X-Ray contrast media. Synthesis of esters of 3,5-diiodopyrid-4-one-N-acetic acid in the presence of KU-2 cation-exchange resin

In a study of the esterification of 3, 5-diiodopyrid-4-one-N-acetic acid with alipathic alcohols in the presence of KU-2 cation-exchange resin as catalyst, it was established that the reaction takes place readily and smoothly and gives the corresponding esters in high yields.     

阳离子树脂催化合成古龙酸甲酯的动力学研究

古龙酸甲酯化反应是生产维生素C的一个重要中间过程,目前工业上主要采用古龙酸和甲醇为原料,以浓硫酸作催化剂催化酯化.这一反应存在副反应较多,甲酯的色泽深,质量差,后续反应中需用碱进行中和等缺点,给后续处理带来困难.     

A microcalorimetric study of mercury(II) sorption on KU-2-8 sulfocationite

The thermokinetic characteristics of the sorption of mercury(II) ions on KU-2-8 strongly acidic cationite from mercury acetate solutions was studied using microcalorimetry. The overall heat of sorption and its dependence on the degree of filling of the cationite were determined.     

Aspects of the super-equivalent sorption of glycine by cation exchanger KU-2-8

The structure formed in a sorbent during the super-equivalent sorption of glycine by cation exchanger KU-2-8 is optimized via quantum chemical simulation. The differential thermodynamic characteristics of ion exchange and super-equivalent sorption in the studied system are calculated using a thermodynamic approach that allows us to describe the simultaneous exchange and super-equivalent sorption of compounds by ion-exchangers.     

Equivalent Electroconductivities of Lysine Cations and Phenylalanine Anions in Ionites KU-2-8 and AV-17

Equivalent conductivities of lysine cations and phenylalanine anions in ion-exchangers KU-2-8 and AV-17, respectively, are studied. The mobility of ions of amino acids in the ionites is lower than that of mineral ions (sodium and chloride). The obtained results are applied to predict the occurrence of electrochemical regeneration of ion-exchangers in the amino acid forms.     

Adsorption of monoclonal antibody variants on analytical cation-exchange resin

Monoclonal antibody (MAb) variants differing by one or two C-terminal lysine residues can be separated by cation-exchange chromatography due to the difference in their charge distribution. The adsorption of the three MAb variants on a weak cation-exchange resin was characterized using directly the raw mixture in spite of the presence of some impurities. The effects of both, pH and eluent salt concentration, on the adsorption isotherm were investigated. Under certain experimental conditions distorted peak shapes and even peak doubling for single variant injections were obtained, in addition to unexpectedly long retention times. These observations were explained based on equilibrium theory. The separation of the MAb variants was designed for an isocratic and a linear salt gradient operation. The corresponding optimal values of pH and salt concentration were determined. The use of salt gradients not only allows reducing the process time and increasing enrichment of the variants, but also leads to some loss in purity. A baseline separation could be obtained under isocratic and strongly adsorbing conditions at pH 6.3. A lumped kinetic model and a procedure for estimating the corresponding parameters were developed and validated by comparison with experimental elution chromatograms in a wide range of operating conditions.     

Influence of Humus Acids on Physicochemical Features of KU-2×8 Cation Exchangers

In prolonged industrial desalination of natural water with KU-2×8 cation exchanger, humic and fulvic acids are accumulated on the resin, which deteriorates its sorption characteristics, desalination efficiency.     

Exchange equilibrium in the H-sulfocationite KU-2 × 8-phenylalanine-histidine system

The equilibrium properties of the joint sorption of phenylalanine and histidine on KU-2 × 8 sulfocationite from mixed solution were studied. The effect of the ratio between the concentrations of the amino acids in the solution on their sorption characteristics was reveled. The coefficients of separation and distribution of the amino acids between the sorbent and solution phases were determined.     

The competitive adsorption of water and toluene on KU-2-8 ion exchanger in the presence of aromatic amino acids

The Weitkamp procedure was used to calculate hydrophobicity indices for several ion exchange systems, including adsorbed aromatic amino acids. The determination of hydrophobicity indices was based on the competitive adsorption of water and toluene from their mixture. Strongly acid KU-2 ion exchanger with hydrophilic properties predominantly sorbed water molecules in the competitive adsorption from their mixture with toluene vapor. The saturation of the ion exchanger with aromatic amino acids substantially decreased its sorption ability because of amino acid structuring and a decrease in permeability. The conclusion was drawn that the saturation of the ion exchanger with amino acids caused not only a decrease in the sorption of water but also a decrease in the sorption of hydrophobic toluene. This contradicted the assertion of an increase in hydrophobicity as a whole.     

High-speed simultaneous ion-exclusion/cation-exchange chromatography of anions and cations on a weakly acidic cation-exchange resin column

The simultaneous ion-exclusion/cation-exchange separation column packed with a polymethacrylate-based weakly acidic cation-exchange resin of 3 microm particle size was used to achieve the simultaneous high-speed separation of anions and cations (Cl(-), NO3(-), SO4(2-), Na(+), K(+), NH4(+), Ca(2+) and Mg(2+)) commonly found in environmental samples. The high-speed simultaneous separation is based on a combination of the ion-exclusion mechanism for the anions and the cation-exchange mechanism for cations. The complete separation of the anions and cations was achieved in 5 min by elution with 15 mM tartaric acid-2.5 mM 18-crown-6 at a flow-rate of 1.5 ml/min. Detection limits at S/N=3 ranged from 0.36 to 0.68 microM for anions and 0.63-0.99 microM for cations. This method has been applied to the simultaneous determination of anions and cations in several environmental waters with satisfactory results.     

Structure and catalytic properties of chromium complexes on cation-exchange resin surfaces

The type of bonding of Cr(III) on the surface of cation-exchange resins has been studied. The complexes of Cr(III) with ethylenediamine were obtained by direct synthesis on the surface. Coordination to nitrogen bases increases the catalytic activity of Cr(III) ions in hydrogen peroxide decomposition.

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Cr(III) . Cr(III) . Cr(III) .

     

Vacancy ion-exclusion chromatography of haloacetic acids on a weakly acidic cation-exchange resin

A new and simple approach is described for the determination of the haloacetic acids (such as mono-, di- and trichloroacetic acids) usually found in drinking water as chlorination by-products after disinfection processes and acetic acid. The new approach, termed vacancy ion-exclusion chromatography, is based on an ion-exclusion mechanism but using the sample solution as the mobile phase, pure water as the injected sample, and a weakly acidic cation-exchange resin column (TSKgel OApak-A) as the stationary phase. The addition of sulfuric acid to the mobile phase results in highly sensitive conductivity detection with sharp and well-shaped peaks, leading to excellent and efficient separations. The elution order was sulfuric acid, dichloroacetic acid, monochloroacetic acid, trichloroacetic acid, and acetic acid. The separation of these acids depends on their pKa values. Acids with lower pKa values were eluted earlier than those with higher pKa, except for trichloroacetic acid due to a hydrophobic-adsorption effect occurring as a side-effect of vacancy ion-exclusion chromatography. The detection limits of these acids in the present study with conductivity detection were 3.4 microM for monochloroacetic acid, 0.86 microM for dichloroacetic acid and 0.15 microM for trichloroacetic acid.     

Entirely solvent-free biocatalytic synthesis of solketal fatty esters from soybean seeds

Solvent-free reactions are the systems of choice in green chemistry. In addition to contributing to lowering the environmental impact of chemical processes, solvent-free systems can reduce production costs, reaction times, and the dimensions of reactors, thereby decreasing investment costs. An improved procedure to prepare 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane (solketal) fatty esters from soybean seeds has been developed. Yields higher than 90% were achieved by combining 15 h of hydrolysis with 6 h of esterification with a stepwise addition of solketal. The synthesis was performed in a solvent-free medium, and the final extraction was accomplished using supercritical CO₂. Hence, we have successfully prepared these esters from soybean beans without using organic solvents. In addition, given the non-toxicity of Rhizopus oryzae and the composition of the remaining solid, it might be used as a raw material for feedstock production.     

Vacancy ion-exclusion chromatography of carboxylic acids on a weakly acidic cation-exchange resin

In this preliminary study, a new approach to ion-exclusion chromatography is proposed to overcome the relatively poor conductivity detection response which occurs in ion-exclusion chromatography when acids are added to the eluent in order to improve peak shape. This approach, termed vacancy ion-exclusion chromatography, requires the sample to be used as eluent and a sample of water to be injected onto a weakly acidic cation-exchange column (TSKgel OApak-A). Vacancy peaks for each of the analytes appear at the retention times of these analytes. Highly sensitive conductivity detection is possible and sharp, well-shaped peaks are produced, leading to efficient separations. Retention times were found to be affected by the concentration of the analytes in the eluent, and also by the presence of an organic modifier such as methanol in the eluent. Detection limits for oxalic, formic, acetic, propionic, butyric and valeric acids were 0.1, 0.2, 0.3, 0.3, 0.4 and 0.5 microM, respectively, and linear ranges for some acids extended over two orders of magnitude. Precision values for retention times were 0.21% and for peak areas were <1.90%. The vacancy ion-exclusion chromatography method was found to give detection responses four to 10 times higher than conventional ion-exclusion chromatography using sulfuric acid eluent and two to five times higher than conventional ion-exclusion chromatography using benzoic acid eluent.