. In order to achieve this, a low-temperature, low-cost desulfurization process to reactivate spent alkali metal sorbents is necessary. UTSI`s anion-exchange, resin-based concept uses the available technology and is believed to satisfy this requirement. In this DOE-sponsored project, UTSI, will perform the following investigations: Screening of commercially available resins; process variables study and improving resin performance; optimization of resin-regeneration step; evaluation of performance enhancers; development of Best-Process Schematic and related economics, and planning for proof-of-concept (POC) scale testing. The above activities have been grouped into five major tasks and the entire project is expected to take thirty-six months to complete.

  3. Boric acid increases the expression levels of human anion exchanger genes SLC4A2 and SLC4A3.

    PubMed

    Akbas, F; Aydin, Z

    2012-04-03

    Boron is an important micronutrient in plants and animals. The role of boron in living systems includes coordinated regulation of gene expression, growth and proliferation of higher plants and animals. There are several well-defined genes associated with boron transportation and tolerance in plants and these genes show close homology with human anion exchanger genes. Mutation of these genes also characterizes some genetic disorders. We investigated the toxic effects of boric acid on HEK293 cells and mRNA expression of anion exchanger (SLC4A1, SLC4A2 and SLC4A3) genes. Cytotoxicity of boric acid at different concentrations was tested by using the methylthiazolyldiphenyl-tetrazolium bromide assay. Gene expression profiles were examined using quantitative real-time PCR. In the HEK293 cells, the nontoxic upper concentration of boric acid was 250 μM; more than 500 μM caused cytotoxicity. The 250 μM boric acid concentration increased gene expression level of SLC4A2 up to 8.6-fold and SLC4A3 up to 2.6-fold, after 36-h incubation. There was no significant effect of boric acid on SLC4A1 mRNA expression levels.

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

    PubMed

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

    2009-07-17

    A simple accurate method for determining amino acid composition of wheat gluten proteins and their gliadin and glutenin fractions using high-performance anion-exchange chromatography with integrated pulsed amperometric detection is described. In contrast to most conventional methods, the analysis requires neither pre- or post-column derivatization, nor oxidation of the sample. It consists of hydrolysis (6.0M hydrochloric acid solution at 110 degrees C for 24h), evaporation of hydrolyzates (110 degrees C), and chromatographic separation of the liberated amino acids. Correction factors (f) accounted for incomplete cleavage of peptide bonds involving Val (f=1.07) and Ile (f=1.13) after hydrolysis for 24h and for Ser (f=1.32) losses during evaporation. Gradient conditions including an extra eluent (0.1M acetic acid solution) allowed multiple sequential sample analyses without risk of Glu contamination on the anion-exchange column. While gluten amino acid compositions by the present method were mostly comparable to those obtained by a conventional method involving oxidation, acid hydrolysis and post-column ninhydrin derivatization, the latter method underestimated Tyr, Val and Ile levels. Results for the other amino acids obtained by the different methods were linearly correlated (r>0.99, slope=1.03).

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

    PubMed

    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.

  6. Preparation of a weak anion exchange/hydrophobic interaction dual-function mixed-mode chromatography stationary phase for protein separation using click chemistry.

    PubMed

    Zhao, Kailou; Yang, Fan; Xia, Hongjun; Wang, Fei; Song, Qingguo; Bai, Quan

    2015-03-01

    In this study, 3-diethylamino-1-propyne was covalently bonded to the azide-silica by a click reaction to obtain a novel dual-function mixed-mode chromatography stationary phase for protein separation with a ligand containing tertiary amine and two ethyl groups capable of electrostatic and hydrophobic interaction functionalities, which can display hydrophobic interaction chromatography character in a high-salt-concentration mobile phase and weak anion exchange character in a low-salt-concentration mobile phase employed for protein separation. As a result, it can be employed to separate proteins with weak anion exchange and hydrophobic interaction modes, respectively. The resolution and selectivity of the stationary phase were evaluated in both hydrophobic interaction and ion exchange modes with standard proteins, respectively, which can be comparable to that of conventional weak anion exchange and hydrophobic interaction chromatography columns. Therefore, the synthesized weak anion exchange/hydrophobic interaction dual-function mixed-mode chromatography column can be used to replace two corresponding conventional weak anion exchange and hydrophobic interaction chromatography columns to separate proteins. Based on this mixed-mode chromatography stationary phase, a new off-line two-dimensional liquid chromatography technology using only a single dual-function mixed-mode chromatography column was developed. Nine kinds of tested proteins can be separated completely using the developed method within 2.0 h.

  7. Separation of Uncharged Oligodeoxynucleotide Analogs by Anion-Exchange Chromatography at High pH

    NASA Technical Reports Server (NTRS)

    Schmidt, Jurgen G.; Nielsen, Peter E.; Orgel, Leslie

    1996-01-01

    Ion-exchange chromatography is a well-established method for the analysis and purification of phosphodiester-linked oligonucleotides. If elution is carried out under alkaline conditions, the secondary structure of G- and C-rich oligomers is disrupted. Furthermore, elution times become more sensitive to the G and T content of the oligomer, because G and T are deprotonated at pH 10. In recent work on peptide-nucleic acids (PNAs) we noted that mixtures of PNA oligomers G(sub 4), G(Sub 6), G(sub 8), and G(sub 10) are readily separated by elution at pH 12 on an RPC-5 column. Here we show that this separation method is more generally applicable.

  8. Separation of 'Uncharged' Oligodeoxynucleotide Analogs by Anion-Exchange Chromatography at High pH

    NASA Technical Reports Server (NTRS)

    Schmidt, Jurgen G.; Orgel, Leslie E.; Nielsen, Peter E.

    1996-01-01

    Ion-exchange chromatography is a well-established method for the analysis and purification of phosphodiester-linked oligonucleotides. If elution is carried out under alkaline conditions, the secondary structure of G- and C-rich oligomers is disrupted. Furthermore, elution times become more sensitive to the G and T content of the oligomer, because G and T are deprotonated at pH 10. In recent work on peptide-nucleic acids (PNAs) we noted that mixtures of PNA oligomers G(sub 4), G(sub 6), G(sub 8), and G9(sub 10) are readily separated by elution at pH 12 on an RPC-5 column. Here we show that this separation method is more generally applicable.

  9. High-throughput methods for miniaturization and automation of monoclonal antibody purification processes.

    PubMed

    Treier, Katrin; Hansen, Sigrid; Richter, Carolin; Diederich, Patrick; Hubbuch, Jürgen; Lester, Philip

    2012-01-01

    In the last decade, high-throughput downstream process development techniques have entered the biopharmaceutical industry. As chromatography is the standard downstream purification method, several high-throughput chromatographic methods have been developed and applied including miniaturized chromatographic columns for utilization on liquid handling stations. These columns were used to setup a complete downstream process on a liquid handling station for the first time. In this article, a monoclonal antibody process was established in lab-scale and miniaturized afterwards. The scale-down methodology is presented and discussed. Liquid handling in miniaturized single and multicolumn processes was improved and applicability was demonstrated by volume balances. The challenges of absorption measurement are discussed and strategies were shown to improve volume balances and mass balances in 96-well microtiter plates. The feasibility of miniaturizing a complete downstream process was shown. In the future, analytical bottlenecks should be addressed to gain the full benefit from miniaturized complete process development.

  10. The comparative effects of gamma radiation and in situ alpha particles on five strong-base anion exchange resins

    SciTech Connect

    Marsh, S.F.

    1991-01-01

    The effects of external gamma radiation and in situ alpha particles were measured on a recently available, macroporous, strong-base polyvinylpyridine resin and on four strong-base polystyrene anion exchange resins. Each resin was irradiated in 7 M nitric acid to 1--10 megaGray of gamma radiation from external {sup 60}Co, or to 5--14 megaGray of alpha particles from sorbed {sup 238}Pu. Each irradiated resin was measured for changes in dry weight, wet volume, weak-base and strong-base chloride exchange capacities, and exchange capacities for Pu(4) from nitric acid. Alpha-induced resin damage was significantly less than that caused by an equivalent dose of gamma radiation. The polyvinylpyridine resin offers the greatest resistance to damage from gamma radiation and from alpha particles. 5 refs., 1 figs. 5 tabs.

  11. Novel simple process for tocopherols selective recovery from vegetable oils by adsorption and desorption with an anion-exchange resin.

    PubMed

    Hiromori, Kousuke; Shibasaki-Kitakawa, Naomi; Nakashima, Kazunori; Yonemoto, Toshikuni

    2016-03-01

    A novel and simple low-temperature process was used to recover tocopherols from a deodorizer distillate, which is a by-product of edible oil refining. The process consists of three operations: the esterification of free fatty acids with a cation-exchange resin catalyst, the adsorption of tocopherols onto an anion-exchange resin, and tocopherol desorption from the resin. No degradation of tocopherols occurred during these processes. In the tocopherol-rich fraction, no impurities such as sterols or glycerides were present. These impurities are commonly found in the product of the conventional process. This novel process improves the overall recovery ratio and the mass fraction of the product (75.9% and 51.0wt%) compared with those in the conventional process (50% and 35wt%).

  12. Inhibitors of pendrin anion exchange identified in a small molecule screen increase airway surface liquid volume in cystic fibrosis.

    PubMed

    Haggie, Peter M; Phuan, Puay-Wah; Tan, Joseph-Anthony; Zlock, Lorna; Finkbeiner, Walter E; Verkman, A S

    2016-06-01

    Pendrin (SLC26A4) is a Cl(-)/anion exchanger expressed in the epithelium of inflamed airways where it is thought to facilitate Cl(-) absorption and HCO3 (-) secretion. Studies using pendrin knockout mice and airway epithelial cells from hearing-impaired subjects with pendrin loss of function suggest involvement of pendrin in inflammatory lung diseases, including cystic fibrosis (CF), perhaps by regulation of airway surface liquid (ASL) volume. Here we identified small-molecule pendrin inhibitors and demonstrated their efficacy in increasing ASL volume. A cell-based, functional high-throughput screen of ∼36,000 synthetic small molecules produced 3 chemical classes of inhibitors of human pendrin. After structure-activity studies, tetrahydropyrazolopyridine and pyrazolothiophenesulfonamide compounds reversibly inhibited pendrin-facilitated Cl(-) exchange with SCN(-), I(-), NO3 (-), and HCO3 (-) with drug concentration causing 50% inhibition down to ∼2.5 μM. In well-differentiated primary cultures of human airway epithelial cells from non-CF and CF subjects, treatment with IL-13, which causes inflammation with strong pendrin up-regulation, strongly increased Cl(-)/HCO3 (-) exchange and the increase was blocked by pendrin inhibition. Pendrin inhibition significantly increased ASL depth (by ∼8 μm) in IL-13-treated non-CF and CF cells but not in untreated cells. These studies implicate the involvement of pendrin-facilitated Cl(-)/HCO3 (-) in the regulation of ASL volume and suggest the utility of pendrin inhibitors in inflammatory lung diseases, including CF.-Haggie, P. M., Phuan, P.-W., Tan, J.-A., Zlock, L., Finkbeiner, W. E., Verkman, A. S. Inhibitors of pendrin anion exchange identified in a small molecule screen increase airway surface liquid volume in cystic fibrosis. PMID:26932931

  13. Potential of chiral anion-exchangers operated in various subcritical fluid chromatography modes for resolution of chiral acids.

    PubMed

    Pell, Reinhard; Lindner, Wolfgang

    2012-07-01

    Anion-exchange-type chiral stationary phases (CSPs) derived from quinine or quinidine were applied in subcritical fluid chromatography (SFC) for the direct separation of chiral acidic compounds. Employing subcritical (sc) mobile phase modes (CO₂ + methanol as co-solvent and acids and bases as additives) first the influence of type and amount of acidic and basic additives on separation performance was investigated. Secondly, water was tested as a neutral additive and the influence of temperature variation on enantioselectivity was studied. Thirdly, we could chromatographically confirm that the often verbalized "inherent acidity" of sc CO₂ + methanol is manifested by the in situ formation of methylcarbonic acids in the sc mobile phase and thus functioning as acidic additive. Accordingly the dissociated methylcarbonic acid, acting as a counterion, enables an anion exchange mechanism between the cationic CSP and the corresponding acidic analyte. In the absence of a dissociable acid in the mobile phase such an ion exchange mode would not work following a stoichiometric displacement model. This finding is further corroborated by the use of ammonia in methanol as co-solvent thus generating in situ the ammonium salt of methylcarbonic acid. In summary, we report on ion-exchange mediated chromatographic separations in SFC modes by merely using (i) sc CO₂ and MeOH, (ii) sc CO₂ and ammonia in MeOH, and (iii) sc CO₂ and MeOH plus acids and bases as additives. Comparisons to HPLC mode have been undertaken to evaluate merits and limitations. This mode exhibits high potential for preparative chromatography of chiral acids combining pronounced enantioselectivity with high column loadability and avoiding possibly troublesome mobile phase additives, as the in situ formed methylcarbonic acid disintegrates to CO₂ and methanol upon pressure release.

  14. High-Throughput, Automated Protein A Purification Platform with Multiattribute LC-MS Analysis for Advanced Cell Culture Process Monitoring.

    PubMed

    Dong, Jia; Migliore, Nicole; Mehrman, Steven J; Cunningham, John; Lewis, Michael J; Hu, Ping

    2016-09-01

    The levels of many product related variants observed during the production of monoclonal antibodies are dependent on control of the manufacturing process, especially the cell culture process. However, it is difficult to characterize samples pulled from the bioreactor due to the low levels of product during the early stages of the process and the high levels of interfering reagents. Furthermore, analytical results are often not available for several days, which slows the process development cycle and prevents "real time" adjustments to the manufacturing process. To reduce the delay and enhance our ability to achieve quality targets, we have developed a low-volume, high-throughput, and high-content analytical platform for at-line product quality analysis. This workflow includes an automated, 96-well plate protein A purification step to isolate antibody product from the cell culture fermentation broth, followed by rapid, multiattribute LC-MS analysis. We have demonstrated quantitative correlations between particular process parameters with the levels of glycosylated and glycated species in a series of small scale experiments, but the platform could be used to monitor other attributes and applied across the biopharmaceutical industry. PMID:27487007

  15. Human kidney anion exchanger 1 interacts with adaptor-related protein complex 1 {mu}1A (AP-1 mu1A)

    SciTech Connect

    Sawasdee, Nunghathai; Junking, Mutita; Ngaojanlar, Piengpaga; Sukomon, Nattakan; Ungsupravate, Duangporn; Limjindaporn, Thawornchai; Akkarapatumwong, Varaporn; Noisakran, Sansanee; Yenchitsomanus, Pa-thai

    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

  16. A general halide-to-anion switch for imidazolium-based ionic liquids and oligocationic systems using anion exchange resins (A- form).

    PubMed

    Alcalde, Ermitas; Dinarès, Immaculada; Ibáñez, Anna; Mesquida, Neus

    2011-03-21

    Further studies on the application of an AER (A(-) form) method broadened the anion exchange scope of representative ionic liquids and bis(imidazolium) systems. Depending on the hydrophobicity nature of the targeted imidazolium species and counteranions, different organic solvents were used to swap halides for assorted anions, proceeding in excellent to quantitative yields.

  17. Facile modification of multi-walled carbon nanotubes-polymeric ionic liquids-coated solid-phase microextraction fibers by on-fiber anion exchange.

    PubMed

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2015-05-01

    In situ anion exchange has been proved to be an efficient method for facile modification of polymeric ionic liquids (PILs)-based stationary phases. In this work, an on-fiber anion exchange process was utilized to tune the extraction performance of a multi-walled carbon nanotubes (MWCNTs)-poly(1-vinyl-3-octylimidazolium bromide) (poly(VOIm(+)Br(-)))-coated solid-phase microextraction (SPME) fiber. MWCNTs were first coated onto the stainless steel wire through a layer-by-layer fabrication method and then the PILs were coated onto the MWCNTs physically. Anion of the MWCNTs-poly(VOIm(+)Br(-)) fiber was changed into bis(triflroromethanesulfonyl)imide (NTf2(-)) and 2-naphthalene-sulfonate (NapSO3(-)) by on-fiber anion exchange. Coupled to gas chromatography, the MWCNTs-poly(VOIm(+)Br(-)) fiber showed acceptable extraction efficiency for hydrophilic and hydrogen-bonding-donating alcohols, with limits of detection (LODs) in the range of 0.005-0.05μgmL(-1); after the anion exchange with NTf2(-), the obtained MWCNTs-poly(VOIm(+)NTf2(-)) fiber brought wide linear ranges for hydrophobic n-alkanes with correlation coefficient (R) ranging from 0.994 to 0.997; aromatic property of the fiber was enhanced by aromatic NapSO3(-) anions to get sufficient extraction capacity for phthalate esters and halogenated aromatic hydrocarbons. The MWCNTs-poly(VOIm(+)NapSO3(-)) fiber was finally applied to determine several halogenated aromatic hydrocarbons in groundwater of industrial park.

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

    NASA Astrophysics Data System (ADS)

    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.

  19. A new anion-exchange/hydrophobic monolith as stationary phase for nano liquid chromatography of small organic molecules and inorganic anions.

    PubMed

    Aydoğan, Cemil

    2015-05-01

    In this study, an anion-exchange/hydrophobic polymethacrylate-based stationary phase was prepared for nano-liquid chromatography of small organic molecules and inorganic anions. The stationary phase was synthesized by in situ polymerization of 3-chloro-2-hydroxypropylmethacrylate and ethylene dimethacrylate inside silanized 100 μm i.d. fused silica capillary. The porogen mixture consisted of toluene and dodecanol. The pore size distrubution profiles of the resulting monolith were determined by mercury intrusion porosimetry and the morphology of the prepared monolith was investigated by scanning electron microscope. Good permeability, stability and column efficiency were observed on the monolithic column with nano flow. The produced monolithic column, which contains reactive chloro groups, was then modified by reaction with N,N-dimethyl-N-dodecylamine to obtain an anion-exchange/hydrophobic monolithic stationary phase. The functionalized monolith contained ionizable amine groups and hydrophobic groups that are useful of anion-exchange/hydrophobic mixed-mode chromatography. The final monolithic column performance with respect to anion-exchange and hydrophobic interactions was assesed by the separation of alkylbenzene derivatives, phenolic compounds and inorganic anions, respectively. Theoretical plate numbers up to 23,000 plates/m were successfully achieved in the separation of inorganic anions.

  20. An anion exchange approach to Bi2WO6 hollow microspheres with efficient visible light photocatalytic reduction of CO2 to methanol.

    PubMed

    Cheng, Hefeng; Huang, Baibiao; Liu, Yuanyuan; Wang, Zeyan; Qin, Xiaoyan; Zhang, Xiaoyang; Dai, Ying

    2012-10-01

    An anion exchange strategy is explored to synthesize Bi(2)WO(6) hollow microspheres based on the microscale Kirkendall effect. The as-prepared Bi(2)WO(6) hollow microspheres display high CO(2) adsorption capacity and visible light photocatalytic conversion efficiency of CO(2) into methanol without the aid of any co-catalyst. PMID:22914674

  1. Chloride anion exchange coprocessing for recovery of plutonium from pyrochemical residues and Cs sub 2 PuCl sub 6 filtrate

    SciTech Connect

    Muscatello, A.C.; Killion, M.E.

    1990-12-07

    Continuing studies of plutonium recovery from direct oxide reduction (DOR) and electrorefining (ER) pyrochemical process residues show that chloride anion exchange coprocessing is useful and effective. Coprocessing utilizes DOR residue salt as a reagent to supply the bulk of chloride ion needed for the chloride anion exchange process and to improve ER residue salt solubility. ER residue salt and ER scrapeout can be successfully treated, either alone or together, using coprocessing. In addition, chloride anion exchange at 2.0M acidity results in improved process performance by greatly reducing disproportionation of plutonium(IV), eliminating restrictions on oxidation time compared to operation at 1.0M acidity. Laboratory-scale experiments show that below-discard effluent plutonium losses are obtained. Resin capacity was 30 g Pu/{ell} or greater. Furthermore, it is feasible to perform chloride anion exchange recovery of plutonium from filtrate resulting from precipitation of dicesium hexachloroplutonate (Cs{sub 2}PuCl{sub 6}, an oxidant salt to be used in the molten salt extraction process) and integration of its preparation with recovery of DOR salts. 10 refs., 9 figs., 10 tabs.

  2. Microcalorimetric study of adsorption and disassembling of virus-like particles on anion exchange chromatography media.

    PubMed

    Yu, Mengran; Zhang, Songping; Zhang, Yan; Yang, Yanli; Ma, Guanghui; Su, Zhiguo

    2015-04-01

    Chromatographic purification of virus-like particles (VLPs) is important to the development of modern vaccines. However, disassembly of the VLPs on the solid-liquid interface during chromatography process could be a serious problem. In this study, isothermal titration calorimetric (ITC) measurements, together with chromatography experiments, were performed on the adsorption and disassembling of multi-subunits hepatitis B virus surface antigen virus-like particles (HB-VLPs). Two gigaporous ion-exchange chromatography (IEC) media, DEAE-AP-280 nm and DEAE-POROS, were used. The application of gigaporous media with high ligand density led to significantly increased irreversible disassembling of HB-VLPs and consequently low antigen activity recovery during IEC process. To elucidate the thermodynamic mechanism of the effect of ligand density on the adsorption and conformational change of VLPs, a thermodynamic model was proposed. With this model, one can obtain the intrinsic molar enthalpy changes related to the binding of VLPs and the accompanying conformational change on the liquid-solid interface during its adsorption. This model assumes that, when intact HB-VLPs interact with the IEC media, the total adsorbed proteins contain two states, the intact formation and the disassembled formation; accordingly, the apparent adsorption enthalpy, ΔappH, which can be directly measured from ITC experiments, presents the sum of three terms: (1) the intrinsic molar enthalpy change associated to the binding of intact HB-VLPs (ΔbindHintact), (2) the intrinsic molar enthalpy change associated to the binding of HB-VLPs disassembled formation (ΔbindHdis), and (3) the enthalpy change accompanying the disassembling of HB-VLPs (ΔconfHdis). The intrinsic binding of intact HB-VLPs and the disassembled HB-VLPs to both kinds of gigaporous media (each of which has three different ligand densities), were all observed to be entropically driven as indicated by positive values of

  3. Microcalorimetric study of adsorption and disassembling of virus-like particles on anion exchange chromatography media.

    PubMed

    Yu, Mengran; Zhang, Songping; Zhang, Yan; Yang, Yanli; Ma, Guanghui; Su, Zhiguo

    2015-04-01

    Chromatographic purification of virus-like particles (VLPs) is important to the development of modern vaccines. However, disassembly of the VLPs on the solid-liquid interface during chromatography process could be a serious problem. In this study, isothermal titration calorimetric (ITC) measurements, together with chromatography experiments, were performed on the adsorption and disassembling of multi-subunits hepatitis B virus surface antigen virus-like particles (HB-VLPs). Two gigaporous ion-exchange chromatography (IEC) media, DEAE-AP-280 nm and DEAE-POROS, were used. The application of gigaporous media with high ligand density led to significantly increased irreversible disassembling of HB-VLPs and consequently low antigen activity recovery during IEC process. To elucidate the thermodynamic mechanism of the effect of ligand density on the adsorption and conformational change of VLPs, a thermodynamic model was proposed. With this model, one can obtain the intrinsic molar enthalpy changes related to the binding of VLPs and the accompanying conformational change on the liquid-solid interface during its adsorption. This model assumes that, when intact HB-VLPs interact with the IEC media, the total adsorbed proteins contain two states, the intact formation and the disassembled formation; accordingly, the apparent adsorption enthalpy, ΔappH, which can be directly measured from ITC experiments, presents the sum of three terms: (1) the intrinsic molar enthalpy change associated to the binding of intact HB-VLPs (ΔbindHintact), (2) the intrinsic molar enthalpy change associated to the binding of HB-VLPs disassembled formation (ΔbindHdis), and (3) the enthalpy change accompanying the disassembling of HB-VLPs (ΔconfHdis). The intrinsic binding of intact HB-VLPs and the disassembled HB-VLPs to both kinds of gigaporous media (each of which has three different ligand densities), were all observed to be entropically driven as indicated by positive values of

  4. Effect of Fe2+ Oxidation on the Removal of 238Pu from Neptunium Solution by Anion Exchange

    SciTech Connect

    KYSER, EDWARD

    2004-06-01

    The effect of ferrous sulfamate (FS) oxidation and variation in nitric acid concentration on the removal of {sup 238}Pu contamination from Np by the HB-Line anion exchange flowsheet has been tested. Significant rejection of {sup 238}Pu was observed by washing with a reductive wash solution containing 6.0 to 6.8 M nitric acid (HNO{sub 3}) with as little as 30% of the Fe{sup 2+} from the FS remaining in its reduced form. To achieve the desired 30% removal of {sup 238}Pu from the process, conditions should be controlled to maintain the Fe{sup 2+}/Fe{sup 3+} ratio in the reductive wash to be greater than 60%/40% (or 1.5). Since Fe{sup 2+} oxidation is strongly affected by temperature and nitric acid concentration, these parameters (as well as time after FS addition) need to be controlled to ensure predictable results. A shortened-height column was utilized in these tests to match changes in the plant equipment. Lab experiments scaled to plant batch sizes of 2000 g Np were observed with modest losses for ''up-flow'' washing. The following are recommended conditions for removing {sup 238}Pu from Np solutions by anion exchange in HB-Line: (1) Feed conditions: ''Up-flow'' 6.4-8.0 M HNO{sub 3}, 0.02 M hydrazine (N{sub 2}H{sub 4}), 0.05 M excess FS. (2) Reductive Wash conditions: ''Up-flow'' 6 Bed volumes (BV) of 6.4 M HNO{sub 3}, 0.05 M FS (minimum 0.03M Fe{sup 2+} during wash cycle), 0.05 M hydrazine, less than 1.8 mL/min/cm{sup 2} flowrate. (3) Decontamination Wash conditions: ''Up-flow'' 1-2 BV of 6.4-8.0 M HNO{sub 3}, no FS, no hydrazine, less than 1.8 mL/min/cm{sup 2} flowrate. (4) Elution conditions: ''Down-flow'' 0.17 M HNO{sub 3}, 0.05 M hydrazine, no FS.

  5. Centrifugal LabTube platform for fully automated DNA purification and LAMP amplification based on an integrated, low-cost heating system.

    PubMed

    Hoehl, Melanie M; Weißert, Michael; Dannenberg, Arne; Nesch, Thomas; Paust, Nils; von Stetten, Felix; Zengerle, Roland; Slocum, Alexander H; Steigert, Juergen

    2014-06-01

    This paper introduces a disposable battery-driven heating system for loop-mediated isothermal DNA amplification (LAMP) inside a centrifugally-driven DNA purification platform (LabTube). We demonstrate LabTube-based fully automated DNA purification of as low as 100 cell-equivalents of verotoxin-producing Escherichia coli (VTEC) in water, milk and apple juice in a laboratory centrifuge, followed by integrated and automated LAMP amplification with a reduction of hands-on time from 45 to 1 min. The heating system consists of two parallel SMD thick film resistors and a NTC as heating and temperature sensing elements. They are driven by a 3 V battery and controlled by a microcontroller. The LAMP reagents are stored in the elution chamber and the amplification starts immediately after the eluate is purged into the chamber. The LabTube, including a microcontroller-based heating system, demonstrates contamination-free and automated sample-to-answer nucleic acid testing within a laboratory centrifuge. The heating system can be easily parallelized within one LabTube and it is deployable for a variety of heating and electrical applications.

  6. A versatile-deployable bacterial detection system for food and environmental safety based on LabTube-automated DNA purification, LabReader-integrated amplification, readout and analysis.

    PubMed

    Hoehl, Melanie M; Bocholt, Eva Schulte; Kloke, Arne; Paust, Nils; von Stetten, Felix; Zengerle, Roland; Steigert, Juergen; Slocum, Alexander H

    2014-06-01

    Contamination of foods is a public health hazard that episodically causes thousands of deaths and sickens millions worldwide. To ensure food safety and quality, rapid, low-cost and easy-to-use detection methods are desirable. Here, the LabSystem is introduced for integrated, automated DNA purification, amplification and detection. It consists of a disposable, centrifugally driven DNA purification platform (LabTube) and a low-cost UV/vis-reader (LabReader). For demonstration of the LabSystem in the context of food safety, purification of Escherichia coli (non-pathogenic E. coli and pathogenic verotoxin-producing E. coli (VTEC)) in water and milk and the product-spoiler Alicyclobacillus acidoterrestris (A. acidoterrestris) in apple juice was integrated and optimized in the LabTube. Inside the LabReader, the purified DNA was amplified, readout and analyzed using both qualitative isothermal loop-mediated DNA amplification (LAMP) and quantitative real-time PCR. For the LAMP-LabSystem, the combined detection limits for purification and amplification of externally lysed VTEC and A. acidoterrestris are 10(2)-10(3) cell-equivalents. In the PCR-LabSystem for E. coli cells, the quantification limit is 10(2) cell-equivalents including LabTube-integrated lysis. The demonstrated LabSystem only requires a laboratory centrifuge (to operate the disposable, fully closed LabTube) and a low-cost LabReader for DNA amplification, readout and analysis. Compared with commercial DNA amplification devices, the LabReader improves sensitivity and specificity by the simultaneous readout of four wavelengths and the continuous readout during temperature cycling. The use of a detachable eluate tube as an interface affords semi-automation of the LabSystem, which does not require specialized training. It reduces the hands-on time from about 50 to 3 min with only two handling steps: sample input and transfer of the detachable detection tube.

  7. Optimization of RNA Purification and Analysis for Automated, Pre-Symptomatic Disease Diagnostics

    SciTech Connect

    Vaidya, A; Nasarabadi, S; Milanovich, F

    2005-06-28

    When diagnosing disease, time is often a more formidable enemy than the pathogen itself. Current detection methods rely primarily on post-symptomatic protein production (i.e. antibodies), which does not occur in noticeable levels until several weeks after infection. As such, a major goal among researchers today is to expedite pre-symptomatic disease recognition and treatment. Since most pathogens are known to leave a unique signature on the genetic expression of the host, one potential diagnostic tool is host mRNA. In my experiments, I examined several methods of isolating RNA and reading its genetic sequence. I first used two types of reverse transcriptase polymerase chain reactions (using commercial RNA) and examined the resultant complementary DNA through gel electrophoresis. I then proceeded to isolate and purify whole RNA from actual human monocytes and THP-1 cells using several published methods, and examined gene expression on the RNA itself. I compared the two RT-PCR methods and concluded that a double step RT-PCR is superior to the single step method. I also compared the various techniques of RNA isolation by examining the yield and purity of the resultant RNA. Finally, I studied the level of cellular IL-8 and IL-1 gene expression, two genes involved in the human immune response, which can serve as a baseline for future genetic comparison with LPS-exposed cells. Based on the results, I have determined which conditions and procedures are optimal for RNA isolation, RT-PCR, and RNA yield assessment. The overall goal of my research is to develop a flow-through system of RNA analysis, whereby blood samples can be collected and analyzed for disease prior to the onset of symptoms. The Pathomics group hopes to automate this process by removing the human labor factor, thereby decreasing the procedure's cost and increasing its availability to the general population. Eventually, our aim is to have an autonomous diagnostic system based on RNA analysis that would

  8. Anion-exchange reactions on a robust phosphonium photopolymer for the controlled deposition of ionic gold nanoclusters.

    PubMed

    Guterman, Ryan; Hesari, Mahdi; Ragogna, Paul J; Workentin, Mark S

    2013-05-28

    UV curing (photopolymerization) is ubiquitous in many facets of industry ranging from the application of paints, pigments, and barrier coatings all the way to fiber optic cable production. To date no reports have focused on polymerizable phosphonium salts under UV irradiation, and despite this dearth of examples, they potentially offer numerous substantial advantages to traditional UV formulation components. We have generated a highly novel coating based on UV-curable trialkylacryloylphosphonium salts that allow for the fast (seconds) and straightforward preparation of ion-exchange surfaces amenable to a roll-to-roll process. We have quantified the surface charges and exploited their accessibility by employing these surfaces in an anion exchange experiment by which [Au25L18](-) (L = SCH2CH2Ph) nanocrystals can be assembled into the solid state. This unprecedented application of such surfaces offers a paradigm shift in the emerging chemistry of Au25 research where the nanocrystals remain single and intact and where the integrity of the cluster and its solution photophysical properties are resilient in the solid state. The specific loading of [Au25L18](-) on the substrates has been determined and the completely reversible loading and unloading of intact nanocrystals to and from the surface has been established. In the solid state, the assembly has an incredible mechanical resiliency, where the surface remains undamaged even when subjected to repeated Scotch tests.

  9. Removal of radioactive caesium from low level radioactive waste (LLW) streams using cobalt ferrocyanide impregnated organic anion exchanger.

    PubMed

    Valsala, T P; Roy, S C; J G Shah; Gabriel, J; Raj, Kanwar; Venugopal, V

    2009-07-30

    The volumes of low level waste (LLW) generated during the operation of nuclear reactor are very high and require a concentration step before suitable matrix fixation. The volume reduction (concentration) is achieved either by co-precipitating technique or by the use of highly selective sorbents and ion exchange materials. The present study details the preparation of cobalt ferrocyanide impregnated into anion exchange resin and its evaluation with respect to removal of Cs in LLW streams both in column mode and batch mode operations. The Kd values of the prepared exchanger materials were found to be very good in actual reactor LLW solutions also. It was observed that the exchanger performed very well in the pH range of 3-9. A batch size of 6 g l(-1) of the exchanger was enough to give satisfactory decontamination for Cs in actual reactor LLW streams. The lab scale and pilot plant scale performance of the exchanger material in both batch mode and column mode operations was very good.

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

    PubMed

    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.

  11. Chitosan Derivatives as Important Biorefinery Intermediates. Quaternary Tetraalkylammonium Chitosan Derivatives Utilized in Anion Exchange Chromatography for Perchlorate Removal

    PubMed Central

    Sayed, Shakeela; Jardine, Anwar

    2015-01-01

    There has recently been great interest in the valorization of biomass waste in the context of the biorefinery. The biopolymer chitosan, derived from chitin, is present in large quantities of crustacean waste. This biomass can be converted into value-added products with applications in energy, fuel, chemicals and materials manufacturing. The many reported applications of this polymer can be attributed to its unique properties, such as biocompatibility, chemical versatility, biodegradability and low toxicity. Cost effective water filters which decontaminate water by removal of specific impurities and microbes are in great demand. To address this need, the development of ion exchange resins using environmentally friendly, renewable materials such as biopolymers as solid supports was evaluated. The identification and remediation of perchlorate contaminated water using an easy, inexpensive method has come under the spotlight recently. Similarly, the use of a low cost perchlorate selective solid phase extraction (SPE) cartridge that can be rapidly employed in the field is desirable. Chitosan based SPE coupled with colorimetric analytical methods showed promise as a renewable anion exchange support for perchlorate analysis or removal. The polymers displayed perchlorate retention comparable to the commercial standard whereby the quaternized iron loaded polymer TMC-Fe(III) displayed the best activity. PMID:25915024

  12. A semi-interpenetrating network approach for dimensionally stabilizing highly-charged anion exchange membranes for alkaline fuel cells.

    PubMed

    He, Steve S; Strickler, Alaina L; Frank, Curtis W

    2015-04-24

    There is a delicate balance between ion exchange capacity (IEC), conductivity, and dimensional stability in anion exchange membranes as higher charge content can lead to increased water uptake, causing excessive swelling and charge dilution. Using highly-charged benzyltrimethylammonium polysulfone (IEC=2.99 mEq g(-1) ) as a benchmark (which ruptured in water even at room temperature), we report the ability to dramatically decrease water uptake using a semi-interpenetrating network wherein we reinforced the linear polyelectrolyte with a crosslinked poly(styrene-co-divinylbenzene) network. These membranes show enhanced dimensional stability as a result of lower water uptake (75 % vs. 301 % at 25 °C) while maintaining excellent hydroxide conductivity (up to 50 mS cm(-1) at 25 °C). These improvements produced an enhanced alkaline fuel cell capable of generating 236 mW cm(-2) peak power density at 80 °C. This method is easily adaptable and can be a viable strategy for stabilizing existing systems.

  13. Mitigating arsenic crisis in the developing world: role of robust, reusable and selective hybrid anion exchanger (HAIX).

    PubMed

    German, Michael; Seingheng, Hul; SenGupta, Arup K

    2014-08-01

    In trying to address the public health crisis from the lack of potable water, millions of tube wells have been installed across the world. From these tube wells, natural groundwater contamination from arsenic regularly puts at risk the health of over 100 million people in South and Southeast Asia. Although there have been many research projects, awards and publications, appropriate treatment technology has not been matched to ground level realities and water solutions have not scaled to reach millions of people. For thousands of people from Nepal to India to Cambodia, hybrid anion exchange (HAIX) resins have provided arsenic-safe water for up to nine years. Synthesis of HAIX resins has been commercialized and they are now available globally. Robust, reusable and arsenic-selective, HAIX has been in operation in rural communities over numerous cycles of exhaustion-regeneration. All necessary testing and system maintenance is organized by community-level water staff. Removed arsenic is safely stored in a scientifically and environmentally appropriate manner to prevent future hazards to animals or people. Recent installations have shown the profitability of HAIX-based arsenic treatment, with capital payback periods of only two years in ideal locations. With an appropriate implementation model, HAIX-based treatment can rapidly scale and provide arsenic-safe water to at-risk populations.

  14. Multivalent sialylation of β-thio-glycoclusters by Trypanosoma cruzi trans sialidase and analysis by high performance anion exchange chromatography.

    PubMed

    Agustí, Rosalía; Cano, María Emilia; Cagnoni, Alejandro J; Kovensky, José; de Lederkremer, Rosa M; Uhrig, María Laura

    2016-10-01

    The synthesis of multivalent sialylated glycoclusters is herein addressed by a chemoenzymatic approach using the trans-sialidase of Trypanosoma cruzi (TcTS). Multivalent β-thio-galactopyranosides and β-thio-lactosides were used as acceptor substrates and 3'-sialyllactose as the sialic acid donor. High performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) was shown to be an excellent technique for the analysis of the reaction products. Different eluting conditions were optimized to allow the simultaneous resolution of the sialylated species, as well as their neutral precursors. The TcTS efficiently transferred sialyl residues to di, tri, tetra and octa β-thiogalactosides. In the case of an octavalent thiolactoside, up to six polysialylated compounds could be resolved. Preparative sialylation reactions were performed using the tetravalent and octavalent acceptor substrates. The main sialylated derivatives could be unequivocally assigned by MALDI mass spectrometry. Inhibition of the transfer to the natural substrate, N-acetyllactosamine, was also studied. The octalactoside caused 82 % inhibition of sialic acid transfer when we used equimolar concentrations of donor, acceptor and inhibitor.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

  17. Determination of saccharides in atmospheric aerosol using anion-exchange high-performance liquid chromatography and pulsed-amperometric detection.

    PubMed

    Caseiro, Alexandre; Marr, Iain L; Claeys, Magda; Kasper-Giebl, Anne; Puxbaum, Hans; Pio, Casimiro A

    2007-11-01

    An improved method is described for the quantification of primary sugars, sugar alcohols and anhydrosugars in atmospheric aerosols, making use of separation by high-performance anion-exchange chromatography (HPAEC) with pulsed amperometric detection (PAD). Quartz fibre filters from high-volume samplers were extracted with water and the extract injected directly. Repeatability is typically 4% RSD, for e.g. levoglucosan at 50 ng m(-3) in air, better for winter levels around 700 ng m(-3). Limits of detection for individual sugars are in the range 0.02-0.05 microg mL(-1) in solution, corresponding to 2-5 ng m(-3) from a 20 m(3) air sample. The overlap of arabitol and levogluocosan is overcome by using a Dionex PA-1 column, with appropriate control of eluent composition, and peak deconvolution software, allowing quantification of both sugars in difficult summer samples containing low-levels of levoglucosan. Analysis of a set of ambient aerosol samples by both GC-flame ionization detection and HPAEC-PAD shows good agreement. The new method has the advantage of requiring no sample pretreatment or derivatization and is thus well suited to handling large numbers of samples.

  18. Characterization of At- species in simple and biological media by high performance anion exchange chromatography coupled to gamma detector.

    PubMed

    Sabatié-Gogova, A; Champion, J; Huclier, S; Michel, N; Pottier, F; Galland, N; Asfari, Z; Chérel, M; Montavon, G

    2012-04-01

    Astatine is a rare radioelement belonging to the halogen group. Considering the trace amounts of astatine produced in cyclotrons, its chemistry cannot be evaluated by spectroscopic tools. Analytical tools, provided that they are coupled with a radioactive detection system, may be an alternative way to study its chemistry. In this research work, high performance anion exchange chromatography (HPAEC) coupled to a gamma detector (γ) was used to evaluate astatine species under reducing conditions. Also, to strengthen the reliability of the experiments, a quantitative analysis using a reactive transport model has been done. The results confirm the existence of one species bearing one negative charge in the pH range 2-7.5. With respect to the other halogens, its behavior indicates the existence of negative ion, astatide At(-). The methodology was successfully applied to the speciation of the astatine in human serum. Under fixed experimental conditions (pH 7.4-7.5 and redox potential of 250 mV) astatine exists mainly as astatide At(-) and does not interact with the major serum components. Also, the method might be useful for the in vitro stability assessment of (211)At-labeled molecules potentially applicable in nuclear medicine. PMID:22405318

  19. Highly stable pyridinium-functionalized cross-linked anion exchange membranes for all vanadium redox flow batteries

    NASA Astrophysics Data System (ADS)

    Zeng, L.; Zhao, T. S.; Wei, L.; Zeng, Y. K.; Zhang, Z. H.

    2016-11-01

    It has recently been demonstrated that the use of anion exchange membranes (AEMs) in vanadium redox flow batteries (VRFBs) can reduce the migration of vanadium ions through the membrane due to the Donnan exclusion effect among the positively charged functional groups and vanadium ions. However, AEMs are plagued by low chemical stability in harsh chemical environments. Here we propose and fabricate a pyridinium-functionalized cross-linked AEM for VRFBs. The pyridinium-functionalized bromomethylated poly (2,6-dimethyl-1,4-phenylene oxide) exhibits a superior chemical stability as a result of the strengthened internal cross-linking networks and the chemical inertness of the polymer backbone. Therefore, the membrane exhibits littler decay in a harsh environment for 20 days during the course of an ex situ immersion test. A cycling test also demonstrates that the VRFB assembled with the membrane enable to retain 80% of the initial discharge capacity over 537 cycles with a capacity decay rate of 0.037% cycle-1. Meanwhile, the membrane also shows a low vanadium permeability and a reasonably high conductivity in supporting electrolytes. Hence, all the measurements and performance tests reported in this work suggest that the membrane is a promising AEM for redox flow batteries to achieve excellent cycling stability and superior cell performance.

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

    PubMed

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

    2013-01-14

    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 1L, 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. PMID:23265737

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

    PubMed

    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.

  2. Anion-exchange resin-based desulfurization process. Quarterly technical progress report, April 1, 1993--June 30, 1993

    SciTech Connect

    Sheth, A.C.; Dharmapurikar, R.

    1993-09-01

    Under the current grant (No. DE-FG22-90PC90309), the University of Tennessee Space Institute (UTSI) will perform the bench scale evaluation and further development of the anion-exchange resin-based desulfurization concept to desulfurize alkali metal sulfates. The developmental program proposed under this DOE grant includes screening of commercially available resins to select three candidate resins for further study. These three resins will undergo a series of experiments designed to test the resins` performance under different process conditions (including the use of spent MHD seed material). The best of these resins will be used in optimizing the regeneration step and in testing the effects of performance enhancers. During this reporting period, April 1, 1993 to June 30, 1993, the procedure to evaluate the cycle efficiency of candidate resins in the fixed-bed mode was slightly modified to ensure complete regeneration of the exhausted resin. Using this revised procedure, ten consecutive cycles for all the three resins have been completed and the results are being analyzed.

  3. Effect of dissolved organic matter on nitrate-nitrogen removal by anion exchange resin and kinetics studies.

    PubMed

    Song, Haiou; Yao, Zhijian; Wang, Mengqiao; Wang, Jinnan; Zhu, Zhaolian; Li, Aimin

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. Characterization of At- species in simple and biological media by high performance anion exchange chromatography coupled to gamma detector.

    PubMed

    Sabatié-Gogova, A; Champion, J; Huclier, S; Michel, N; Pottier, F; Galland, N; Asfari, Z; Chérel, M; Montavon, G

    2012-04-01

    Astatine is a rare radioelement belonging to the halogen group. Considering the trace amounts of astatine produced in cyclotrons, its chemistry cannot be evaluated by spectroscopic tools. Analytical tools, provided that they are coupled with a radioactive detection system, may be an alternative way to study its chemistry. In this research work, high performance anion exchange chromatography (HPAEC) coupled to a gamma detector (γ) was used to evaluate astatine species under reducing conditions. Also, to strengthen the reliability of the experiments, a quantitative analysis using a reactive transport model has been done. The results confirm the existence of one species bearing one negative charge in the pH range 2-7.5. With respect to the other halogens, its behavior indicates the existence of negative ion, astatide At(-). The methodology was successfully applied to the speciation of the astatine in human serum. Under fixed experimental conditions (pH 7.4-7.5 and redox potential of 250 mV) astatine exists mainly as astatide At(-) and does not interact with the major serum components. Also, the method might be useful for the in vitro stability assessment of (211)At-labeled molecules potentially applicable in nuclear medicine.

  7. Assemblies of protective anion exchange membrane on air electrode for its efficient operation in aqueous alkaline electrolyte

    NASA Astrophysics Data System (ADS)

    Bertolotti, Bruno; Chikh, Linda; Vancaeyzeele, Cédric; Alfonsi, Séverine; Fichet, Odile

    2015-01-01

    Aqueous alkaline metal-air batteries represent promising energy storage devices when supplied with atmospheric air. However, under this condition, the air electrode shows a very short life time (i.e. 50 h of operation in 5 M LiOH at -10 mA cm-2), mainly due to the precipitation of carbonates inside the electrode porosity. The air electrode can then be protected by an anion exchange membrane on the electrolyte side. In this paper, we demonstrate that the efficiency of this protective membrane depends on the assembly method on the electrode. When a modified poly(epichlorohydrin) (PECH) network is synthesized directly on the electrode, the polymer seeps inside the electrode porosity, and a suitable interface inducing negligible additional polarization in comparison with classical pressure-assembled membranes is obtained. This protected electrode shows improved stability of up to 160 h of operation in 5 M LiOH. This performance is improved to 350 h by adjusting the conductivity and the ionic exchange capacity. Finally, the interest of interpenetrating polymer network (IPN) architecture compared to a single network is confirmed. Indeed, an electrode protected with a PECH/poly(2-hydroxyethyl methacrylate) (PHEMA) IPN is stable for 650 h in 5 M LiOH. In addition, degradation process becomes reversible since the assembly can be regenerated, which is not possible for the bare electrode.

  8. Anion Exchange HPLC Isolation of High-Density Lipoprotein (HDL) and On-Line Estimation of Proinflammatory HDL

    PubMed Central

    Ji, Xiang; Xu, Hao; Zhang, Hao; Hillery, Cheryl A.; Gao, Hai-qing; Pritchard, Kirkwood A.

    2014-01-01

    Proinflammatory high-density lipoprotein (p-HDL) is a biomarker of cardiovascular disease. Sickle cell disease (SCD) is characterized by chronic states of oxidative stress that many consider to play a role in forming p-HDL. To measure p-HDL, apolipoprotein (apo) B containing lipoproteins are precipitated. Supernatant HDL is incubated with an oxidant/LDL or an oxidant alone and rates of HDL oxidation monitored with dichlorofluorescein (DCFH). Although apoB precipitation is convenient for isolating HDL, the resulting supernatant matrix likely influences HDL oxidation. To determine effects of supernatants on p-HDL measurements we purified HDL from plasma from SCD subjects by anion exchange (AE) chromatography, determined its rate of oxidation relative to supernatant HDL. SCD decreased total cholesterol but not triglycerides or HDL and increased cell-free (cf) hemoglobin (Hb) and xanthine oxidase (XO). HDL isolated by AE-HPLC had lower p-HDL levels than HDL in supernatants after apoB precipitation. XO+xanthine (X) and cf Hb accelerated purified HDL oxidation. Although the plate and AE-HPLC assays both showed p-HDL directly correlated with cf-Hb in SCD plasma, the plate assay yielded p-HDL data that was influenced more by cf-Hb than AE-HPLC generated p-HDL data. The AE-HPLC p-HDL assay reduces the influence of the supernatants and shows that SCD increases p-HDL. PMID:24609013

  9. Characterization of pore structure of a strong anion-exchange membrane adsorbent under different buffer and salt concentration conditions.

    PubMed

    Tatárová, Ivana; Fáber, René; Denoyel, Renaud; Polakovic, Milan

    2009-02-01

    The quantitative characterization of pore structure of Sartobind Q, a strongly basic membrane anion exchanger that is formed by cross-linked cellulose support and a hydrogel layer on its pore surface, was made combining the results obtained by several experimental techniques: liquid impregnation, batch size-exclusion, inverse size-exclusion chromatography, and permeability. Mercury intrusion and nitrogen sorption porosimetry were carried out for a dry cellulose support membrane in order to get additional information for building a model of the bimodal pore structure. The model incorporated the distribution of the total pore volume between transport and gel-layer pores and the partitioning of solutes of different molecular weights was expressed through the cylindrical pore model for the transport pores and random plane model for the gel layer. The effect of composition of liquid phase on the pore structure was investigated in redistilled water, phosphate and Tris-HCl buffers containing up to 1M NaCl. Evident differences in the bimodal pore structure were observed here when both the specific volume and size of the hydrogel layer pores significantly decreased with the ionic strength of liquid phase. PMID:19117574

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

    NASA Astrophysics Data System (ADS)

    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.

  11. 1,2,3-Triazolium-Based Poly(2,6-Dimethyl Phenylene Oxide) Copolymers as Anion Exchange Membranes.

    PubMed

    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

  12. A semi-interpenetrating network approach for dimensionally stabilizing highly-charged anion exchange membranes for alkaline fuel cells.

    PubMed

    He, Steve S; Strickler, Alaina L; Frank, Curtis W

    2015-04-24

    There is a delicate balance between ion exchange capacity (IEC), conductivity, and dimensional stability in anion exchange membranes as higher charge content can lead to increased water uptake, causing excessive swelling and charge dilution. Using highly-charged benzyltrimethylammonium polysulfone (IEC=2.99 mEq g(-1) ) as a benchmark (which ruptured in water even at room temperature), we report the ability to dramatically decrease water uptake using a semi-interpenetrating network wherein we reinforced the linear polyelectrolyte with a crosslinked poly(styrene-co-divinylbenzene) network. These membranes show enhanced dimensional stability as a result of lower water uptake (75 % vs. 301 % at 25 °C) while maintaining excellent hydroxide conductivity (up to 50 mS cm(-1) at 25 °C). These improvements produced an enhanced alkaline fuel cell capable of generating 236 mW cm(-2) peak power density at 80 °C. This method is easily adaptable and can be a viable strategy for stabilizing existing systems. PMID:25820199

  13. New ammunition for the proteomic reactor: strong anion exchange beads and multiple enzymes enhance protein identification and sequence coverage.

    PubMed

    Zhou, Hu; Hou, Weimin; Lambert, Jean-Philippe; Figeys, Daniel

    2010-08-01

    The enrichment and processing of proteomic samples prior to multi-dimensional chromatography remain a challenge in 'gel-free' proteomics. We previously reported the development of a microfluidic device called the "proteomic reactor" that relied on enriching proteins by using strong cation exchange (SCX) followed by trypsin digestion in an interstitial volume as little as 50 nL. Here, we report a novel proteomic reactor that is based on polymeric strong anion exchange (SAX) material to analyse proteomic samples. We also compare the performance of the SAX proteomic reactor to our previously reported SCX proteomic reactor for analysing complex yeast proteomes. Our results indicate that the SAX protein reactor preferentially identifies more acidic peptides and proteins compared to the SCX reactor. We show that the SAX and SCX reactors are complementary and that their combination increases the number of unique peptides and proteins identified by 50%. Furthermore, we show that the number of protein identified can be increased further by up to 40% using different proteolytic enzymes on the proteomic reactor.

  14. Bioregeneration of perchlorate-laden gel-type anion-exchange resin in a fluidized bed reactor.

    PubMed

    Venkatesan, Arjun K; Sharbatmaleki, Mohamadali; Batista, Jacimaria R

    2010-05-15

    Selective ion-exchange resins are very effective to remove perchlorate from contaminated waters. However, these resins are currently incinerated after one time use, making the ion-exchange process incomplete and unsustainable for perchlorate removal. Resin bioregeneration is a new concept that combines ion-exchange with biological reduction by directly contacting perchlorate-laden resins with a perchlorate-reducing bacterial culture. In this research, feasibility of the bioregeneration of perchlorate-laden gel-type anion-exchange resin was investigated. Bench-scale bioregeneration experiments, using a fluidized bed reactor and a bioreactor, were performed to evaluate the feasibility of the process and to gain insight into potential mechanisms that control the process. The results of the bioregeneration tests suggested that the initial phase of the bioregeneration process might be controlled by kinetics, while the later phase seems to be controlled by diffusion. Feasibility study showed that direct bioregeneration of gel-type resin was effective in a fluidized-bed reactor, and that the resin could be defouled, reused, and repeatedly regenerated using the method applied in this research.

  15. Rapid concentration of bacteria using submicron magnetic anion exchangers for improving PCR-based multiplex pathogen detection.

    PubMed

    Yang, Kun; Jenkins, Daniel M; Su, Wei Wen

    2011-07-01

    Rapid concentration of bacterial targets from dilute solutions to improve subsequent PCR detection is investigated in this study. Submicron (average size 500nm) superparamagnetic anion-exchangers (SiMAG-DEAE) were used successfully to concentrate target bacteria from very dilute solutions. A mass-balance model predicted that for Escherichia coli, the extent of cell concentrating increases almost linearly with increasing sample/SiMAG volume ratio up to about 2000, accompanied by only a slight decrease in the capture efficiency (<10%). Our experimental data generally support this analysis in that the SiMAG beads concentrated bacterial targets by two to three orders of magnitude using a sample/bead volume ratio of about 1000, and lowered the PCR detection limit to a level of 10(2)CFU/mL, from 10(4) to 10(5)CFU/mL without concentrating. Several target bacteria can be concentrated concurrently and detected via multiplex PCR, as illustrated using E. coli and Agrobacterium tumefaciens as model bacteria. Finally, concentration and detection of bacteria in fresh produce samples were demonstrated. The integration of submicron magnetic ion exchangers and PCR detection provides an appealing alternative to immunomagnetic separation/PCR in improving pathogen detection.

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

    NASA Astrophysics Data System (ADS)

    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.

  17. Dissolved organic matter removal using magnetic anion exchange resin treatment on biological effluent of textile dyeing wastewater.

    PubMed

    Fan, Jun; Li, Haibo; Shuang, Chendong; Li, Wentao; Li, Aimin

    2014-08-01

    This study investigated the removal of dissolved organic matter (DOM) from real dyeing bio-treatment effluents (DBEs) with the use of a novel magnetic anion exchange resin (NDMP). DOMs in two typical DBEs were fractionized using DAX-8/XAD-4 resin and ultrafiltration membranes. The hydrophilic fractions and the low molecular weight (MW) (<3kDa) DOM fractions constituted a major portion (>50%) of DOMs for the two effluents. The hydrophilic and low MW fractions of both effluents were the greatest contributors of specific UV254 absorbance (SUVA254), and the SUVA254 of DOM fractions decreased with hydrophobicity and MW. Two DBEs exhibited acute and chronic biotoxicities. Both acute and chronic toxicities of DOM fractions increased linearly with the increase of SUVA254 value. Kinetics of dissolved organic carbon (DOC) removal via NDMP treatment was performed by comparing it with that of particle active carbon (PAC). Results indicated that the removal of DOC from DBEs via NDMP was 60%, whereas DOC removals by PAC were lower than 15%. Acidic organics could be significantly removed with the use of NDMP. DOM with large MW in DBE could be removed significantly by using the same means. Removal efficiency of NDMP for DOM decreased with the decrease of MW. Compared with PAC, NDMP could significantly reduce the acute and chronic bio-toxicities of DBEs. NaCl/NaOH mixture regenerants, with selected concentrations of 10% NaCl (m/m)/1% NaOH (m/m), could improve desorption efficiency. PMID:25108712

  18. Mitigating arsenic crisis in the developing world: role of robust, reusable and selective hybrid anion exchanger (HAIX).

    PubMed

    German, Michael; Seingheng, Hul; SenGupta, Arup K

    2014-08-01

    In trying to address the public health crisis from the lack of potable water, millions of tube wells have been installed across the world. From these tube wells, natural groundwater contamination from arsenic regularly puts at risk the health of over 100 million people in South and Southeast Asia. Although there have been many research projects, awards and publications, appropriate treatment technology has not been matched to ground level realities and water solutions have not scaled to reach millions of people. For thousands of people from Nepal to India to Cambodia, hybrid anion exchange (HAIX) resins have provided arsenic-safe water for up to nine years. Synthesis of HAIX resins has been commercialized and they are now available globally. Robust, reusable and arsenic-selective, HAIX has been in operation in rural communities over numerous cycles of exhaustion-regeneration. All necessary testing and system maintenance is organized by community-level water staff. Removed arsenic is safely stored in a scientifically and environmentally appropriate manner to prevent future hazards to animals or people. Recent installations have shown the profitability of HAIX-based arsenic treatment, with capital payback periods of only two years in ideal locations. With an appropriate implementation model, HAIX-based treatment can rapidly scale and provide arsenic-safe water to at-risk populations. PMID:24321388

  19. Carbon supported Ag nanoparticles as high performance cathode catalyst for H2/O2 anion exchange membrane fuel cell

    PubMed Central

    Xin, Le; Zhang, Zhiyong; Wang, Zhichao; Qi, Ji; Li, Wenzhen

    2013-01-01

    A solution phase-based nanocapsule method was successfully developed to synthesize non-platinum metal catalyst—carbon supported Ag nanoparticles (Ag/C). XRD patterns and TEM image show Ag nanoparticles with a small average size (5.4 nm) and narrow size distribution (2–9 nm) are uniformly dispersed on the carbon black Vulcan XC-72 support. The intrinsic activity and pathway of oxygen reduction reaction (ORR) on the Ag/C and commercial Pt/C were investigated using rotating ring disk electrode (RRDE) tests at room temperature. The results confirmed that the 4-electron pathway of ORR proceeds on small Ag nanoparticles, and showed comparable ORR activities on the self-prepared Ag/C and a commercial Pt/C. A single H2-O2 anion exchange membrane fuel cell (AEMFC) with the Ag/C cathode catalyst exhibited an open circuit potential of 0.98 V and a peak power density of 190 mW/cm2 at 80°C. PMID:24790944

  20. Enhancement of molecular shape selectivity by in situ anion-exchange in poly(octadecylimidazolium) silica column.

    PubMed

    Qiu, Hongdeng; Mallik, Abul K; Takafuji, Makoto; Liu, Xia; Jiang, Shengxiang; Ihara, Hirotaka

    2012-04-01

    This paper demonstrates that in situ anion exchange could be successfully applied as a new method for modifying the surface properties of a poly(octadecylimidazolium)-grafted silica stationary phase to tune and enhance selectivity. Specifically, the original stationary phase was prepared by surface-initiated radical chain-transfer polymerization of 1-vinyl-3-octadecylimidazolium bromide as an ionic liquid monomer; the Br(-) counter anion was then exchanged for methyl orange via an in-column process. As evaluated via the separation of constrained isomers of polycyclic aromatic hydrocarbons (PAHs), the in situ exchange enhanced the molecular shape-selectivity performance. Enhanced selectivity was also confirmed using Standard Reference Material (SRM) 869b (column selectivity test mixture) and SRM 1647e (16 priority pollutant PAHs). The reproducibility of new column was tested via the separation of pyrene, triphenylene, benzo[a]anthracene and chrysene with methanol as eluent at 10 °C and the RSD values (n=12) of the retention factors of them are within 0.27-0.77%. PMID:22099220

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

    PubMed

    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 %.

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

    PubMed

    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

  3. Anion-exchange resin-based desulfurization process. Annual technical progress report, October 1, 1991--September 30, 1992

    SciTech Connect

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

    1992-12-31

    Under the current grant, the University of Tennessee Space Institute (UTSI) will carry out the bench scale evaluation and further development of the anion-exchange resin-based desulfurization concept to desulfurize alkali metal sulfates. This concept has been developed and patented by UTSI under US Patent No. 4,917,874. The developmental program proposed under this DOE grant includes screening of commercially available resins to select three candidate resins for further study. These three resins will undergo a series of experiments designed to test the resins` performance under different process conditions (including the use of spent MHD seed material). The best of these resins will be used in optimizing the regeneration step and in testing the effects of performance enhancers. The process schematic developed from the results will be used to estimate the related economics. During this reporting period, October 1, 1991 to September 30, 1992, analysis of batch mode screening experiments was completed to select three candidate resins for process variables study in the fixed-bed set-up. This setup was modified and the experiments were carded out to evaluate effects of major process variables. The analysis of fixed-bed experiments is going on and we have also started simple batch mode experiments to identify desirable conditions for resin regeneration step. We have also started simple process engineering type calculations to determine the trade-off between the solution concentration and the resulting evaporation/concentration load.

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

    PubMed

    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

  5. Radioanalytical determination of 239+240Pu and 241Am in bioassay samples by anion exchange and extraction chromatography: Preliminary considerations about the two methods

    NASA Astrophysics Data System (ADS)

    Ridone, S.; Arginelli, D.; Berton, G.; Bortoluzzi, S.; Canuto, G.; Montalto, M.; Nocente, M.; Vegro, M.

    2006-01-01

    During the radiation protection surveillance of exposed workers samples of urine and faeces were collected. Anion exchange chromatography was used for the separation of Pu. We investigated a technique to purify and separate Pu and Am isotopes using extraction chromatography with TRU resin. We tested different procedures to dissolve organic matter and eliminate interferences for chromatographic elution. At the end of the proces we have succeeded in electroplating the two radionuclides separately. We have also studied extraction chromatography with UTEVA resin to purify Pu isotopes and separate it from natural uranium radioisotopes, present in some biological samples. We validated a method for the determination of Pu in biological samples and a rather constant chemical yield and resolved peaks were obtained. The preliminary studies on TRU resin have indicated that it is possible to combine extraction and anion-exchange chromatography for analysing separately Pu and Am isotopes from the same sample aliquote.

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

    NASA Technical Reports Server (NTRS)

    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.

  7. Kinetics and mechanism of exogenous anion exchange in FeFbpA-NTA: significance of periplasmic anion lability and anion binding activity of ferric binding protein A.

    PubMed

    Heymann, Jared J; Gabricević, Mario; Mietzner, Timothy A; Crumbliss, Alvin L

    2010-02-01

    The bacterial transferrin ferric binding protein A (FbpA) requires an exogenous anion to facilitate iron sequestration, and subsequently to shuttle the metal across the periplasm to the cytoplasmic membrane. In the diverse conditions of the periplasm, numerous anions are known to be present. Prior in vitro experiments have demonstrated the ability of multiple anions to fulfill the synergistic iron-binding requirement, and the identity of the bound anion has been shown to modulate important physicochemical properties of iron-bound FbpA (FeFbpA). Here we address the kinetics and mechanism of anion exchange for the FeFbpA-nitrilotriacetate (NTA) assembly with several biologically relevant anions (citrate, oxalate, phosphate, and pyrophosphate), with nonphysiologic NTA serving as a representative synergistic anion/chelator. The kinetic data are consistent with an anion-exchange process that occurs in multiple steps, dependent on the identity of both the entering anion and the leaving anion. The exchange mechanism may proceed either as a direct substitution or through an intermediate FeFbpA-X* assembly based on anion (X) identity. Our kinetic results further develop an understanding of exogenous anion lability in the periplasm, as well as address the final step of the iron-free FbpA (apo-FbpA)/Fe(3+) sequestration mechanism. Our results highlight the kinetic significance of the FbpA anion binding site, demonstrating a correlation between apo-FbpA/anion affinity and the FeFbpA rate of anion exchange, further supporting the requirement of an exogenous anion to complete tight sequestration of iron by FbpA, and developing a mechanism for anion exchange within FeFbpA that is dependent on the identity of both the entering anion and the leaving anion. PMID:19813031

  8. The separation of platinum, palladium and gold from silicate rocks by the anion exchange separation of chloro complexes after a sodium peroxide fusion: an investigation of low recoveries.

    PubMed

    Enzweiler, J; Potts, P J

    1995-10-01

    A series of experiments was undertaken to measure the recovery efficiency of platinum, palladium and gold from silicate rocks using a sodium peroxide fusion followed by anion exchange separation of the analytes as chloro complexes. Results obtained by graphite furnace atomic absorption spectrometric analysis of standard solutions prepared in dilute HCl or HCl-acidified sodium peroxide solution showed that recoveries were near quantitative. However, when standard solutions were added to an alkaline sodium peroxide solution, which was then acidified, low results were obtained for platinum and gold (46% and 76% respectively). Low and variable results were also obtained when standard solutions were added to a peridotite sample that had been dissolved by the state procedure, and in the analysis of the South African Bureau of Standards certified reference material, SARM 7. Various experiments were undertaken to investigate these low recoveries, but the reason proposed here is the formation of hydroxychloro compounds in alkaline solution which are not, on acidification with HCl, converted quantitatively to the chloro complex necessary for quantitative anion exchange separation. It is concluded that a sodium peroxide fusion followed by an anion-exchange separation does not appear to form the basis of a successful technique for the determination of platinum, palladium and gold in silicate rocks. PMID:18966370

  9. Anion Exchange Behavior Of Ti, Zr, Hf, Nb And Ta As Homologues Of Rf And Db In Mixed HF--Acetone Solutions

    SciTech Connect

    Aksenov, N. V.; Bozhikov, G. A.; Starodub, G. Ya.; Dmitriev, S. N.; Filosofov, D. V.; Sun Jin, Jon; Radchenko, V. I.; Lebedev, N. A.; Novgorodov, A. F.

    2010-04-30

    We studied in detail the sorption behavior of Ti, Zr, Hf, Nb and Ta on AG 1 anion exchange resin in HF-acetone mixed solutions as a function of organic cosolvent and acid concentrations. Anion exchange behavior was found to be strongly acetone concentration dependent. The distribution coefficients of Ti, Zr, Hf and Nb increased and those of Ta decreased with increasing content of acetone in HF solutions. With increasing HF concentration anion exchange equilibrium analysis indicated the formation of fluoride complexes of group 4 elements with charge-3 and Ta---2. For Nb the slope of-2 increased up to-5. Optimal conditions for separation of the elements using AIX chromatography were found. Group 4 elements formed MF{sub 7}{sup 3-} (M = Ti, Zr, Hf) complexes whose sorption decreased Ti>Hf>Zr in reverse order of complex stability. This fact is of particular interest for studying ion exchange behavior of Rf compared to Ti. The advantages of studying chemical properties of Rf and Db in aqueous HF solutions mixed with organic solvents are briefly discussed.

  10. Fast Anion-Exchange in Highly Luminescent Nanocrystals of Cesium Lead Halide Perovskites (CsPbX3, X = Cl, Br, I)

    PubMed Central

    2015-01-01

    Postsynthetic chemical transformations of colloidal nanocrystals, such as ion-exchange reactions, provide an avenue to compositional fine-tuning or to otherwise inaccessible materials and morphologies. While cation-exchange is facile and commonplace, anion-exchange reactions have not received substantial deployment. Here we report fast, low-temperature, deliberately partial, or complete anion-exchange in highly luminescent semiconductor nanocrystals of cesium lead halide perovskites (CsPbX3, X = Cl, Br, I). By adjusting the halide ratios in the colloidal nanocrystal solution, the bright photoluminescence can be tuned over the entire visible spectral region (410–700 nm) while maintaining high quantum yields of 20–80% and narrow emission line widths of 10–40 nm (from blue to red). Furthermore, fast internanocrystal anion-exchange is demonstrated, leading to uniform CsPb(Cl/Br)3 or CsPb(Br/I)3 compositions simply by mixing CsPbCl3, CsPbBr3, and CsPbI3 nanocrystals in appropriate ratios. PMID:26207728

  11. Experimental and theoretical study of anion-exchange preparative chromatography for neptunium: the first application to thorium(IV) and its equilibrium and kinetics.

    PubMed

    Yamamura, Tomoo; Miyakoshi, Takeshi; Shiokawa, Yoshinobu; Mitsugashira, Toshiaki

    2007-10-26

    In order to study equilibrium and kinetic parameters in anion-exchange chromatography for preparatory purpose, a quantitative model for nonlinear anion-exchange chromatography in porous media was constructed, by paying special attention to interstitial length along void structure (cm) distinguished from apparent length (cm*). Langmuir-type adsorption isotherm for thorium(IV), as a natural substitution for neptunium(IV), in 6 mol dm(-3) nitric acid to anion-exchanger MSA-1 (200-400 mesh) was investigated in batch-wise and chromatographic experiments. The equilibrium parameters determined by batch-wise experiments determined as k=2.4x10(2) mol(-1) dm3 s(-1) and s0=0.5 mol dm(-3) agrees very well with the values of k=222 mol(-1) dm3 s(-1) and s0=0.5 mol dm(-3) derived from fitting by the numerical calculation. Kinetic parameters of ks and D affect band profile similarly, thereby maximum value of each parameter was evaluated as ks=1.3 mol(-1) dm3 s(-1) and D=9x10(-4) cm2 s(-1) by the numerical calculations.

  12. Understanding the Adsorption of PFOA on MIL-101(Cr)-Based Anionic-Exchange Metal-Organic Frameworks: Comparing DFT Calculations with Aqueous Sorption Experiments.

    PubMed

    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. PMID:26066631

  13. Fast Anion-Exchange in Highly Luminescent Nanocrystals of Cesium Lead Halide Perovskites (CsPbX3, X = Cl, Br, I).

    PubMed

    Nedelcu, Georgian; Protesescu, Loredana; Yakunin, Sergii; Bodnarchuk, Maryna I; Grotevent, Matthias J; Kovalenko, Maksym V

    2015-08-12

    Postsynthetic chemical transformations of colloidal nanocrystals, such as ion-exchange reactions, provide an avenue to compositional fine-tuning or to otherwise inaccessible materials and morphologies. While cation-exchange is facile and commonplace, anion-exchange reactions have not received substantial deployment. Here we report fast, low-temperature, deliberately partial, or complete anion-exchange in highly luminescent semiconductor nanocrystals of cesium lead halide perovskites (CsPbX3, X = Cl, Br, I). By adjusting the halide ratios in the colloidal nanocrystal solution, the bright photoluminescence can be tuned over the entire visible spectral region (410-700 nm) while maintaining high quantum yields of 20-80% and narrow emission line widths of 10-40 nm (from blue to red). Furthermore, fast internanocrystal anion-exchange is demonstrated, leading to uniform CsPb(Cl/Br)3 or CsPb(Br/I)3 compositions simply by mixing CsPbCl3, CsPbBr3, and CsPbI3 nanocrystals in appropriate ratios. PMID:26207728

  14. Electrodialytic Transport Properties of Anion-Exchange Membranes Prepared from Poly(vinyl alcohol) and Poly(vinyl alcohol-co-methacryloyl aminopropyl trimethyl ammonium chloride)

    PubMed Central

    Jikihara, Atsushi; Ohashi, Reina; Kakihana, Yuriko; Higa, Mitsuru; Kobayashi, Kenichi

    2012-01-01

    Random-type anion-exchange membranes (AEMs) have been prepared by blending poly(vinyl alcohol) (PVA) and the random copolymer-type polycation, poly(vinyl alcohol-co-methacryloyl aminopropyl trimethyl ammonium chloride) at various molar percentages of anion-exchange groups to vinyl alcohol groups, Cpc, and by cross-linking the PVA chains with glutaraldehyde (GA) solution at various GA concentrations, CGA. The characteristics of the random-type AEMs were compared with blend-type AEMs prepared in our previous study. At equal molar percentages of the anion exchange groups, the water content of the random-type AEMs was lower than that of the blend-type AEMs. The effective charge density of the random-type AEMs increased with increasing Cpc and reached a maximum value. Further, the maximum value of the effective charge density increased with increasing CGA. The maximum value of the effective charge density, 0.42 mol/dm3, was obtained for the random-type AEM with Cpc = 4.2 mol % and CGA = 0.15 vol %. A comparison of the random-type and blend-type AEMs with almost the same Cpc showed that the random-type AEMs had lower membrane resistance than the blend-type ones. The membrane resistance and dynamic transport number of the random-type AEM with Cpc = 6.0 mol % and CGA = 0.15 vol % were 4.8 Ω cm2 and 0.83, respectively. PMID:24958543

  15. Understanding the Adsorption of PFOA on MIL-101(Cr)-Based Anionic-Exchange Metal-Organic Frameworks: Comparing DFT Calculations with Aqueous Sorption Experiments.

    PubMed

    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.

  16. The separation of platinum, palladium and gold from silicate rocks by the anion exchange separation of chloro complexes after a sodium peroxide fusion: an investigation of low recoveries.

    PubMed

    Enzweiler, J; Potts, P J

    1995-10-01

    A series of experiments was undertaken to measure the recovery efficiency of platinum, palladium and gold from silicate rocks using a sodium peroxide fusion followed by anion exchange separation of the analytes as chloro complexes. Results obtained by graphite furnace atomic absorption spectrometric analysis of standard solutions prepared in dilute HCl or HCl-acidified sodium peroxide solution showed that recoveries were near quantitative. However, when standard solutions were added to an alkaline sodium peroxide solution, which was then acidified, low results were obtained for platinum and gold (46% and 76% respectively). Low and variable results were also obtained when standard solutions were added to a peridotite sample that had been dissolved by the state procedure, and in the analysis of the South African Bureau of Standards certified reference material, SARM 7. Various experiments were undertaken to investigate these low recoveries, but the reason proposed here is the formation of hydroxychloro compounds in alkaline solution which are not, on acidification with HCl, converted quantitatively to the chloro complex necessary for quantitative anion exchange separation. It is concluded that a sodium peroxide fusion followed by an anion-exchange separation does not appear to form the basis of a successful technique for the determination of platinum, palladium and gold in silicate rocks.

  17. Identification of biomarkers for ovarian cancer using strong anion-exchange ProteinChips: potential use in diagnosis and prognosis.

    PubMed

    Kozak, Katherine R; Amneus, Malaika W; Pusey, Suzanne M; Su, Feng; Luong, Mui N; Luong, Sam A; Reddy, Srinivasa T; Farias-Eisner, Robin

    2003-10-14

    One hundred eighty-four serum samples from patients with ovarian cancer (n = 109), patients with benign tumors (n = 19), and healthy donors (n = 56) were analyzed on strong anion-exchange surfaces using surface-enhanced laser desorption/ionization time-of-flight mass spectrometry technology. Univariate and multivariate statistical analyses applied to protein-profiling data obtained from 140 training serum samples identified three biomarker protein panels. The first panel of five candidate protein biomarkers, termed the screening biomarker panel, effectively diagnosed benign and malignant ovarian neoplasia [95.7% sensitivity, 82.6% specificity, 89.2% accuracy, and receiver operating characteristic (ROC) area under the curve of 0.94]. The other two panels, consisting of five and four candidate protein biomarkers each, effectively distinguished between benign and malignant ovarian neoplasia and were therefore referred to as validation biomarker panel I (81.5% sensitivity, 94.9% specificity, 88.2% accuracy, and ROC = 0.94) and validation biomarker panel II (72.8% sensitivity, 94.9% specificity, 83.9% accuracy, and ROC = 0.90). The three ovarian cancer biomarker protein panels correctly diagnosed 41 of the 44 blinded test samples: 21 of 22 malignant ovarian neoplasias [10 of 11 early-stage ovarian cancer (I/II) and 11 of 11 advanced-stage ovarian cancer (III/IV)], 6 of 6 low malignant potential, 5 of the 6 benign tumors, and 9 of 10 normal patient samples. In conclusion, we have discovered three ovarian cancer biomarker protein panels that, when used together, effectively distinguished serum samples from healthy controls and patients with either benign or malignant ovarian neoplasia.

  18. Evaluation of anion exchange resins Tulsion A-30 and Indion-930A by application of radioanalytical technique

    NASA Astrophysics Data System (ADS)

    Singare, P. U.

    2014-07-01

    Radioanalytical technique using 131I and 82Br was employed to evaluate organic based anion exchange resins Tulsion A-30 and Indion-930A. The evaluation was based on performance of these resins during iodide and bromide ion-isotopic exchange reactions. It was observed that for iodide ion-isotopic exchange reaction by using Tulsion A-30 resin, the values of specific reaction rate (min-1), amount of iodide ion exchanged (mmol), initial rate of iodide ion exchange (mmol/min) and log K d were 0.238, 0.477, 0.114, and 11.0, respectively, which was higher than 0.155, 0.360, 0.056, and 7.3, respectively as that obtained by using Indion-930A resins under identical experimental conditions of 40.0°C, 1.000 g of ion exchange resins and 0.003 M labeled iodide ion solution. Also at a constant temperature of 40.0°C, as the concentration of labeled iodide ion solution increases 0.001 to 0.004 M, for Tulsion A-30 resins the percentage of iodide ions exchanged increases from 59.0 to 65.1%, and from 46.4 to 48.8% for Indion-930A resins under identical experimental conditions. The identical trend was observed for both the resins during bromide ion-isotopic exchange reactions. The overall results indicate that under identical experimental conditions, Tulsion A-30 show superior performance over Indion-930A resins. The results of present experimental work have demonstrated that the radioanalytical technique used here can be successfully applied for characterization of different ion exchange resins so as to evaluate their performance under various process parameters.

  19. Compensatory role of inducible annexin A2 for impaired biliary epithelial anion-exchange activity of inflammatory cholangiopathy.

    PubMed

    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

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

    PubMed

    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.

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

    PubMed

    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.

  2. Polyethylenimine modified poly(ethylene terephthalate) capillary channeled-polymer fibers for anion exchange chromatography of proteins.

    PubMed

    Jiang, Liuwei; Jin, Yi; Marcus, R Kenneth

    2015-09-01

    Native poly(ethylene terephthalate) (PET) capillary-channeled polymer (C-CP) fibers have been previously studied as stationary phases for reversed phase and affinity protein separations. In this study, surface modified PET C-CP fibers were evaluated for the anion exchange separation of proteins. The native PET C-CP fibers were aminated using polyethylenimine (PEI) followed by a 1,4-butanediol diglycidyl ether (BUDGE) cross-linking step. Subsequent PEI/BUDGE treatments can be employed to further develop the polyamine layer on the fiber surfaces. The PEI densities of the modified fibers were quantified through the ninhydrin reaction, yielding values of 0.43-0.89μmolg(-1). The surface modification impact on column permeability was found to be 0.66×10(-11) to 1.33×10(-11)m(2), depending on the modification time and conditions. The dynamic binding capacities of the modified fiber media were determined to be 1.99-8.54mgmL(-1) bed volume, at linear velocities of 88-438cmmin(-1) using bovine serum albumin as the model protein. It was found that increasing the mobile phase linear velocity (up to 438cmmin(-1)) had no effect on the separation quality for a synthetic protein mixture, reflecting the lack of van Deemter C-term effects for the C-CP fiber phase. The low-cost, easy modification method and the capability of fast protein separation illustrate great potential in the use of PEI/BUDGE-modified PET C-CP fibers for high-throughput protein separation and downstream processing. PMID:26253835

  3. Determination of propofol glucuronide from hair sample by using mixed mode anion exchange cartridge and liquid chromatography tandem mass spectrometry.

    PubMed

    Kwak, Jae-Hwan; Kim, Hye Kyung; Choe, Sanggil; In, Sangwhan; Pyo, Jae Sung

    2016-03-15

    The main objective of this study was to develop and validate a simpler and less time consuming analytical method for determination of propofol glucuronide from hair sample, by using mixed mode anion exchange cartridge and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The study uses propofol glucuronide, a major metabolite of propofol, as a marker for propofol abuse. The hair sample was digested in sodium hydroxide solution and loaded in mixed-mode anion cartridge for solid phase extraction. Water and ethyl acetate were used as washing solvents to remove interfering substances from the hair sample. Consequently, 2% formic acid in ethyl acetate was employed to elute propofol glucuronide from the sorbent of mixed-mode anion cartridge, and analyzed by LC-MS/MS. The method validation parameters such as selectivity, specificity, LOD, LLOQ, accuracy, precision, recovery, and matrix effect were also tested. The linearity of calibration curves showed good correlation, with correlation coefficient 0.998. The LOD and LLOQ of the propofol glucuronide were 0.2 pg/mg and 0.5 pg/mg, respectively. The intra and inter-day precision and accuracy were acceptable within 15%. The mean values of recovery and matrix effect were in the range of 91.7-98.7% and 87.5-90.3%, respectively, signifying that the sample preparation, washing and extraction procedure were efficient, and there was low significant hair matrix effect for the extraction of propofol glucuronide from hair sample on the mixed mode anion cartridge. To evaluate the suitability of method, the hair of propofol administered rat was successfully analyzed with this method.

  4. Study on adsorption properties of QCS/PS-G8-2-8 anion exchange membrane for Rhodamine B

    NASA Astrophysics Data System (ADS)

    Zhang, Yang; Wang, Jilin; Wang, Lulu; Feng, Ruijiang; Zhang, Fan

    2015-06-01

    A series of novel anion exchange composite membrane (QCS/PS-G8-2-8) were synthesized based on the quaternized chitosan (QCS, DQ = 89.20 (±3.50)%) blended with block polymer of polystyrene (PS) and G8-2-8 (maleic acid diethyl brace base pairs [octyl dimethyl chloride/ammonium bromide]). Then the QCS was cross-linked by glutaraldehyde (GA). The parameters including adsorption time (t), pH, and initial concentration of Rhodamine B (C0), temperature (T), the mass fraction of G8-2-8 and GA (WGA) on the adsorption were investigated to determine the optimum condition for the removal of RB. The kinetic and thermodynamic properties of the adsorption process were also discussed. The optimum adsorption condition was that the adsorption time was 100 min, pH was 4, the initial concentration of RB was 100 mg L-1, the mass fraction of G8-2-8 was 5.0 wt%, the mass fraction of GA was 2.0 wt%, the temperature was 40 °C. Thus, RB optimum adsorption capacity (q) of the composite membrane QCS/PS-G8-2-8 (5.0%) (G8-2-8 mass content (wt.%) was 5.0%) was 17.04 mg g-1. The adsorption isotherm of the RB on the composite membrane can be well fitted with the Temkin equation. The adsorption kinetics can be well described by the pseudo-second-order kinetics model. The values of ΔG, ΔH and ΔS indicated that the adsorption of RB onto QCS/PS-G8-2-8 was spontaneous and exothermic.

  5. Determination of levoglucosan in biomass combustion aerosol by high-performance anion-exchange chromatography with pulsed amperometric detection

    NASA Astrophysics Data System (ADS)

    Engling, Guenter; Carrico, Christian M.; Kreidenweis, Sonia M.; Collett, Jeffrey L.; Day, Derek E.; Malm, William C.; Lincoln, Emily; Min Hao, Wei; Iinuma, Yoshiteru; Herrmann, Hartmut

    Atmospheric particulate matter can be strongly affected by smoke from biomass combustion, including wildfires, prescribed burns, and residential wood burning. Molecular source tracer techniques help determine contributions of biomass smoke to particle concentrations if representative source profiles are available. Various wood smoke source profiles have been generated for residential wood burning; however, few emission data are available for the combustion of biomass under open-burning conditions. Anhydrosugars, produced as thermal degradation products of cellulose and hemicellulose, are typically analyzed by gas chromatography-mass spectrometry (GC-MS) after chemical derivatization. A simpler alternative analytical method, based on high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD), was developed here and utilized to measure several isomeric anhydrosugars (levoglucosan, mannosan, and galactosan) in primary smoke aerosol from various types of biomass and from different combustion conditions representative of prescribed and wildfires. Highly varying patterns were observed in the emission profiles of various molecular markers as a function of fuel type and combustion conditions. Emission factors of levoglucosan were a strong function of fuel type, combustion phase, and uphill versus downhill burn direction, varying from 36 to 1368 μg mg -1 organic carbon. Fuel type was the most important determinant, causing variations in emission factors of levoglucosan over an order of magnitude, while combustion phase and burn direction generally affected emission factors by a factor of 2-3. Mannosan and galactosan showed emission trends similar to levoglucosan. Levoglucosan emission factors from selected samples were compared to data obtained by two independent analytical methods, high-performance liquid chromatography (HPLC-MS) and GC-MS, showing rather good agreement. The HPAEC-PAD analytical method offers a simple alternative to GC

  6. Selective colorimetric determination of TNT partitioned between an alkaline solution and a strongly basic Dowex 1-X8 anion exchanger.

    PubMed

    Uzer, Ayşem; Erçağ, Erol; Apak, Reşat

    2008-01-30

    The Meisenheimer anions formed from TNT in KOH solutions in alcohol or acetone were used in screening tests for TNT among possible nitro-explosives. The same reaction was used for the spectrophotometric assay of TNT in soil by CRREL (Cold Regions Research & Engineering Laboratory of the U.S. Army) method, also known as Jenkins' method, but the color stability was too dependent on the solution composition and the water tolerance was low, necessitating complete drying of soil samples (which may cause partial analyte decomposition) prior to analysis. This study reports the development of a colorimetric method based on the solid phase extraction (SPE) of the Meisenheimer anion formed from TNT and aqueous NaOH into a strongly basic anion exchange resin Dowex 1-X8 (OH(-) form). The orange-red color that developed both in the solid resin and solution phases was persistent for at least 1h. The resin was let to swell in alcohol, washed first with 1M aqueous NaOH, and then with H(2)O before use. To 5 mL of 4-400 ppm TNT solutions in 1:1 (v/v) acetone-water, 0.5 mL of 5% NaOH was added, diluted to 50 mL with 1:1 acetone-water, and the resulting solutions (containing the orange-red Meisenheimer anion of TNT) were agitated at room temperature with 0.9 g resin for < or =50 min. TNT exhibited a reasonably constant distribution coefficient between the resin and aqueous phases. The absorbance of the filtered solutions was measured against a reagent blank at 500nm. The TNT-loaded resins were regenerated with 1M HCl containing sodium sulfite. The calibration line of filtrate absorbance versus analytical concentration was linear over two orders of magnitude between 0.4 and 40 ppm TNT in final solution. Unlike Jenkins' method, the method was tolerant to 100-fold (by mass) of common soil anions like sulfate, nitrate, and chloride. The basic advantages of the developed colorimetric method over the similar CRREL/Jenkins' method may be summarized as color stability, water and common ion

  7. Selective colorimetric determination of TNT partitioned between an alkaline solution and a strongly basic Dowex 1-X8 anion exchanger.

    PubMed

    Uzer, Ayşem; Erçağ, Erol; Apak, Reşat

    2008-01-30

    The Meisenheimer anions formed from TNT in KOH solutions in alcohol or acetone were used in screening tests for TNT among possible nitro-explosives. The same reaction was used for the spectrophotometric assay of TNT in soil by CRREL (Cold Regions Research & Engineering Laboratory of the U.S. Army) method, also known as Jenkins' method, but the color stability was too dependent on the solution composition and the water tolerance was low, necessitating complete drying of soil samples (which may cause partial analyte decomposition) prior to analysis. This study reports the development of a colorimetric method based on the solid phase extraction (SPE) of the Meisenheimer anion formed from TNT and aqueous NaOH into a strongly basic anion exchange resin Dowex 1-X8 (OH(-) form). The orange-red color that developed both in the solid resin and solution phases was persistent for at least 1h. The resin was let to swell in alcohol, washed first with 1M aqueous NaOH, and then with H(2)O before use. To 5 mL of 4-400 ppm TNT solutions in 1:1 (v/v) acetone-water, 0.5 mL of 5% NaOH was added, diluted to 50 mL with 1:1 acetone-water, and the resulting solutions (containing the orange-red Meisenheimer anion of TNT) were agitated at room temperature with 0.9 g resin for < or =50 min. TNT exhibited a reasonably constant distribution coefficient between the resin and aqueous phases. The absorbance of the filtered solutions was measured against a reagent blank at 500nm. The TNT-loaded resins were regenerated with 1M HCl containing sodium sulfite. The calibration line of filtrate absorbance versus analytical concentration was linear over two orders of magnitude between 0.4 and 40 ppm TNT in final solution. Unlike Jenkins' method, the method was tolerant to 100-fold (by mass) of common soil anions like sulfate, nitrate, and chloride. The basic advantages of the developed colorimetric method over the similar CRREL/Jenkins' method may be summarized as color stability, water and common ion

  8. Purification of prostatic acid phosphatase (PAP) for structural and functional studies.

    PubMed

    Herrala, Annakaisa M; Quintero, Ileana B; Vihko, Pirkko T

    2013-01-01

    High-scale purification methods are required for several protein studies such as crystallography, mass spectrometry, circular dichroism, and function. Here we describe a purification method for PAP based on anion exchange, L-(+)-tartrate affinity, and gel filtration chromatographies. Acid phosphatase activity and protein concentration were measured for each purification step, and to collect the fractions with the highest acid phosphatase activity the p-nitrophenyl phosphate method was used. The purified protein obtained by the procedure described here was used for the determination of the first reported three-dimensional structure of prostatic acid phosphatase.

  9. 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.

    PubMed

    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.

  10. 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.

    PubMed

    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

  11. Sodium citrate-assisted anion exchange strategy for construction of Bi{sub 2}O{sub 2}CO{sub 3}/BiOI photocatalysts

    SciTech Connect

    Song, Peng-Yuan; Xu, Ming; Zhang, Wei-De

    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.

  12. A novel method to differentiate between ping-pong and simultaneous exchange kinetics and its application to the anion exchanger of the HL60 cell

    PubMed Central

    1992-01-01

    We have developed a new test to differentiate between ping-pong and simultaneous mechanisms for tightly coupled anion exchange. This test requires the use of a dead-end reversible noncompetitive inhibitor. As an example, we have applied the test to the anion exchanger of the HL60 cell using the salicylic acid derivative 3,5-diiodosalicylic acid (DIS), which reversibly inhibits HL60 cell Cl/Cl exchange. The concentration of DIS that causes 50% inhibition (ID50) increased only slightly as either intra- or extracellular chloride was increased, indicating that DIS inhibits HL60 anion exchange in a noncompetitive manner. In agreement with this observation, plots of the slope of the Dixon plot as a function of 1/[Clo] or 1/[Cli] were fit with straight lines with nonzero intercepts, indicating that DIS does not compete with either of the substrates ([Clo] and [Cli]). The secondary Dixon slope test is based on the fact that, for a dead-end inhibitor such as DIS, the slope of the Dixon plot slope vs. 1/[Cli] (secondary Dixon slope or SDS) is independent of extracellular Cl when the exchange mechanism follows ping-pong kinetics. Similarly, the SDS calculated from a plot as a function of 1/[Clo] is also independent of intracellular Cl for a ping-pong exchanger. In contrast to this prediction, we found that for DIS inhibition of Cl/Cl exchange in HL60 cells the slope of the Dixon plot slope vs. 1/[Cli] decreased by a factor of 2.5-fold when [Clo] was increased from 1 to 11 mM (P < 0.0001). This change in the SDS rules out ping-pong kinetics, but is consistent with a simultaneous model of Cl/Cl exchange in which there are extra- and intracellular anion binding sites, both of which must be occupied by suitable anions in order to allow simultaneous exchange of the ions. PMID:1474373

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

    PubMed

    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

  14. Heterodimers formed through a partial anionic exchange process: scanning tunneling spectroscopy to monitor bands across the junction vis-à-vis photoinduced charge separation

    NASA Astrophysics Data System (ADS)

    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

  15. Purification and characterization of a novel phospholipid transfer protein from filamentous fungi.

    PubMed

    Grondin, P; Vergnolle, C; Chavant, L; Kader, J C

    1990-01-01

    1. We have isolated from mycelia of Mucor mucedo, a filamentous fungus, a phospholipid transfer protein. 2. The purification steps were gel filtration, hydroxyapatite chromatography, blue affinity column and fast protein liquid chromatography on anion exchanger. 3. A purified protein was obtained with a molecular mass of 24 kDa and a pI of 5.05 and its N-terminal sequence was established. 4. This protein transfers phosphatidylinositol, as well as phosphatidylcholine and phosphatidylethanolamine.

  16. High Throughput Identification, Purification and Structural Characterization of Water Soluble Protein Complexes in Desulfovibrio vulgaris

    SciTech Connect

    Dong,, Ming; Han, Bong-Gyoon; Liu, Hui-Hai; Malik, J.; Geller, Jil; Yang, Li; Choi, M.; Chandonia, John-Marc; Arbelaez, Pablo; Sterling, H. J.; Typke, Dieter; Shatsky, Max; Brenner, Steve; Fisher, Susan; Williams, Evan; Szakal, Evelin; Allen, S.; Hall, S. C.; Hazen, Terry; Witkowska, H. E.; Jin, Jiming; Glaeser, Robert; Biggin, Mark

    2010-05-17

    Our scheme for the tagless purification of water soluble complexes. 10 g of protein from a crude bacterial extract is first fractionated by ammonium sulfate precipitation and then by a series of chromatographic steps: anion exchange (IEX), hydrophobic interaction (HIC), and finally size exclusion (Gel Filtration). Fractions from the last chromatography step are trypsin digested and peptides labeled with iTRAQ reagents to allow multiplexing and quantitation during mass spectrometric analysis. Elution profiles of identified proteins are then subjected to clustering analysis.

  17. Rare cancer cell analyzer for whole blood applications: automated nucleic acid purification in a microfluidic disposable card.

    PubMed

    Kokoris, M; Nabavi, M; Lancaster, C; Clemmens, J; Maloney, P; Capadanno, J; Gerdes, J; Battrell, C F

    2005-09-01

    One current challenge facing point-of-care cancer detection is that existing methods make it difficult, time consuming and too costly to (1) collect relevant cell types directly from a patient sample, such as blood and (2) rapidly assay those cell types to determine the presence or absence of a particular type of cancer. We present a proof of principle method for an integrated, sample-to-result, point-of-care detection device that employs microfluidics technology, accepted assays, and a silica membrane for total RNA purification on a disposable, credit card sized laboratory-on-card ('lab card") device in which results are obtained in minutes. Both yield and quality of on-card purified total RNA, as determined by both LightCycler and standard reverse transcriptase amplification of G6PDH and BCR-ABL transcripts, were found to be better than or equal to accepted standard purification methods. PMID:16199179

  18. Surface- vs Diffusion-Limited Mechanisms of Anion Exchange in CsPbBr3 Nanocrystal Cubes Revealed through Kinetic Studies.

    PubMed

    Koscher, Brent A; Bronstein, Noah D; Olshansky, Jacob H; Bekenstein, Yehonadav; Alivisatos, A Paul

    2016-09-21

    Ion-exchange transformations allow access to nanocrystalline materials with compositions that are inaccessible via direct synthetic routes. However, additional mechanistic insight into the processes that govern these reactions is needed. We present evidence for the presence of two distinct mechanisms of exchange during anion exchange in CsPbX3 nanocrystals (NCs), ranging in size from 6.5 to 11.5 nm, for transformations from CsPbBr3 to CsPbCl3 or CsPbI3. These NCs exhibit bright luminescence throughout the exchange, allowing their optical properties to be observed in real time, in situ. The iodine exchange presents surface-reaction-limited exchanges allowing all anionic sites within the NC to appear chemically identical, whereas the chlorine exchange presents diffusion-limited exchanges proceeding through a more complicated exchange mechanism. Our results represent the first steps toward developing a microkinetic description of the anion exchange, with implications not only for understanding the lead halide perovskites but also for nanoscale ion exchange in general. PMID:27606934

  19. Monitoring of enzymatic hydrolysis of starch by microdialysis sampling coupled on-line to anion exchange chromatography and integrated pulsed electrochemical detection using post-column switching

    SciTech Connect

    Torto, N.; Gorton, L.; Emneus, J.; Laurell, T.; Marko-Varga, G.; Akerberg, C.; Zacchi, G. |

    1997-12-05

    A quantitative evaluation of the hydrolysis of wheat starch using Termamyl, a thermostable {alpha}-amylase, is reported. Data from the monitoring of the hydrolysis of wheat starch indicated that, after 1 h, glucose and maltooligosaccharides up to DP 7 were the main hydrolysis products and thus enabled optimization of a liquefaction step during the production of L-lactic acid. The monitoring system used, both in the on- and off-line mode, was based on continuous flow microdialysis sampling (CFMS) coupled to anion exchange chromatography and integrated pulsed electrochemical detection (IPED). A microdialysis probe equipped with a 5-mm polysulfone (SPS 4005) membrane, with a molecular-weight cut-off of 5 kDa, was used to sample the hydrolysis products of native wheat starch at 90 C. Characteristic fingerpoint separations were achieved by anion exchange chromatography after enzymatic hydrolysis. Post-column switching improved the detection and, consequently, also quantification of the hydrolysates as fouling of the electrode could be reduced. Maltooligosaccharide standards were used for quantification and to verify the elution of the hydrolysates by spiking the off-line samples.

  20. Use of a new tandem cation/anion exchange system with clinical-scale generators provides high specific volume solutions of technetium-99m and rhenium-188

    SciTech Connect

    Knapp, F.R. Jr.; Beets, A.L.; Mirzadeh, S.; Guhlke, S. |

    1998-03-01

    In this paper the authors describe the first application of a simple and inexpensive post elution tandem cation-anion exchange column system which is based on generator elution with salts of weak acids such as ammonium acetate instead of saline solution to provide very high specific volume solutions of technetium-99m and rhenium-188 from clinical scale molybdenum-99/technetium-99m generator prepared from low specific activity (n,y) molybdenum-99, and tungsten-188/rhenium-188 generators, respectively. Initial passage of the bolus through a strong cation exchange cartridge converts the ammonium acetate to acetic acid which is essentially not ionized at the acidic pH, allowing specific subsequent amine type (QMA SepPak{trademark}) anion exchange cartridge column trapping of the microscopic levels of the pertechnetate or perrhenate. Subsequent elution of the anion cartridge with a small volume (< 1 mL) of saline then provides high specific volume solutions of technetium-99m by concentration of the high eluant volumes obtained by elution of clinical-scale (1 Ci) generators. This new approach also works very effectively to obtain high specific volume solutions of rhenium-188 (> 500 mCi/mL) from the alumina-based tungsten-188/rhenium-188 generator.

  1. Capture and recovery of indole from methylnaphthalene oil in a continuous supercritical CO{sub 2} extraction apparatus over a fixed bed of anion-exchange resin

    SciTech Connect

    Sakanishi, Kinya; Obata, Hiroaki; Mochida, Isao; Sakaki, Tsuyoshi

    1996-01-01

    Capture and recovery of nonbasic aromatic nitrogen compounds such as indole from crude methylnaphthalene oil in coal tar fractions were examined using a continuous supercritical CO{sub 2} extraction apparatus with the fixed bed of an anion-exchange resin. A model feed consisting of 10 wt% indole with 10 wt% quinoline in 1-methylnaphthalene and crude methylnaphthalene oil (CMNO) was used for the supercritical CO{sub 2} separation procedures. Indole was selectively adsorbed on an anion-exchange resin (Amberlite IRA-904) for the first 120 min, with quinoline and 1-methylnaphthalene being eluted under the supercritical CO{sub 2} (323 K, 80 atm) conditions. After the resin was saturated with indole, the feed was stopped and the adsorbed indole was recovered. Preextraction of the resin with supercritical CO{sub 2} before the recovery of indole from the adsorbent improved the concentration of recovered indole through the selective elution of quinoline and 1-methylnaphthalene remaining in the dead space in the flow line and fixed bed. Indole in CMNO was also effectively separated by the same procedures as described above. The adsorption and desorption mechanisms of indole are briefly discussed based on the above results.

  2. Novel tentacle-type polymer stationary phase grafted with anion exchange polymer chains for open tubular CEC of nucleosides and proteins.

    PubMed

    Aydoğan, Cemil; Çetin, Kemal; Denizli, Adil

    2014-08-01

    A novel and simple method for preparation of a tentacle-type polymer stationary phase grafted with polyethyleneimine (PEI) anion exchanger was developed for open tubular capillary electrochromatography (OT-CEC) of nucleosides and proteins. The polymeric stationary phase was prepared using 3-chloro-2-hydroxypropyl methacrylate (HPMA-Cl)-based reactive monomer. The preparation procedure included pretreatment of the capillary inner wall, silanization, in situ graft polymerization with HPMA-Cl and PEI modification. To compare with the tentacle-type capillary column with PEI functionalization, a monolayer capillary column without PEI functionalization was also prepared. The electrochromatographic characterization of the prepared open tubular column was performed using alkylbenzenes. The electroosmotic flow (EOF) with regard to PEI concentrations and the running buffer pH was investigated. The separation conditions of the nucleosides and the proteins were optimized. The modified tentacle-type column with high anion exchange capacity has proven to afford better retention and resolution for the separation of nucleosides and proteins. The PEI functionalization column can also provide long-term stable use for biomolecule separation using a single capillary with relative standard deviation values of retention times of less than 2%. The results indicate that the present method for open tubular capillary preparation with a HPMA-Cl-based reactive monomer is promising for OT-CEC biomolecule separation.

  3. Single vial sample preparation of markers of nerve agents by dispersive solid-phase extraction using magnetic strong anion exchange resins.

    PubMed

    Singh, Varoon; Chinthakindi, Sridhar; Purohit, Ajay Kumar; Pardasani, Deepak; Tak, Vijay; Dubey, Devendra Kumar

    2015-05-22

    A sample preparation method involving extraction, enrichment and derivatization of acidic degradation products of nerve agents was developed using magnetic strong anion exchange resins (MSAX). The method was performed in a single vial involving magnetic dispersive solid phase extraction (MDSPE). Analytes were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) in the presence of resins. MSAX were custom synthesized using Fe3O4 nanoparticles as core, 4-vinylpyridine-co-divinylbenzene as polymer shell and quaternary pyridinium function as anion-exchanger. Hydroxide ions were the counter-anions of MSAX to effectively capture the acidic alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs). Quantitative measurements of analytes were performed in the selected ion monitoring mode of GC-MS. Full scan mode of analysis was followed for identifications. Under the optimized conditions analytes were recovered in the range of 39.7-98.8% (n=3, relative standard deviations (RSD) from 0.3 to 6.5%). Limits of detection (LODs) were in the range of 0.1-1.1ngmL(-1); and the linear dynamic range was 5-1000ngmL(-1) with r(2) of 0.9977-0.9769. Applicability of the method was tested with rain-, tap-, muddy-water and Organization for Prohibition of Chemical Weapons (OPCW) Proficiency Test samples.

  4. Vinylbenzyl quaternary ammonium-based polymeric monolith with hydrophilic interaction/strong anion exchange mixed-mode for pressurized capillary electrochromatography.

    PubMed

    Lin, Xucong; Feng, Shuhui; Jia, Wenchao; Ding, Kang; Xie, Zenghong

    2013-11-01

    A novel polymeric monolith with hydrophilic interaction and strong anion-exchange mixed-mode has been fabricated for pressurized capillary electrochromatography by an in situ copolymerization of vinylbenzyl trimethylammonium chloride (VBTA) and bisphenol A glycerolate dimethacrylate (BisGMA). The optimization of the polymerization mixture composition has been investigated, and column characteristics in terms of mechanical stability, permeability and reproducibility have been studied in detail. Linear responses between back pressure and flow rate have been achieved in different solvents. The absolute value of swelling propensity (SP) factor for poly(VBTA-co-BisGMA) monolith is 0.41, and the degree of permeability drop from pure ACN to water is about 45%. An acceptable mechanical stability of the column is obtained. The suitable reproducibility is also measured with the RSD for day-to-day (n=3) of retention time and column efficiency less than 3.3%, and the RSD for batch-to-batch (n=3) less than 5.3%, respectively. Under the optimum conditions, the mixed-mode of hydrophilic interaction and strong anion-exchange has been carried out, and efficient electrochromatography profiling of various polar compounds including neutral phenols, negatively charged benzoic acids and positively charged nucleic acid bases and nucleosides are achieved, respectively. PMID:24125728

  5. Single vial sample preparation of markers of nerve agents by dispersive solid-phase extraction using magnetic strong anion exchange resins.

    PubMed

    Singh, Varoon; Chinthakindi, Sridhar; Purohit, Ajay Kumar; Pardasani, Deepak; Tak, Vijay; Dubey, Devendra Kumar

    2015-05-22

    A sample preparation method involving extraction, enrichment and derivatization of acidic degradation products of nerve agents was developed using magnetic strong anion exchange resins (MSAX). The method was performed in a single vial involving magnetic dispersive solid phase extraction (MDSPE). Analytes were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) in the presence of resins. MSAX were custom synthesized using Fe3O4 nanoparticles as core, 4-vinylpyridine-co-divinylbenzene as polymer shell and quaternary pyridinium function as anion-exchanger. Hydroxide ions were the counter-anions of MSAX to effectively capture the acidic alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs). Quantitative measurements of analytes were performed in the selected ion monitoring mode of GC-MS. Full scan mode of analysis was followed for identifications. Under the optimized conditions analytes were recovered in the range of 39.7-98.8% (n=3, relative standard deviations (RSD) from 0.3 to 6.5%). Limits of detection (LODs) were in the range of 0.1-1.1ngmL(-1); and the linear dynamic range was 5-1000ngmL(-1) with r(2) of 0.9977-0.9769. Applicability of the method was tested with rain-, tap-, muddy-water and Organization for Prohibition of Chemical Weapons (OPCW) Proficiency Test samples. PMID:25863924

  6. Band 3, the human red cell chloride/bicarbonate anion exchanger (AE1, SLC4A1), in a structural context.

    PubMed

    Reithmeier, Reinhart A F; Casey, Joseph R; Kalli, Antreas C; Sansom, Mark S P; Alguel, Yilmaz; Iwata, So

    2016-07-01

    The crystal structure of the dimeric membrane domain of human Band 3(1), the red cell chloride/bicarbonate anion exchanger 1 (AE1, SLC4A1), provides a structural context for over four decades of studies into this historic and important membrane glycoprotein. In this review, we highlight the key structural features responsible for anion binding and translocation and have integrated the following topological markers within the Band 3 structure: blood group antigens, N-glycosylation site, protease cleavage sites, inhibitor and chemical labeling sites, and the results of scanning cysteine and N-glycosylation mutagenesis. Locations of mutations linked to human disease, including those responsible for Southeast Asian ovalocytosis, hereditary stomatocytosis, hereditary spherocytosis, and distal renal tubular acidosis, provide molecular insights into their effect on Band 3 folding. Finally, molecular dynamics simulations of phosphatidylcholine self-assembled around Band 3 provide a view of this membrane protein within a lipid bilayer. PMID:27058983

  7. [Effects and mechanism on removing organics and reduction of membrane fouling using granular macro-porous anion exchange resin in drinking water treatment].

    PubMed

    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.

  8. Selective determination of ammonium ions by high-speed ion-exclusion chromatography on a weakly basic anion-exchange resin column.

    PubMed

    Mori, Masanobu; Tanaka, Kazuhiko; Helaleh, Murad I H; Xu, Qun; Ikedo, Mikaru; Ogura, Yutaka; Sato, Shinji; Hu, Wenzhi; Hasebe, Kiyoshi

    2003-05-16

    This paper describes an ion-exclusion chromatographic system for the rapid and selective determination of ammonium ion. The optimized ion-exclusion chromatographic system was established with a polymethacrylate-based weakly basic anion-exchange resin column (TSKgel DEAE-5PW) as the separation column, an aqueous solution containing 0.05 mM tetramethylammonium hydroxide (pH 9.10) as eluent with conductimetric detection for the analyte determination. Under the optimum chromatographic conditions, ammonium ion was determined within 2.3 min with a detection limit (S/N=3) better than 0.125 microM. Ammonium ion in rain and river waters was precisely determined using this ion-exclusion chromatographic system.

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

    PubMed

    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.

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

    PubMed

    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.

  11. Large-Scale Synthesis of Highly Luminescent Perovskite-Related CsPb2 Br5 Nanoplatelets and Their Fast Anion Exchange.

    PubMed

    Wang, Kun-Hua; Wu, Liang; Li, Lei; Yao, Hong-Bin; Qian, Hai-Sheng; Yu, Shu-Hong

    2016-07-11

    All-inorganic cesium lead-halide perovskite nanocrystals have emerged as attractive optoelectronic nanomaterials owing to their stabilities and highly efficient photoluminescence. Herein we report a new type of highly luminescent perovskite-related CsPb2 Br5 nanoplatelets synthesized by a facile precipitation reaction. The layered crystal structure of CsPb2 Br5 promoted an anisotropic two-dimensional (2D) crystal growth during the precipitation process, thus enabling the large-scale synthesis of CsPb2 Br5 nanoplatelets. Fast anion exchange has also been demonstrated in as-synthesized CsPb2 Br5 nanoplatelets to extend their photoluminescence spectra to the entire visible spectral region. The large-scale synthesis and optical tunability of CsPb2 Br5 nanoplatelets will be advantageous in future applications of optoelectronic devices. PMID:27213688

  12. Identification of PCR-amplified genetically modified organisms (GMOs) DNA by peptide nucleic acid (PNA) probes in anion-exchange chromatographic analysis.

    PubMed

    Rossi, Stefano; Lesignoli, Francesca; Germini, Andrea; Faccini, Andrea; Sforza, Stefano; Corradini, Roberto; Marchelli, Rosangela

    2007-04-01

    PCR products obtained by selective amplification of transgenic DNA derived from food samples containing Roundup Ready soybean or Bt-176 maize have been analyzed by anion-exchange HPLC. Peptide nucleic acids (PNAs), oligonucleotide analogues known to bind to complementary single-stranded DNA with high affinity and specificity, have been used as specific probes in order to assess the identity of the peaks observed. Two different protocols were adopted in order to obtain single-stranded DNA: amplification with an excess of one primer or digestion of one DNA strand. The single-stranded DNA was mixed with the PNA probe, and the presence of a specific sequence was revealed through detection of the corresponding PNA:DNA peak with significantly different retention time. Advantages and limits of this approach are discussed. The method was tested with reference materials and subsequently applied to commercial samples.

  13. The automated radiosynthesis and purification of the opioid receptor antagonist, [6-O-methyl-11C]diprenorphine on the GE TRACERlab FXFE radiochemistry module.

    PubMed

    Fairclough, Michael; Prenant, Christian; Brown, Gavin; McMahon, Adam; Lowe, Jonathan; Jones, Anthony

    2014-05-15

    [6-O-Methyl-(11)C]diprenorphine ([(11)C]diprenorphine) is a positron emission tomography ligand used to probe the endogenous opioid system in vivo. Diprenorphine acts as an antagonist at all of the opioid receptor subtypes, that is, μ (mu), κ (kappa) and δ (delta). The radiosynthesis of [(11)C]diprenorphine using [(11)C]methyl iodide produced via the 'wet' method on a home-built automated radiosynthesis set-up has been described previously. Here, we describe a modified synthetic method to [(11)C]diprenorphine performed using [(11)C]methyl iodide produced via the gas phase method on a GE TRACERlab FXFE radiochemistry module. Also described is the use of [(11)C]methyl triflate as the carbon-11 methylating agent for the [(11)C]diprenorphine syntheses. [(11)C]Diprenorphine was produced to good manufacturing practice standards for use in a clinical setting. In comparison to previously reported [(11)C]diprenorphine radiosyntheisis, the method described herein gives a higher specific activity product which is advantageous for receptor occupancy studies. The radiochemical purity of [(11)C]diprenorphine is similar to what has been reported previously, although the radiochemical yield produced in the method described herein is reduced, an issue that is inherent in the gas phase radiosynthesis of [(11)C]methyl iodide. The yields of [(11)C]diprenorphine are nonetheless sufficient for clinical research applications. Other advantages of the method described herein are an improvement to both reproducibility and reliability of the production as well as simplification of the purification and formulation steps. We suggest that our automated radiochemistry route to [(11)C]diprenorphine should be the method of choice for routine [(11)C]diprenorphine productions for positron emission tomography studies, and the production process could easily be transferred to other radiochemistry modules such as the TRACERlab FX C pro.

  14. 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.

    PubMed

    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

  15. Selectivity issues in targeted metabolomics: Separation of phosphorylated carbohydrate isomers by mixed-mode hydrophilic interaction/weak anion exchange chromatography.

    PubMed

    Hinterwirth, Helmut; Lämmerhofer, Michael; Preinerstorfer, Beatrix; Gargano, Andrea; Reischl, Roland; Bicker, Wolfgang; Trapp, Oliver; Brecker, Lothar; Lindner, Wolfgang

    2010-11-01

    Phosphorylated carbohydrates are important intracellular metabolites and thus of prime interest in metabolomics research. Complications in their analysis arise from the existence of structural isomers that do have similar fragmentation patterns in MS/MS and are hard to resolve chromatographically. Herein, we present selective methods for the liquid chromatographic separation of sugar phosphates, such as hexose and pentose phosphates, 2- and 3-phosphoglycerate, dihydroxyacetone phosphate and glyceraldehyde 3-phosphate, as well as glucosamine 1- and 6-phosphate utilizing mixed-mode chromatography with reversed-phase/weak anion-exchangers and a charged aerosol detector. The best results were obtained when the reversed-phase/weak anion-exchanger column was operated under hydrophilic interaction liquid chromatography elution conditions. The effects of various chromatographic parameters were examined and are discussed on the basis of a simple stoichiometric displacement model for explaining ion-exchange processes. Employed acidic conditions have led to the complete separation of α- and β-anomers of glucose 6-phosphate at low temperature. The anomers coeluted in a single peak at elevated temperatures (>40°C) (peak coalescence), while at intermediate temperatures on-column interconversion with a plateau in-between resolved anomer peaks was observed with apparent reaction rate constants between 0.1 and 27.8×10(-4) s(-1). Dynamic HPLC under specified conditions enabled to investigate mutarotation of phosphorylated carbohydrates, their interconversion kinetics, and energy barriers for interconversion. A complex mixture of six hexose phosphate structural isomers could be resolved almost completely.

  16. In situ redox speciation analysis of chromium in water by diffusive gradients in thin films using a DE81 anion exchange membrane.

    PubMed

    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

  17. Determination of Cr(VI) in welding fumes by anion-exchange fast protein liquid chromatography with electrothermal atomic absorption spectrometric detection.

    PubMed

    Milacic, Radmila; Scancar, Janez; Tusek, Janez

    2002-02-01

    The applicability of an anion-exchange fast protein liquid chromatographic-electrothermal atomic absorption spectrometric procedure (FPLC-ETAAS) was investigated for the determination of Cr(VI) in welding fumes after alkaline extraction of aerosols loaded on filters. Gas tungsten arc welding (GTAW) of stainless steel was applied. Samples of welding fumes were collected during regular welding on polycarbonate membrane filters of 8 microm and 0.4 microm pore size (inhalable and respirable aerosols). Alkaline extraction (2% NaOH-3% Na2CO3) of filters in a heated ultrasonic bath was applied to leach Cr from the airborne particulate matter. 0.5 cm3 of sample extract was then injected onto an anion-exchange FPLC column. Tris-HCl buffer (0.005 mol dm(-3), pH 8.0) and the same buffer with NaCl (0.5 mol dm(-3)) were employed in gradient elution (15 min, flow rate 1 cm3 min(-1)). The separated Cr species were determined "off line" by ETAAS in 0.5 cm3 fractions. Cr(VI) was reproducibly and quantitatively eluted from 12.0 to 13.0 min with a maximum peak at 12.5 min. Good repeatability of measurement (+/-3.0%) of alkaline extracts was obtained for Cr(VI). The LOD (3s) was found to be 0.035 microg m(-3) Cr(VI), when 2 m3 of aerosols were collected on the filter. Validation of the procedure was performed by spiking alkaline extracts and by the analysis of standard reference material CRM 545, Cr(VI) in welding dust loaded on a filter. The technique was successfully applied for the determination of Cr(VI) in welding fumes.

  18. 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

    PubMed Central

    Druschel, Greg K; Schoonen, Martin AA; Nordstrom, D Kirk; Ball, James W; 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 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 1C 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.

  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

    USGS Publications Warehouse

    Druschel, G.K.; Schoonen, M.A.A.; Nordstorm, D.K.; Ball, J.W.; Xu, Y.; Cohn, C.A.

    2003-01-01

    A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad??? AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab) and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern) and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan). Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad??? AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns. ?? The Royal Society of Chemistry and the Division of Geochemistry of the American Chemical Society 2003.

  20. Integrated DNA and RNA extraction and purification on an automated microfluidic cassette from bacterial and viral pathogens causing community-acquired lower respiratory tract infections.

    PubMed

    Van Heirstraeten, Liesbet; Spang, Peter; Schwind, Carmen; Drese, Klaus S; Ritzi-Lehnert, Marion; Nieto, Benjamin; Camps, Marta; Landgraf, Bryan; Guasch, Francesc; Corbera, Antoni Homs; Samitier, Josep; Goossens, Herman; Malhotra-Kumar, Surbhi; Roeser, Tina

    2014-05-01

    In this paper, we describe the development of an automated sample preparation procedure for etiological agents of community-acquired lower respiratory tract infections (CA-LRTI). The consecutive assay steps, including sample re-suspension, pre-treatment, lysis, nucleic acid purification, and concentration, were integrated into a microfluidic lab-on-a-chip (LOC) cassette that is operated hands-free by a demonstrator setup, providing fluidic and valve actuation. The performance of the assay was evaluated on viral and Gram-positive and Gram-negative bacterial broth cultures previously sampled using a nasopharyngeal swab. Sample preparation on the microfluidic cassette resulted in higher or similar concentrations of pure bacterial DNA or viral RNA compared to manual benchtop experiments. The miniaturization and integration of the complete sample preparation procedure, to extract purified nucleic acids from real samples of CA-LRTI pathogens to, and above, lab quality and efficiency, represent important steps towards its application in a point-of-care test (POCT) for rapid diagnosis of CA-LRTI. PMID:24615272

  1. Purification of infective baculoviruses by monoliths.

    PubMed

    Gerster, Petra; Kopecky, Eva-Maria; Hammerschmidt, Nikolaus; Klausberger, Miriam; Krammer, Florian; Grabherr, Reingard; Mersich, Christa; Urbas, Lidija; Kramberger, Petra; Paril, Tina; Schreiner, Matthias; Nöbauer, Katharina; Razzazi-Fazeli, Ebrahim; Jungbauer, Alois

    2013-05-17

    A chromatographic process based on monoliths for purification of infective baculovirus without prior concentration step has been established. Baculovirus produced in Spodoptera frugiperda cells (Sf-9) were harvested by centrifugation, filtered through 0.8 μm filters and directly loaded onto radial 1 mL anion exchange monoliths with a channel size of 1.5-2.0 μm operated at a volumetric flow rate of one bed volume per minute. Optional an epoxy monolith was used as pre-column to reduce interfering compounds and substances influencing the capacity of anion exchange monoliths for baculovirus infectious virus could be eluted with a step gradient at salt concentrations of 440 mM NaCl. Recovery of infectious virus was highly influenced by composition and age of supernatant and ranged from 20 to >99% active baculovirus. Total protein content could be reduced to 1-8% and DNA content to 38-48% in main virus fraction. Infective virus could be 52-fold concentrated within 20.5h and simultaneously an 82-fold volume reduction was possible when loading 1150 mL (2.1×10(8) pfu/mL) onto 1 mL scale support.

  2. Automated gas-phase purification for accurate, multiplexed quantification on a stand-alone ion trap mass spectrometer

    PubMed Central

    Vincent, Catherine E.; Rensvold, Jarred W.; Westphall, Michael S.; Pagliarini, David J.; Coon, Joshua J.

    2012-01-01

    Isobaric tagging enables the acquisition of highly-multiplexed proteome quantification but is hindered by the pervasive problem of precursor interference. The elimination of co-isolated contaminants prior to reporter tag generation can be achieved through the use of gas-phase purification via proton transfer ion/ion reactions (QuantMode); however, the original QuantMode technique was implemented on the high resolution linear ion trap-Orbitrap hybrid mass spectrometer enabled with electron transfer dissociation (ETD). Here we extend this technology to stand-alone linear ion trap systems (trapQuantMode). Facilitated by the use of inlet beam-type activation (i.e., trapHCD) for production and observation of the low mass-to-charge reporter region, this scan sequence comprises three separate events to maximize peptide identifications, minimize duty cycle requirements, and increase quantitative accuracy, precision, and dynamic range. Significant improvements in quantitative accuracy were attained over standard methods when using trapQuantMode (trapQM) to analyze an interference model system comprising tryptic peptides of yeast that we contaminated with human peptides. Finally, we demonstrate practical benefits of this method by analysis of the proteomic changes that occur during mouse skeletal muscle myoblast differentiation. While trapQM’s reduced duty cycle led to the identification of fewer proteins than conventional operation (4,050 vs. 2,964), trapQM identified more significant differences (>1.5 fold, 1,362 vs 1,132, respectively; P<0.05) between the proteomes of undifferentiated myoblasts and differentiated myotubes and nearly ten-fold more differences with changes greater than 5-fold (96 vs. 12). We further show that our trapQM dataset is superior for identifying changes in protein abundance that are consistent with the metabolic and structural changes known to accompany myotube formation. PMID:23046161

  3. Evidence of a Structural and Functional Ammonium Transporter RhBG·Anion Exchanger 1·Ankyrin-G Complex in Kidney Epithelial Cells*

    PubMed Central

    Genetet, Sandrine; Ripoche, Pierre; Le Van Kim, Caroline; Colin, Yves; Lopez, Claude

    2015-01-01

    The renal ammonium transporter RhBG and anion exchanger 1 kAE1 colocalize in the basolateral domain of α-intercalated cells in the distal nephron. Although we have previously shown that RhBG is linked to the spectrin-based skeleton through ankyrin-G and that its NH3 transport activity is dependent on this association, there is no evidence for an interaction of kAE1 with this adaptor protein. We report here that the kAE1 cytoplasmic N terminus actually binds to ankyrin-G, both in yeast two-hybrid analysis and by coimmunoprecipitation in situ in HEK293 cells expressing recombinant kAE1. A site-directed mutagenesis study allowed the identification of three dispersed regions on kAE1 molecule linking the third and fourth repeat domains of ankyrin-G. One secondary docking site corresponds to a major interacting loop of the erythroid anion exchanger 1 (eAE1) with ankyrin-R, whereas the main binding region of kAE1 does not encompass any eAE1 determinant. Stopped flow spectrofluorometry analysis of recombinant HEK293 cells revealed that the Cl−/HCO3− exchange activity of a kAE1 protein mutated on the ankyrin-G binding site was abolished. This disruption impaired plasma membrane expression of kAE1 leading to total retention on cytoplasmic structures in polarized epithelial Madin-Darby canine kidney cell transfectants. kAE1 also directly interacts with RhBG without affecting its surface expression and NH3 transport function. This is the first description of a structural and functional RhBG·kAE1·ankyrin-G complex at the plasma membrane of kidney epithelial cells, comparable with the well known Rh·eAE1·ankyrin-R complex in the red blood cell membrane. This renal complex could participate in the regulation of acid-base homeostasis. PMID:25616663

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

    PubMed

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

    2013-01-01

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

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

    PubMed

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

    2013-01-01

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

  6. Mixed-mode isolation of triazine metabolites from soil and aquifer sediments using automated solid-phase extraction

    USGS Publications Warehouse

    Mills, M.S.; Thurman, E.M.

    1992-01-01

    Reversed-phase isolation and ion-exchange purification were combined in the automated solid-phase extraction of two polar s-triazine metabolites, 2-amino-4-chloro-6-(isopropylamino)-s-triazine (deethylatrazine) and 2-amino-4-chloro-6-(ethylamino)-s-triazine (deisopropylatrazine) from clay-loam and slit-loam soils and sandy aquifer sediments. First, methanol/ water (4/1, v/v) soil extracts were transferred to an automated workstation following evaporation of the methanol phase for the rapid reversed-phase isolation of the metabolites on an octadecylresin (C18). The retention of the triazine metabolites on C18 decreased substantially when trace methanol concentrations (1%) remained. Furthermore, the retention on C18 increased with decreasing aqueous solubility and increasing alkyl-chain length of the metabolites and parent herbicides, indicating a reversed-phase interaction. The analytes were eluted with ethyl acetate, which left much of the soil organic-matter impurities on the resin. Second, the small-volume organic eluate was purified on an anion-exchange resin (0.5 mL/min) to extract the remaining soil pigments that could foul the ion source of the GC/MS system. Recoveries of the analytes were 75%, using deuterated atrazine as a surrogate, and were comparable to recoveries by soxhlet extraction. The detection limit was 0.1 ??g/kg with a coefficient of variation of 15%. The ease and efficiency of this automated method makes it viable, practical technique for studying triazine metabolites in the environment.

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

    PubMed Central

    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

  8. A Pd/C-CeO2 Anode Catalyst for High-Performance Platinum-Free Anion Exchange Membrane Fuel Cells.

    PubMed

    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) . PMID:27062251

  9. Advanced treatment of textile dyeing secondary effluent using magnetic anion exchange resin and its effect on organic fouling in subsequent RO membrane.

    PubMed

    Yang, Cheng; Li, Li; Shi, Jialu; Long, Chao; Li, Aimin

    2015-03-01

    Strict regulations are forcing dyeing factory to upgrade existing waste treatment system. In this study, advanced treatment of dyeing secondary effluent by magnetic anion exchange resin (NDMP) was investigated and compared with ultrafiltration (UF); NDMP as a pre-treatment of reverse osmosis (RO) was also studied. NDMP resin (20 mL/L) gave higher removal of dissolved organic carbon (DOC) (83.9%) and colority (94.9%) than UF with a cut-off of 10 kDa (only 48.6% and 44.1%, respectively), showing that NDMP treatment was effective to meet the stringent discharge limit of DOC and colority. Besides, NDMP resin (20 mL/L) as a pretreatment of RO increased the permeate flux by 12.5% and reduced irreversible membrane fouling by 6.6%, but UF pretreatment did not mitigate RO membrane fouling. The results of excitation-emission matrix fluorescence spectra and resin fractions showed that NDMP had more efficient removal than UF for transphilic acid and hydrophilic fraction, such as protein-like organic matters and soluble microbial products, which contributed to a significant proportion of RO membrane fouling. In sum, NDMP resin treatment not only gave effective removal of DOC and colority of dyeing secondary effluent, but exhibited some improvement for RO membrane flux and irreversible fouling. PMID:25463217

  10. Interplay between water uptake, ion interactions, and conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) anion exchange membrane

    SciTech Connect

    Pandey, Tara P.; Maes, Ashley M.; Sarode, Himanshu N.; Peters, Bethanne D.; Lavina, Sandra; Vezzu, Keti; Yang, Yuan; Poynton, Simon D.; Varcoe, John R.; Seifert, Soenke; Liberatore, Matthew W.; Di Noto, Vito; Herring, Andrew M.

    2014-12-23

    We demonstrate that the true hydroxide conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) [ETFE] anion exchange membrane (AEM) is as high as 132 mS cm-1 at 80 °C and 95% RH, comparable to a proton exchange membrane, but with very much less water present in the film. To understand this behaviour we studied ion transport of hydroxide, carbonate, bicarbonate and chloride, as well as water uptake and distribution. Water uptake of the AEM in water vapor is an order of magnitude lower than when submerged in liquid water. In addition 19F pulse field gradient spin echo NMR indicates that there is little tortuosity in the ionic pathways through the film. A complete analysis of the IR spectrum of the AEM and the analyses of water absorption using FT-IR led to conclusion that the fluorinated backbone chains do not interact with water and that two types of water domains exist within the membrane. Furthermore, the reduction in conductivity was measured during exposure of the OH- form of the AEM to air at 95% RH and was seen to be much slower than the reaction of CO2 with OH- as the amount of water in the film determines its ionic conductivity and at relative wet RHs its re-organization is slow.

  11. Trafficking defect of mutant kidney anion exchanger 1 (kAE1) proteins associated with distal renal tubular acidosis and Southeast Asian ovalocytosis.

    PubMed

    Sawasdee, Nunghathai; Udomchaiprasertkul, Wandee; Noisakran, Sansanee; Rungroj, Nanyawan; Akkarapatumwong, Varaporn; Yenchitsomanus, Pa-thai

    2006-11-24

    Compound heterozygous anion exchanger 1 (AE1) SAO/G701D mutations result in distal renal tubular acidosis with Southeast Asian ovalocytosis. Interaction, trafficking and localization of wild-type and mutant (SAO and G701D) kAE1 proteins fused with hemagglutinin, six-histidine, Myc, or green fluorescence protein (GFP) were examined in human embryonic kidney (HEK) 293 cells. When individually expressed, wild-type kAE1 was localized at cell surface while mutant kAE1 SAO and G701D were intracellularly retained. When co-expressed, wild-type kAE1 could form heterodimer with kAE1 SAO or kAE1 G701D and could rescue mutant kAE1 proteins to express on the cell surface. Co-expression of kAE1 SAO and kAE1 G701D also resulted in heterodimer formation but intracellular retention without cell surface expression, suggesting their trafficking defect and failure to rescue each other to the plasma membrane, most likely the molecular mechanism of the disease in the compound heterozygous condition. PMID:17027918

  12. Interplay between water uptake, ion interactions, and conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) anion exchange membrane

    DOE PAGES

    Pandey, Tara P.; Maes, Ashley M.; Sarode, Himanshu N.; Peters, Bethanne D.; Lavina, Sandra; Vezzu, Keti; Yang, Yuan; Poynton, Simon D.; Varcoe, John R.; Seifert, Soenke; et al

    2014-12-23

    We demonstrate that the true hydroxide conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) [ETFE] anion exchange membrane (AEM) is as high as 132 mS cm-1 at 80 °C and 95% RH, comparable to a proton exchange membrane, but with very much less water present in the film. To understand this behaviour we studied ion transport of hydroxide, carbonate, bicarbonate and chloride, as well as water uptake and distribution. Water uptake of the AEM in water vapor is an order of magnitude lower than when submerged in liquid water. In addition 19F pulse field gradient spin echo NMR indicates that there ismore » little tortuosity in the ionic pathways through the film. A complete analysis of the IR spectrum of the AEM and the analyses of water absorption using FT-IR led to conclusion that the fluorinated backbone chains do not interact with water and that two types of water domains exist within the membrane. Furthermore, the reduction in conductivity was measured during exposure of the OH- form of the AEM to air at 95% RH and was seen to be much slower than the reaction of CO2 with OH- as the amount of water in the film determines its ionic conductivity and at relative wet RHs its re-organization is slow.« less

  13. New reversed-phase/anion-exchange/hydrophilic interaction mixed-mode stationary phase based on dendritic polymer-modified porous silica.

    PubMed

    Li, Yun; Yang, Jiajia; Jin, Jing; Sun, Xiaoli; Wang, Longxing; Chen, Jiping

    2014-04-11

    A novel dendritic polymer-modified silica (DPS) stationary phase was prepared by a divergent synthesis scheme starting from propylamine on silica by consecutive amine-epoxy reactions with 1,4-butanedioldiglycidyl ether and aniline. Both elemental analysis and infrared spectra data shows the successful growth of dendritic polymer on silica particles. The carbon and nitrogen contents increased with an increasing number of reaction cycles and achieved 25.2% and 2.1% (w/w) after 11 reaction cycles. The combination of a phenyl ring with a quaternary ammonium, or a tertiary amine at the branch point along with embedded polar functionalities (including ether and hydroxyl groups) in the branch, generated hydrophobic, electrostatic, as well as hydrophilic interactive domains. Depending on solute structure and mobile phase composition, the DPS stationary phase provided multiple retention mechanisms, including reversed phase (RP), anion-exchange (AEX), and hydrophilic interactions. The RP capability achieved separation of polycyclic aromatic hydrocarbons. Basic, neutral and acidic molecules were well separated under RP/AEX mixed mode. Effective separation of small polar compounds (such as nucleobases and nucleosides) was also obtained under hydrophilic interaction liquid chromatography (HILIC) mode. PMID:24630062

  14. A Pd/C-CeO2 Anode Catalyst for High-Performance Platinum-Free Anion Exchange Membrane Fuel Cells.

    PubMed

    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) .

  15. Anion-Exchange Induced Strong π-π Interactions in Single Crystalline Naphthalene Diimide for Nitroexplosive Sensing: An Electronic Prototype for Visual on-Site Detection.

    PubMed

    Kalita, Anamika; Hussain, Sameer; Malik, Akhtar Hussain; Barman, Ujjwol; Goswami, Namami; Iyer, Parameswar Krishnan

    2016-09-28

    A new derivative of naphthalene diimide (NDMI) was synthesized that displayed optical, electrical, and visual changes exclusively for the most widespread nitroexplosive and highly water-soluble toxicant picric acid (PA) due to strong π-π interactions, dipole-charge interaction, and a favorable ground state electron transfer process facilitated by Coulombic attraction. The sensing mechanism and interaction between NDMI with PA is demonstrated via X-ray diffraction analysis, (1)H NMR studies, cyclic voltammetry, UV-visible/fluorescence spectroscopy, and lifetime measurements. Single crystal X-ray structure of NDMI revealed the formation of self-assembled crystalline network assisted by noncovalent C-H···I interactions that get disrupted upon introducing PA as a result of anion exchange and strong π-π stacking between NDMI and PA. Morphological studies of NDMI displayed large numbers of single crystalline microrods along with some three-dimensional (3D) daisy-like structures which were fabricated on Al-coated glass substrate to construct a low-cost two terminal sensor device for realizing vapor mode detection of PA at room temperature and under ambient conditions. Furthermore, an economical and portable electronic prototype was developed for visual and on-site detection of PA vapors under exceptionally realistic conditions.

  16. One-step isolation of adenosine triphosphate from crude fermentation broth of Saccharomyces cerevisiae by anion-exchange chromatography using supermacroporous cryogel.

    PubMed

    Yun, Junxian; Shen, Shaochuan; Chen, Fang; Yao, Kejian

    2007-12-01

    Adenosine triphosphate (ATP) is an important high-energy compound widely used in biological and therapeutic fields. It can be produced by phosphorylation of adenosine monophosphate (AMP) with microbial cells in industrial scale and the effective isolation of ATP from microbial fermentation broth is a challenging work. In this work, we develop a novel one-step method to directly separate ATP from fermentation broth of Saccharomyces cerevisiae by anion-exchange chromatography using supermacroporous cryogel. The cryogel bed with tertiary amine groups was prepared by grafting N,N-dimethylaminoethyl methacrylate (DMAEMA) monomer chains onto the matrix of a polyacrylamide-based cryogel in a glass column and its properties of liquid dispersion, water permeability, porosity as well as the ligand density were measured. Chromatographic separation of ATP from the fermentation broth by the cryogel was carried out using deionised water and 0.01 M HCl as running buffer, respectively. The breakthrough characteristics and elution performance in the cryogel bed were revealed and analyzed. The purities of the obtained ATP were analyzed quantitatively by high performance liquid chromatography (HPLC). The maximal purity of ATP by the one-step separation method was 95.5% using 0.01 M HCl as running buffer in this work. The corresponding chromatographic behaviors were investigated and analyzed.

  17. Glycosylation of alpha1-acid glycoprotein in inflammatory disease: analysis by high-pH anion-exchange chromatography and concanavalin A crossed affinity immunoelectrophoresis.

    PubMed

    Rydén, I; Skude, G; Lundblad, A; Påhlsson, P

    1997-06-01

    High-pH anion-exchange chromatography with pulsed amperometric detection is a highly sensitive technique that can be used for detecting changes in sialylation and fucosylation, as well as different branching patterns of N-linked oligosaccharides in glycoproteins. We examined the N-glycans of alpha1-acid glycoprotein obtained from twelve patients with various inflammatory conditions with this technique, as well as traditional concanavalin A crossed affinity immunoelectrophoresis. We found the chromatographic profiles of N-glycans in all patients with rheumatoid arthritis to be very similar, but significantly different from normal controls. N-glycans from patients with ulcerative colitis also showed specific alterations in their chromatographic profiles. However, some heterogeneity was found between these patients, perhaps reflecting changes in glycosylation secondary to certain states of the disease, or to medical treatment. We conclude that this technique is useful for detailed mapping of glycosylation changes in alpha1-acid glycoprotein in clinical samples, and that it may be used to further increase our knowledge about glycosylation changes in response to inflammatory disease.

  18. Durability and performance of polystyrene- b -poly(vinylbenzyl trimethylammonium) diblock copolymer and equivalent blend anion exchange membranes

    SciTech Connect

    Vandiver, Melissa A.; Caire, Benjamin R.; Poskin, Zach; Li, Yifan; Seifert, Sönke; Knauss, Daniel M.; Herring, Andrew M.; Liberatore, Matthew W.

    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.

  19. An efficient method for decoloration of polysaccharides from the sprouts of Toona sinensis (A. Juss.) Roem by anion exchange macroporous resins.

    PubMed

    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

  20. X-ray Lithography on Perovskite Nanocrystals Films: From Patterning with Anion-Exchange Reactions to Enhanced Stability in Air and Water

    PubMed Central

    2015-01-01

    Films of colloidal CsPbX3 (X = I, Br or Cl) nanocrystals, prepared by solution drop-casting or spin-coating on a silicon substrate, were exposed to a low flux of X-rays from an X-ray photoelectron spectrometer source, causing intermolecular C=C bonding of the organic ligands that coat the surface of the nanocrystals. This transformation of the ligand shell resulted in a greater stability of the film, which translated into the following features: (i) Insolubility of the exposed regions in organic solvents which caused instead complete dissolution of the unexposed regions. This enabled the fabrication of stable and strongly fluorescent patterns over millimeter scale areas. (ii) Inhibition of the irradiated regions toward halide anion exchange reactions, when the films were exposed either to halide anions in solution or to hydrohalic vapors. This feature was exploited to create patterned regions of different CsPbIxBryClz compositions, starting from a film with homogeneous CsPbX3 composition. (iii) Resistance of the films to degradation caused by exposure to air and moisture, which represents one of the major drawbacks for the integration of these materials in devices. (iv) Stability of the film in water and biological buffer, which can open interesting perspectives for applications of halide perovskite nanocrystals in aqueous environments. PMID:26617344

  1. Interplay between water uptake, ion interactions, and conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) anion exchange membrane

    DOE PAGES

    Pandey, Tara P.; Maes, Ashley M.; Sarode, Himanshu N.; Peters, Bethanne D.; Lavina, Sandra; Vezzù, Keti; Yang, Yuan; Poynton, Simon D.; Varcoe, John R.; Seifert, Soenke; et al

    2014-12-23

    We demonstrate that the true hydroxide conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) [ETFE] anion exchange membrane (AEM) is as high as 132 mS cm-1 at 80 °C and 95% RH, comparable to a proton exchange membrane, but with very much less water present in the film. To understand this behaviour we studied ion transport of hydroxide, carbonate, bicarbonate and chloride, as well as water uptake and distribution. Water uptake of the AEM in water vapor is an order of magnitude lower than when submerged in liquid water. In addition 19F pulse field gradient spin echo NMR indicates that there ismore » little tortuosity in the ionic pathways through the film. A complete analysis of the IR spectrum of the AEM and the analyses of water absorption using FT-IR led to conclusion that the fluorinated backbone chains do not interact with water and that two types of water domains exist within the membrane. The reduction in conductivity was measured during exposure of the OH- form of the AEM to air at 95% RH and was seen to be much slower than the reaction of CO2 with OH- as the amount of water in the film determines its ionic conductivity and at relative wet RHs its re-organization is slow.« less

  2. Imidazolium-Functionalized Poly(arylene ether sulfone) Anion-Exchange Membranes Densely Grafted with Flexible Side Chains for Fuel Cells.

    PubMed

    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

  3. Advanced treatment of textile dyeing secondary effluent using magnetic anion exchange resin and its effect on organic fouling in subsequent RO membrane.

    PubMed

    Yang, Cheng; Li, Li; Shi, Jialu; Long, Chao; Li, Aimin

    2015-03-01

    Strict regulations are forcing dyeing factory to upgrade existing waste treatment system. In this study, advanced treatment of dyeing secondary effluent by magnetic anion exchange resin (NDMP) was investigated and compared with ultrafiltration (UF); NDMP as a pre-treatment of reverse osmosis (RO) was also studied. NDMP resin (20 mL/L) gave higher removal of dissolved organic carbon (DOC) (83.9%) and colority (94.9%) than UF with a cut-off of 10 kDa (only 48.6% and 44.1%, respectively), showing that NDMP treatment was effective to meet the stringent discharge limit of DOC and colority. Besides, NDMP resin (20 mL/L) as a pretreatment of RO increased the permeate flux by 12.5% and reduced irreversible membrane fouling by 6.6%, but UF pretreatment did not mitigate RO membrane fouling. The results of excitation-emission matrix fluorescence spectra and resin fractions showed that NDMP had more efficient removal than UF for transphilic acid and hydrophilic fraction, such as protein-like organic matters and soluble microbial products, which contributed to a significant proportion of RO membrane fouling. In sum, NDMP resin treatment not only gave effective removal of DOC and colority of dyeing secondary effluent, but exhibited some improvement for RO membrane flux and irreversible fouling.

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

    SciTech Connect

    Doucet, L.; De Veyrac, B.; Delaage, M.; Cailla, H.; Bernheim, C.; Devissaguet, M. )

    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.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  7. Preparing alkaline anion exchange membrane with enhanced hydroxide conductivity via blending imidazolium-functionalized and sulfonated poly(ether ether ketone)

    NASA Astrophysics Data System (ADS)

    Li, Zhen; Jiang, Zhongyi; Tian, Huimin; Wang, Siwen; Zhang, Bei; Cao, Ying; He, Guangwei; Li, Zongyu; Wu, Hong

    2015-08-01

    The development of alkaline anion exchange membrane (AEM) with both high ion conductivity and stabilities is of great significance for fuel cell applications. In this study, a facile acid-base blending method is designed to improve AEM performances. Basic imidazolium-functionalized poly (ether ether ketone) with a high functionalization degree is employed as polymer matrix to pursue high ion-exchange capacity (IEC) as well as high hydroxide conductivity, meanwhile acidic sulfonated poly (ether ether ketone) (SPEEK) is employed as the cross-linking agent to enhance the stabilities of the blend membranes. Particularly, an in-situ Menshutkin/crosslinking method is exploited to prevent the flocculation in the preparation process of blend membranes. As a result, dense and defect-free blend membranes are obtained. The blend membranes exhibit high level of IEC up to 3.15 mmol g-1, and consequently possess elevated hydroxide conductivity up to 31.59 mS cm-1 at 30 °C. In addition, benefiting from the strong electrostatic interaction introduced by the acid-base blending, the stabilities and methanol resistance of blend membranes are enhanced.

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

    PubMed

    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

  9. The effects of ionizing radiation on Reillex trademark HPQ, a new macroporous polyvinylpyridine resin, and on four conventional polystyrene anion exchange resins

    SciTech Connect

    Marsh, S.F.

    1990-11-01

    This study compares the effects of ionizing radiation on Reillex{trademark} HPQ, a recently available macroporous copolymer of 1-methyl-4-vinylpyridine/divinylbenzene, and on four conventional strong-base polystyrene anion exchange resins. The polystyrene resins investigated included one gel type, Dowex{trademark} 1 {times} 4, and three macroporous resins: Dow{trademark} MSA-1, Amberlite{trademark} IRA-900, and Lewatit{trademark} MP-500-FK. Each resin, in 7 M nitric acid, was subjected to seven different levels of {sup 60}Co gamma radiation ranging from 100 to 1000 megarads. Irradiated resins were measured for changes in dry weight, wet volume, chloride and Pu(IV) exchange capacities, and thermal stability. In separate experiments, each resin was subjected to approximately 340 megarads of in situ alpha particles from sorbed plutonium. Resin damage from alpha particles was less than half that caused by gamma rays, which may be a consequence of different production rates of radiolytic nitrite and nitro radicals in the two systems. Reillex{trademark} HPQ resin provided the greatest radiation stability, whereas Lewatit{trademark} MP-500-FK was the least stable of the resins tested. Thermogravimetric analyses of dry, nitrate-form resin revealed that dry Reillex{trademark} HPQ resin offered the best thermal stability for absorbed gamma doses to 370 megarads, but the worst thermal stability after exposures of 550 megarads or more. 25 refs., 11 figs., 13 tabs.

  10. Simultaneous analysis of acetaminophen, p-aminophenol and aspirin metabolites by hydrophilic interaction and strong anion exchange capillary liquid chromatography coupled to amperometric detection.

    PubMed

    Zheng, Minmin; Wu, Yimin; Lu, Lanxiang; Ding, Kang; Tang, Fengxiang; Lin, Zian; Wu, Xiaoping

    2011-08-01

    A simple and sensitive method has been developed for the simultaneous determination of polar nonsteroidal pharmaceuticals and metabolites, including acetaminophen, p-aminophenol and several aspirin metabolites (salicylic acid, gentisic acid, salicyluric acid and 2,3-dihydroxybenzoic acid), by capillary liquid chromatography with amperometric detection. Using a capillary monolithic column with mixed mode stationary phases and a mobile phase composed of acetonitrile and Tris buffer, rapid separation of six polar analytes was achieved within 8 min, and a hydrophilic interaction and strong anion exchange separation mechanism were exhibited. Method detection limits of six analytes ranged from 10 to 50 ng/mL. In terms of precision, the intra- and interday relative standard deviation values in all analytes never exceeded 3.1% for migration time and 8.9% for peak areas, respectively. This method provided a simple, rapid and cost-effective approach for the analysis of polar pharmaceuticals. The applicability of the method in pharmacokinetics was verified by spiking human serum samples with the compounds and analyzing the recoveries. PMID:21644253

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

    PubMed

    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.

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

    PubMed

    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.

  13. Anion exchange membrane prepared from simultaneous polymerization and quaternization of 4-vinyl pyridine for non-aqueous vanadium redox flow battery applications

    NASA Astrophysics Data System (ADS)

    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.

  14. Cross-Linked Quaternized Poly(styrene-b-(ethylene-co-butylene)-b-styrene) for Anion Exchange Membrane: Synthesis, Characterization and Properties.

    PubMed

    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

  15. Interplay between water uptake, ion interactions, and conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) anion exchange membrane

    SciTech Connect

    Pandey, Tara P.; Maes, Ashley M.; Sarode, Himanshu N.; Peters, Bethanne D.; Lavina, Sandra; Vezzù, Keti; Yang, Yuan; Poynton, Simon D.; Varcoe, John R.; Seifert, Soenke; Liberatore, Matthew W.; Di Noto, Vito; Herring, Andrew M.

    2014-12-23

    We demonstrate that the true hydroxide conductivity in an e-beam grafted poly(ethylene-co-tetrafluoroethylene) [ETFE] anion exchange membrane (AEM) is as high as 132 mS cm-1 at 80 °C and 95% RH, comparable to a proton exchange membrane, but with very much less water present in the film. To understand this behaviour we studied ion transport of hydroxide, carbonate, bicarbonate and chloride, as well as water uptake and distribution. Water uptake of the AEM in water vapor is an order of magnitude lower than when submerged in liquid water. In addition 19F pulse field gradient spin echo NMR indicates that there is little tortuosity in the ionic pathways through the film. A complete analysis of the IR spectrum of the AEM and the analyses of water absorption using FT-IR led to conclusion that the fluorinated backbone chains do not interact with water and that two types of water domains exist within the membrane. The reduction in conductivity was measured during exposure of the OH- form of the AEM to air at 95% RH and was seen to be much slower than the reaction of CO2 with OH- as the amount of water in the film determines its ionic conductivity and at relative wet RHs its re-organization is slow.

  16. Assembly of graphene and nickel nanoparticles on anion exchange resin microspheres for the amperometric detection of carbohydrates in combination with capillary electrophoresis.

    PubMed

    Zhang, Ren; Lu, Sijie; Zhang, Luyan; Chen, Gang

    2014-12-29

    Graphene and nickel nanoparticles (NiNPs) were assembled on anion exchange resin (AER) microspheres based on the electrostatic interaction between graphene oxide sheets and AER and the subsequent chemical reduction. The prepared AER@graphene-NiNP composite core-shell microspheres were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. Moreover, they were embedded in the bores of pipette tips to fabricate electrodes. The performance of the novel electrodes was demonstrated by measuring sucrose, glucose and fructose in combination with capillary electrophoresis. The three analytes were well separated within 8min in a 40cm long capillary at a separation voltage of 12kV. The graphene-NiNP composite microsphere electrodes exhibited higher sensitivity (213.578-317.064nAmM(-1)), lower detection limits (0.75-1.05μM) and enhanced separation efficiency in the detection of these carbohydrates. The advantages of the electrodes include ease of fabrication, low cost and pronounced electrocatalytic activity toward carbohydrates, indicating great promise for a wide range of applications.

  17. On-line anion exchange solid-phase extraction coupled to liquid chromatography with fluorescence detection to determine quinolones in water and human urine.

    PubMed

    Lara, Francisco J; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M

    2013-10-01

    An analytical method based on on-line solid-phase extraction coupled to liquid chromatography with fluorescence detection has been developed to determine quinolones in tap water and human urine. A home-made setup was used to percolate 10 mL of sample through a solid-phase extraction column. Analytes were retained onto the sorbent by an anion exchange mechanism which ensures an optimum compatibility with the subsequent chromatographic separation. A C-18 column containing core-shell particles (2.6 μm) was used to achieve peak efficiencies up to 200,000 plates/m, at a flow rate of 1.2 mL/min and without the need for special pumps. The method allowed the determination of 11 quinolones directly in tap water samples in less than 20 min and with limits of detection ranging between 7 and 110 ng/L. The sensitivity achieved made possible the direct determination of 9 quinolones in human urine without any sample treatment, just dilution with water. Relative recoveries between 94 and 109% were obtained meaning that the matrix effect in human urine is negligible after dilution. Satisfactory results were also obtained in terms of precision since relative standard deviations were always below 13%. PMID:23992844

  18. One-step isolation of adenosine triphosphate from crude fermentation broth of Saccharomyces cerevisiae by anion-exchange chromatography using supermacroporous cryogel.

    PubMed

    Yun, Junxian; Shen, Shaochuan; Chen, Fang; Yao, Kejian

    2007-12-01

    Adenosine triphosphate (ATP) is an important high-energy compound widely used in biological and therapeutic fields. It can be produced by phosphorylation of adenosine monophosphate (AMP) with microbial cells in industrial scale and the effective isolation of ATP from microbial fermentation broth is a challenging work. In this work, we develop a novel one-step method to directly separate ATP from fermentation broth of Saccharomyces cerevisiae by anion-exchange chromatography using supermacroporous cryogel. The cryogel bed with tertiary amine groups was prepared by grafting N,N-dimethylaminoethyl methacrylate (DMAEMA) monomer chains onto the matrix of a polyacrylamide-based cryogel in a glass column and its properties of liquid dispersion, water permeability, porosity as well as the ligand density were measured. Chromatographic separation of ATP from the fermentation broth by the cryogel was carried out using deionised water and 0.01 M HCl as running buffer, respectively. The breakthrough characteristics and elution performance in the cryogel bed were revealed and analyzed. The purities of the obtained ATP were analyzed quantitatively by high performance liquid chromatography (HPLC). The maximal purity of ATP by the one-step separation method was 95.5% using 0.01 M HCl as running buffer in this work. The corresponding chromatographic behaviors were investigated and analyzed. PMID:18024244

  19. Imidazolium-Functionalized Poly(arylene ether sulfone) Anion-Exchange Membranes Densely Grafted with Flexible Side Chains for Fuel Cells.

    PubMed

    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.

  20. Phenolphthalein-based Poly(arylene ether sulfone nitrile)s Multiblock Copolymers As Anion Exchange Membranes for Alkaline Fuel Cells.

    PubMed

    Lai, Ao Nan; Wang, Li Sha; Lin, Chen Xiao; Zhuo, Yi Zhi; Zhang, Qiu Gen; Zhu, Ai Mei; Liu, Qing Lin

    2015-04-22

    A series of phenolphthalein-based poly(arylene ether sulfone nitrile)s (PESN) multiblock copolymers containing 1-methylimidazole groups (ImPESN) were synthesized to prepare anion exchange membranes (AEMs) for alkaline fuel cells. The ion groups were introduced selectively and densely on the unit of phenolphthalein as the hydrophilic segments, allowing for the formation of ion clusters. Strong polar nitrile groups were introduced into the hydrophobic segments with the intention of improving the dimensional stability of the AEMs. A well-controlled multiblock structure was responsible for the well-defined hydrophobic/hydrophilic phase separation and interconnected ion-transport channels, as confirmed by atomic force microscopy and small angle X-ray scattering. The ImPESN membranes with low swelling showed a relatively high water uptake, high hydroxide ion conductivity together with good mechanical, thermal and alkaline stability. The ionic conductivity of the membranes was in the range of 3.85-14.67×10(-2) S·cm(-1) from 30 to 80 °C. Moreover, a single H2/O2 fuel cell with the ImPESN membrane showed an open circuit voltage of 0.92 V and a maximum power density of 66.4 mW cm(-2) at 60 °C.

  1. Minicircle DNA purification using a CIM® DEAE-1 monolithic support.

    PubMed

    Diamantino, Tatiana; Pereira, Patrícia; Queiroz, João A; Sousa, Ângela; Sousa, Fani

    2016-09-01

    Minicircle DNA is a new biotechnological product with beneficial therapeutic perspectives for gene therapy because it is constituted only by the eukaryotic transcription unit. These features improve minicircle DNA safety and increase its therapeutic effect. However, being a recently developed product, there is a need to establish efficient purification methodologies, enabling the recovery of the supercoiled minicircle DNA isoform. Thus, this work describes the minicircle DNA purification using an anion exchange monolithic support. The results show that with this column it is possible to achieve a good selectivity, which allows the isolation of the supercoiled minicircle DNA isoform from impurities. Overall, this study shows a promising approach to obtain the minicircle DNA sample with adequate quality for future therapeutic applications. PMID:27600622

  2. Purification process of recombinant monoclonal antibodies with mixed mode chromatography.

    PubMed

    Maria, Sophie; Joucla, Gilles; Garbay, Bertrand; Dieryck, Wilfrid; Lomenech, Anne-Marie; Santarelli, Xavier; Cabanne, Charlotte

    2015-05-01

    An innovative process to purify mAb from CHO cell culture supernatant was developed. This three-step process involved two mixed mode resins and an anion exchange membrane. We used a human IgG mixture to determine the optimal conditions for each purification step. Thereafter, the whole process was evaluated and improved for the purification of a recombinant mAb produced in the supernatant of CHO cells. Once optimized, yield and purity of 88% and 99.9%, respectively were comparable to those obtained in a conventional process based on a capture step using protein A. In addition, aggregates, HCPs and DNA levels in the purified fraction were below regulatory specifications. Then we used mass spectrometry to identify contaminating proteins in the antibody fraction in order to highlight the behavior of HCPs.

  3. Studies of removal of platinum(IV) ion microquantities from the model solutions of aluminium, copper, iron, nickel and zinc chloride macroquantities on the anion exchanger Duolite S 37.

    PubMed

    Hubicki, Z; Wójcik, G

    2006-08-25

    Platinum has been widely applied in catalytic industry and the recovery of noble metals from industrial wastes becomes an economic issue. The laboratory studies of platinum(IV) microquantities removal from 1M aluminium, copper, iron, nickel and zinc chloride solutions in 0.1M hydrochloric acid solutions on the anion exchanger Duolite S 37 of the functional secondary and tertiary amine groups were carried out. For this anion exchanger the fraction extracted values (%E, Pt(IV)) as well as the sorption isotherms were determined depending on the kind of aqueous phase and phase contact time. Moreover, the bed and weight distribution coefficients as well as working and total ion-exchange capacities were calculated from the platinum(IV) breakthrough curves. Kinetic parameters were determined. PMID:16469435

  4. Effects of the transport site conformation on the binding of external NAP-taurine to the human erythrocyte anion exchange system: evidence for intrinsic asymmetry

    SciTech Connect

    Knauf, P.A.; Law, F.Y.; Tarshis, T.; Furuya, W.

    1984-05-01

    External N-(4-azido (NAP-taurine) inhibits human red cell chloride exchange by binding to a site that is distinct from the chloride transport site. Increases in the intracellular chloride concentration (at constant external chloride) cause an increase in the inhibitory potency of external NAP-taurine. This effect is not due to the changes in pH or membrane potential that usually accompany a chloride gradient, since even when these changes are reversed or eliminated the inhibitory potency remains high. According to the ping-pong model for anion exchange, such transmembrane effects of intracellular chloride on external NAP-taurine can be explained if NAP-taurine only binds to its site when the transport site is in the outward-facing (E/sub o/ or ECl/sub o/) form. Since NAP-taurine prevents the conformational change from ECl/sub o/ to ECl/sub i/, it must lock the system in the outward-facing form. NAP-taurine can therefore be used just like the competitive inhibitor H/sub 2/DIDS (4,4'-diisothiocyano-1,2-diphenylethane-2,2'-disulfonic acid) to monitor the fraction of transport sites that face outward. A quantitative analysis of the effects of chloride gradients on the inhibitory potency of NAP-taurine and H/sub 2/DIDS reveals that the transport system is intrinsically asymmetric, such that when Cl/sub i/ = Cl/sub o/, most of the unloaded transport sites face the cytoplasmic side of the membrane. 30 references, 7 figures, 3 tables.

  5. Role of adaptor proteins and clathrin in the trafficking of human kidney anion exchanger 1 (kAE1) to the cell surface.

    PubMed

    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. PMID:24698155

  6. Characterisation of legumes by enzymatic hydrolysis, microdialysis sampling, and micro-high-performance anion-exchange chromatography with electrospray ionisation mass spectrometry.

    PubMed

    Okatch, Harriet; Torto, Nelson; Armateifio, Joan

    2003-04-11

    An assay based on enzymatic hydrolysisand microdialysis sampling, micro-high-performance anion-exchange chromatography (micro-HPAEC) with electrospray ionisation mass spectrometry (ESI-MS) for the characterisation of legumes is presented. Characterisation of two bean varieties; Phaseolus mungo and P. acutifilous was based upon enzymatic hydrolysis using an endo-beta-mannanase from Aspergillus niger with subsequent analysis of the hydrolysates with HPAEC-MS. The hydrolysates were detected in the positive ionisation mode after desalting the chromatographic effluent, employing a cation-exchange membrane desalting device with water as the regenerating liquid. Mass chromatograms, acquiredafter hydrolysis of both bean samples for 12 h, showed two different profiles of hydrolysates. The P. mungo bean hydrolysate showed the presence of saccharides with a degree of polymerisation (DP) in the range of 2-6, whereas that of P. acutifilous showed only DPs of 2-5. Both bean samples had one type of DP 2, but showed different types of DPs 3, 4 and 5. Only the P. mungo sample showed the presence of DP 6. The most abundant fraction for P. mungo was DP 4, whereas that for P. acutifilous was DP 5. Tandem MS of the hydrolysates showed that the DP 2 hydrolysates observed for the samples were of the same type, having a 1,6 linkage. Also tandem MS data for DPs 3, 4, and 5 showed that similar hydrolysates were present within the same sample as well as among the two samples. The data also showed the existence of 1,6 linkages for DP 3, 4, and 5 hydrolysates. The single enzymatic hydrolysis in combination with microdialysis and HPAEC with ESI-MS proved to be sufficient and reproducible for profiling and showing the difference between the two bean samples. PMID:12735463

  7. Improvements to in-line desalting of oligosaccharides separated by high-pH anion exchange chromatography with pulsed amperometric detection.

    PubMed

    Thayer, J R; Rohrer, J S; Avdalovic, N; Gearing, R P

    1998-02-15

    High-pH anion exchange chromatography with pulsed amperometric detection (HPAEC/PAD) (1) is routinely used to separate neutral and charged oligosaccharides differing by branch, linkage, and positional isomerism. Oligosaccharides are eluted in 0.1 M NaOH with gradients of sodium acetate (up to 0.25 M). Analyses of HPAEC/PAD-purified oligosaccharides generally require neutralization and removal of eluent salts. To facilitate the process, we designed and produced a cation-exchange system to remove sodium ions (Na+) from the eluent after oligosaccharide detection [the Carbohydrate Membrane Desalter (CMD), with a volatile regenerant]. Exchange of >99.5% of eluent Na+ for hydronium ions (H3O+) within the CMD generates dilute acetic acid (removable by vacuum evaporation). The exchange process desalts up to 0.35 M Na+ at 1.0 ml/min. Oligosaccharides collected after on-line desalting, evaporated and resuspended in their original volume of deionized water contained < or = 350 muM residual Na+ when the eluting sodium concentration was 300 mM. This represents a desalting efficiency of >99.8%. Recovery of neutral and sialylated oligosaccharides under these conditions ranged from 75 to 100%. With the CMD system and postcollection evaporation, HPAEC/PAD can purify oligosaccharides ready for further characterization. As a proof test, oligosaccharides from a human monoclonal antibody were separated by HPAEC/PAD, desalted with the CMD system, dried, and analyzed by matrix-assisted laser desorption-ionization, time-of-flight mass spectrometry. PMID:9473279

  8. Effect of long-term organic removal on ion exchange properties and performance during sewage tertiary treatment by conventional anion exchange resins.

    PubMed

    Sun, Jian; Li, Xiaofeng; Quan, Ying; Yin, Yunjun; Zheng, Shaokui

    2015-10-01

    This study evaluated the long-term dissolved organic matter (DOM), phosphorus and nitrogen removal performance of a commercially available conventional anion exchange resin (AER) from actual secondary effluent (SE) in a sewage treatment plant based on a pilot-scale operation (2.2 m(3) d(-1), 185 cycles, 37,000 bed volume, 1.5 years). Particular emphasis was given to the potential effect of DOM fouling on the ion exchange properties and performance during the long-term operation. Despite the large range of COD (15.6-33.5 mg L(-1)), BOD5 (3.0-5.6 mg L(-1)), DOC (6.5-24.2 mg L(-1)), and UV254 (UV absorption at 254 nm) (0.108-0.229 cm(-1)) levels in the SE, the removal efficiencies of the AER for the aforementioned parameters were 43±12%, 46±15%, 45±9%, and 72±4%, respectively. Based on three-dimensional fluorescence excitation-emission matrix data, i.e., the fluorescence intensities of four regions (peaks A-D), all organic components of the SE were effectively removed (peak A 74%, peak B 48%, peak C 55%, and peak D 45%) following the adsorption. The AER effluent still has considerable polycyclic aromatic hydrocarbons' ecological hazard on freshwater fishes when they were significantly removed from SE. The obvious DOM fouling on the AER, identified by color change, had no significant influence on the long-term removal of the representative inorganic anions (averaging 95±4% phosphate, 100±0% SO4(2-), and 62±17% NO3(-)) and AER properties (including total exchange capacity, moisture content, and true density). The conventional AER can produce high quality reclaimed water from SE at a low operational cost.

  9. Retention prediction of highly polar ionizable solutes under gradient conditions on a mixed-mode reversed-phase and weak anion-exchange stationary phase.

    PubMed

    Balkatzopoulou, P; Fasoula, S; Gika, H; Nikitas, P; Pappa-Louisi, A

    2015-05-29

    In the present work the retention of three highly polar and ionizable solutes - uric acid, nicotinic acid and ascorbic acid - was investigated on a mixed-mode reversed-phase and weak anion-exchange (RP/WAX) stationary phase in buffered aqueous acetonitrile (ACN) mobile phases. A U-shaped retention behavior was observed for all solutes with respect to the eluent organic modifier content studied in a range of 5-95% (v/v). This retention behavior clearly demonstrates the presence of a HILIC-type retention mechanism at ACN-rich hydro-organic eluents and an RP-like retention at aqueous-rich hydro-organic eluents. Hence, this column should be promising for application under both RP and HILIC gradient elution modes. For this reason, a series of programmed elution runs were carried out with increasing (RP) and decreasing (HILIC) organic solvent concentration in the mobile phase. This dual gradient process was successfully modeled by two retention models exhibiting a quadratic or a cubic dependence of the logarithm of the solute retention factor (lnk) upon the organic modifier volume fraction (φ). It was found that both models produced by gradient retention data allow the prediction of solute retention times for both types of programmed elution on the mixed-mode column. Four, in the case of the quadratic model, or five, in the case of the cubic model, initial HILIC- and RP-type gradient runs gave satisfactory retention predictions of any similar kind elution program, even with different flow rate, with an overall error of only 2.5 or 1.7%, respectively.

  10. Use of strong anion exchange resins for the removal of perfluoroalkylated substances from contaminated drinking water in batch and continuous pilot plants.

    PubMed

    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

  11. Topology studies with biosynthetic fragments identify interacting transmembrane regions of the human red-cell anion exchanger (band 3; AE1).

    PubMed Central

    Groves, J D; Tanner, M J

    1999-01-01

    The red-cell anion exchanger (band 3; AE1) is a multispanning membrane protein that traverses the bilayer up to 14 times and is N-glycosylated at Asn-642. We have shown that the integrity of six different loops are not essential for stilbene disulphonate-sensitive chloride uptake in Xenopus oocytes. We used an N-glycosylation mutagenesis approach to examine the orientation of the N-terminus and the endogenous glycosylation site of each C-terminal fragment by cell-free translation. The fragments initiating in the loops preceding spans 2, 9 and 11 did not insert into the membrane with the expected orientation. Furthermore, N-glycosylation of Asn-642 might facilitate the membrane integration of span 7. The correct integration of spans 2-3 required the presence of the region containing span 4 and that the luminal exposure of the C-terminus of span 7 is increased in the presence of the region including span 6 or span 8. The results suggest the span 8 region is required for the correct folding of spans 9-10, at least in the presence of the span 11-12 region. Our results suggest that there are intramolecular interactions between the regions of transmembrane spans 1 and 2, 2 and 4, 4 and 5, 7 and 8, 8 and 9-10, and 9-10 and 11-12. Spans 1, 4, 5, 6 and 8 might act as a scaffold for the assembly of spans 2-3, 7 and 9-10. This approach might provide a general method for dissecting the interactions between membrane-spanning regions of polytopic membrane proteins. PMID:10585855

  12. Use of strong anion exchange resins for the removal of perfluoroalkylated substances from contaminated drinking water in batch and continuous pilot plants.

    PubMed

    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.

  13. 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.

    PubMed

    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.

  14. Ae4 (Slc4a9) Anion Exchanger Drives Cl- Uptake-dependent Fluid Secretion by Mouse Submandibular Gland Acinar Cells.

    PubMed

    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.

  15. Bicarbonate uptake via an anion exchange protein is the main mechanism of inorganic carbon acquisition by the giant kelp Macrocystis pyrifera (Laminariales, Phaeophyceae) under variable pH.

    PubMed

    Fernández, Pamela A; Hurd, Catriona L; Roleda, Michael Y

    2014-12-01

    Macrocystis pyrifera is a widely distributed, highly productive, seaweed. It is known to use bicarbonate (HCO3 (-) ) from seawater in photosynthesis and the main mechanism of utilization is attributed to the external catalyzed dehydration of HCO3 (-) by the surface-bound enzyme carbonic anhydrase (CAext ). Here, we examined other putative HCO3 (-) uptake mechanisms in M. pyrifera under pHT 9.00 (HCO3 (-) : CO2  = 940:1) and pHT 7.65 (HCO3 (-) : CO2  = 51:1). Rates of photosynthesis, and internal CA (CAint ) and CAext activity were measured following the application of AZ which inhibits CAext , and DIDS which inhibits a different HCO3 (-) uptake system, via an anion exchange (AE) protein. We found that the main mechanism of HCO3 (-) uptake by M. pyrifera is via an AE protein, regardless of the HCO3 (-) : CO2 ratio, with CAext making little contribution. Inhibiting the AE protein led to a 55%-65% decrease in photosynthetic rates. Inhibiting both the AE protein and CAext at pHT 9.00 led to 80%-100% inhibition of photosynthesis, whereas at pHT 7.65, passive CO2 diffusion supported 33% of photosynthesis. CAint was active at pHT 7.65 and 9.00, and activity was always higher than CAext , because of its role in dehydrating HCO3 (-) to supply CO2 to RuBisCO. Interestingly, the main mechanism of HCO3 (-) uptake in M. pyrifera was different than that in other Laminariales studied (CAext -catalyzed reaction) and we suggest that species-specific knowledge of carbon uptake mechanisms is required in order to elucidate how seaweeds might respond to future changes in HCO3 (-) :CO2 due to ocean acidification.

  16. Effect of long-term organic removal on ion exchange properties and performance during sewage tertiary treatment by conventional anion exchange resins.

    PubMed

    Sun, Jian; Li, Xiaofeng; Quan, Ying; Yin, Yunjun; Zheng, Shaokui

    2015-10-01

    This study evaluated the long-term dissolved organic matter (DOM), phosphorus and nitrogen removal performance of a commercially available conventional anion exchange resin (AER) from actual secondary effluent (SE) in a sewage treatment plant based on a pilot-scale operation (2.2 m(3) d(-1), 185 cycles, 37,000 bed volume, 1.5 years). Particular emphasis was given to the potential effect of DOM fouling on the ion exchange properties and performance during the long-term operation. Despite the large range of COD (15.6-33.5 mg L(-1)), BOD5 (3.0-5.6 mg L(-1)), DOC (6.5-24.2 mg L(-1)), and UV254 (UV absorption at 254 nm) (0.108-0.229 cm(-1)) levels in the SE, the removal efficiencies of the AER for the aforementioned parameters were 43±12%, 46±15%, 45±9%, and 72±4%, respectively. Based on three-dimensional fluorescence excitation-emission matrix data, i.e., the fluorescence intensities of four regions (peaks A-D), all organic components of the SE were effectively removed (peak A 74%, peak B 48%, peak C 55%, and peak D 45%) following the adsorption. The AER effluent still has considerable polycyclic aromatic hydrocarbons' ecological hazard on freshwater fishes when they were significantly removed from SE. The obvious DOM fouling on the AER, identified by color change, had no significant influence on the long-term removal of the representative inorganic anions (averaging 95±4% phosphate, 100±0% SO4(2-), and 62±17% NO3(-)) and AER properties (including total exchange capacity, moisture content, and true density). The conventional AER can produce high quality reclaimed water from SE at a low operational cost. PMID:25996990

  17. Transcellular oxalate and Cl- absorption in mouse intestine is mediated by the DRA anion exchanger Slc26a3, and DRA deletion decreases urinary oxalate.

    PubMed

    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.

  18. Role of adaptor proteins and clathrin in the trafficking of human kidney anion exchanger 1 (kAE1) to the cell surface.

    PubMed

    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.

  19. Solvent-extraction purification of neptunium

    SciTech Connect

    Kyser, E.A.; Hudlow, S.L.

    2008-07-01

    The Savannah River Site (SRS) has recovered {sup 237}Np from reactor fuel that is currently being processed into NpO{sub 2} for future production of {sup 238}Pu. Several purification flowsheets have been utilized. An oxidizing solvent-extraction (SX) flowsheet was used to remove Fe, sulfate ion, and Th while simultaneously {sup 237}Np, {sup 238}Pu, u, and nonradioactive Ce(IV) was extracted into the tributyl phosphate (TBP) based organic solvent. A reducing SX flowsheet (second pass) removed the Ce and Pu and recovered both Np and U. The oxidizing flowsheet was necessary for solutions that contained excessive amounts of sulfate ion. Anion exchange was used to perform final purification of Np from Pu, U, and various non-actinide impurities. The Np(IV) in the purified solution was then oxalate-precipitated and calcined to an oxide for shipment to other facilities for storage and future target fabrication. Performance details of the SX purification and process difficulties are discussed. (authors)

  20. Automated Water-Purification System

    NASA Technical Reports Server (NTRS)

    Ahlstrom, Harlow G.; Hames, Peter S.; Menninger, Fredrick J.

    1988-01-01

    Reverse-osmosis system operates and maintains itself with minimal human attention, using programmable controller. In purifier, membranes surround hollow cores through which clean product water flows out of reverse-osmosis unit. No chemical reactions or phase changes involved. Reject water, in which dissolved solids concentrated, emerges from outer membrane material on same side water entered. Flow controls maintain ratio of 50 percent product water and 50 percent reject water. Membranes expected to last from 3 to 15 years.

  1. Extraction and Purification of R-phycoerythrin from Marine Red Algae.

    PubMed

    Dumay, Justine; Morançais, Michèle; Nguyen, Huu Phuo Trang; Fleurence, Joël

    2015-01-01

    This chapter focuses on the recovery of an R-Phycoerythrin (R-PE)-enriched fraction from marine algae. Since R-PE is a proteinaceous pigment, we have developed a simple and rapid two-step method devoted to the extraction and purification of R-PE from marine red algae. Here we describe a phosphate buffer extraction followed by anion exchange chromatography carried on a DEAE Sepharose Fast Flow column. To ensure the quality and quantity of R-PE recovery, we also indicate different methods to monitor each fraction obtained, such as spectrophotometric indicators, gel filtration, and SDS-PAGE analysis.

  2. Extraction and Purification of R-phycoerythrin from Marine Red Algae.

    PubMed

    Dumay, Justine; Morançais, Michèle; Nguyen, Huu Phuo Trang; Fleurence, Joël

    2015-01-01

    This chapter focuses on the recovery of an R-Phycoerythrin (R-PE)-enriched fraction from marine algae. Since R-PE is a proteinaceous pigment, we have developed a simple and rapid two-step method devoted to the extraction and purification of R-PE from marine red algae. Here we describe a phosphate buffer extraction followed by anion exchange chromatography carried on a DEAE Sepharose Fast Flow column. To ensure the quality and quantity of R-PE recovery, we also indicate different methods to monitor each fraction obtained, such as spectrophotometric indicators, gel filtration, and SDS-PAGE analysis. PMID:26108500

  3. Purification design and practice for pertactin, the third component of acellular pertussis vaccine, from Bordetella pertussis.

    PubMed

    Li, Zenglan; Zhang, Yan; Wang, Qi; Li, Zhengjun; Liu, Yongdong; Zhang, Songping; Zhang, Guifeng; Ma, Guanghui; Luo, Jian; Su, Zhiguo

    2016-07-25

    Development of acellular pertussis vaccine (aPV) requires purification of several components from Bordetella pertussis. While the components pertussis toxin (PT) and filamentous hemagglutinin (FHA) have been successfully purified, the third component, pertactin, proves to be a difficult target due to its very low concentration. In order to solve its purification problem, we performed the surface potential analysis with GRASP2 program. The results demonstrated that there are two major charge patches, one negative and one positive, which are located separately on this linear protein. For this special feature, we designed a dual ion exchange chromatography strategy including an anionic exchange and a cationic exchange process for separation of pertactin from the heat extract of B. pertussis. The initial anionic exchange chromatography concentrated the product from 1.7% to 14.6%, with recovery of 80%. The second cationic exchange chromatography increased the purity to 33%, with recovery of 83%. The final purification was accomplished by hydrophobic interaction chromatography, yielding a purity of 96%. The total recovery of the three columns was 61%. Characterization of the purified antigen was performed with CD, intrinsic fluorescence, HP-SEC and western-blot, showing that the purified protein kept its natural conformation and immune-reactivity. The rationally designed process proved to be feasible, and it is suitable for large-scale preparation of the third aPV component pertactin.

  4. Isolation and purification of monosialotetrahexosylgangliosides from pig brain by extraction and liquid chromatography.

    PubMed

    Bian, Liujiao; Yang, Jianting; Sun, Yu

    2015-10-01

    Monosialotetrahexosylganglioside (GM1), one of glycosphingolipids containing sialic acid, plays particularly important role in fighting against paralysis, dementia and other diseases caused by brain and nerve damage. In this work, a simple and highly efficient method with high yield was developed for isolation and purification of GM1 from pig brain. The method consisted of an extraction by chloroform-methanol-water and a two-step chromatographic separation by DEAE-Sepharose Fast Flow anion-exchange medium and Sephacryl S-100 HR size-exclusion medium. The purified GM1 was proved to be homogeneous and had a purity of >98.0% by high-performance anion-exchange and size-exclusion chromatography. The molecular weight was 30.0 kDa by high-performance size-exclusion chromatography and 1546.9 Da by electrospray ionization mass spectrometry. The chromogenic reaction by resorcinol-hydrochloric acid solution indicated that the purified GM1 showed a specific chromogenic reaction of sialic acid. Through this isolation and purification program, ~1.0 mg of pure GM1 could be captured from 500 g wet pig brain tissue and the yield of GM1 was around 0.022%, which was higher than the yields by other methods. The method may provide an alternative for isolation and purification of GM1 in other biological tissues.

  5. The Center for Optimized Structural Studies (COSS) platform for automation in cloning, expression, and purification of single proteins and protein-protein complexes.

    PubMed

    Mlynek, Georg; Lehner, Anita; Neuhold, Jana; Leeb, Sarah; Kostan, Julius; Charnagalov, Alexej; Stolt-Bergner, Peggy; Djinović-Carugo, Kristina; Pinotsis, Nikos

    2014-06-01

    Expression in Escherichia coli represents the simplest and most cost effective means for the production of recombinant proteins. This is a routine task in structural biology and biochemistry where milligrams of the target protein are required in high purity and monodispersity. To achieve these criteria, the user often needs to screen several constructs in different expression and purification conditions in parallel. We describe a pipeline, implemented in the Center for Optimized Structural Studies, that enables the systematic screening of expression and purification conditions for recombinant proteins and relies on a series of logical decisions. We first use bioinformatics tools to design a series of protein fragments, which we clone in parallel, and subsequently screen in small scale for optimal expression and purification conditions. Based on a scoring system that assesses soluble expression, we then select the top ranking targets for large-scale purification. In the establishment of our pipeline, emphasis was put on streamlining the processes such that it can be easily but not necessarily automatized. In a typical run of about 2 weeks, we are able to prepare and perform small-scale expression screens for 20-100 different constructs followed by large-scale purification of at least 4-6 proteins. The major advantage of our approach is its flexibility, which allows for easy adoption, either partially or entirely, by any average hypothesis driven laboratory in a manual or robot-assisted manner.

  6. Improving impurities clearance by amino acids addition to buffer solutions for chromatographic purifications of monoclonal antibodies.

    PubMed

    Ishihara, Takashi; Hosono, Mareto

    2015-07-15

    The performance of amino acids in Protein A affinity chromatography, anion exchange chromatography and cation exchange chromatography for monoclonal antibody purification was investigated. Glycine, threonine, arginine, glutamate, and histidine were used as buffer components in the equilibration, washing, and elution steps of these chromatographies. Improved clearance of impurity, high molecular weight species (HMW) and host cell proteins (HCP) was observed in the purification processes when using the amino acids as base-buffer constituents, additives or eluents compared with that of buffers without these amino acids. In addition, we designed a buffer system in which the mobile phases were composed of only a single amino acid, histidine, and applied it to the above three chromatographies. Effective HMW and HCP clearance was also obtained in this manner. These results suggest that amino acids may enhance impurity clearance during the purification of monoclonal antibodies. PMID:26057847

  7. Purification and preliminary characterization of agglutinogen 3 from Bordetella pertussis.

    PubMed

    Fredriksen, J H; Frøholm, L O; Paulsen, B S

    1985-01-01

    One serotype antigen, agglutinogen 3, from Bordetella pertussis, (strain M2, serotype 1.3), has been purified. The purification procedure included acetone drying of cells harvested from shaking cultures. Agglutinogens were extracted in phosphate buffered saline. Crude extract was heat treated at 80 degrees C for 5 min and precipitated by ammonium sulphate between 25 and 60% saturation at 4 degrees C, providing 50% of the total activity and a five-fold purification. Further purification was attempted by gel filtration chromatography using a TSK-G3000 SW column. The ammonium sulphate precipitated fraction was also separated by anion exchange chromatography using a Mono Q HR 5/5 column. The purification work indicated that agglutinogen 3 is associated with several other substances and that this property can lead to purification difficulties. The isolation procedure was monitored by an agglutination-inhibition assay. The peak fraction from the ion exchange chromatography was purified up to 27-fold according to the specific activities (inhibition units per mg protein). The yield was only 1% due to severe loss of activity. In the gel filtration chromatography agglutinogen 3-activity eluted with a maximum activity corresponding to a molecular weight near 450,000. SDS-PAGE analysis indicated that agglutinogen 3 might have a subunit molecular weight of 20,800. PMID:2872104

  8. MC ICP-MS δ(34)S(VCDT) measurement of dissolved sulfate in environmental aqueous samples after matrix separation by means of an anion exchange membrane.

    PubMed

    Hanousek, Ondrej; Berger, Torsten W; Prohaska, Thomas

    2016-01-01

    Analysis of (34)S/(32)S of sulfate in rainwater and soil solutions can be seen as a powerful tool for the study of the sulfur cycle. Therefore, it is considered as a useful means, e.g., for amelioration and calibration of ecological or biogeochemical models. Due to several analytical limitations, mainly caused by low sulfate concentration in rainwater, complex matrix of soil solutions, limited sample volume, and high number of samples in ecosystem studies, a straightforward analytical protocol is required to provide accurate S isotopic data on a large set of diverse samples. Therefore, sulfate separation by anion exchange membrane was combined with precise isotopic measurement by multicollector inductively coupled plasma mass spectrometry (MC ICP-MS). The separation method proved to be able to remove quantitatively sulfate from matrix cations (Ca, K, Na, or Li) which is a precondition in order to avoid a matrix-induced analytical bias in the mass spectrometer. Moreover, sulfate exchange on the resin is capable of preconcentrating sulfate from low concentrated solutions (to factor 3 in our protocol). No significant sulfur isotope fractionation was observed during separation and preconcentration. MC ICP-MS operated at edge mass resolution has enabled the direct (34)S/(32)S analysis of sulfate eluted from the membrane, with an expanded uncertainty U (k = 2) down to 0.3 ‰ (a single measurement). The protocol was optimized and validated using different sulfate solutions and different matrix compositions. The optimized method was applied in a study on solute samples retrieved in a beech (Fagus sylvatica) forest in the Vienna Woods. Both rainwater (precipitation and tree throughfall) and soil solution δ (34)SVCDT ranged between 4 and 6 ‰, the ratio in soil solution being slightly lower. The lower ratio indicates that a considerable portion of the atmospherically deposited sulfate is cycled through the organic S pool before being released to the soil solution

  9. Anion-exchangeable layered materials based on rare-earth phosphors: unique combination of rare-earth host and exchangeable anions.

    PubMed

    Geng, Fengxia; Ma, Renzhi; Sasaki, Takayoshi

    2010-09-21

    Layered materials, three-dimensional crystals built from stacking two-dimensional components, are attracting intense interest because of their structural anisotropy and the fascinating properties that result. However, the range of such layered materials that can exchange anions is quite small. Continuing efforts have been underway to identify a new class of anion-exchangeable materials. One major goal is the incorporation of rare-earth elements within the host because researchers expect that the marriage of rare-earth skeleton host and the exchangeable species within the interlayer will open up new avenues both for the assembly of layered materials and for the understanding of rare-earth element chemistry. Such lanthanide layered solids have industrial potential. These materials are also of academic importance, serving as an ideal model for studying the cationic size effect on structure stability associated with lanthanide contraction. In this Account, we present the work done by ourselves and others on this novel class of materials. We examine the following four subtopics regarding these layered anionic materials: (1) synthesis strategy and composition diversity, (2) structural features, (3) structure stability with relative humidity, and (4) applications. These materials can be synthesized either by hydrothermal reactions or by homogeneous precipitation, and a variety of anions can be intercalated into the gallery. Although only cations with a suitable size can form the layered structure, the possible range is wide, from early to late lanthanides. We illustrate the effect of lanthanide contraction on properties including morphology, lattice dimensions, and coordination numbers. Because each lanthanide metal ion coordinates water molecules, and the water molecules point directly into the gallery space, this feature plays a critical role in stabilizing the layered structure. In the 9-fold monocapped square antiprism structure, the humidity-triggered transition

  10. Dendrimer-functionalized mesoporous silica as a reversed-phase/anion-exchange mixed-mode sorbent for solid phase extraction of acid drugs in human urine.

    PubMed

    Li, Yun; Yang, Jiajia; Huang, Chaonan; Wang, Longxing; Wang, Jincheng; Chen, Jiping

    2015-05-01

    A new dendrimer-functionalized mesoporous silica material based on large-pore 3D cubic Korea Advanced Institute of Science and Technology-6 (KIT-6) was synthesized by the growing of dendritic branches inside the mesopores of aminopropyl functionalized KIT-6. Detailed physical characterizations using transmission electron microscopy, nitrogen adsorption-desorption measurements, Fourier transform infrared (FTIR) spectroscopy, and elemental analysis reveal that the multifunctional dendrimers have been grown successfully within the confined spaces of mesopores. Although the 3D ordered mesoporous architecture of KIT-6 was well preserved, there was a significant and continuous decrease in pore size, specific surface area (SBET) and pore volume when increasing dendrimer generation up to six. In order to get a compromise between the SBET, pore size and density of functionalities, the dendrimer-functionalized KIT-6 (DF-KIT-6) for generation 2 (SBET, 314.2 m(2) g(-1); pore size, 7.9 nm; carbon and nitrogen contents, 19.80% and 1.92%) was selected for solid phase extraction (SPE) applications. The DF-KIT-6 was then evaluated as a reversed-phase/anion-exchange mixed-mode sorbent for extraction of the selected acidic drugs (ketoprofen, KEP; naproxen, NAP; and ibuprofen, IBU), since the dendrimers contained both hydrocarbonaceous and amine functionalities. The effective parameters on extraction efficiency such as sample pH and volume, type and volume of eluent and wash solvents were optimized. Under the optimized experimental conditions, the DF-KIT-6 based SPE coupled with HPLC-UV method demonstrated good sensitivity (0.4-4.6 ng mL(-1) detection of limits) and linearity (R(2)>0.990 for 10-2000 ng mL(-1) of KEP and IBU, and 1-200 ng mL(-1) of NAP). The potential use of DF-KIT-6 sorbent for preconcentration and cleanup of acid drugs in human urine samples was also demonstrated. Satisfactory recoveries at two spiking levels (30 and 300 ng mL(-1) for KEP and IBU, 3 and 30 ng mL(-1

  11. 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.

    PubMed

    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

  12. Basolateral chloride loading by the anion exchanger type 2: role in fluid secretion by the human airway epithelial cell line Calu-3

    PubMed Central

    Huang, Junwei; Shan, Jiajie; Kim, Dusik; Liao, Jie; Evagelidis, Alexandra; Alper, Seth L; Hanrahan, John W

    2012-01-01

    Anion exchanger type 2 (AE2 or SLC4A2) is an electroneutral Cl−/HCO3− exchanger expressed at the basolateral membrane of many epithelia. It is thought to participate in fluid secretion by airway epithelia. However, the role of AE2 in fluid secretion remains uncertain, due to the lack of specific pharmacological inhibitors, and because it is electrically silent and therefore does not contribute directly to short-circuit current (Isc). We have studied the role of AE2 in Cl− and fluid secretion by the airway epithelial cell line Calu-3. After confirming expression of its mRNA and protein, a knock-down cell line called AE2-KD was generated by lentivirus-mediated RNA interference in which AE2 mRNA and protein levels were reduced ≥90%. Suppressing AE2 increased the expression of the cystic fibrosis transmembrane conductance regulator (CFTR) by ∼70% without affecting the levels of NKCC1 (Na+–K+–2Cl− cotransporter) or NBCe1 (Na+–nHCO3− cotransporter). cAMP agonists stimulated fluid secretion by parental Calu-3 and scrambled shRNA cells >6.5-fold. In AE2-KD cells this response was reduced by ∼70%, and the secreted fluid exhibited elevated pH and [HCO3−] as compared with the control lines. Unstimulated equivalent short-circuit current (Ieq) was elevated in AE2-KD cells, but the incremental response to forskolin was unaffected. The modest bumetanide-induced reductions in both Ieq and fluid secretion were more pronounced in AE2-KD cells. Basolateral Cl−/HCO3− exchange measured by basolateral pH-stat in cells with permeabilized apical membranes was abolished in AE2-KD monolayers, and the intracellular alkalinization resulting from basolateral Cl− removal was reduced by ∼80% in AE2-KD cells. These results identify AE2 as a major pathway for basolateral Cl− loading during cAMP-stimulated secretion of Cl− and fluid by Calu-3 cells, and help explain the large bumetanide-insensitive component of fluid secretion reported previously in airway

  13. Basolateral chloride loading by the anion exchanger type 2: role in fluid secretion by the human airway epithelial cell line Calu-3.

    PubMed

    Huang, Junwei; Shan, Jiajie; Kim, Dusik; Liao, Jie; Evagelidis, Alexandra; Alper, Seth L; Hanrahan, John W

    2012-11-01

    Anion exchanger type 2 (AE2 or SLC4A2) is an electroneutral Cl(-)/HCO(3)(-) exchanger expressed at the basolateral membrane of many epithelia. It is thought to participate in fluid secretion by airway epithelia. However, the role of AE2 in fluid secretion remains uncertain, due to the lack of specific pharmacological inhibitors, and because it is electrically silent and therefore does not contribute directly to short-circuit current (I(sc)). We have studied the role of AE2 in Cl(-) and fluid secretion by the airway epithelial cell line Calu-3. After confirming expression of its mRNA and protein, a knock-down cell line called AE2-KD was generated by lentivirus-mediated RNA interference in which AE2 mRNA and protein levels were reduced 90%. Suppressing AE2 increased the expression of the cystic fibrosis transmembrane conductance regulator (CFTR) by ∼70% without affecting the levels of NKCC1 (Na(+)-K(+)-2Cl(-) cotransporter) or NBCe1 (Na(+)-nHCO(3)(-) cotransporter). cAMP agonists stimulated fluid secretion by parental Calu-3 and scrambled shRNA cells >6.5-fold. In AE2-KD cells this response was reduced by ∼70%, and the secreted fluid exhibited elevated pH and [HCO(3)(-)] as compared with the control lines. Unstimulated equivalent short-circuit current (I(eq)) was elevated in AE2-KD cells, but the incremental response to forskolin was unaffected. The modest bumetanide-induced reductions in both I(eq) and fluid secretion were more pronounced in AE2-KD cells. Basolateral Cl(-)/HCO(3)(-) exchange measured by basolateral pH-stat in cells with permeabilized apical membranes was abolished in AE2-KD monolayers, and the intracellular alkalinization resulting from basolateral Cl(-) removal was reduced by ∼80% in AE2-KD cells. These results identify AE2 as a major pathway for basolateral Cl(-) loading during cAMP-stimulated secretion of Cl(-) and fluid by Calu-3 cells, and help explain the large bumetanide-insensitive component of fluid secretion reported previously in

  14. Anion-exchangeable layered materials based on rare-earth phosphors: unique combination of rare-earth host and exchangeable anions.

    PubMed

    Geng, Fengxia; Ma, Renzhi; Sasaki, Takayoshi

    2010-09-21

    Layered materials, three-dimensional crystals built from stacking two-dimensional components, are attracting intense interest because of their structural anisotropy and the fascinating properties that result. However, the range of such layered materials that can exchange anions is quite small. Continuing efforts have been underway to identify a new class of anion-exchangeable materials. One major goal is the incorporation of rare-earth elements within the host because researchers expect that the marriage of rare-earth skeleton host and the exchangeable species within the interlayer will open up new avenues both for the assembly of layered materials and for the understanding of rare-earth element chemistry. Such lanthanide layered solids have industrial potential. These materials are also of academic importance, serving as an ideal model for studying the cationic size effect on structure stability associated with lanthanide contraction. In this Account, we present the work done by ourselves and others on this novel class of materials. We examine the following four subtopics regarding these layered anionic materials: (1) synthesis strategy and composition diversity, (2) structural features, (3) structure stability with relative humidity, and (4) applications. These materials can be synthesized either by hydrothermal reactions or by homogeneous precipitation, and a variety of anions can be intercalated into the gallery. Although only cations with a suitable size can form the layered structure, the possible range is wide, from early to late lanthanides. We illustrate the effect of lanthanide contraction on properties including morphology, lattice dimensions, and coordination numbers. Because each lanthanide metal ion coordinates water molecules, and the water molecules point directly into the gallery space, this feature plays a critical role in stabilizing the layered structure. In the 9-fold monocapped square antiprism structure, the humidity-triggered transition

  15. The use of strong anion-exchange (SAX) magnetic particles for the extraction of therapeutic siRNA and their analysis by liquid chromatography/mass spectrometry.

    PubMed

    Ye, Guofeng; Beverly, Michael

    2011-11-15

    Traditional methods for extracting oligonucleotides from serum and other biological fluids are often time-consuming and require multiple steps. Magnetic particle based separation of oligonucleotides has gained importance recently due to the advantages of simplicity and high efficiency. Here we report the development and optimization of commercially available strong anion-exchange (SAX) magnetic beads for the extraction of siRNA from human serum. The beads allowed for rapid extraction of siRNA from human serum in 100-200 μL of liquid chromatography/mass spectrometry (LC/MS)-compatible buffer in less than 1 h for a 96-well plate with no further drying steps. Due to the strong cation-binding properties of oligonucleotides, volatile ammonium salts such as triethylammonium bicarbonate (TEAB), ammonium bicarbonate, and NH(4) Cl were used to elute the siRNA from the beads. For more hydrophobic siRNA sequences, the addition of 5-10% organic solvent was required for elution. The recovery of chemically modified siRNA from human serum was around 80% for two types of beads examined; however, the recovery for highly modified sequences differed greatly between the two types of beads. In addition to extracting highly modified oligonucleotides, the SAX beads were also able to extract liposomal formulated siRNAs from serum with no interference from the lipid formulation. The extraction of siRNA from human serum was linear over the tested range of 50 ng/mL to 10 µg/mL. Using this extraction methodology, we have created a workflow to monitor siRNA serum stability by LC/MS. Initial observations confirm that RNase A type degradation with strand cleavage on the 3' side of uridine or cytosine is the dominant cleavage pattern in serum. This finding has implications for the selection and modification of therapeutic siRNAs and demonstrates the utility of magnetic beads as a simple and rapid extraction technique for siRNA.

  16. 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.

    PubMed

    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

  17. Functional comparison of mouse slc26a6 anion exchanger with human SLC26A6 polypeptide variants: differences in anion selectivity, regulation, and electrogenicity.

    PubMed

    Chernova, Marina N; Jiang, Lianwei; Friedman, David J; Darman, Rachel B; Lohi, Hannes; Kere, Juha; Vandorpe, David H; Alper, Seth L

    2005-03-01

    The unusually low 78% amino acid identity between the orthologous human SLC26A6 and mouse slc26a6 polypeptides prompted systematic comparison of their anion transport functions in Xenopus oocytes. Multiple human SLC26A6 variant polypeptides were also functionally compared. Transport was studied as unidirectional fluxes of (36)Cl(-), [(14)C]oxalate, and [(35)S]sulfate; as net fluxes of HCO(3)(-) by fluorescence ratio measurement of intracellular pH; as current by two-electrode voltage clamp; and as net Cl(-) flux by fluorescence intensity measurement of relative changes in extracellular and intracellular [Cl(-)]. Four human SLC26A6 polypeptide variants each exhibited rates of bidirectional [(14)C]oxalate flux, Cl(-)/HCO(3)(-) exchange, and Cl(-)/OH(-) exchange nearly equivalent to those of mouse slc26a6. Cl(-)/HCO(3)(-) exchange by both orthologs was cAMP-sensitive, further enhanced by coexpressed wild type cystic fibrosis transmembrane regulator but inhibited by cystic fibrosis transmembrane regulator DeltaF508. However, the very low rates of (36)Cl(-) and [(35)S]sulfate transport by all active human SLC26A6 isoforms contrasted with the high rates of the mouse ortholog. Human and mouse orthologs also differed in patterns of acute regulation. Studies of human-mouse chimeras revealed cosegregation of the high (36)Cl(-) transport phenotype with the transmembrane domain of mouse slc26a6. Mouse slc26a6 and human SLC26A6 each mediated electroneutral Cl(-)/HCO(3)(-) and Cl(-)/OH(-) exchange. In contrast, whereas Cl(-)/oxalate exchange by mouse slc26a6 was electrogenic, that mediated by human SLC26A6 appeared electroneutral. The increased currents observed in oocytes expressing either mouse or human ortholog were pharmacologically distinct from the accompanying monovalent anion exchange activities. The human SLC26A6 polypeptide variants SLC26A6c and SLC26A6d were inactive as transporters of oxalate, sulfate, and chloride. Thus, the orthologous mouse and human SLC26A6

  18. Tens of micron-sized unilamellar nanosheets of Y/Eu layered rare-earth hydroxide: efficient exfoliation via fast anion exchange and their self-assembly into oriented oxide film with enhanced photoluminescence

    NASA Astrophysics Data System (ADS)

    Zhu, Qi; Li, Ji-Guang; Li, Xiaodong; Sun, Xudong; Qi, Yang; Zhu, Miaoyong; Sakka, Yoshio

    2014-02-01

    Layered rare-earth hydroxide (LRH) crystals of (Y0.95Eu0.05)2(OH)5NO3·nH2O with a lateral size of ˜ 300 μm and a thickness of ˜ 9 μm have been synthesized via a hydrothermal reaction of mixed nitrate solutions in the presence of mineralizer NH4NO3 at 200 °C for 24 h. LRH exhibits the ability to undergo intercalation and anion exchange with DS- (C12H25OSO3-) via hydrothermal treatment. Compared with traditional anion exchange at room temperature, hydrothermal processing not only shortens the anion exchange time from 720 to 24 h but also increases the basal spacing. The arrangements of DS- in the interlayer of LRH are significantly affected by the DS- concentration and reaction temperature, and the basal spacing of the LRH-DS sample in the crystal edge is assumed to be larger than that in the crystal center. A higher DS- concentration and reaction temperature both induce more intercalation of DS- anions into the interlayer gallery, thus yielding a larger basal spacing. Unilamellar nanosheets with a lateral size of ⩾60 μm and a thickness of ˜ 1.6 nm can be obtained by delaminating LRH-DS in formamide. The resultant unilamellar nanosheets are single crystalline. Transparent (Y0.95Eu0.05)2O3 phosphor films with a uniform [111] orientation and a layer thickness of ˜ 90 nm were constructed with the nanosheets as building blocks via spin-coating, followed by proper annealing. The oriented oxide film exhibits a strong red emission at 614 nm (the 5D0-7F2 transition of Eu3+), whose intensity is ˜ 2 times that of the powder form owing to the significant exposure of the (222) facets.

  19. Identification of a matrix effect in the MC-ICP-MS due to sample purification using ion exchange resin

    NASA Astrophysics Data System (ADS)

    Pietruszka, Aaron J.; Reznik, Audrey D.

    2008-02-01

    Multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) has become the preferred method for precise and accurate measurements of the relative abundances of many radiogenic and stable isotopes in natural materials. Isotopic analyses by MC-ICP-MS require a correction for instrumental mass-dependent isotopic fractionation ("instrumental mass bias"). Two techniques have been used to correct for instrumental mass bias in the MC-ICP-MS: (1) standard-sample bracketing (SSB) or (2) double spiking. SSB is often cited as the preferred method, but it is more susceptible to matrix effects. Here we demonstrate that a matrix effect in the MC-ICP-MS may arise indirectly from the chemical separation and purification of molybdenum using anion exchange resin. The results of our experiments show that a Mo standard passed through a column of anion exchange resin or a Mo standard added to a Mo-free solution that had been collected from anion exchange resin appears to be isotopically lighter than expected from direct analysis of the same standard. Using amounts of Mo similar to what might be expected from most natural samples (~3 [mu]g per column cut), these offsets span a significant fraction (~10-60%) of the total known range of mass-dependent Mo isotopic variation in nature. This "column matrix effect" appears to be caused by organic material stripped from the resin. All of our attempts to eliminate or control this column matrix effect have failed, making it difficult (if not impossible) to obtain accurate measurements of mass-dependent Mo isotopic variations in natural materials using the anion exchange resin procedure described in this study and SSB techniques to correct for instrumental mass bias in the MC-ICP-MS. It is currently unknown if this type of column matrix effect will affect measurements of other stable or radiogenic isotopes by MC-ICP-MS when SSB is used to correct for instrumental mass bias.

  20. Activity and distribution of intracellular carbonic anhydrase II and their effects on the transport activity of anion exchanger AE1/SLC4A1

    PubMed Central

    Al-Samir, Samer; Papadopoulos, Symeon; Scheibe, Renate J; Meißner, Joachim D; Cartron, Jean-Pierre; Sly, William S; Alper, Seth L; Gros, Gerolf; Endeward, Volker

    2013-01-01

    We have investigated the previously published ‘metabolon hypothesis’ postulating that a close association of the anion exchanger 1 (AE1) and cytosolic carbonic anhydrase II (CAII) exists that greatly increases the transport activity of AE1. We study whether there is a physical association of and direct functional interaction between CAII and AE1 in the native human red cell and in tsA201 cells coexpressing heterologous fluorescent fusion proteins CAII-CyPet and YPet-AE1. In these doubly transfected tsA201 cells, YPet-AE1 is clearly associated with the cell membrane, whereas CAII-CyPet is homogeneously distributed throughout the cell in a cytoplasmic pattern. Förster resonance energy transfer measurements fail to detect close proximity of YPet-AE1 and CAII-CyPet. The absence of an association of AE1 and CAII is supported by immunoprecipitation experiments using Flag-antibody against Flag-tagged AE1 expressed in tsA201 cells, which does not co-precipitate native CAII but co-precipitates coexpressed ankyrin. Both the CAII and the AE1 fusion proteins are fully functional in tsA201 cells as judged by CA activity and by cellular HCO3− permeability () sensitive to inhibition by 4,4′-Diisothiocyano-2,2′-stilbenedisulfonic acid. Expression of the non-catalytic CAII mutant V143Y leads to a drastic reduction of endogenous CAII and to a corresponding reduction of total intracellular CA activity. Overexpression of an N-terminally truncated CAII lacking the proposed site of interaction with the C-terminal cytoplasmic tail of AE1 substantially increases intracellular CA activity, as does overexpression of wild-type CAII. These variously co-transfected tsA201 cells exhibit a positive correlation between cellular and intracellular CA activity. The relationship reflects that expected from changes in cytoplasmic CA activity improving substrate supply to or removal from AE1, without requirement for a CAII–AE1 metabolon involving physical interaction. A functional

  1. Purification of gibberellin sub 53 -oxidase from spinach

    SciTech Connect

    Wilson, T.M.; Zeevaart, J.A.D. )

    1989-04-01

    Spinach is a long-day rosette plants, in which stem growth is mediated by gibberellins. It has been shown that two enzymatic steps, GA{sub 53}-oxidase and GA{sub 19}-oxidase, are controlled by light. To develop an understanding into this light regulation, purification of GA{sub 53}-oxidase has been undertaken. The original assay relied on the HPLC separation of the product and substrate, but was considered too slow for the development of a purification scheme. A TLC system was developed which in conjunction with improvements to the assay conditions was sensitive and gave rapid results. The partial purification of the GA{sub 53}-oxidase is achieved by a high speed centrifugation, 40-55% ammonium sulfate precipitation, an hydroxyapatite column, Sephadex G-100 column and an anion exchange FPLC column, Mono Q HR10/10, yielding 1000-fold purification and 15% recovery. Monoclonal antibodies to the protein will be raised and used to further characterize the enzyme.

  2. 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.

    PubMed

    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.

  3. Efficient expression and purification of biologically active human cystatin proteins.

    PubMed

    Chauhan, Sakshi; Tomar, Raghuvir S

    2016-02-01

    Cystatins are reversible cysteine protease inhibitor proteins. They are known to play important roles in controlling cathepsins, neurodegenerative disease, and in immune system regulation. Production of recombinant cystatin proteins is important for biochemical and function characterization. In this study, we cloned and expressed human stefin A, stefin B and cystatin C in Escherichia coli. Human stefin A, stefin B and cystatin C were purified from soluble fraction. For cystatin C, we used various chaperone plasmids to make cystatin C soluble, as it is reported to localize in inclusion bodies. Trigger factor, GroES-GroEL, DnaK-DnaJ-GrpE chaperones lead to the presence of cystatin C in the soluble fraction. Immobilized metal affinity chromatography, glutathione sepharose and anion exchange chromatography techniques were employed for efficient purification of these proteins. Their biological activities were tested by inhibition assays against cathepsin L and H3 protease.

  4. Advanced purification strategy for CueR, a cysteine containing copper(I) and DNA binding protein.

    PubMed

    Balogh, Ria K; Gyurcsik, Béla; Hunyadi-Gulyás, Éva; Christensen, Hans E M; Jancsó, Attila

    2016-07-01

    Metal ion regulation is essential for living organisms. In prokaryotes metal ion dependent transcriptional factors, the so-called metalloregulatory proteins play a fundamental role in controlling the concentration of metal ions. These proteins recognize metal ions with an outstanding selectivity. A detailed understanding of their function may be exploited in potential health, environmental and analytical applications. Members of the MerR protein family sense a broad range of mostly late transition and heavy metal ions through their cysteine thiolates. The air sensitivity of latter groups makes the expression and purification of such proteins challenging. Here we describe a method for the purification of the copper-regulatory CueR protein under optimized conditions. In order to avoid protein precipitation and/or eventual aggregation and to get rid of the co-purifying Escherichia coli elongation factor, our procedure consisted of four steps supplemented by DNA digestion. Subsequent anion exchange on Sepharose FF Q 16/10, affinity chromatography on Heparin FF 16/10, second anion exchange on Source 30 Q 16/13 and gel filtration on Superdex 75 26/60 resulted in large amounts of pure CueR protein without any affinity tag. Structure and functionality tests performed with mass spectrometry, circular dichroism spectroscopy and electrophoretic gel mobility shift assays approved the success of the purification procedure.

  5. ERYTHROPOIETIC FACTOR PURIFICATION

    DOEpatents

    White, W.F.; Schlueter, R.J.

    1962-05-01

    A method is given for purifying and concentrating the blood plasma erythropoietic factor. Anemic sheep plasma is contacted three times successively with ion exchange resins: an anion exchange resin, a cation exchange resin at a pH of about 5, and a cation exchange resin at a pH of about 6. (AEC)

  6. Centrifugal partition chromatography as a tool for preparative purification of pea albumin with enhanced yields.

    PubMed

    Bérot, Serge; Le Goff, Elisabeth; Foucault, Alain; Quillien, Laurence

    2007-01-15

    A new procedure including the use of centrifugal partition chromatography (CPC) is proposed to purify PA1b and its isoforms. These pea (Pisum sativum L.) seed proteins are toxic against weevils and can be used as an environment-friendly insecticide. CPC was applied to a whole albumin fraction prepared from pea flour. The butanol:aqueous TFA system used in CPC allowed the separation of PA1b from other albumins and a degree of purification above 95%. Compared to analytical procedures based on methanol extraction, anion exchange and then reversed-phase chromatography (RPC), CPC recovered PA1b in much better yield, which is indispensable for large-scale purification of a biodegradable insecticide.

  7. High pH solubilization and chromatography-based renaturation and purification of recombinant human granulocyte colony-stimulating factor from inclusion bodies.

    PubMed

    Li, Ming; Fan, Hua; Liu, Jiahua; Wang, Minhong; Wang, Lili; Wang, Chaozhan

    2012-03-01

    Recombinant human granulocyte colony-stimulating factor (rhG-CSF) is a very efficient therapeutic protein drug which has been widely used in human clinics to treat cancer patients suffering from chemotherapy-induced neutropenia. In this study, rhG-CSF was solubilized from inclusion bodies by using a high-pH solution containing low concentration of urea. It was found that solubilization of the rhG-CSF inclusion bodies greatly depended on the buffer pH employed; alkalic pH significantly favored the solubilization. In addition, when small amount of urea was added to the solution at high pH, the solubilization was further enhanced. After solubilization, the rhG-CSF was renatured with simultaneous purification by using weak anion exchange, strong anion exchange, and hydrophobic interaction chromatography, separately. The results indicated that the rhG-CSF solubilized by the high-pH solution containing low concentration of urea had much higher mass recovery than the one solubilized by 8 M urea when using anyone of the three refolding methods employed in this work. In the case of weak anion exchange chromatography, the high pH solubilized rhG-CSF could get a mass recovery of 73%. The strategy of combining solubilization of inclusion bodies at high pH with refolding of protein using liquid chromatography may become a routine method for protein production from inclusion bodies.

  8. Automated DNA Sequencing System

    SciTech Connect

    Armstrong, G.A.; Ekkebus, C.P.; Hauser, L.J.; Kress, R.L.; Mural, R.J.

    1999-04-25

    Oak Ridge National Laboratory (ORNL) is developing a core DNA sequencing facility to support biological research endeavors at ORNL and to conduct basic sequencing automation research. This facility is novel because its development is based on existing standard biology laboratory equipment; thus, the development process is of interest to the many small laboratories trying to use automation to control costs and increase throughput. Before automation, biology Laboratory personnel purified DNA, completed cycle sequencing, and prepared 96-well sample plates with commercially available hardware designed specifically for each step in the process. Following purification and thermal cycling, an automated sequencing machine was used for the sequencing. A technician handled all movement of the 96-well sample plates between machines. To automate the process, ORNL is adding a CRS Robotics A- 465 arm, ABI 377 sequencing machine, automated centrifuge, automated refrigerator, and possibly an automated SpeedVac. The entire system will be integrated with one central controller that will direct each machine and the robot. The goal of this system is to completely automate the sequencing procedure from bacterial cell samples through ready-to-be-sequenced DNA and ultimately to completed sequence. The system will be flexible and will accommodate different chemistries than existing automated sequencing lines. The system will be expanded in the future to include colony picking and/or actual sequencing. This discrete event, DNA sequencing system will demonstrate that smaller sequencing labs can achieve cost-effective the laboratory grow.

  9. Purification of phosphatidylinositol kinase from bovine brain myelin.

    PubMed Central

    Saltiel, A R; Fox, J A; Sherline, P; Sahyoun, N; Cuatrecasas, P

    1987-01-01

    A membrane-bound phosphatidylinositol (PI) kinase (EC 2.7.1.67) was purified by affinity chromatography from bovine brain myelin. This enzyme activity was solubilized with non-ionic detergent and chromatographed on an anion-exchange column. Further purification was achieved by affinity chromatography on PI covalently coupled to epoxy-activated Sepharose, which was eluted with a combination of PI and detergent. The final step in the purification was by gel filtration on an Ultrogel AcA44 column. This procedure afforded greater than 5500-fold purification of the enzyme from whole brain myelin. The resulting activity exhibited a major silver-stained band on SDS/polyacrylamide-gel electrophoresis with an apparent Mr 45,000. The identity of this band as PI kinase was corroborated by demonstration of enzyme activity in the gel region corresponding to that of the stained protein. The purified enzyme exhibited a non-linear dependence on PI as substrate, with two apparent kinetic components. The lower-affinity component exhibited a Km similar to that observed for the phosphorylation of phosphatidylinositol 4-phosphate by the enzyme. PMID:3036072

  10. Sensitive determination of aspirin and its metabolites in plasma by LC-UV using on-line solid-phase extraction with methylcellulose-immobilized anion-exchange restricted access media.

    PubMed

    Yamamoto, Eiichi; Takakuwa, Susumu; Kato, Takashi; Asakawa, Naoki

    2007-02-01

    We describe a sensitive determination of aspirin (ASA) and its three metabolites (salicylic acid [SA], 2,3-dihydroxybenzoic acid [2,3-DHBA], and 2,5-dihydroxybenzoic acid [gentisic acid (GA)]) in rat plasma. Analysis was carried out by on-line solid-phase extraction (SPE) using a methylcellulose-immobilized-strong anion-exchanger (MC-SAX), followed by liquid chromatography (LC) coupled with UV detection. The lower limits of quantitation for ASA and SA were 60 ng/mL in 100 microL of plasma, respectively. This method was validated with respect to intra- and inter-day precision, accuracy, and linearity up to concentrations of 20,000 ng/mL for ASA, SA, 2,3-DHBA and gentisic acid, respectively. The method was successfully applied to an analysis of the pharmacokinetics of ASA and SA in rats. PMID:16959551

  11. Method of uranium reclamation from aqueous systems by reactive ion exchange. [US DOE patent application; anion exchange resin of copolymerized divinyl-benzene and styrene having quarternary ammonium groups and bicarbonate ligands

    DOEpatents

    Maya, L.

    1981-11-05

    A reactive ion exchange method for separation and recovery of values of uranium, neptunium, plutonium, or americium from substantially neutral aqueous systems of said metals comprises contacting said system with an effective amount of a basic anion exchange resin of copolymerized divinyl-benzene and styrene having quarternary ammonium groups and bicarbonate ligands to achieve nearly 100% sorption of said actinyl ion onto said resin and an aqueous system practically free of said actinyl ions. The method is operational over an extensive range of concentrations from about 10/sup -6/ M to 1.0 M actinyl ion and a pH range of about 4 to 7. The method has particulr application to treatment of waste streams from Purex-type nuclear fuel reprocessing facilities and hydrometallurgical processes involving U, Np, P, or Am.

  12. An empirical study into the effect of long term storage (-36±2 °C) of electron-beamed ETFE on the properties of radiation-grafted alkaline anion-exchange membranes

    NASA Astrophysics Data System (ADS)

    Kizewski, Jamie Peter; Mudri, Nurul H.; Varcoe, John R.

    2013-08-01

    The application of alkaline anion-exchange membranes (AAEM) in solid alkaline fuel cells is growing in prominence mainly due to enhanced tolerance to carbon dioxide, compared to alkaline fuel cells containing aqueous electrolytes, and the potential for using non precious metal catalysts. Radiation grafting is a common methodology for the production of functional polymers and membranes. This statistical study examines the synthesis of radiation grafted AAEMs that are formed from electron beam irradiated poly(ethylene-co-tetrafluoroethylene), EB-ETFE. It is shown that EB-ETFE can be cold stored for at least 16 months and still be used to produce ionically conductive AAEMs. The limitations of routine measurements of properties, such as dimensional increases, ion-exchange capacity, water uptakes and ionic conductivities, are also highlighted.

  13. Determination of a flame retardant hydrolysis product in human urine by SPE and LC-MS. Comparison of molecularly imprinted solid-phase extraction with a mixed-mode anion exchanger.

    PubMed

    Möller, Kristina; Crescenzi, Carlo; Nilsson, Ulrika

    2004-01-01

    Diphenyl phosphate is a hydrolysis product and possible metabolite of the flame retardant and plasticiser additive triphenyl phosphate. A molecularly imprinted polymer solid-phase extraction (MISPE) method for extracting diphenyl phosphate from aqueous solutions has been developed and compared with SPE using a commercially available mixed-mode anion exchanger. The imprinted polymer was prepared using 2-vinylpyridine (2-Vpy) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, and a structural analogue of the analyte as the template molecule. The imprinted polymer was evaluated for use as a SPE sorbent, in tests with both aqueous standards and spiked urine samples, by comparing recovery and breakthrough data obtained using the imprinted form of the polymer and a non-imprinted form (NIP). Extraction from aqueous solutions resulted in more than 80% recovery. Adsorption by the molecularly imprinted polymer (MIP) was non-selective, but selectivity was achieved by selective desorption in the wash steps. Diphenyl phosphate could also be selectively extracted from urine samples, although the urine matrix reduced the capacity of the MISPE cartridges. Recoveries from urine extraction were higher than 70%. It was important to control pH during sample loading. The MISPE method was found to yield a less complex LC-ESI-MS chromatogram of the urine extracts compared with the mixed-mode anion-exchanger method. An LC-ESI-MS method using a Hypercarb LC column with a graphitised carbon stationary phase was also evaluated for organophosphate diesters. LC-ESI-MS using negative-ion detection in selected ion monitoring (SIM) mode was shown to be linear for diphenyl phosphate in the range 0.08-20 ng microL(-1). PMID:14614582

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

    PubMed

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

    2012-05-01

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

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

    PubMed

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

    2016-02-01

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

  16. Improved synthesis of [(18)F]FLETT via a fully automated vacuum distillation method for [(18)F]2-fluoroethyl azide purification.

    PubMed

    Ackermann, Uwe; Plougastel, Lucie; Goh, Yit Wooi; Yeoh, Shinn Dee; Scott, Andrew M

    2014-12-01

    The synthesis of [(18)F]2-fluoroethyl azide and its subsequent click reaction with 5-ethynyl-2'-deoxyuridine (EDU) to form [(18)F]FLETT was performed using an iPhase FlexLab module. The implementation of a vacuum distillation method afforded [(18)F]2-fluoroethyl azide in 87±5.3% radiochemical yield. The use of Cu(CH3CN)4PF6 and TBTA as catalyst enabled us to fully automate the [(18)F]FLETT synthesis without the need for the operator to enter the radiation field. [(18)F]FLETT was produced in higher overall yield (41.3±6.5%) and shorter synthesis time (67min) than with our previously reported manual method (32.5±2.5% in 130min).

  17. Extraction, purification, methylation and GC-MS analysis of short-chain carboxylic acids for metabolic flux analysis.

    PubMed

    Tivendale, Nathan D; Jewett, Erin M; Hegeman, Adrian D; Cohen, Jerry D

    2016-08-15

    Dynamic metabolic flux analysis requires efficient and effective methods for extraction, purification and analysis of a plethora of naturally-occurring compounds. One area of metabolism that would be highly informative to study using metabolic flux analysis is the tricarboxylic acid (TCA) cycle, which consists of short-chain carboxylic acids. Here, we describe a newly-developed method for extraction, purification, derivatization and analysis of short-chain carboxylic acids involved in the TCA cycle. The method consists of snap-freezing the plant material, followed by maceration and a 12-15h extraction at -80 °C. The extracts are then subject to reduction (to stabilize β-keto acids), purified by strong anion exchange solid phase extraction and methylated with methanolic HCl. This method could also be readily adapted to quantify many other short-chain carboxylic acids.

  18. Extraction, purification, methylation and GC-MS analysis of short-chain carboxylic acids for metabolic flux analysis.

    PubMed

    Tivendale, Nathan D; Jewett, Erin M; Hegeman, Adrian D; Cohen, Jerry D

    2016-08-15

    Dynamic metabolic flux analysis requires efficient and effective methods for extraction, purification and analysis of a plethora of naturally-occurring compounds. One area of metabolism that would be highly informative to study using metabolic flux analysis is the tricarboxylic acid (TCA) cycle, which consists of short-chain carboxylic acids. Here, we describe a newly-developed method for extraction, purification, derivatization and analysis of short-chain carboxylic acids involved in the TCA cycle. The method consists of snap-freezing the plant material, followed by maceration and a 12-15h extraction at -80 °C. The extracts are then subject to reduction (to stabilize β-keto acids), purified by strong anion exchange solid phase extraction and methylated with methanolic HCl. This method could also be readily adapted to quantify many other short-chain carboxylic acids. PMID:27348709

  19. Strep-Tagged Protein Purification.

    PubMed

    Maertens, Barbara; Spriestersbach, Anne; Kubicek, Jan; Schäfer, Frank

    2015-01-01

    The Strep-tag system can be used to purify recombinant proteins from any expression system. Here, protocols for lysis and affinity purification of Strep-tagged proteins from E. coli, baculovirus-infected insect cells, and transfected mammalian cells are given. Depending on the amount of Strep-tagged protein in the lysate, a protocol for batch binding and subsequent washing and eluting by gravity flow can be used. Agarose-based matrices with the coupled Strep-Tactin ligand are the resins of choice, with a binding capacity of up to 9 mg ml(-1). For purification of lower amounts of Strep-tagged proteins, the use of Strep-Tactin magnetic beads is suitable. In addition, Strep-tagged protein purification can also be automated using prepacked columns for FPLC or other liquid-handling chromatography instrumentation, but automated purification is not discussed in this protocol. The protocols described here can be regarded as an update of the Strep-Tag Protein Handbook (Qiagen, 2009).

  20. Strep-Tagged Protein Purification.

    PubMed

    Maertens, Barbara; Spriestersbach, Anne; Kubicek, Jan; Schäfer, Frank

    2015-01-01

    The Strep-tag system can be used to purify recombinant proteins from any expression system. Here, protocols for lysis and affinity purification of Strep-tagged proteins from E. coli, baculovirus-infected insect cells, and transfected mammalian cells are given. Depending on the amount of Strep-tagged protein in the lysate, a protocol for batch binding and subsequent washing and eluting by gravity flow can be used. Agarose-based matrices with the coupled Strep-Tactin ligand are the resins of choice, with a binding capacity of up to 9 mg ml(-1). For purification of lower amounts of Strep-tagged proteins, the use of Strep-Tactin magnetic beads is suitable. In addition, Strep-tagged protein purification can also be automated using prepacked columns for FPLC or other liquid-handling chromatography instrumentation, but automated purification is not discussed in this protocol. The protocols described here can be regarded as an update of the Strep-Tag Protein Handbook (Qiagen, 2009). PMID:26096503

  1. Anion-exchange and anthracene-encapsulation within copper(II) and manganese(II)-triazole metal-organic confined space in a single crystal-to-single crystal transformation fashion.

    PubMed

    Liu, Ju-Yan; Wang, Qian; Zhang, Li-Jun; Yuan, Bin; Xu, Yao-Yao; Zhang, Xin; Zhao, Cong-Ying; Wang, Dan; Yuan, Yue; Wang, Ying; Ding, Bin; Zhao, Xiao-Jun; Yue, Min Min

    2014-06-16

    A new multidentate ligand 1-(9-(1H-1,2,4-triazol-1-yl)anthracen-10-yl)-1H-1,2,4-triazole (tatrz) was designed and synthesized. Using tatrz as a building block, three novel coordination frameworks, namely, {[Cu(tatrz)2(NO3)2]·(CH3OH)·4H2O}n (1), {[Cu(tatrz)2(H2O)2](BF4)2}n (2), and [Mn(tatrz)2(SCN)2(CH3OH)]·2H2O (3) can be isolated. Anion-exchange experiment indicates that NO3(-) anions in the two-dimensional (2D) copper framework of 1 can be completely exchanged by ClO4(-) in an irreversible single crystal-to-single crystal (SC-SC) transformation fashion, as evidenced by the anion-exchange products of {[Cu(tatrz)2(H2O)2](ClO4)2·4CH3OH} (1a). Further, if 1a was employed as a precursor in N,N-dimethylformamide (DMF), an isomorphic solvate of {[Cu(tatrz)2(DMF)2](ClO4)2·2H2O}n (1b) can be generated during the reversible dynamic transformation process. When 1 was immersed in CH3OH, a distinct 2D layer {[Cu(tatrz)2(NO3)2]·4.4CH3OH·0.6H2O}n (1c) was isolated. Interestingly, the solvent-exchange conversion is also invertible between 1 and 1c, which exhibits spongelike dynamic behavior with retention of crystalline integrity. If the 2-fold interpenetrating three-dimensional (3D) framework 2 is selected, it can be transformed into another 2-fold interpenetrating 3D framework {[Cu(tatrz)2(H2O)2](ClO4)2·5.56H2O}n (2a) in a reversible SC-SC transformation fashion. However, when the light yellow crystals of mononuclear complex 3 were exposed to trichloromethane containing aromatic organic anthracene (atan), through our careful observation, the crystals of 3 were dissolved and reassembled into dark brown crystals of 2D crystalline coordination framework {[Mn(tatrz)2(SCN)2]·(atan)}n (3a). X-ray diffraction revealed that in 3a, atan acting as an organic template was encapsulated in the confined space of the 2D grid. Luminescent measurements illustrate that 3a is the first report of multidimensional polymers based on triazole derivatives as luminescent probes of Mg(2+).

  2. Hamiltonian purification

    SciTech Connect

    Orsucci, Davide; Burgarth, Daniel; Facchi, Paolo; Pascazio, Saverio; Nakazato, Hiromichi; Yuasa, Kazuya; Giovannetti, Vittorio

    2015-12-15

    The problem of Hamiltonian purification introduced by Burgarth et al. [Nat. Commun. 5, 5173 (2014)] is formalized and discussed. Specifically, given a set of non-commuting Hamiltonians (h{sub 1}, …, h{sub m}) operating on a d-dimensional quantum system ℋ{sub d}, the problem consists in identifying a set of commuting Hamiltonians (H{sub 1}, …, H{sub m}) operating on a larger d{sub E}-dimensional system ℋ{sub d{sub E}} which embeds ℋ{sub d} as a proper subspace, such that h{sub j} = PH{sub j}P with P being the projection which allows one to recover ℋ{sub d} from ℋ{sub d{sub E}}. The notions of spanning-set purification and generator purification of an algebra are also introduced and optimal solutions for u(d) are provided.

  3. Hamiltonian purification

    NASA Astrophysics Data System (ADS)

    Orsucci, Davide; Burgarth, Daniel; Facchi, Paolo; Nakazato, Hiromichi; Pascazio, Saverio; Yuasa, Kazuya; Giovannetti, Vittorio

    2015-12-01

    The problem of Hamiltonian purification introduced by Burgarth et al. [Nat. Commun. 5, 5173 (2014)] is formalized and discussed. Specifically, given a set of non-commuting Hamiltonians {h1, …, hm} operating on a d-dimensional quantum system ℋd, the problem consists in identifying a set of commuting Hamiltonians {H1, …, Hm} operating on a larger dE-dimensional system ℋdE which embeds ℋd as a proper subspace, such that hj = PHjP with P being the projection which allows one to recover ℋd from ℋdE. The notions of spanning-set purification and generator purification of an algebra are also introduced and optimal solutions for 𝔲(d) are provided.

  4. Assay, Purification, and Partial Characterization of Choline Monooxygenase from Spinach.

    PubMed

    Burnet, M.; Lafontaine, P. J.; Hanson, A. D.

    1995-06-01

    The osmoprotectant glycine betaine is synthesized via the path-way choline -> betaine aldehyde -> glycine betaine. In spinach (Spinacia oleracea), the first step is catalyzed by choline monooxygenase (CMO), and the second is catalyzed by betaine aldehyde dehydrogenase. Because betaine aldehyde is unstable and not easily detected, we developed a coupled radiometric assay for CMO. [14C]Choline is used as substrate; NAD+ and betaine aldehyde dehydrogenase prepared from Escherichia coli are added to oxidize [14C]betaine aldehyde to [14C]glycine betaine, which is isolated by ion exchange. The assay was used in the purification of CMO from leaves of salinized spinach. The 10-step procedure included polyethylene glycol precipitation, polyethyleneimine precipitation, hydrophobic interaction, anion exchange on choline-Sepharose, dimethyldiethanolamine-Sepharose, and Mono Q, hydroxyapatite, gel filtration, and sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Following gel filtration, overall purification was about 600-fold and recovery of activity was 0.5%. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis showed a polypeptide with a molecular mass of 45 kD. Taken with the value of 98 kD estimated for native CMO (R. Brouquisse, P. Weigel, D. Rhodes, C.F. Yocum, A.D. Hanson [1989] Plant Physiol 90: 322-329), this indicates that CMO is a homodimer. CMO preparations were red-brown, showed absorption maxima at 329 and 459 nm, and lost color upon dithionite addition, suggesting that CMO is an iron-sulfur protein.

  5. Purification and characterization of paraoxon hydrolase from rat liver.

    PubMed Central

    Rodrigo, L; Gil, F; Hernandez, A F; Marina, A; Vazquez, J; Pla, A

    1997-01-01

    Paraoxonase (paraoxon hydrolase), an enzyme that hydrolyses paraoxon (O,O-diethyl O-p-nitrophenyl phosphate), is located in mammals primarily in the serum and liver. Although considerable information is available regarding serum paraoxonase, little is known about the hepatic form of this enzyme. The present work represents the first study on the purification of rat liver paraoxonase. This enzyme has been purified 415-fold to apparent homogeneity with a final specific activity of 1370 units/mg using a protocol consisting of five steps: solubilization of the microsomal fraction, hydroxyapatite adsorption, chromatography on DEAE-Sepharose CL-6B, non-specific affinity chromatography on Cibacron Blue 3GA and anion exchange on Mono Q HR 5/5. The presence of Ca2+ and Triton X-100 in the buffers throughout the purification procedure was essential for maintaining enzyme activity. SDS/PAGE of the final preparation indicated a single protein-staining band with an apparent Mr of 45 000. N-terminal and internal amino acid sequences were determined and compared with those of paraoxonases from human and rabbit serum and mouse liver, showing a high similarity. The pH profile showed optimum activity at pH 8.5. The pH stability and heat inactivation of the enzyme were also studied. The Km for liver paraoxonase was 1.69 mM. PMID:9032442

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

    PubMed

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

    2006-12-01

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

  7. Polybenzimidazole-crosslinked poly(vinylbenzyl chloride) with quaternary 1,4-diazabicyclo (2.2.2) octane groups as high-performance anion exchange membrane for fuel cells

    NASA Astrophysics Data System (ADS)

    Lu, Wangting; Zhang, Geng; Li, Jin; Hao, Jinkai; Wei, Feng; Li, Wenhui; Zhang, Jiying; Shao, Zhi-Gang; Yi, Baolian

    2015-11-01

    Development of anion exchange membrane (AEM) with high conductivity, good dimensional stability, desirable toughness and long life-time simultaneously is still a challenge for the practical application of AEM fuel cells. Herein, a novel AEM (denoted as PBI-c-PVBC/OH) is fabricated by applying polybenzimidazole (PBI) and 1,4-diazabicyclo (2.2.2) octane (DABCO) as the macromolecular crosslinker and quaternizing reagent for poly(vinylbenzyl chloride) (PVBC), respectively. With the aid of crosslinking by PBI, PBI-c-PVBC/OH exhibits good flexibility and strength both in dry and water-saturated state. Moreover, high hydroxide conductivity (>25 mS cm-1 at room temperature) and low swelling ratio (∼13%) is obtained, especially the swelling ratio nearly does not increase with temperature. The membrane is also advanced for the superior chemical stability in alkaline environment due to the stable polymer backbone and ionic conductive group (only one nitrogen atom in a DABCO molecule is quaternized). Furthermore, a peak power density of 230 mW cm-2 at 50 °C is obtained on the H2/O2 fuel cell using PBI-c-PVBC/OH, and the membrane presents high durability both in the constant current and continuous open circuit voltage testing. Therefore, it is considered that the PBI crosslinking together with DABCO quaternization can be regarded as a promising strategy in the development of AEM for fuel cells.

  8. High-performance liquid chromatography separation of cis-trans anthocyanin isomers from wild Lycium ruthenicum Murr. employing a mixed-mode reversed-phase/strong anion-exchange stationary phase.

    PubMed

    Jin, Hongli; Liu, Yanfang; Guo, Zhimou; Yang, Fan; Wang, Jixia; Li, Xiaolong; Peng, Xiaojun; Liang, Xinmiao

    2015-01-21

    The cis-trans isomerism is a common phenomenon for acylated anthocyanins. Nevertheless, few studies reported effective methods for the preparation of isomeric anthocyanins from natural products. In this work, a high-performance liquid chromatography (HPLC) method was developed to efficiently purify anthocyanin isomers from Lycium ruthenicum Murr. based on a mixed-mode reversed-phase/strong anion-exchange column (named XCharge C8SAX). Four commercially available columns were evaluated with a pair of isomeric anthocyanins, and the results demonstrated that the XCharge C8SAX column exhibited improved selectivity and column efficiency for the isomers. The chromatographic parameters, including pH, organic content, and ionic strength, were investigated. Optimal separation quality for the anthocyanin isomers was achieved on the XCharge C8SAX column. Six pure anthocyanins, including two pairs of cis-trans isomeric anthocyanins with one new anthocyanin, were purified from L. ruthenicum and identified. All of the results indicated that this method is an effective way to separate anthocyanins, especially for cis-trans isomers. PMID:25539032

  9. Nitrogen-induced surface area and conductivity modulation of carbon nanohorn and its function as an efficient metal-free oxygen reduction electrocatalyst for anion-exchange membrane fuel cells.

    PubMed

    Unni, Sreekuttan M; Bhange, Siddheshwar N; Illathvalappil, Rajith; Mutneja, Nisha; Patil, Kasinath R; Kurungot, Sreekumar

    2015-01-21

    Nitrogen-doped carbon morphologies have been proven to be better alternatives to Pt in polymer-electrolyte membrane (PEM) fuel cells. However, efficient modulation of the active sites by the simultaneous escalation of the porosity and nitrogen doping, without affecting the intrinsic electrical conductivity, still remains to be solved. Here, a simple strategy is reported to solve this issue by treating single-walled carbon nanohorn (SWCNH) with urea at 800 °C. The resulting nitrogen-doped carbon nanohorn shows a high surface area of 1836 m2 g(-1) along with an increased electron conductivity, which are the pre-requisites of an electrocatalyst. The nitrogen-doped nanohorn annealed at 800 °C (N-800) also shows a high oxygen reduction activity (ORR). Because of the high weight percentage of pyridinic nitrogen coordination in N-800, the present catalyst shows a clear 4-electron reduction pathway at only 50 mV overpotential and 16 mV negative shift in the half-wave potential for ORR compared to Pt/C along with a high fuel selectivity and electrochemical stability. More importantly, a membrane electrode assembly (MEA) based on N-800 provides a maximum power density of 30 mW cm(-2) under anion-exchange membrane fuel cell (AEMFC) testing conditions. Thus, with its remarkable set of physical and electrochemical properties, this material has the potential to perform as an efficient Pt-free electrode for AEMFCs.

  10. 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.

    PubMed

    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.

  11. High-performance liquid chromatography separation of cis-trans anthocyanin isomers from wild Lycium ruthenicum Murr. employing a mixed-mode reversed-phase/strong anion-exchange stationary phase.

    PubMed

    Jin, Hongli; Liu, Yanfang; Guo, Zhimou; Yang, Fan; Wang, Jixia; Li, Xiaolong; Peng, Xiaojun; Liang, Xinmiao

    2015-01-21

    The cis-trans isomerism is a common phenomenon for acylated anthocyanins. Nevertheless, few studies reported effective methods for the preparation of isomeric anthocyanins from natural products. In this work, a high-performance liquid chromatography (HPLC) method was developed to efficiently purify anthocyanin isomers from Lycium ruthenicum Murr. based on a mixed-mode reversed-phase/strong anion-exchange column (named XCharge C8SAX). Four commercially available columns were evaluated with a pair of isomeric anthocyanins, and the results demonstrated that the XCharge C8SAX column exhibited improved selectivity and column efficiency for the isomers. The chromatographic parameters, including pH, organic content, and ionic strength, were investigated. Optimal separation quality for the anthocyanin isomers was achieved on the XCharge C8SAX column. Six pure anthocyanins, including two pairs of cis-trans isomeric anthocyanins with one new anthocyanin, were purified from L. ruthenicum and identified. All of the results indicated that this method is an effective way to separate anthocyanins, especially for cis-trans isomers.

  12. URANIUM RECOVERY AND PURIFICATION PROCESS AND PRODUCTION OF HIGH PURITY URANIUM TETRAFLUORIDE

    DOEpatents

    Bailes, R.H.; Long, R.S.; Grinstead, R.R.

    1957-09-17

    A process is described wherein an anionic exchange technique is employed to separate uramium from a large variety of impurities. Very efficient and economical purification of contamimated uranium can be achieved by treatment of the contaminated uranium to produce a solution containing a high concentration of chloride. Under these conditions the uranium exists as an aniomic chloride complex. Then the uranium chloride complex is adsorbed from the solution on an aniomic exchange resin, whereby a portion of the impurities remain in the solution and others are retained with the uramium by the resin. The adsorbed impurities are then removed by washing the resin with pure concentrated hydrochloric acid, after which operation the uranium is eluted with pure water yielding an acidic uranyl chloride solution of high purity.

  13. Automation in medicinal chemistry.

    PubMed

    Reader, John C

    2004-01-01

    The implementation of appropriate automation can make a significant improvement in productivity at each stage of the drug discovery process, if it is incorporated into an efficient overall process. Automated chemistry has evolved rapidly from the 'combinatorial' techniques implemented in many industrial laboratories in the early 1990's which focused primarily on the hit discovery phase, and were highly dependent on solid-phase techniques and instrumentation derived from peptide synthesis. Automated tools and strategies have been developed which can impact the hit discovery, hit expansion and lead optimization phases, not only in synthesis, but also in reaction optimization, work-up, and purification of compounds. This article discusses the implementation of some of these techniques, based especially on experiences at Millennium Pharmaceuticals Research and Development Ltd.

  14. Polonium purification

    SciTech Connect

    Baker, J.D.

    1996-09-01

    Three processes for the purification of {sup 210}Po from irradiated bismuth targets are described. Safety equipment includes shielded hotcells for the initial separation from other activation products, gloveboxes for handling the volatile and highly toxic materials, and provisions for ventilation. All chemical separations must be performed under vacuum or in inerted systems. Two of the processes require large amounts of electricity; the third requires vessels made from exotic materials.

  15. Pool Purification

    NASA Technical Reports Server (NTRS)

    1988-01-01

    Caribbean Clear, Inc. used NASA's silver ion technology as a basis for its automatic pool purifier. System offers alternative approach to conventional purification chemicals. Caribbean Clear's principal markets are swimming pool owners who want to eliminate chlorine and bromine. Purifiers in Caribbean Clear System are same silver ions used in Apollo System to kill bacteria, plus copper ions to kill algae. They produce spa or pool water that exceeds EPA Standards for drinking water.

  16. Purification and Characterization of Chloroplastic NADP-Isocitrate Dehydrogenase from Mixotrophic Tobacco Cells (Comparison with the Cytosolic Isoenzyme).

    PubMed Central

    Galvez, S.; Bismuth, E.; Sarda, C.; Gadal, P.

    1994-01-01

    Green, mixotrophic tobacco (Nicotiana tabacum) cell cultures in the exponential growth phase were found to have two clearly distinguishable NADP-isocitrate dehydrogenase (ICDH; EC 1.1.1.42) isoenzymes. Their elution behavior during anion-exchange column chromatography was similar to that described previously for the cytosolic (ICDH1) and chloroplastic (ICDH2) enzymes from pea (Pisum sativum) leaves. ICDH2 was absent in etiolated tobacco cell suspensions and appeared during the greening process. Both isoforms were purified to apparent electrophoretic homogeneity by ammonium sulfate fractionation and anion-exchange and affinity chromatography. The isoenzymes were separated on a DEAE-Sephacel column, but the most effective step was a Matrex Red-A column, which enabled an overall purification of 833- and 1328-fold for ICDH1 and ICDH2, respectively. Polyclonal antibodies were raised against each isoform. The ICDH2-specific antibody was used to localize tobacco leaf ICDH2 in situ by an immunogold labeling technique. The enzyme was found largely, if not exclusively, in the chloroplasts of green leaves. ICDH1 and ICDH2 were shown to have apparent native molecular weights of 117,000 and 136,000, respectively, and to consist of identical, 48.5-kD subunits. Similar apparent Km values for NADP, D(+)isocitrate, and Mg2+ were found for the two enzymes when assayed with Mg2+ as the metal cofactor. PMID:12232226

  17. Efficiency of pretreatment of aqueous samples using a macroporous strong anion-exchange resin on the determination of nerve gas hydrolysis products by gas chromatography-mass spectrometry after tert.-butyldimethylsilylation.

    PubMed

    Kataoka, M; Tsuge, K; Seto, Y

    2000-09-01

    A pretreatment procedure, using a macroporous strong anion-exchange resin (MSA) has been established for the determination of nerve gas hydrolysis products by gas chromatography-mass spectrometry (GC-MS) after tert.-butyldimethylsilyl (TBDMS) derivatization. Aqueous solutions of methylphosphonic acid (MPA) and three alkyl methylphosphonic acids (AMPAs) (ethyl, isopropyl and pinacolyl methylphosphonic acid), were retained on the MSA column, and then quantitatively eluted with 0.1 M hydrochloric acid. The neutralized column eluate was dried, and MPA and AMPAs were derivatized with N-methyl-N-(tert.-butyldimethylsilyl)-trifluoroacetamide and analyzed by GC-MS. The column eluate was also analyzed in order to determine the exact hydrolysis product levels by capillary electrophoresis using borate and benzoate buffer (pH 6). The MSA pretreatment was examined for the clean-up of aqueous extracts of three types of soils and an aqueous solution containing 10% sucrose, which is regarded as model for a typical soft drink, after spiking with MPA and AMPAs. MPA and AMPAs were quantitatively recovered in the MSA eluate fraction from those samples, except for MPA from volcanic acid and alluvial soils. The yields of TBDMS derivatives were remarkably improved, compared with for which no pretreatment was used and also for those in which a strong cation-exchange resin was used. The achieved detection limits of MPA and AMPAs ranged from 0.12 to 0.18 microg/g of soil (S/N=3). The established MSA method was applied to the pretreatment of spiked sea water, two types of beverages, Pepsi Cola and canned coffee. Although the yields of TBDMS derivatives of MPA and AMPAs in sea water (in a range between 44 and 96%) and AMPAs in Pepsi Cola (in a range between 58 and 92%) were rather high, those for MPA in the Pepsi Cola (27%) and those for MPA and AMPAs in the canned coffee (in a range between 5 and 17%) were low.

  18. Sequential photocatalyst-assisted digestion and vapor generation device coupled with anion exchange chromatography and inductively coupled plasma mass spectrometry for speciation analysis of selenium species in biological samples.

    PubMed

    Tsai, Yun-ni; Lin, Cheng-hsing; Hsu, I-hsiang; Sun, Yuh-chang

    2014-01-01

    We have developed an on-line sequential photocatalyst-assisted digestion and vaporization device (SPADVD), which operates through the nano-TiO2-catalyzed photo-oxidation and reduction of selenium (Se) species, for coupling between anion exchange chromatography (LC) and inductively coupled plasma mass spectrometry (ICP-MS) systems to provide a simple and sensitive hyphenated method for the speciation analysis of Se species without the need for conventional chemical digestion and vaporization techniques. Because our proposed on-line SPADVD allows both organic and inorganic Se species in the column effluent to be converted on-line into volatile Se products, which are then measured directly through ICP-MS, the complexity of the procedure and the probability of contamination arising from the use of additional chemicals are both low. Under the optimized conditions for SPADVD - using 1g of nano-TiO2 per liter, at pH 3, and illuminating for 80 s - we found that Se(IV), Se(VI), and selenomethionine (SeMet) were all converted quantitatively into volatile Se products. In addition, because the digestion and vaporization efficiencies of all the tested selenicals were improved when using our proposed on-line LC/SPADVD/ICP-MS system, the detection limits for Se(IV), Se(VI), and SeMet were all in the nanogram-per-liter range (based on 3σ). A series of validation experiments - analysis of neat and spiked extracted samples - indicated that our proposed methods could be applied satisfactorily to the speciation analysis of organic and inorganic Se species in the extracts of Se-enriched supplements. PMID:24331052

  19. Application of high-performance anion-exchange chromatography-pulsed amperometric detection for measuring carbohydrates in routine daily filter samples collected by a national network: 2. Examination of sugar alcohols/polyols, sugars, and anhydrosugars in the upper Midwest

    NASA Astrophysics Data System (ADS)

    Sullivan, A. P.; Frank, N.; Kenski, D. M.; Collett, J. L., Jr.

    2011-04-01

    Carbohydrate measurements of ambient samples can provide insights into the biogenic fraction of the organic carbon (OC) aerosol. However, lack of measurement on a routine basis limits data analysis. In a companion paper, 1 year of archived 1-in-6 day FRM (Federal Reference Monitor) filter samples from the PM2.5 NAAQS compliance monitoring network collected at 10 sites in the upper Midwest were analyzed using high-performance anion-exchange chromatography with pulsed amperometric detection to determine the regional impact of biomass burning. Along with levoglucosan, 13 other carbohydrates were simultaneously measured, including two more anhydrosugars (mannosan and galactosan), five sugars (arabinose, galactose, glucose, mannose, xylose), and six sugar alcohols/polyols (glycerol, methyltetrols, threitol/erythritol, xylitol, sorbitol, mannitol). This paper focuses on the results from these carbohydrates in order to investigate their sources and trends both spatially and temporally. Mannosan, galactosan, arabinose, xylose, and threitol/erythritol all correlated with levoglucosan (R2 from 0.43 to 0.97), suggesting biomass burning as their main source. Glucose and mannitol exhibited higher concentrations in summer and at more southern sites, likely due to vegetation differences at the sites. Using mannitol, the contribution of spores to OC was found to be <1%. Methyltetrols were highly correlated with water-soluble OC (R2 from 0.63 to 0.95) and in higher concentrations at more eastern sites. This spatial pattern is possibly due to these sites being downwind of the high isoprene emission zones that occur in the western part of the Midwest from oak forests in the Ozarks and spruce forests in the northern lake states.

  20. Efficiency of pretreatment of aqueous samples using a macroporous strong anion-exchange resin on the determination of nerve gas hydrolysis products by gas chromatography-mass spectrometry after tert.-butyldimethylsilylation.

    PubMed

    Kataoka, M; Tsuge, K; Seto, Y

    2000-09-01

    A pretreatment procedure, using a macroporous strong anion-exchange resin (MSA) has been established for the determination of nerve gas hydrolysis products by gas chromatography-mass spectrometry (GC-MS) after tert.-butyldimethylsilyl (TBDMS) derivatization. Aqueous solutions of methylphosphonic acid (MPA) and three alkyl methylphosphonic acids (AMPAs) (ethyl, isopropyl and pinacolyl methylphosphonic acid), were retained on the MSA column, and then quantitatively eluted with 0.1 M hydrochloric acid. The neutralized column eluate was dried, and MPA and AMPAs were derivatized with N-methyl-N-(tert.-butyldimethylsilyl)-trifluoroacetamide and analyzed by GC-MS. The column eluate was also analyzed in order to determine the exact hydrolysis product levels by capillary electrophoresis using borate and benzoate buffer (pH 6). The MSA pretreatment was examined for the clean-up of aqueous extracts of three types of soils and an aqueous solution containing 10% sucrose, which is regarded as model for a typical soft drink, after spiking with MPA and AMPAs. MPA and AMPAs were quantitatively recovered in the MSA eluate fraction from those samples, except for MPA from volcanic acid and alluvial soils. The yields of TBDMS derivatives were remarkably improved, compared with for which no pretreatment was used and also for those in which a strong cation-exchange resin was used. The achieved detection limits of MPA and AMPAs ranged from 0.12 to 0.18 microg/g of soil (S/N=3). The established MSA method was applied to the pretreatment of spiked sea water, two types of beverages, Pepsi Cola and canned coffee. Although the yields of TBDMS derivatives of MPA and AMPAs in sea water (in a range between 44 and 96%) and AMPAs in Pepsi Cola (in a range between 58 and 92%) were rather high, those for MPA in the Pepsi Cola (27%) and those for MPA and AMPAs in the canned coffee (in a range between 5 and 17%) were low. PMID:11043790

  1. 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.

    PubMed

    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.

  2. 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.

    PubMed

    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%.

  3. 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.

    PubMed

    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 %.

  4. High-performance anion-exchange chromatography coupled with pulsed amperometric detection and capillary zone electrophoresis with indirect ultra violet detection as powerful tools to evaluate prebiotic properties of fructooligosaccharides and inulin.

    PubMed

    Corradini, C; Bianchi, F; Matteuzzi, D; Amoretti, A; Rossi, M; Zanoni, S

    2004-10-29

    Fructooligosaccharides (FOS) and inulin are food grade non-digestible carbohydrates that exert beneficial nutritional effect. This paper describes the suitability of high-performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD) and capillary zone electrophoresis (CZE) to evaluate fermentation properties of FOS and inulin in pure Bifidobacterium cultures; and to study their effects on faecal cultures (microbial population and short-chain fatty acids). Prebiotic effectiveness of FOS and inulin of different degrees of polymerization was evaluated monitoring the changes in their molecular weight distribution during the in vitro growth of selected Bifidobacterium strains. The qualitative analysis of the residual soluble oligosaccharides or polysaccharides from Raftilose Synergy, Raftiline HP and Raftilose P95 was carried out by HPAEC-PAD, using a CarboPac PA 100 column and an appositely optimized gradient elution program. Under the optimized gradient elution conditions, glucose, fructose, sucrose were resolved from each other and from fructans with a DP ranging from 3 (1-kestose) to 60. The chromatographic profiles of the spent broths pointed out that almost every strain presented a different capability to ferment fructan chains of variable DP, indicating wide strain to strain differences. To explore the prebiotic effect of FOS and inulin, related to of short chain fatty acids (SCFAs) accumulation in faecal cultures due to fermentative metabolism of intestinal microflora, analysis of SCFAs, acetic and lactic acid was achieved by co-electroosmotic capillary electrophoresis, where the electrophoretic mobility of the anionic analytes and electroosmotic flow (EOF) were similarly directed. Moreover, the use of UV detection for the analyses of our organic anions required a running electrolyte which allowed indirect detection. The optimization of the capillary electrophoretic conditions was carried out by applying a chemometric study

  5. 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.

    PubMed

    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 %. PMID:27072011

  6. 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.

    PubMed

    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

  7. Chromatography purification of canine adenoviral vectors.

    PubMed

    Segura, María Mercedes; Puig, Meritxell; Monfar, Mercè; Chillón, Miguel

    2012-06-01

    Canine adenovirus vectors (CAV2) are currently being evaluated for gene therapy, oncolytic virotherapy, and as vectors for recombinant vaccines. Despite the need for increasing volumes of purified CAV2 preparations for preclinical and clinical testing, their purification still relies on the use of conventional, scale-limited CsCl ultracentrifugation techniques. A complete downstream processing strategy for CAV2 vectors based on membrane filtration and chromatography is reported here. Microfiltration and ultra/diafiltration are selected for clarification and concentration of crude viral stocks containing both intracellular and extracellular CAV2 particles. A DNase digestion step is introduced between ultrafiltration and diafiltration operations. At these early stages, concentration of vector stocks with good recovery of viral particles (above 80%) and removal of a substantial amount of protein and nucleic acid contaminants is achieved. The ability of various chromatography techniques to isolate CAV2 particles was evaluated. Hydrophobic interaction chromatography using a Fractogel propyl tentacle resin was selected as a first chromatography step, because it allows removal of the bulk of contaminating proteins with high CAV2 yields (88%). An anion-exchange chromatography step using monolithic supports is further introduced to remove the remaining contaminants with good recovery of CAV2 particles (58-69%). The main CAV2 viral structural components are visualized in purified preparations by electrophoresis analyses. Purified vector stocks contained intact icosahedral viral particles, low contamination with empty viral capsids (10%), and an acceptable total-to-infectious particle ratio (below 30). The downstream processing strategy that was developed allows preparation of large volumes of high-quality CAV2 stocks. PMID:22799886

  8. Neptunium Valence Chemistry in Anion Exchange Processing

    SciTech Connect

    KYSER, EDWARD

    2003-02-01

    The current anion resin in use in HB-Line Phase II, Reillex{trademark} HPQ, was tested in the laboratory under expected plant conditions for Np processing and was found to load between 50 and 70 g Np per liter of resin. Losses varied from 0.2 to 15 percent depending on a number of parameters. Hydrazine in the feed at 0.02 to 0.05 M appeared to keep the Np from oxidizing and increasing the losses within four to seven days after the FS addition. Losses of up to three percent were observed five days after FS addition when hydrazine was not used in the feed, compared with 0.3 percent when the feed was loaded immediately after FS addition. Based on these test results the following processing conditions are recommended: (1) Feed conditions: 8 M HNO{sub 3}, 0.02 M hydrazine, 0.05 M excess FS, less than 5 days storage of solution after FS addition. (2) Wash conditions: 100 liters of 8 M HNO{sub 3}, no FS, no hydrazine. (3) Elution conditions: 0.17 M HNO{sub 3}, 0.05 M hydrazine, no FS. (4) Precipitation feed conditions: 0.03 M excess ascorbic acid, no additional hydrazine, no FS, precipitation within three days.

  9. Automated radioanalytical system incorporating microwave-assisted sample preparation, chemical separation, and online radiometric detection for the monitoring of total 99Tc in nuclear waste processing streams.

    PubMed

    Egorov, Oleg B; O'Hara, Matthew J; Grate, Jay W

    2012-04-01

    An automated fluidic instrument is described that rapidly determines the total (99)Tc content of aged nuclear waste samples, where the matrix is chemically and radiologically complex and the existing speciation of the (99)Tc is variable. The monitor links microwave-assisted sample preparation with an automated anion exchange column separation and detection using a flow-through solid scintillator detector. The sample preparation steps acidify the sample, decompose organics, and convert all Tc species to the pertechnetate anion. The column-based anion exchange procedure separates the pertechnetate from the complex sample matrix, so that radiometric detection can provide accurate measurement of (99)Tc. We developed a preprogrammed spike addition procedure to automatically determine matrix-matched calibration. The overall measurement efficiency that is determined simultaneously provides a self-diagnostic parameter for the radiochemical separation and overall instrument function. Continuous, automated operation was demonstrated over the course of 54 h, which resulted in the analysis of 215 samples plus 54 hly spike-addition samples, with consistent overall measurement efficiency for the operation of the monitor. A sample can be processed and measured automatically in just 12.5 min with a detection limit of 23.5 Bq/mL of (99)Tc in low activity waste (0.495 mL sample volume), with better than 10% RSD precision at concentrations above the quantification limit. This rapid automated analysis method was developed to support nuclear waste processing operations planned for the Hanford nuclear site.

  10. Automated Radioanalytical System Incorporating Microwave-Assisted Sample Preparation, Chemical Separation, and Online Radiometric Detection for the Monitoring of Total 99Tc in Nuclear Waste Processing Streams

    SciTech Connect

    Egorov, Oleg; O'Hara, Matthew J.; Grate, Jay W.

    2012-04-03

    An automated fluidic instrument is described that rapidly determines the total 99Tc content of aged nuclear waste samples, where the matrix is chemically and radiologically complex and the existing speciation of the 99Tc is variable. The monitor links microwave-assisted sample preparation with an automated anion exchange column separation and detection using a flow-through solid scintillator detector. The sample preparation steps acidify the sample, decompose organics, and convert all Tc species to the pertechnetate anion. The column-based anion exchange procedure separates the pertechnetate from the complex sample matrix, so that radiometric detection can provide accurate measurement of 99Tc. We developed a preprogrammed spike addition procedure to automatically determine matrix-matched calibration. The overall measurement efficiency that is determined simultaneously provides a self-diagnostic parameter for the radiochemical separation and overall instrument function. Continuous, automated operation was demonstrated over the course of 54 h, which resulted in the analysis of 215 samples plus 54 hly spike-addition samples, with consistent overall measurement efficiency for the operation of the monitor. A sample can be processed and measured automatically in just 12.5 min with a detection limit of 23.5 Bq/mL of 99Tc in low activity waste (0.495 mL sample volume), with better than 10% RSD precision at concentrations above the quantification limit. This rapid automated analysis method was developed to support nuclear waste processing operations planned for the Hanford nuclear site.

  11. PURIFICATION PROCESS

    DOEpatents

    Wibbles, H.L.; Miller, E.I.

    1958-01-14

    This patent deals with the separation of uranium from molybdenum compounds, and in particular with their separation from ether solutions containing the molybdenum in the form of acids, such as silicomolybdic and phosphomolybdic acids. After the nitric acid leach of pitchblende, the molybdenum values present in the ore are found in the leach solution in the form of complex acids. The uranium bearing solution may be purified of this molybdenum content by comtacting it with activated charcoal. The purification is improved when the acidity of the solution is low ad agitation is also beneficial. The molybdenum may subsequently be recovered from the charcosl ad the charcoal reused.

  12. Water Purification

    NASA Technical Reports Server (NTRS)

    1992-01-01

    Silver ionization water purification technology was originally developed for Apollo spacecraft. It was later used to cleanse swimming pools and has now been applied to industrial cooling towers and process coolers. Sensible Technologies, Inc. has added two other technologies to the system, which occupies only six square feet. It is manufactured in three capacities, and larger models are custom built on request. The system eliminates scale, corrosion, algae, bacteria and debris, and because of the NASA technology, viruses and waterborne bacteria are also destroyed. Applications include a General Motors cooling tower, amusement parks, ice manufacture and a closed-loop process cooling system.

  13. Purification of HIV-1 gag virus-like particles and separation of other extracellular particles.

    PubMed

    Steppert, Petra; Burgstaller, Daniel; Klausberger, Miriam; Berger, Eva; Aguilar, Patricia Pereira; Schneider, Tobias A; Kramberger, Petra; Tover, Andres; Nöbauer, Katharina; Razzazi-Fazeli, Ebrahim; Jungbauer, Alois

    2016-07-15

    Enveloped virus-like particles (VLPs) are increasingly used as vaccines and immunotherapeutics. Frequently, very time consuming density gradient centrifugation techniques are used for purification of VLPs. However, the progress towards optimized large-scale VLP production increased the demand for fast, cost efficient and scale able purification processes. We developed a chromatographic procedure for purification of HIV-1 gag VLPs produced in CHO cells. The clarified and filtered cell culture supernatant was directly processed on an anion-exchange monolith. The majority of host cell impurities passed through the column, whereas the VLPs were eluted by a linear or step salt gradient; the major fraction of DNA was eluted prior to VLPs and particles in the range of 100-200nm in diameter could be separated into two fractions. The earlier eluted fraction was enriched with extracellular particles associated to exosomes or microvesicles, whereas the late eluting fractions contained the majority of most pure HIV-1 gag VLPs. DNA content in the exosome-containing fraction could not be reduced by Benzonase treatment which indicated that the DNA was encapsulated. Many exosome markers were identified by proteomic analysis in this fraction. We present a laboratory method that could serve as a basis for rapid downstream processing of enveloped VLPs. Up to 2000 doses, each containing 1×10(9) particles, could be processed with a 1mL monolith within 47min. The method compared to density gradient centrifugation has a 220-fold improvement in productivity. PMID:27286649

  14. Online eluent-switching technique coupled anion-exchange liquid chromatography–ion trap tandem mass spectrometry for analysis of non-steroidal anti-inflammatory drugs in pig serum.

    PubMed

    Chang, Kai Chun; Lin, Jyh Shiun; Cheng, Cheanyeh

    2015-11-27

    A novel method for online extraction, pH-gradient separation, and analysis of nine non-steroidal anti-inflammatory drugs (NSAIDs) was developed by coupling online eluent-switching technique to single anion-exchange chromatographic column/ion trap mass spectrometer (MS) and used for monitoring NSAIDs residues in pig serum. A neutral eluent and a pH-gradient eluent were used for extraction and separation of NSAIDs, respectively. Each of nine NSAIDs has an MS precursor ion of either [M−H]− or [M−Na]−. The extracted ion chromatogram for a specific product ion of each NSAID was used for its quantitative analysis. The dynamic linear ranges of calibration curves were all 0–200 ng mL−1 (R2 > 0.9950). The analysis accuracies estimated by spiking standard concentrations at 20, 100, and 200 ng mL−1 were 80.5–99.9%. The corresponding intra-day and inter-day precisions (RSD%) were 2.5–14.5% and 2.9–15.2%, respectively. The limit of detection/limit of quantitation of NSAIDs were 1.3/4.3, 0.5/1.6, 0.2/0.5, 2.5/8.2, 1.5/4.9, 0.6/2.1, 0.6/2.0, 0.5/1.7, and 0.6/2.1 ng mL−1 for carprofen, diclofenac, flunixin, ibuprofen, ketoprofen, meclofenamic acid sodium, mefenamic acid, niflumic acid, and tolfenamic acid, respectively. After 1 h injection of a dose containing 2 mg kg−1 weight pig of flunixin and tolfenamic acid to the pigs, a residue amount of 3480 ± 36 ng mL−1 and 431 ± 13 ng mL−1, respectively, was reached for the incurred pig serum specimens and both residues were reduced to about 20 ng mL−1 at the time of 24 h. PMID:26601710

  15. Determination of S-2-(N,N-diisopropylaminoethyl)- and S-2-(N,N-diethylaminoethyl) methylphosphonothiolate, nerve agent markers, in water samples using strong anion-exchange disk extraction, in vial trimethylsilylation, and gas chromatography-mass spectrometry analysis.

    PubMed

    Subramaniam, Raja; Åstot, Crister; Juhlin, Lars; Nilsson, Calle; Östin, Anders

    2012-03-16

    Since the establishment of the Chemical Weapons Convention in 1997, the development of analytical methods for unambiguous identification of large numbers of chemicals related t