The chromatography of a number of metals on cellulose phosphate layers in sulfuric acid and ammonium sulfate media

Summary The thin-layer chromatographic behavior of 58 metals on an intermediately acidic cation exchanger, cellulose phosphate (P-cellulose), has been surveyed systematically in sulfuric acid and ammonium sulfate media (0.01–2.0 M). The R_f values for many bivalent and univalent metal ions on P-cellulose plates increase with increasing concentration of sulfate ions. Howerver, manganese (II), arsenic (III) and selenium (IV) are not adsorbed on the cellulose to any great extent. Beryllium (II) and other metals, which form either strong phosphate complexes or insoluble sulfate precipitates, are strongly retained on the P-cellulose. The thin-layer chromatographic separations of various metal ions of analytical interest were accomplished to demonstrate the use of R_f measurements for predicting separations in the acid and the sulfate media.     

Chromatography of inorganic ions on cellulose phosphate layer in hydrochlorid acid and in acid ammonium thiocyanate media

Summary Thin-layers of an intermediately acidic cation exchanger, cellulose phosphate (P-cellulose), have systematically been used to study the chromatographic behavior of 58 inorganic ions in both hydrochloric acid and acid ammonium thiocyanate media (0.01–2.0 mol dm⁻³). In both solvent systems, the R _f values of many bivalent cations increase with increasing concentration of the acid and thiocyanate. Polyvalent metal ions including beryllium (II) and the others are strongly retained on the P-cellulose in the acid and thiocyanate systems tested. Palladium(II), mercury(II), ruthenium(III), rhenium(VII), arsenic(III), selenium(IV) and tellurium(IV) are not adsorbed on P-cellulose to any great extent. For silver(I), indium(III), gold(III), and platinum(IV), there are marked differences in the chromatographic behavior between hydrochloric acid and acid ammonium thiocyanate systems. Multicomponent separations conducted on P-cellulose plates with these eluents are presented.     

Thin-layer chromatography of inorganic ions on polyethyleneimine cellulose in sulfuric acid and acid-ammonium sulfate media

Summary The thin-layer chromatographic behavior of 49 inorganic ions on polyethyleneimine (PEI) cellulose, a weakly basic anion-exchanger, has been systematically studied in sulfuric acid and ammonium sulfate media (both 0.01–1.0 moldm⁻³). The sorption on the cellulose decreases with increasing concentration of the acid or sulfate for most of the ions and to a lesser extent for Hg(II), Bi(III), Th(IV), Nb(V), and U(VI). The R_f values of Pd(II), Ru(III), Au(III), Pt(IV), and Ta(V) are extremely low in both systems. Ba(II), Pb(II), Sb(III), Mo(VI), and W(VI) are also strongly retained on the layer. Oxy-anions such as As(III) and Se(VI) are not adsorbed on the cellulose to any great extent, but Re(VII) distributes on the plate with a R_f value of about 0.5. The characteristic retention on PEI-cellulose layer of several polyvalent ions, which form anionic sulfato complexes, can be observed in ammonium sulfate media. Possibilities for separations of analytical interest are also demonstrated in both systems.     

Thin-layer chromatography of a number of metals on cellulose phosphate in phosphoric acid media

Summary The thin-layer chromatographic behavior of 48 metals on cellulose phosphate (P-cellulose), an interediately acidic cation exchanger, has been examined systematically in aqueous phosphoric acid media (0.01–2 M). Differences in the R_f values among the metals in 1 M phosphoric acid are large enough to permit multicomponent separations of analytical interest.     

Chromatography of inorganic ions on sulfoethyl cellulose layer in mixed sulfuric acid-organic solvent media

Summary The thin-layer chromatographic behavior of 49 inorganic ions has been systematically studied on layers of sulfoethyl (SE) cellulose, a strongly acidic cation-exchanger, with binary solvent mixtures consisting of sulfuric acid and an organic solvent such as methanol or acetone. The characteristic retention on the cellulose layer can be recognized for some ions forming sulfato complexes in the acid-organic solvent medium, and some aspects of the behavior are discussed. Chromatographic separations of analytical interest are also demonstrated on the SE-cellulose layer with acid-methanol and acid-acetone solutions used as mobile phases.     

Thin-Layer chromatography of inorganic ions on cellulose phosphate in sulfuric acid-organic solvent media

Summary Thin-layer chromatographic behavior of 49 inorganic ions on cellulose phosphate (P-cellulose) has systematically been surveyed with binary solvent mixtures consisting of sulfuric acid and an organic solvent such as methanol or acetone. The R_f values of many bivalent and monovalent ions as well as Te(VI) decrease on the P-cellulose layer with an increasing concentration of the organic solvent. Polyvalent ions which form strong phosphato-complexes and precipitate insoluble sulfate are strongly retained on P-cellulose. Oxy-anions, Au(III) and Pt(IV) are not adsorbed on the cellulose to any great extent. Feasibilities of the separation of multicomponent mixtures are demonstrated on the P-cellulose layer.     

Thin-layer chromatography of inorganic ions on sulphoethyl cellulose in sulphuric acid and ammonium sulphate media

Summary Thin-layer chromatographic (TLC) behaviour of 51 inorganic ions on a strongly acidic cation-exchanger, sulphoethyl (SE) cellulose, has been studied systematically in sulphuric acid and ammonium sulphate media (0.01–0.2 mol dm⁻³). Some aspects of the adsorption behaviour of the inorganic ions on the SE-cellulose are compared with those on other cation-exchangers in the same eluent systems. The possibilities for TLC separations of analytical interest are also proposed on SE-cellulose in sulphuric acid and acid ammonium sulphate media.     

Chromatography of inorganic ions o sulfoethyl cellulose layer in hydrochloric acid and in hydrochloric acid-ammonium thiocyanate media

Summary Chromatographic behavior of 51 inorganic ions has been systematically studied on layers of sulfoethyl (SE) cellulose, a strongly acidic exchanger, in hydrochloric acid and in acid-ammonium thiocyanate media. The sorption of most of the ions on he SE-cellulose decreases with increasing concentration of the acid and the thiocyanate. The characteristic retention of some metal ions of SE-cellulose layer can be recognized over a low concentration of the acid or the salt. Feasibilities for separations of analytical interest are also presented in both systems.     

Thin-layer chromatography of a number of inorganic ions on sulfoethyl cellulose in acetic acid and in acetic acid-ammonium acetate media

Summary The thin-layer chromatographic behaviour of 51 inorganic ions has been studied on a strongly acidic cation exchanger, sulfoethyl cellulose, using acetic acid and acetic acid-ammonium acetate media. Feasibilities for effective separations of analytical interest are demonstrated on the cellulose layer (0.50mm thick) in both media.     

HPTLC on inert pre-coated layers of cellulose and of silica 50000

Summary In a manner analogous to that for surface-active silica gel, HPTLC pre-coated plates for nano TLC have also been developed from two inactive sorbents. The two materials are microcrystalline cellulose and a synthetically produced, porous silica (Silica 50000) with a very low specific surface area. The chromatographic properties of these inert sorbents and of the new HPTLC pre-coated plates prepared therefrom are examined in relation to separations of amino acid mixtures and carbohydrate mixtures and are related to the chromatographic properties of the inactive sorbents and TLC precoated plates used hitherto. The figure 50000 characterizes the type of silica. The average pore diameter of this sorbent is about 5000 nm.     

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.     

Simultaneous Determination of Cadmium,Cobalt, Copper,Lead, Mercury and Nickel in Zinc Sulfate Plant Electrolyte Using Liquid Chromatography with Electrochemical and Spectrophotometric Detection

Abstract

The current efficiency (cost) of electrolytic production of high purity metallic zinc from zinc sulfate plant electrolyte is critically dependent on the concentration of a number of trace elements. The matrix, containing a very large concentration excess of zinc sulfate in concentrated sulfuric acid presents difficulties for determining low concentrations of other metals with many analytical methods. In this work it is shown that Cd, Co, Cu, Pb, Hg and Ni impurities may be simultaneously determined at concentrations less than or equal to 1 ppm using a combination of solvent extraction, high performance liquid chromatography and electrochemical or spectrophotometrie detection. Solvent extraction utilizes the formation of pyrrolidine dithiocarbamate complexes, which after removal of zinc complexes and excess ligand on an anion exchange column can be separated on a C-18 reverse phase chromatographic column and detected by UV/Visible spectrophotometrie or electrochemical detection. Other combinations of chromatographic and detection procedures were thwarted by the very large concentration excess of zinc and other problems.     

Thin-layer chromatography of inorganic lons phosphate on cellulose in acetic acid and in acetic acid-ammonium acetate media

Summary Systematic study for the chromatographic behaviour of 49 inorganic ions has been carried out on cellulose phosphate layer in acetic acid and acetic acid — ammonium acetate media. Feasibilities for the effective separations of analytical interest are demonstrated on the 0.25 mm layer in both media.     

Chiral nematic phase formation by aqueous suspensions of cellulose nanocrystals prepared by oxidation with ammonium persulfate

There is continuing interest in the growing family of nanocellulosic materials prepared from plant cell wall material. While most of the research on cellulose nanocrystals has focused on the product of sulfuric acid hydrolysis stabilized by surface sulfate half-esters, cellulose nanocrystals with surface carboxyl groups have also been prepared by oxidation of lignocellulosic materials with ammonium persulfate. The major difference is that the persulfate oxidation leads to nanocrystals stabilized by surface carboxyl groups. Some properties of cellulose nanocrystals from cotton and wood, prepared by persulfate oxidation, are compared with those observed for nanocrystals prepared by sulfuric acid hydrolysis. Evidence from polarized light microscopy showed that the nanocrystal suspensions prepared by persulfate oxidation also form chiral nematic ordered phases in water.     

Ion-exchange behaviour of metals on deae-cellulose in methanol-thiocyanate-hydrochloric acid media

Only a few metals can be adsorbed on DEAE-cellulose from aqueous thiocyanate-chloride media. However, several metal ions, including Cu(II), Zn, Cd, In, Bi and U(VI), exhibit enhanced adsorption on DEAE-cellulose from methanol-thiocyanate-hydrochloric acid mixtures. The distribution coefficients for these metals are given as functions of methanol, ammonium thiocyanate and hydrochloric add concentration. Differences in adsorption among metals permit many useful separations, including those of two-, three- and four-component mixtures, on short columns containing 1-1.5 g of DEAE-cellulose.     

Adsorption of ammonia by sulfuric acid treated zirconium hydroxide

The adsorption of ammonia on Zr(OH)(4), as well as Zr(OH)(4) treated with sulfuric acid, were examined. The results show that treating Zr(OH)(4) with sulfuric acid leads to the formation of a sulfate on the surface of the material, and that the sulfate contributes to the ammonia adsorption capacity through the formation of an ammonium sulfates species. Calcination of Zr(OH)(4) decreases the ammonia adsorption capacity of the material and limits the formation of sulfate species. NMR and FTIR spectroscopy results are presented that show the presence of two distinct ammonium species on the surface of the material. The adsorption capacity of the materials is shown to be a complex phenomenon that is impacted by the surface area, the sulfur content, and the pH of the material. The results illustrate that Zr(OH)(4), which is known to adsorb acidic gases, can be modified and used to adsorb basic gases.     

Anion-exchange behaviour of metals on deae-cellulose in hydrochloric acid-acetic acid media

The anion-exchange behaviour of 35 metal ion species on a weakly basic cellulosic ion-exchanger (DEAE-cellulose) in mixed hydrochloric acid-acetic acid media has been investigated. The sorption of metal chloro-complexes on DEAE-cellulose is greatly enhanced with increasing concentration of acetic acid. Differences in sorbability of metals allow many useful analytical separations to be conducted on short columns, containing approximately 1 g of DEAE-cellulose(Cl(-)). Procedures for the chromatographic separations of two-, three-, four- and five-component mixtures are given.     

Ce(Ⅳ)盐引发丙烯酰胺在聚乙烯醇微球表面接枝聚合的研究

以硫酸铈铵为引发剂,采用水溶液聚合体系,在酸性介质中实施了丙烯酰胺(AM)在聚乙烯醇交联微球(CPVA)表面的接枝聚合,制备了接枝微粒CPVA-g-PAM,重点研究了各种因素对接枝聚合的影响规律,探讨了铈盐引发接枝聚合的机理.实验结果表明,在Ce(Ⅳ)盐的氧化作用下,在含有大量羟基的CPVA微球表面会产生自由基,顺利地实现丙烯酰胺的自由基接枝聚合反应.PAM的接枝度首先取决于水介质中硫酸的浓度,接枝度随硫酸浓度的增大呈现先增大后减小的变化规律,当H+离子浓度为0.36mol/L时,PAM的接枝度最高,酸浓度对接枝度的影响反映了铈盐引发接枝聚合的微观机理.引发剂Ce4+盐的浓度过大,将会促进氧化终止过程,降低接枝度,适宜的Ce4+盐浓度为5.98×10-3mol/L.在接枝聚合过程中,单体丙烯酰胺浓度和反应温度也会对接枝聚合产生影响.在本研究所确定的适宜条件下,可制得PAM接枝度为27.13g/100g的接枝微粒CPVA-g-PAM.     

Effect of eluent composition on retention behavior of anions in ion chromatography on anion-exchangers modified with heparin

Effects of eluent composition on retention behavior of inorganic anions have been investigated in ion chromatography using anion-exchangers modified with heparin. Both cation and anion of the eluent affected the retention of analyte anions and unusual retention behavior was observed on the modified stationary phase. The retention time of anions decreased with decreasing eluent concentration when sodium sulfate, magnesium sulfate and chlorides of alkali metals were used as the eluent, whereas it increased with decreasing eluent concentration when aluminum sulfate, copper sulfate and sulfuric acid were used as the eluent. The retention of nitrate increased in the order of Li⁺, Na⁺, K⁺, Rb⁺ and Cs⁺ when their chlorides were used as the eluent. When sodium perchlorate and chlorides of alkaline-earth metals were used as the eluent, the eluent should include heparin. Otherwise, the modifier was partially bled from the column.     

Chromatographic behaviour of a number of metal ions on DEAE-cellulose layers in thiosulfate media

The adsorption behavior of 47 metal ions on DEAE-cellulose (Cl⁻) has been surveyed in aqueous thiosulfate solution by thin-layer chromatographic technique. The R_f values are measured as a function of thiosulfate concentration (0.010–2.0M) and are compared with those obtained on a microcrystalline cellulose Avicel SF. Generally, the ion-exchange adsorption of metal ions are weak or moderate over the thiosulfate concentration range tested except for a few metal ions like Mo(VI), Sb(III), Bi(III) etc., which have high preference to DEAE-cellulose. A variety of chromatographic distribution exhibited by metal ions allows to develop a number of separations of analytical and radiochemical interest.