A study of the mechanical, thermal and morphological properties of microcrystalline cellulose particles prepared from cotton slivers using different acid concentrations

Microcrystalline cellulose (MCC) particles are mostly prepared by acid hydrolysis of various agro sources. Acid hydrolysis is usually carried out with high concentration (64 wt%) of sulfuric acid. Here, an attempt has been made to optimize lower acid concentrations which can effectively produce MCC particles. In this work, different concentrations of sulfuric acid (20, 30, 35, 40, 47 and 64 wt%) have been used to prepare MCC particles, which have been characterized by XRD, particle size analysis, scanning electron microscopy, transmission electron microscopy, nanoindentation and thermogravimetric analysis. MCC prepared with 35 and 47% sulfuric acid (MCC 35 and MCC 47) had finest particle size and fibrils were produced in the range of 15–25 nm. MCC 20 showed wide particle size distribution, indicating low breakdown of the cellulose chains. The energy absorption behavior and mechanical properties of the MCC pellets were determined by nanoindentation test for the first time. MCC 35 pellets exhibited lowest modulus and hardness.     

Removal of interferences in absorptiometric determination of bismuth with thorin

Bismuth can be separated by ion-exchange adsorption on Dowex 21 K resin from ca. 0.25 M HCl, after removal of volatile interferences by distillation in acid-oxidizing medium. Bismuth is eluted from the column with 1 M sulfuric acid. The method is useful in the absorptiometric determination of bismuth with thorin, as well as in other photometric methods.     

Estimation of the surface sulfur content of cellulose nanocrystals prepared by sulfuric acid hydrolysis

The conditions required for the accurate measurement of the sulfur content of cellulose nanocrystals (CNCs) by conductometric titration are discussed. CNCs from sulfuric acid hydrolysis are electrostatically stabilized in aqueous suspension due to the introduction of charged sulfate ester groups onto the surface of the crystallites during reaction. The sulfur content thus largely reflects the surface charge of the crystals, and is crucial to the characterization and understanding of material properties. Conductometric titration is commonly used to quantify the sulfur content of CNCs, however, the exhaustive removal of free acid by dialysis and the necessity, type, quantity and duration of ion-exchange resin treatments are not always consistent. Here we explore the standard conditions of dialysis, ion-exchange, and the reproducibility of titration results. Extensive dialysis is found to be effective in the removal of free acid, but similar results are also achieved in shorter times and with less water using membrane ultrafiltration. It is also shown that the conditions of ion-exchange most commonly employed in the literature can lead to inaccurate sulfur contents. Finally, good agreement is obtained between the sulfur contents of different CNC batches prepared using the same hydrolysis conditions, and from titration and elemental analysis when thoroughly purified, well-dispersed samples, and appropriate resin conditions are used.     

Re-assessment of chelating ion-exchange resins for trace metal analysis of sea water

The behaviour of the chelating ion-exchange resin Chelex-100 for collection of trace metals from sea water has been studied by anodic stripping voltammetry after acid digestion of the sea water sample and the resin effluent. All the naturally occurring, electrochemically reducible species of Cu, Pb, Cd and Zn are chelated by the resin; this fraction of these metals is regarded as the dissolved fraction. Centrifugation showed that some of the metal liberated by acid digestion is associated with colloidal species. Neither this nor the metal adsorbed on fine particles is affected or removed by the chelating resin.     

A novel method for the determination of iodide in table salt by X-ray fluorescence

A novel HI generation technique was developed and evaluated for the determination of iodide in table salt. HI was generated from the samples by the addition of concentrated sulfuric acid and adsorbed onto an ion-exchange resin loaded paper disk. The disk was then measured by X-ray fluorescence. The method compared favorably to the cellulose pellet technique, being more sensitive and reproducible and requiring less time per analysis. The method was applied to six samples of table salt and one of sea salt.     

Etherification of dimethylbutene with methanol over clay-based acid catalysts

Etherification of a typical C₆ olefin, 2,3-dimethyl-1-butene, with methanol was investigated over commercial ion-exchange resins and several clay-based acid solids prepared by sulfuric acid treatment or impregnation of sulfated zirconia and Nafion. The commercial resin catalyst Amberlyst 15 is effective but nonselective to ether production, while Nafion is less active. For two clay systems, montmorillonite-based catalysts generally exhibit higher activities than bentonite and MT-H₂SO₄will be a highly active and selective catalyst than the supported sulfated zirconia and Nafion.     

离子交换法分离乳酸的连续流动板模型

本文对乳酸在D354树脂上的离子交换行为进行了详细的研究，并在乳酸的超摩尔离子交换等温线方程的基础上，进一步采用简单的连续流动板模型对乳酸的固定床离子交换行为进行描述，模型拟合结果与实验值能较好的符合。     

Conductivity stopped-flow study of the kinetics of solutes uptake by colloidal particles of synthetic resins

The uptake rates of acids (hydrochloric acid, sulfuric acid, perchloric acid and acetic acid) by colloidal solid particles (mean diameter 0.35 microm) of DEAE (diethylaminoethyl Sephadex) resin was studied by the means of the stopped flow technique equipped with a conductivity detection. This original experimental approach allows to avoid hydrodynamics perturbations during data acquisition. For the sake of comparison NaOH uptake or K(+)/H(+) exchange by sulfonic Dowex resin particles experiments have also been performed. As stated in the literature we observed that the uptake rate limiting step is the solute diffusion in the solution layer surrounding the particles. To fit the experimental conductivity versus time curves on the basis of solutes diffusion concepts a simple mathematical equation fitting perfectly well the experimental data is proposed. The mathematical modeling of kinetic data obtained in non-stationary diffusion proposed here can substitute to the empiric pseudo-first- and -second-order models often used in environmental research.     

离子交换树脂的选择及柠檬酸溶液循环使用研究

用离子交换树脂法吸附柠檬酸溶液中的金属离子,苯乙烯系阳离子交换树脂的吸附性能较好,它对镍、铝离子的吸附容量均较大,且吸附前后柠檬酸溶液的浓度变化较小.静态条件下树脂对镍的吸附容量为16.83mg Ni/g干树脂,对铝为21.36mg Al/g干树脂;动态条件下树脂对镍的吸附容量为6.78mg Ni/g干树脂,对铝为31.8mgAl/g干树脂,吸附液流速为1m/h～3m/h.吸附后的柠檬酸溶液可循环使用.当用1mol/L硫酸解吸时,树脂对镍铝的解吸率可达90%以上.当硫酸中Ni2 为1.70mmol/L,Al3 为7.40mmol/L时,树脂的解吸率仍可达80%以上.     

Anion-exchange resin modified with bismuthiol-II, as a new functional resin for the selective collection of selenium(IV)

A functional resin for the collection of selenium(IV) has been prepared simply by the conversion of a common ion-exchange resin with bismuthiol-II which has three functional properties, namely the capabilities of selective reaction with selenium(IV), ion-exchange reaction with ion-exchange resin and strong physical sorption to the ion-exchange resin matrix. The binding ratio of selenium(IV) to bismuthiol-II on the resin was confirmed to be 1:4. The reaction was represented as follows: 4RSH + H(2)SeO(3)--> R-S-Se-S-R + R-S-S-R + 3H(2)O. Highly selective sorption of selenium(IV) was achieved, based on the formation of stable selenotrisulphide on the resin. Selenium(IV) sorbed on bismuthiol-II resin was eluted effectively with 8-13M nitric acid or some thiols, such as cysteine and penicillamine. In the cases of thiols, the elution of selenium was found to be also based on the formation of selenotrisulphide, and the bismuthiol-II resin was regenerated. Satisfactory results were obtained when this resin was applied to the determination of selenium(IV) in river, estuarine or sea water samples.     

Ion-exchange selectivity of anion exchange resin modified with polystyrenesulfonic acid.

In order to change the ion-exchange selectivity of anion-exchange resin, the surface of a gel-type anion exchange resin was modified with anionic polyelectrolyte, polystyrenesulfonic acid. Using this modified resin, the ion-exchange rate of nitrate was little decreased, but that of sulfate was evidently decreased. It is considered that the ion-exchange reaction of the multivalent anion is suppressed by the greater electrostatic repulsive force against the modification layer than that against the monovalent anion. Thus, this modified resin may be suitable for the selective separation of monovalent anions. The influence of the modified condition on the ion-exchange rate was examined. Furthermore, this modified resin was used to separate nitrate ions from sulfate ions in the aqueous solution.     

Ion Exchange and Protonation Equilibria of an Amphoteric Ion-exchange Resin in the Presence of Simple Salt

The influence of simple salts on the ion exchange and protonation equilibria of an amphoteric ion-exchange resin, which has strong base and weak acid moieties in a single functional group fixed onto the styrene-DVB matrix, has been investigated. Concentrations of ionic species in the amphoteric ion-exchange resin in equilibrium with various sodium salt solutions were estimated by (23)Na NMR spectroscopy. For the NaClO(4) system, the ratio of sodium ion concentration in the resin phase to that in the equilibrium solution was greater than 1 and increased with a decrease in the salt concentration. In contrast to an ordinary cation-exchange resin, the ion exchange behavior of Mg(2+) and Ca(2+) on the amphoteric ion-exchange resin showed a marked dependence on the kinds of salts: the distribution coefficients for the NaCl system were independent of the salt concentration, while the log D vs. log[Na(+)] plots for the NaClO(4) system showed linear relationships with slopes being neither -2 nor 0. Apparent protonation constants of the carboxylate in the functional group of the resin in equilibrium with NaClO(4) solutions were greater than those with NaCl solutions. The ion exchange and protonation properties of the amphoteric ion-exchange resin were elucidated on the basis of the information about the salt concentrations in the resin phase estimated by the NMR method.     

A STUDY OF THE HEAT OF HYDRATION OF SULFONIC ACID RESINS

The heat of hydration of dry sulfonic acid resin in different comcentrations of sulfuric acid has been determined. The heat of hydration of the resin in H2O is 143.4J/g(resin). The greater the concentration of sulfuric acid,the less the heat will be released.The hydrate formed from three sulfonic acid groups and one water molecule is the most stable one of all the hydrates of sulfonic acid resin and water.     

Preparation of ion exchange resins from carbonaceous adsorbents

Carbonaceous adsorbents are obtained by thermolysis of sulfonated macroreticular polystyrene ion exchange resins at 300-500°C. The hard, spherical, carbonaceous particles react exothermally with elemental chlorine to form products containing up to 38% Cl. The chlorinated particles react readily with polyamines to form anion exchange resins with capacities of up to 2.2 meq/g dry resin. Less than 60% of the nitrogen atoms in the particles are utilized as ion exchange sites. The carbonaceous particles can also be chloromethylated with chloromethyl methyl ether or chlorinated with sulfuryl chloride and then aminated with polyamines to form anion exchange resins, sulfonated with sulfuric acid or chlorosulfonic acid to form strongly acidic cation exchange resins, or chlorosulfonated and then aminated with polyamines to form anion exchange resins. Model structures of the thermolyzed resins containing polycyclic aromatic hydrocarbon fragments are proposed to explain their chemical reactivities.     

Selective collection of selenium(IV) on anion-exchange resin with azothiopyrine disulphonic acid

Azothiopyrine disulphonic acid (ATPS) has been shown to be terfunctional, namely it can form a selenotrisulphide by reaction of its thiol group with selenium(IV), bind to an anion-exchange resin by ion-exchange through its sulphonate group, and be strongly physically adsorbed on the ion-exchange resin, ATPS adsorbed on the resin does not bleed into solution even in the presence of sodium chloride and hydrochloric acid. The collection of seleniurn(IV) is practically complete when ATPS is added to a selenium(IV) solution and the reaction product is collected on the anion-exchange resin. Selenium(IV) is not satisfactorily collected, however, by reaction with anion-exchange resin loaded with ATPS. The sorbed selenium can be eluted [as Se(IV)] with 13M nitric acid and directly determined fluorometrically in the eluate.     

Adsorption behavior of various metals on a weakly basic anion-exchange resin in sulfuric acid media

A systematic study is presented on the adsorption behavior of some 20 metals on a weakly basic condensed phenol resin, Amberlite CG-4B, in sulfuric acid media. The distribution coefficients were determined over a sulfuric acid concentration range of 0.005 M to 2 M. The metals adsorbed are similar to those which exhibit strong adsorption on a strongly basic resin, but the magnitudes of the distribution coefficients and the adsorption sequences differ considerably between the two types of the resin. Several two- and three-component separations of analytical interest are possible. A new method for the separation of titanium(IV) is described; this is based on its high adsorption on CG-4B from sulfuric acid media containing hydrogen peroxide.     

Metal palladium dispersed inside macroporous ion-exchange resins: the issue of the accessibility to gaseous reactants

Commercial macroporous ion-exchange resins (Lewatit SPC 118 and UCP 118) were used to support Pd metal by a two step ion-exchange and reduction procedure. The textural features of the resins were determined by Inverse Steric Exclusion Chromatography (ISEC) measurements. TEM characterization of the obtained Pd/resin composite showed the presence of uniformly sized Pd crystallites located at the macropore “surface”. Pulse chemisorption analysis gave evidence for the lack of accessibility of the crystallites when the resin composite is in the dry state. This suggests that the metal particles are in fact embedded in a gel-type resin layer at the “surface” of the macropores and therefore practically unaccessible to the molecules of a gaseous phase unless the support is in the swollen state.     

Selective extraction of benzoic acid from landfill leachate by solid-phase extraction and ion-exchange chromatography

In this work a simple method was described for selective extraction of benzoic acid from landfill leachate samples. The samples were submitted to solid-phase extraction (SPE) with XAD-4 resin as the stationary phase and ion-exchange chromatography (IEC) using the ion-exchange resin Amberlyst A-27. The instrumental analysis was performed by gas chromatography with mass spectrometric detection (GC-MSD). Benzoic acid was isolated, identified and quantified. The extraction process is rapid, simple and of low cost. It was also environmental friendly, that is, it was used a minimum amounts of hazardous organic solvents and produced also minimum quantities of residues.     

Equilibrium sorption of sulfuric acid by weakly basic polyacrylic anionites

The sorption of sulfuric acid on Amberlite IRA 67 and (2) Lewatit VP.OC.1072 weakly basic polyacrylic anionites in the free-base form was studied. It was demonstrated that the bisulfate form of the anionites was not produced. In contrast to the sorption of hydrochloric acid, the solution of resinates formed during the sorption of sulfuric acid is nonideal. A model of exchange of doubly charged anions on fixed singly charged ion-exchange sites of polyacrylic anionites was developed based on the theory of ion-exchange equilibria. The model was used to analyze the isotherms of equilibrium sorption of sulfuric acid on IRA 67 and Lewatit VP.OC.1072 anionites in the free-base form.     

Ion exhange and molecular sorption of oxalic acid with a highly basic anion exchanger

Ab initio modeling of a matrix fragment of resin and geometry optimization of the molecular structure of oxalic acid were performed. The isotherm of oxalic acid sorption with AV-17-8 anion exchange resin was obtained by the variable concentrations technique. The ion-exchange and molecular components of sorbate fixation with the ion exchanger were determined. The hydration of the highly basic anion exchanger that absorbed different quantities of dicarboxylic acid was evaluated by the centrifuging method. The dependence of the amount of water and sorbate concentration in the resin was linear antibatic.