Preconcentration and separation of iron, zinc, cadmium and mercury, from waste water using Nile blue a grafted polyurethane foam

The present work describes a novel method for the incorporation of Nile blue A into polyurethane foam matrix. This foam material was found to be very suitable for the extraction of metal ions from aqueous solutions. The characterization of Nile blue A grafted foam and the effect of halide concentration, pH, shaking time, extraction isotherm and capacity have been investigated. This foam material was found to be suitable for the separation and preconcentration of iron (III), zinc (II), cadmium (II) and mercury (II) from waste water. The extraction was accomplished in (15-20) minutes. Iron was separated from acid medium (2-4 M HCl), zinc from (3-5 M HCl), cadmium from (4-6 M HCl) as thiocyanate complexes and mercury was separated from (1-2 M HCl) as chloride.     

Liquid–liquid extraction of Cu(II), Co(II) and Ni(II) with salicylidèneaniline from sulphate media

For a fundamental study on the development of novel extraction divalent metal, the extraction behaviour of copper(II), cobalt(II) and nickel(II) is studied with salicylidèneaniline (SAN). The phenol group in the Schiff base moiety leads to a large increase in the percentage of transition metal ions. SAN has both good reactivity towards metal ions and solubility in organic solvents. The solvent extraction of copper(II), cobalt(II) and nickel(II) with salicylidèneaniline from sulphate media is studied with the following parameters: pH, concentration of the extractant and the nature of diluent. The stoichiometry coefficients of the extracted species are determined by the slope analysis method. The extraction reaction proceeds by cation exchange mechanism and the extracted species are: CuL₂HL, CoL₂HL and NiL₂. The extaction constants are evaluated for the different diluents. Under suitable conditions of pH, the solvent extraction of cobalt(II) and nickel(II) in different diluents leads to third phase formation. This tendency is confirmed from numerical extraction constants for both metal cations (log?K _ex?=??15.10?±?0.03 for nickel(II) in CHCl₃) and (log?K _ex?=??12.56?±?0.04 for cobalt(II) in CHCl₃). The extraction efficiency is found to follow the order Cu(II)?>?Co(II)?>?Ni(II).     

Sensitive detection and semiquantitative determination of mercury(II) and lead(II) in aqueous media using polyurethane foam immobilized 1,5-di-(2-fluorophenyl)-3-mercaptoformazan

1,5-Di-(2-fluorophenyl)-3-mercaptoformazan (F(2)H(2)Dz) immobilized and plasticized with tri-n-butylphosphate (TBP) polyurethane foam (PUF) were found suitable for the detection of mercury(II) and lead(II) in extremely dilute aqueous solutions. In batch mode of extraction with immobilized F(2)H(2)Dz-foam as low as 0.05 and 0.15 mug ml(-1) of mercury(II) and lead(II), respectively were detected and the colored chelates were found more stable over 72 h. Lower concentrations of these metal ions (相似文献   

Application of stripping voltammetry method for the analysis of available copper,zinc and manganese contents in soil samples

Determination of copper (Cu), zinc (Zn) and manganese (Mn) micronutrients in soil samples have been studied for an efficient fertiliser application. Plant-available micronutrients of soils were extracted with DTPA extraction procedure, then differential pulse stripping voltammetry (DPSV) and square wave stripping voltammetry (SWSV) methods were performed with inexpensive and disposable pencil graphite electrode for determination of Cu(II), Zn(II) and Mn(II). Parameters such as deposition potential, deposition time, pH and concentration of the supporting electrolyte were optimised for these ions. Under optimised conditions, the limits of detection were found as 0.01 mg L^?1 for Cu(II) and 0.02 mg L^?1 for Zn(II) and 0.25 mg L^?1 for Mn(II). Relative standard deviation (%RSD) was 6.80, 8.86 and 3.29 for Cu(II), Zn(II) and Mn(II), respectively. The experimental study was conducted using a flame atomic absorption spectroscopy. The described stripping voltammetry methods were successfully applied for the determination of Mn(II), Cu(II) and Zn(II) in soil samples.     

Manganese(II) extraction from chloride nickel solutions with the use of trioctylamine

The influence of the nature of a modificator added to an extraction mixture containing trioctylamine, of the chloride supporting solution concentration, and of temperatures on the manganese(II) extraction from chloride nickel solutions was studied. The composition of an extracted complex was determined. The possibility of using trioctylamine with a 2-octanone addition for deep cleaning of manganese(II) from chloride nickel solutions was shown.     

Development of an analytical method based on microwave-assisted extraction and solid phase extraction cleanup for the determination of organochlorine pesticides in animal feed

A method to determine 21 organochlorine pesticides in animal feed samples using microwave assisted extraction and solid phase extraction cleanup was optimised regarding its main parameters. After extraction with hexane-acetone (50:50), three different sorbents (alumina/ENVI-Florisil, ENVI-Carb and ENVI-Carb II/PSA) were assayed for the cleanup step. Analytes were eluted with hexane-ethyl acetate (80:20) and determined by gas chromatography and electron capture detection followed by gas chromatography-mass spectrometry. ENVI-Carb and ENVI-Carb II/PSA provided colourless eluates but fewer interferent compounds were found in ENVI-Carb II/PSA chromatograms, so this system was selected to carry out the purification of the extracts. The analytical recoveries obtained with this method were close to 100% in most cases with relative standard deviations lower than 10%. These percentages were similar to those obtained with the Soxhlet extraction procedure, which shows the method suitable for the determination of organochlorine pesticides in animal feed material. The method was also validated with the analysis of a certified reference material (CRM-115 BCR), and the results obtained were in good accordance with the certified values.     

Triphenyltetrazoliumchlorid als Extraktionsreagens für Molybdän(VI)

Zusammenfassung Triphenyltetrazoliumchlorid eignet sich als Extraktionsreagens für das aus Molybdän und Brenzcatechin entstandene Komplexion. Die optimalen Extraktionsbedingungen des ternären Komplexionenassoziates mit Dichloräthan zur nachfolgenden photometrischen Bestimmung wurden ausgearbeitet. Der Extraktionsfaktor beträgt 71,4%. Fremdionen haben im allgemeinen keinen Einfluß, abgesehen von Au(III), Os(IV), Pt(IV) und Hg(II) in mehr als 6facher Menge. Die Analyse eines Molybdänkonzentrates wurde beschrieben.

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Triphenyltetrazolium chloride as extraction reagent for molybdenum(VI)

Summary Triphenyltetrazolium chloride is suitable for use as extraction reagent for the complex ion produced from molybdenum and pyrocatechol. The optimal extraction conditions for the ternary complex ion associate with dichloroethane to the subsequent photometric determination were worked out. The extraction factor is 71.4%. In general foreign ions have no influence, with the exception of Au (III), Os(IV), Pt(IV) and Hg(II), in more than 6-fold amounts. The analysis of a molybdenum concentrate is described.

     

Determination of niobium in pyrochlore ore by differential pulse polarography

A differential pulse polarographic method has been developed for the quantitative determination of niobium in pyrochlore ore. One-step polarographic curves were obtained in 0.01 mol L(-1) EDTA as supporting electrolyte. Analytical curves indicated that response was linearly dependent on Nb(V) concentration between 1.6 and 8.6 mg L(-1) in the pH range 2-5. The system is quasi-reversible and controlled by diffusion in 0.01 mol L(-1) EDTA as supporting electrolyte; the electrode process involves one-electron reduction of Nb(V) to Nb(IV). The results obtained so far for niobium in pyrochlore ore were comparable with those obtained by X-ray fluorescence determination. Ions such as Fe(III), Cr(III), As(III), Cu(II), Ni(II), Co(II), Mn(II), Sn(IV), Zn(II), V(V), Ta(V), W(VI), Ce(IV), and Ti(IV) did not interfere. Possible interference from Pb(II) can be avoided by complexation with the supporting electrolyte in the pH range 3.5 to 4.6; Mo(VI) ions can be tolerated when their concentration is one-tenth that of Nb(V).     

Spectrophotometric determination of palladium using 4-methyl-l ,2-cyclohexanedionedioxime

A procedure for the determination of palladium with 4-methyl-1,2-cyclohexanedionedioxime by an extraction -spectrophotometric method has been developed. Interference by coppcr(II), cobalt(Il), iron(II), or iron(III) can be eliminated by suitable masking agents. Ruthenium(III) must be absent or separated prior to the determination of palladium. The molar absorptivity of the bis(4-methyl-1,2-cyclohexanedionedioximato-N,N') palladium(II) complex has been calculated and found to be 1.51?10⁴ 1/moles-cm in chloroform at 280 mμ.     

Extraction titrimetric determination of copper

Lead xanthate undergoes a quantitative, stoichiometric and fast exchange reaction with copper(II), even near the equivalence point, making it a suitable reagent for an extraction titration of copper. Many other metal ions do not participate in exchange reactions with lead xanthate. making this method selective for copper.     

Application of polyethylene glycol for "electrochemical masking" in direct-current polarography

The use of polyethylene glycols (PEG) of molecular weight from 200 to 15,000 for electrochemical masking has been investigated. A pH-4.4 tartrate buffer was found to be the most suitable supporting electrolyte, and 0.1% the optimum PEG concentration. PEGs of m.w. below 600 had little effect on the waves examined, and are useless for electrochemical masking. Under the conditions chosen, the waves of Bi(III), Sb(III) and In(III) are completely suppressed; the Cd(II) and Pb(II) waves are shifted to more negative potentials, and the Tl(I) wave is scarcely affected by PEGs. The Cu(II) wave behaves differently from the others. A method is proposed for the determination of lead and/or thallium in the presence of up to 5000-fold w/w ratios of bismuth, antimony or indium. The determination of both lead and thallium is only possible when the amounts are not too different, as the waves are quite close. Copper(II) interferes.     

The reactions of diphenylcarbazide and diphenylcarbazone with cations : Part V. Extraction dissociation constants of the carbazone complexes

Extraction experiments in the system water-toluene on the diphenylcarbazone complexes of Mn(II), Fe(II) and (III). Co(II), Ni(II), Cu(ll), Zn(ll), Cd(II), Hg(I) and (II), Sn(II) and Pb(II) are described. Only uncharged complexes are formed, the formulae of which are for mercury HgD, Hg(HD)₂, Hg₂D and Hg₂(HD)₂ and for the other ions mentioned M(HD)_n, depending on the valence _n of the cation. The extraction dissociation constants, the molar extinction coefficients and the partition coefficients of the complexes funned by the cations studied were obtained, The complexes prove to be far less stable than the corresponding dithizone compounds so that diphenylcarbazone is less suitable for general analytical use than its sulphur analogue.     

Evaluation of unsymmetrical dithiodiglycolamide as novel extractant for application in selective separation of palladium(II) from aqueous solutions

A novel unsymmetrical multidentate ligand namely; N,N'-dimetyl-N,N'-didecyldithiodiglycolamide (DMD³TDGA) was synthesized and used as agent for the selective extraction of palladium(II) from hydrochloric acid solutions. A systematic investigation was carried out on the extraction of Pd(II) using DMD³TDGA. The quantitative extraction of Pd(II) with DMD³TDGA in n-dodecane is observed at ~4 M HCl. The main extracted species of Pd(II) is PdC_l2. DMD³TDGA and IR spectra of the extracted species were investigated. The extraction of palladium(II) from various concentrations of hydrochloric acid solutions in the presence of metal ions, such as Pt(IV), Rh(III), Cr(II), Ni(II), Fe(III), Nd(III), Zr(II), and Mn(II) was carried. DMD³TDGA showed very high selectivity and extractability for Pd(II). Quantitative back extraction of Pd(II) was obtained in single contact using thiourea solution. The results obtained indicated that, excellent separation of Pd(II) from the investigated metal ions can be achieved. Five successive cycles of extraction/back-extraction, indicating excellent stability and re-utilization of this new extractant can be used for selective separation of Pd(II) from other elements in hydrochloric acid medium.     

Determination of extraction constants for metal pyrrolidinedithiocarbamates and chloride-mixed metal pyrrolidinedithiocarbamates by substoichiometric extraction

Substoichiometric extraction in conjunction with a double tracer technique is employed to simultaneous determination of extraction constants of simple metal pyrrolidinedithiocarbamates and chloride-mixed metal pyrrolidinedithiocarbamates. The metals involved include Hg(II), Bi(III), In(III), As(III), Cd(II) and Fe(II). The extraction constants for Bi(III) and Cd(II) obtained are compared with the values available in the literature. The extraction constants for all the other metals are reported for the first time.     

Palladium Biosensor

In this paper we proposed a palladium(II) biosensor. The biosensor is based on determining of interactions between palladium(II) and metallothionein modified hanging mercury drop electrode by means of differential pulse voltammetry. We studied influence of two supporting electrolytes (potassium or sodium chloride) on the signals of the biosensor. Based on the results obtained we found potassium chloride (0.05 M) as the most suitable supporting electrolyte to determine palladium(II). The detection limit of the biosensor for palladium ions was evaluated as 100 nM with RSD about 10%. Moreover, we utilized the biosensor for measurement of the target molecule in the presence of human blood serum and human urine.     

the extraction of some metallic bromides from aqueous solutions with methyl ethyl ketone and methyl iso-butyl ketone

The extraction of the following metals from aqueous solutions containing excess bromide with methyl ethyl ketone (MEK), and methyl isobutyl ketone MIBK has been investigated:—Cu(I), Cu(II), Zn(II), Ni(II), Co(II), Fe(II), Fe(III), Al(III), Mn(II), Sn(II) and Sn(IV). The use of MEK was found to be strictly limited by its solubility in acidic aqueous solutions. Determinations of the formulae of the extracted compounds were attempted in two cases but were found to be not wholly satisfactory and were discontinued. An interesting reaction between the cupric bromide complex and the solvents was noticed. Separations of Fe(IIl) from Mn(II), Fe(III) from Al(III), Fe(III) from Co(Il) and Fe(III) from Ni(II) could be achieved under suitable conditions.     

Electrochemical behaviour of some naturally occurring hydroxy derivatives of 9,10-anthraquinone in chloroform at mercury and glassy carbon electrodes: application of AC polarography to the analysis of rhubarb roots

Electrochemical behaviour of some naturally occurring hydroxy derivatives of 9,10-anthraquinone such as chrysophanic acid (Ch), rhein (Rh) and emodin (Em) at mercury and glassy carbon electrodes using two different supporting electrolytes in chloroform is described. In the presence of piperidinium perchlorate (0.75M) + piperidine (0.25M) as a suitable acid supporting electrolyte, the reduction of Ch and Rh was a reversible two-electron process without complicating chemical reactions or adsorption phenomena, but the reduction process of these compounds in the presence of tetrabutylammonium perchlorate (TBAP) 0.5M + 5% acetic acid (AcOH) in chloroform was quasi-reversible. In both supporting electrolytes the overall reduction process of Em was irreversible. In the AC polarography and DP voltammetry at a GC electrode, the detection limit for Ch, Rh and Em was acceptably low and the relative standard deviation for the determination of 5 x 10(-6)M level, never exceeded 2%. AC polarography has been used for the determination of Ch and Em in a local rhubarb sample after extraction into chloroform and separation by column chromatography.     

Fluorescent sensing and selective Pb(II) extraction by a dansylamide ion-exchanger

The (bis)dansylated sulfonamide 1,2-C6H4(NHSO2C10H6-5-N(CH3)2)2 (1) extracted Pb(II) selectively from water into 1,2-dichloroethane via an ion-exchange mechanism and showed fluorescence quenching upon Pb(II) extraction. The distribution ratios for metal extraction (determined by ICP-MS) for Pb(II) were 133-1410 times higher than those for other metal cations [Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)] under identical conditions. Fluorescence quenching was observed upon Pb(II) extraction, which was dependent on Pb(II) concentration. The monodansylated control, C6H5NHSO2C10H6-5-N(CH3)2 (2), showed neither extraction nor quenching, indicating that the fluorescence effects are a direct result of Pb coordination to 1. The observed selectivity for Pb(II) is ascribed to the formation of a low-coordinate binary Pb(II)-Sulfonamido complex in the organic phase.     

Solvent extraction of zinc by 2-hexylpyridine in benzene from aqueous mineral acid — Thiocyanate media

Solvent extraction of Zn(II) by 2-hexylpyridine (HPy) in benzene has been studied from aqueous mineral acid—thiocyanate media. The extraction, though dependent on the acidity of the aqueous phase, is poor from mineral acids (HCl, HNO₃ or H₂SO₄). Addition of 0.02M KSCN to the aqueous phase enhances the distribution ratio by a factor of almost one thousand. The stoichiometry of the extracted complex established by the usual slope analysis method indicates that an ionic type complex, e.g. Zn(SCN)₄·(HPyH)₂, is responsible for extraction. Complexing anions like acetate, oxalate or citrate at 1 M concentration mask the extraction of Zn(II) almost completely. Separation factors determined at optimal conditions (0.1M HPy in benzene −0.05M H₂SO₄+0.2M SCN⁻) indicate that Zn(II), along with Hg(II), can be separated in a single extraction from a number of metals, e.g. Cs(I), Sr(II), Ln(III), Y(III), Cr(III) and (VI). Other metals of interest like Cu(II), Co(II), Fe(III), Mo(VI), U(VI) and Tc(VII) are coextracted but the separation factors are large enough to allow separation in a multistage extraction process.     

Extraction of zinc thiocyanate complex by tributyl phosphate in benzene

The species extracted is shown to be Zn(SCN)X.2TBP, where X is a common anion. Good separation factors are obtained for extraction of zinc from solutions containing silver(I), manganese(II), cobalt(II), cadmium(II), mercury(II) and thallium(III).