Organic acid solutions in the chromatography of inorganic ions. VII. Cation exchange of Mg(II), Ca(II), Sr(II), Ba(II), Mn(II), Cd(II), Co(II), Ni(II), Zn(II), Cu(II) and Fe(III) in succinate media

Summary The cation-exchange behaviour of Mg(II), Ca(II), Sr(II), Ba(II), Mn(II), Cd(II), Co(II), Ni(II), Zn(II), Cu(II) and Fe(III) in succinate media at various concentrations and pH, was studied with Dowex 50 WX8 resin (200–400 mesh) in the NH ₄ ⁺ form. As examples separations of Cd(II)/Co(II), Cd (II)/Ni(II), Fe(III)/Cu(II)/Ni(II) and Mg(II)/Ca(II)/Sr(II)/Ba(II) have been achieved.This work was supported by C.N.R. of Italy.     

Determination of trace elements of some Egyptian crops by instrumental neutron activation,inductively coupled plasma-atomic emission spectrometric and flameless atomic absorption spectrophotometric analysis

Instrumental neutron activation analysis was used for the determination of Al, Br, Ca, Ce, Cl, Co, Cr, Cs, Eu, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc, Se, Ti, Th, V and Zn, ICP-AES for the determination Al, Ag, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, K, Li, Mg, Mn, Na, Ni, P, Sc, Sr, Ti, V and Zn and flameless AAS for the determination of Cd, Hg and Pb in egg plant, potatoes, green pepper (Leguminosae), vegetable marrow (Cucurbitaceae), pears, apple (Rosaceae), castor oil plant (Euphorbiaceae), lettuce (compositae), dill, parsley, coriander (Umbelliferae), and in some soil samples collected from Aswan province.     

A cation affinity series for a phosphinic acid ion-exchange resin

A cation affinity series was determined by the batch method for an ion-exchange resin with a phenylphosphinic acid group attached to a polystyrene/10% divinylbenzene matrix. The series in order of decreasing affinity is Pb(II), Mn(II), Cd(II), Ca(II), Zn(II), Mg(II), Ni(II), Ba(II), Sr(II), Co(II), Fe(III), Cs(I), Li(I), Na(I), Rb(I). These affinities are expressed quantitatively in terms of selectivity coefficients, and all ion-exchange reactions can be described in terms of simple displacement equations.     

Investigations on the usefulness of tiron in separation of metal ions on the macroporous anion-exchanger amberlyst A-26

The possibility of application of a sulpho-derivative of an aromatic organic complexing agent-tiron-for separation of cations on the macroporous anion-exchanger Amberlyst A-26 has been investigated. Comparative results obtained with Amberlite IRA 400 have proved the macroporous exchanger to be the more useful. The dependence of retention on pH obtained has been established by the batch method for: Ag, Ni, Co(II), Mn(II), Zn, Cd, Pb, Cr(III), Fe(III), Ga, Al, In, Bi, Ti(IV), V(V) By taking advantage of selectivity differences, the following mixtures have been separated: AlGa, AlTi(IV), Ti(IV)Ni, NiFe(III), NiFe(III)Ti(IV).     

Adsorption of metal ions on activated carbon from aqueous solutions at pH 1-13

Adsorption of microgram amounts of 20 metal species on activated carbon powder from aqueous solutions of pH 1-13 was investigated. The species examined were Cs(I), Y(III), Ce(III), Ti(IV), Zr(IV), Cr(III), Cr(VI), Mn(II), Fe(III), Co(II), Ni(II), Ru(III), Cu(II), Ag(I), Zn(II), Cd(II), Al(III), Pb(II), Sb(III) and Bi(III).     

Separation of tervalent rare earths and scandium from aluminium, iron(iii), titanium(iv), and other elements by cation-exchange chromatography in hydrochloric acid-ethanol

Tervalent rare earths and Sc are separated from the silicate-forming elements Al, Fe(III), Mg and Ti(IV), and also from Mn(II), U(VI), Be, Ga, In(III), Tl(III), Bi(III), Ni, Zn, Cu(II), Cd and Pb by cation-exchange chromatography. The other elements are eluted with 3.0 M HC1 containing 50% ethanol from a column of 60 ml of AG50W-X8 resin (200-400 mesh) while the rare earths are retained. Separation factors are larger than in aqueous hydrochloric acid. Th, Zr, Hf, Ba, Sr, Ca, K, and Rb are the only elements which accompany the rare earths group, but these can easily be separated by other methods which are described. Relevant distribution coefficients, elution curves and accurate results of quantitative separations of synthetic mixtures are presented.     

Potassium thiocarbonate as a precipitant for platinum metals

Potassium thiocarbonate reagent is proposed for the gravimetric determination of ruthenium(III), rhodium(III), palladium(II) and platinum(IV) in a highly acidic medium (pH 0.5-0.7) under suitable conditions. Ni, Zn, Mn(II), Al, Fe(III), Ti(IV), Zr, Th, Ca, Ba, Sr and Mg do not interfere. The largest relative error is 0.7% and the average error 0.2%.     

Trace elements in Variegated Bolete (Suillus variegatus) fungi

Metallic elements such as Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Rb, Sr, and Zn were determined using ICP-OES in a representative set of fifteen fruiting bodies of the edible fungus Suillus variegatus. Fruiting bodies were collected from unpolluted areas near the village of Lubichowo of the Bory Tucholskie forest complex in northern Poland in 2007?C2008. The caps were richer in Ag, Al, Cd, Cr, Cu, Fe, K,Mg, Ni, Rb, and Zn, and the stipes in Ba, Ca, Mn, Na, Pb, and Sr. Cobalt concentration in the caps and stipes was similar. In the caps, the content of the elements decreased in the order (mg per kg of dry weight): K 29000 ± 3700, Fe 1600 ± 80, Mg 990 ± 110, Rb 320 ± 86, Zn 90 ± 19, Ca 75 ± 34, Al 68 ± 32, Na 40 ± 18, Cu 19 ± 7, Mn 13 ± 7, Cd 1.0 ± 0.5, Ni 0.64 ± 0.32, Ag 0.40 ± 0.20, Cr 0.33 ± 0.06, Pb 0.20 ± 0.17, Ba 0.19 ± 0.11, Sr 0.15 ± 0.09, and Co 0.070 ± 0.050. Apparently, S. variegatus collected from background areas are relatively low in Pb and Cd and so are suitable for human consumption.     

Synthesis and analytical properties of a chelating resin functionalised with bis-(N,N'-salicylidene)1,3-propanediamine ligands

A polystyrenedivinylbenzene-based macroreticular resin was functionalised with bis-(N,N'-salicylidene)1,3-propanediamine ligands and its analytical properties have been investigated. The pH dependence of metal resin chelation has been determined for Cu(II), Ni(II), Co(II), Zn(II), Fe(II), Mn(II), Pb(II), Cd(II) and Cr(III). Trace amounts of these metal ions were quantitatively retained on the resin at neutral pH and easily recovered by elution with 1 N hydrochloric acid. The resin exhibits good chemical stability and fast equilibration with the metal ion making it useful for rapid concentration of trace amounts of metal ions on the resin columns.     

Assessment of atmospheric deposition of metals in Ha Noi using the moss bio-monitoring technique and proton induced X-ray emission

Journal of Radioanalytical and Nuclear Chemistry - The concentration of 22 metal elements including Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, As, Br, Rb, Sr, Zr, Ba and Pb in Barbula...     

Indirect cerimetric determination of gold at the milligram level

Summary A rapid volumetric method has been worked out for the indirect determination of 0.25–2.5 mg of gold in presence of many common ions. It is based on the reduction of gold(III) to metal with excess of cobalt(II) in the presence of 1,10-phenanthroline at pH 3 and 50°, and estimation of the unreacted cobalt(II) in the filtrate by visual, potentiometric or biamperometric titration with standardized cerium(IV) sulphate solution. It has been found that there is no interference from Ni(II), Pb(II), Zn(II), Cd(II), Mn(II), Mg(II), Ca(II), Al(III), Cr(III), Ti(IV), V(V) and W(VI). Interference due to Pd(II) and Ag(I) can be eliminated. Fe(III), Cu(II), Mo(VI), Hg(II) and Pt(IV) interfere, even present in small amounts.

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Zusammenfassung Ein schnelles maßanalytisches Verfahren zur indirekten Bestimmung von 0,25–2,5 mg Gold in Gegenwart vieler Ionen wurde ausgearbeitet. Es beruht auf der Reduktion zu metallischem Gold mit überschüssigem Kobalt(II) in Anwesenheit von 1,10-Phenanthrolin bei pH 3 und 50°. Die Rückbestimmung des unverbrauchten Kobalts im Filtrat erfolgt durch potentiometrische oder biamperometrische Titration mit Cer(IV)sulfat. Ni(II), Pb(II), Zn(II), Cd(II), Mn(II), Mg(II), Ca(II), Al(II), Cr(III), Ti(IV), V(V) und W(VI) stören nicht. Eine Störung durch Pd(II) oder Ag(I) kann man ausschalten. Fe(III), Cu(II), Mo(VI), Hg(II) und Pt(IV) stören auch in geringen Mengen.

     

Quantitative separation of calcium from magnesium,aluminium, iron(III) and many other elements by cation-exchange chromatography in methanolic hydrochloric acid on a macroporous resin

Calcium can be separated from Mg, Al, Cu(II), Fe(III), Ga, Zn, Mn(II), Co(II), U(VI) and Ti(IV) by cation-exchange chromatography on a column of AG MP-50 macroporous resin. Sr, Ba, Sc, Y, the lanthanides, Zr, Hf and Th are retained together with calcium. The separation factor for the Ca—Mg pair in 3 M HCl containing 50% methanol is about 20 which is considerably larger than those obtained by other ion-exchange procedures. Separations with the cation-exchange resin are sharp and quantitative. A column containing only 2 g (5.4ml) of resin is sufficient to separate up to 0.2 mmol of calcium from 2 mmol of magnesium and larger amounts of Fe(III), Cu(II) and Zn. On a 10-g column, up to 2.5 mmol of calcium can be separated easily from similar and larger amounts of other elements. Distribution coefficients for calcium and magnesium with variation of cross-linkage and variation of methanol concentration are presented, together with relevant elution curves and results for synthetic mixtures.     

Systematic study of the solvent extraction of metal β-diketonates

The extraction of 30 metals (Be, Mg, Ca. Sr, Ba, Sc, La, Ti, Zr, Th, Cr, Mo, U, Mn, Co, Fe, Ni, Pd, Cu, Ag, Zn, Cd, Hg, Al, Ga, In, Tl, Sn, Pb and Bi) by solutions of acetylacetone, benzoylacetone and dibenzoylmethane in benzene has been studied in relation to the pH values for extraction. The extraction constants and two-phase stability constants of the β-diketonates were calculated; these can be used to determine the optimum conditions for the separation of many metals. The linear relationship between the distribution coefficients of β-diketones and their corresponding β-diketonates has been confirmed.     

Systematic study of the solvent extraction of metal oxinates

The extraction of 32 metals (Be, Mg, Ca, Sr, Ba, Sc, La, Ti, Zr, Th, V, Nb, Cr, Mo, W, U, Mn, Fe, Co, Ni, Pd, Cu, Ag, Zn, Cd, Hg, Al, Ga, In, Tl, Pb and Bi) with oxine solution has been studied. The effects of pH, oxine concentration and water-soluble complexing agents (oxalic acid, tartaric acid, hydrocyanic acid, nitrilotriacetic acid, ethylenediaminetetraacetic acid and 1,2-diaminocyclohexanetetraacetic acid) have been investigated. From these results the extraction constants and stability constants ot the metal complexes with the various complexing agents investigated have been calculated.     

A rapid and precise microheterometric determination of mercury with p-dimethylamino-benzylidene-rhodanine

1. In citrate or tartrate solutions mercury formed three different compounds with p-dimethyl-amino-benzylidene-rhodanine at pH ~5,~7 and ~9.The composition of the compounds is discussed. 2. Analytical methods are presented for the determination of 0.1 mg mercury in 20 ml solution which contained 99.5–99.9% foreign metals. In most cases the error lay between zero and 1%. The foreign metals were :Ca, Ba, Mg, Zn, Mn, Ni, Co, Al, Cr(III), Fe(III), Cd, Cu, Pb, U(VI), Tl(I), Th, Ce(III), Sb(III) and Bi(III). Methods for the determination of 0.1 mg mercury in gold (III), Pt(VI), Pd(II) and silver are also presented.     

Evaluation of strontium isotope abundance ratios in combination with multi-elemental analysis as a possible tool to study the geographical origin of ciders

In order to evaluate alternative analytical methodologies to study the geographical origin of ciders, both multi-elemental analysis and Sr isotope abundance ratios in combination with multivariate statistical analysis were estimated in 67 samples from England, Switzerland, France and two Spanish regions (Asturias and the Basque Country). A methodology for the precise and accurate determination of the ⁸⁷Sr/⁸⁶Sr isotope abundance ratio in ciders by multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) was developed. Major elements (Na, K, Ca and Mg) were measured by ICP-AES and minor and trace elements (Li, Be, B, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Cd, Sn, Sb, Cs, Ba, La, Ce, W, Tl, Pb, Bi, Th and U) were measured by ICP-MS using a collision cell instrument operated in multitune mode. An analysis of variance (ANOVA test) indicated that group means for B, Cr, Fe, Ni, Cu, Se, Cd, Cs, Ce, W, Pb, Bi and U did not show any significant differences at the 95% confidence level, so these elements were rejected for further statistical analysis. Another group of elements (Li, Be, Sc, Co, Ga, Y, Sn, Sb, La, Tl, Th) was removed from the data set because concentrations were close to the limits of detection for many samples. Therefore, the remaining elements (Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba) together with ⁸⁷Sr/⁸⁶Sr isotope abundance ratio were considered for principal component analysis (PCA) and linear discriminant analysis (LDA). Finally, LDA was able to classify correctly 100% of cider samples coming from different Spanish regions, France, England and Switzerland when considering Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba and ⁸⁷Sr/⁸⁶Sr isotope abundance ratio as original variables.     

Synthesis of spherical macroporous epoxy-dicyandiamide chelating resin and properties of concentration and separation of trace metal ions from samples

A novel spherical macroporous epoxy-dicyandiamide chelating resin is synthesized simply and rapidly from epoxy resin and use for the preconcentration and separation of trace Ga(III), In(III), Bi(III), Sn(IV), Pb(II), V(V) and Ti(IV) ions from solution samples. The analyzed ions can be quantitatively concentrated by the resin at flow rate of 3.0 ml min(-1) at pH 3, and can also be desorbed with 10 ml of 4 M HCl+0.2 g thiourea from the resin column with recoveries of 97-100%. The chelating resin is reused for eight times, the recoveries of these ions are still over 92%, and a 100-1000 times of excess of Fe(III), Al(III),Ca(II), Mg(III), Ni(II), Mn(II), Co(II), Cu(II), Zn(II), and Cd(II) cause no interference in the determination of these ions by inductively-coupled plasma atomic emission spectrometry. The capacities of the resin for the analytes are in the range of 0.66-4.20 mmol g(-1). The results show the relative standard deviation for the determination of 50.0 ng ml(-1) Ga(III), In(III), Bi(III), Sn(IV) and Pb(II), 5.0 ng ml(-1) V(V) and Ti(IV) are in the range of 1.2-4.0%. The recoveries of a standard added in real solution samples are between 96 and 100%, and the concentration of each ion in mineral sample detected by the method is in good agreement with the certified value.     

Quantitative separation of beryllium from magnesium,calcium, aluminium,iron and other elements by cation-exchange chromatography in nitric acid-methanol

Beryllium is separated from Mg, Ca, Mn(II), Fe(III), Al, Co(II). Zn. U(VI), La and Gd by elution with 2.0 M nitric acid in 70 % methanol from a column of AG50W-X8 sulphonated polystyrene cation exchanger, while the other elements are retained quantitatively. Sr, Ba, Sc, Y, the other lanthanides, Zr, Hf, Th, Ga, In, Cd and Ni(II) should also be separated according to their distribution coefficients or elution behaviour. Separations are sharp and recoveries quantitative from millimolar amounts down to 10 μg of beryllium. The separation of Ti(IV) and Cu(II) from beryllium is not satisfactory and requires rather large columns. Bi(III), Pb(II), Hg(II) and the alkali metals are eluted together with beryllium, but can be separated by other methods. Typical elution curves and results for the quantitative separation of binary synthetic mixtures are presented.     

Studies on metallochromic indicators--I. Pyrocatecholphthalein as metallochromic indicator

Pyrocatecholphthalein has been used as a metallochromic indicator for the direct complexometric titrations of a number of metal ions with EDTA, both in acidic and in alkaline medium. Th, Bi(III), Ba, Sr, Ca, Mg, Mn(II), Pb(II), Cu(II), Cd, Ni, Co(II) and Zn have been successfully titrated. In comparison with Pyrocatechol Violet, this dyestuff gives sharper end-points when the titrations are done at high pH.     

Rapid coprecipitation technique using yttrium hydroxide for the preconcentration and separation of trace elements in saline water prior to their ICP-AES determination.

Yttrium hydroxide quantitatively coprecipitated Be(II), Ti(IV), Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II) at pH 9.6 - 10.0 for seawater and pH 10.5 - 11.4 for a table-salt solution. The coprecipitated elements could be determined by inductively coupled plasma atomic emission spectrometry; yttrium was used as an internal standard element. The detection limits ranged from 0.001(6) microg (Mn(II)) to 0.22 microg (Zn(II)) in 100 mL of sample solutions. The operation time required to separate 11 elements was approximately 30 min.