Studies on Environmental Pollutants: Selective Separation and Recovery of Pb(II) on Ferric Phosphate Columns

Abstract

A new method is described for the recovery and selective separation of Pb(II). The following mixtures have been separated: Hg (II) -Pb (II), Zro(II) -Pb (II), Cd (II) -Pb (II), Cu (II) -Pb (II), Mn (II) -Pb(II), Zn (II) -Pb (II), Sr (II) -Pb(II) and Ni (II)-Pb (II), on ferric phosphate columns. Cu (II), Cd (II), Ni (II), Hg (II), Mn (II), Zn (II), Sr (II) and Zro(II) were eluted with 0.01M-NH₄NO₃ and Pb(II) with a mixture of 0.1M-HNO₃ + 1.0M-NH₄NO₃ solution. Proposed studies can be applied to pollution analysis and alloy analysis.     

Spectrophotometric determination of traces of metallic ions and their mixtures with 3-methyl-1,2-cyclopentanodione dithiosemicarbazone: II. Bismuth,copper, and cobalt

The properties of bismuth, copper, and cobalt complexes of 3-methyl-1,2-cyclopentanodione dithiosemicarbazone and the optimal conditions for their formation are described. The complexes were used with success in the photometric determination of traces of bismuth, copper, and cobalt. Nine procedures are proposed for the accurate analysis of Bi(III)-Cu(II), Bi(III)-Co(II), Zn(II)-Cu(II), Cd(II)-Cu(II), Hg(II)-Cu(II), Zn(II)-Co(II), Cd(II)-Co(II), Hg(II)-Co(II), and Cu(II)-Co(II) mixtures. Satisfactory results were obtained.     

Metal complexes of isonicotinic acid hydrazide

Complexes of platinum(IV), ruthenium(III), rhodium(III), iridium(III), gold(III), dioxouranium(II), zinc(II), cadmium(II), mercury(II) and manganese(II) with isonicotinic acid hydrazide were prepared and characterized on the basis of analytical, conductometric, magnetic susceptibility and spectral data. Platinum(IV) ruthenium(III), rhodium(III), iridium(III), dioxouranium(II) and manganese(II) form six-coordinate complexes while gold(III), zinc(II), cadmium(II) and mercury(II) form four coordinate complexes.     

Organic acid solutions in the chromatography of inorganic ions VIII. Cation-exchange of Mn(II), Cd(II), Co(II), Ni(II), Zn(II), Cu(II), Fe(III), Sc(III), Y(III), Eu(III), Dy(III), Ho(III), Yb(III), Ti(IV) and Nb(V) in malate media

Summary The cation-exchange behaviour of Mn(II), Cd(II), Co(II), Ni(II), Zn(II), Cu(II), Fe(III), Sc(III), Y(III), Eu(III), Dy(III), Ho(III), Yb(III), Ti(IV) and Nb(V) in malate media at various concentrations and pH, was studied with Dowex 50 WX8 resin (200–400 mesh) in the ammonium form. Separation of Fe(III)/Cu(II), Fe(III)/Cu(II)/Zn(II), Fe(III)/Co(II)/Mn(II), Cu(II)/Ni(II)/Mn(II), Fe(III)/Cu(II)/Co(II)/Mn(II), Fe(III)/Cu(II)/Ni(II)/Cd(II), Yb(III)/Eu(III), Sc(III)/Y(III),Sc(III)/Yb(III)/Dy(III) and Nb(V)/Yb(III)/Ho(III) has been achieved, among others.This work was supported by C.N.R. of Italy.     

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.     

Dynamic adsorption and desorption of heavy metal ions on poly(acrylaminophosphonic-carboxyl-hydrazide) chelating fiber

The dynamic adsorption and desorption properties, including the effect of pH value and flow rate on the adsorption, eluent acidity and volume, eluting velocity and re-use, of Cu(II), Pb(II), Zn(II), Cd(II), Mn(II), Ni(II), Co(II) and Hg(II) ions on the column loaded with poly(acrylaminophosphonic-carboxyl-hydrazide) chelating fiber were investigated. The recovery of Mn(II), Co(II), Cd(II), Ni(II) and Zn(II) ions in the presence of Na, K, Ca and Mg ions was examined. The preconcentration of trace amounts of Mn(II), Co(II), Cd(II), Ni(II) and Zn(II) ions from model solution samples was carried out with satisfactory results. The amount of the metal ions detected after preconcentration and recovery by this technique was basically in agreement with the added amount. The method is rapid, precise and simple. Received: 15 October 1997 / Revised: 17 March 1998 / Accepted: 20 March 1998     

Thermal analysis of some metal benzohydroxamates

The preparation and thermal analysis of metal chelates of benzohydroxarnic acid (BHA) with Al(III), Cd(II), Co(II), Cu(II) (two compounds), Fe(III), La(III), Pb(II), Mn(II), Ni(II), U(VI) and Zn(II) is discussed. The Al(III), La(III), Pb(II) and Mn(II) chelates are new compounds. DTA and TGA curves of the chelates and of BHA are presented, and the heats of decomposition of the chelates are estimated.     

Organic acid solutions in the chromatography of inorganic ions-IV: cation-exchange of Mn(II), Cd(II), Co(II), Ni(II), Cu(II), Al(III) and Fe(III) in tartrate media

The cation-exchange behaviour of Mn(II), Cd(II), Co(II), Ni(II), Cu(II), Al(III) and Fe(III), in tartaric acid media was studied. Separations of Fe(III), Cu(II), Ni(II), Co(II), Cd(II) and Mn(II) on Dowex 50W X8 have been achieved.     

Formation of 1 D and 3 D coordination polymers in the solid state induced by mechanochemical and annealing treatments: bis(3-cyano-pentane-2,4-dionato) metal complexes

Bis(3-cyano-pentane-2,4-dionato) (CNacac) metal complex, [M(CNacac)(2)], which acts as both a metal-ion-like and a ligand-like building unit, forms supramolecular structures by self-assembly. Co-grinding of the metal acetates of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) with CNacacH formed a CNacac complex in all cases: mononuclear complex was formed in the cases of Mn(II), Cu(II) and Zn(II), whereas polymeric ones were formed in the cases of Fe(II), Co(II) and Ni(II). Subsequent annealing converted the mononuclear complexes of Mn(II), Cu(II) and Zn(II) to their corresponding polymers as a result of dehydration of the mononuclear complexes. The resultant Mn(II), Fe(II), Co(II), Ni(II) and Zn(II) polymeric complexes had a common 3 D structure with high thermal stability. In the case of Cu(II), a 1 D polymer was obtained. The Mn(II), Cu(II) and Zn(II) polymeric complexes returned to their original mononuclear complexes on exposure to water vapour but they reverted to the polymeric complexes by re-annealing. Co-grinding of metal chlorides with CNacacH and annealing of the mononuclear CNacac complexes prepared from solution reactions were also examined for comparison. [Mn(CNacac)(2)(H(2)O)(2)], [M(CNacac)(2)(H(2)O)] (M=Cu(II) and Zn(II)) and [M(CNacac)(2)](infinity) (M=Mn(II), Fe(II) and Zn(II)) are new compounds, which clearly indicated the power of the combined mechanochemical/annealing method for the synthesis of varied metal coordination complexes.     

Solvent extraction of metals with potassium-dihydro-bispyrazolyl-borate

The extraction of Cu(II), Ni(II), Co(II), Cd(II), Zn(II), Pb(II) and Mn(II) with potassium-dihydro-bispyrazolyl-borate (H(2)BPz(2)(-)) in dichloromethane has been studied. Extraction constants (logK(ex)) have been calculated for all metal systems and were compared with those obtained with dibenzoylmethane (DBM), thenoyltrifluoroacetone (HTTA) and 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (HPMBP). The method has been used for the determination of Cu(II), Co(II), Cd(II), Zn(II), Pb(II) and Mn(II) in standard alloys and for preconcentration of metal ions in synthetic samples.     

A new chelating ion-exchanger containing p-bromophenylhydroxamic acid as functional group-IV: column separations on a hydroxamic acid resin

A new chelating resin based on macroreticular acrylonitrile-divinylbenzene copolymer and containing hydroxamic acid functional groups has been synthesized. It is highly stable in acidic and alkaline solutions. The sorption characteristics of Cu(II), Cd(II), Pb(II), Zn(II), U(VI), Cr(VI), V(V), Co(II), Ni(II), Ca(II) and Mg(II) have been investigated over the pH range 1.0-6.0. The effect of various electrolytes at different ionic strengths on the K(d) values for Cu(II), Cd(II), Pb(II) and Zn(II) has been studied systematically. Chromatographic separations of copper(II) and nickel(II) from cobalt (II), and of uranium(VI) from chromium(VI) by selective sorption at controlled pH, have been developed. The ion-exchanger can be used for purification of inorganic salts, and analysis of brass and bauxite.     

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.

     

Capillary gas chromatographic analysis of pyrrolidinedithiocarbamate metal chelates

Pyrrolidinedithiocarbamate (PDTC) chelates of Zn(II), Cu(II), Ni(II), Co(III), Fe(III), Mn(II), Cr(III), and VO(II) were analysed by capillary GC on a DB-1701 column (30 m x 0.25 mm id) with flame ionisation detection (FID). Linear calibrations were attained within "1-30 microg/mL" for Ni(II), Fe(III), Mn(II), Cr(III), Cu(II), and VO(II), and within "2-50 microg/mL" for Co(III) and Zn(II). The limits of detection were in the "150-500 ng/mL" range, corresponding to 15-50 pg amounts reaching the FID system. The optimised method was applied to the determination of Cu(II) and Ni(II) in coins, and that of Zn(II), Cu(II), Ni(II), Fe(III), Mn(II), Cr(III), and VO(II) in pharmaceutical preparations with relative standard deviations within 1.1-5.2%. The results obtained are in good agreement with sewage water samples and the declared values for the pharmaceutical formulations, or with the results of AAS of metal contents in coins, pharmaceutical preparations, and sewage water samples.     

Selective Electrochemical Analysis of Various Metal Ions at an EDTA Bonded Conducting Polymer Modified Electrode

An EDTA‐bonded conducting polymer modified electrode was prepared and characterized by FT‐IR. The modified electrode was used for the selective electrochemical analysis of various trace metal ions such as, Cu(II), Hg(II), Pb(II), Co(II), Ni(II), Fe(II), Cd(II), and Zn(II) at the different pHs by linear sweep and square wave voltammetry. Dynamic ranges were obtained using square wave voltammetry from 0.1 μM to 10.0 μM for Co(II), Ni(II), Cd(II), Fe(II), and Zn(II) and 0.5 nM to 20 nM for Cu(II), Hg(II), and Pb(II) after 10 min of preconcentration. The detection limits were determined to be 0.1 nM, 0.3 nM, 0.4 nM, 50.0 nM, 60.0 nM, 65.0 nM, 80.0 nM, and 90.0 nM for Cu(II), Hg(II), Pb(II), Co(II), Ni(II), Cd(II), Fe(II), and Zn(II), respectively. The technique offers an excellent way for the selective trace determination of various heavy metal ions in a solution.     

Dynamic adsorption and desorption of heavy metal ions on poly(acrylaminophosphonic-carboxyl-hydrazide) chelating fiber

The dynamic adsorption and desorption properties, including the effect of pH value and flow rate on the adsorption, eluent acidity and volume, eluting velocity and re-use, of Cu(II), Pb(II), Zn(II), Cd(II), Mn(II), Ni(II), Co(II) and Hg(II) ions on the column loaded with poly(acrylaminophosphonic-carboxyl-hydrazide) chelating fiber were investigated. The recovery of Mn(II), Co(II), Cd(II), Ni(II) and Zn(II) ions in the presence of Na, K, Ca and Mg ions was examined. The preconcentration of trace amounts of Mn(II), Co(II), Cd(II), Ni(II) and Zn(II) ions from model solution samples was carried out with satisfactory results. The amount of the metal ions detected after preconcentration and recovery by this technique was basically in agreement with the added amount. The method is rapid, precise and simple. Received: 15 October 1997 / Revised: 17 March 1998 / Accepted: 20 March 1998     

Synthesis, spectroscopic characterization and magnetic properties of homo- and heterodinuclear complexes of transition and non-transition metal ions with a new Schiff base ligand

Four homodinuclear complexes of Ni(II)-Ni(II), Cu(II)-Cu(II), Co(II)-Co(II) and Co(III)-Co(II) and five heterodinuclear complexes of Co(III)-Zn(II), Co(III)-Cu(II), Co(III)-Ni(II), Cu(II)-Zn(II) and Zn(II)-Cu(II) with the octadentate Schiff base compartmental ligand 1,8-N-bis(3-carboxy)disalicylidene-3,6-diazaoctane-1,8-diamine (H4fsatrien) have been synthesized. The complexes have been characterized with the help of elemental analyses, molecular weights, molar conductances, magnetic susceptibilities and spectroscopic (UV-vis, IR, ESR) data. Cryomagnetic data also helped to elucidate the structural features of the Cu(II) complexes.     

Spectrophotometric determination of traces of metallic ions and their mixtures with 3-methyl-1,2-cyclopentanodione dithiosemicarbazone: I. Zinc,cadmium, and mercury

The properties of zinc, cadmium, and mercury complexes of 3-methyl-1,2-cyclopentanodione dithiosemicarbazone and the optimal conditions for their formation are described. The complexes were used with success in the photometric determination of traces of zinc, cadmium, and mercury. Seven procedures are proposed for the accurate analysis of Zn(II)-Cd(II), Zn(II)-Hg(II), Zn(II)-Bi(III), Cd(II)-Hg(II), Cd(II)-Bi(III), Hg(II)-Bi(III), and Zn(II)-Cd(II)-Hg(II) mixtures. Satisfactory results were obtained.     

Mononuclear transition and non-transition complexes of amlodipine besylate as antihypertensive agent: synthesis,spectral, thermal,and antimicrobial studies

Mononuclear Mn(II), Co(II), Ni(II), Zn(II), Cd(II), Mg(II), Sr(II), Ba(II), Ca(II), Pt(IV), Au(III), and Pd(II) complexes of the drug amlodipine besylate (HL) have been synthesized and characterized by elemental analysis, spectroscopic technique (IR, UV–Vis, solid reflectance, scanning electron microscopy, X-ray powder diffraction, and ¹H-NMR) and magnetic measurements. The elemental analyses of the complexes are confirmed by the stoichiometry of the types [M(HL)(X)₂(H₂O)]·nH₂O [M = Mn(II), Co(II), Zn(II), Ni(II), Mg(II), Sr(II), Ba(II), and Ca(II); X = Cl^? or NO₃ ^?], [Cd(HL)(H₂O)]Cl₂, [Pd(HL)₂]Cl₂, [Pt(L)₂]Cl₂, and [Au(L)₂]Cl, respectively. Infrared data revealed that the amlodipine besylate drug ligand chelated as monobasic tridentate through NH₂, oxygen (ether), and OH of besylate groups in Mn(II), Co(II), Ni(II), Zn(II), Cd(II), Mg(II), Sr(II), Ba(II), Ca(II), and Au(III) complexes, but in Pt(IV) and Pd(II) complexes, the amlodipine besylate coordinates via NH₂ and OH (besylate) groups. An octahedral geometry is proposed for all complexes except for the Cd(II), Pt(IV), and Pd(II) complexes. The amlodipine besylate free ligand and the transition and non-transition complexes showed antibacterial activity towards some Gram-positive and Gram-negative bacteria and the fungi (Aspergillus flavus and Candida albicans).     

Beiträge zur Ringofenmethodik. XV

Microchimica Acta - Ein Trennungsschema für Cs(I), Ag(I), Ba(II), Zn(II), Cd (II), Mn(II), Pb(II), Cu(II), Ni(II), Co(II), Bi(III), Al(III) und Fe(III) unter Verwendung von Dithiooxamid als...     

The stability constants of some metal chelates of triethylenetetraminehexaacetic acid (ttha)

Stability constants for Al(III), Cd(II), Co(II), Cu(II), Fe(III), Hg(II), La(III), Nd(III), Er(III), Mg(II). Mn(II), Ni(II), Pb(II), Th(IV) and Zn(II) complexes of triethylenetetraminehexaacetic acid (TTHA) have been evaluated from data obtained by pH and pM measurements. The pM method based on measurements with the mercury electrode and the redox system Fe(III)/Fe(II) proved to be very useful when binuclear complexes are formed.