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Sample records for cobaltii niii cuii

  1. Structural characterization and antioxidant properties of Cu(II) and Ni(II) complexes derived from dicyandiamide

    Science.gov (United States)

    Kertmen, Seda Nur; Gonul, Ilyas; Kose, Muhammet

    2018-01-01

    New Cu(II) and Ni(II) complexes derived from dicyandiamide were synthesized and characterised by spectroscopic and analytical methods. Molecular structures of the complexes were determined by single crystal X-ray diffraction studies. In the complexes, the Cu(II) or Ni(II) ions are four-coordinate with a slight distorted square planar geometry. The ligands (L-nPen and L-iPen) derived from dicyandiamide formed via nucleophilic addition of alcohol solvent molecule in the presence Cu(II) or Ni(II) ions. Complexes were stabilised by intricate array of hydrogen bonding interactions. Antioxidant activity of the complexes was evaluated by DPPH radical scavenging and CUPRAC methods. The complexes exhibit antioxidant activity, however, their activities were much lower than standard antioxidants (Vitamin C and trolox).

  2. Sequestration of Cu(II), Ni(II), and Co(II) by ethyleneimine immobilized on silica

    International Nuclear Information System (INIS)

    Arakaki, Luiza N.H.; Alves, Ana Paula M.; Silva Filho, Edson C. da; Fonseca, Maria G.; Oliveira, Severino F.; Espinola, Jose Geraldo P.; Airoldi, Claudio

    2007-01-01

    Thermodynamic data on interaction of Cu(II), Ni(II), and Co(II) with silica modified with ethyleneimine are obtained by calorimetric titration. The amount of ethyleneimine anchored on silica surface was estimated to be 0.70 mmol g -1 . The enthalpies of binding Ni(II), Cu(II) and Co(II), are -3.59 ± 0.001, -4.88 ± 0.001, and -7.75 ± 0.003 kJ mol -1 , respectively

  3. Artificial neural networks study of the catalytic reduction of resazurin: stopped-flow injection kinetic-spectrophotometric determination of Cu(II) and Ni(II)

    International Nuclear Information System (INIS)

    Magni, Diana M.; Olivieri, Alejandro C.; Bonivardi, Adrian L.

    2005-01-01

    An artificial neural network (ANN) procedure was used in the development of a catalytic spectrophotometric method for the determination of Cu(II) and Ni(II) employing a stopped-flow injection system. The method is based on the catalytic action of these ions on the reduction of resazurin by sulfide. ANNs trained by back-propagation of errors allowed us to model the systems in a concentration range of 0.5-6 and 1-15 mg l -1 for Cu(II) and Ni(II), respectively, with a low relative error of prediction (REP) for each cation: REP Cu(II) = 0.85% and REP Ni(II) = 0.79%. The standard deviations of the repeatability (s r ) and of the within-laboratory reproducibility (s w ) were measured using standard solutions of Cu(II) and Ni(II) equal to 2.75 and 3.5 mg l -1 , respectively: s r [Cu(II)] = 0.039 mg l -1 , s r [Ni(II)] = 0.044 mg l -1 , s w [Ni(II)] = 0.045 mg l -1 and s w [Ni(II)] = 0.050 mg l -1 . The ANNs-kinetic method has been applied to the determination of Cu(II) and Ni(II) in electroplating solutions and provided satisfactory results as compared with flame atomic absorption spectrophotometry method. The effect of resazurin, NaOH and Na 2 S concentrations and the reaction temperature on the analytical sensitivity is discussed

  4. Spectrophotometric determination of cobalt(II), nickel(II) and copper (II) with 1-(2 pyridylazo)-2-naphthol in micellar medium

    International Nuclear Information System (INIS)

    Shar, G.A.; Soomro, G.A.

    2004-01-01

    Spectrophotometric determination of cobalt(II), nickel(II) and copper(II) is carried out with 1-(2 pyridylazo)-2-naphthol as a complexing reagent in aqueous phase using non-ionic surfactant Tween 80. Beer's law is obeyed for Co(II), Ni(II) and Cu(II) over the range 0.5 - 4.0, 0.5 - 4.0 and 0.5 - 3.0 ngmL/sup -1/ with detection limit (2 σ) of 6.7, 3.2 and 3.9 ngmL/sup -1/. The max molar absorption, molar absorptivity, Sandell's sensitivity of Co(II), Ni(II) and Cu(II) are 580 nm, 570 nm and 555 nm; max (104 mol/sup -1/ cm /sup -1/) is 0.87, 1.8 and 1.6 and 6.8, 3.3 and 3.9 ng cm-2 respectively. The pH at which complex is formed for Co(II), Ni(II) and Cu(II) is 5, 5.5 and 6.5 respectively. The critical micelle concentration (CMC) of Tween 80 is 5%. The present method is compared with that of atomic absorption spectroscopy and no significant difference is noted between the two methods at 95% confidence level. The method has been applied to the determination of Co(II), Ni(II) and Cu(II) in industrial waste water and pharmaceutical samples. (author)

  5. Biologically active new Fe(II, Co(II, Ni(II, Cu(II, Zn(II and Cd(II complexes of N-(2-thienylmethylenemethanamine

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    C. SPÎNU

    2008-04-01

    Full Text Available Iron(II, cobalt(II, nickel (II, copper (II, zinc(II and cadmium(II complexes of the type ML2Cl2, where M is a metal and L is the Schiff base N-(2-thienylmethylenemethanamine (TNAM formed by the condensation of 2-thiophenecarboxaldehyde and methylamine, were prepared and characterized by elemental analysis as well as magnetic and spectroscopic measurements. The elemental analyses suggest the stoichiometry to be 1:2 (metal:ligand. Magnetic susceptibility data coupled with electronic, ESR and Mössbauer spectra suggest a distorted octahedral structure for the Fe(II, Co(II and Ni(II complexes, a square-planar geometry for the Cu(II compound and a tetrahedral geometry for the Zn(II and Cd(II complexes. The infrared and NMR spectra of the complexes agree with co-ordination to the central metal atom through nitrogen and sulphur atoms. Conductance measurements suggest the non-electrolytic nature of the complexes, except for the Cu(II, Zn(II and Cd(II complexes, which are 1:2 electrolytes. The Schiff base and its metal chelates were screened for their biological activity against Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa and the metal chelates were found to possess better antibacterial activity than that of the uncomplexed Schiff base.

  6. DNA binding and biological activity of mixed ligand complexes of Cu(II, Ni(II and Co(II with quinolones and N donor ligand

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    S.M M Akram

    2015-10-01

    Full Text Available  AbstractMixed ligand complexes of  Cu(II, Ni(II and Co(II have been synthesized by using levofloxacin and bipyridyl and characterized using spectral and analytical techniques. The binding behavior of the Ni(II and Cu(II complexes with herring sperm DNA(Hs-DNA were determined using electronic absorption titration, viscometric measurements and cyclic voltammetry measurements. The binding constant calculated  for Cu(II and Ni(II complexes are 2.0 x 104 and 4.0 x 104 M-1 respectively. Detailed analysis reveals that these metal complexes interact with DNA through intercalative binding mode. The nuclease activity of  Cu(II and Ni(II complexes with ct-DNA was carried out using agarose gel electrophoresis technique. The antioxidant activities for the synthesized complexes have been tested and the antibacterial activity for Ni(II complex was also checked.Key words: Intercalation, hypochromism, red shift and  peak potential.

  7. Complexes of Cu(II), Ni(II), Co(II), oxovanadium(IV) and dioxouranium(VI) with N,N'-ethylenebis (2-hydroxy-4-methylpropiophenoneimine)

    International Nuclear Information System (INIS)

    Patel, M.M.; Patel, M.R.; Patel, M.N.; Patel, R.P.

    1982-01-01

    Complexes of Cu(II), Ni(II), Co(II), oxovanadium(IV) and dioxouranium(VI) with the schiff base, N,N'-ethylenebis(2-hydroxy-4-methylpropiophenoneimine)(4-MeOHPEN), have been synthesised and characterised on the basis of elemental analyses, conductivity, magnetic moment, electronic and infrared spectral data. Square-planar structures are suggested for Cu(II), Ni(II) and Co(II) complexes while a distorted square-pyramidal structure is suggested for the oxovanadium(IV) complex. (author)

  8. Synthesis and properties of complexes of copper(II), nickel(II), cobalt(II) and uranyl ions with 3-(p-tolylsulphonamido)rhodamine

    International Nuclear Information System (INIS)

    El-Bindary, A.A.; El-Sonbati, A.Z.

    2000-01-01

    Metal complexes of copper(II), nickel(II), cobalt(II) and uranyl ions with 3-(p-tolylsulphonamido)rhodamine (HL) have been prepared and characterized by chemical and thermal analyses, molar conductivity , magnetic susceptibility measurements, and infrared, electronic and EPR spectra. The visible and EPR spectra indicated that the Cu(II) complex has a tetragonal geometry. From EPR spectrum of the Cu(II) complex,various parameters were calculated. The crystal field parameters of Ni(II) complex were calculated and were found to agree fairly well with the values reported for known square pyramidal complexes. The infrared spectral studies showed a monobasic bidentate behaviour with the oxygen and nitrogen donor system. Thermal stabilities of the complexes are also reported. (author)

  9. Ni(II) and Cu(II) binding with a 14-aminoacid sequence of Cap43 protein, TRSRSHTSEGTRSR.

    Science.gov (United States)

    Zoroddu, M A; Kowalik-Jankowska, T; Kozlowski, H; Salnikow, K; Costa, M

    2001-03-01

    The tetradecapeptide containing the 10 aminoacid repeated sequence on the C-terminus of the Ni(II)-induced Cap43 protein, was analyzed for Ni(II) and Cu(II) binding. A combined pH-metric and spectroscopic UV-VIS, EPR, CD and NMR study of Ni(II) and Cu(II) binding to the blocked CH3CO-Thr-Arg-Ser-Arg-Ser-His-Thr-Ser-Glu-Gly-Thr-Arg-Ser-Arg-NH2 (Ac-TRSRSHTSEGTRSR-Am) peptide, modeling a part of the C-terminal sequence of the Cap43 protein, revealed the formation of octahedral complexes involving imidazole nitrogen of histidine, at pH 5.5 and pH 7 for Cu(II) and Ni(II), respectively; a major square planar 4N-Ni(II) complex (about 100% at pH 9, log K* = -28.16) involving imidazole nitrogen of histidine and three deprotonated amide nitrogens of the backbone of the peptide was revealed; a 3N-Cu(II) complex (maximum about 70% at pH 7, log K*=-13.91) and a series of 4N-Cu(II) complexes starting at pH 5.5 (maximum about 90% at pH 8.7, log K* = -21.39 for CuH(-3)L), were revealed. This work supports the existence of a metal binding site at the COOH-terminal part of the Cap43 peptide.

  10. Synthesis and characterization of Ni(II, Cu(II and Co(III complexes with polyamine-containing macrocycles bearing an aminoethyl pendant arm

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    K. S. SIDDIQI

    2004-09-01

    Full Text Available Reaction of [M(ppn2]X2 (where M = Cu(II, Ni(II, Co(II and ppn = 1,3-diaminopropane with formaldehyde and ethylenediamine in methanol results in the ready formation of a 16-membered macrocyclic complex. The complexes were characterized by elemental anlysis, IR, EPR, electronic spectral data, magnetic moments and conductance measurements. The Cu(II, Ni(II and Co(III complexes are coordinated axially with both pendant groups of the hexadentate macrocycle. These pendant donors are attached to the macrocycle by a carbon chain. The electrical conductivities of the Cu(II and Ni(II chelates indicated them to be 1:2 electrolytes whilst those of Co(III is a 1:3 electrolyte in DMSO. The EPR spectrum of the copper complex exhibited G at 3.66, which indicates a considerable exchange interaction in the complex. Spectroscopic evidence suggests that in all of the complexes the metal ion is in an octahedral environment.

  11. Synthesis and characterisation of Cu(II), Ni(II), Mn(II), Zn(II) and VO(II ...

    Indian Academy of Sciences (India)

    Unknown

    Synthesis and characterisation of Cu(II), Ni(II), Mn(II), Zn(II) and VO(II) Schiff base complexes derived from o-phenylenediamine and acetoacetanilide. N RAMAN*, Y PITCHAIKANI RAJA and A KULANDAISAMY. Department of Chemistry, VHNSN College, Virudhunagar 626 001, India e-mail: ra_man@123india.com.

  12. Solar photocatalytic removal of Cu(II), Ni(II), Zn(II) and Pb(II): Speciation modeling of metal-citric acid complexes

    International Nuclear Information System (INIS)

    Kabra, Kavita; Chaudhary, Rubina; Sawhney, R.L.

    2008-01-01

    The present study is targeted on solar photocatalytic removal of metal ions from wastewater. Photoreductive deposition and dark adsorption of metal ions Cu(II), Ni(II), Pb(II) and Zn(II), using solar energy irradiated TiO 2 , has been investigated. Citric acid has been used as a hole scavenger. Modeling of metal species has been performed and speciation is used as a tool for discussing the photodeposition trends. Ninety-seven percent reductive deposition was obtained for copper. The deposition values of other metals were significantly low [nickel (36.4%), zinc (22.2%) and lead (41.4%)], indicating that the photocatalytic treatment process, using solar energy, was more suitable for wastewater containing Cu(II) ions. In absence of citric acid, the decreasing order deposition was Cu(II) > Ni(II) > Pb(II) > Zn(II), which proves the theoretical thermodynamic predictions about the metals

  13. SEPARATION OF Fe (III, Cr(III, Cu(II, Ni(II, Co(II, AND Pb(II METAL IONS USING POLY(EUGENYL OXYACETIC ACID AS AN ION CARRIER BY A LIQUID MEMBRANE TRANSPORT METHOD

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    La Harimu

    2010-06-01

    Full Text Available Fe (III, Cr(III, Cu(II, Ni(II, Co(II, and Pb(II  metal ions had been separated using poly(eugenyl oxyacetic acid as an ion carrier by bulk liquid membrane transport method. The effect of pH, polyeugenyl oxyacetic acid ion carrier concentration, nitric acid concentration in the stripping solution, transport time, and metal concentration were optimized. The result showed that the optimum condition for transport of metal ions was at pH 4 for ion Fe(III and at pH 5 for Cr(III, Cu(II, Ni(II, Co(II, and Pb(II ions. The carrier volumes were optimum with concentration of 1 x 10-3 M at 7.5 mL for Cr(III, Cu (II,  Ni(II, Co(II ions and at 8.5 mL for Fe(III and Pb(II ions. The concentration of HNO3 in stripping phase was optimum at 2 M for Fe(III and Cu(II ions, 1 M for Cr(III, Ni(II and Co(II ions, and 0.5 M for Pb(II ion. The optimum transport times were 36 h for Fe(III and Co(II ions, and 48 h for Cr(III, Cu (II, Ni(II, and Pb(II ions. The concentration of metal ions accurately transported were 2.5 x 10-4 M for Fe(III and Cr(III ions, and 1 M for Cu (II, Ni(II, Co(II, and Pb(II ions. Compared to other metal ions the transport of Fe(III was the highest with selectivity order of Fe(III > Cr(III > Pb(II > Cu(II > Ni(II > Co(II. At optimum condition, Fe(III ion was transported through the membrane at 46.46%.   Keywords: poly(eugenyl oxyacetic acid, transport, liquid membrane, Fe (III, Cr(III, Cu(II, Ni(II, Co(II, and Pb(II ions

  14. Coordination behavior of tetraaza [N4] ligand towards Co(II), Ni(II), Cu(II), Cu(I) and Pd(II) complexes: Synthesis, spectroscopic characterization and anticancer activity

    Science.gov (United States)

    El-Boraey, Hanaa A.

    2012-11-01

    Novel eight Co(II), Ni(II), Cu(II), Cu(I) and Pd(II) complexes with [N4] ligand (L) i.e. 2-amino-N-{2-[(2-aminobenzoyl)amino]ethyl}benzamide have been synthesized and structurally characterized by elemental analysis, spectral, thermal (TG/DTG), magnetic, and molar conductivity measurements. On the basis of IR, mass, electronic and EPR spectral studies an octahedral geometry has been proposed for Co(II), Ni(II) complexes and Cu(II) chloride complex, square-pyramidal for Cu(I) bromide complex. For Cu(II) nitrate complex (6), Pd(II) complex (8) square planar geometry was proposed. The EPR data of Cu(II) complexes in powdered form indicate dx2-y2 ground state of Cu(II) ion. The antitumor activity of the synthesized ligand and some selected metal complexes has been studied. The palladium(II) complex (8) was found to display cytotoxicity (IC50 = 25.6 and 41 μM) against human breast cancer cell line MCF-7 and human hepatocarcinoma HEPG2 cell line.

  15. Studies on some VO(IV, Ni(II and Cu(II complexes of non-symmetrical tetradentate Schiff-bases

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    Aderoju A. Osowole

    2008-08-01

    Full Text Available The coordination chemistry of VO(IV, Ni(II and Cu(II with unsymmetrical Schiff base ligands, [HO(OCH3C6H3C(CH3:N(CH2CH2N:C(CH3CH:C(C6H5OH], H2L and [HO(OCH3C6H3C(CH3:N(CH2CH2N:C(CH3CH:C(CH3OH], H2L1 (derived from condensation of 1-phenyl-1,3-butanedione/2,4-pentanedione, ethylenediamine and 5-methoxy-2-hydroxy acetophenone is discussed. The metal complexes were characterized by elemental analysis, molar conductance, magnetic susceptibility, infrared and electronic spectral measurements. They are magnetically dilute, non-electrolytes in nitromethane. The ligands are tetradentately coordinating via the imine N and enolic O atoms, resulting in 5-coordinate square-pyramidal geometry for the VO(IV complexes and 4-coordinate square-planar geometry for the Ni(II and Cu(II complexes. The assignment of geometry is supported by magnetic and spectral measurements.

  16. Unsaturated b-ketoesters and their Ni(II, Cu(II and Zn(II complexes

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    MUHAMMED BASHEER UMMATHUR

    2009-03-01

    Full Text Available A new series of b-ketoesters in which the keto group is attached to the olefinic linkage were synthesized by the reaction of methyl acetoacetate and aromatic aldehydes under specified conditions. The existence of these compounds predominantly in the intramolecularly hydrogen bonded enol form was well demonstrated from their IR, 1H-NMR and mass spectral data. Details on the formation of their [ML2] complexes with Ni(II, Cu(II and Zn(II and the nature of the bonding are discussed on the basis of analytical and spectral data.

  17. New complexes of Co(II, Ni(II, Cu(II with Schiff base N,N’-bis-(3-methoxy-saliciliden-3,3’-dimethylbenzidine

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    Alan Ionela

    2013-01-01

    Full Text Available The new N,N’-bis-(3-methoxy-saliciliden-3,3’-dimetilbenzidine (H2L Schiff base and complexes with Co(II, Ni(II and Cu(II of type [M(HLCl(H2O] (M=Co(II, Cu(II [M2L(H2O4]X2 (M=Co(II, X=ClO4 and M=Cu(II, X=NO3 and [M2L(CH3COO2] (M=Co(II, Ni(II, Cu(II were synthesised. The ligand and complexes were characterized by elemental analysis, conductibility measurements, magnetic moments at room temperature, IR, NMR, UV-VIS-NIR, EPR spectra and thermogravimetric analysis. A molar ratio of 1:1 or 1:2 between ligand and metal was determined from the elemental analysis. Except for perchlorate complex that behave as electrolyte, the rest of complexes are non-electrolytes. The spectral data suggest a tetrahedral, pseudo-tetrahedral or square-planar stereochemistry respectively, data confirmed by magnetic behaviour of complexes. The antimicrobial tests indicate a fungicide effect both for ligand and complexes.

  18. Synthesis, Characterization and Antimicrobial Activity of Cu(II, Co(II and Ni(II Complexes with O, N, and S Donor Ligands

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    Vidyavati Reddy

    2008-01-01

    Full Text Available The complexes of the type ML2 [where M = Cu(II, Co(II, and Ni(II] L = 1-phenyl-1-ene-3-(2-hydroxyphenyl-prop-2-ene with 3- substituted-5-mercapto-4-amino-1,2,4-triazoles. Schiff base ligands have been prepared by reacting 3-(2-hydroxyphenyl-1-phenylprop-2-en-1-one and 3-phenyl/pyridyl-4-amino-5-mercapto-1,2,4-triazoles in an alcoholic medium. The complexes are non-electrolytes in DMF. The resulting complexes were characterized by elemental analysis, magnetic measurements, conductivity measurements and spectral studies. The Schiff base acts as a tridentate dibasic and coordinating through the deprotonated oxygen, thioenolic sulphur and azomethine nitrogen atoms. It is found that Cu(II, Co(II, and Ni(II complexes exhibited octahedral geometry. The antimicrobial activities of ligands and its complexes were screened by cup plate method.

  19. Theoretical study of the magnetic behavior of hexanuclear Cu(II) and Ni(II) polysiloxanolato complexes.

    Science.gov (United States)

    Ruiz, Eliseo; Cano, Joan; Alvarez, Santiago; Caneschi, Andrea; Gatteschi, Dante

    2003-06-04

    A theoretical density functional study of the exchange coupling in hexanuclear polysiloxanolato-bridged complexes of Cu(II) and Ni(II) is presented. By calculating the energies of three different spin configurations, we can obtain estimates of the first-, second-, and third-neighbor exchange coupling constants. The study has been carried out for the complete structures of the Cu pristine cluster and of the chloroenclathrated Ni complex as well as for the hypotethical pristine Ni compound and for magnetically dinuclear analogues M(2)Zn(4) (M = Cu, Ni).

  20. Effect of the competition of Cu(II) and Ni(II) on the kinetic and thermodynamic stabilities of Cr(III)-organic ligand complexes using competitive ligand exchange (EDTA).

    Science.gov (United States)

    Cunha, Graziele da Costa; Goveia, Danielle; Romão, Luciane Pimenta Cruz; de Oliveira, Luciana Camargo

    2015-05-01

    The effect of competition of Cu(II) and Ni(II) on the kinetic stability of Cr(III) complexed with natural organic matter (NOM) was characterized using EDTA exchange with single-stage tangential-flow ultrafiltration. For a water sample from Serra de Itabaiana, 3% of spiked Cr(III) was exchanged, while for a sample from the Itapanhaú River, 7, 10, 10, and 21% was exchanged in experiments using Cr(III) alone and in combination with Cu(II), Ni(II), or Cu(II) + Ni(II), respectively. Times required to reach exchange equilibrium with EDTA were less than 360 min. The influence of competition from Ni(II) and Cu(II) on the availability of complexed Cr(III) was low, demonstrating preference of the ligand sites for Cr(III). This was correlated with sample humification, as confirmed by EPR and (13)C NMR analyses. Exchange efficiency was in the order Cu > Ni > Cr, and the process could be readily described by first order kinetics, with average rate constants of 0.35-0.37 h(-1). Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. Adsorption of Cu(II), Hg(II), and Ni(II) ions by modified natural wool chelating fibers

    International Nuclear Information System (INIS)

    Monier, M.; Ayad, D.M.; Sarhan, A.A.

    2010-01-01

    The graft copolymerization of ethyl acrylate (EA) onto natural wool fibers initiated by potassium persulphate and Mohr's salt redox initiator system in limited aqueous medium was carried out in heterogeneous media. Ester groups of the grafted copolymers were partially converted into hydrazide function groups followed by hydrazone formation through reaction with isatin. Also the application of the modified fibers for metal ion uptake was studied using Cu(II), Hg(II) and Ni(II). The modified chelating fibers were characterized using FTIR spectroscopy, SEM and X-ray diffraction.

  2. Adsorption of Cu(II), Hg(II), and Ni(II) ions by modified natural wool chelating fibers

    Energy Technology Data Exchange (ETDEWEB)

    Monier, M., E-mail: monierchem@yahoo.com [Chemistry Department, Drexel University, Philadelphia, PA (United States); Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt); Ayad, D.M.; Sarhan, A.A. [Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt)

    2010-04-15

    The graft copolymerization of ethyl acrylate (EA) onto natural wool fibers initiated by potassium persulphate and Mohr's salt redox initiator system in limited aqueous medium was carried out in heterogeneous media. Ester groups of the grafted copolymers were partially converted into hydrazide function groups followed by hydrazone formation through reaction with isatin. Also the application of the modified fibers for metal ion uptake was studied using Cu(II), Hg(II) and Ni(II). The modified chelating fibers were characterized using FTIR spectroscopy, SEM and X-ray diffraction.

  3. Adsorption of Cu(II), Hg(II), and Ni(II) ions by modified natural wool chelating fibers.

    Science.gov (United States)

    Monier, M; Ayad, D M; Sarhan, A A

    2010-04-15

    The graft copolymerization of ethyl acrylate (EA) onto natural wool fibers initiated by potassium persulphate and Mohr's salt redox initiator system in limited aqueous medium was carried out in heterogeneous media. Ester groups of the grafted copolymers were partially converted into hydrazide function groups followed by hydrazone formation through reaction with isatin. Also the application of the modified fibers for metal ion uptake was studied using Cu(II), Hg(II) and Ni(II). The modified chelating fibers were characterized using FTIR spectroscopy, SEM and X-ray diffraction. 2009 Elsevier B.V. All rights reserved.

  4. Synthesis, spectral, antitumor, antioxidant and antimicrobial studies on Cu(II), Ni(II) and Co(II) complexes of 4-[(1H-Benzoimidazol-2-ylimino)-methyl]-benzene-1,3-diol.

    Science.gov (United States)

    El-wakiel, Nadia; El-keiy, Mai; Gaber, Mohamed

    2015-08-05

    A new Schiff base of 2-aminobenzimidazole with 2,4-dihydroybezaldehyde (H₃L), and its Cu(II), Ni(II) and Co(II) complexes have been synthesized and characterized by elemental analyses, molar conductance, thermal analysis (TGA), inductive coupled plasma (ICP), magnetic moment measurements, IR, EI-mass, UV-Vis. and ESR spectral studies. On the basis of spectral studies and analytical data, it is evident that the Schiff base acts as dibasic tridentate ligand coordinating via deprotonated OH, NH and azomethine nitrogen atom. The results showed that Co(II) and Ni(II) complexes have tetrahedral structure while Cu(II) complexes has octahedral geometry. The kinetic and thermodynamic parameters of the thermal decomposition stages have been evaluated. The studied complexes were tested for their in vitro antimicrobial activities against some bacterial strains. The anticancer activity of the ligand and its metal complexes is evaluated against human liver Carcinoma (HEPG2) cell. These compounds exhibited a moderate and weak activity against the tested HEPG2 cell lines with IC₅₀ of 9.08, 18.2 and 19.7 μg/ml for ligand, Cu(II) and Ni(II) complexes, respectively. In vitro antioxidant activity of the newly synthesized compounds has also been evaluated. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Extraction studies of Cd(II), Cu(II), Mn(II), Ni(II) and Zn(II) using N, N', N, N' -Bis((2-hydroxy-3,5-di-tert-butylbenzyl) (2-pyridylmethyl)) -ethylenediamine as a novel ligand

    International Nuclear Information System (INIS)

    Laus, R.; Anjos, A.D.; Naves, A.

    2008-01-01

    In the present study, the use of N,N',N,N'-bis((2-hydroxy-3,5-di-tert-butylbenzyl) (2- pyridylmethyl))-ethylenediamine (H2L) as ligand was evaluated in the liquid-liquid (water- chloroform) extraction of Cd(II), Cu(II), Mn(II), Ni(II) and Zn(II). Experiments were carried out to determine the pH for maximum extraction for each metal ion by ligand, maximum extraction capacity, extraction kinetics and extraction selectivity. The results revealed that the extraction of metal ions is dependent on the pH: maximum extraction maximum was obtained in the pH range of 4.5 - 6.0 for Cu(II) and 8.0 - 9.0 for Zn(II). Cd(II) and Mn(II) were best extracted at pH 9.0 and Ni(II) at 10.0. The ligand H2L was effective for the extraction of Cd(II), Cu(II) and Zn(II) (extraction efficient, %E equal 100%), whereas %E of 76% and 23.5% were observed for Mn(II) and Ni(II), respectively. The ligand presented high selectivity for the extraction of Cu(II) at pH 4.0. (author)

  6. The Formation of Metal (M=Co(II), Ni(II), and Cu(II)) Complexes by Aminosilanes Immobilized within Mesoporous Molecular Sieves

    International Nuclear Information System (INIS)

    Park, Dong Ho; Park, Sung Soo; Choe, Sang Joon

    1999-01-01

    The immobilization of APTMS(3-(2-aminoethylamino)propyltrimethoxysilane) and AAPTMS(3-(2-(2-aminoethyl) aminoethylamino)propyltrimethoxysilane) on the surface of high quality mesoporous molecular sieves MCM-41 and MCM-48 have been confirmed by F.T.-IR spectroscopy, Raman spectroscopy, 29 Si solid state NMR, and a surface polarity measurement using Reichardt's dye. The formation of metal (Co(II), Ni(II), and Cu(II)) complexes by immobilized aminosilanes have been investigated by photoacoustic spectroscopy(PAS). The assignment of UV-Vis. PAS bands makes it possible to identify the structure of metal complexes within mesoporous molecular sieves. Co(II) ion may be coordinated mainly in a tetrahedral symmetry by two APTMS onto MCM-41, and in an octahedral one by two AAPTMS. Both Ni(II) and Cu(II) coordinated by aminosilanes within MCM-41 form possibly the octahedral complexes such as [Ni(APTMS) 2 (H 2 O) 2 ] 2+ , [Ni(AAPTMS) 2 ] 2+ , [Cu(APTMS) 2 (H 2 O) 2 ] 2+ , and [Cu(AAPTMS)(H 2 O) 3 ] 2+ , respectively. The PAS band shapes of complexes onto MCM-48 are similar to those of corresponding MCM-41 with the variation of PAS intensity. Most of metal ion(II) within MCM-41 and MCM-48 are coordinated by aminosilanes without the impregnation on the surface

  7. Spectroscopic evaluation of Co(II), Ni(II) and Cu(II) complexes derived from thiosemicarbazone and semicarbazone

    Science.gov (United States)

    Chandra, Sulekh; Kumar, Anil

    2007-12-01

    Co(II), Ni(II) and Cu(II) complexes were synthesized with thiosemicarbazone (L 1) and semicarbazone (L 2) derived from 2-acetyl furan. These complexes were characterized by elemental analysis, molar conductance, magnetic moment, mass, IR, electronic and EPR spectral studies. The molar conductance measurement of the complexes in DMSO corresponds to non-electrolytic nature. All the complexes are of high-spin type. On the basis of different spectral studies six coordinated geometry may be assigned for all the complexes except Co(L) 2(SO 4) and Cu(L) 2(SO 4) [where L = L 1 and L 2] which are of five coordinated square pyramidal geometry.

  8. Microwave synthesis, spectral, thermal and antimicrobial studies of some Ni(II) and Cu(II) Schiff base complexes

    OpenAIRE

    Mishra, A. P.; Sharma, Neha; Jain, Rajendra K.

    2012-01-01

    Se sintetizaron bases de Schiff bidentadas y tridentadas (NO), (ONO) a través de la reacción de condensación entre la metil-isobutilcetona y el 2-amino-4clorofonol y 2-hidroxiacetofenona con la hidracina del ácido isonicotínico. Los complejos metálicos 1:1 o 1:2 han sido preparados mediante la interacción de estas bases de Schiff y los iones Ni(II) y Cu(II). La síntesis fue realizada empleando el método convencional y el de microondas, y los productos fueron caracterizados por análisis elemen...

  9. Adsorption of Pb(II), Cu(II), Cd(II), Zn(II), Ni(II), Fe(II), and As(V) on bacterially produced metal sulfides.

    Science.gov (United States)

    Jong, Tony; Parry, David L

    2004-07-01

    The adsorption of Pb(II), Cu(II), Cd(II), Zn(II), Ni(II), Fe(II) and As(V) onto bacterially produced metal sulfide (BPMS) material was investigated using a batch equilibrium method. It was found that the sulfide material had adsorptive properties comparable with those of other adsorbents with respect to the specific uptake of a range of metals and, the levels to which dissolved metal concentrations in solution can be reduced. The percentage of adsorption increased with increasing pH and adsorbent dose, but decreased with increasing initial dissolved metal concentration. The pH of the solution was the most important parameter controlling adsorption of Cd(II), Cu(II), Fe(II), Ni(II), Pb(II), Zn(II), and As(V) by BPMS. The adsorption data were successfully modeled using the Langmuir adsorption isotherm. Desorption experiments showed that the reversibility of adsorption was low, suggesting high-affinity adsorption governed by chemisorption. The mechanism of adsorption for the divalent metals was thought to be the formation of strong, inner-sphere complexes involving surface hydroxyl groups. However, the mechanism for the adsorption of As(V) by BPMS appears to be distinct from that of surface hydroxyl exchange. These results have important implications to the management of metal sulfide sludge produced by bacterial sulfate reduction.

  10. Synthesis, spectral characterization thermal stability, antimicrobial studies and biodegradation of starch–thiourea based biodegradable polymeric ligand and its coordination complexes with [Mn(II), Co(II), Ni(II), Cu(II), and Zn(II)] metals

    OpenAIRE

    Nahid Nishat; Ashraf Malik

    2016-01-01

    A biodegradable polymer was synthesized by the modification reaction of polymeric starch with thiourea which is further modified by transition metals, Mn(II), Co(II), Ni(II), Cu(II) and Zn(II). All the polymeric compounds were characterized by (FT-IR) spectroscopy, 1H NMR spectroscopy, 13C NMR spectroscopy, UV–visible spectra, magnetic moment measurements, thermogravimetric analysis (TGA) and antibacterial activities. Polymer complexes of Mn(II), Co(II) and Ni(II) show octahedral geometry, wh...

  11. Synthesis, spectral characterization thermal stability, antimicrobial studies and biodegradation of starch–thiourea based biodegradable polymeric ligand and its coordination complexes with [Mn(II, Co(II, Ni(II, Cu(II, and Zn(II] metals

    Directory of Open Access Journals (Sweden)

    Nahid Nishat

    2016-09-01

    Full Text Available A biodegradable polymer was synthesized by the modification reaction of polymeric starch with thiourea which is further modified by transition metals, Mn(II, Co(II, Ni(II, Cu(II and Zn(II. All the polymeric compounds were characterized by (FT-IR spectroscopy, 1H NMR spectroscopy, 13C NMR spectroscopy, UV–visible spectra, magnetic moment measurements, thermogravimetric analysis (TGA and antibacterial activities. Polymer complexes of Mn(II, Co(II and Ni(II show octahedral geometry, while polymer complexes of Cu(II and Zn(II show square planar and tetrahedral geometry, respectively. The TGA revealed that all the polymer metal complexes are more thermally stable than their parental ligand. In addition, biodegradable studies of all the polymeric compounds were also carried out through ASTM-D-5338-93 standards of biodegradable polymers by CO2 evolution method which says that coordination decreases biodegradability. The antibacterial activity was screened with the agar well diffusion method against some selected microorganisms. Among all the complexes, the antibacterial activity of the Cu(II polymer–metal complex showed the highest zone of inhibition because of its higher stability constant.

  12. Synthesis, investigation and spectroscopic characterization of piroxicam ternary complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with glycine and DL-phenylalanine

    Science.gov (United States)

    Mohamed, Gehad G.; El-Gamel, Nadia E. A.

    2004-11-01

    The ternary piroxicam (Pir; 4-hydroxy-2-methyl- N-(2-pyridyl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with various amino acids (AA) such as glycine (Gly) or DL-phenylalanine (PhA) were prepared and characterized by elemental analyses, molar conductance, IR, UV-Vis, magnetic moment, diffuse reflectance and X-ray powder diffraction. The UV-Vis spectra of Pir and the effect of metal chelation on the different interligand transitions are discussed in detailed manner. IR and UV-Vis spectra confirm that Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine- N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its carboxylic group, in addition PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its carboxylic and amino groups. All the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. The molar conductance data reveal that most of these chelates are non electrolytes, while Fe(III)-Pir-Gly, Co(II)-, Ni(II)-, Cu(II)- and Zn(II)-Pir-PhA cheletes were 1:1 electrolytes. X-ray powder diffraction is used as a new tool to estimate the crystallinity of chelates as well as to elucidate their geometrical structures.

  13. Synthesis and characterization of heterobimetallic complexes of the type [Cu(pn2][MCl4] where M = Co(II, Ni(II, Cu(II, Zn(II, Cd(II, and Hg(II

    Directory of Open Access Journals (Sweden)

    Seema Yadav

    2016-11-01

    Full Text Available A series of new bimetallic transition metal complexes of the type [Cu(pn2] [MCl4] have been synthesized (where M = Co(II, Ni(II, Cu(II, Zn(II, Cd(II and Hg(II, pn = 1,3-diaminopropane and characterized by elemental analysis, molar conductance, TGA, IR and electronic spectra. All the compounds are 1:1 electrolyte in DMF. The Cu(II ion is square-planar while metal ions in the anionic moiety acquire their usual tetrahedral arrangement. On the basis of these studies it is concluded that anionic moiety is electrically stabilized by its cationic counterpart.

  14. Synthesis, characterization and anti-fungal evaluation of Ni(II and Cu(II complexes with a derivative of 4-aminoantipyrine

    Directory of Open Access Journals (Sweden)

    Monika Tyagi

    2017-01-01

    Full Text Available Transition metal complexes of Ni(II and Cu(II metal ions with the general stoichiometry [M(LX]X and [M(LSO4], where M = Ni(II and Cu(II, L = (1E-N-((5-((E-(2,3-dimethyl-1-phenyl-4-pyrazolineiminomethylthiophen-2-ylmethylene-2,3-dimethyl-1-phenyl-4-pyrazolineamine and X = Cl−, NO3− and SO42−, have been synthesized and characterized. The synthesized ligand and metal complexes were characterized by 1H NMR, IR, mass spectrometry, UV–Vis spectra and EPR. In molecular modelling, the geometries of the Schiff's base and metal complexes were fully optimized with respect to the energy using the 6-31g(d,p basis set. The nickel(II complexes were found to have octahedral geometry, whereas the copper(II complexes were of tetragonal geometry. The covalency factor (β and orbital reduction factor (k suggest the covalent nature of the complexes. To develop broad spectrum new molecules against seed-borne fungi, the minimum inhibitory concentration (MIC of the ligand and its metal complexes was evaluated by the serial dilution method.

  15. Physicochemical properties of 3,4,5-trimethoxybenzoates of Mn(II, Co(II, Ni(II and Zn(II

    Directory of Open Access Journals (Sweden)

    W. FERENC

    2005-09-01

    Full Text Available The complexes of Mn(II, Co(II, Ni(II, Cu(II and Zn(II with 3,4,5-trimethoxybenzoic acid anion of the formula: M(C10H11O52·nH2O, where n = 6 for Ni(II, n = 1 for Mn(II, Co(II, Cu(II, and n = 0 for Zn, have been synthesized and characterized by elemental analysis, IR spectroscopy, X–ray diffraction measurements, thermogravimetry and magnetic studies. They are crystalline compounds characterized by various symmetry. They decompose in various ways when heated in air to 1273 K. At first, they dehydrate in one step and form anhydrous salts. The final products of decomposition are oxides of the respective metals (Mn2O3, Co3O4, NiO, CuO, ZnO. The solubilities of the analysed complexes in water at 293 K are in the orders of 10-2 – 10-4 mol dm-3. The magnetic susceptibilities of the Mn(II, Co(II, Ni(II and Cu(II complexes were measured over the range of 76–303 K and the magnetic moments were calculated. The results show that the 3,4,5-trimethoxybenzoates of Mn(II, Co(II and Ni(II are high-spin complexes but that of Cu(II forms a dimer [Cu2(C10H11O54(H2O2]. The carboxylate groups bind as monodentate or bidentate chelating or bridging ligands.

  16. Antibacterial Co(II, Ni(II, Cu(II and Zn(II complexes with biacetyl-derived Schiff bases

    Directory of Open Access Journals (Sweden)

    MUHAMMAD IMRAN

    2010-08-01

    Full Text Available The condensation reactions of biacetyl with ortho-hydroxyaniline and 2-aminobenzoic acid to form bidendate NO donor Schiff bases were studied. The prepared Schiff base ligands were further utilized for the formation of metal chelates having the general formula [ML2(H2O2] where M = Co(II, Ni(II, Cu(II and Zn(II and L = HL1 and HL2. These new compounds were characterized by conductance measurements, magnetic susceptibility measurements, elemental analysis, and IR, 1H-NMR, 13C-NMR and electronic spectroscopy. Both Schiff base ligands were found to have a mono-anionic bidentate nature and octahedral geometry was assigned to all metal complexes. All the complexes contained coordinated water which was lost at 141–160 °C. These compounds were also screened for their in vitro antibacterial activity against four bacterial species, namely: Escherichia coli, Staphylococcus aureus, Salmonella typhi and Bacillus subtilis. The metal complexes were found to have greater antibacterial activity than the uncomplexed Schiff base ligands.

  17. Synthesis, Spectral and Antimicrobial Studies of Some Co(II, Ni(II and Cu(II Complexes Containing 2-Thiophenecarboxaldehyde Moiety

    Directory of Open Access Journals (Sweden)

    A. P. Mishra

    2012-01-01

    Full Text Available Some new Schiff base metal complexes of Co(II, Ni(II and Cu(II derived from 3-chloro-4-fluoroaniline (HL1 and 4-fluoroaniline (HL2 with 2-thiophenecarboxaldehyde have been synthesized and characterized by elemental analysis, FT-IR, FAB-mass, molar conductance, electronic spectra, ESR and magnetic susceptibility. The complexes exhibit coordination number 4 or 6. The complexes are colored and stable in air. Analytical data revealed that all the complexes exhibited 1:2 (metal: ligand ratio. FAB-mass data show degradation pattern of the complexes. The Schiff base and metal complexes show a good activity against the bacteria; B. subtilis, E. coli and S. aureus and fungi A. niger, A. flavus and C. albicans. The antimicrobial results also indicate that the metal complexes are better antimicrobial agents as compared to the Schiff bases.

  18. Synthesis, characterization and biological studies of 2-(4-nitro phenylaminocarbonyl)benzoic acid and its complexes with Cr(III), Co(II), Ni(II), Cu(II) and Zn(II)

    International Nuclear Information System (INIS)

    Aqeel Ashraf, M.; Jamil Maah, M.; Yusuf, I.

    2012-01-01

    Cr(III), Co(II), Ni(II), Cu(II) and Zn(II) salts of 2-(4-nitro phenylaminocarbonyl)benzoic acid were characterized by physical, analytical and spectroscopic studies and checked for their in-vitro antimicrobial activity against three bacterial strains, Mycobacterium smegmatis (Gram +ve), Escherichia coli (Gram -ve), Pseudomonas aeuroginosa (Gram -ve) and three fungal strains, Nigrospora oryzae, Aspergillus niger and Candida albicans. The antimicrobial activities of the metal complexes - were found to be greater than those of 2-(4-nitro phenylaminocarbonyl)benzoic acid alone.

  19. Synthesis and characterization of polychelates of Cu(II), Ni(II), Co(II), Mn(II), Zn(II), oxovanadium(IV) and dioxouranium(VI) with 2,4-dihydroxybenzaldehyde-urea-formaldehyde polymer

    International Nuclear Information System (INIS)

    Patel, G.C.; Pancholi, H.B.; Patel, M.M.

    1991-01-01

    Polychelates of Cu(II), Ni(II), Co(II), Mn(II), Zn(II), oxovandium(IV) and dioxouranium(VI) with 2,4-dihydroxybenzaldehyde (2,4-DB)-urea(U)-formaldehyde(F) polymer (2,4-DBUF) have been prepared. Elemental analyses of the polychelates indicate a metal:ligand ratio of 1:2. The structures of the polychelates have been assigned on the basis of their elemental analyses, IR, reflectance spectra, magnetic moment, thermal data and their electrical conductivity behaviour. (author). 1 tab., 18 refs

  20. Ni(II) ion-imprinted solid-phase extraction and preconcentration in aqueous solutions by packed-bed columns

    International Nuclear Information System (INIS)

    Ersoez, Arzu; Say, Ridvan; Denizli, Adil

    2004-01-01

    Solid-phase extraction (SPE) columns packed with materials based on molecularly imprinted polymers (MIPs) were used to develop selective separation and preconcentration for Ni(II) ion from aqueous solutions. SPE is more rapid, simple and economical method than the traditional liquid-liquid extraction. MIPs were used as column sorbent to increase the grade of selectivity in SPE columns. In this study, we have developed a polymer obtained by imprinting with Ni(II) ion as a ion-imprinted SPE sorbent. For this purpose, NI(II)-methacryloylhistidinedihydrate (MAH/Ni(II)) complex monomer was synthesized and polymerized with cross-linking ethyleneglycoldimethacrylate to obtain [poly(EGDMA-MAH/Ni(II))]. Then, Ni(II) ions were removed from the polymer getting Ni(II) ion-imprinted sorbent. The MIP-SPE preconcentration procedure showed a linear calibration curve within concentration range from 0.3 to 25 ng/ml and the detection limit was 0.3 ng/ml (3 s) for flame atomic absorption spectrometry (FAAS). Ni(II) ion-imprinted microbeads can be used several times without considerable loss of adsorption capacity. When the adsorption capacity of nickel imprinted microbeads were compared with non-imprinted microbeads, nickel imprinted microbeads have higher adsorption capacity. The K d (distribution coefficient) values for the Ni(II)-imprinted microbeads show increase in K d for Ni(II) with respect to both K d values of Zn(II), Cu(II) and Co(II) ions and non-imprinted polymer. During that time K d decreases for Zn(II), Cu(II) and Co(II) ions and the k' (relative selectivity coefficient) values which are greater than 1 for imprinted microbeads of Ni(II)/Cu(II), Ni(II)/Zn(II) and Ni(II)/Co(II) are 57.3, 53.9, and 17.3, respectively. Determination of Ni(II) ion in sea water showed that the interfering matrix had been almost removed during preconcentration. The column was good enough for Ni determination in matrixes containing similar ionic radii ions such as Cu(II), Zn(II) and Co(II)

  1. Micellar effect on metal-ligand complexes of Co(II, Ni(II, Cu(II and Zn(II with citric acid

    Directory of Open Access Journals (Sweden)

    Nageswara Rao Gollapalli

    2009-12-01

    Full Text Available Chemical speciation of citric acid complexes of Co(II, Ni(II, Cu(II and Zn(II was investigated pH-metrically in 0.0-2.5% anionic, cationic and neutral micellar media. The primary alkalimetric data were pruned with SCPHD program. The existence of different binary species was established from modeling studies using the computer program MINIQUAD75. Alkalimetric titrations were carried out in different relative concentrations (M:L:X = 1:2:5, 1:3:5, 1:5:3 of metal (M to citric acid. The selection of best chemical models was based on statistical parameters and residual analysis. The species detected were MLH, ML2, ML2H and ML2H2. The trend in variation of stability constants with change in mole fraction of the medium is explained on the basis of electrostatic and non-electrostatic forces. Distributions of the species with pH at different compositions of micellar media are also presented.

  2. Foam separation of Cu (II) and Ni(II) from aqueous solutions and simulated wastewaters

    International Nuclear Information System (INIS)

    Shakir, K.; Beheir, Sh.G.; Aziz, M.

    2003-01-01

    Batch experiments on the removal of Cu(II) and Ni(II) from aqueous solutions were performed through two foam separation techniques: precipitate flotation (PTF) an adsorbing colloid flotation (ACF). In ACF, Fe(III), oxyhydroxide was used as co precipitant and/or adsorbing colloid and sodium lauryl sulfate was used as a collector. ACF required a lower collector concentration than PTF. foreign ions were found to decrease the percent removal, the extent of decrease being higher by divalent ions than that by monovalent ones. However, the percent removal could be improved, even in presence of foreign ions, by addition of Al(II) as an activator. High removals could be attained for Cu(II) and Ni(II) from simulated wastewaters containing different concentrations of both metal ions. The addition of concentrations below the limits recommended by the egyptian regulations for environmental discharge

  3. Synthesis, characterisation and electrochemical behaviour of Cu(II)

    Indian Academy of Sciences (India)

    Neutral tetradentate N2O2 type complexes of Cu(II), Ni(II), Co(II) and Zn(II) have been synthesised using the Schiff base formed by the condensation of acetylacetone and p-anisidine. Microanalysis, molar conductance, magnetic susceptibility, IR, UV-Vis, 1H NMR, CV and EPR studies have been carried out to determine the ...

  4. Synthesis and studies on Cu(II), Co(II), Ni(II) complexes of Knoevenagel β-diketone ligands

    Science.gov (United States)

    Sumathi, S.; Tharmaraj, P.; Sheela, C. D.; Anitha, C.

    2012-11-01

    Transition metal complexes of various acetylacetone based ligands of the type ML [where M = Cu(II), Ni(II), Co(II); L = 3-(aryl)-pentane-2,4-dione] have been synthesized. The structural features have been derived from their elemental analysis, magnetic susceptibility, molar conductance, IR, UV-Vis, 1H NMR, Mass and ESR spectral studies. Conductivity measurements reveal that all the complexes are non-electrolytic in nature. Spectroscopic and other analytical data of the complexes suggest octahedral geometry for other metal(II) complexes. The redox behavior of the copper(II) complexes have been studied by cyclic voltammetry. The free ligands and their metal complexes have been screened for their in vitro biological activities against the bacteria Pseudomonas aeruginosa, Escherichia coli and Staphylococcus aureus as well as the fungus Candida albicans by well diffusion method. The zone of inhibition value indicates that the most of the metal(II) complexes are found to possess increased activities compared to those of the free ligands. All synthesized compounds may serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic generation (SHG) efficiency of the ligands (L1-L3) was found to be considerable effect than that of urea and KDP (potassium dihydrogen phosphate).

  5. Application of Zr/Ti-Pic in the adsorption process of Cu(II), Co(II) and Ni(II) using adsorption physico-chemical models and thermodynamics of the process; Aplicacao de Zr/Ti-PILC no processo de adsorcao de Cu(II), Co(II) e Ni(II) utilizando modelos fisico-quimicos de adsorcao e termodinamica do processo

    Energy Technology Data Exchange (ETDEWEB)

    Guerra, Denis Lima; Airoldi, Claudio [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Quimica. Dept. de Quimica Inorganica]. E-mail: dlguerra@iqm.unicamp.br; Lemos, Vanda Porpino; Angelica, Romulo Simoes [Universidade Federal do Para (UFPa), Belem (Brazil); Viana, Rubia Ribeiro [Universidade Federal do Mato Grosso (UFMT), Cuiaba (Brazil). Inst. de Ciencias Exatas e da Terra. Dept. de Recursos Minerais

    2008-07-01

    The aim of this investigation is to study how Zr/Ti-Pic adsorbs metals. The physico-chemical proprieties of Zr/Ti-Pic have been optimized with pillarization processes and Cu(II), Ni(II) and Co(II) adsorption from aqueous solution has been carried out, with maximum adsorption values of 8.85, 8.30 and 7.78 x-1 mmol g{sup -1}, respectively. The Langmuir, Freundlich and Temkin adsorption isotherm models have been applied to fit the experimental data with a linear regression process. The energetic effect caused by metal interaction was determined through calorimetric titration at the solid-liquid interface and gave a net thermal effect that enabled the calculation of the exothermic values and the equilibrium constant. (author)

  6. Application of Carrier Element-Free Co-precipitation Method for Ni(II), Cu(II) and Zn(II) Ions Determination in Water Samples Using Chrysin

    International Nuclear Information System (INIS)

    Layth Imad Abd Ali; Wan Aini Wan Ibrahim; Azli Sulaiman; Mohd Marsin Sanagi

    2015-01-01

    A co-precipitation method was developed to separate and pre-concentrate Ni(II), Cu(II) and Zn(II) ions using an organic co precipitant, chrysin without adding any carrier element termed as carrier element-free co-precipitation (CEFC). Analytes were determined using flame atomic absorption spectrometry (FAAS). The influence of analytical conditions, such as pH of the solution, quantity of co-precipitant, standing time, centrifugation rate and time, sample volume, and interference of concomitant ions were investigated over the recovery yields of the trace metals. The limit of detection, the limit of quantification and linearity range obtained from the FAAS measurements were found to be in the range of 0.64 to 0.86 μg L -1 , 2.13 to 2.86 μg L -1 and 0.9972 to 0.9989 for Ni(II), Cu(III) and Zn(II) ions, respectively. The precision of the method, evaluated as the relative standard deviation (RSD) obtained after analyzing a series of 10 replicates, was between 2.6 % to 3.9 % for the trace metal ions. The proposed procedure was applied and validated by analyzing river water reference material for trace metals (SLRS-5) and spiking trace metal ions in some water samples. The recoveries of the analyte metal ions were between 94.7-101.2 %. (author)

  7. Synthesis and Characterization of Some New Cu(II, Ni(II and Zn(II Complexes with Salicylidene Thiosemicarbazones: Antibacterial, Antifungal and in Vitro Antileukemia Activity

    Directory of Open Access Journals (Sweden)

    Tudor Rosu

    2013-07-01

    Full Text Available Thirty two new Cu(II, Ni(II and Zn(II complexes (1–32 with salicylidene thiosemicarbazones (H2L1–H2L10 were synthesized. Salicylidene thiosemicarbazones, of general formula (XN-NH-C(S-NH(Y, were prepared through the condensation reaction of 2-hydroxybenzaldehyde and its derivatives (X with thiosemicarbazide or 4-phenylthiosemicarbazide (Y = H, C6H5. The characterization of the new formed compounds was done by 1H-NMR, 13C-NMR, IR spectroscopy, elemental analysis, magnetochemical, thermoanalytical and molar conductance measurements. In addition, the structure of the complex 5 has been determined by X-ray diffraction method. All ligands and metal complexes were tested as inhibitors of human leukemia (HL-60 cells growth and antibacterial and antifungal activities.

  8. Synthesis, characterization and biological studies of 2-(4-nitrophenylamino-carbonyl)benzoic acid and its complexes with Cr(III), Co(II), Ni(II), Cu(II) and Zn(II)

    International Nuclear Information System (INIS)

    Imran, M; Nazir, S.; Latif, S.; Mahmood, Z.

    2010-01-01

    Cr(III), Co(II), Ni(II), Cu(II) and Zn(II) complexes of 2-(4-Nitrophenyl aminocarbonyl)benzoic acid were synthesized and characterized on the basis of physical, analytical and spectroscopic data. The ligands, as well as its metal complexes were checked for their in-vitro antimicrobial activity against three bacterial strains, Mycobacterium smegmatis, Escherichia coli, Pseudomonas aeuroginosa, and three fungal strains, Nigrospora oryzae, Aspergillus niger and Candida albicans. Disc diffusion method and Tube diffusion test were used for antibacterial and antifungal activities, respectively. The synthesized complexes only show significant antifungal activity but inactive for antibacterial, however, in general, the metal complexes were found to be more active against antimicrobial activities as compared to their un complexed ligand. (author)

  9. Synthesis, characterization and antibacterial activity of some novel symmetrical n/sup 3/, n/sup 3/-bis(disubstituted)isophthalyl-bis(thioureas) and their Cu(II) and Ni(II) complexes

    International Nuclear Information System (INIS)

    Jamil, M.; Zubair, M.; Rasool, N.; Bukhari, I.H.; Farid, M.A.; Altaf, A.A.

    2013-01-01

    A series of some novel N/sup 3/,N/sup 3/-bis(disubstituted) isophthalyl-bis(thioureas) compounds with general formula (C/sub 6/H/sub 4/(CONHCSNHR)/sub 2/), where R = 4-C/sub 6/H/sub 4/COOH(L/sub 1/), 3-NO/sub 2/C/sub 6/H/sub 4/(L/sub 2/), 2-NO/sub 2/C/sub 6/H/sub 4/(L/sub 3/), 4-CH/sub 3/C/sub 6/H/sub 4/(L/sub 4/), 2-CH/sub 3/C/sub 6/H/sub 4/(L/sub 5/), 3-CH/sub 3/C/sub 6/H/sub 4/(L/sub 6/) and their Cu(II) and Ni(II) complexes have been synthesized. (L/sub 1/-L/sub 6/) have been prepared in good to excellent yields by reaction of isophthaloyl isothiocyanate with primary amines using dry acetone as solvent. The stoichiometric reaction between the metal (II) ion and synthesized ligands in molar ratio of M : L (1 : 1) resulted in the formation of the metal complexes of type (ML)2 (where M = Cu(II) and Ni(II). These compounds (L/sub 1/-L/sub 6/) and their metal (II) complexes have been characterized by elemental analyses, Infrared spectroscopy, /sup 1/H-NMR spectroscopy, magnetic moments, and electronic spectral measurements. These compounds (L/sub 1/-L/sub 6/) and their metal (II) complexes were also screened for their antibacterial activity against bacterial species, Bacillus subtilis, Staphylococcus aureus, Escherichia coli, Shigella sonnei, Salmonella typhi and Pseudomonas aeroginosa. Some compounds showed potential activity against a number of bacterial strains. The results of these studies also show the metal (II) complexes to be having stronger antibacterial activityl against one or more species as compared to the uncomplexed ligands. It was concluded that these compounds may be the potential source of active antibacterial agents. (author)

  10. Synthesis, physico-chemical characterization and biological activity of 2-aminobenzimidazole complexes with different metal ions

    Directory of Open Access Journals (Sweden)

    Podunavac-Kuzmanović Sanja O.

    2004-01-01

    Full Text Available Complexes of 2-aminobenzimidazole (L with nitrates of cobalt(II nickel(II, copper (II, zinc(II and silver(I were synthesized. The molar ratio metal:ligand in the reaction of the complex formation was 1:2. It should be noticed, that the reaction of all the metal salts yielded bis(ligand complexes of the general formula M(L2(NO32 × nH2O (M=Co, Ni Cu, Zn or Ag; n=0, 1, 2 or 6. The complexes were characterized by elemental analysis of the metal, molar conductivity, magnetic susceptibility measurements and IR spectra. Co(II, Ni(II and Cu(II complexes behave as non-electrolytes, whilst Zn(II and Ag(I are 1:1 electrolytes. Cu(II complex has a square-planar stereochemistry, Ag(I complex is linear, whilst the Co(II, Ni(II and Zn(II complexes have a tetrahedral configuration. In all the complexes ligand is coordinated by participation of the pyridine nitrogen of the benzimidazole ring. The antimicrobial activity of the ligand and its complexes against Pseudomonas aeruginosa, Bacillus sp. Staphylococcus aureus and Saccharomyces cerevisiae was investigated. The effect of metal on the ligand antimicrobial activity is discussed.

  11. Physico - chemical investigation on Co(II), Ni(II), Cu(II), Zn(II), Cd(II), UO2+2 and VO+2 ions-O-(-N-3,5-dichloro-α-pyridone imino)

    International Nuclear Information System (INIS)

    Mathur, Praveen; Trivedi, Pradeep; Mehta, R.K.

    1983-01-01

    Studies on the interaction of newly synthesised ligand, O-(N-3, 5-dichloro-α-pyridone imino) benzene sulphonic acid (H 2 PB) with Co(II), Ni(II), Cu(II), Zn(II), Cd(II), UO 2 +2 and VO +2 have been carried out potentiometrically. Many physico-chemical studies on thermodynamics, elemental analysis, molecular weight, magnetic moment, conductance, electronic and IR spectra have also been made on the solid chelates and their adducts. The dissociation constants of H 2 PB and stabilities of its bivalent chelates have been evaluated potentiometrically at 25deg, 35deg and 45degC in aqueous medium (0.01M, 0.05M and 0.1M NaClO 4 ) by Bjerrum's method. The stability sequence is in agreement with the Irving-William's rule. (author)

  12. Preparation of Schiff s base complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II) and their spectroscopic, magnetic, thermal, and antifungal studies

    International Nuclear Information System (INIS)

    Parekh, H.M.; Patel, M.N.

    2006-01-01

    The potassium salt of salicylidene-DL-alanine (KHL), bis(benzylidene)ethylenediamine (A 1 ), thiophene-o-carboxaldene-p-toluidine (A 2 ), and its metal complexes of the formula [(M II (L)(A)(H 2 O)] (M=Mn(II), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II); A = A 1 or A 2 ) are prepared. They are characterized by elemental analysis, magnetic susceptibility measurements, thermogravimetric analysis, and infrared and electronic spectral studies. The electronic spectral and magnetic moment data suggest an octahedral geometry for the complexes. All of these complexes, metal nitrates, fungicides (bavistin and emcarb), and ligands are screened for their antifungal activity against Aspergillus niger, Fusarium oxysporum, and Aspergillus flavus using a plate poison technique. The complexes show higher activity than those of the free ligands, metal nitrate, and the control (DMSO) and moderate activity against bavistin and emcarb [ru

  13. Chemical speciation of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II binary complexes of l-methionine in 1,2-propanediol-water mixtures

    Directory of Open Access Journals (Sweden)

    M. Padma Latha

    2007-04-01

    Full Text Available Chemical speciation of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II complexes of L-methionine in 0.0-60 % v/v 1,2-propanediol-water mixtures maintaining an ionic strength of 0.16 M at 303 K has been studied pH metrically. The active forms of ligand are LH2+, LH and L-. The predominant species detected are ML, MLH, ML2, ML2H, ML2H2 and MLOH. Models containing different numbers of species were refined by using the computer program MINIQUAD 75. The best-fit chemical models were arrived at based on statistical parameters. The trend in variation of complex stability constants with change in the dielectric constant of the medium is explained on the basis of electrostatic and non-electrostatic forces.

  14. Syntheses, spectroscopic and thermal analyses of cyanide bridged heteronuclear polymeric complexes: [M(L)2Ni(CN)4]n (Ldbnd N-methylethylenediamine or N-ethylethylenediamine; Mdbnd Ni(II), Cu(II), Zn(II) or Cd(II))

    Science.gov (United States)

    Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla

    2016-02-01

    Polymeric tetracyanonickelate(II) complexes of the type [M(L)2Ni(CN)4]n (Ldbnd N-methylethylenediamine (men) or N-ethylethylenediamine (neen); Mdbnd Ni(II), Cu(II), Zn(II) or Cd(II)) have been prepared and characterized by FT-IR, Raman spectroscopy, thermal and elemental analysis techniques. Additionally, FT-IR and Raman spectral analyses of men and neen have experimentally and theoretically investigated in the range of 4000-250 cm-1. The corresponding vibration assignments of men and neen are performed by using B3LYP density functional theory (DFT) method together with 6-31 G(d) basis set. The spectral features of the complexes suggest that the coordination environment of the M(II) ions are surrounded by the two symmetry related men and neen ligands and the two symmetry related N atom of cyanide groups, whereas the Ni(II) atoms are coordinated with a square-planar to four C atoms of the cyanide groups. Polymeric structures of the complexes consist of one dimensional alternative chains of [M(L)2]2+ and [Ni(CN)4]2- moieties. The thermal decompositions in the temperature range 30-700 °C of the complexes were investigated in the static air atmosphere.

  15. The n-propyl 3-azido-2,3-dideoxy-β-D-arabino-hexopyranoside: Syntheses, crystal structure, physical properties and stability constants of their complexes with Cu(II), Ni(II) and VO(II)

    Science.gov (United States)

    Barabaś, Anna; Madura, Izabela D.; Marek, Paulina H.; Dąbrowska, Aleksandra M.

    2017-11-01

    The structure, conformation and configuration of the n-propyl 3-azido-2,3-dideoxy-β-D-arabino-hexopyranoside (BAra-nPr) were determined by 1H NMR, 13C NMR, and IR spectroscopy, as well as by optical rotation. The crystal structure was confirmed by single-crystal X-ray diffraction studies at room temperature. The compound crystallizes in P21 space group symmetry of the monoclinic system. The molecule has a 4C1 chair conformation with azide group in the equatorial position both in a solution as well as in the crystal. The spatial arrangement of azide group is compared to other previously determined azidosugars. The hydrogen bonds between the hydroxyl group of sugar molecules lead to a ribbon structure observed also for the ethyl homolog. The packing of ribbons is dependent on the alkyl substituent length and with the elongation changes from pseudohexagonal to lamellar. Acidity constants for the n-propyl 3-azido-2,3-dideoxy-β-D-arabino-hexopyranoside (BAra-nPr) in an aqueous solution were evaluated by the spectrophotometric and potentiometric titrations methods. Title compound exhibit blue absorption with the maximum wavelengths in the range of 266 nm and 306 nm. Based on these measurements we showed equilibria existing in a particular solution and a distribution of species which have formed during the titration. We also investigated interactions between Cu(II), Ni(II) and VO(II) and title compound (as ligand L) during complexometric titration. On these bases we identified that in [CuII-BAra-nPr]2+ the ratio of the ligand L to metal ion M(II) was 3:1, while in [NiII-BAra-nPr]2+ and [VOII-BAra-nPr]2+ complexes 2:1 ratios were found. The cumulative stability constants (as log β) occurring in an aqueous solution for the complexes of BAra-nPr with Cu(II), Ni(II) and VO(IV) were 14.57; 11.71 and 4.20, respectively.

  16. The synthesis and characterization of 1,2-dihydroxyimino-3,6-di-aza-8,9-O-iso-butylidene nonane and its complexes with Ni(II), Cu(II), Zn(II) and Cd(II)

    International Nuclear Information System (INIS)

    Canpolat, E.; Kaya, M.; Gorgulu, A.O.

    2002-01-01

    1,2-dihydroxyimino-3,6-di-aza-8,9-O-iso-butylidene nonane (H 2 L) was synthesized starting from 1,2-O-iso-butylidene-4-aza-6-amino hexane (RNH 2 ) and antichloroglyoxime. Ni(II) and Cu(II) complexes of H 2 L have a metal:ligand ratio 1:2 and the ligand coordinates through two N atoms, as do most of the vic-dioximes. However, Zn(II) and Cd(II) complexes of H 2 L have a metal: ligand ratio 1:1 and one chloride ion and one water molecule are also coordinated to the metal ion. Structures of the ligand and its transition-metal complexes are proposed, according to elemental analysis, IR, 13 C and 1 H NMR spectra, magnetic susceptibility measurements and thermogravimetric analyses (TGA). (author)

  17. Synthesis, Characterization, and Biological Activity of Mn(II, Fe(II, Co(II, Ni(II, Cu(II, Zn(II, and Cd(II Complexes of N-Thiophenoyl-N′-Phenylthiocarbohydrazide

    Directory of Open Access Journals (Sweden)

    M. Yadav

    2013-01-01

    Full Text Available Mn(II, Fe(II, Co(II, Ni(II, Cu(II, Zn(II, and Cd(II complex of N-thiophenoyl -N′-phenylthiocarbohydrazide (H2 TPTH have been synthesized and characterized by elemental analysis, magnetic susceptibility measurements, infrared, NMR, electronic, and ESR spectral studies. The complexes were found to have compositions [Mn(H TPTH2], [Co(TPTH (H2O2], [Ni(TPTH (H2O2], [Cu(TPTH], [Zn(H TPTH], [Cd(H TPTH2], and [Fe(H TPTH2(EtOH]. The magnetic and electronic spectral studies suggest square planar geometry for [Cu(TPTH], tetrahedral geometry for [Zn(TPTH] and [Cd(H TPTH2], and octahedral geometry for rest of the complexes. The infrared spectral studies of the 1 : 1 deprotonated complexes suggest bonding through enolic oxygen, thiolato sulfur, and both the hydrazinic nitrogens. Thus, H2TPTH acts as a binegative tetradentate ligand. H2 TPTH and its metal complexes have been screened against several bacteria and fungi.

  18. Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Duran, Celal [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Gundogdu, Ali [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Giresun Faculty of Art and Science, Karadeniz Technical University, 28049 Giresun (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Art and Science, Erciyes University, 38039 Kayseri (Turkey)]. E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Art and Science, Pamukkale University, 20020 Denizli (Turkey); Sentuerk, Hasan Basri [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Tuefekci, Mehmet [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2007-07-19

    A new method using a column packed with Amberlite XAD-2010 resin as a solid-phase extractant has been developed for the multi-element preconcentration of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), and Pb(II) ions based on their complex formation with the sodium diethyldithiocarbamate (Na-DDTC) prior to flame atomic absorption spectrometric (FAAS) determinations. Metal complexes sorbed on the resin were eluted by 1 mol L{sup -1} HNO{sub 3} in acetone. Effects of the analytical conditions over the preconcentration yields of the metal ions, such as pH, quantity of Na-DDTC, eluent type, sample volume and flow rate, foreign ions etc. have been investigated. The limits of detection (LOD) of the analytes were found in the range 0.08-0.26 {mu}g L{sup -1}. The method was validated by analyzing three certified reference materials. The method has been applied for the determination of trace elements in some environmental samples.

  19. Thermal, spectral, magnetic and biological studies of thiosemicarbazones complexes with metal ions: Cu(II), Co(II), Ni(II), Fe(III), Zn(II), Mn(II) and UO2(VI)

    International Nuclear Information System (INIS)

    Mashaly, M.M.; Seleem, H.S.; El-Behairy, M.A.; Habib, H.A.

    2004-01-01

    Thiosemicarbazones ligands, isatin-3-thiosemicarbazone(HIT) and N-acetylisatin-3-thiosemicarbazone (HAIT), which have tridentate ONN coordinating sites were prepared. The complexes of both ligands with Cu(II), Co(II), Ni(II), Fe(III), Zn(II), Mn(II) and UO 2 (VI) ions were isolated. The ligands and their metal complexes were characterized by elemental analysis, IR, UV-Vis and mass spectra, also by conductance, magnetic moment and TG-DSC measurements. All the transition metal complexes have octahedral configurations, except Cu-complexes which have planar geometry and the UO 2 (VI) complexes which have coordination number 8 and may acquire the distorted dodecahedral geometry. Thermal studies explored the possibility of obtaining new complexes. Inversion from octahedral to square-planar configuration occurred upon heating the parent Ni-HIAT complex to form the corresponding pyrolytic product. The antifungal activity against the tested organisms showed that some metal complexes enhanced the activity with respect to the parent ligands. (author)

  20. DFT investigation of Ni(II) adsorption onto MA-DTPA/PVDF chelating membrane in the presence of coexistent cations and organic acids.

    Science.gov (United States)

    Song, Laizhou; Zhao, Xiaodan; Fu, Jie; Wang, Xiuli; Sheng, Yiping; Liu, Xiaowei

    2012-01-15

    Melamine-diethylenetriaminepentaacetic acid/polyvinylidene fluoride (MA-DTPA/PVDF) chelating membrane bearing polyaminecarboxylate groups was used to remove Ni(II) from nickel plating effluents. Adsorption experiments were conducted to study the adsorption of the membrane towards Ni(II) in Ni(II)-Ca(II), Ni(II)-NH(4)(+), Ni(II)-Fe(III) binary systems, and Ni(II)-lactic acid, Ni(II)-succinic acid and Ni(II)-citric acid complex systems. For the ternary nickel plating processes, the effects of 3d transition metals including Fe(II), Co(II), Cu(II) and Zn(II) on Ni(II) adsorption were evaluated. The influences of the aforementioned coexistent cations and organic acids were elucidated by the continuum solvation model (COSMO)-corrected density functional theory (DFT) method. Geometries and complexation energies were analyzed for metal-MA-DTPA and Ni(II)-organic acid complexes. DFT results accord with the experimental data, indicating that DFT is helpful to evaluate the complexation between the membrane and metal cations. The coexistent Ca(II) tends to form more stable complex with MA-DTPA ligand than NH(4)(+) and Fe(III), and can interfere with the formation of Ni(II)-MA-DTPA complex. The complexing sequence of 3d metals with MA-DTPA ligand is Zn(II)Cu(II) have the considerable competition with Ni(II). The stabilities of Ni(II)-organic acid complexes follow the order of lactic acid

  1. Synthesis, crystal structure, antibacterial activity and theoretical studies on a novel mononuclear cobalt(II) complex based on 2,4,6-tris(2-pyridyl)-1,3,5-triazine ligand

    Science.gov (United States)

    Maghami, Mahboobeh; Farzaneh, Faezeh; Simpson, Jim; Ghiasi, Mina; Azarkish, Mohammad

    2015-08-01

    A cobalt complex was prepared from CoCl2·6H2O and 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tptz) in methanol and designated as [Co(tptz)(CH3OH)Cl2]·CH3OH·0.5H2O (1). It was characterized by several techniques including TGA analysis and FT-IR, UV-Vis and 1H NMR spectral studies. The crystal structure of 1 was determined by single-crystal X-ray diffraction. The Co(II) metal center in 1 is six coordinated with a distorted octahedral geometry. The tptz ligand is tridentate and coordinates to the cobalt through coplanar nitrogen atoms from the triazine and two pyridyl rings. Two chloride anions and a methanol molecule complete the inner coordination sphere of the metal ion. The optimized geometrical parameters obtained by DFT calculation are in good agreement with single XRD data. The in vitro antibacterial activity of various tptz complexes of Co(II), Ni(II), Cu(II), Mn(II) and Rh(III) were evaluated against Gram-positive (Bacillus subtilis, Staphylococcus aureus and Gram-negative (Escherichia coli and Pseudomonas aeruginosa) bacteria. Whereas all complexes exhibited good activity in comparison to standard antibacterial drugs, the inhibitory effects of complexes were found to be more than that of the parent ligand. Overall, the obtained results strongly suggest that the cobalt(II) complex is a suitable candidate for counteracting antibiotic resistant microorganisms.

  2. DNA incision evaluation, binding investigation and biocidal screening of Cu(II), Ni(II) and Co(II) complexes with isoxazole Schiff bases.

    Science.gov (United States)

    Ganji, Nirmala; Chityala, Vijay Kumar; Marri, Pradeep Kumar; Aveli, Rambabu; Narendrula, Vamsikrishna; Daravath, Sreenu; Shivaraj

    2017-10-01

    Two new series of binary metal complexes [M(L 1 ) 2 ] and [M(L 2 ) 2 ] where, M=Cu(II), Ni(II) & Co(II) and L 1 =4-((3,4-dimethylisoxazol-5-ylimino)methyl)benzene-1,3-diol; L 2 =2-((3,4-dimethylisoxazol-5-ylimino)methyl)-5-methoxyphenol were synthesized and characterized by elemental analysis, 1 H NMR, 13 C NMR, FT-IR, ESI mass, UV-Visible, magnetic moment, ESR, SEM and powder XRD studies. Based on these results, a square planar geometry is assigned for all the metal complexes where the Schiff base acts as uninegatively charged bidentate chelating agent via the hydroxyl oxygen and azomethine nitrogen atoms. DNA binding studies of all the complexes with calf thymus DNA have been comprehensively investigated using electronic absorption spectroscopy, fluorescence quenching and viscosity studies. The oxidative and photo cleavage affinity of metal complexes towards supercoiled pBR322 DNA has been ascertained by agarose gel electrophoresis assay. From the results, it is observed that all the metal complexes bind effectively to CT-DNA via an intercalative mode of binding and also cleave pBR322 DNA in a promising manner. Further the Cu(II) complexes have shown better binding and cleavage properties towards DNA. The antimicrobial activities of the Schiff bases and their metal complexes were studied on bacterial and fungal strains and the results denoted that the complexes are more potent than their Schiff base ligands. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Structural and antimicrobial studies of coordination compounds of VO(II, Co(II, Ni(II and Cu(II with some Schiff bases involving 2-amino-4-chlorophenol

    Directory of Open Access Journals (Sweden)

    A. P. MISHRA

    2009-05-01

    Full Text Available Complexes of tailor-made ligands with life essential metal ions may be an emerging area to answer the problem of multi-drug resistance (MDR. The coordination complexes of VO(II, Co(II, Ni(II and Cu(II with the Schiff bases derived from 2-hydroxyacetophenone/2-chlorobenzaldehyde with 2-ami¬no-4-chlorophenol were synthesized and characterized by elemental analysis, molar conductance, electronic spectra, FT-IR, ESR, FAB mass, thermal and magnetic susceptibility measurements. The FAB mass and thermal data show degradation of the complexes. The ligand A (2-hydroxyacetophenone-2amino-4-chlorophenol behaved as tridentate and ligand B (2-chlorobenzylidene-2-amino-4-chlorophenol as bidentate, coordinating through O and N donors. The complexes [VO(A(H2O]×xH2O, [M(A(H2On]×xH2O for Co and Ni, [Cu(A(H2O] and [VO(B2]×xH2O, [M(B2(H2On] for Co and Cu and [Ni(B2] exhibited coordination numbers 4, 5 or 6. X-ray powder diffraction data (a = 11.00417 Å, b = 11.706081 Å and c = 54.46780 Å showed that [Cu(CACP2(H2O2], complex 8, crystallized in the orthorhombic system. The in vitro biological screening effects of the investigated compounds were tested against the bacteria Escherichia coli, Staphylococcus aureus and Streptococcus fecalis and the fungi Aspergillus niger, Trichoderma polysporum and Candida albicans by the serial dilution method. A comparative study of the MIC values of the Schiff base and their [M(B2(H2O2] complexes (Co(II, complex 6 and Cu(II, complex 8, indicated that the metal complexes exhibited a higher or lower antimicrobial activity than 2-chlorobenzylidene-2-amino-4-chlorophenol as the free ligand (B.

  4. Computer augumented modelling studies of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II complexes of L-glutamic acid in 1,2-propanediol–water mixtures

    Directory of Open Access Journals (Sweden)

    MAHESWARA RAO VEGI

    2008-12-01

    Full Text Available Chemical speciation of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II complexes of L-glutamic acid was studied at 303 K in 0–60 vol. % 1,2-propanediol–water mixtures, whereby the ionic strength was maintained at 0.16 mol dm-3. The active forms of the ligand are LH3+, LH2 and LH–. The predominant detected species were ML, ML2, MLH, ML2H and ML2H2. The trend of the variation in the stability constants with changing dielectric constant of the medium is explained based on the cation stabilizing nature of the co-solvents, specific solvent–water interactions, charge dispersion and specific interactions of the co-solvent with the solute. The effect of systematic errors in the concentrations of the substances on the stability constants is in the order alkali > > acid > ligand > metal. The bioavailability and transportation of metals are explained based on distribution diagrams and stability constants.

  5. Determination of kinetic and equilibrium parameters of the batch adsorption of Mn(II), Co(II), Ni(II) and Cu(II) from aqueous solution by black carrot (Daucus carota L.) residues

    International Nuclear Information System (INIS)

    Guezel, Fuat; Yakut, Hakan; Topal, Giray

    2008-01-01

    In this study, the effect of temperature on the adsorption of Mn(II), Ni(II), Co(II) and Cu(II) from aqueous solution by modified carrot residues (MCR) was investigated. The equilibrium contact times of adsorption process for each heavy metals-MCR systems were determined. Kinetic data obtained for each heavy metal by MCR at different temperatures were applied to the Lagergren equation, and adsorption rate constants (k ads ) at these temperatures were determined. These rate constants related to the adsorption of heavy metal by MCR were applied to the Arrhenius equation, and activation energies (E a ) were determined. In addition, the isotherms for adsorption of each heavy metal by MCR at different temperatures were also determined. These isothermal data were applied to linear forms of isotherm equations that they fit the Langmuir adsorption isotherm, and the Langmuir constants (q m and b) were calculated. b constants determined at different temperatures were applied to thermodynamic equations, and thermodynamic parameters such as enthalpy (ΔH), free energy (ΔG), and entropy (ΔS) were calculated and these values show that adsorption of heavy metal on MCR was an endothermic process and process of adsorption was favoured at high temperatures

  6. Crystal structure, DNA binding, cleavage, antioxidant and antibacterial studies of Cu(II), Ni(II) and Co(III) complexes with 2-((furan-2-yl)methylimino)methyl)-6-ethoxyphenol Schiff base

    Science.gov (United States)

    Venkateswarlu, Kadtala; Kumar, Marri Pradeep; Rambabu, Aveli; Vamsikrishna, Narendrula; Daravath, Sreenu; Rangan, Krishnan; Shivaraj

    2018-05-01

    Three novel binary metal complexes; 1 [Cu(L)2], 2 [Ni(L)2] and 3 [Co(L)3] where, L (2-(((furan-2-yl) methylimino)methyl)-6-ethoxyphenol, C14H15NO3), were synthesized and characterized by various spectral techniques. Based on spectral studies square planar geometry is assigned for Cu(II) and Ni(II) complexes, whereas Co(III) owned octahedral geometry. Ligand, [Cu(L)2] and [Ni(L)2] are crystallized and found to be monoclinic crystal systems. CT-DNA absorption binding studies revealed that the complexes show good binding propensity (Kb = 5.02 × 103 M-1, 2.77 × 103 M-1, 1.63 × 104 M-1 for 1, 2 and 3 respectively). The role of these complexes in the oxidative and photolytic cleavage of supercoiled pBR322 DNA was studied and found that the complexes cleave the pBR322 DNA effectively. The catalytic ability of 1, 2 and 3 follows the order: 3 > 1 >2. Antioxidant studies of the new complexes revealed that they exhibit significant antioxidant activity against DPPH radical. The Schiff base and its metal complexes have been screened for antibacterial studies by Minimum Inhibitory Concentration method. It is observed that all metal complexes showed more activity than free ligand.

  7. Indolenine meso-substituted dibenzotetraaza[14]annulene and its coordination chemistry toward the transition metal ions Mn(III), Fe(III), Co(II), Ni(II), Cu(II), and Pd(II).

    Science.gov (United States)

    Khaledi, Hamid; Olmstead, Marilyn M; Ali, Hapipah Mohd; Thomas, Noel F

    2013-02-18

    A new dibenzotetraaza[14]annulene bearing two 3,3-dimethylindolenine fragments at the meso positions (LH(2)), has been synthesized through a nontemplate method. X-ray crystallography shows that the whole molecule is planar. The basicity of the indolenine ring permits the macrocycle to be protonated external to the core and form LH(4)(2+)·2Cl(-). Yet another structural modification having strong C-H···π interactions was found in the chloroform solvate of LH(2). The latter two modifications are accompanied by a degree of nonplanar distortion. The antiaromatic core of the macrocycle can accommodate a number of metal ions, Mn(III), Fe(III), Co(II), Ni(II) and Cu(II), to form complexes of [Mn(L)Br], [Mn(L)Cl], [Fe(LH(2))Cl(2)](+)·Cl(-), [Co(L)], [Ni(L)], and [Cu(L)]. In addition, the reaction of LH(2) with the larger Pd(II) ion leads to the formation of [Pd(2)(LH(2))(2)(OAc)(4)] wherein the macrocycle acts as a semiflexible ditopic ligand to coordinate pairs of metal ions via its indolenine N atoms into dinuclear metallocycles. The compounds LH(2), [Co(L)], and [Ni(L)] are isostructural and feature close π-stacking as well as linear chain arrangements in the case of the metal complexes. Variable temperature magnetic susceptibility measurements showed thermally induced paramagnetism in [Ni(L)].

  8. Coordination compounds of cobalt(II), nickel(II), copper(II), and zinc(II) with pantothenic acid

    Energy Technology Data Exchange (ETDEWEB)

    Shabilalov, A.A.; Yunuskhodzhaev, A.N.; Khodzhaev, O.F.; Azizov, M.A.

    1986-11-01

    The compounds Ni(PANA - H)/sub 2/ x 4H/sub 2/O (PANA stands for pantothenic acid, and - H indicates a deprotonated ligand), Cu(PANA - H)/sub 2/ x 2H/sub 2/O, Zn(PANA - H)/sub 2/ x H/sub 2/O, Co(PANA - H)Cl x H/sub 2/O, and Ni(PANA - H)Cl x 3H/sub 2/O have been synthesized on the basis of pantothenic acid and Co(II), Ni(II), Cu(II), and Zn(II) salts in aqueous media. The compounds have been identified by elemental and x-ray diffraction analysis. Some physicochemical properties (solubility, melting point, molar conductivity) of the compounds obtained have been studied. The structure of the compounds isolated has been established on the basis of an analysis of their IR, ESR, and electronic spectra, as well as derivatograms.

  9. Synthesis and characterization of chromium(III), manganese(II), iron(III), cobalt(II), nickel(II), copper(II), cadmium(II) and dioxouranium(VI) complexes of 4(2-pyridyl)-1-(2,4-dihydroxybenzaldehyde)-3-thiosemicarbazone

    International Nuclear Information System (INIS)

    Abu El-Reash, G.M.; Ibrahim, M.M.; Kenawy; El-Ayaan, Usama; Khattab, M.A.

    1994-01-01

    A few complexes of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and dioxouranium(VI) with 4(2-pyridyl)-1-(2,4-dihydroxybenzaldehyde)-3-thiosemicarbazone have been synthesised and characterized on the basis of elemental analysis, IR, electronic NMR, and magnetic moment data. An octahedral structure is proposed for the Cr(III), Fe(III), Co(II) and Ni(H 3 PBT) 2 Cl 2 .2H 2 O complexes; a tetrahedral structure for the Mn(II) and Ni 2 (PBT)OAc.H 2 0 complexes and a square planar structure for the Cu(II) complexes. The antimicrobial and antifungal activities of H 3 PBT and of its metal(II) complexes are investigated. The results reveal that H 3 PBT exhibits greater antimicrobial activities than its complexes. (author). 34 refs., 4 figs., 2 tabs

  10. Synthesis and Spectral Investigations of Manganese(II, Cobalt(II, Nickel(II, Copper(II and Zinc(II Complexes of New Polydentate Ligands Containing a 1,8-Naphthyridine Moiety

    Directory of Open Access Journals (Sweden)

    Sunkari Jyothi

    2006-12-01

    Full Text Available 2-(o-Hydroxyphenyl-1,8-naphthyridine (HN, 2-(4-hydroxy-6-methylpyran-2-one-3-yl-1,8-naphthyridine (HMPN and 2-(benzimidazol-2-yl-1,8-naphthyridine(BN react with acetates of Mn(II, Co(II, Ni(II, Cu(II and Zn(II to yield metal ioncomplexes of definite composition. These compounds were characterized by elementalanalyses, molar conductivity, magnetic susceptibility measurements, thermal studies, IR,UV-visible, NMR and mass spectral investigations. The complexes are found to have theformulae [M(HN2(H2O2], [M(HMPN2(H2O2] and [M(BN2(OAc2], respectively.

  11. Synthesis and spectral studies of manganese(II), cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II) and mercury(II) complexes of 4-oxo-4H-1-benzopyran-3-carboxaldehyde hydrazone derivatives

    International Nuclear Information System (INIS)

    Nawar, N.; Khattab, M.A.; Bekheit, M.M.; El-Kaddah, A.H.

    1996-01-01

    A few complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) with 4-oxo-4H-1-benzopyran-3-(carboxaldehyde-4-chlorobenzylhydrazone) (BCBH) and 4-oxo-4H-1-benzopyran-3-(carboxaldehyde-4-methylbenzylhydrazone) (BMBH) have been synthesised and characterized by elemental analysis, molar conductivities, magnetic measurements and infrared (IR) and visible spectral studies. The IR spectra show that BCBH and BMBH behave as bidentate ligands either in the keto or enol form. (author). 24 refs., 2 tabs

  12. The use of a polymer inclusion membrane in a paper-based sensor for the selective determination of Cu(II).

    Science.gov (United States)

    Jayawardane, B Manori; Coo, Lilibeth dlC; Cattrall, Robert W; Kolev, Spas D

    2013-11-25

    A disposable paper-based sensor (PBS) is described for the determination of Cu(II) in natural and waste waters at approximately 2 cents per measurement. The device makes use of a polymer inclusion membrane (PIM) to provide the selectivity for Cu(II). The PIM consists of 40 wt% di(2-ethlyhexyl) phosphoric acid (D2EHPA) as the carrier, 10 wt% dioctyl phthalate (DOP) as a plasticizer, 49.5 wt% poly(vinyl chloride) (PVC) as the base polymer and 0.5 wt% (mm(-1)) 1-(2'-pyridylazo)-2-naphthol (PAN) as the colourimetric reagent. High selectivity under mildly acidic conditions (HCl, pH 2.0) is achieved for Cu(II) in the presence of frequently encountered metal ions in natural and waste waters such as Fe(III), Al(III), Zn(II), Cd(II), Pb(II), Ca(II), Mg(II), and Ni(II). The laminated PBS consists of a PIM sensing disc (2mm in diameter) attached to the centre of a circular hydrophilic zone (7 mm in diameter) pretreated with 0.01 M HCl. This hydrophilic zone separates the sample port (a circular hole in the plastic cover) from the PIM sensing disc. After introducing 19.2 μL of a sample/standard solution to the sample port, Cu(II) diffuses across the hydrophilic zone and is extracted into the PIM disc as the Cu(II)-D2EHPA complex which subsequently reacts with PAN to produce the red-purple coloured Cu(II)-PAN complex. The colour intensity of the PIM disc is measured 15 min after sample/standard introduction by scanning using a flatbed scanner. Under optimal conditions the device is characterized by a limit of detection (LOD) and limit of quantitation (LOQ) of 0.06 and 0.21 mg L(-1) Cu(II), respectively, with two linear ranges together covering the Cu(II) concentration range from 0.1 to 30.0 mg L(-1). The PBS was successfully applied to the determination of Cu(II) in hot tap water and mine tailings water. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Structural and biological evaluation of some metal complexes of vanillin-4N-(2-pyridyl) thiosemicarbazone

    Science.gov (United States)

    Yousef, T. A.; Abu El-Reash, G. M.; Al-Jahdali, M.; El-Rakhawy, El-Bastawesy R.

    2013-12-01

    The synthesis and characterization of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II) and U(VI)O2 complexes of vanillin-4N-(2-pyridyl) thiosemicarbazone (H2PVT) are reported. Theoretical calculations have been performed to obtain IR spectra of ligand and its complexes using AM1, Zindo/1, MM+ and PM3, methods. The Schiff base and its metal complexes have been screened for antibacterial Pseudomonas aeruginosa, Escherichia coli, Bacillus subtilis and Staphylococcus saprophyticus. H2VPT shows no apparent digestion effect on the egg albumin while Mn(II), Hg(II) and Cu(II) complexes exhibited a considerable digestion effect following the order Cu(II) > Mn(II) > Hg(II). Moreover, Ni(II) and Co(II) complexes revealed strong digestion effect. Fe(II), Mn(II), Cu(II), Zn(II) and Ni(II) acted as metal co- SOD enzyme factors, which are located in different compartments of the cell.

  14. Syntheses of polystyrene supported chelating resin containing the Schiff base derived from salicylaldehyde and triethylene tetramine and its copper(II), nickel(II), cobalt(II), iron(III), zinc(II), cadmium(II), molybdenum(VI), zirconium(IV) and uranium(VI) complexes

    International Nuclear Information System (INIS)

    Syamal, A.; Singh, M.M.

    1998-01-01

    A new polymer-anchored chelating ligand has been synthesized by the reaction of chloromethylated polystyrene (containing 0.94 mmol of Cl per gram of resin and 1% cross-linked with divinylbenzene) and the Schiff base derived from salicylaldehyde and triethylenetetramine. A new series of polystyrene supported, Cu(II), Ni(II), Co(II), Fe(III), Zn(II), Cd(II), Zr(IV), dioxomolybdenum (VI) and dioxouranium (VI) complexes of the formulae PS-LCu, PS-LNi, PS-LCo, PS-LFeCl.DMF, PS-LZn, PS-LCd, PS-LZr(OH) 2 . DMF, PS L MoO 2 and PS-LUO 2 (where PS-LH 2 = polymer-anchored Schiff base and DMF dimethyl-formamide) have been synthesized and characterised by elemental analysis, infrared, electronic spectra and magnetic susceptibility measurements. The complexes PS-LCu, PS-LNi and PS-LCo have square planar structure, PS-LFeCl.DMF, PS-LMoO 2 and PS-LUO 2 have octahedral structure, PS L Zn and PS-LCd are tetrahedral and PS-LZr(OH) 2 .DMF is pentagonal bipyramidal. The polymer-anchored Cu(II), Co(II) and Fe(III) complexes are paramagnetic while Ni(II), Zn(II), Cd(II), Zr(IV), dioxomolybdenum(VI) and dioxouranium(VI) complexes are diamagnetic. The negative shift of the v (C=N) (azomethine) and the positive shift of v (C--O)(phenolic) are indicative of ONNO donor behaviour of the polymer-anchored Schiff base. (author)

  15. A spin-frustrated cobalt(II) carbonate pyrochlore network.

    Science.gov (United States)

    Zheng, Yanzhen; Ellern, Arkady; Kögerler, Paul

    2011-11-01

    The crystal structure of the cobalt(II) carbonate-based compound cobalt(II) dicarbonate trisodium chloride, Co(CO(3))(2)Na(3)Cl, grown from a water-ethanol mixture, exhibits a three-dimensional network of corner-sharing {Co(4)(μ(3)-CO(3))(4)} tetrahedral building blocks, in which the Co(II) centres define a pyrochlore lattice and reside in a slightly distorted octahedral Co(O-CO(2))(6) environment. The space outside the hexagonal framework defined by these interlinked groups is occupied by Na(+) and Cl(-) ions. Antiferromagnetic coupling between adjacent Co(II) centres, mediated by carbonate bridges, results in geometric spin frustration which is typical for pyrochlore networks. The Co and Cl atoms reside on the special position 3, one Na atom on position 2 and a carbonate C atom on position 3.

  16. Synthesis and Characterization of the Adducts of Morpholinedithioccarbamate Complexes of Oxovanadium (IV, Nickel(II, and Copper(II with Piperidine and Morpholine

    Directory of Open Access Journals (Sweden)

    Mousami Sharma

    2012-01-01

    Full Text Available A series of 1:1 adducts of bis(morpholinedithiocarbamato complex of VO(IV, 1:1 and 1:2 adducts of bis(morpholinedithiocarbamato complexes of Ni(II and Cu(II with piperidine and morpholine have been synthesized and characterized by elemental analysis, molar conductance, magnetic susceptibility, IR, UV-Vis, and TGA/DTA techniques. Analytical data reveals that VO(IV complex forms only 1:1 adducts with the formula [VO(morphdtc2L].H2O while Ni(II and Cu(II complexes form both 1:1 and 1:2 adducts with 1:1 adducts having general formula Ni(morphdtc2.L and Cu(morphdtc2.L and 1:2 adducts having general formula Ni(morphdtc2.L2 and Cu(morphdtc2.L2 (morphdtc = morpholinedithiocarbamate, L = morpholine and piperidine. Antifungal activity of some complexes has been carried out against the fungal strain Fusarium oxysporium. Thermal studies indicate a continuous weight loss. A square pyramidal geometry has been proposed for the 1:1 adducts of Ni(II and Cu(II complexes while an octahedral geometry has been proposed for the 1:1 adducts of VO(IV and for the 1:2 adducts of Ni(II and Cu(II complexes.

  17. Synthesis and phosphatase activity of a Cobalt(II) phenanthroline ...

    Indian Academy of Sciences (India)

    MAMONI GARAI

    2017-09-19

    Sep 19, 2017 ... Synthesis and phosphatase activity of a Cobalt(II) phenanthroline complex. MAMONI GARAIa ... tion, cobalt complexes have gained importance because of their application as ... 2.3 Physical measurements. Infrared spectrum ...

  18. Synthesis and Characterization of Cu(II), Co(II) and Ni(II) Complexes of Trithiocyanuric Acid: The Structure of {N,N'-Bis(3-Aminopropyl)-1,3-Propanediamine}-(Trithiocyanurato)Nickel(II)

    Czech Academy of Sciences Publication Activity Database

    Kopel, P.; Trávníček, Zdeněk; Kvítek, L.; Černošek, Z.; Wrzeszcz, G.; Marek, J.

    2003-01-01

    Roč. 56, č. 1 (2003), s. 1-11 ISSN 0095-8972 R&D Projects: GA ČR GA203/00/0152; GA AV ČR IBS5038351 Institutional research plan: CEZ:AV0Z5038910 Keywords : Copper(II) * cobalt(II) and nickel(II) complexes * Trithiocyanuric acid Subject RIV: CE - Biochemistry Impact factor: 0.841, year: 2003

  19. Pelletized ponderosa pine bark for adsorption of toxic heavy metals from water

    Directory of Open Access Journals (Sweden)

    Tshabalala, M. A.

    2007-02-01

    Full Text Available Bark flour from ponderosa pine (Pinus ponderosa was consolidated into pellets using citric acid as cross-linking agent. The pellets were evaluated for removal of toxic heavy metals from synthetic aqueous solutions. When soaked in water, pellets did not leach tannins, and they showed high adsorption capacity for Cu(II, Zn(II, Cd(II, and Ni(II under both equilibrium and dynamic adsorption conditions. The experimental data for Cd(II and Zn(II showed a better fit to the Langmuir than to the Freundlich isotherm. The Cu(II data best fit the Freundlich isotherm, and the Ni(II data fitted both Freundlich and Langmuir isotherms equally. According to the Freundlich constant KF, adsorption capacity of pelletized bark for the metal ions in aqueous solution, pH 5.1 ± 0.2, followed the order Cd(II > Cu(II > Zn(II >> Ni(II; according to the Langmuir constant b, adsorption affinity followed the order Cd(II >> Cu(II ≈ Zn(II >> Ni(II. Although data from dynamic column adsorption experiments did not show a good fit to the Thomas kinetic adsorption model, estimates of sorption affinity series of the metal ions on pelletized bark derived from this model were not consistent with the series derived from the Langmuir or Freundlich isotherms and followed the order Cu(II > Zn(II ≈ Cd(II > Ni(II. According to the Thomas kinetic model, the theoretical maximum amounts of metal that can be sorbed on the pelletized bark in a column at influent concentration of ≈10 mg/L and flow rate = 5 mL/min were estimated to be 57, 53, 50, and 27 mg/g for copper, zinc, cadmium, and nickel, respectively. This study demonstrated the potential for converting low-cost bark residues to value-added sorbents using starting materials and chemicals derived from renewable resources. These sorbents can be applied in the removal of toxic heavy metals from waste streams with heavy metal ion concentrations of up to 100 mg/L in the case of Cu(II.

  20. Studies on complexation of a tridentate ONS Schiff base with lighter and heavier metals ions, and investigation into their biological properties

    International Nuclear Information System (INIS)

    Tarafder, M.T.H.; Ali, A.M.; Juan, W.D.; Crouse, K.A.; Silong, S.

    1999-05-01

    Several new complexes of a tridentate ONS Schiff base derived from the condensation of S-benzyldithiocarbazate with salicylaldehyde have been characterised by elemental analyses, molar conductivity measurements, infrared, and electronic spectral studies. The tridentate Schiff base (HONSH) behaves as a dinegatively charged ligand coordinating through the thiolo sulphur, the azomethine nitrogen atom and the hydroxyl oxygen atom. It forms mono-ligand complexes of the general formula, [M(ONS)X], [M = Ni(II), Cu(II), Cr(III), Sb(III), Zn(II), Zr(IV) or U(VI) and X = H 2 O, Cl]. The ligand produced bis-chelated complex with Th(IV) of composition, [Th(ONS) 2 ]. Square-planar structures were proposed for the Ni(II) and Cu(II) complexes. Antimicrobial tests indicated that the Schiff base and five of the metal complexes of Cu(II), Ni(II), U(VI), Zn(II) and Sb(III) were found to be strongly active against bacteria. Ni(II) and Sb(III) complexes were the most effective against Pseudomonas aeruginosa (gram negative) while the Cu(II) complex proved to be the best against Bacillus cereus (gram positive bacteria). Antifungal activities were also noted with the Schiff base and the U(VI) complex. These compounds have shown results against Candida albicans fungi. But none of these compounds were effective against Aspergillus ochraceous fungi. (author)

  1. Facile and green preparation of novel adsorption materials by combining sol-gel with ion imprinting technology for selective removal of Cu(II) ions from aqueous solution

    Science.gov (United States)

    Ren, Zhongqi; Zhu, Xinyan; Du, Jian; Kong, Delong; Wang, Nian; Wang, Zhuo; Wang, Qi; Liu, Wei; Li, Qunsheng; Zhou, Zhiyong

    2018-03-01

    A novel green adsorption polymer was prepared by ion imprinted technology in conjunction with sol-gel process under mild conditions for the selective removal of Cu(II) ions from aqueous solution. Effects of preparation conditions on adsorption performance of prepared polymers were studied. The ion-imprinted polymer was prepared using Cu(II) ion as template, N-[3-(2-aminoethylamino) propyl] trimethoxysilane (AAPTMS) as functional monomer and tetraethyl orthosilicate (TEOS) as cross-linker. Water was used as solvent in the whole preparation process. The imprinted and non-imprinted polymers were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), atomic force microscope (AFM), Brunauer, Emmett and Teller (BET) and zeta potential. Three-dimensional network structure was formed and functional monomer was successfully cross-linked into the network structure of polymers. Effects of adsorption conditions on adsorption performance of prepared polymers were studied too. The pH value is of great influence on adsorption behavior. Adsorption by ion-imprinted polymer was fast (adsorption equilibrium was reached within 60 min). The adsorption capacity of Cu(II) ion-imprinted polymer was always larger than that of non-imprinted polymer. Pseudo-second-order kinetics model and Freundlich isotherm model fitted well with adsorption data. The maximum adsorption capacity of Cu(II) ion-imprinted polymer was 39.82 mg·g-1. However, the preparation conditions used in this work are much milder than those reported in literatures. The Cu(II) ion-imprinted polymer showed high selectivity and relative selectivity coefficients for Pb(II), Ni(II), Cd(II) and Co(II). In addition, the prepared ion-imprinted polymer could be reused several times without significant loss of adsorption capacity.

  2. Synthesis and structural studies of first row transition metal complexes of N-(2-nitro-benzilidine-3-hydrazino quinoxaline-2-one

    Directory of Open Access Journals (Sweden)

    P.V. Anantha Lakshmi

    2008-12-01

    Full Text Available Cr(III, Mn(II, Fe(III, Co(II, Ni(II and Cu(II complexes of N-(2-nitro-benzilidene-3-hydrazino quinoxaline-2-one (NBHQO have been synthesized and characterized by elemental analysis, conductance, thermal, spectral and magnetic data. NBHQO acts as a bidentate ON donor in all the complexes except in Ni(II complex in which it acts as a tridentate ONO donor. Octahedral geometries have been proposed for all the complexes except for Cu(II complex to which the square planar geometry is assigned.

  3. Biosorption of heavy metals using a dead macro fungus schizophyllum commune fries: evaluation of equilibrium and kinetic models

    International Nuclear Information System (INIS)

    Javid, A.; Bajwa, R.; Javid, A.

    2010-01-01

    Biomass of a wood rotting fungus viz., Schizophyllum commune Fries was utilized for the treatment of electroplating wastewater that contained Cu(II), Ni(II), Zn(II) and Cr(VI) ions. Preliminary batch assays were conducted with synthetic pure metal-bearing solutions. Results obtained showed that among various parameters studied, solution pH between a range of 2.0-6.0 induced negligible uptake at pH < 3.5 and exhibited maximum at around 4.5-5.5 for Ni(II), Cu(II) and Zn(II) ions, while for Cr(VI) ion the highest was evidenced at pH 2.0-2.5. The kinetics of all metal ions was fast and biosorption equilibrium was established in 1 hour with appropriateness of pseudo-second-order. A temperature change in the range of 15 - 45 deg. C did not affect the biosorption capacity of the candidate fungus. The biosorption of metal ion increased on elevating initial metal ions concentrations (20-100 mg L/sup -1/) in the medium. The maximum biosorption capacity of fungus biomass was 9.0, 21.27, 4.83, 18.54 mg g/sup -1/ for Ni(II), Cu(II) and Zn(II) and Cr(VI), respectively. The experimental data was best adjusted by Langmuir, Freundlich and modified Langmuir models. Biosorption assays conducted with actual electroplating effluents under pre-optimized conditions revealed efficiency of 72.01, 53.16, 7.08 and 19.87% for Cu(II), Ni(II), Zn(II) and Cr(VI) ions, respectively by candidate biomass. (author)

  4. Determination of cobalt(II) and nickel(II) with isoamylxanthate as a complexing reagent in micellar media

    International Nuclear Information System (INIS)

    Shar, G.A.; Soomro, G.A.

    2008-01-01

    Cobalt(II) and nickel(II) were determined spectrophotometrically using sodium isoamyl xanthate as a complexing reagent in aqueous phase in the presence of anionic surfactant sodium dodecylsulphate (SDS). Beer's law was obeyed for Co(ll) and Ni(ll) over the concentration range 3.0-35 and 2.0-37 micro gmL/sup -1/ respectively. The lambda/sub max/ molar absorptivity and Sandell's sensitivity of Co(ll) and Ni(ll) were 360 nm and 416 nm; is 0.19 and 0.2 (x 10/sup 4/ mol/sup -1/ cm/sup -1/) 31.1 and 29.3 ng cm/sup -2/ respectively. Maximum absorbance at 1:2 (M: L) molar ratio suggested the formation of M(C/sub 6/H/sub 11/ OS/sub 2/)/sub 2/ where M = Co(II) and Ni(II). The complex remained stable for more than 2 h. The optimized reagent concentration 0.5% was used throughout the study. Surfactant concentration of 1.0% SDS caused significant enhancement in absorbance. Maximum absorption was observed at 360 nm and 416 nm for Co and Ni complexes, respectively. The absorption maxima were obtained at optimized pH of 7.0. Validation of method has been made by comparing the results with Atomic Absorption Spectrometry, no significant difference was obtained between the two methods at 95% confidence interval. The method is simple, accurate, economical and has been applied to the determination of cobalt(ll) and nickel(ll) in industrial wastewater, pharmaceutical and edible oil samples. (author)

  5. Synthesis, characterization and biological activity of symmetric dinuclear complexes derived from a novel macrocyclic compartmental ligand

    Energy Technology Data Exchange (ETDEWEB)

    Mruthyunjayaswamy, B.H.M.; Ijare, Omkar B.; Jadegoud, Y. [Gulbarga University (India). Dept. of Chemistry]. E-mail: bhmmswamy53@rediffmail.com

    2005-07-15

    A phenol based novel macrocyclic binucleating compartmental ligand N,N-bis(2,6-diiminomethyl-4-methyl-1-hydroxyphenyl)malonoyldicarboxamide was prepared. The complexes were prepared by template method by reacting 2,6-diformyl-4-methylphenol, malonoyl dihydrazide and the metal chlorides of Cu(II), Ni(II), Co(II), Cd(II), Zn(II) and Hg(II) in methanol to get a series of dinuclear complexes. The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibility data, IR, UV-Vis, ESR, NMR and FAB mass spectral data. The dinuclear nature of the complexes was confirmed on the basis of elemental analyses, magnetic susceptibility, ESR and FAB mass spectral data. The ligand as well as Cu(II), Ni(II), Co(II) and Zn(II) complexes were tested for their antibacterial and antifungal properties against Escherichia coli, Staphyloccocus aureus, Aspergillus niger and Fusarium oxysporum. Magnetic susceptibility measurements of Cu(II), Ni(II) and Co(II) complexes reveal that these complexes exhibit antiferromagnetic coupling behavior due to the presence of two metal ions in close proximity. FAB mass spectrum of the Cu(II) complex gave a clear evidence for the dinuclear nature. The ligand and the complexes were found to be less active against the tested bacteria, but the ligand alone was found active against the fungus Fusarium oxysporum. (author)

  6. Synthesis, characterization and biological activity of symmetric dinuclear complexes derived from a novel macrocyclic compartmental ligand

    International Nuclear Information System (INIS)

    Mruthyunjayaswamy, B.H.M.; Ijare, Omkar B.; Jadegoud, Y.

    2005-01-01

    A phenol based novel macrocyclic binucleating compartmental ligand N,N-bis(2,6-diiminomethyl-4-methyl-1-hydroxyphenyl)malonoyldicarboxamide was prepared. The complexes were prepared by template method by reacting 2,6-diformyl-4-methylphenol, malonoyl dihydrazide and the metal chlorides of Cu(II), Ni(II), Co(II), Cd(II), Zn(II) and Hg(II) in methanol to get a series of dinuclear complexes. The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibility data, IR, UV-Vis, ESR, NMR and FAB mass spectral data. The dinuclear nature of the complexes was confirmed on the basis of elemental analyses, magnetic susceptibility, ESR and FAB mass spectral data. The ligand as well as Cu(II), Ni(II), Co(II) and Zn(II) complexes were tested for their antibacterial and antifungal properties against Escherichia coli, Staphyloccocus aureus, Aspergillus niger and Fusarium oxysporum. Magnetic susceptibility measurements of Cu(II), Ni(II) and Co(II) complexes reveal that these complexes exhibit antiferromagnetic coupling behavior due to the presence of two metal ions in close proximity. FAB mass spectrum of the Cu(II) complex gave a clear evidence for the dinuclear nature. The ligand and the complexes were found to be less active against the tested bacteria, but the ligand alone was found active against the fungus Fusarium oxysporum. (author)

  7. Adsorption study on orange peel: Removal of Ni(II) ions from ...

    African Journals Online (AJOL)

    orange peel was investigated to evaluate the effects of pH, initial nickel ion concentration and adsorbent dose on the removal of Ni(II) systematically. The optimal pH value for Ni(II) adsorption onto the orange peel was found to be 5.0. Greater ...

  8. Biosorption of Cu(II) onto agricultural materials from tropical regions

    KAUST Repository

    Acheampong, Mike A.

    2011-04-26

    Background: In Ghana, the discharge of untreated gold mine wastewater contaminates the aquatic systems with heavy metals such as copper (Cu), threatening ecosystem and human health. The undesirable effects of these pollutants can be avoided by treatment of the mining wastewater prior to discharge. In this work, the sorption properties of agricultural materials, namely coconut shell, coconut husk, sawdust and Moringa oleifera seeds for Cu(II) were investigated. Results: The Freundlich isotherm model described the Cu(II) removal by coconut husk (R2 = 0.999) and sawdust (R2 = 0.993) very well and the Cu(II) removal by Moringa oleifera seeds (R2 = 0.960) well. The model only reasonably described the Cu(II) removal by coconut shell (R2 = 0.932). A maximum Cu(II) uptake of 53.9 mg g-1 was achieved using the coconut shell. The sorption of Cu(II) onto coconut shell followed pseudo-second-order kinetics (R2 = 0.997). FTIR spectroscopy indicated the presence of functional groups in the biosorbents, some of which were involved in the sorption process. SEM-EDX analysis confirmed an exchange of Mg(II) and K(I) for Cu(II) on Moringa oleifera seeds and K(I) for Cu(II) on coconut shell. Conclusion: This study shows that coconut shell can be an important low-cost biosorbent for Cu(II) removal. The results indicate that ion exchange, precipitation and electrostatic forces were involved in the Cu(II) removal by the biosorbents investigated. © 2011 Society of Chemical Industry.

  9. Cu(II) promotes amyloid pore formation

    International Nuclear Information System (INIS)

    Zhang, Hangyu; Rochet, Jean-Christophe; Stanciu, Lia A.

    2015-01-01

    The aggregation of α-synuclein is associated with dopamine neuron death in Parkinson's disease. There is controversy in the field over the question of which species of the aggregates, fibrils or protofibrils, are toxic. Moreover, compelling evidence suggested the exposure to heavy metals to be a risk of PD. Nevertheless, the mechanism of metal ions in promoting PD remains unclear. In this research, we investigated the structural basis of Cu(II) induced aggregation of α-synuclein. Using transmission electron microscopy experiments, Cu(II) was found to promote in vitro aggregation of α-synuclein by facilitating annular protofibril formation rather than fibril formation. Furthermore, neuroprotective baicalein disaggregated annular protofibrils accompanied by considerable decrease of β-sheet content. These results strongly support the hypothesis that annular protofibrils are the toxic species, rather than fibrils, thereby inspiring us to search novel therapeutic strategies for the suppression of the toxic annular protofibril formation. - Highlights: • Cu(II) promoted the annular protofibril formation of α-synuclein in vitro. • Cu(II) postponed the in vitro fibrillization of α-synuclein. • Neuroprotective baicalein disaggregated annular protofibrils

  10. Cu(II) promotes amyloid pore formation

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Hangyu, E-mail: hangyuz@uw.edu [Weldon School of Biomedical Engineering, Purdue University, West Lafayette, IN 47907 (United States); Rochet, Jean-Christophe [Department of Medicinal Chemistry and Molecular Pharmacology, Purdue University, West Lafayette, IN 47907 (United States); Stanciu, Lia A. [Weldon School of Biomedical Engineering, Purdue University, West Lafayette, IN 47907 (United States); School of Materials Engineering, Purdue University, West Lafayette, IN 47907 (United States)

    2015-08-14

    The aggregation of α-synuclein is associated with dopamine neuron death in Parkinson's disease. There is controversy in the field over the question of which species of the aggregates, fibrils or protofibrils, are toxic. Moreover, compelling evidence suggested the exposure to heavy metals to be a risk of PD. Nevertheless, the mechanism of metal ions in promoting PD remains unclear. In this research, we investigated the structural basis of Cu(II) induced aggregation of α-synuclein. Using transmission electron microscopy experiments, Cu(II) was found to promote in vitro aggregation of α-synuclein by facilitating annular protofibril formation rather than fibril formation. Furthermore, neuroprotective baicalein disaggregated annular protofibrils accompanied by considerable decrease of β-sheet content. These results strongly support the hypothesis that annular protofibrils are the toxic species, rather than fibrils, thereby inspiring us to search novel therapeutic strategies for the suppression of the toxic annular protofibril formation. - Highlights: • Cu(II) promoted the annular protofibril formation of α-synuclein in vitro. • Cu(II) postponed the in vitro fibrillization of α-synuclein. • Neuroprotective baicalein disaggregated annular protofibrils.

  11. A tetrahedrally coordinated cobalt(II) aminophosphonate containing one-dimensional channels

    International Nuclear Information System (INIS)

    Gemmill, William R.; Smith, Mark D.; Reisner, Barbara A.

    2005-01-01

    A tetrahedrally coordinated cobalt(II) phosphonate, Co(O 3 PCH 2 CH 2 NH 2 ), has been synthesized using hydrothermal techniques. X-ray diffraction indicates that this material is a three-dimensional open framework with rings aligned along a single axis forming infinite one-dimensional channels. The framework decomposes just above 400 deg. C. Magnetic susceptibility data are consistent with weak antiferromagnetic ordering at low temperatures

  12. Adsorption study on orange peel: Removal of Ni(II) ions from ...

    African Journals Online (AJOL)

    Yomi

    2012-01-16

    Jan 16, 2012 ... The optimal pH value for Ni(II) adsorption onto the orange peel was found to be 5.0. ... Various bio-sorbents have been examined for the removal of diverse type of ... modifications such as alkaline, acid, ethanol and acetone treatment (Pérez et .... To find a suitable pH for the effective adsorption of. Ni(II) ions ...

  13. Biosorption of Cu(II) onto agricultural materials from tropical regions

    KAUST Repository

    Acheampong, Mike A.; Pereira, Joana P.C.; Meulepas, Roel J.W.; Lens, Piet N.L.

    2011-01-01

    model described the Cu(II) removal by coconut husk (R2 = 0.999) and sawdust (R2 = 0.993) very well and the Cu(II) removal by Moringa oleifera seeds (R2 = 0.960) well. The model only reasonably described the Cu(II) removal by coconut shell (R2 = 0.932). A

  14. co-removal with nucleated Cu(II) precipitation in continuous-flow ...

    African Journals Online (AJOL)

    A compact nucleated precipitation technology using two fluidised sand columns in series was developed to pretreat model metal-plating wastewater containing high concentrations of Cu(II) and Cr(VI). Since either Cu(II) precipitation or Cr(VI) co-removal with Cu(II) precipitation was found to be highly pH dependent in batch ...

  15. Ni(II) complexes of dithiophosphonic acids

    Indian Academy of Sciences (India)

    aDepartment of Chemistry, Science and Research Branch, Islamic Azad ... The compounds were characterized by 1H, 13C and 31P NMR, IR spectroscopy and elemental analysis. The ... design and synthesize Ni(II) complexes with new ..... Yield: 86%. ..... 28 65. 18. Greenwood D 1989 Antimicrobial chemotherapy (New.

  16. Synthesis, spectroscopic and DNA binding ability of CoII, NiII, CuII and ZnII complexes of Schiff base ligand (E)-1-(((1H-benzo[d]imidazol-2-yl)methylimino)methyl)naphthalen-2-ol. X-ray crystal structure determination of cobalt (II) complex.

    Science.gov (United States)

    Yarkandi, Naeema H; El-Ghamry, Hoda A; Gaber, Mohamed

    2017-06-01

    A novel Schiff base ligand, (E)-1-(((1H-benzo[d]imidazol-2-yl)methylimino)methyl)naphthalen-2-ol (HL), has been designed and synthesized in addition to its metal chelates [Co(L) 2 ]·l2H 2 O, [Ni(L)Cl·(H 2 O) 2 ].5H 2 O, [Cu(L)Cl] and [Zn(L)(CH 3 COO)]. The structures of the isolated compounds have been confirmed and identified by means of different spectral and physicochemical techniques including CHN analysis, 1 H & 13 C NMR, mass spectral analysis, molar conductivity measurement, UV-Vis, infrared, magnetic moment in addition to TGA technique. The infrared spectral results ascertained that the ligand acts as monobasic tridentate binding to the metal centers via deprotonated hydroxyl oxygen, azomethine and imidazole nitrogen atoms. The UV-Vis, magnetic susceptibility and molar conductivity data implied octahedral geometry for Co(II) & Ni(II) complexes, tetrahedral for Zn(II) complex and square planar for Cu(II) complex. X-ray structural analysis of Co(II) complex 1 has been reported and discussed. Moreover, the type of interaction between the ligand & its complexes towards salmon sperm DNA (SS-DNA) has been examined by the measurement of absorption spectra and viscosity which confirmed that the ligand and its complexes interact with DNA via intercalation interaction as concluded from the values of binding constants (K b ). Copyright © 2017 Elsevier B.V. All rights reserved.

  17. New Cu (II), Co(II) and Ni(II) complexes of chalcone derivatives: Synthesis, X-ray crystal structure, electrochemical properties and DFT computational studies

    Science.gov (United States)

    Tabti, Salima; Djedouani, Amel; Aggoun, Djouhra; Warad, Ismail; Rahmouni, Samra; Romdhane, Samir; Fouzi, Hosni

    2018-03-01

    The reaction of nickel(II), copper(II) and cobalt(II) with 4-hydroxy-3-[(2E)-3-(1H-indol-3-yl)prop-2-enoyl]-6-methyl-2H-pyran-2-one (HL) leads to a series of new complexes: Ni(L)2(NH3), Cu(L)2(DMF)2 and Co(L)2(H2O). The crystal structure of the Cu(L)2(DMF)2 complex have been determined by X-ray diffraction methods. The Cu(II) lying on an inversion centre is coordinated to six oxygen atoms forming an octahedral elongated. Additionally, the electrochemical behavior of the metal complexes were investigated by cyclic voltammetry at a glassy carbon electrode (GC) in CH3CN solutions, showing the quasi-reversible redox process ascribed to the reduction of the MII/MI couples. The X-ray single crystal structure data of the complex was matched excellently with the optimized monomer structure of the desired compound; Hirschfeld surface analysis supported the packed crystal lattice 3D network intermolecular forces. HOMO/LUMO energy level and the global reactivity descriptors quantum parameters are also calculated. The electrophilic and nucleophilic potions in the complex surface are theoretically evaluated by molecular electrostatic potential and Mulliken atomic charges analysis.

  18. Electron spin resonance and electron spin echo modulation studies of Cu(II) ions in the aluminosilicate chabazite: A comparison of Cu(II) cation location and adsorbate interaction with isostructural silicoaluminophosphate-34

    International Nuclear Information System (INIS)

    Zamadics, M.; Kevan, L.

    1992-01-01

    This study focuses on Cu(II) ions exchanged in the aluminosilicate zeolite chabazite. The various Cu(II) species formed after dehydration, rehydration, and exposure to adsorbates are characterized by electron spin resonance and electron spin echo modulation spectroscopies. These results are interpreted in terms of Cu(II) ion location and adsorbate interaction. The results of this study are compared to the results found earlier for SAPO-34, chabazite's structural analog from the silicoaluminophosphate group. In a hydrated sample of chabazite the Cu(II) ions are found to be in a near octahedral environment coordinated to three nonequivalent water molecules and three framework oxygens. The most probable location of the Cu(II) ion in a hydrated sample is above the plane of the six-membered ring slightly displaced into the ellipsoidal cavity. A somewhat similar location and coordination is found for Cu(II) ions in H-SAPO-34. A feature common to both CuH-chabazite and CuH-SAPO-34 is the generation of two distinct Cu(II) species upon dehydration. It is found that Cu(II) cations in chabazite interact with the various adsorbate molecules in a similar manner as Cu(II) cation in H-chabazite and three molecules of ethanol and three propanol molecules. Only the Cu(II) ions located in the hexagonal rings after dehydration were found to complex with ethylene. The differences observed in the interaction of the Cu(II) in with water, propanol, and ehtylene between SAPO-34 and chabazite can be related to the differing cation densities of these two materials. 32 refs., 7 figs., 21 tabs

  19. Synthesis and characterization of transition metal complexes derived from some biologically active furoic acid hydrazones

    Directory of Open Access Journals (Sweden)

    P. Venkateswar Rao

    2007-04-01

    Full Text Available Two new physiologically active ligands, N’-2-[(E-1-hydroxy-4-methyl-2-oxo-2H-8-chromenyl ethylidene-2-furan carbohydrazide (HMCFCH and N’-2-[(Z-1-(4-hydroxy-6-methyl-2-oxo-2H-pyranyl ethylidene]-furan carbohydrazide (HMPFCH and their VO(II, Mn(II, Fe(II, Co(II, Ni(II and Cu(II complexes have been prepared. The ligands and the metal complexes have been characterized by elemental analyses, electrical conductance, magnetic susceptibility measurements, UV-Vis, IR, and ESR spectroscopic data. Basing on the above data, Fe(II and Co(II complexes of HMCFCH and HMPFCH have been assigned a dimeric octahedral geometry. VO(II complexes of HMCFCH and HMPFCH have been assigned sulfate bridged dimeric square pyramidal geometry. Mn(II complex of HMCFCH has been assigned a dimeric octahedral geometry, where as Mn(II complex of HMPFCH has been ascribed to monomeric octahedral geometry. Cu(II and Ni(II complexes of HMCFCH have been ascribed to a polymeric structure. Ni(II complex of HMPFCH has been assigned a dimeric square planar geometry. Cu(II complex of HMPFCH has been proposed an octahedral geometry. The ligands and their metal chelates were screened against S. aureus and P. aeruginosa. The ligands and the metal complexes have been found to be active against these microorganisms. The ligands show more activity than the metal complexes.

  20. Preparation of thiol-functionalized activated carbon from sewage sludge with coal blending for heavy metal removal from contaminated water.

    Science.gov (United States)

    Li, Juan; Xing, Xing; Li, Jiao; Shi, Mei; Lin, Aijun; Xu, Congbin; Zheng, Jianzhong; Li, Ronghua

    2018-03-01

    Sewage sludge produced from wastewater treatment is a pressing environmental issue. Mismanagement of the massive amount of sewage sludge would threat our valuble surface and shallow ground water resources. Use of activated carbon prepared from carbonization of these sludges for heavy metal removal can not only minimize and stabilize these hazardous materials but also realize resources reuse. In this study, thiol-functionalized activated carbon was synthesized from coal-blended sewage sludge, and its capacity was examined for removing Cu(II), Pb(II), Cd(II) and Ni(II) from water. Pyrolysis conditions to prepare activated carbons from the sludge and coal mixture were examined, and the synthesized material was found to achieve the highest BET surface area of 1094 m 2 /g under 500 °C and 30 min. Batch equilibrium tests indicated that the thiol-functionalized activated carbon had a maximum sorption capacity of 238.1, 96.2, 87.7 and 52.4 mg/g for Pb(II), Cd(II), Cu(II) and Ni(II) removal from water, respectively. Findings of this study suggest that thiol-functionalized activated carbon prepared from coal-blended sewage sludge would be a promising sorbent material for heavy metal removal from waters contaminated with Cu(II), Pb(II), Cd(II) and Ni(II). Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Chitosan/sporopollenin microcapsules: preparation, characterisation and application in heavy metal removal.

    Science.gov (United States)

    Sargın, İdris; Arslan, Gulsin

    2015-04-01

    Use of natural polymers as biosorbents for heavy metal removal is advantageous. This paper reports a study aiming to design a novel biosorbent from two biomacromolecules; chitosan, a versatile derivative of chitin, and sporopollenin, a biopolymer with excellent mechanical properties and great resistance to chemical and biological attack. Chitosan/sporopollenin microcapsules were prepared via cross-linking and characterised by employing scanning electron microscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis. Sorption performance of the microcapsules and the plain chitosan beads were tested for Cu(II), Cd(II), Cr(III), Ni(II) and Zn(II) ions at different metal ion concentration, pH, amount of sorbent, temperature and sorption time. The adsorption pattern followed Langmuir isotherm model and the sorption capacity of the chitosan/sporopollenin microcapsules was found to be Cu(II): 1.34, Cd(II): 0.77, Cr(III): 0.99, Ni(II): 0.58 and Zn(II): 0.71 mmol g(-1). Plain chitosan beads showed higher affinity for the ions; Cu(II): 1.46, Cr(III): 1.16 and Ni(II): 0.81 mmol g(-1) but lower for Cd(II): 0.15 and Zn(II): 0.25 mmol g(-1). Sporopollenin enhanced Cd(II) and Zn(II) ions sorption capacity of the chitosan microcapsules. Chitosan/sporopollenin microcapsules can be used in Cd(II) and Zn(II) metal removal. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Reactions of green and black teas with Cu(II).

    Science.gov (United States)

    Goodman, B A; Ferreira Severino, J; Pirker, K F

    2012-04-01

    Electron paramagnetic resonance (EPR) measurements of the products of reactions between Cu(II) and samples of green and black teas showed spectral components from at least six different Cu(II) complexes with both tea types. Several of these complexes were common to both teas in spite of major differences in their polyphenol compositions. The pH range observed for complex formation, and the total signal intensity in the pH range 4-8, were greatly different from those for the reactions of Cu(II) with (-)-epigallocatechin gallate and gallic acid, the main polyphenols responsible for the free radical signals observed during oxidation of these beverages. Components with spectral parameters similar to those of Cu(II) complexes with theanine, the major amino acid in tea, may contribute to two of the spectra recorded under acidic conditions. However, the initial complexes formed at the lowest pH values investigated are still unidentified. EPR spectra with parameters consistent with Cu(II) polyphenol complexes were only observed under alkaline conditions, thus suggesting that components of tea other than polyphenols might be more important in reactions with copper, and possibly other transition metals, in solutions under physiological conditions. This journal is © The Royal Society of Chemistry 2012

  3. Hydrothermal synthesis of silico-manganese nanohybrid for Cu(II) adsorption from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Qiufeng, E-mail: zhuqiufeng@th.btbu.edu.cn; Wang, Liting; An, Zehuan; Ye, Hong; Feng, Xudong

    2016-05-15

    Highlights: • A novel silico-manganese nanohybrid adsorbent (SMNA) was synthesized by a hydrothermal method. • The adsorption capacities of the SMNA for Cu(II) are lower pH dependency. • As-adsorbents are very efficient at low metal concentration and substantial amounts of Cu(II) can be removed from aqueous solution. - Abstract: A novel silico-manganese nanohybrid adsorbent (SMNA) was synthesized by a facile hydrothermal method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption-desorption, Fourier transform infrared spectroscopy (FT-IR) and zeta potential measurement. The adsorption of Cu(II) ions from aqueous solution on the SMNA was investigated with variations in contact time, pH and initial Cu(II) concentration. The results showed that hydrothermal method would generate nanowire/nanorod incomplete crystallite (δ-MnO{sub 2}) adsorbent. The adsorption of Cu(II) onto SMNA increased sharply within 25 min and reached equilibrium gradually. The maximum adsorption capacities of SMNA for Cu(II) were ∼40–88 mg g{sup −1}, which was lower than δ-MnO{sub 2} (92.42 mg g{sup −1}) but had a lower pH dependency. As compared with δ-MnO{sub 2}, higher adsorption capacities of SMNA (7.5–15 wt% of silica doping amount) for Cu(II) could be observed when pH of the aqueous solution was low (<4). The pseudo-second-order model was the best choice to describe the adsorption behavior of Cu(II) onto SMNA, suggesting that the removal of Cu(II) by the as-prepared adsorbents was dominated by migration of Cu(II). The possibility of Cu(II) recovery was also investigated and it revealed that SMNA was a promising recyclable adsorbent for removal of heavy metal ions in water and wastewater treatment.

  4. Spectrophotometric determination of metal complexes of 1-nitroso-2-naphthol in micellar medium

    International Nuclear Information System (INIS)

    Shar, G.A.; Bhanger, M.I.

    2002-01-01

    Spectrophotometric determination of iron(III), nickel(II) and cobalt(II) is carried out with 1-nitroso-2-naphthol as complexing reagent in aqueous phase using non-ionic surfactant Tween 40. This replaces a tedious and time consuming solvent extraction method, because these solvents are costly and also toxic. Beer's law was obeyed, for Fe(III), Ni(II) and Co(II) over the range 0.5 - 4.0, 0.5 - 4.0 and 0.12 - 3.0 micro g ml/sup -1/ with detection limit (2 sigma ) of 3.3, 5.8 and 3.1 ng ml/sup -1/ respectively. The lambda /sub max/ molar absorption, molar absorptivity and Sandell's sensitivity of Fe(III), Ni(II) and Co(II) were (lambda /sub max/ 446 nm), (lambda/sub max/ 483.5 nm) and (lambda/sub max/ 444.5 nm); sigma/sub max/ x 10/sp 4/ mol/sp -1/ cm/sup -1/) is 1.69, 1.0 and 1.86, 3.3, 5.8 and 3.1 ng cm/sup -2/, respectively. The pH at which the complex is formed for Fe(III), Ni(II) and Co(II) is 1, 8 and 5 respectively. The critical micelle concentration (cmc) of 1-nitroso-2-naphthol is 5% solution. The present method is compared with that of atomic absorption spectroscopy and no significant difference is noted between the two methods at 95% confidence level. The method has been applied to the determination of iron(III), nickel(II) and cobalt(II) in pharmaceutical and industrial wastewater samples. (author)

  5. The influence of Fe(II) competition on the sorption and migration of Ni(II) in MX-80 bentonite

    International Nuclear Information System (INIS)

    Pfingsten, Wilfried; Bradbury, Mike; Baeyens, Bart

    2011-01-01

    Highlights: → We model the diffusion of Ni(II) through bentonite using different sorption models. → We examine sorption competition of Fe(II) and Ni(II) at different concentrations. → Ni(II) breakthrough is 15 times earlier with Fe(II) sorption competition. → Ni(II) sorption is non-linear and depends on the Fe(II) concentration levels. → Sorption competition is important and has to be modelled by reactive transport codes. - Abstract: The results from batch sorption experiments on montmorillonite systems have demonstrated that bivalent transition metals compete with one another for sorption sites. For safety analysis studies of high level radioactive waste repositories with compacted bentonite near fields, the importance of competitive sorption on the migration of radionuclides needs to be evaluated. Under reducing conditions, the bentonite porewater chosen has a Fe(II) concentration of ∼5.3 x 10 -5 M through saturation with siderite. The purpose of this paper is to assess the influence of such high Fe(II) concentrations on the transport of Ni(II) through compacted bentonite, Ni(II) was chosen as an example of a bivalent transition metal. The one-dimensional calculations were carried out at different Ni(II) equilibrium concentrations at the boundary (Ni(II) EQBM ) with the reactive transport code MCOTAC incorporating the two site protolysis non electrostatic surface complexation/cation exchange sorption model, MCOTAC-sorb. At a Ni(II) EQBM level of 10 -7 M without Fe(II) competition, the reactive transport calculations using a constant K d approach and the MCOTAC-sorb calculation yielded the same breakthrough curves. At higher Ni(II) EQBM (10 -5 M), the model calculations with MCOTAC-sorb indicated a breakthrough which was shifted to later times by a factor of ∼5 compared with the use of the constant K d approach. When sorption competition was included in the calculations, the magnitude of the influence depended on the sorption characteristics of the

  6. Spectral, magnetic and biological studies of 1,4-dibenzoyl-3 ...

    Indian Academy of Sciences (India)

    Unknown

    MS received 29 January 2001; revised 30 March 2001. Abstract. ... Room temperature ESR spectra of the Mn(II) and Cu(II) complexes yield ... H)Cl] (M = Cu(II), Ni(II) or Zn(II)) and [Mn(DBtsc)Cl2] were prepared by refluxing ... 5.1 In vitro DNA synthesis inhibition assay ..... 3⋅86 (s, 2H) 7⋅86 (t, 2H), 7⋅46 (d, 3H). DBtsc.

  7. Behavior and mechanism of Ni(II) uptake on MnO2 by a combination of macroscopic and EXAFS investigation

    International Nuclear Information System (INIS)

    Guodong Sheng; Jiang Sheng; Shitong Yang; Ju Hu; Xiangke Wang

    2011-01-01

    The effects of pH, ionic strength, competing ions and initial metal concentrations on the uptake behavior and mechanism of radioactive Ni(II) onto MnO 2 was investigated using a combination of classical macroscopic methods and the extended X-ray absorption fine structure (EXAFS) spectroscopy technique. The results indicated that the uptake of Ni(II) on MnO 2 is obviously dependent on pH but independent of ionic strength, which suggested that the uptake of Ni(II) onto MnO 2 is attributed to an inner-sphere surface complex rather than an outer-sphere surface complex. EXAFS analysis shows that the hydrated Ni(II) is adsorbed through six-fold coordination with an average Ni-O interatomic distance of 2.04 ± 0.01 A. It can be inferred from the EXAFS analysis that the inner-sphere surface complex of Ni(II) onto MnO 2 is involved in both edge-sharing and corner-sharing linkages. Both the macroscopic uptake data and the molecular level evidence of Ni(II) surface speciation at the MnO 2 -water interfaces should be factored into better prediction of the bioavailability and mobility of Ni(II) in soil and water environment. (author)

  8. Nanostructured cobalt(II) tetracarboxyphthalocyanine complex supported within the MWCNT frameworks: electron transport and charge storage capabilities

    CSIR Research Space (South Africa)

    Pillay, S

    2015-02-01

    Full Text Available The electrochemical redox properties of a surface-confined thin solid film of nanostructured cobalt(II) tetracarboxyphthalocyanine integrated with multiwalled carbon nanotube (nanoCoTCPc/MWCNT) have been investigated. This novel nanoCoTCPc/MWCNT...

  9. Sorption of Ni(II) on GMZ bentonite: effects of pH, ionic strength, foreign ions, humic acid and temperature.

    Science.gov (United States)

    Yang, Shitong; Li, Jiaxing; Lu, Yi; Chen, Yixue; Wang, Xiangke

    2009-09-01

    Bentonite has been widely studied in nuclear waste management because of its special physicochemical properties. In this work, the sorption of Ni(II) from aqueous solution onto GMZ bentonite as a function of contact time, pH, ionic strength, foreign ions, humic acid (HA) and temperature was investigated under ambient conditions. The results indicated that the pseudo-second-order rate equation simulated the kinetic sorption process well. The sorption of Ni(II) on GMZ bentonite was strongly dependent on pH and on ionic strength. At low pH, the sorption of Ni(II) was dominated by outer-sphere surface complexation and ion exchange with Na(+)/H(+) on GMZ bentonite surfaces, whereas inner-sphere surface complexation was the main sorption mechanism at high pH. A positive effect of HA on Ni(II) sorption was found at pH8. The Langmuir, Freundlich, and D-R models were used to simulate the sorption isotherms of Ni(II) at three different temperatures: 303.15, 318.15 and 333.15K. The thermodynamic parameters (DeltaH(0), DeltaS(0) and DeltaG(0)) of Ni(II) sorption on GMZ bentonite at the three different temperatures were calculated from the temperature-dependent sorption isotherms. The results indicated that the sorption process of Ni(II) on GMZ bentonite was endothermic and spontaneous. Experimental results indicate that GMZ bentonite is a suitable sorbent for pre-concentration and solidification of Ni(II) from large volume solutions.

  10. Sorption of Ni(II) on GMZ bentonite: Effects of pH, ionic strength, foreign ions, humic acid and temperature

    International Nuclear Information System (INIS)

    Yang Shitong; Li Jiaxing; Lu Yi; Chen Yixue; Wang Xiangke

    2009-01-01

    Bentonite has been widely studied in nuclear waste management because of its special physicochemical properties. In this work, the sorption of Ni(II) from aqueous solution onto GMZ bentonite as a function of contact time, pH, ionic strength, foreign ions, humic acid (HA) and temperature was investigated under ambient conditions. The results indicated that the pseudo-second-order rate equation simulated the kinetic sorption process well. The sorption of Ni(II) on GMZ bentonite was strongly dependent on pH and on ionic strength. At low pH, the sorption of Ni(II) was dominated by outer-sphere surface complexation and ion exchange with Na + /H + on GMZ bentonite surfaces, whereas inner-sphere surface complexation was the main sorption mechanism at high pH. A positive effect of HA on Ni(II) sorption was found at pH 8. The Langmuir, Freundlich, and D-R models were used to simulate the sorption isotherms of Ni(II) at three different temperatures: 303.15, 318.15 and 333.15 K. The thermodynamic parameters (ΔH 0 , ΔS 0 and ΔG 0 ) of Ni(II) sorption on GMZ bentonite at the three different temperatures were calculated from the temperature-dependent sorption isotherms. The results indicated that the sorption process of Ni(II) on GMZ bentonite was endothermic and spontaneous. Experimental results indicate that GMZ bentonite is a suitable sorbent for pre-concentration and solidification of Ni(II) from large volume solutions.

  11. Extractive separation of Al(III) and Ni(II) by Di-2-Ethylhexyl phosphoric acid-kerosene system from aqueous fluoride medium

    International Nuclear Information System (INIS)

    Islam, M.F.; Begum, D.A.; Rahman, M.; Rahman, M.S.

    2009-01-01

    In the study of the extractive separation of Al(III) and Ni(II) by di-2-ethylhexyl phosphoric acid D2EHPA-kerosene from aqueous fluoride medium, about 94% Al(III) and 2% Ni(II) were extracted with 0.3 M D2EHPA (pH 2.1 and temperature 30+-1 degree C). Extraction of Ni(II) decreased with increasing extractant concentration. D2EHPA-kerosene-fluoride system showed better extraction of Al(III) with higher extractant concentration and aqueous pH and vice versa for the extraction of Ni(II). The maximum separation factor (beta 1380) was obtained for Al(III) at 20 degree C and decreased to (beta 732) at 60 degree C. The separation of Al(III) from Ni(II) was favoured at normal temperature. Extraction followed the order Al(III), Ni(II). About 99% stripping of Al(III) was attained from the loaded 0.20 M D2EHPA. Much faster extraction of Al(III) compared to Ni(II) and preferential loading were shown by D2EHPA-kerosene in the presence of fluoride ion in the aqueous phase. Separation of Al(III) was the most outstanding from Ni-Al-F-complex solution. (author)

  12. Ni(II immobilization by bio-apatite materials: Appraisal of chemical, thermal and combined treatments

    Directory of Open Access Journals (Sweden)

    Šljivić-Ivanović Marija

    2016-01-01

    Full Text Available Animal bones are natural and rich source of calcium hydroxyapatite (HAP, which was found to be a good sorbent material for heavy metals and radionuclides. Various treatments can reduce the content of bone organic phase and improve sorption properties. In this study, sorption capacities of raw bovine bones (B and samples obtained by chemical treatment with NaOH (BNaOH, by heating at 400 oC (B400 and by combined chemical and thermal treatment (BNaOH+400, were compared, using Ni(II ions as sorbates. Maximum sorption capacities increased in the order BNi(II sorption was found to be complex, with participation of both HAP and organic phase (when present. Sequential extraction analysis was applied for testing the stability of Ni(II ions sorbed by BNaOH+400. Majority of Ni(II was found in residual phase (65% at lower level of sorbent loading, while with the increase of sorbent saturation carbonate fraction became dominant (39 %. According to the results, BNaOH+400 can be utilized in water purification systems. As an apatite based material with low organic content and high efficiency for Ni(II sorption, it is also a good candidate for in-situ soil remediation, particularly at lower contamination levels. [Projekat Ministarstva nauke Republike Srbije, br. III 43009

  13. Solid-phase extraction of cobalt(II) from lithium chloride solutions using a poly(vinyl chloride)-based polymer inclusion membrane with Aliquat 336 as the carrier.

    Science.gov (United States)

    Kagaya, Shigehiro; Cattrall, Robert W; Kolev, Spas D

    2011-01-01

    The extraction of cobalt(II) from solutions containing various concentrations of lithium chloride, hydrochloric acid, and mixtures of lithium chloride plus hydrochloric acid is reported using a poly(vinyl chloride) (PVC)-based polymer inclusion membrane (PIM) containing 40% (w/w) Aliquat 336 as a carrier. The extraction from lithium chloride solutions and mixtures with hydrochloric acid is shown to be more effective than extraction from hydrochloric acid solutions alone. The solution concentrations giving the highest amounts of extraction are 7 mol L(-1) for lithium chloride and 8 mol L(-1) lithium chloride plus 1 mol L(-1) hydrochloric acid for mixed solutions. Cobalt(II) is easily stripped from the membrane using deionized water. The cobalt(II) species extracted into the membrane are CoCl(4)(2-) for lithium chloride solutions and HCoCl(4)(-) for mixed solutions; these form ion-pairs with Aliquat 336. It is also shown that both lithium chloride and hydrochloric acid are extracted by the PIM and suppress the extraction of cobalt(II) by forming ion-pairs in the membrane (i.e. R(3)MeN(+)·HCl(2)(-) for hydrochloric acid and R(3)MeN(+)·LiCl(2)(-) for lithium chloride). 2011 © The Japan Society for Analytical Chemistry

  14. NMR spectroscopic determination of an equilibrium isotope effect on the hydration of cobalt(II)

    International Nuclear Information System (INIS)

    Evilia, R.F.; Saunders, M.

    1985-01-01

    A recently reported NMR method for the measurement of deuterium equilibrium isotope effects is applied to the hydration of the paramagnetic cobalt(II) ion. An isotope effect of about 1.3% is measured. A substantial difference between the intrinsic shift of H 2 O and D 2 O when coordinated to cobalt is also measured

  15. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Cyclodiphosphazanes as synthetic probes: P-C/P-N bond formation from the reaction ... Studies on cluster, salt and molecular complex of zinc-quinolinate ..... lithium iminophosphonamides and homoleptic bis-chelates of Co(II), Ni(II) and Cu(II).

  16. Azadirachta indica leaf powder as a biosorbent for Ni(II) in aqueous medium

    Energy Technology Data Exchange (ETDEWEB)

    Bhattacharyya, Krishna G., E-mail: krishna2604@sify.com [Department of Chemistry, Gauhati University, Guwahati 781014, Assam (India); Sarma, Jyotirekha [Department of Chemistry, Gauhati University, Guwahati 781014, Assam (India); Sarma, Arunima [Department of Chemistry, Morigaon College, Morigaon 782105, Assam (India)

    2009-06-15

    Azadirachta indica leaves are converted to a fine powder for use as a biosorbent for the removal of metal ions in aqueous solution. In this work, the adsorptive interactions between Ni(II) and the powder were studied under a variety of conditions involving variations in pH, Ni(II) concentration, biosorbent amount, interaction time and temperature, all in single batch processes. The experimental data have been interpreted on the basis of existing mathematical models of equilibrium kinetics and thermodynamics. The biosorption of Ni(II) increased in the pH range of 2.0-5.0 with {approx}92.6% adsorption at pH 5.0 for the highest amount of the biosorbent (4 g/L). The biosorption followed second-order kinetics and intra-particle diffusion was likely to have significant influence in controlling the process. The Langmuir monolayer adsorption capacity varied from 2.4 to 9.1 mg/g and the equilibrium coefficient from 1.09 to 2.78 L/g with strong indication that the Ni(II) ions were held on the biosorbent surface by formation of an adsorption complex. The thermodynamic parameters showed the process to be exothermic in nature supported by appropriate ranges of values of enthalpy change, entropy change and Gibbs energy change.

  17. Synthesis and Structural Studies on Transition Metal Complexes Derived from 4-Hydroxy-4-methyl–2-pentanone-1H-benzimidazol-2-yl-hydrazone

    Directory of Open Access Journals (Sweden)

    M. Neelamma

    2011-01-01

    Full Text Available Transition metal complexes of Cr(III, Fe(III, Mn(II, Co(II, Ni(II, Cu(II and Zn(II with a tridentate ligand, 4-hydroxy-4-methyl-2-pentanone-1H-benzimidazole-2yl-hydrazone (H-HPBH derived from the condensation of 2-hydrazinobenzimidazole and diacetone alcohol was synthesized. Characterization has been done on the basis of analytical, conductance, thermal and magnetic data, infrared, 1H NMR, electronic, mass and ESR spectral data. From analytical and thermal data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand. Divalent complexes have the general formula [M(HPBHCl(H2O2] in octahedral geometry, [M(HPBHCl] in tetrahedral and square planar stereochemistries and trivalent complexes [M(HPBHCl2(H2O] in octahedral disposition. Infrared spectral data suggest that the ligand HPBH behaves as a monobasic tridentate ligand with N: N: O donor sequence towards the metal ions. On the basis of the above physicochemical data, octahedral, tetrahedral and square planar geometries were assigned for the complexes. The ligand and metal complexes were screened for their physiological activities against E. coli and S. aureus. The order of physiological activity has been found to be Cu(II > Ni(II > Zn(II > Co(II > Cr(III > Mn(II > Fe (III > ligand against E.coli and Ni(II > Cu(II > Zn(II > Mn(II > Cr(III > Fe(III > Co(II > ligand against S. aureus.

  18. trans-Dichloridotetrakis[1-(2-hydroxyethyl-1H-tetrazole-κN4]cobalt(II

    Directory of Open Access Journals (Sweden)

    Alexander S. Lyakhov

    2009-11-01

    Full Text Available The title cobalt(II complex, [CoCl2(C3H6N4O4], was obtained from metallic cobalt by direct synthesis. There are two Co atoms in the asymmetric unit, each lying on an inversion centre and adopting a distorted octahedral coordination. Classical and non-classical hydrogen bonds are responsible for formation of a three-dimensional polymeric network in the crystal.

  19. Syntheses and Characterization of Some Tetradentate Schiff-Base Complexes and Their Heteroleptic Analogues

    Directory of Open Access Journals (Sweden)

    A. A. Osowole

    2008-01-01

    Full Text Available VO(IV, Ni(II and Cu(II complexes of the asymmetric Schiff base [(HOC6H3(OCH3C(C6H5:N(CH2CH2N:C(CH3CH:C(C6H5OH], and their heteroleptic analogues with triphenyl phosphine and 2,2’-bipyridine have been synthesized and characterized by elemental analyses, conductance, magnetic, infrared and electronic spectral measurements. The ligand is tetradentate coordinating via the imine N and enolic O atoms. The Ni(II and Cu(II complexes adopt a four coordinate square planar geometry, the VO(IV complex is five coordinate square-pyramidal and the heteroleptic complexes are 6-coordinate, octahedral. The assignment of geometry is collaborated by magnetic moments and electronic spectra measurements. The compounds are non-electrolyte in nitromethane and are magnetically dilute.

  20. Site-specific tagging proteins with a rigid, small and stable transition metal chelator, 8-hydroxyquinoline, for paramagnetic NMR analysis

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Yin; Huang, Feng [Nankai University, State Key Laboratory of Elemento-Organic Chemistry, Collaborative Innovation Center of Chemical Science and Engineering (Tianjin) (China); Huber, Thomas [Australian National University, Research School of Chemistry (Australia); Su, Xun-Cheng, E-mail: xunchengsu@nankai.edu.cn [Nankai University, State Key Laboratory of Elemento-Organic Chemistry, Collaborative Innovation Center of Chemical Science and Engineering (Tianjin) (China)

    2016-02-15

    Design of a paramagnetic metal binding motif in a protein is a valuable way for understanding the function, dynamics and interactions of a protein by paramagnetic NMR spectroscopy. Several strategies have been proposed to site-specifically tag proteins with paramagnetic lanthanide ions. Here we report a simple approach of engineering a transition metal binding motif via site-specific labelling of a protein with 2-vinyl-8-hydroxyquinoline (2V-8HQ). The protein-2V-8HQ adduct forms a stable complex with transition metal ions, Mn(II), Co(II), Ni(II), Cu(II) and Zn(II). The paramagnetic effects generated by these transition metal ions were evaluated by NMR spectroscopy. We show that 2V-8HQ is a rigid and stable transition metal binding tag. The coordination of the metal ion can be assisted by protein sidechains. More importantly, tunable paramagnetic tensors are simply obtained in an α-helix that possesses solvent exposed residues in positions i and i + 3, where i is the residue to be mutated to cysteine, i + 3 is Gln or Glu or i − 4 is His. The coordination of a sidechain carboxylate/amide or imidazole to cobalt(II) results in different structural geometries, leading to different paramagnetic tensors as shown by experimental data.

  1. Biosorption of cobalt(II) with sunflower biomass from aqueous solutions in a fixed bed column and neural networks modelling.

    Science.gov (United States)

    Oguz, Ensar; Ersoy, Muhammed

    2014-01-01

    The effects of inlet cobalt(II) concentration (20-60 ppm), feed flow rate (8-19 ml/min) and bed height (5-15 cm), initial solution pH (3-5) and particle size (0.25shells of sunflower biomass was found to be 1.82 m(2)/g. A relationship between the predicted results of the ANN model and experimental data was conducted. The ANN model yielded determination coefficient of (R(2) 0.972), standard deviation ratio (0.166), mean absolute error (0.0158) and root mean square error (0.0141). The results indicated that the shells of the sunflower biomass is a suitable biosorbent for the uptake of cobalt(II) in fixed bed columns. © 2013 Published by Elsevier Inc.

  2. Adsorptive removal of Cu(II) from aqueous solutions using collagen-tannin resin

    Energy Technology Data Exchange (ETDEWEB)

    Sun Xia; Huang Xin [Department of Biomass Chemistry and Engineering, Sichuan University, Chengdu 610065 (China); Liao Xuepin, E-mail: xpliao@scu.edu.cn [Department of Biomass Chemistry and Engineering, Sichuan University, Chengdu 610065 (China); National Engineering Laboratory for Clean Technology of Leather Manufacture, Sichuan University, Chengdu 610065 (China); Shi Bi, E-mail: shibi@scu.edu.cn [National Engineering Laboratory for Clean Technology of Leather Manufacture, Sichuan University, Chengdu 610065 (China)

    2011-02-28

    The collagen-tannin resin (CTR), as a novel adsorbent, was prepared via a reaction of collagen with black wattle tannin and aldehyde, and its adsorption properties to Cu(II) were systematically investigated, including pH effect, adsorption equilibrium, adsorption kinetics, and column adsorption. The adsorption capacity of Cu(II) on CTR was pH-dependent, and it increased with the increase of solution pH. The adsorption isotherms were well described by Langmuir isotherm model with correlating constant (R{sup 2}) higher than 0.99. The adsorption capacity determined at 303 K was high up to 0.26 mmol/g, which was close to the value (0.266 mmol/g) estimated from Langmuir equation. The adsorption capacity was increased with the increase of temperature, and thermodynamic calculations suggested that the adsorption of Cu(II) on CTR is an endothermic process. The adsorption kinetics were well fitted by the pseudo-second-order rate model. Further column studies suggested that CTR was effective for the removal of Cu(II) from solutions, and more than 99% of Cu(II) was desorbed from column using 0.1 mol/L HNO{sub 3} solution. The CTR column can be reused to adsorb Cu(II) without any loss of adsorption capacity.

  3. Removal of copper and nickel from water using nanocomposite of magnetic hydroxyapatite nanorods

    Science.gov (United States)

    Thanh, Dong Nguyen; Novák, Pavel; Vejpravova, Jana; Vu, Hong Nguyen; Lederer, Jaromír; Munshi, Tasnim

    2018-06-01

    A nanocomposite of magnetic hydroxyapatite was synthesized and tested as an adsorbent for the removal of copper (Cu (II)) and nickel (Ni(II)) from aqueous solution. The adsorbent was investigated using Transmission Electron Microscopy (TEM), Scanning Electron Microscopy equipped with an Energy Dispersive Spectrometer (SEM/EDS), X-ray powder diffraction (XRD) and the Brunauer-Elmet-Teller nitrogen adsorption technique (BET-N2 adsorption). Batch experiments were carried out to determine and compare the adsorption parameters of Fe3O4 and its composite with hydroxyapatite. It was found that the adsorbent is nanostructured and has a specific surface area of 101.2 m2 g-1. The Langmuir adsorption isotherm was found to be an appropriate model to describe the adsorption processes, showing the adsorption capacities of Cu(II) and Ni(II) of 48.78 mg g-1 and 29.07 mg g-1, respectively. In addition to the high adsorption capacity, the fully-adsorbed material could be easily separated from aqueous media using an external magnetic field. These results suggested that the utilization of new hydroxyapatite - Fe3O4 nanocomposite for the removal of Cu(II) and Ni(II) is a promising method in water technology.

  4. Synthesis, structure, properties and immobilization on a gold surface of the monoribbed-functionalized tris-dioximate cobalt(II) clathrochelates and an electrocatalytic hydrogen production from H+ ions.

    Science.gov (United States)

    Voloshin, Y Z; Belov, A S; Vologzhanina, A V; Aleksandrov, G G; Dolganov, A V; Novikov, V V; Varzatskii, O A; Bubnov, Y N

    2012-05-28

    The cycloaddition of the mono- and dichloroglyoximes to the cobalt(II) bis-α-benzyldioximate afforded the cobalt(II) mono- and dichloroclathrochelates in moderate yields (40-60%). These complexes undergo nucleophilic substitution of their reactive chlorine atoms with aliphatic amines, alcohols and thiolate anions. In the case of ethylenediamine and 1,2-ethanedithiol, only the macrobicyclic products with α,α'-N(2)- and α,α'-S(2)-alicyclic six-numbered ribbed fragments were obtained. The cobalt(II) cage complexes with terminal mercapto groups were synthesized using aliphatic dithiols. The crystal and molecular structures of the six cobalt(II) clathrochelates were obtained by X-ray diffraction. Their CoN(6)-coordination polyhedra possess a geometry intermediate between a trigonal prism and a trigonal antiprism, and the encapsulated cobalt(II) ions are shifted from their centres due to the structural Jahn-Teller effect with the Co-N distances varying significantly (by 0.10-0.26 Å). The electrochemistry of the complexes obtained was studied by cyclic voltammetry (CV). The anodic waves correspond to the quasi-reversible Co(2+/3+) oxidations, whereas the cathodic ranges contain the quasi-reversibile waves assigned to the Co(2+/+) reductions; all the cobalt(i)-containing clathrochelate anions formed are stable in the CV time scale. The electrocatalytic properties of the cobalt complexes obtained were studied in the production of hydrogen from H(+) ions: the addition of HClO(4) resulted in the formation of the same catalytic cathodic reduction Co(2+/+) waves. The controlled-potential electrolysis with gas chromatography analysis confirmed the production of H(2) in high Faraday yields. The efficiency of this electrocatalytic process was enhanced by an immobilization of the complexes with terminal mercapto groups on a surface of the working gold electrode.

  5. Asymmetric synthesis of α-amino acids via homologation of Ni(II) complexes of glycine Schiff bases; Part 1: alkyl halide alkylations.

    Science.gov (United States)

    Sorochinsky, Alexander E; Aceña, José Luis; Moriwaki, Hiroki; Sato, Tatsunori; Soloshonok, Vadim A

    2013-10-01

    Alkylations of chiral or achiral Ni(II) complexes of glycine Schiff bases constitute a landmark in the development of practical methodology for asymmetric synthesis of α-amino acids. Straightforward, easy preparation as well as high reactivity of these Ni(II) complexes render them ready available and inexpensive glycine equivalents for preparing a wide variety of α-amino acids, in particular on a relatively large scale. In the case of Ni(II) complexes containing benzylproline moiety as a chiral auxiliary, their alkylation proceeds with high thermodynamically controlled diastereoselectivity. Similar type of Ni(II) complexes derived from alanine can also be used for alkylation providing convenient access to quaternary, α,α-disubstituted α-amino acids. Achiral type of Ni(II) complexes can be prepared from picolinic acid or via recently developed modular approach using simple secondary or primary amines. These Ni(II) complexes can be easily mono/bis-alkylated under homogeneous or phase-transfer catalysis conditions. Origin of diastereo-/enantioselectivity in the alkylations reactions, aspects of practicality, generality and limitations of this methodology is critically discussed.

  6. Equilibrium and spectral studies on ligational behaviour of N,N ...

    Indian Academy of Sciences (India)

    Unknown

    The solid complexes of Mn(II), Fe(II), Co(II), Ni(II), Cu(II),. Zn(II) and Pb(II) with DFH have been synthesized, and have been characterized by elemental analysis ... Magnetic susceptibilities of the metal chelates were measured at room ...

  7. KINETIC AND EQUILIBRIUM STUDY FOR THE SORPTION OF Pb(II ...

    African Journals Online (AJOL)

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    passive process for adsorption of the metal ions by metabolically inactive biomass. ..... split in the concentration gradient between solute concentration in the .... binding capacity of Cd(II), Cr(III), Cu(II), Ni(II), Pb(II) and Sn(II) ions increased with ...

  8. Adsorption behavior of multiwall carbon nanotube/iron oxide magnetic composites for Ni(II) and Sr(II)

    International Nuclear Information System (INIS)

    Chen Changlun; Hu Jun; Shao Dadong; Li Jiaxing; Wang Xiangke

    2009-01-01

    Multiwall carbon nanotube (MWCNT)/iron oxide magnetic composites were prepared, and were characterized by scan electron microscopy using a field emission scanning electron microscope, X-ray diffraction and vibrating sample magnetometer. The adsorptions of Ni(II) and Sr(II) onto MWCNT/iron oxide magnetic composites were studied as a function of pH and ionic strength. The results show that the adsorptions of Ni(II) and Sr(II) on the magnetic composites is strongly dependent on pH and ionic strength. The adsorption capacity of the magnetic composites is much higher than that of MWCNTs and iron oxides. The solid magnetic composites can be separated from the solution by a magnetic process. The Langmuir model fits the adsorption isotherm data of Ni(II) better than the Freundlich model. Results of desorption study shows that Ni(II) adsorbed onto the magnetic composites can be easily desorbed at pH < 2.0. MWCNT/iron oxide magnetic composites may be a promising candidate for pre-concentration and solidification of heavy metal ions and radionuclides from large volumes of aqueous solution, as required for remediation purposes.

  9. Photochemical activation and reactivity of polynuclear transition-metal-complex molecules. Progress report, June 1981-May 31, 1982

    International Nuclear Information System (INIS)

    Endicott, J.F.; Lintvedt, R.L.

    1982-01-01

    Significant results obtained during the year are summarized for the following programs: (1) reversible, two electron transfer at a single potential in binuclear complexes; (2) photophysics of polyketonate complexes; (3) synthetic strategies and characterization of heavy metal heterobinuclear complexes; (4) high yield synthesis of ligands capable of binding 3 and 4 metal ions per molecule. Electrochemical studies have uncovered a number of new binuclear metal complexes that undergo reversible two-electron reduction at single potential including Cu(II) complexes with two different coordination environments, mixed Ni(II), Cu(II) complexes and binuclear Ni(II) complexes. In each case the species that exhibit these electron transfer properties have been shown to be Na + ion-paired complexes. Several new trinuclear molecular complexes have been prepared and characterized that contain two UO 2 2+ ions and one transition metal ion. The electrochemistry, absorption spectra, and luminescence have been investigated

  10. Poly (furfural-acetone as New Adsorbent for Removal of Cu(II from Aqueous Solution: Equilibrium Study

    Directory of Open Access Journals (Sweden)

    Tariq S. Najim

    2010-01-01

    Full Text Available The batch removal of Cu(II from aqueous solution using poly (furfural-acetone, (PFA as adsorbent was investigated in this study. The influences of initial Cu(II ion concentration (10 to 120 ppm, pH (4-8 and contact time have been reported. Adsorption of Cu(II is highly pH-dependent and the result indicate that the optimum pH for the removal was found to be 6. At this pH a small amount of PFA, 2 g/L, could remove as much as 97% of Cu(II from a solution of initial concentration 10 ppm. It was observed that an increase in initial concentration of Cu(II leads to decrease in percent removal of Cu(II and increase in amount of Cu(II adsorbed per unit mass of PFA. The adsorption process of Cu(II is tested with four isotherm models, Langmuir, Freundlich, Temkin and Dubinin–Radushkevich (D-R. It was found that all models were applicable and the maximum adsorption capacity was found to be 13.66 mg/g. From the isotherm constants it was confirmed that, the sorption process was physisorption.

  11. Selective peptide bond hydrolysis of cysteine peptides in the presence of Ni(II) ions.

    Science.gov (United States)

    Protas, Anna Maria; Bonna, Arkadiusz; Kopera, Edyta; Bal, Wojciech

    2011-01-01

    Recently, we described a sequence-specific R1-(Ser/Thr) peptide bond hydrolysis reaction in peptides of a general sequence R1-(Ser/Thr)-Xaa-His-Zaa-R, which occurs in the presence of Ni(II) ions [A. Krężel, E. Kopera, A. M. Protas, A. Wysłouch-Cieszyńska, J. Poznański, W. Bal, J. Am. Chem. Soc. 132 (2010) 3355-3366]. In this study we explored the possibility of substituting the Ser/Thr and the His residues, necessary for the reaction to occur according to the Ni(II)-assisted acyl shift reaction mechanism, with Cys residues. We tested this concept by synthesizing three homologous peptides: R1-Ser-Arg-Cys-Trp-R2, R1-Cys-Arg-His-Trp-R2, and R1-Cys-Arg-Cys-Trp-R2, and the R1-Ser-Arg-His-Trp-R2 peptide as comparator (R1 and R2 were CH3CO-Gly-Ala and Lys-Phe-Leu-NH2, respectively). We studied their hydrolysis in the presence of Ni(II) ions, under anaerobic conditions and in the presence of TCEP as a thiol group antioxidant. We measured hydrolysis rates using HPLC and identified products of reaction using electrospray mass spectrometry. Potentiometry and UV-vis spectroscopy were used to assess Ni(II) complexation. We demonstrated that Ni(II) is not compatible with the Cys substitution of the Ser/Thr acyl acceptor residue, but the substitution of the Ni(II) binding His residue with a Cys yields a peptide susceptible to Ni(II)-related hydrolysis. The relatively high activity of the R1-Ser-Arg-Cys-Trp-R2 peptide at pH 7.0 suggests that this peptide and its Cys-containing analogs might be useful in practical applications of Ni(II)-dependent peptide bond hydrolysis. Copyright © 2010 Elsevier Inc. All rights reserved.

  12. Simultaneous decomplexation in blended Cu(II)/Ni(II)-EDTA systems by electro-Fenton process using iron sacrificing electrodes.

    Science.gov (United States)

    Zhao, Zilong; Dong, Wenyi; Wang, Hongjie; Chen, Guanhan; Tang, Junyi; Wu, Yang

    2018-05-15

    This research explored the application of electro-Fenton (E-Fenton) technique for the simultaneous decomplexation in blended Cu(II)/Ni(II)-EDTA systems by using iron sacrificing electrodes. Standard discharge (0.3 mg L -1 for Cu and 0.1 mg L -1 for Ni in China) could be achieved after 30 min reaction under the optimum conditions (i.e. initial solution pH of 2.0, H 2 O 2 dosage of 6 mL L -1  h -1 , current density of 20 mA/cm 2 , inter-electrode distance of 2 cm, and sulfate electrolyte concentration of 2000 mg L -1 ). The distinct differences in apparent kinetic rate constants (k app ) and intermediate removal efficiencies corresponding to mere and blended systems indicated the mutual promotion effect toward the decomplexation between Cu(II) and Ni(II). Massive accumulation of Fe(Ⅲ) favored the further removal of Cu(II) and Ni(II) by metal ion substitution. Species distribution results demonstrated that the decomplexation of metal-EDTA in E-Fenton process was mainly contributed to the combination of various reactions, including Fenton reaction together with the anodic oxidation, electro-coagulation (E-coagulation) and electrodeposition. Unlike hypophosphite and citrate, the presence of chlorine ion displayed favorable effects on the removal efficiencies of Cu(II) and Ni(II) at low dosage, but facilitated the ammonia nitrogen (NH 4 + -N) removal only at high dosage. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Cu(II) AND Zn(II)

    African Journals Online (AJOL)

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    SYNTHESIS OF 2,2-DIMETHYL-4-PHENYL-[1,3]-DIOXOLANE USING ZEOLITE. ENCAPSULATED Co(II), Cu(II) AND Zn(II) COMPLEXES. B.P. Nethravathi1, K. Rama Krishna Reddy2 and K.N. Mahendra1*. 1Department of Chemistry, Bangalore University, Bangalore-560001, India. 2Department of Chemistry, Government ...

  14. Removal of Cu(II) from acidic electroplating effluent by biochars generated from crop straws.

    Science.gov (United States)

    Tong, Xuejiao; Xu, Renkou

    2013-04-01

    The removal efficiency of copper (Cu(II)) from an actual acidic electroplating effluent by biochars generated from canola, rice, soybean and peanut straws was investigated. The biochars simultaneously removed Cu(II) from the effluent, mainly through the mechanisms of adsorption and precipitation, and neutralized its acidity. The removal efficiency of Cu(II) by the biochars followed the order: peanut straw char > soybean straw char > canola straw char > rice straw char > a commercial activated carbonaceous material, which is consistent with the alkalinity of the biochars. The pH of the effluent was a key factor determining the removal efficiency of Cu(II) by biochars. Raising the initial pH of the effluent enhanced the removal of Cu(II) from it. The optimum pyrolysis temperature was 400 degrees C for producing biochar from crop straws for acidic wastewater treatment, and the optimum reaction time was 8 hr.

  15. Investigation of solution chemistry effects on sorption behavior of radionuclide 64Cu(II) on illite

    International Nuclear Information System (INIS)

    Shitong Yang; Guodong Sheng; Zhiqiang Guo; Yubing Sun; Donglin Zhao

    2011-01-01

    In this work, a series of batch experiments were carried out to investigate the effect of various environmental factors such as contact time, pH, ionic strength, coexisting electrolyte ions, humic substances and temperature on the sorption behavior of illite towards 64 Cu(II). The results indicated that 64 Cu(II) sorption on illite achieved equilibrium quickly. The pH- and ionic strength-dependent sorption suggested that 64 Cu(II) sorption on illite was dominated by ion exchange or outer-sphere surface complexation at pH 7. A positive effect of humic substances on 64 Cu(II) sorption was found at pH 6.5. The Langmuir and Freundlich models were used to simulate the sorption isotherms of 64 Cu(II) at three different temperatures of 293, 313, and 333 K. The thermodynamic parameters (ΔH 0 , ΔS 0 , and ΔG 0 ) of 64 Cu(II) sorption on illite were calculated from the temperature dependent sorption isotherms, and the results indicated that the sorption of 64 Cu(II) on illite was endothermic and spontaneous. From the experimental results, it is possible to conclude that illite has good potentialities for cost-effective treatments of 64 Cu(II)-contaminated wastewaters. (author)

  16. Synthesis, NMR characterization, X-ray crystal structure of Co(II) Ni(II) and Cu(II) complexes of a pyridine containing self-assembling

    International Nuclear Information System (INIS)

    Ranjbar, M.; Taghavipour, M.; Moghimi, A.; Aghabozorg, H.

    2002-01-01

    In the recent years, the self-assembling systems have been attracted chemists. The intermolecular bond in such systems mainly consists of ion pairing and hydrogen bonding [1,2]. The reaction between self-assembling system liquid LH 2 (py dc=2,6-pyridinedicarboxylic acid and py da=2,6- pyridine diamin) with cobalt (II) nitrate, nickel (II) chloride, and copper (II) acetate in water leads to the formation of self- assemble coordination complexes, [py da.H] 2 [M(py dc) 2 ]. H 2 O, M=Co(II),Ni(II), and Cu(II). The characterization was performed using elemental analysis, ESI mass spectroscopy, 1 H and 13 C NMR and X-ray crystallography. The crystal systems are monoclinic with space group P2 1 /n and four molecules per unit cell. These complexes shows 13 C NMR resonances of cationic counter ion [(py dc,H)] + in DMSO- d 6 but no signal corresponding to the two coordinated ligands [py dc] 2- The metal atoms are six-coordinated with a distorted octahedral geometry. The two [py de] 2- units are almost perpendicular to each other

  17. Competitive metal sorption and desorption onto Kappaphycus alvarezii, seaweed waste biomass

    International Nuclear Information System (INIS)

    Lee, K.O.; Nazaruddin Ramli; Mamot Said; Musa Ahmad; Suhaimi Mohd Yasir; Arbakariya Ariff

    2011-01-01

    Competitive metal sorption and desorption onto Kappaphycus alvarezii waste biomass were investigated. Metal sorption capacities were 0.82 mg Cr (III)/ g, 0.73 mg Ni (II)/ g, 0.67 mg Cd (II)/ g, 0.65 mg Cu( II)/ g and 0.64 mg Zn (II)/ g in multi metal system. Whereas, desorption efficiencies were 66.08 %, 71.50 % and 80.44 % using 0.1 M HNO 3 , 0.1 M HCl and 0.1 M H 2 SO 4 , respectively. The metal sorption sequence were Cr(III) > Ni(II) > Cd(II) > Cu(II) > Zn(II), while metal desorption sequence were Cd(II) > Zn(II) > Cu(II) > Ni(II) > Cr(III). Fourier transformed infrared spectroscopy (FTIR) technique was used to characterize the seaweed waste biomass. FTIR analysis shown that carbonyl (-C-O) and nitrile (-C≡N) groups interact with the metal ions. The experiments result revealed that Kappaphycus alvarezii waste biomass represent an attractive candidate to remove multi metal ions. (author)

  18. Structural characterization and antimicrobial activities of transition metal complexes of a hydrazone ligand

    Science.gov (United States)

    Bakale, Raghavendra P.; Naik, Ganesh N.; Machakanur, Shrinath S.; Mangannavar, Chandrashekhar V.; Muchchandi, Iranna S.; Gudasi, Kalagouda B.

    2018-02-01

    A hydrazone ligand has been synthesized by the condensation of 2-nitrobenzaldehyde and hydralazine, and its Co(II), Ni(II), Cu(II) and Zn(II) complexes have been reported. Structural characterization of the ligand and its metal complexes has been performed by various spectroscopic [IR, NMR, UV-Vis, Mass], thermal and other physicochemical methods. The structure of the ligand and its Ni(II) complex has been characterized by single crystal X-ray diffraction studies. All the synthesized compounds have been screened for in vitro antimicrobial activity. The antibacterial activity is tested against Gram-positive strains Enterococcus faecalis, Streptococcus mutans and Staphylococcus aureus and Gram-negative strains Escherichia coli, Pseudomonas aeruginosa and Klebsiella pneumoniae using ciprofloxacin as the reference standard. Antifungal activity is tested against Candida albicans, Aspergillus fumigatus and Aspergillus niger using ketoconazole as the reference standard. The minimum inhibitory concentration (MIC) was determined for test compounds as well as for reference standard. Ligand, Cu(II) and Zn(II) complexes have shown excellent activity against Candida albicans.

  19. Biosorption of heavy metals by pretreated biomass of aspergillus niger

    International Nuclear Information System (INIS)

    Javaid, A.; Bajwa, R.; Manzoor, T.

    2011-01-01

    The present study reports the bio sorption potential of chemically pretreated mycelial biomass of fungus Aspergillus niger van. Tieghem for Cu(II) and Ni(II) ions from aqueous phase. Fungal biomass was pretreated with different types of alkaline/salts (NaOH, NaHCO/sub 3/, Na/sub 2/CO/sub 3/, NaCl and CaCl/sub 2/), acids (HCl and H/sub 2/SO/sub 4/) and detergent. Pretreatment of biomass with Na/sub 2/CO/sub 3/ and NaOH were proved to increase or maintain adsorption efficiency and capacity in comparison to untreated biomass. Pretreatment with NaHCO/sub 3/, detergent, NaCl and CaCl/sub 2/ significantly reduce (10-40%) metal sequestering efficiency of the adsorbent. Whereas, acid treatments resulted in drastic loss (80%) in metal uptake efficiency of the biomass. Amongst various pretreatments, Na/sub 2/CO/sub 3/ could be use efficiently for the removal of Ni(II) and Cu(II) ions from aqueous solution using A. niger. (author)

  20. Competitive metal sorption and desorption onto Kappaphycus alvarezii, seaweed waste biomass

    Energy Technology Data Exchange (ETDEWEB)

    Lee, K O; Ramli, Nazaruddin; Said, Mamot; Ahmad, Musa [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia (UKM), Bangi, selangor (Malaysia); Yasir, Suhaimi Mohd [School of Sciences and Technology, Universiti Malaysia Sabah (UMS), Sabah (Malaysia); Arbakariya Ariff, E-mail: naza@ukm.my [Faculty of Biotechnology and Biomolecular science, Universiti Putra Malaysia (UPM), Serdang, Selangor (Malaysia)

    2011-07-15

    Competitive metal sorption and desorption onto Kappaphycus alvarezii waste biomass were investigated. Metal sorption capacities were 0.82 mg Cr (III)/ g, 0.73 mg Ni (II)/ g, 0.67 mg Cd (II)/ g, 0.65 mg Cu( II)/ g and 0.64 mg Zn (II)/ g in multi metal system. Whereas, desorption efficiencies were 66.08 %, 71.50 % and 80.44 % using 0.1 M HNO{sub 3}, 0.1 M HCl and 0.1 M H{sub 2}SO{sub 4}, respectively. The metal sorption sequence were Cr(III) > Ni(II) > Cd(II) > Cu(II) > Zn(II), while metal desorption sequence were Cd(II) > Zn(II) > Cu(II) > Ni(II) > Cr(III). Fourier transformed infrared spectroscopy (FTIR) technique was used to characterize the seaweed waste biomass. FTIR analysis shown that carbonyl (-C-O) and nitrile (-C{identical_to}N) groups interact with the metal ions. The experiments result revealed that Kappaphycus alvarezii waste biomass represent an attractive candidate to remove multi metal ions. (author)

  1. Removal of Heavy Metals by Adsorption onto Activated Carbon Derived from Pine Cones of Pinus roxburghii.

    Science.gov (United States)

    Saif, Muhammad Jawwad; Zia, Khalid Mahmood; Fazal-ur-Rehman; Usman, Muhammad; Hussain, Abdullah Ijaz; Chatha, Shahzad Ali Shahid

    2015-04-01

    Activated carbon derived from cones of Pinus roxburghii (Himalayan Pine) was used as an adsorbent for the removal of copper, nickel and chromium ions from waste water. Surface analysis was carried out to determine the specific surface area and pore size distribution of the pine cone derived activated carbon. Optimal parameters, effect of adsorbent quantity, pH, equilibrium time, agitation speed and temperature were studied. Equilibrium data were evaluated by Langmuir and Freundlich isotherm models. Langmuir isotherm afforded the best fit to the equilibrium data with a maximum adsorption capacity of 14.2, 31.4 and 29.6 mg/g for Cu(II), Ni(II) and Cr(VI) respectively. Maximum adsorption of Cu(II), Ni(II) was observed in the pH range 4.0 to 4.5, whereas the best adsorption of Cr(VI) was observed at pH 2.5. It was found that 180 minutes was sufficient to gain adsorption equilibrium. The adsorption process follows a pseudo-second-order kinetic model.

  2. Rapid adsorption of heavy metals by Fe3O4/talc nanocomposite and optimization study using response surface methodology.

    Science.gov (United States)

    Kalantari, Katayoon; Ahmad, Mansor B; Masoumi, Hamid Reza Fard; Shameli, Kamyar; Basri, Mahiran; Khandanlou, Roshanak

    2014-07-21

    Fe3O4/talc nanocomposite was used for removal of Cu(II), Ni(II), and Pb(II) ions from aqueous solutions. Experiments were designed by response surface methodology (RSM) and a quadratic model was used to predict the variables. The adsorption parameters such as adsorbent dosage, removal time, and initial ion concentration were used as the independent variables and their effects on heavy metal ion removal were investigated. Analysis of variance was incorporated to judge the adequacy of the models. Optimal conditions with initial heavy metal ion concentration of 100, 92 and 270 mg/L, 120 s of removal time and 0.12 g of adsorbent amount resulted in 72.15%, 50.23%, and 91.35% removal efficiency for Cu(II), Ni(II), and Pb(II), respectively. The predictions of the model were in good agreement with experimental results and the Fe3O4/talc nanocomposite was successfully used to remove heavy metals from aqueous solutions.

  3. 14N nuclear quadrupole interaction in Cu(II) doped L-alanine

    International Nuclear Information System (INIS)

    Murgich, J.; Calvo, R.; Oseroff, S.B.; Instituto Venezolano de Investigaciones Cientificas, Caracas. Dept. de Quimica)

    1980-01-01

    The 14 N nuclear quadrupole interaction tensor Psub(N) measured by ENDOR in Cu(II) doped L-alanine is analyzed in terms of the Townes and Daily theory assuming a tetra-hedrally bonded N atom. The results of this analysis are compared with those for the 14 N in pure L-alanine and it is found that the principal directions of the Psub(N) tensor are drastically changed upon metal complexation as a consequence of the higher electron affinity of Cu(II) with respect to C and H. Comparison of the corresponding bond populations in pure and Cu(II) doped L-alanine indicates that the Cu draws 0.11 more electron from the N than the substituted H atom. (orig.)

  4. Removal of Cu(II) in water by polymer enhanced ultrafiltration: Influence of polymer nature and pH.

    Science.gov (United States)

    Kochkodan, Olga D; Kochkodan, Viktor M; Sharma, Virender K

    2018-01-02

    This study presents an efficient removal of Cu(II) in water using the polymer enhanced ultrafiltration (PEUF) method. Polymer of different molecular weight (MW) (polyethyleneimine (PEI), sodium lignosulfonates (SLS) and dextrans) were investigated to evaluate efficiency in removal of Cu(II) in water by the PEUF method. The decomposition of Cu(II)-polymer complex was also evaluated in order to reuse polymers. Cu(II) complexation depends on the MW of chelating polymer and the pH of feed solution. It was found that the Cu(II) rejection increased with the polymer dosage with high removal of Cu(II) when using PEI and SLS at a 10:20 (mg/mg) ratio ([Cu(II)]:[polymer]). It was found that the maximum chelating capacity was 15 mg of Cu(II) per 20 mg of PEI. The Cu(II)-PEI complex could be decomposed by acid addition and the polymer could be efficiently reused with multiple complexation-decomplexation cycles. A conceptual flow chart of the integrated process of efficient removal of Cu(II) by PEUF method is suggested.

  5. Preconcentration of trace elements by using 1-(2-Pyridylazo-2-naphthol functionalized Amberlite XAD-1180 resin and their determination by FAAS

    Directory of Open Access Journals (Sweden)

    Tokalioglu Serife

    2006-01-01

    Full Text Available In this study, Amberlite XAD-1180 resin functionalized by 1-(2-pyridylazo-2-naphthol (PAN was synthesized and the resulting resin was used for preconcentration of Cr(III, Mn(II, Fe(III, Ni(II, Cu(II, Cd(II and Pb(II elements present at trace levels in different matrices. For this purpose, the copolymer was nitrated, reduced to the corresponding amine, converted to the diazonium salt with nitrite and reacted with PAN to produce the XAD-1180-PAN chelating resin. For the described method, the effect of some analytical parameters, such as pH, sample volume, resin amount, flow rates of uptake and stripping, volume and type of eluent, on the recovery of the trace elements was investigated. The metals retained on the XAD-1180-PAN resin were eluted by 2 mol L-1 HNO3. The influence of matrix ions, i.e., Na(I, K(I, Ca(II and Mg(II, on the recovery of trace elements was also examined by using the developed method when they occurred both individually and together. The repeatability of the method at the optimum conditions determined experimentally was investigated. The recovery values for all the elements, except for Cr(III, were found to be >92% and the relative standard deviation was <8.5%. The 3s/b detection limits for Cr(III, Mn(II, Fe(III, Ni(II, Cu(II, Cd(II and Pb(II were found to be 4.1, 0.13, 2.7, 1.2, 0.19, 0.06 and 0.13 µg L-1, respectively. The developed method was utilized for preconcentration and determination of Mn(II, Fe(III, Ni(II, Cu(II, Cd(II and Pb(II in tap water, rain water, and stream water, and of Ni(II, Cd(II and Pb(II in a certified reference material (RM 8704 Buffalo river sediment by flame atomic absorption spectrometry (FAAS.

  6. AUTHOR INDEX

    Indian Academy of Sciences (India)

    Unknown

    Exogenous bridging and nonbridging in. Cu(II) complexes of Mannich base ligands: Synthesis and physical properties. 559. Thander A. Charge-transfer spectra of ferrocene in halo- carbon solvents under photoexcitation 475. Thimmaiah K N see Kalpana H N. 51. Umamaheswari V. Isomorphous substitution of Mn(II), Ni(II).

  7. Synthesis, spectral characterization, antimicrobial, DNA interactions ...

    Indian Academy of Sciences (India)

    KUNCHE SUDEEPA

    2018-05-04

    May 4, 2018 ... structural aspects of FMBC and its Cu(II), Ni(II) and. Zn(II) complexes ... of DNA was down- loaded from protein data bank24 (www.rcsb.org) pdb id: ... the reaction mixture was refluxed on water bath for 4–8 h maintaining the ...

  8. Contaminant Immobilization and Nutrient Release by Biochar Soil Amendment: Roles of Natural Organic Matter

    Science.gov (United States)

    Contamination of soil interstitial waters by labile heavy metals such as CuII, CdII, and NiII is of worldwide concern. Carbonaceous materials such as char and activated carbon have received considerable attention in recent years as soil amendment for both sequestering heavy metal contaminants and r...

  9. Characterization of Schiff base derived from 2-hydroxo-1 ...

    African Journals Online (AJOL)

    MBI

    2014-03-04

    Mar 4, 2014 ... derived from 2, 2' bis(p-methoxylphenylamine) and salicylic ... containing Co(II), Ni(II), Cu(II) and Zn(II) synthesized from ..... pKa = 12.55. Ka = 2.81E-13 .... 20, no. 3, 297 – 300. Gaowen Y., Xiaping X. , Huan T. and Chenxue Z.

  10. Template synthesis, characterization and antimicrobial activity of the complex combinations of some transitional metals with isonicotinoylhydrazone -2,4,6- trimethylbenzaldehyde

    International Nuclear Information System (INIS)

    Mitu, L.ITU; Imran, M.

    2011-01-01

    The complexes of Cu(II), Ni(II), Co(II), Mn(II), and Zn(II) with isonicotinoyl-hydrazone -2,4,6-trimethylbenzaldehyde (INHTB) are reported. The complexes have been characterized by analytical data, IR, UV-Vis, NMR spectra, magnetic susceptibility, thermal analysis and for the Cu(II) complex the ESR spectrum has been recorded. The anti-bacterial activity of these complexes were investigated against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Salmonella enteritidis, Shigella flexneri bacteria. The INHTB ligand is coordinated at the metallic ions by oxygen amide (O=C) and the azomethine nitrogen. (author)

  11. Poly (furfural-acetone) as New Adsorbent for Removal of Cu(II) from Aqueous Solution: Equilibrium Study

    OpenAIRE

    Najim, Tariq S.

    2010-01-01

    The batch removal of Cu(II) from aqueous solution using poly (furfural-acetone), (PFA) as adsorbent was investigated in this study. The influences of initial Cu(II) ion concentration (10 to 120 ppm), pH (4-8) and contact time have been reported. Adsorption of Cu(II) is highly pH-dependent and the result indicate that the optimum pH for the removal was found to be 6. At this pH a small amount of PFA, 2 g/L, could remove as much as 97% of Cu(II) from a solution of initial concentration 10 ppm....

  12. Magnetic Study of the Novel Polynuclear Compound [Cu(II)(6-Mercaptopurinolate 2-)] n

    Science.gov (United States)

    Acevedo-Chávez, Rodolfo; Costas, María. Eugenia; Escudero, Roberto

    1997-08-01

    Chemical reactions between Cu(II) and 6-mercaptopurine, both in aqueous and in methanolic media, yield the novel amorphous polynuclear compound [Cu(II)(6-mercaptopurinolate)2-]n, which is also obtained from diverse Cu(II)-heterocyclic ligand competitive reactions. The kinetic and thermodynamic stabilities associated with the formation of this compound are inferred as remarkable. The spectroscopic data let us suggest the involvement of the exocyclic S(6) donor site and the N atoms in the imidazolic moiety of the deprotonated heterocyclic ligand in the coordination to Cu(II) atoms, forming a distorted bidimensional metallic network. The magnetic studies show the existence of very weak antiferromagnetic coupling in the solid sample. This system represents the first example of a 1 : 1 metal : 6-mercaptopurinolate2-system with ad-type open shell metallic center. The magnetic study carried out also represents the first example of magnetic characterization for this type of polynuclear Cu(II) systems with the dianionic 6-mercaptopurine ligand.

  13. Coordination conversion of cobalt(II) in binary aqueous-organic solvents

    Energy Technology Data Exchange (ETDEWEB)

    Khvostova, N.O.; Karapetyan, G.O.; Yanush, O.V.

    1985-11-01

    It has been shown that the thermochromic conversions of cobalt(II) in binary solvents are influenced by a number of factors: the nature of the solvent, the strength of the complexes of octahedral symmetry formed, the outer-sphere influence of the solvent on the complexes, the form of the anion, the solvation of the participants in the reaction, and the interaction of the components of the solvent with one another. A correlation between the strength and the spectral position of the absorption bands of the complexes of the activator has been established, and a spectroscopic criterion for selecting the solvents has been proposed. The expediency of using binary solvents to create effective thermochromic media with variable phototransmission has been substantiated.

  14. Utilization of m-Phenylenediamine-Furfural Resin for Removal of Cu(II) from Aqueous Solution-A Thermodynamic Study

    OpenAIRE

    Najim, Tariq S.; Zainal, Israa G.; Ali, Dina A.

    2010-01-01

    m-Phenylenediamine was condensed with furfural in absence of catalyst at room temperature. The produced m-phenylenediamine-furfural resin was used for the removal of Cu(II) from aqueous solution. The pH for the optimum removal of Cu(II) was 6. The negative values of Gibbs free energy at low concentration of Cu(II) (20, 30 ppm) indicative of the spontaneous adsorption process, while, at higher Cu(II) concentration (40,50 ppm) the positive and weak values of ∆G° indicate that the process is fea...

  15. Computational studies of a paramagnetic planar dibenzotetraaza[14]annulene Ni(II) complex.

    Science.gov (United States)

    Rabaâ, Hassan; Khaledi, Hamid; Olmstead, Marilyn M; Sundholm, Dage

    2015-05-28

    A square-planar Ni(II) dibenzotetraaza[14]annulene complex substituted with two 3,3-dimethylindolenine groups in the meso positions has recently been synthesized and characterized experimentally. In the solid-state, the Ni(II) complex forms linear π-interacting stacks with Ni···Ni separations of 3.448(2) Å. Measurements of the temperature dependence of the magnetic susceptibility revealed a drastic change in the magnetic properties at a temperature of 13 K, indicating a transition from low-to-high spin states. The molecular structures of the free-base ligand, the lowest singlet, and triplet states of the monomer and the dimer of the Ni complex have been studied computationally using density functional theory (DFT) and ab initio correlation levels of theory. In calculations at the second-order Møller-Plesset (MP2) perturbation theory level, a large energy of 260 kcal mol(-1) was obtained for the singlet-triplet splitting, suggesting that an alternative explanation of the observed magnetic properties is needed. The large energy splitting between the singlet and triplet states suggests that the observed change in the magnetism at very low temperatures is due to spin-orbit coupling effects originating from weak interactions between the fine-structure states of the Ni cations in the complex. The lowest electronic excitation energies of the dibenzotetraaza[14]annulene Ni(II) complex calculated at the time-dependent density functional theory (TDDFT) levels are in good agreement with values deduced from the experimental UV-vis spectrum. Calculations at the second-order algebraic-diagrammatic construction (ADC(2)) level on the dimer of the meso-substituted 3,3-dimethylindolenine dibenzotetraaza[14] annulene Ni(II) complex yielded Stokes shifts of 85-100 nm for the lowest excited singlet states. Calculations of the strength of the magnetically induced ring current for the free-base 3,3-dimethylindolenine-substituted dibenzotetraaza[14]annulene show that the annulene

  16. Synthesis, spectral, thermal and antimicrobial studies on cobalt(II), nickel(II), copper(II), zinc(II) and palladium(II) complexes containing thiosemicarbazone ligand

    Science.gov (United States)

    El-Sawaf, Ayman K.; El-Essawy, Farag; Nassar, Amal A.; El-Samanody, El-Sayed A.

    2018-04-01

    The coordination characteristic of new N4-morpholinyl isatin-3-thiosemicarbazone (HL) towards Co(II), Ni(II), Cu(II), Zn(II) and Pd(II) has been studies. The structures of the complexes were described by elemental analyses, molar conductivity, magnetic, thermal and spectral (IR, UV-Vis, 1H and 13C NMR and ESR) studies. On the basis of analytical and spectral studies the ligand behaves as monobasic tridentate ONS donor forming two five membered rings towards cobalt, copper and palladium and afforded complexes of the kind [M(L)X], (Mdbnd Co, Cu or Pd; Xdbnd Cl, Br or OAc). Whereas the ligand bound to NiCl2 as neutral tridentate ONS donor and with ZnCl2 as neutral bidentate NS donor. The newly synthesized thiosemicarbazone ligand and some of its complexes were examined for antimicrobial activity against 2 gram negative bacterial strains (Escherichia coli Pseudomonas and aeruginosa), 2 gram positive bacterial strains (Streptococcus pneumoniae and Staphylococcus aureus)} and two Pathogenic fungi (Aspergillus fumigatus and Candida albicans). All metal complexes possess higher antimicrobial activity comparing with the free thiosemicarbazone ligand. The high potent activities of the complexes may arise from the coordination and chelation, which tends to make metal complexes act as more controlling and potent antimicrobial agents, thus hindering the growing of the microorganisms. The antimicrobial results also show that copper bromide complex is better antimicrobial agent as compared to the Schiff base and its metal complexes.

  17. Dendritic chelating agents. 1. Cu(II) binding to ethylene diamine core poly (amidoamine) denderimers in aqueous solutions

    International Nuclear Information System (INIS)

    Diallo, Mamadou S.; Christie, Simone; Swaminathan, Pirabalini; Balogh, Lajos; Shi, XIANGYANG; Um, Wooyong; Papelis, Charalambos; Goddard, William A.; Johnson, J. H.

    2004-01-01

    The overall results of the proton and metal ion binding measurements suggest that the uptake of Cu(II) by EDA core PAMAM dendrimers involves both the dendrimer tertiary amine and terminal groups. However, the extents of protonation of these groups control the ability of the dentrimers to bind Cu(II). Analysis of the EXAFS spectra suggests that Cu(II) forms octahedral complexes involving the tertiary amine groups of Gx-NH2 EDA core PAMAM dendrimers at pH 7.0. The central Cu(II) metal ion of each of these complexes appears to be coordinated to 2-4 dendrimer tertiary amine groups located in the equatorial plane and 2 axial water molecules. Finally, we combine the results of our experiments with literature data to formulate and evaluate a phenomenological model of Cu(II) uptake by Gx-NH2 PAMAM dendrimers in aqueous solutions. At low metal ion-dendrimer loadings, the model provides a good fit of the measured extent of binding of Cu(II) in aqueous solutions of G4-NH2 PAMAM dendrimers at pH 7.0

  18. Adsorption of Cu(II) on Oxidized Multi-Walled Carbon Nanotubes in the Presence of Hydroxylated and Carboxylated Fullerenes

    Science.gov (United States)

    Wang, Jing; Li, Zhan; Li, Shicheng; Qi, Wei; Liu, Peng; Liu, Fuqiang; Ye, Yuanlv; Wu, Liansheng; Wang, Lei; Wu, Wangsuo

    2013-01-01

    The adsorption of Cu(II) on oxidized multi-walled carbon nanotubes (oMWCNTs) as a function of contact time, pH, ionic strength, temperature, and hydroxylated fullerene (C60(OH)n) and carboxylated fullerene (C60(C(COOH)2)n) were studied under ambient conditions using batch techniques. The results showed that the adsorption of Cu(II) had rapidly reached equilibrium and the kinetic process was well described by a pseudo-second-order rate model. Cu(II) adsorption on oMWCNTs was dependent on pH but independent of ionic strength. Compared with the Freundlich model, the Langmuir model was more suitable for analyzing the adsorption isotherms. The thermodynamic parameters calculated from temperature-dependent adsorption isotherms suggested that Cu(II) adsorption on oMWCNTs was spontaneous and endothermic. The effect of C60(OH)n on Cu(II) adsorption of oMWCNTs was not significant at low C60(OH)n concentration, whereas a negative effect was observed at higher concentration. The adsorption of Cu(II) on oMWCNTs was enhanced with increasing pH values at pH adsorption of Cu(II) onto oMWCNTs at pH 4–6. The double sorption site model was applied to simulate the adsorption isotherms of Cu(II) in the presence of C60(OH)n and fitted the experimental data well. PMID:24009683

  19. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Synthesis, characterisation and electrochemical behaviour of Cu(II), Co(II), Ni(II) and Zn(II) complexes derived from acetylacetone and p-anisidine and their antimicrobial activity · N Raman V Muthuraj S Ravichandran A Kulandaisamy · More Details Abstract Fulltext PDF. Neutral tetradentate N2O2 type complexes of Cu(II), ...

  20. Mn(II), Zn(II) and VO(II) Schiff

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 113; Issue 3. Synthesis and characterisation of Cu(II), Ni(II), Mn(II), Zn(II) and VO(II) Schiff base complexes derived from o-phenylenediamine and acetoacetanilide. N Raman Y Pitchaikani Raja A Kulandaisamy. Inorganic Volume 113 Issue 3 June 2001 pp 183-189 ...

  1. Synthesis, characterization and antimicrobial activities of a Schiff ...

    African Journals Online (AJOL)

    Complexes of Cu(II), Ni(II) and Mn(II) with a Schiff base derived from condensation reaction of phenylalanine and acetylacetone have been synthesized and characterized analytically and spectroscopically. Melting point of the Schiff base was 188oC and the complexes decompose within a temperature range of 210-242oC.

  2. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Equilibrium and solution structural study of mixed-metal-mixed-ligand complexes of Cu(II), Ni(II) and Zn(II) with L-cysteine, L-threonine and imidazole are conducted in aqueous solution by potentiometry and spectrophotometry. Stability constants of the binary, ternary and quaternary complexes are determined at 25 ± 1 ° C ...

  3. 1D and 2D Cobalt(II) Coordination Polymers, Co(ox)(en):Synthesis, Structures and Magnetic Properties

    International Nuclear Information System (INIS)

    Kang, Jae Un; Lee, Yu Mi; Kim, Seung Joo; Yun, Ho Seop; Do, Jung Hwan

    2014-01-01

    Two ethylenediamine cobalt(II) oxalate complexes Co(ox)(en), 1 and Co(ox)(en)·2H 2 O, 2 have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR spectrum, TG analysis, and magnetic measurements. In 1, Co atoms are coordinated by two bis-bidentate oxalate ions in transconfiguration to form Co(ox) chains, which are further bridged by ethylenediamine molecules to produce 2D grid layers, Co(ox)(en). In 2, Co atoms are coordinated by bridging oxalate ions in cis - configuration to form Co(ox) chains, and the additional chelation of ethylenediamine to Co atoms completes 1D zigzag chain, Co(en)(ox). Two lattice water molecules stabilize the chains through hydrogen bonding. Magnetic susceptibility measurements indicate that both complexes exhibit weak antiferromagnetic coupling between cobalt(II) ions with the susceptibility maxima at 23 K for 1 and 20 K for 2, respectively. In 1 and 2, the oxalate ligands afford a much shorter and more effective pathway for the magnetic interaction between cobalt ions compared to the ethylenediamine ligands, so the magnetic behaviors of both complexes could be well described with 1D infinite magnetic chain model

  4. Electrochemical behavior of phytochelatins and related peptides at the hanging mercury drop electrode in the presence of cobalt(II) ions.

    Science.gov (United States)

    Dorcák, Vlastimil; Sestáková, Ivana

    2006-01-01

    Direct current voltammetry and differential pulse voltammetry have been used to investigate the electrochemical behaviour of two phytochelatins: heptapeptide (gamma-Glu-Cys)3-Gly and pentapeptide (gamma-Glu-Cys)2-Gly, tripeptide glutathione gamma-Glu-Cys-Gly and its fragments: dipeptides Cys-Gly and gamma-Glu-Cys at the hanging mercury drop electrode in the presence of cobalt(II) ions. Most interesting results were obtained with direct current voltammetry in the potential region of -0.80 V up to -1.80 V. Differential pulse voltammetry of the same solutions of Co(II) with peptides gives more complicated voltammograms with overlapping peaks, probably in connection with the influence of adsorption at slow scan rates necessarily used in this method. However, in using Brdicka catalytic currents for analytical purposes, differential pulse voltammograms seem to be more helpful. Presented investigations have shown that particularly the prewave of cobalt(II) allows distinguishing among phytochelatins, glutathione, and its fragments.

  5. Electrodialytic separation of Cu(II) and As(V) in acidic electrolytes; Separacion electrodialitica de Cu(II) y As(V) en electrolitos acidos

    Energy Technology Data Exchange (ETDEWEB)

    Ibanez, J. P.; Ipinza, J.; Cifuentes, L.

    2007-07-01

    The separation of copper and arsenic from acidic electrolytes by electrodialysis was investigated at room temperature. the effect of current density and pH was studied in a batch cell during 3 hours. The kinetic parameters showed that Cu(II) transport rate was 0.75 mol/m''2/h and the As(V) transport rate was 0.002 mol/m''2/h. An efficient separation between Cu(II) and As(V) was achieved; Generating a concentrated solution of copper with no arsenic, which was obtained independently of the electrolyte acidity and current density used. The effect of the arsenic speciation with pH is discussed as well. (Author) 23 refs.

  6. Macroscopic and molecular approaches of enrofloxacin retention in soils in presence of Cu(II).

    Science.gov (United States)

    Graouer-Bacart, Mareen; Sayen, Stéphanie; Guillon, Emmanuel

    2013-10-15

    The co-adsorption of copper and the fluoroquinolone antibiotic enrofloxacin (ENR) at the water-soil interface was studied by means of batch adsorption experiments, and extended X-ray absorption fine structure (EXAFS) spectroscopy. The system was investigated over a pH range between 6 and 10, at different contact times, ionic strengths, and ENR concentrations. Adsorption coefficient - Kd - was determined at relevant environmental concentrations and the value obtained in water at a ionic strength imposed by the soil and at soil natural pH was equal to 0.66Lg(-1). ENR adsorption onto the soil showed strong pH dependence illustrating the influence of the electrostatic interactions in the sorption processes. The simultaneous co-adsorption of ENR and Cu(II) on the soil was also investigated. The presence of Cu(II) strongly influenced the retention of the antibiotic, leading to an increase up to 35% of adsorbed ENR amount. The combined quantitative and spectroscopic results showed that Cu(II) and ENR directly interacted at the water-soil interface to form ternary surface complexes. Cu K-edge EXAFS data indicated a molecular structure where the carboxylate and carbonyl groups of ENR coordinate to Cu(II) to form a 6-membered chelate ring and where Cu(II) bridges between ENR and the soil surface sites. Cu(II) bonds bidentately to the surface in an inner-sphere mode. Thus, the spectroscopic data allowed us to propose the formation of ternary surface complexes with the molecular architecture soil-Cu(II)-ENR. Copyright © 2013 Elsevier Inc. All rights reserved.

  7. Spectral studies, thermal investigation and biological activity of some metal complexes derived from (E)-N‧-(1-(4-aminophenyl)ethylidene)morpholine-4-carbothiohydrazide

    Science.gov (United States)

    El-Samanody, El-Sayed A.; Polis, Magdy W.; Emara, Esam M.

    2017-09-01

    A new series of biologically active Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes derived from the novel thiosemicarbazone ligand; (E)-N‧-(1-(4-aminophenyl)ethylidene)morpholine-4-carbothiohydrazide (HL) were synthesized. The mode of bonding of the ligand and the geometrical structures of its metal complexes were achieved by different analytical and spectral methods. The ligand coordinated with metal ions in a neutral bidentate fashion through the thione sulfur and azomethine nitrogen atoms. All metal complexes adopted octahedral geometry, except Cu(II) complexes (3, 6, 7) which have a square planar structure. The general thermal decomposition pathways of the ligand along with its metal complexes were explained. The thermal stability of the complexes is controlled by the number of outer and inner sphere water molecules, ionic radii and the steric hindrance. The activation thermodynamic parameters; (activation energy (E*), enthalpy of activation (ΔH*), entropy of activation (ΔS*) and Gibbs free energy (ΔG*)) along with order of reaction (n) were estimated from DTG curves. The ESR spectra of Cu(II) complexes indicated that (dx2-y2)1 is the ground state with covalence character of metal-ligand bonds. The molluscicidal and biochemical effects of the ligand and its Ni(II); Cu(II) complexes (2; 3, 5, 7) along with their combinations with metaldehyde were screened in vitro on the mucous gland of Eobania vermiculata. The tested compounds exhibited a significant toxicity against the tested animals and have almost the same toxic effect of metaldehyde which increases the mucous secretion of the snails and leads to death.

  8. Synthesis, spectroscopic characterization, electrochemistry and biological evaluation of some metal (II) complexes with ONO donor ligand containing benzo[b]thiophene and coumarin moieties

    Science.gov (United States)

    Mahendra Raj, K.; Mruthyunjayaswamy, B. H. M.

    2014-09-01

    Schiff base ligand 3-chloro-N‧-((7-hydroxy-4-methyl-2-oxo-2H-chromen-8-yl)methylene)benzo[b]thiophene-2-carbohydrazide and its Cu(II), Co(II), Ni(II) and Zn(II) complexes were synthesized, characterized by elemental analysis and various physico-chemical techniques like, IR, 1H NMR, ESI-mass, UV-Visible, thermogravimetry - differential thermal analysis, magnetic measurements and molar conductance. Spectral analysis indicates octahedral geometry for all the complexes. Cu(II) complex have 1:1 stoichiometry of the type [M(L)(Cl)(H2O)2], whereas Co(II), Ni(II) and Zn(II) complexes have 1:2 stoichiometric ratio of the type [M(L)2]. The bonding sites are the oxygen atom of amide carbonyl, nitrogen of azomethine function and phenolic oxygen of the Schiff base ligand via deprotonation. The thermogravimetry - differential thermal analysis studies gave evidence for the presence of coordinated water molecules in the composition of Cu(II) complex which was further supported by IR measurements. All the complexes were investigated for their electrochemical activity, but only the Cu(II) complex showed the redox property. In order to evaluate the effect of antimicrobial potency of metal ions upon chelation, ligand and its metal complexes along with their respective metal chlorides were screened for their antibacterial and antifungal activities by minimum inhibitory concentration (MIC) method. The results showed that the metal complexes were found to be more active than free ligand. Ligand and its complexes were screened for free radical scavenging activity by DPPH method and DNA cleavage activity using Calf-thymus DNA (Cat. No-105850).

  9. Optimizing Cu(II) removal from aqueous solution by magnetic nanoparticles immobilized on activated carbon using Taguchi method.

    Science.gov (United States)

    Ebrahimi Zarandi, Mohammad Javad; Sohrabi, Mahmoud Reza; Khosravi, Morteza; Mansouriieh, Nafiseh; Davallo, Mehran; Khosravan, Azita

    2016-01-01

    This study synthesized magnetic nanoparticles (Fe(3)O(4)) immobilized on activated carbon (AC) and used them as an effective adsorbent for Cu(II) removal from aqueous solution. The effect of three parameters, including the concentration of Cu(II), dosage of Fe(3)O(4)/AC magnetic nanocomposite and pH on the removal of Cu(II) using Fe(3)O(4)/AC nanocomposite were studied. In order to examine and describe the optimum condition for each of the mentioned parameters, Taguchi's optimization method was used in a batch system and L9 orthogonal array was used for the experimental design. The removal percentage (R%) of Cu(II) and uptake capacity (q) were transformed into an accurate signal-to-noise ratio (S/N) for a 'larger-the-better' response. Taguchi results, which were analyzed based on choosing the best run by examining the S/N, were statistically tested using analysis of variance; the tests showed that all the parameters' main effects were significant within a 95% confidence level. The best conditions for removal of Cu(II) were determined at pH of 7, nanocomposite dosage of 0.1 gL(-1) and initial Cu(II) concentration of 20 mg L(-1) at constant temperature of 25 °C. Generally, the results showed that the simple Taguchi's method is suitable to optimize the Cu(II) removal experiments.

  10. Flame atomic absorption spectrometric determination of heavy metals in aqueous solution and surface water preceded by co-precipitation procedure with copper(II) 8-hydroxyquinoline

    Science.gov (United States)

    Ipeaiyeda, Ayodele Rotimi; Ayoade, Abisayo Ruth

    2017-12-01

    Co-precipitation procedure has widely been employed for preconcentration and separation of metal ions from the matrices of environmental samples. This is simply due to its simplicity, low consumption of separating solvent and short duration for analysis. Various organic ligands have been used for this purpose. However, there is dearth of information on the application of 8-hydroxyquinoline (8-HQ) as ligand and Cu(II) as carrier element. The use of Cu(II) is desirable because there is no contamination and background adsorption interference. Therefore, the objective of this study was to use 8-HQ in the presence of Cu(II) for coprecipitation of Cd(II), Co(II), Cr(III), Ni(II) and Pb(II) from standard solutions and surface water prior to their determinations by flame atomic absorption spectrometry (FAAS). The effects of pH, sample volume, amount of 8-HQ and Cu(II) and interfering ions on the recoveries of metal ions from standard solutions were monitored using FAAS. The water samples were treated with 8-HQ under the optimum experimental conditions and metal concentrations were determined by FAAS. The metal concentrations in water samples not treated with 8-HQ were also determined. The optimum recovery values for metal ions were higher than 85.0%. The concentrations (mg/L) of Co(II), Ni(II), Cr(III), and Pb(II) in water samples treated with 8-HQ were 0.014 ± 0.002, 0.03 ± 0.01, 0.04 ± 0.02 and 0.05 ± 0.02, respectively. These concentrations and those obtained without coprecipitation technique were significantly different. Coprecipitation procedure using 8-HQ as ligand and Cu(II) as carrier element enhanced the preconcentration and separation of metal ions from the matrix of water sample.

  11. Author Details

    African Journals Online (AJOL)

    Osunlaja, AA. Vol 8, No 1 (2009) - Articles Synthesis, physico-chemical and antimicrobial properties of Co(II), Ni(II) and Cu(II) mixed-ligand complexes of dimethylglyoxime - Part I Abstract PDF. ISSN: 1684-5315. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More ...

  12. and amino acids

    Indian Academy of Sciences (India)

    Unknown

    P RABINDRA REDDY* and A MOHAN REDDY. Department of ... The mixed ligand complexes of Cu(II), Ni(II) and Co(II) with uridine and amino acids ..... Sabat M, Satyashur K A and Sundaralingam M 1983 J. Am. Chem. Soc. ... Uemura T, Shimura T, Nakamishi H, Tomahiro T, Nagawa Y and Okuno (Yohmei) H 1991. Inorg.

  13. Synthesis, Spectral, Thermogravimetric, XRD, Molecular Modelling and Potential Antibacterial Studies of Dimeric Complexes with Bis Bidentate ON–NO Donor Azo Dye Ligands

    Directory of Open Access Journals (Sweden)

    Bipin Bihari Mahapatra

    2013-01-01

    Full Text Available The dimeric complexes of Co(II, Ni(II, Cu(II, Zn(II, Cd(II, and Hg(II with two new symmetrical ON–NO donor bis bidentate (tetradentate azo dye ligands, LH2 = 4,4′-bis(4′-hydroxyquinolinolinylazodiphenylsulphone, and L′H2 = 4,4′-bis(acetoacetanilideazodiphenylsulphone have been synthesized. The metal complexes have been characterised by elemental analytical, conductance, magnetic susceptibility, IR, electronic spectra, ESR, NMR, thermogravimetry, X-ray diffraction (powder pattern spectra, and molecular modelling studies. The Co(II and Ni(II complexes are found to be octahedral, Cu(II complexes are distorted octahedral, and a tetrahedral stereochemistry has been assigned to Zn(II, Cd(II, and Hg(II complexes. The thermogravimetric study indicates that compounds are quite stable. The energy optimized structures are proposed using the semiempirical ZINDO/1 quantum mechanical calculations. The potential antibacterial study of the ligands and some metal complexes has been made with one gram positive bacteria Staphylococcus aureus and one gram negative bacteria E. coli which gives encouraging results. Both the Co(II complexes are found to possess monoclinic crystal system.

  14. Synthesis, Characterization and Spectral Studies of Noble Heterobinuclear Complexes of Transition Metal Ions and their Biological Activity

    Directory of Open Access Journals (Sweden)

    Netra Pal Singh

    2011-01-01

    Full Text Available Some noble heterobinuclear complexes of transition metal ions with bis(salicylaldehydemalonyl-dihydrazone in the presence of 5-nitroindazole Cu(II / Ni(II- chloride of the type [ML1M‘L2Cl2] or [ML1FeL2Cl2]Cl, where M = Ni(II, Cu(II and M' = Mn(II, Co(II, have been prepared. All the complexes have been characterized by IR, UV vis and EPR spectroscopy, elemental analysis, magnetic moment and molar conductance measurement. Spectral studies and magnetic moment measurement in DMF suggest the covalent nature of the complexes, except the [ML1FeL2Cl2]Cl complex which is 1:1 electrolyte. An octahedral geometry is proposed for M‘ and square planer for M for the heterobinuclear complexes. The low value of magnetic moment and overlapping EPR signals are due to spin crossover since both of the metals have unpaired electrons with same molecular symmetry. The lowering of the magnetic moment has been discussed. The biological activity (antifungal and antibacterial of the represented compounds has been studied.

  15. Stability Constants of Mixed Ligand Complexes of Transition Metal(II Ions with Salicylidene-4-methoxyaniline as Primary Ligand and 5-Bromosalicylidene-4-nitroaniline as Secondary Ligand

    Directory of Open Access Journals (Sweden)

    N. G. Nadkarni

    2011-01-01

    Full Text Available Binary and ternary complexes of the type M-Y and M-X-Y [M = Mn(II, Ni(II, Cu(II and Zn(II; X = salicylidene-4-methoxyaniline and Y=5-bromosalicylidene-4-nitroaniline] have been examined pH-metrically at 27±0.5 °C and at constant ionic strength, μ= 0.1 M (KCl in 75 : 25(v/v 1,4-dioxne-water medium. The stability constants for binary (M-Y and ternary (M-X-Y systems were calculated. The relative stability (Δ log KT values of the ternary complexes with corresponding binary complexes for all the metal(II ions in the present study found to be negative indicating that ternary 1:1:1 (M-X-Y complexes are less stable than binary 1:1 (M-Y complexes. In the ternary system studied, the order of stability constants of mixed ligand complexes with respect to the metal ions was found to be Cu(II > NI(II > Mn(II > Zn(II; which is same as in the corresponding binary (M-Y systems.

  16. Kinetic and thermodynamic aspects of Cu(II) and Cr(III) removal from aqueous solutions using rose waste biomass

    International Nuclear Information System (INIS)

    Iftikhar, Abdur Rauf; Bhatti, Haq Nawaz; Hanif, Muhammad Asif; Nadeem, Razyia

    2009-01-01

    Distillation waste of rose petals was used to remove Cu(II) and Cr(III) from aqueous solutions. The results demonstrated the dependency of metal sorption on pH, sorbent dose, sorbent size, initial bulk concentration, time and temperature. A dosage of 1 g/L of rose waste biomass was found to be effective for maximum uptake of Cu(II) and Cr(III). Optimum sorption temperature and pH for Cu(II) and Cr(III) were 303 ± 1 K and 5, respectively. The Freundlich regression model and pseudo-second-order kinetic model were resulted in high correlation coefficients and described well the sorption of Cu(II) and Cr(III) on rose waste biomass. At equilibrium q max (mg/g) of Cu(II) and Cr(III) was 55.79 and 67.34, respectively. The free energy change (ΔG o ) for Cu(II) and Cr(III) sorption process was found to be -0.829 kJ/mol and -1.85 kJ/mol, respectively, which indicates the spontaneous nature of sorption process. Other thermodynamic parameters such as entropy change (ΔS o ), enthalpy (ΔH o )and activation energy (ΔE) were found to be 0.604 J mol -1 K -1 , -186.95 kJ/mol and 68.53 kJ/mol, respectively for Cu(II) and 0.397 J mol -1 K -1 , -119.79 kJ/mol and 114.45 kJ/mol, respectively for Cr(III). The main novelty of this work was the determination of shortest possible sorption time for Cu(II) and Cr(III) in comparison to earlier studies. Almost over 98% of Cu(II) and Cr(III) were removed in only first 20 min at an initial concentration of 100 mg/L

  17. Constituting fully integrated visual analysis system for Cu(II) on TiO₂/cellulose paper.

    Science.gov (United States)

    Li, Shun-Xing; Lin, Xiaofeng; Zheng, Feng-Ying; Liang, Wenjie; Zhong, Yanxue; Cai, Jiabai

    2014-07-15

    As a cheap and abundant porous material, cellulose filter paper was used to immobilize nano-TiO2 and denoted as TiO2/cellulose paper (TCP). With high adsorption capacity for Cu(II) (more than 1.65 mg), TCP was used as an adsorbent, photocatalyst, and colorimetric sensor at the same time. Under the optimum adsorption conditions, i.e., pH 6.5 and 25 °C, the adsorption ratio of Cu(II) was higher than 96.1%. Humic substances from the matrix could be enriched onto TCP but the interference of their colors on colorimetric detection could be eliminated by the photodegradation. In the presence of hydroxylamine, neocuproine, as a selective indicator, was added onto TCP, and a visual color change from white to orange was generated. The concentration of Cu(II) was quantified by the color intensity images using image processing software. This fully integrated visual analysis system was successfully applied for the detection of Cu(II) in 10.0 L of drinking water and seawater with a preconcentration factor of 10(4). The log-linear calibration curve for Cu(II) was in the range of 0.5-50.0 μg L(-1) with a determination coefficient (R(2)) of 0.985 and its detection limit was 0.073 μg L(-1).

  18. Estudo da estabilidade do complexo ácido fítico e o íon Ni(II Study of stability of phytic acid with Ni(II complex

    Directory of Open Access Journals (Sweden)

    Ligia De Carli

    2006-03-01

    Full Text Available A técnica de titulação potenciométrica foi utilizada para verificar as propriedades ácida-base do ácido fítico [1,2,3,4,5,6-hexaquis(dihidrogenofosfato-mio-inositol] e do complexo ácido fítico e Ni(II, em solução aquosa, em temperatura e força iônica constantes. Para avaliar o comportamento térmico e a complexação do ácido fítico com o íon Ni(II foram realizadas análises de Termogravimetria (TG, Termogravimetria Derivada (DTG, Calorimetria Exploratória Diferencial (DSC e estudos de Espectrofotometria de Infravermelho. Foram obtidas oito constantes de protonação da amostra de ácido fítico na forma de sal de dipotássio e sete constantes de estabilidade do complexo ácido fítico e Ni(II. As reações de protonação e de formação ocorrem na faixa de pH de 2,0 a 11,0. Os dados obtidos mostram que o ácido fítico encontra-se totalmente deprotonado em pH 12,0 no qual a espécie ML (um ligante para um íon metálico encontra-se totalmente formada no mesmo valor de pH. Os resultados obtidos por TG e DSC revelaram tanto para o ácido fítico como para o complexo boa estabilidade até a temperatura próxima a 200ºC. Por TG, DTG e DSC conclui-se também que a estequiometria do complexo estudado foi de um mol de ligante para um mol de íon metálico. A Espectrofotometria de Infravermelho comprovou a estabilidade do ácido fítico e a sua interação com o íon Ni(II.The technique of potenciometric titration was used to verify the acid-basic properties of the phytic acid, [1,2,3,4,5,6-hexakis(dihydrogen phosphate-myo-inositol] and the Phytic Acid-Ni(II complex, in aqueous solution, in constant temperature and ionic strength. To evaluate the thermal behavior end complexation of the isolated phytic acid with the Ni(II were performed analyses of thermogravimetry (TG, calorimetric scanning differential (DSC and studies Spectroscopy Infrared (IR. Eight protonation constants of the phytic acid sample as dipotassium salt were

  19. Quinonoid functionality redox properties Diiminic functionality Lewis ...

    African Journals Online (AJOL)

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    there is a 2:1 stoichiometry between ligand with studied metalic cations and ... biological chemistry [5], and in the synthesis of materials showing interesting optical or ... metallic cations [Cu(II), Ni(II), Co(II), Zn(II)] have been studied using UV–Vis ... where D is a matrix, the rows of which are formed by the absorption spectra ...

  20. Antibacterial activity of cobalt(II complexes with some benzimidazole derivatives

    Directory of Open Access Journals (Sweden)

    S. O. PODUNAVAC-KUZMANOVIC

    2008-12-01

    Full Text Available The antibacterial activities of cobalt(II complexes with two series of benzimidazoles were evaluated in vitro against three Gram-positive bacterial strains (Bacillus cereus, Staphylococcus aureus, and Sarcina lutea and one Gram-negative isolate (Pseudomonas aeruginosa. The minimum inhibitory concentration was determined for all the complexes. The majority of the investtigated complexes displayed in vitro inhibitory activity against very persistent bacteria. They were found to be more active against Gram-positive than Gram-negative bacteria. It may be concluded that the antibacterial activity of the compounds is related to the cell wall structure of the tested bacteria. Comparing the inhibitory activities of the tested complexes, it was found that the 1-substituted-2-aminobenzimidazole derivatives were more active than complexes of 1-substituted-2-amino-5,6-dimethylbenzimidazoles. The effect of chemical structure on the antibacterial activity is discussed.

  1. Degradation of TCE by TEOS Coated nZVI in the Presence of Cu(II) for Groundwater Remediation

    International Nuclear Information System (INIS)

    Ramamurthy, A.S.; Eglal, M.M.

    2014-01-01

    The removal of TCE by nanofer zero valent iron (nanofer ZVI) coated with tetraethyl orthosilicate (TEOS) in the presence of Cu(II) at different environmental conditions was studied. The kinetics of TCE degradation by nanofer ZVI was determined. At a dosage of 10 mg of nanofer ZVI, almost 63% of TCE was removed, when Cu(II) and TCE were present. It contrasts with 42% degradation of TCE in the absence of Cu(II). SEM/EDS images indicated that Cu(II) is reduced to form Cu 0 and Cu 2 O. These formations are considered to be responsible for enhancing TCE degradation. Direct reduction involves hydrogenolysis and β-elimination in the transformation of TCE, while indirect reduction involves atomic hydrogen and no direct electron transfer from the metal to reactants. The reduction of activation energy was also noted indicating that the rate limiting step for TCE degradation in the presence of Cu(II) is surface chemical reaction rather than diffusion. Most of iron present in nanofer ZVI get dissolved causing the generation of localized positive charge regions and form metal chlorides. Local accumulation of hydrochloric acid inside the pits regenerates new reactive surfaces to serve as sources of continuous electron generation. No significant effect of TCE was noticed for Cu(II) sequestration.

  2. Recovery of Cd(II), Co(II) and Ni(II) from Chloride Medium by Solvent Extraction Using CYANEX 923 and CYANEX 272 I

    International Nuclear Information System (INIS)

    Ahmed, M.; El Dessouky, S.I.; El-Nadi, Y.A.; Daoud, J.A.; Saad, E.A.

    2008-01-01

    The paper aims to study the extraction and separation of Cd(II), Co(II) and Ni(II) from their mixtures in hydrochloric acid medium with CYANEX 923 in kerosene. Preliminary investigations showed that only Cd(II) is extracted with CYANEX 923 while Co(II) and Ni(II) are not extracted. Different parameters affecting the extraction of Cd(II) with CYANEX 923 such as hydrochloric acid, hydrogen ion, extractant and metal concentrations, temperature investigations were also investigated. The stoichiometry of the extracted metal species investigated was found to be HCdCl 3 . 2 CYANEX 923. The stripping of the extracted Cd(II) species is obtained with 0.1 M HCl solution. Co(II) was found to be extracted with CYANEX 272 at ph 5.8 leaving Ni(II) in the solution. A developed process for the sequential of Cd(II), Co(II) and Ni(II) from their mixture in hydrochloric acid medium is proposed

  3. Preparation and characterization of Schiff base Cu(II) complex and its applications on textile materials

    Science.gov (United States)

    Oylumluoglu, G.; Oner, J.

    2017-10-01

    Schiff base ligands are regarded as an important class of organic compounds on account of the fact that their complexation ability with transition metal ions. A new monomeric Schiff base Cu(II) complex, [Cu(HL)2], 1 [H2L = 2-((E)-(2-hydroxypropylimino)methyl)-4-nitrophenol] has been synthesized and characterized by elemental analysis, UV and IR spectroscopy, single crystal X-ray diffraction and photoluminescence study. While the Schiff base ligand and its Cu(II) complex are excited at λex = 349 nm in UV region, the Schiff base ligand shows a blue emission band at λmax = 480 nm whereas its Cu(II) complex shows a strong green emission band at λmax = 520 nm in the solid state at room temperature. The luminescent properties showed that the Schiff base ligand and its Cu(II) complex can be used as novel potential candidates for applications in textile such as UV-protection, antimicrobial, laundry and functional bleaching treatments.

  4. Spectral studies of coordination compounds of cobalt(II) with thiosemicarbazone of heterocyclic ketone

    Science.gov (United States)

    Chandra, Sulekh; Kumar, Umendra

    2005-12-01

    The paper presents the spectral analysis of cobalt(II) complexes with indoxyl thiosemicarbazone (ITSC) of general composition [CoL 2X 2] (where L = ITSC, X = Cl -, NO 3-, (1/2)SO 42-, NCS -). The geometry of the complexes have been characterized by elemental analysis, molar conductance, magnetic susceptibility measurements and spectral (electronic, IR, EPR, 1H NMR, mass) studies. The various physico-chemical techniques suggested a coordination number of six (octahedral) for chloro, nitrato and thiocyanato complexes. Whereas sulfato complex was found to have five coordinate trigonal-bipyramidal geometry. All the complexes are of high spin type showing magnetic moment corresponding to three unpaired electrons.

  5. Direct Observation of Reduction of Cu(II) to Cu(I) by Terminal Alkynes

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Guanghui; Yi, Hong; Zhang, Guoting; Deng, Yi; Bai, Ruopeng; Zhang, Heng; Miller, Jeffrey T.; Kropf, Arthur J.; Bunel, Emilio E.; Lei, Aiwen

    2014-01-06

    ABSTRACT: X-ray absorption spectroscopy and in situ electron paramagnetic resonance evidence were provided for the reduction of Cu(II) to Cu(I) species by alkynes in the presence of tetramethylethylenediamine (TMEDA), in which TMEDA plays dual roles as both ligand and base. The structures of the starting Cu(II) species and the obtained Cu(I) species were determined as (TMEDA)- CuCl2 and [(TMEDA)CuCl]2 dimer, respectively.

  6. Sensitive and selective detection of Cu(II) ion: A new effective 1,8-naphthalimide-based fluorescence 'turn off' sensor.

    Science.gov (United States)

    Huang, Guozhen; Li, Chuang; Han, Xintong; Aderinto, Stephen Opeyemi; Shen, Kesheng; Mao, Shanshan; Wu, Huilu

    2018-06-01

    The present study reports the development of a new 1,8-naphthalimide-based fluorescent sensor V for monitoring Cu(II) ions. The sensor exhibited pH independence over a wide pH range 2.52-9.58, and indicated its possible use for monitoring Cu(II) ions in a competitive pH medium. The sensor also showed high selectivity and sensitivity towards the Cu(II) ions over other competitive metal ions in DMSO-HEPES buffer (v/v, 1:1; pH 7.4) with a fluorescence 'turn off' mode of 79.79% observed. A Job plot indicated the formation of a 1:1 binding mode of the sensor with Cu(II) ions. The association constant and detection limit were 1.14 × 10 6  M -1 and 4.67 × 10 -8 M, respectively. The fluorescence spectrum of the sensor was quenched due to the powerful paramagnetic nature of the Cu(II) ions. Potential application of this sensor was also demonstrated when determining Cu(II) ion levels in two different water samples. Copyright © 2018 John Wiley & Sons, Ltd.

  7. Utilization of m-Phenylenediamine-Furfural Resin for Removal of Cu(II from Aqueous Solution-A Thermodynamic Study

    Directory of Open Access Journals (Sweden)

    Tariq S. Najim

    2010-01-01

    Full Text Available m-Phenylenediamine was condensed with furfural in absence of catalyst at room temperature. The produced m-phenylenediamine-furfural resin was used for the removal of Cu(II from aqueous solution. The pH for the optimum removal of Cu(II was 6. The negative values of Gibbs free energy at low concentration of Cu(II (20, 30 ppm indicative of the spontaneous adsorption process, while, at higher Cu(II concentration (40,50 ppm the positive and weak values of ∆G° indicate that the process is feasible but non spontaneous. The values of ∆H° were positive indicating that the sorption process is endothermic. On the other hand, the values of activation energy (Ea were inconsistent with the values of ∆H° both are positive and lie in the range of physisorption. The entropy ∆S° of the process was positive indicative of the randomness of the Cu(II ions at the solid / liquid interface. The values of sticking probability S* were less than one which indicate a preferable adsorption process and the mechanism is physisorption.

  8. Thermodynamic model of Ni(II) solubility, hydrolysis and complex formation with ISA

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez-Siso, Maria Rosa; Duro, Lara; Bruno, Jordi [Amphos21, Barcelona (Spain); Gaona, Xavier; Altmaier, Marcus [Karlsruhe Institute of Technology (KIT), Karlsruhe (Germany). Inst. for Nuclear Waste Disposal

    2018-04-01

    The solubility of β-Ni(OH){sub 2}(cr) was investigated at T=(22±2) C in the absence and presence of α-isosaccharinic acid (ISA), the main degradation product of cellulose under alkaline pH conditions. Batch solubility experiments were performed from undersaturation conditions under inert gas (Ar) atmosphere. Solubility experiments in the absence of ISA were conducted in 0.5 and 3.0 M NaCl-NaOH solutions at 7.5 ≤ pH{sub m} ≤ 13 (with pH{sub m} = -log{sub 10}[H{sup +}]). XRD analyses of selected solid phases collected after completing the solubility experiments (∼300 days) confirmed that β-Ni(OH){sub 2}(cr) remains as solid phase controlling the solubility of Ni(II) in all investigated conditions. Based on the slope analysis (log{sub 10}[Ni] vs. pH{sub m}) of the solubility data and solid phase characterization, the equilibrium reactions β-Ni(OH){sub 2}(cr)+2 H{sup +} <=> Ni{sup 2+}+2 H{sub 2}O(l) and β-Ni(OH){sub 2}(cr) <=> Ni(OH){sub 2}(aq) were identified as controlling the solubility of Ni(II) within the investigated pH{sub m} region. The conditional equilibrium constants determined from the solubility experiments at different ionic strengths were evaluated with the specific ion interaction theory (SIT). In contrast to the current thermodynamic selection in the NEA-TDB, solubility data collected in the present work does not support the formation of the anionic hydrolysis species Ni(OH){sub 3}{sup -} up to pH{sub m} ≤ 13.0. Solubility experiments in the presence of ISA were conducted in 0.5 M NaCl-NaOH-NaISA solutions with 0.01 M ≤ [NaISA] ≤ 0.2 M and 9 ≤ pH{sub m} ≤ 13. XRD analyses confirmed that β-Ni(OH){sub 2}(cr) is also the solid phase controlling the solubility of Ni(II) in the presence of ISA. Solubility data of all investigated systems can be properly explained with chemical and thermodynamic models including the formation of the complexes NiOHISA(aq), Ni(OH){sub 2}ISA{sup -} and Ni(OH){sub 3}ISA{sup 2-}. The reported data confirm

  9. Syntheses, crystal structures and Hirshfeld surface analysis of a coordination polymer of Cu(II) chlorido and a tris-octahedral complex of Ni(II) containing isonicotinoylhydrazone blockers

    Science.gov (United States)

    Mahmoudi, Ghodrat; Chowdhury, Habibar; Ghosh, Barindra K.; Lofland, Samuel E.; Maniukiewicz, Waldemar

    2018-05-01

    One-pot reactions of pre-assigned molar ratios of appropriate metal (II) salts and HL1 (2-acetylpyridine nicotinoylhydrazone) or HL2 (2-acetylpyridine isonicotinoylhydrazone) in MeOH solutions at room temperature afford 1D coordination polymeric chain [Cu(μ-L1) (Cl)]n (1) and a mononuclear complex [Ni(L2)2] (2). The compounds (1) and (2) were characterized using elemental analyses, spectral and other physicochemical methods. Single crystal X-ray diffraction measurements for (1) and (2) have been made to define the molecular aggregates and crystalline architectures. In (1), each copper (II) center adopts a distorted square pyramidal geometry with a CuN3OCl chromophore linked through μ-L1 to form the 1D polymeric chain. While in (2) each Ni(II) cation is six-coordinate with octahedral structure having NiN4O2 chromophore containing two L2 units each functioning as a classical tridentate (N,N,O) chelator. Different weak non-covalent interactions promote dimensionalities in the compounds. A Hirshfeld surface analysis was employed to gain additional insight into interactions responsible for packing of (1) and (2). Magnetic susceptibility measurement of (1) in the 4-300 K range reveals simple paramagnetism.

  10. Complex Formation in a Liquid-Liquid Extraction System Containing Cobalt(II), 4-(2-Pyridylazo)resorcinol, and Nitron

    OpenAIRE

    Racheva, Petya Vassileva; Gavazov, Kiril Blazhev; Lekova, Vanya Dimitrova; Dimitrov, Atanas Nikolov

    2013-01-01

    Complex formation and liquid-liquid extraction were studied in a system containing cobalt(II), 4-(2-pyridylazo)resorcinol (PAR), 1,4-diphenyl-3-(phenylamino)-1H-1,2,4-triazole (Nitron, Nt), water, and chloroform. The effect of some experimental parameters (pH, shaking time, concentration of PAR, and concentration of Nt) was systematically investigated, and the optimum conditions for cobalt extraction as an ion-association complex, (NtH+)[Co3+(PAR)2], were found. The following key equilibrium ...

  11. Glutamate Ligation in the Ni(II)- and Co(II)-Responsive Escherichia coli Transcriptional Regulator, RcnR

    Energy Technology Data Exchange (ETDEWEB)

    Carr, Carolyn E. [Department of Chemistry, University of Massachusetts, Amherst, Massachusetts 01003, United States; Musiani, Francesco [Laboratory; Huang, Hsin-Ting [Department of Chemistry, University of Massachusetts, Amherst, Massachusetts 01003, United States; Chivers, Peter T. [Departments of Biosciences and Chemistry, Durham University, Durham DH1 3LE, United Kingdom; Ciurli, Stefano [Laboratory; Maroney, Michael J. [Department of Chemistry, University of Massachusetts, Amherst, Massachusetts 01003, United States

    2017-05-18

    Escherichia coli RcnR (resistance to cobalt and nickel regulator, EcRcnR) is a metal-responsive repressor of the genes encoding the Ni(II) and Co(II) exporter proteins RcnAB by binding to PRcnAB. The DNA binding affinity is weakened when the cognate ions Ni(II) and Co(II) bind to EcRcnR in a six-coordinate site that features a (N/O)5S ligand donor-atom set in distinct sites: while both metal ions are bound by the N terminus, Cys35, and His64, Co(II) is additionally bound by His3. On the other hand, the noncognate Zn(II) and Cu(I) ions feature a lower coordination number, have a solvent-accessible binding site, and coordinate protein ligands that do not include the N-terminal amine. A molecular model of apo-EcRcnR suggested potential roles for Glu34 and Glu63 in binding Ni(II) and Co(II) to EcRcnR. The roles of Glu34 and Glu63 in metal binding, metal selectivity, and function were therefore investigated using a structure/function approach. X-ray absorption spectroscopy was used to assess the structural changes in the Ni(II), Co(II), and Zn(II) binding sites of Glu → Ala and Glu → Cys variants at both positions. The effect of these structural alterations on the regulation of PrcnA by EcRcnR in response to metal binding was explored using LacZ reporter assays. These combined studies indicate that while Glu63 is a ligand for both metal ions, Glu34 is a ligand for Co(II) but possibly not for Ni(II). The Glu34 variants affect the structure of the cognate metal sites, but they have no effect on the transcriptional response. In contrast, the Glu63 variants affect both the structure and transcriptional response, although they do not completely abolish the function of EcRcnR. The structure of the Zn(II) site is not significantly perturbed by any of the glutamic acid variations. The spectroscopic and functional data obtained on the mutants were used to calculate models of the metal-site structures of EcRcnR bound to Ni(II), Co(II), and Zn(II). The results are interpreted

  12. Adsorption of As(III), As(V) and Cu(II) on zirconium oxide immobilized alginate beads in aqueous phase.

    Science.gov (United States)

    Kwon, Oh-Hun; Kim, Jong-Oh; Cho, Dong-Wan; Kumar, Rahul; Baek, Seung Han; Kurade, Mayur B; Jeon, Byong-Hun

    2016-10-01

    A composite adsorbent to remove arsenite [As(III)], arsenate [As(V)], and copper [Cu(II)] from aqueous phase was synthesized by immobilizing zirconium oxide on alginate beads (ZOAB). The composition (wt%) of ZOAB (Zr-34.0; O-32.7; C-21.3; Ca-1.0) was confirmed by energy dispersive X-ray (EDX) analysis. Sorption studies were conducted on single and binary sorbate systems, and the effects of contact time, initial adsorbate concentration, and pH on the adsorption performance of ZOAB (pHPZC = 4.3) were monitored. The sorption process for As(III)/As(V) and Cu(II) reached an equilibrium state within 240 h and 24 h, respectively, with maximum sorption capacities of 32.3, 28.5, and 69.9 mg g(-1), respectively. The addition of Cu(II) was favorable for As(V) sorption in contrast to As(III). In the presence of 48.6 mg L(-1) Cu(II), the sorption capacity of As(V) increased from 1.5 to 3.8 mg g(-1) after 240 h. The sorption data for As(III)/As(V) and Cu(II) conformed the Freundlich and Langmuir isotherm models, respectively. The adsorption of As(III), As(V), and Cu(II) followed pseudo second order kinetics. The effect of arsenic species on Cu(II) sorption was insignificant. The results of present study demonstrated that the synthesized sorbent could be useful for the simultaneous removal of both anionic and cationic contaminants from wastewaters. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Experiment, modeling and optimization of liquid phase adsorption of Cu(II) using dried and carbonized biomass of Lyngbya majuscula

    Science.gov (United States)

    Kushwaha, Deepika; Dutta, Susmita

    2017-05-01

    The present work aims at evaluation of the potential of cyanobacterial biomass to remove Cu(II) from simulated wastewater. Both dried and carbonized forms of Lyngbya majuscula, a cyanobacterial strain, have been used for such purpose. The influences of different experimental parameters viz., initial Cu(II) concentration, solution pH and adsorbent dose have been examined on sorption of Cu(II). Kinetic and equilibrium studies on Cu(II) removal from simulated wastewater have been done using both dried and carbonized biomass individually. Pseudo-second-order model and Langmuir isotherm have been found to fit most satisfactorily to the kinetic and equilibrium data, respectively. Maximum 87.99 and 99.15 % of Cu(II) removal have been achieved with initial Cu(II) concentration of 10 and 25 mg/L for dried and carbonized algae, respectively, at an adsorbent dose of 10 g/L for 20 min of contact time and optimum pH 6. To optimize the removal process, Response Surface Methodology has been employed using both the dried and carbonized biomass. Removal with initial Cu(II) concentration of 20 mg/L, with 0.25 g adsorbent dose in 50 mL solution at pH 6 has been found to be optimum with both the adsorbents. This is the first ever attempt to make a comparative study on Cu(II) removal using both dried algal biomass and its activated carbon. Furthermore, regeneration of matrix was attempted and more than 70% and 80% of the adsorbent has been regenerated successfully in the case of dried and carbonized biomass respectively upto the 3rd cycle of regeneration study.

  14. Syntheses and characterizations of the cyanide-bridged ...

    African Journals Online (AJOL)

    The spectral features of the complexes suggest that the Ni(II) ion is four coordinate with four cyanide-carbon atoms in a square planar geometry, whereas the Cu(II) and the Zn(II) ions of the Cu–Ni–etim and the Zn–Ni–etim complexes are completed by nitrogen atoms of two cyano groups of [Ni(CN)4]2- coordinated to the ...

  15. Synthesis and Characterization of Some Macrocylic Complexes Incorporating Indole and 2,2'-Bipyridine or 1,10-Phenanthroline

    Directory of Open Access Journals (Sweden)

    Muhammad S. Khan

    2015-06-01

    Full Text Available Complexes of anionic pentadentate macrocyclic ligands by the template condensation of bis(hydrazino2,2'-bipyridine or 1,10-phenanthroline with an indoledialdehyde have been synthesized. The new Mn(II, Fe(II, Co(II, Ni(II, Cu(II and Zn(II macrocyclic complexes have been characterized by analytical and spectroscopic techniques and by conductivity and magnetic susceptibility measurements.

  16. Synthesis, spectroscopic and redox properties of the mononuclear

    Indian Academy of Sciences (India)

    In the trinuclear CuII-NiII-CuII metal complexes, the NiII ion centered into the main oxime core by the coordination of the imino groups while the two CuII ions coordinate dianionic oxygen donors of the oxime groups and linked to the ligands of 1,10-phenanthroline, 2,2'-bipyridine, and 4,4'-bipyridine. The ligand and their ...

  17. One electron reduction of 1,2 dihydroxy 9,10 anthraquinone and its transition metal complexes in aqueous-isopropanol-acetone mixed solvent: a steady state-state and pulse radiolysis study

    International Nuclear Information System (INIS)

    Das, Saurabh; Mandal, Parikshit C.; Rath, Madhab C.; Mukherjee, Tulsi

    1998-01-01

    One electron reduction of 1,2 dihydroxy 9,10 anthraquinone and its Cu(II) and Ni(II) and Fe(III) complexes have been studied in aqueous-isopropanol-acetone solvent. Results indicate that the reducing ketyl radical generated reacts with the ligand forming semiquinones which undergoes a disproportionation reaction. Formation and decay rates of semiquinones was calculated using pulse radiolysis. (author)

  18. Kinetic study on adsorption of Cr(VI), Ni(II), Cd(II) and Pb(II) ions from aqueous solutions using activated carbon prepared from Cucumis melo peel

    Science.gov (United States)

    Manjuladevi, M.; Anitha, R.; Manonmani, S.

    2018-03-01

    The adsorption of Cr(VI), Ni(II), Cd(II) and Pb(II), ions from aqueous solutions by Cucumis melo peel-activated carbon was investigated under laboratory conditions to assess its potential in removing metal ions. The adsorption behavior of metal ions onto CMAC was analyzed with Elovich, intra-particle diffusion rate equations and pseudo-first-order model. The rate constant of Elovich and intra-particle diffusion on CMAC increased in the sequence of Cr(VI) > Ni(II) > Cd(II) > Pb(II). According to the regression coefficients, it was observed that the kinetic adsorption data can fit better by the pseudo-first-order model compared to the second-order Lagergren's model with R 2 > 0.957. The maximum adsorption of metal ions onto the CMAC was found to be 97.95% for Chromium(VI), 98.78% for Ni(II), 98.55% for Pb(II) and 97.96% for Cd(II) at CMAC dose of 250 mg. The adsorption capacities followed the sequence Ni(II) ≈ Pb(II) > Cr(VI) ≈ Cd(II) and Ni(II) > Pb(II) > Cd(II) > Cr(VI). The optimum adsorption conditions selected were adsorbent dosage of 250 mg, pH of 3.0 for Cr(VI) and 6.0 for Ni(II), Cd(II) and Pb(II), adsorption concentration of 250 mg/L and contact time of 180.

  19. Selective and sensitized spectrophotometric determination of trace amounts of Ni(II) ion using α-benzyl dioxime in surfactant media

    Science.gov (United States)

    Ghaedi, Mehrorang

    2007-02-01

    Highly sensitive and interference-free sensitized spectrophotometric method for the determination of Ni(II) ions is described. The method is based on the reaction between Ni(II) ion and benzyl dioxime in micellar media in the presence of sodium dodecyl sulfate (SDS). The absorbance is linear from 0.1 up to 25.0 μg mL -1 in aqueous solution with repeatability (RSD) of 1.0% at a concentration of 1 μg mL -1 and a detection limit of 0.12 ng mL -1 and molar absorption coefficient of 68,600 L mol -1 cm -1. The influence of reaction variables including type and amount of surfactant, pH, and amount of ligand and complexation time and the effect of interfering ions are investigated. The proposed procedure was applied to the determination of trace amounts of Ni(II) ion in tap water, river water, chocolate and vegetable without separation or organic solvent extraction.

  20. A new one-dimensional NiII coordination polymer with a two-dimensional supramolecular architecture

    Directory of Open Access Journals (Sweden)

    Kai-Long Zhong

    2017-02-01

    Full Text Available A new one-dimensional NiII coordination polymer of 1,3,5-tris(imidazol-1-ylmethylbenzene, namely catena-poly[[aqua(sulfato-κOhemi(μ-ethane-1,2-diol-κ2O:O′[μ3-1,3,5-tris(1H-imidazol-1-ylmethylbenzene-κ3N3,N3′,N3′′]nickel(II] ethane-1,2-diol monosolvate monohydrate], {[Ni(SO4(C18H18N6(C2H6O20.5(H2O]·C2H6O2·H2O}n, was synthesized and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The NiII cation is coordinated by three N atoms of three different 1,3,5-tris(imidazol-1-ylmethylbenzene ligands, one O atom of an ethane-1,2-diol molecule, by a sulfate anion and a water molecule, forming a distorted octahedral NiN3O3 coordination geometry. The tripodal 1,3,5-tris(imidazol-1-ylmethylbenzene ligands link the NiII cations, generating metal–organic chains running along the [100] direction. Adjacent chains are further connected by O—H...O hydrogen bonds, resulting in a two-dimensional supermolecular architecture running parallel to the (001 plane. Another water molecule and a second ethane-1,2-diol molecule are non-coordinating and are linked to the coordinating sulfate ions via O—H...O hydrogen bonds.

  1. Study on the adsorption of Cu(II) by folic acid functionalized magnetic graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Cuicui [Shandong Provincial Key Laboratory of Preparation and Measurement of Building Materials, University of Jinan, Jinan 250022 (China); School of Material Science and Engineering, University of Jinan, Jinan 250022 (China); Ge, Heyi, E-mail: geheyi@sina.com [Shandong Provincial Key Laboratory of Preparation and Measurement of Building Materials, University of Jinan, Jinan 250022 (China); School of Material Science and Engineering, University of Jinan, Jinan 250022 (China); Zhao, Yueying [Shandong Xiaguang Industrial Co., Ltd., Jining 272000 (China); Liu, Shanshan; Zou, Yu; Zhang, Wenbo [Shandong Provincial Key Laboratory of Preparation and Measurement of Building Materials, University of Jinan, Jinan 250022 (China); School of Material Science and Engineering, University of Jinan, Jinan 250022 (China)

    2017-02-01

    The folic acid functionalized magnetic graphene oxide (FA-mGO) as a new adsorbent has been synthesized in this work for the elimination of Cu(II) from waste water. The as-prepared FA-mGO was tested by SEM, TEM, particle size analyzer, FTIR, XRD, Roman spectrum, TGA and magnetic properties analyzer. Some factors, such as adsorbent dose, pH, contact time, initial concentration of adsorbate and temperature were explored. The results showed that the FA-mGO had the better adsorption performance than mGO. After 40 min, the adsorption equilibrium could be reached. Furthermore, the adsorption property obeyed the pseudo-second order kinetic model and the Temkin isotherms well. The maximum adsorption capacity was 283.29 mg/g for Cu(II) from Pseudo-second-order model at pH=5 and 318 K. The chelation action between FA and Cu(II) along with electrostatic incorporation between GO and Cu(II) determined the favourable adsorption property. Besides, thermodynamic studies results ∆G{sup 0}<0, ∆H{sup 0}>0, ∆S{sup 0}>0 suggested that the adsorption mechanism was an endothermic and spontaneous process essentially. Finally, desorption and reusability studies imply FA-mGO has an excellent reproducibility and is benefit to environmental protection and resource conservation. - Graphical abstract: Schematic illustration of preparing FA-mGO. - Highlights: • The FA-mGO was synthesized for the removal of Cu(II). • The chelation action and electrostatic incorporation determined the favourable adsorption property. • The adsorption property obeyed the pseudo-second-order and Temkin models well. • The adsorption mechanism was an endothermic and spontaneous process. • The FA-mGO has an excellent reproducibility.

  2. Three novel metal-organic frameworks based on flexible porphyrin tetracarboxylic acids as highly effective catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Zengqi [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry & Materials Science, Northwest University, Xi’an, Shaanxi 710069 (China); Su, Xiaoqin [School of Materials and Chemical Engineering, Xi’an Technological University, Xi’an, Shaanxi 710021 (China); Yu, Fan; Li, Jun [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry & Materials Science, Northwest University, Xi’an, Shaanxi 710069 (China)

    2016-06-15

    Targeted synthesis of metalloporphyrinic frameworks (MPFs) with Cu(II) (1), Ni(II) (2, 3) 5, 10, 15, 20-tetrakis[4-(carboxymethyleneoxy)phenyl]porphyrin (Cu(TCMOPP) and Ni(TCMOPP)) as building blocks afforded three new extended coordination polymers inter-linked by Zn(II) (1) and K(I) (2, 3). 1 shows 2D frameworks while 2, 3 are 3D frameworks. The open channel are 7–17 Å wide and accessible to guest/solvent molecules. Besides, the thermogravimetric analyses (TGA) indicate that the framework structures of the three compounds are stable until 300 °C. In addition, the catalytic activities of 1–3 to the alkylbenzenes oxidation are examined, and the results indicate that 1 exhibit high catalytic activity to oxidation of ethylbenzene and 1,2,3,4-tetrahydronaphthalene with conversion of 64.1% and 80.3% respectively. - Graphical abstract: Three novel metalloporphyrinic frameworks (1, 2, 3) were synthesized based on tetracarboxylic Cu(II) (1), Ni(II) (2, 3) metalloporphyrin inter-linked by Zn(II) (1) , K(I) (2, 3), and 1 shows high catalytic activity to oxidation reaction of alkylbenzenes with conversion 80.3%. Display Omitted.

  3. Mixed ligand complexes of essential metal ions with L-glutamine and succinic acid in SLS-water mixtures

    Directory of Open Access Journals (Sweden)

    Bindu Hima Gandham

    2012-01-01

    Full Text Available Speciation of mixed ligand complexes of Co(II, Ni(II and Cu(II with L-glutamine and succinic acid was studied in varying amounts (0.0-2.5% w/v of sodium lauryl sulphate in aqueous solutions maintaining an ionic strength of 0.16 mol L-1 (NaCl at 303.0 K. Titrations were carried out in the presence of different relative concentrations (M : L : X = 1 : 2 : 2, 1 : 4 : 2, 1 : 2 : 4 of metal (M to L-glutamine (L to succinic acid (X with sodium hydroxide. Stability constants of ternary complexes were refined with MINIQUAD75. The best-fit chemical models were selected based on statistical parameters and residual analysis. The species detected were ML2X, MLX, MLXH and MLXH2 for Co(II, Ni(II and Cu(II. Extra stability of ternary complexes compared to their binary complexes was believed to be due to electrostatic interactions of the side chains of ligands, charge neutralization, chelate effect, stacking interactions and hydrogen bonding. The species distribution with pH at different compositions of SLS and plausible equilibria for the formation of species were also presented.

  4. STUDIES OF Ni(II) & Cu(II) COMPLEXES WITH AMPICILLIN

    African Journals Online (AJOL)

    akg

    Acidity measurements of organic compounds have a long history dating back to the end of the 19th century, when the ... is influenced by both the electronic effects of the substituents and the solvent effects of the medium. ... derivatives in water and organic solvent-water mixtures has been published so far [21-23]. There have ...

  5. STUDIES OF Ni(II) & Cu(II) COMPLEXES WITH AMPICILLIN

    African Journals Online (AJOL)

    akg

    dimethyl aniline with some acyl hydrazines. The product yield varied from ... distilled water and both solutions were kept in a preheated water bath at 30 - 50oC ... The para and meta substituted isomer were found to have higher yield than the ortho.

  6. STUDIES OF Ni(II) & Cu(II) COMPLEXES WITH AMPICILLIN

    African Journals Online (AJOL)

    akg

    Nigeria Journal of Chemical Research. Vol. 11, 2006. 37 ... b Rubber Research Institute of Nigeria, End-Use Division, P.M.B. 1049, Benin. City.Nigeria ... renewable biomaterial of photosynthesis, .... thought that this process accounts for the.

  7. STUDIES OF Ni(II) & Cu(II) COMPLEXES WITH AMPICILLIN

    African Journals Online (AJOL)

    akg

    ABSTRACT. The Kolo Creek E2.0 reservoir oils from the Nigerian Niger Delta region have been studied for molecular marker by characterisation using full scan GC-MS and GC-MS-MS transition from 412 → 369. An existing molecular marker compound normally found in coals and lignites has been observed in some these ...

  8. Synthesis and characterization of iron(III), manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) complexes of salicylidene-N-anilinoacetohydrazone (H2L1) and 2-hydroxy-1-naphthylidene-N-anilinoacetohydrazone (H2L2).

    Science.gov (United States)

    AbouEl-Enein, S A; El-Saied, F A; Kasher, T I; El-Wardany, A H

    2007-07-01

    Salicylidene-N-anilinoacetohydrazone (H(2)L(1)) and 2-hydroxy-1-naphthylidene-N-anilinoacetohydrazone (H(2)L(2)) and their iron(III), manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) complexes have been synthesized and characterized by IR, electronic spectra, molar conductivities, magnetic susceptibilities and ESR. Mononuclear complexes are formed with molar ratios of 1:1, 1:2 and 1:3 (M:L). The IR studies reveal various modes of chelation. The electronic absorption spectra and magnetic susceptibility measurements show that the iron(III), nickel(II) and cobalt(II) complexes of H(2)L(1) have octahedral geometry. While the cobalt(II) complexes of H(2)L(2) were separated as tetrahedral structure. The copper(II) complexes have square planar stereochemistry. The ESR parameters of the copper(II) complexes at room temperature were calculated. The g values for copper(II) complexes proved that the Cu-O and Cu-N bonds are of high covalency.

  9. Complexos metálicos com o herbicida glifosato: revisão

    OpenAIRE

    Coutinho,Cláudia F. B.; Mazo,Luiz Henrique

    2005-01-01

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature.

  10. Metallic complexes with glyphosate: a review

    OpenAIRE

    Coutinho, Cláudia F. B.; Mazo, Luiz Henrique

    2005-01-01

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature.

  11. Application of proton induced x-ray emission (PIXE) in estimation of trace metals entrapped in silica matrix

    International Nuclear Information System (INIS)

    Jal, P.K.; Patel, Sabita; Mishra, B.K.; Sudarshan, M.; Saha, A.

    2005-01-01

    Proton induced x-ray emission technique is used for multielemental analysis of metal ions adsorbed on nanosilica surface. At pH 3.5, silica traps uranium selectively from a mixture of solutions of 13 different metal ions viz., K(I), Ca(II), Fe(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Sr(II), Cd(II). Ba(II), Hg(II) and UO 2 (VI). (author)

  12. SYNTHESIS, CHARACTERIZATION AND ANTIMICROBIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    The synthesized chelating agent and metal(II) complexes were screened for ... Coordination compounds, Antimicrobial study ... The biological activity of Zn(II), Cu(II), Co(II) and Ni(II) with imidazole derivative (DIPO) ... product in 86% yield. .... [Ni(DIPO)Br2]. 2.0. 2.5. 2.5. 3.0. 3.0. 3.0. 9. Maxipime. 10.6. D iam eter o f in h ib itio.

  13. Removal of Cu(II) ions from contaminated waters using a conducting microfiltration membrane.

    Science.gov (United States)

    Wang, Xueye; Wang, Zhiwei; Chen, Haiqin; Wu, Zhichao

    2017-10-05

    Efficient removal of toxic metals using low-pressure membrane processes from contaminated waters is an important but challenging task. In the present work, a conducting microfiltration membrane prepared by embedding a stainless steel mesh in the active layer of a polyvinylidene fluoride membrane is developed to remove Cu(II) ions from contaminated waters. Results showed that the conducting membrane had favorable electrochemical properties and stability as cathode. Batch tests showed that Cu(II) removal efficiency increased with the increase of voltages and leveled off with the further enhancement of electric field. The optimal voltages were determined to be 1.0V and 2.0V for the influent Cu(II) concentrations of 5mg/L and 30mg/L, respectively. X-ray photoelectron spectroscopy and X-ray diffraction results demonstrated the presence of Cu(0) and Cu(OH) 2 on the membrane surface. The removal mechanisms involved the intrinsic adsorption of membrane, electrosorption of membrane, adsorption of deposited layer, chemical precipitation of Cu(OH) 2 and deposition of Cu(0) which were aided by electrophoresis and electrochemical oxidation-reduction. Long-term tests showed that the major contributors for Cu(II) removal were the deposition of Cu(0) by electrochemical reduction-oxidation (47.3%±8.5%) and chemical precipitation (41.1%±0.2%), followed by electrosorption, adsorption by the fouling layer and membrane intrinsic sorption. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Theoretical study of heavy metal Cd, Cu, Hg, and Ni(II) adsorption on the kaolinite(0 0 1) surface

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Jian, E-mail: zhaojian0209@aliyun.com [Institute of Applied Physics and Computational Mathematics, PO Box 8009, Beijing 100088 (China); State Key Laboratory of Geomechanics and Deep Underground Engineering, China University of Mining and Technology, Beijing 100083 (China); He, Man-Chao [State Key Laboratory of Geomechanics and Deep Underground Engineering, China University of Mining and Technology, Beijing 100083 (China)

    2014-10-30

    Highlights: • We investigated the adsorption of Cd, Cu, Hg, and Ni(II) on kaolinite(0 0 1) surface. • The adsorption capabilities of the kaolinite for HM atoms were Ni > Cu > Cd > Hg(II). • The adsorption energy increases with the coverage for Cd, Cu, and Hg(II) atoms. • The adsorption energy decreases with the coverage for Ni(II) atoms. - Abstract: Heavy metal pollution is currently of great concern because it has been recognized as a potential threat to air, water, and soil. Adsorption was one of the most popular methods for the removal of heavy metal. The adsorption of heavy metal Cd, Cu, Hg, and Ni(II) atoms on the hydroxylated (0 0 1) surface of kaolinite was investigated using density-functional theory within the generalized gradient approximation and a supercell approach. The coverage dependence of the adsorption structures and energetics were systematically studied for a wide range of coverage Θ [from 0.11 to 1.0 monolayers (ML)] and adsorption sites. The most stable among all possible adsorption sites for Cd(II) atom was the two-fold bridge site followed by the one-fold top site, and the top site was the most favorite adsorption site for Cu and Ni(II) atoms, while the three-fold hollow site was the most stable adsorption site for Hg(II) atom followed by the two-fold bridge site. The adsorption energy increases with the coverage for Cd, Cu, and Hg(II) atoms, thus indicating the higher stability of surface adsorption and a tendency to the formation of adsorbate islands (clusters) with increasing the coverage. However, the adsorption energy of Ni(II) atoms decreases when increasing the coverage. The adsorption capabilities of the kaolinite clay for the heavy metal atoms were in the order of Ni > Cu > Cd > Hg(II). The other properties of the Cd, Cu, Hg, and Ni(II)/kaolinite(0 0 1) system including the different charge distribution, the lattice relaxation, and the electronic density of states were also studied and discussed in detail.

  15. Theoretical study of heavy metal Cd, Cu, Hg, and Ni(II) adsorption on the kaolinite(0 0 1) surface

    International Nuclear Information System (INIS)

    Zhao, Jian; He, Man-Chao

    2014-01-01

    Highlights: • We investigated the adsorption of Cd, Cu, Hg, and Ni(II) on kaolinite(0 0 1) surface. • The adsorption capabilities of the kaolinite for HM atoms were Ni > Cu > Cd > Hg(II). • The adsorption energy increases with the coverage for Cd, Cu, and Hg(II) atoms. • The adsorption energy decreases with the coverage for Ni(II) atoms. - Abstract: Heavy metal pollution is currently of great concern because it has been recognized as a potential threat to air, water, and soil. Adsorption was one of the most popular methods for the removal of heavy metal. The adsorption of heavy metal Cd, Cu, Hg, and Ni(II) atoms on the hydroxylated (0 0 1) surface of kaolinite was investigated using density-functional theory within the generalized gradient approximation and a supercell approach. The coverage dependence of the adsorption structures and energetics were systematically studied for a wide range of coverage Θ [from 0.11 to 1.0 monolayers (ML)] and adsorption sites. The most stable among all possible adsorption sites for Cd(II) atom was the two-fold bridge site followed by the one-fold top site, and the top site was the most favorite adsorption site for Cu and Ni(II) atoms, while the three-fold hollow site was the most stable adsorption site for Hg(II) atom followed by the two-fold bridge site. The adsorption energy increases with the coverage for Cd, Cu, and Hg(II) atoms, thus indicating the higher stability of surface adsorption and a tendency to the formation of adsorbate islands (clusters) with increasing the coverage. However, the adsorption energy of Ni(II) atoms decreases when increasing the coverage. The adsorption capabilities of the kaolinite clay for the heavy metal atoms were in the order of Ni > Cu > Cd > Hg(II). The other properties of the Cd, Cu, Hg, and Ni(II)/kaolinite(0 0 1) system including the different charge distribution, the lattice relaxation, and the electronic density of states were also studied and discussed in detail

  16. Effective removal of Ni(II) from aqueous solutions by modification of nano particles of clinoptilolite with dimethylglyoxime.

    Science.gov (United States)

    Nezamzadeh-Ejhieh, Alireza; Kabiri-Samani, Mehdi

    2013-09-15

    In this work an Iranian natural clinoptilolite tuff was pre-treated and changed to the micro (MCP) and nano (NCP) particles by mechanical method. Modification of micro and nano particles and also their Ni-exchanged forms were done by dimethylglyoxime (DMG). The raw and modified samples were characterized by XRD, FT-IR, SEM, BET, TG-DTG and energy dispersive analysis X-ray spectroscopy (EDAX). Removal of Ni(II) by modified and unmodified samples was investigated in batch procedure. It was found that NCP-DMG has higher capacity for removal of Ni(II). The effects of analytical parameters such as pH, dose of DMG, concentration of nickel solution, contact time and selectivity were studied and the optimal operation parameters were found as follows: pHPZC: 7.6, CNi(II): 0.01 M, contact time: 360 min and DMG dosage: 5mM. The results of selectivity experiments showed that the modified zeolite has a good selectivity for nickel in the presence of different multivalent cations. Langmuir and Freundlich isotherm models were adopted to describe the adsorption isotherms. Adsorption isotherms of Ni(II) ions could be best modelled by Langmuir equation, that indicate the monolayer sorption of Ni(II). Comparison of two kinetic models indicates that the adsorption kinetic can be well described by the pseudo-second-order rate equation that indicates that the rate limiting step for the process involves chemical reaction. The negative ΔH and ΔG indicate an exothermic and spontaneously process. The negative ΔS indicates that the adsorption of nickel cations from solution occurs with lower amount ion replacement, thus chemisorptions due to complex formation are dominant process in nickel removal. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Cu(II) recognition materials: Fluorophores grafted on mesoporous silica supports

    International Nuclear Information System (INIS)

    Kledzik, Krzysztof; Orlowska, Maja; Patralska, Dorota; Gwiazda, Marcin; Jezierska, Julia; Pikus, Stanislaw; Ostaszewski, Ryszard; Klonkowski, Andrzej M.

    2007-01-01

    There were designed and synthesized naphthalene and pyrene derivatives consisting of fluorophore group and of receptor fragment with donor N and O atoms. These fluorosensors were covalently attached by grafting carboxyl group to surfaces of silica xerogel or mesoporous silicas (MCM-41 and MCM-48) functionalized either with 3-aminopropyl or 3-glycidoxypropyl groups. The pyrene derivatives 2 and 3 covalently grafted on MCM-48 silica functionalized with 3-aminopropyl groups are potential recognition elements of a fluorescence chemical sensor. Fluorescence emission of the prepared recognition materials is quenched specifically owing to photoinduced electron transfer (PET) effect after coordination reactions with Cu(II) ions. Moreover, both the materials exhibit selectivity for Cu(II) ions in aqueous solutions in presence of such metal ions as: alkali, alkaline earth and transition. During UV irradiation the studied recognition elements undergo slowly photochemical degradation

  18. Functionalization of mesoporous silica membrane with a Schiff base fluorophore for Cu(II) ion sensing

    Energy Technology Data Exchange (ETDEWEB)

    Chen Xiaotong [Department of Chemistry, Graduate School of Science, Tohoku University, Aoba-ku 980-8578, Sendai, Miyagi Prefecture (Japan); Department of Chemistry, Tsinghua University, Beijing 100084 (China); Yamaguchi, Akira [College of Science, Ibaraki University, Bunkyo 2-1-1, Mito, Ibaraki 310-8512 (Japan); Frontier Research Center for Applied Atomic Sciences, Ibaraki University, Tokai, Ibaraki 319-1106 (Japan); Namekawa, Manato [Department of Chemistry, Graduate School of Science, Tohoku University, Aoba-ku 980-8578, Sendai, Miyagi Prefecture (Japan); Kamijo, Toshio [Department of Chemistry, Graduate School of Science, Tohoku University, Aoba-ku 980-8578, Sendai, Miyagi Prefecture (Japan); Tsuruoka National College of Technology, Aza-Sawada, Tsuruoka 997-8511 (Japan); Teramae, Norio, E-mail: teramae@m.tohoku.ac.jp [Department of Chemistry, Graduate School of Science, Tohoku University, Aoba-ku 980-8578, Sendai, Miyagi Prefecture (Japan); Tong, Aijun, E-mail: tongaj@mail.tsinghua.edu.cn [Department of Chemistry, Tsinghua University, Beijing 100084 (China)

    2011-06-24

    Graphical abstract: Highlights: > A hybrid mesoporous membrane (SB-HMM) functionalized by Schiff base fluorophores was fabricated. > SB-HMM showed strong fluorescence with aggregation-induced emission enhancement properties. > SB-HMM was applicable for the detection of Cu(II) in an aqueous solution with good reversibility and reproducibility. - Abstract: A Schiff base (SB) immobilized hybrid mesoporous silica membrane (SB-HMM) was prepared by immobilizing a Schiff base onto the pore surface of mesoporous silica (pore size = 3.1 nm) embedded in the pores of a porous anodic alumina membrane. In contrast to the non-fluorescent analogous SB molecule in homogeneous solutions, SB-HMM exhibited intense fluorescence due to emission enhancement caused by aggregation of SB groups on the pore surface. The high quantum efficiency of the surface SB groups allows SB-HMM to function as a fluorescent sensor for Cu(II) ions in an aqueous solution with good sensitivity, selectivity and reproducibility. Under the optimal conditions described, the linear ranges of fluorescence intensity for Cu(II) are 1.2-13.8 (M (R{sup 2} = 0.993) and 19.4-60 (R{sup 2} = 0.992) (M. The limit of detection for Cu(II) is 0.8 {mu}M on basis of the definition by IUPAC (C{sub LOD} = 3.3S{sub b}/m).

  19. Solid phase selective separation and preconcentration of Cu(II) by Cu(II)-imprinted polymethacrylic microbeads.

    Science.gov (United States)

    Dakova, Ivanka; Karadjova, Irina; Ivanov, Ivo; Georgieva, Ventsislava; Evtimova, Bisera; Georgiev, George

    2007-02-12

    Ion-imprinted polymer (IIP) particles are prepared by copolymerization of methacrylic acid as monomer, trimethylolpropane trimethacrylate as crosslinking agent and 2,2'-azo-bis-isobutyronitrile as initiator in the presence of Cu(II), a Cu(II)-4-(2-pyridylazo)resorcinol (Cu(II)-PAR) complex, and PAR only. A batch procedure is used for the determination of the characteristics of the Cu(II) solid phase extraction from the IIP produced. The results obtained show that the Cu(II)-PAR IIP has the greatest adsorption capacity (37.4 micromol g(-1) of dry copolymer) among the IIPs investigated. The optimal pH value for the quantitative preconcentration is 7, and full desorption is achieved by 1 M HNO(3). The selectivity coefficients (S(Cu/Me)) for Me=Ni(II), Co(II) are 45.0 and 38.5, respectively. It is established that Cu(II)-PAR IIPs can be used repeatedly without a considerable adsorption capacity loss. The determination of Cu(II) ions in seawater shows that the interfering matrix does not influence the preconcentration and selectivity values of the Cu(II)-PAR IIPs. The detection and quantification limits are 0.001 micromol L(-1) (3sigma) and 0.003 micromol L(-1) (6sigma), respectively.

  20. Carbonato-bridged Ni(II)2Ln(III)2 (Ln(III) = Gd(III), Tb(III), Dy(III)) complexes generated by atmospheric CO2 fixation and their single-molecule-magnet behavior: [(μ4-CO3)2{Ni(II)(3-MeOsaltn)(MeOH or H2O)Ln(III)(NO3)}2]·solvent [3-MeOsaltn = N,N'-bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato].

    Science.gov (United States)

    Sakamoto, Soichiro; Fujinami, Takeshi; Nishi, Koshiro; Matsumoto, Naohide; Mochida, Naotaka; Ishida, Takayuki; Sunatsuki, Yukinari; Re, Nazzareno

    2013-06-17

    Atmospheric CO2 fixation of [Ni(II)(3-MeOsaltn)(H2O)2]·2.5H2O [3-MeOsaltn = N,N'-bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato], Ln(III)(NO3)3·6H2O, and triethylamine occurred in methanol/acetone, giving a first series of carbonato-bridged Ni(II)2Ln(III)2 complexes [(μ4-CO3)2{Ni(II)(3-MeOsaltn)(MeOH)Ln(III)(NO3)}2] (1Gd, 1Tb, and 1Dy). When the reaction was carried out in acetonitrile/water, it gave a second series of complexes [(μ4-CO3)2{Ni(II)(3-MeOsaltn)(H2O)Ln(III)(NO3)}2]·2CH3CN·2H2O (2Gd, 2Tb, and 2Dy). For both series, each Ni(II)2Ln(III)2 structure can be described as two di-μ-phenoxo-bridged Ni(II)Ln(III) binuclear units bridged by two carbonato CO3(2-) units to form a carbonato-bridged (μ4-CO3)2{Ni(II)2Ln(III)2} structure. The high-spin Ni(II) ion has octahedral coordination geometry, and the Ln(III) ion is coordinated by O9 donor atoms from Ni(II)(3-MeOsaltn), bidentate NO3(-), and one and two oxygen atoms of two CO3(2-) ions. The NO3(-) ion for the first series roughly lie on Ln-O(methoxy) bonds and are tilted toward the outside, while for the second series, the two oxygen atoms roughly lie on one of the Ln-O(phenoxy) bonds due to the intramolecular hydrogen bond. The temperature-dependent magnetic susceptibilities indicated a ferromagnetic interaction between the Ni(II) and Ln(III) ions (Ln(III) = Gd(III), Tb(III), Dy(III)) for all of the complexes, with a distinctly different magnetic behavior between the two series in the lowest-temperature region due to the Ln(III)-Ln(III) magnetic interaction and/or different magnetic anisotropies of the Tb(III) or Dy(III) ion. Alternating-current susceptibility measurements under the 0 and 1000 Oe direct-current (dc) bias fields showed no magnetic relaxation for the Ni(II)2Gd(III)2 complexes but exhibited an out-of-phase signal for Ni(II)2Tb(III)2 and Ni(II)2Dy(III)2, indicative of slow relaxation of magnetization. The energy barriers, Δ/kB, for the spin flipping were estimated from the Arrhenius

  1. Removal of Cu(II) from aqueous solution by agricultural by-product: Peanut hull

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Chunshui, E-mail: silk588@126.com [School of Environment Science and Spatial Informatics, China university of Mining and technology, Xuzhou, Jiangsu 221008 (China) and School of Chemical Engineering, Huai-hai institute of Technology, Lian Yungang, Jiangsu 222005 (China); Wang Liping [School of Environment Science and Spatial Informatics, China university of Mining and technology, Xuzhou, Jiangsu 221008 (China); Chen Wenbin [School of Environment Science and Spatial Informatics, China university of Mining and technology, Xuzhou, Jiangsu 221008 (China); School of Chemical Engineering, Huai-hai institute of Technology, Lian Yungang, Jiangsu 222005 (China)

    2009-09-15

    Peanut hull, an agricultural by-product abundant in China, was used as adsorbent for the removal of Cu(II) from aqueous solutions. The extent of adsorption was investigated as a function of pH, contact time, adsorbate concentration and reaction temperature. The Cu(II) removal was pH-dependent, reaching a maximum at pH 5.5. The biosorption process followed pseudo-second-order kinetics and equilibrium was attained at 2 h. The rate constant increased with the increase of temperature indicates endothermic nature of biosorption. The activation energy (E{sub a}) of Cu(II) biosorption was determined at 17.02 kJ/mol according to Arrhenius equation which shows that biosorption may be an activated chemical biosorption. Other activation parameters such as {Delta}H{sup numbersign}, {Delta}S{sup numbersign}, and {Delta}G{sup numbersign} were also determined from Eyring equation. The equilibrium data were analyzed using the Langmuir, Freundlich, and Dubinin-Radushkevich (D-R) isotherm models depending on temperature. The equilibrium biosorption capacity of Cu(II) determined from the Langmuir equation was 21.25 mg/g at 30 deg. C. The mean free energy E (kJ/mol) got from the D-R isotherm also indicated a chemical ion-exchange mechanism. The thermodynamic parameters such as changes in Gibbs free energy ({Delta}G{sup 0}), enthalpy ({Delta}H{sup 0}) and entropy ({Delta}S{sup 0}) were used to predict the nature of biosorption process. The negative {Delta}G{sup 0} values at various temperatures confirm the biosorption processes are spontaneous.

  2. pH-dependence of the specific binding of Cu(II) and Zn(II) ions to the amyloid-β peptide

    International Nuclear Information System (INIS)

    Ghalebani, Leila; Wahlström, Anna; Danielsson, Jens; Wärmländer, Sebastian K.T.S.; Gräslund, Astrid

    2012-01-01

    Highlights: ► Cu(II) and Zn(II) display pH-dependent binding to the Aβ(1–40) peptide. ► At pH 7.4 both metal ions display residue-specific binding to the Aβ peptide. ► At pH 5.5 the binding specificity is lost for Zn(II). ► Differential Cu(II) and Zn(II) binding may help explain metal-induced AD toxicity. -- Abstract: Metal ions like Cu(II) and Zn(II) are accumulated in Alzheimer’s disease amyloid plaques. The amyloid-β (Aβ) peptide involved in the disease interacts with these metal ions at neutral pH via ligands provided by the N-terminal histidines and the N-terminus. The present study uses high-resolution NMR spectroscopy to monitor the residue-specific interactions of Cu(II) and Zn(II) with 15 N- and 13 C, 15 N-labeled Aβ(1–40) peptides at varying pH levels. At pH 7.4 both ions bind to the specific ligands, competing with one another. At pH 5.5 Cu(II) retains its specific histidine ligands, while Zn(II) seems to lack residue-specific interactions. The low pH mimics acidosis which is linked to inflammatory processes in vivo. The results suggest that the cell toxic effects of redox active Cu(II) binding to Aβ may be reversed by the protective activity of non-redox active Zn(II) binding to the same major binding site under non-acidic conditions. Under acidic conditions, the protective effect of Zn(II) may be decreased or changed, since Zn(II) is less able to compete with Cu(II) for the specific binding site on the Aβ peptide under these conditions.

  3. Determination of Ni(II) crystal structure by powder x-ray diffraction ...

    African Journals Online (AJOL)

    X-ray powder diffraction pattern was used to determine the length of the unit cell, “a”, the lattice structure type, and the number of atoms per unit cell of Ni(II) crystal. The “a” value was determined to be 23.66 ± 0.005 Å, particle size of 34.87 nm, volume 13.24 Å and Strain value ε = 9.8 x 10-3. The cell search on PXRD patterns ...

  4. Synthesis, crystal structure and photoluminescence study of green light emitting bis(1[(4-butylphenylimino]methyl naphthalen-2-ol Ni(II complex

    Directory of Open Access Journals (Sweden)

    M. Srinivas

    2016-09-01

    Full Text Available Synthetically feasible and cost effective Ni(II complex phosphor (4 as green organic light emitting diode (OLED was prepared by using Schiff base 1-[(4-butylphenylimino]methyl naphthalen-2-ol (3. The single crystals of Ni(II complex were grown from chloroform and hexane (1:1 v/v solution. The green crystals of the complex were characterized by using single crystal XRD studies and were evaluated for their photophysical properties. From the Diffused Reflectance Spectrum of the complex, the measured band gap energy was found to be 1.83 eV and the PL spectrum of the complex showed emission peak at 519 nm. The excitation peaks at 519 nm were appeared at 394 nm and 465 nm. The Commission Internationale De L'Eclairage (CIE chromaticity diagram indicated that, the complex exhibit green color. Hence, Ni(II complex (4 could be a promising green OLED for developing strong electroluminescent materials for flat panel display applications.

  5. Spectral, thermal, kinetic, molecular modeling and eukaryotic DNA degradation studies for a new series of albendazole (HABZ) complexes

    Science.gov (United States)

    El-Metwaly, Nashwa M.; Refat, Moamen S.

    2011-01-01

    This work represents the elaborated investigation for the ligational behavior of the albendazole ligand through its coordination with, Cu(II), Mn(II), Ni(II), Co(II) and Cr(III) ions. Elemental analysis, molar conductance, magnetic moment, spectral studies (IR, UV-Vis and ESR) and thermogravimetric analysis (TG and DTG) have been used to characterize the isolated complexes. A deliberate comparison for the IR spectra reveals that the ligand coordinated with all mentioned metal ions by the same manner as a neutral bidentate through carbonyl of ester moiety and NH groups. The proposed chelation form for such complexes is expected through out the preparation conditions in a relatively acidic medium. The powder XRD study reflects the amorphous nature for the investigated complexes except Mn(II). The conductivity measurements reflect the non-electrolytic feature for all complexes. In comparing with the constants for the magnetic measurements as well as the electronic spectral data, the octahedral structure was proposed strongly for Cr(III) and Ni(II), the tetrahedral for Co(II) and Mn(II) complexes but the square-pyramidal for the Cu(II) one. The thermogravimetric analysis confirms the presence or absence of water molecules by any type of attachments. Also, the kinetic parameters are estimated from DTG and TG curves. ESR spectrum data for Cu(II) solid complex confirms the square-pyramidal state is the most fitted one for the coordinated structure. The albendazole ligand and its complexes are biologically investigated against two bacteria as well as their effective effect on degradation of calf thymus DNA.

  6. Microwave-Assisted Synthesis of 3,5-Dibenzyl-4-amino-1,2,4-triazole and its Diazo Ligand, Metal Complexes Along with Anticancer Activity

    Directory of Open Access Journals (Sweden)

    Anjali Jha

    2010-01-01

    Full Text Available Synthesis of 3,5-dibenzyl-4-amino-1,2,4-triazole was accomplished via a conventional method as well as microwave irradiation method, followed by diazotization and coupling with 2,4-pentanedione. The dinucleating ligand was isolated and complexed with Ni(II, Cu(II and Ru(III chlorides. These complexes were screened on Jurkat, Raji & PBMC cell lines for anticancer activity. Ruthenium complexes showed potential anticancer activities.

  7. Metallic complexes with glyphosate: a review; Complexos metalicos com o herbicida glifosato: revisao

    Energy Technology Data Exchange (ETDEWEB)

    Coutinho, Claudia F.B.; Mazo, Luiz Henrique [Sao Paulo Univ., Sao Carlos, SP (Brazil). Inst. de Quimica]. E-mail: claudiabreda@iqsc.usp.br

    2005-11-15

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature. (author)

  8. Metallic complexes with glyphosate: a review

    International Nuclear Information System (INIS)

    Coutinho, Claudia F.B.; Mazo, Luiz Henrique

    2005-01-01

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature. (author)

  9. Protein immobilization on Ni(II) ion patterns prepared by microcontact printing and dip-pen nanolithography

    NARCIS (Netherlands)

    Wu, Chien-Ching; Reinhoudt, David N; Otto, Cees; Velders, Aldrik H; Subramaniam, Vinod

    2010-01-01

    An indirect method of protein patterning by using Ni(II) ion templates for immobilization via a specific metal-protein interaction is described. A nitrilotriacetic acid (NTA)-terminated self-assembled monolayer (SAM) allows oriented binding of histidine-tagged proteins via complexation with late

  10. One-Pot Synthesis of Cu(II Complex with Partially Oxidized TTF Moieties

    Directory of Open Access Journals (Sweden)

    Hiroki Oshio

    2012-07-01

    Full Text Available The one-pot synthesis of a Cu(II complex with partially oxidized tetrathiafulvalene (TTF moieties in its capping MT-Hsae-TTF ligands, [CuII(MT-sae-TTF2] [CuICl2] was realized by the simultaneous occurrence of Cu(II complexation and CuIICl2 mediated oxidation of TTF moieties. The crystal structure was composed of one-dimensional columns formed by partially oxidized TTF moieties and thus the cation radical salt showed relatively high electrical conductivity. Tight binding band structure calculations indicated the existence of a Peierls gap due to the tetramerization of the TTF moieties in the one-dimensional stacking column at room temperature, which is consistent with the semiconducting behavior of this salt.

  11. Removal of Cu(II) metal ions from aqueous solution by amine functionalized magnetic nanoparticles

    Science.gov (United States)

    Kothavale, V. P.; Karade, V. C.; Waifalkar, P. P.; Sahoo, Subasa C.; Patil, P. S.; Patil, P. B.

    2018-04-01

    The adsorption behavior of Cu(II) metal cations was investigated on the amine functionalized magnetic nanoparticles (MNPs). TheMNPs were synthesized by thesolvothermal method and functionalized with (3-Aminopropyl)triethoxysilane (APTES). MNPs were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and vibrating sample magnetometer (VSM). The MNPs have pure magnetite phase with particle size around 10-12 nm. MNPs exhibits superparamagnetic behavior with asaturation magnetization of 68 emu/g. The maximum 38 % removal efficiency was obtained for Cu(II) metal ions from the aqueous solution.

  12. Solid phase extraction-inductively coupled plasma spectrometry for adsorption of Co(II) and Ni(II) from radioactive wastewaters by natural and modified zeolites

    International Nuclear Information System (INIS)

    Akbar Malekpour; Mohammad Edrisi; Shamsollah Shirzadi; Saeed Hajialigol

    2011-01-01

    Natural and modified clinoptilolite as low-cost adsorbents have been used for adsorption of Co(II) and Ni(II) from nuclear wastewaters both in batch and continuous experiments. Zeolite X was also synthesized and its ability towards the selected cations was examined. Kinetic and thermodynamic behaviors for the process were investigated and adsorption equilibrium was interpreted in term of Langmuir and Freundlich equations. The effect of various parameters including the initial concentration, temperature, ionic strength and pH of solution were examined to achieve the optimized conditions. The clinoptilolite was shown good sorption potential for Co(II) and Ni(II) ions at pH values 4-6. Based on desorption studies, nearly 74 and 85% of adsorbed Co(II) and Ni(II) were removed from clinoptilolite by HCl. The Na + and NH 4 + forms of clinoptilolite were the best modified forms for the removal of investigated cations. It is concluded that the selectivity of clinoptilolite is higher for Co(II) than Ni(II). The synthesized zeolite showed more ability to remove cobalt and nickel ions from aqueous solution than the natural clinoptilolite. The microwave irradiation was found to be more rapid and effective for ion exchange compared to conventional ion exchange process. (author)

  13. Aromatic carboxylate effect on dimensionality of three bis(benzimidazole)-based cobalt(II) coordination polymers: Syntheses, structures and properties

    International Nuclear Information System (INIS)

    Zhang, Ju-Wen; Gong, Chun-Hua; Hou, Li-Li; Tian, Ai-Xiang; Wang, Xiu-Li

    2013-01-01

    Three new metal-organic coordination polymers [Co(4-bbc) 2 (bbbm)] (1), [Co(3,5-pdc)(bbbm)]·2H 2 O (2) and [Co(1,4-ndc)(bbbm)] (3) (4-Hbbc=4-bromobenzoic acid, 3,5-H 2 pdc=3,5-pyridinedicarboxylic acid, 1,4-H 2 ndc=1,4-naphthalenedicarboxylic acid and bbbm=1,1-(1,4-butanediyl)bis-1H-benzimidazole) were hydrothermally synthesized and structurally characterized. Polymer 1 is a 1D chain formed by the bbbm ligands and Co II ions. Polymer 2 exhibits a 2D network with a (3·4·5)(3 2 ·4·5·6 2 ·7 4 ) topology. Polymer 3 possesses a 3D three-fold interpenetrating framework. The versatile structures of title polymers indicate that the aromatic carboxylates have an important influence on the dimensionality of 1–3. Moreover, the thermal stability, electrochemical and luminescent properties of 1–3 were investigated. - graphical abstract: Three bis(benzimidazole)-based cobalt(II) coordination polymers tuned by aromatic carboxylates were hydrothermally synthesized and structurally characterized. The aromatic carboxylates play a key role in the dimensionality of three polymers. The electrochemical and luminescent properties of three polymers were investigated. Display Omitted - Highlights: • Three bis(benzimidazole)-based cobalt(II) coordination polymers tuned by aromatic carboxylates were obtained. • The aromatic carboxylates have an important influence on the dimensionality of three polymers. • The electrochemical and luminescent properties of three polymers were investigated

  14. Macroscopic and microscopic investigation of Ni(II) sequestration on diatomite by batch, XPS, and EXAFS techniques.

    Science.gov (United States)

    Sheng, Guodong; Yang, Shitong; Sheng, Jiang; Hu, Jun; Tan, Xiaoli; Wang, Xiangke

    2011-09-15

    Sequestration of Ni(II) on diatomite as a function of time, pH, and temperature was investigated by batch, XPS, and EXAFS techniques. The ionic strength-dependent sorption at pH < 7.0 was consistent with outer-sphere surface complexation, while the ionic strength-independent sorption at pH = 7.0-8.6 was indicative of inner-sphere surface complexation. EXAFS results indicated that the adsorbed Ni(II) consisted of ∼6 O at R(Ni-O) ≈ 2.05 Å. EXAFS analysis from the second shell suggested that three phenomena occurred at the diatomite/water interface: (1) outer-sphere and/or inner-sphere complexation; (2) dissolution of Si which is the rate limiting step during Ni uptake; and (3) extensive growth of surface (co)precipitates. Under acidic conditions, outer-sphere complexation is the main mechanism controlling Ni uptake, which is in good agreement with the macroscopic results. At contact time of 1 h or 1 day or pH = 7.0-8.0, surface coprecipitates occur concurrently with inner-sphere complexes on diatomite surface, whereas at contact time of 1 month or pH = 10.0, surface (co)precipitates dominate Ni uptake. Furthermore, surface loading increases with temperature increasing, and surface coprecipitates become the dominant mechanism at elevated temperature. The results are important to understand Ni interaction with minerals at the solid-water interface, which is helpful to evaluate the mobility of Ni(II) in the natural environment.

  15. Spectroscopic characterization of some Cu(II) complexes

    International Nuclear Information System (INIS)

    Singh, Puja; Sharma, S.

    2014-01-01

    3-hydroxy-4-methoxy benzaldehyde semicarbazone (HMBS) is a biologically active compound which has several potential donor sites. This compound has been used for complexation with Cu(II) ions to synthesize complexes of general formula [Cu(HMBS) 2 X 2 ] where X is Cl − , NO 3 − and CH 3 COO − . Cu(II) is a d 9 system for which 2 D term is generated. Under O h symmetry, this term splits into 2 E g and 2 T 2g . the ground term 2 Eg is doubly degenerate and hence suffers strong Jahn-Teller effect and accordingly the further splitting of terms occur to lower the symmetry from perfect O h . Here, the ligand occupies four planar positions while the two axial positions have been varied by using different ions like Cl − , NO 3 − and CH 3 COO − . These variations on the axial positions also add to the distortion in O h symmetry. Under strong distortion, the electronic spectral band splits into multiplets exhibiting tetragonal distortion in complexes. The extent of distortion has been derived by the derivation of the two radial parameters D s and D t from electronic spectral bands. The ESR spectra of complexes reveal the real position of the only unpaired electron of the d 9 system in complexes

  16. The facile synthesis of a chitosan Cu(II) complex by solution plasma process and evaluation of their antioxidant activities.

    Science.gov (United States)

    Ma, Fengming; Li, Pu; Zhang, Baiqing; Wang, Zhenyu

    2017-10-01

    Synthesis of chitosan-Cu(II) complex by solution plasma process (SPP) irradiation was investigated. The effects of the distance between the electrodes, initial Cu(II) concentration, and initial pH on the Cu(II) adsorption capacity were evaluated. The results showed that narrower distance between the electrodes, higher initial Cu(II) concentration and higher initial pH (at pHchitosan-Cu(II) complex by ultraviolet-visible (UV-vis), fourier transform infrared (FT-IR) and electron spin resonance (ESR) spectroscopy revealed that the main structure of chitosan was not changed after irradiation. Thermogravimetry (TG) analysis indicated that Cu(II) ions were well incorporated into the chitosan. The antioxidant activity of the chitosan-Cu(II) complex was evaluated by DPPH, ABTS, and reducing power assays. The chitosan-Cu(II) complex exhibited greater antioxidant activity than the original chitosan. Thus, SPP could be used for preparation of chitosan-Cu(II) complexes. Copyright © 2017. Published by Elsevier B.V.

  17. Synthesis, characterization and thermal study of some transition metal complexes of an asymmetrical tetradentate Schiff base ligand

    Directory of Open Access Journals (Sweden)

    ACHUT S. MUNDE

    2010-03-01

    Full Text Available Complexes of Cu(II, Ni(II, Co(II, Mn(II and Fe(III with an asymmetric tetradentate Schiff base ligand derived from dehydroacetic acid, 4-methyl-o-phenylenediamine and salicylic aldehyde were synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV–Vis, IR, 1H-NMR spectroscopy, X-ray diffraction analysis of powdered samples and thermal analysis, and screened for antimicrobial activity. The IR spectral data suggested that the ligand behaves as a dibasic tetadentate ligand towards the central metal ion with an ONNO donor atoms sequence. From the microanalytical data, the stoichiometry of the complexes 1:1 (metal:ligand was found. The physico-chemical data suggested square planar geometry for the Cu(II and Ni(II complexes and octahedral geometry for the Co(II, Mn(II and Fe(III complexes. The thermal behaviour (TGA/DTA of the complexes was studied and kinetic parameters were determined by Horowitz–Metzger and Coats–Redfern methods. The powder X-ray diffraction data suggested a monoclinic crystal system for the Co(II, Mn(II and Fe(III complexes. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus niger and Trichoderma viride.

  18. A study of the removal of heavy metals from aqueous solutions by Moringa oleifera seeds and amine-based ligand 1,4-bis[N,N-bis(2-picoyl)amino]butane

    International Nuclear Information System (INIS)

    Obuseng, Veronica; Nareetsile, Florence; Kwaambwa, Habauka M.

    2012-01-01

    Highlights: ► Materials are effective and selective in simultaneous removal of heavy metal ions. ► Use of composite adsorbent of both materials may result in more effective material. ► Seeds biomass has various functional groups involves in metal removal. ► Attainment of sorption equilibrium is rapid for the seeds biomass. ► Seeds biomass effectiveness is not affected over wide effective pH range. - Abstract: Uptake for lead, copper, cadmium, nickel and manganese from aqueous solution using the Moringa oleifera seeds biomass (MOSB) and amine-based ligand (ABL) was investigated. Experiments on two synthetic multi-solute systems revealed that MOSB performed well in the biosorption and followed the decreasing orders Pb(II) > Cu(II) > Cd(II) > Ni(II) > Mn(II) and Zn(II) > Cu(II) > Ni(II). The general trend of the heavy metal ions uptake by the amine-based ligand followed decreased in the order Mn > Cd > Cu > Ni > Pb, which is the reverse trend for what was observed for MOSB. Comparing the single- and multi-metal solutions, there was no clear effect in the biosorption capacity of MOSB suggesting the presence of sufficient active binding sites for all metal ions studied. The MOSB performance is also not affected by pH in the range 3.5–8.

  19. Structural, theoretical and corrosion inhibition studies on some transition metal complexes derived from heterocyclic system

    Science.gov (United States)

    Gupta, Shraddha Rani; Mourya, Punita; Singh, M. M.; Singh, Vinod P.

    2017-06-01

    A Schiff base, (E)-N‧-((1H-indol-3-yl)methylene)-2-aminobenzohydrazide (Iabh) and its Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) complexes have been synthesized. These compounds have been characterized by different physico-chemical and spectroscopic tools (UV-Vis, IR, NMR and ESI-Mass). The molecular structure of Iabh is determined by single crystal X-ray diffraction technique. The ligand Iabh displays E-configuration about the >Cdbnd N- bond. The structure of ligand is stabilized by intra-molecular H-bonding. In all the metal complexes the ligand coordinates through azomethine-N and carbonyl-O resulting a distorted octahedral geometry for Mn(II), Co(II) and Cu(II) complexes in which chloride ions occupy axial positions. Ni(II) and Zn(II) complexes, however, form 4-coordinate distorted square planer and tetrahedral geometry around metal ion, respectively. The structures of the complexes have been satisfactorily modeled by calculations based on density functional theory (DFT) and time dependent-DFT (TD-DFT). The corrosion inhibition study of the compounds have been performed against mild steel in 0.5 M H2SO4 solution at 298 K by using weight loss, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). They show appreciable corrosion inhibition property.

  20. Synthesis and spectroscopic studies of biologically active tetraazamacrocyclic complexes of Mn(II, Co(II, Ni(II, Pd(II and Pt(II

    Directory of Open Access Journals (Sweden)

    Monika Tyagi

    2014-01-01

    Full Text Available Complexes of Mn(II, Co(II, Ni(II, Pd(II and Pt(II were synthesized with the macrocyclic ligand, i.e., 2,3,9,10-tetraketo-1,4,8,11-tetraazacycoletradecane. The ligand was prepared by the [2 + 2] condensation of diethyloxalate and 1,3-diamino propane and characterized by elemental analysis, mass, IR and 1H NMR spectral studies. All the complexes were characterized by elemental analysis, molar conductance, magnetic susceptibility measurements, IR, electronic and electron paramagnetic resonance spectral studies. The molar conductance measurements of Mn(II, Co(II and Ni(II complexes in DMF correspond to non electrolyte nature, whereas Pd(II and Pt(II complexes are 1:2 electrolyte. On the basis of spectral studies an octahedral geometry has been assigned for Mn(II, Co(II and Ni(II complexes, whereas square planar geometry assigned for Pd(II and Pt(II. In vitro the ligand and its metal complexes were evaluated against plant pathogenic fungi (Fusarium odum, Aspergillus niger and Rhizoctonia bataticola and some compounds found to be more active as commercially available fungicide like Chlorothalonil.

  1. Cobalt(II Complexes with N,N,N-Scorpionates and Bidentate Ligands: Comparison of Hydrotris(3,5-dimethylpyrazol-1-ylborate Tp* vs. Phenyltris(4,4-dimethyloxazolin-2-ylborate ToM to Control the Structural Properties and Reactivities of Cobalt Centers

    Directory of Open Access Journals (Sweden)

    Toshiki Nishiura

    2018-06-01

    Full Text Available Scorpionate ligands Tp* (hydrotris(3,5-dimethylpyrazol-1-ylborate and ToM (tris(4,4-dimethyloxazolin-2-ylphenylborate complexes of cobalt(II with bidentate ligands were synthesized. Both Tp* and ToM coordinate to cobalt(II in a tridentate fashion when the bidentate ligand is the less hindered acetylacetonate. In crystal structures, the geometry of cobalt(II supported by the N3O2 donor set in the Tp* complex is a square-pyramid, whereas that in the ToM complex is close to a trigonal-bipyramid. Both Tp*- and ToM-acac complexes exhibit solvatochromic behavior, although the changing structural equilibria of these complexes in MeCN are quite different. In the bis(1-methylimidazol-2-ylmethylphenylborate (LPh complexes, Tp* retains the tridentate (к3 mode, whereas ToM functions as the bidentate (к2 ligand, giving the tetrahedral cobalt(II complex. The bowl-shaped cavity derived from the six methyl groups on ToM lead to susceptibility to the bulkiness of the opposite bidentate ligand. The entitled scorpionate compounds mediate hydrocarbon oxidation with organic peroxides. Allylic oxidation of cyclohexene occurs mainly on the reaction with tert-butyl hydroperoxide (TBHP, although the catalytic efficiency of the scorpionate ligand complexes is lower than that of Co(OAc2 and Co(acac2. On cyclohexane oxidation with meta-chloroperbenzoic acid (mCPBA, both ToM and Tp* complexes function as catalysts for hydroxylation. The higher electron-donating ToM complexes show faster initial reaction rates compared to the corresponding Tp* complexes.

  2. Characterization of the Unusual Product from the Reaction between Cobalt(II) Chloride, Ethane-1,2-diamine, and Hydrochloric Acid: An Undergraduate Project Involving an Unknown Metal Complex.

    Science.gov (United States)

    Curtis, Neil F.; And Others

    1986-01-01

    Discusses the need for student research-type chemistry projects based upon "unknown" metal complexes. Describes an experiment involving the product from the reaction between cobalt(II) chloride, ethane-1,2-diamine (en) and concentrated hydrochloric acid. Outlines the preparation of the cobalt complex, along with procedure, results and…

  3. Bioassay studies of metal(II complexes of 2,2'-(ethane-1,2-diyldiiminodiacetic acid

    Directory of Open Access Journals (Sweden)

    Saeed-ur-Rehman

    2011-08-01

    Full Text Available Ni(II, Cu(II and Zn(II coordination compounds with modified diammine 2,2'-(ethane-1,2-diyldiiminodiacetic acid (EDDA were prepared and characterized. Coordination complexes of the EDDA were characterized by physical measurements including elemental analysis, IR, UV-Visible, magnetic susceptibilities and conductance measurements. The complexes were screened against four pathogenic bacteria like Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumoniae and Staphylococcus aureus and their concentrations for maximum inhibition zones were obtained.

  4. Voltammetric determination of zirconium using azo compounds

    International Nuclear Information System (INIS)

    Orshulyak, O.O.; Levitskaya, G.D.

    2008-01-01

    The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

  5. Determination of Proton Relaxivities of Mn(II, Cu(II and Cr(III added to Solutions of Serum Proteins

    Directory of Open Access Journals (Sweden)

    Ali Yilmaz

    2009-04-01

    Full Text Available Relaxometric studies are still of scientific interest due to their use in medicine and biology. In this study, proton T1 and T2 relaxivities of Mn(II, Cu(II and Cr(III in water were determined in the presence and absence of various proteins (albumin, α-globulin, γ-globulin, lysozyme, fibrinogen. The 1/T1 and 1/T2 in all solutions are linearly proportional to the concentration of the paramagnetic ions. Mn(II has the great influence to alter relaxations in all protein solutions, while Cu(II and Cr(III have a poor influence on the relaxations. In addition, Mn(II and Cu(II are bound to each protein, but Cr(III is not bound to any protein.

  6. Sorption of Cu(II) Ions on Chitosan-Zeolite X Composites: Impact of Gelling and Drying Conditions.

    Science.gov (United States)

    Djelad, Amal; Morsli, Amine; Robitzer, Mike; Bengueddach, Abdelkader; di Renzo, Francesco; Quignard, Françoise

    2016-01-19

    Chitosan-zeolite Na-X composite beads with open porosity and different zeolite contents were prepared by an encapsulation method. Preparation conditions had to be optimised in order to stabilize the zeolite network during the polysaccharide gelling process. Composites and pure reference components were characterized using X-ray diffraction (XRD); scanning electron microscopy (SEM); N₂ adsorption-desorption; and thermogravimetric analysis (TG). Cu(II) sorption was investigated at pH 6. The choice of drying method used for the storage of the adsorbent severely affects the textural properties of the composite and the copper sorption effectiveness. The copper sorption capacity of chitosan hydrogel is about 190 mg·g(-1). More than 70% of this capacity is retained when the polysaccharide is stored as an aerogel after supercrititcal CO₂ drying, but nearly 90% of the capacity is lost after evaporative drying to a xerogel. Textural data and Cu(II) sorption data indicate that the properties of the zeolite-polysaccharide composites are not just the sum of the properties of the individual components. Whereas a chitosan coating impairs the accessibility of the microporosity of the zeolite; the presence of the zeolite improves the stability of the dispersion of chitosan upon supercritical drying and increases the affinity of the composites for Cu(II) cations. Chitosan-zeolite aerogels present Cu(II) sorption properties.

  7. Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

    Science.gov (United States)

    Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

    2017-09-01

    Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

  8. Antiferromagnetic Coupling in the Polynuclear Compound [Cu(II) (Allopurinolate) (OH-)] n

    Science.gov (United States)

    Acevedo-Chávez, Rodolfo; Costas, María. Eugenia; Escudero-Derat, Roberto

    1994-11-01

    Synthetic, spectral, and magnetic studies of the Cu(II) polynuclear coordination compound [Cu(HL(OH-)]n with bridging OH- and HL (allopurinolate; C5H3N4O-) ligands are reported. The compound is obtained from aqueous media (at several pH values and from CI-, Br-, NO-3, SO2-4, ClO-4, and CH3CO-2 Cu(II) salts), from DMSO at ca. 70°C using several of the above salts, and under refluxing methanol employing Cu(SO4) or Cu(CH3CO2)2. The results suggest that the compound [Cu(HL)(OH-)]n has a polynuclear form in which the bridging allopurinolate is coordinated through the N(1) and N(2) atoms of the pyrazolic moiety. All attempts to grow crystals suitable for X-ray studies were unsuccessful, and an amorphous compound was always obtained. Magnetic studies show the existence of a strong antiferromagnetic coupling, which may be associated with a favorable structural arrangement between the metallic centers and the bridging ligands. This magnetic behavior is remarkable for a Cu(II) polynuclear coordination compound. Spectral and magnetic results together with the coordination modes of the bridging groups let us postulate as a possible arrangement a cyclic polynuclear structure presenting the allopurinolate and OH- bridging ligands in a mutually trans configuration. This work is the first EPR spectral and magnetic study reported for a coordination compound with the allopurinol heterocycle as a ligand and, thus for the first example of a polynuclear coordination compound combining allopurinolate and OH- as bridging groups.

  9. Complexes cobalt(II, zinc(II and copper(II with some newly synthesized benzimidazole derivatives and their antibacterial activity

    Directory of Open Access Journals (Sweden)

    S. O. PODUNAVAC-KUZMANOVIC

    1999-05-01

    Full Text Available The preparation and properties of some complexes of cobalt(II, zinc(II and copper(II with several newly synthesized benzimidazole derivatives (L are reported. The complexes, of the general formula [MCl2L2] (M=Co(II, Zn(II and [CuCl2L(H2O], have a tetrahedral structure. The complexes were characterized by elemental analysis, molar conductivity, magnetic susceptibility measurements, IR and absorption electronic spectra. The antibacterial activitiy of the benzimidazoles and their complexes was evaluated against Erwinia carotovora subsp. carotovora and Erwinia amylovora. The complexes were found to be more toxic than the ligands.

  10. Cu(II) salen complex with propylene linkage: An efficient catalyst in the formation of Csbnd X bonds (X = N, O, S) and biological investigations

    Science.gov (United States)

    Azam, Mohammad; Dwivedi, Sourabh; Al-Resayes, Saud I.; Adil, S. F.; Islam, Mohammad Shahidul; Trzesowska-Kruszynska, Agata; Kruszynski, Rafal; Lee, Dong-Ung

    2017-02-01

    The catalytic property of a mononuclear Cu(II) salen complex in Chan-Lam coupling reaction with phenyl boronic acid at room temperature is reported. The studied complex is found to be potential catalyst in the preparation of carbon-heteroatom bonds with excellent yields. The studied Cu(II) salen complex is monoclinic with cell parameters, a = 9.6807(5) (α 90°), (b = 17.2504(8) (β 112.429 (2), c = 11.1403 (6) (γ = 90°), and has distorted square planar environment around Cu(II) ion. Furthermore, there is no π⋯π interactions in the reported complex due to large distance between the centroid of aromatic rings. In addition, DNA binding study of Cu(II) salen complex by fluorescence and absorption spectroscopy is also reported. Moreover, the reported Cu(II) salen complex exhibits significant anticancer activity against MCF-7 cancer cell lines, and displays potential antimicrobial biofilm activity against P. aeruginosa, suggesting antimicrobial biofilm an important tool for suppression of resistant infections caused by P. aeruginosa.

  11. Hybrid porous phosphate heterostructures as adsorbents of Hg(II) and Ni(II) from industrial sewage

    International Nuclear Information System (INIS)

    Jimenez-Jimenez, J.; Algarra, M.; Rodriguez-Castellon, E.; Jimenez-Lopez, A.; Esteves da Silva, J.C.G.

    2011-01-01

    Porous phosphate heterostructures (PPH), functionalized with different ratios of aminopropyl and mercaptopropyl groups, labelled as N x=5,25,50 -PPH and S x=5,25,50 -PPH, respectively, were tested as adsorbents for Ni(II) and Hg(II) found in industrial sewage from electroplating processes and button battery recycling. X-ray diffraction was used to study the structures. The specific surface area of the pristine material (PPH) was 620 m 2 g -1 , whereas the specific surface areas of the modified mercaptopropyl (S 5 -PPH) and aminopropyl (N 5 -PPH) were 472 and 223 m 2 g -1 , respectively. The adsorption data were fitted to a Langmuir isotherm model. The S 5 -PPH material was saturated by 120 mmol Hg(II) per 100 g of material, whereas for Ni(II) adsorption, N 25 -PPH material displayed the highest adsorption with a saturation value of 43.5 mmol per 100 g. These results suggest that functionalized PPH materials may be promising toxic metal scavengers and that they may provide an alternative environmental technology.

  12. Hybrid porous phosphate heterostructures as adsorbents of Hg(II) and Ni(II) from industrial sewage

    Energy Technology Data Exchange (ETDEWEB)

    Jimenez-Jimenez, J., E-mail: jjimenez@uma.es [Departamento de Quimica Inorganica, Facultad de Ciencias, Universidad de Malaga, Campus de Teatinos s/n, 29071 Malaga (Spain); Algarra, M. [Centro de Geologia do Porto, Faculdade de Ciencias, Universidade do Porto. Rua do, Campo Alegre 687, 4169-007 Porto (Portugal); Rodriguez-Castellon, E.; Jimenez-Lopez, A. [Departamento de Quimica Inorganica, Facultad de Ciencias, Universidad de Malaga, Campus de Teatinos s/n, 29071 Malaga (Spain); Esteves da Silva, J.C.G. [Centro de Investigacao em Quimica (CIQ-UP), Faculdade de, Ciencias da Universidade do Porto, Rua do Campo Alegre 687, 4169-007 Porto (Portugal)

    2011-06-15

    Porous phosphate heterostructures (PPH), functionalized with different ratios of aminopropyl and mercaptopropyl groups, labelled as N{sub x=5,25,50}-PPH and S{sub x=5,25,50}-PPH, respectively, were tested as adsorbents for Ni(II) and Hg(II) found in industrial sewage from electroplating processes and button battery recycling. X-ray diffraction was used to study the structures. The specific surface area of the pristine material (PPH) was 620 m{sup 2} g{sup -1}, whereas the specific surface areas of the modified mercaptopropyl (S{sub 5}-PPH) and aminopropyl (N{sub 5}-PPH) were 472 and 223 m{sup 2} g{sup -1}, respectively. The adsorption data were fitted to a Langmuir isotherm model. The S{sub 5}-PPH material was saturated by 120 mmol Hg(II) per 100 g of material, whereas for Ni(II) adsorption, N{sub 25}-PPH material displayed the highest adsorption with a saturation value of 43.5 mmol per 100 g. These results suggest that functionalized PPH materials may be promising toxic metal scavengers and that they may provide an alternative environmental technology.

  13. Synthesis of Highly Branched Polyolefins Using Phenyl Substituted α-Diimine Ni(II Catalysts

    Directory of Open Access Journals (Sweden)

    Fuzhou Wang

    2016-04-01

    Full Text Available A series of α-diimine Ni(II complexes containing bulky phenyl groups, [ArN = C(NaphthC = NAr]NiBr2 (Naphth: 1,8-naphthdiyl, Ar = 2,6-Me2-4-PhC6H2 (C1; Ar = 2,4-Me2-6-PhC6H2 (C2; Ar = 2-Me-4,6-Ph2C6H2 (C3; Ar = 4-Me-2,6-Ph2C6H2 (C4; Ar = 4-Me-2-PhC6H3 (C5; Ar = 2,4,6-Ph3C6H2 (C6, were synthesized and characterized. Upon activation with either diethylaluminum chloride (Et2AlCl or modified methylaluminoxane (MMAO, all Ni(II complexes showed high activities in ethylene polymerization and produced highly branched amorphous polyethylene (up to 145 branches/1000 carbons. Interestingly, the sec-butyl branches were observed in polyethylene depending on polymerization temperature. Polymerization of 1-alkene (1-hexene, 1-octene, 1-decene and 1-hexadecene with C1-MMAO at room temperature resulted in branched polyolefins with narrow Mw/Mn values (ca. 1.2, which suggested a living polymerization. The polymerization results indicated the possibility of precise microstructure control, depending on the polymerization temperature and types of monomers.

  14. Determination of gold by substoichiometric extraction with N-thioacetyl benzamide

    International Nuclear Information System (INIS)

    Madhumita Bag; Pabitra Chattopadhyay; Sukalyan Basu

    2011-01-01

    Estimation of gold has been successfully carried out by substoichiometric radiochemical solvent extraction method using a newly designed organic moiety, N-thioacetyl benzamide as extractant and chloroform as solvent at aqueous pH 4. The interference effects of different closely related diverse ions like Fe(III), Cu(II), Co(II), Zn(II), Ni(II) etc. were also critically studied. The validity of this method has been verified by the study of recovery of gold in mud samples. (author)

  15. Selective dispersive liquid–liquid microextraction and preconcentration of Ni(II) into a micro droplet followed by ETAAS determination using a yellow Schiff's base bisazanyl derivative

    International Nuclear Information System (INIS)

    Alizadeh, Kamal; Nemati, Hadi; Zohrevand, Somaieh; Hashemi, Payman; Kakanejadifard, Ali; Shamsipur, Mojtaba; Ganjali, Mohammad Reza; Faridbod, Farnoush

    2013-01-01

    A simple, rapid and sensitive method was developed for the selective separation and preconcentration of Ni(II) using dispersive liquid–liquid microextraction, by a yellow Schiff's base bisazanyl derivative, as a selective complexing agent. In this method, a mixture of 45 μL chloroform (extraction solvent) and 450 μL tetrahydrofuran (dispersive solvent) is rapidly injected by syringe into a 5 mL aqueous sample containing 3% (w/v) sodium chloride and an appropriate amount of the Schiff's base. As a result, a cloudy solution is formed by entire dispersion of the extraction solvent into the aqueous phase. After centrifuging for 5 min at 5000 rpm, the sedimented phase is directly injected into the electrothermal atomic absorption spectrometry for Ni(II) determination. Some important parameters, such as kind and volume of extraction and dispersive solvents, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor for the presented method is 138. The calibration curve was linear over a nickel concentration range of 10–50 ng mL −1 . The detection limit and relative standard deviation were 0.04 ng mL −1 and 2.1%, respectively. The method was successfully applied to the extraction and determination of Ni(II) in different water samples. - Highlights: ► A new synthesized schiff's base was used for selective separation of Ni(II) ions. ► The method based on DLLME was successfully applied to the determination of Ni(II). ► A cloudy solution is formed by entire dispersion of the extraction solvent into the aqueous phase. ► In this work, the response surface analysis was used for the optimization purpose. ► The curvature of response surface reflects the interactive effect of the variables.

  16. EPR-study of reversible oxygenation process of coordination compounds of cobalt(II) with S-substituted N1,N4-di(salicylidene)-isothiosemicarbazides

    International Nuclear Information System (INIS)

    Gerbeleu, N.V.; Revenko, M.D.; Rusu, V.G.; Shames, A.T.

    1987-01-01

    The reaction between molecular oxygen and coordination compounds of cobalt(II) with S-substituted N 1 ,N 4 -di(salicylidene)isothiosemicarbazides in dimethyl sulfoxide solution was studied by the EPR method. It was found that paramagnetic monomeric adducts and diamagnetic μ-peroxo-dimers are formed. The spin-Hamiltonian parameters of the EPR spectra of the initial cobalt complexes, as well as of the paramagnetic adducts were determined. The nature of the Co-O 2 bond is discussed

  17. Cu(II) Complexes of Isoniazid Schiff Bases: DNA/BSA Binding and Cytotoxicity Studies on A549 Cell Line

    OpenAIRE

    Ramadevi, Pulipaka; Singh, Rinky; Prajapati, Akhilesh; Gupta, Sarita; Chakraborty, Debjani

    2014-01-01

    A series of isonicotinoyl hydrazones have been synthesized via template method and were complexed to Cu(II). The ligands are coordinated to Cu(II) ion through the enolic oxygen and azomethine nitrogen resulting in a square planar geometry. The CT-DNA and bovine serum albumin binding propensities of the compounds were determined spectrophotometrically, the results of which indicate good binding propensity of complexes to DNA and BSA with high binding constant values. Furthermore, the compounds...

  18. Study of new rubber to steel adhesive systems based on Co(II and Cu(II sulphides coats

    Directory of Open Access Journals (Sweden)

    Labaj Ivan

    2018-01-01

    Full Text Available The presented paper deals with the preparation of new rubber to steel adhesive systems using the steel surface treatment with deposition of adhesive coats based on Co(II and Cu(II sulphides. Efficiency of new prepared adhesive systems containing Co(II and Cu(II sulphides has been compared with the efficiency of double layer adhesive system commonly used in industry. The chemical composition of prepared adhesive systems was determined using the EDX analysis. Scanning Electron Microscopy (SEM was used for study of topography and microstructure of prepared rubber to steel adhesive systems (Co(II, Cu(II sulphide, double layer adhesive system. For determination of adhesion strength between rubber blends and metal pieces with various adhesive systems deposited on these pieces, the test according to ASTM D429 standard relating to Rubber to metal adhesion, method A was used. For all test samples, the same type of rubber blend and the same curing conditions have been used.

  19. Synthesis, characterization and biological assay of Salicylaldehyde Schiff base Cu(II) complexes and their precursors

    Science.gov (United States)

    Iftikhar, Bushra; Javed, Kanwal; Khan, Muhammad Saif Ullah; Akhter, Zareen; Mirza, Bushra; Mckee, Vickie

    2018-03-01

    Three new Schiff base ligands were synthesized by the reaction of Salicylaldehyde with semi-aromatic diamines, prepared by the reduction of corresponding dinitro-compounds, and were further used for the formation of complexes with Cu(II) metal ion. The structural features of the synthesized compounds were confirmed by their physical properties and infrared, electronic and NMR spectroscopic techniques. The studies revealed that the synthesized Schiff bases existed as tetradentate ligands and bonded to the metal ion through the phenolic oxygen and azomethine nitrogen. One of the dinitro precursors was also analyzed by single crystal X-ray crystallography, which showed that it crystallizes in monoclinic system with space group P2/n. The thermal behavior of the Cu(II) complexes was determined by thermogravimetric analysis (TGA) and kinetic parameters were evaluated from the data. Schiff base ligands, their precursors and metal complexes were also screened for antibacterial, antifungal, antitumor, Brine shrimp lethality, DPPH free radical scavenging and DNA damage assays. The results of these analyses indicated the substantial potential of the synthesized Schiff bases, their precursors and Cu(II) complexes in biological field as future drugs.

  20. Synthesis of poly(aminopropyl/methyl)silsesquioxane particles as effective Cu(II) and Pb(II) adsorbents.

    Science.gov (United States)

    Lu, Xin; Yin, Qiangfeng; Xin, Zhong; Li, Yang; Han, Ting

    2011-11-30

    Poly(aminopropyl/methyl)silsesquioxane (PAMSQ) particles have been synthesized by a one-step hydrolytic co-condensation process using 3-aminopropyltriethoxysilane (APTES) and methyltrimethoxysilane (MTMS) as precursors in the presence of base catalyst in aqueous medium. The amino functionalities of the particles could be controlled by adjusting the organosilanes feed ratio. The compositions of the amino-functionalized polysilsesquioxanes were confirmed by FT-IR spectroscopy, solid-state (29)Si NMR spectroscopy, and elemental analysis. The strong adsorbability of Cu(II) and Pb(II) ions onto PAMSQ particles was systematically examined. The effect of adsorption time, initial metal ions concentration and pH of solutions was studied to optimize the metal ions adsorbability of PAMSQ particles. The kinetic studies indicated that the adsorption process well fits the pseudo-second-order kinetics. Adsorption phenomena appeared to follow Langmuir isotherm. The PAMSQ particles demonstrate the highest Cu(II) and Pb(II) adsorption capacity of 2.29 mmol/g and 1.31 mmol/g at an initial metal ions concentration of 20mM, respectively. The PAMSQ particles demonstrate a promising application in the removal of Cu(II) and Pb(II) ions from aqueous solutions. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Catalytic role of Cu(II) in the reduction of Cr(VI) by citric acid under an irradiation of simulated solar light.

    Science.gov (United States)

    Li, Ying; Chen, Cheng; Zhang, Jing; Lan, Yeqing

    2015-05-01

    The catalytic role of Cu(II) in the reduction of Cr(VI) by citric acid with simulated solar light was investigated. The results demonstrated that Cu(II) could significantly accelerate Cr(VI) reduction and the reaction obeyed to pseudo zero-order kinetics with respect to Cr(VI). The removal of Cr(VI) was related to the initial concentrations of Cu(II), citric acid, and the types of organic acids. The optimal removal of Cr(VI) was achieved at pH 4, and the rates of Cu(II) photocatalytic reduction of Cr(VI) by organic acids were in the order: tartaric acid (two α-OH groups, two -COOH groups)>citric acid (one α-OH group, three -COOH groups)>malic acid (one α-OH group, two -COOH groups)>lactic acid (one α-OH group, one -COOH group)≫succinic acid (two -COOH groups), suggesting that the number of α-OH was the key factor for the reaction, followed by the number of -COOH. The formation of Cu(II)-citric acid complex could generate Cu(I) and radicals through a pathway of metal-ligand-electron transfer, promoting the reduction of Cr(VI). This study is helpful to fully understanding the conversion of Cr(VI) in the existence of both organic acids and Cu(II) with solar light in aquatic environments. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Nickel(II) and copper(II) complexes of N,N-dialkyl-N‧-3-chlorobenzoylthiourea: Synthesis, characterization, crystal structures, Hirshfeld surfaces and antimicrobial activity

    Science.gov (United States)

    Binzet, Gun; Gumus, Ilkay; Dogen, Aylin; Flörke, Ulrich; Kulcu, Nevzat; Arslan, Hakan

    2018-06-01

    We synthesized four new N,N-dialkyl-N‧-3-chlorobenzoylthiourea ligands (Alkyl: Dimethyl, diethyl, di-n-propyl and di-n-butyl) and their metal complexes with copper and nickel atoms. The structure of all synthesized compounds was fully characterized by physicochemical, spectroscopic and single crystal X-ray diffraction analysis techniques. The physical, spectral and analytical data of the newly synthesized metal complexes have shown the formation of 1:2 (metal:ligand) ratio. The benzoylthiourea ligands coordinate with metal atoms through oxygen and sulphur atoms. The metal atoms are in slightly distorted square-planar coordination geometry in Ni(II) or Cu(II) complex. Two oxygen and two sulphur atoms are mutually cis to each other in Ni(II) or Cu(II) complex. The intermolecular contacts in the compounds, which are HL1 and HL3, were examined by Hirshfeld surfaces and fingerprint plots using the data obtained from X-ray single crystal diffraction measurement. Besides these, their antimicrobial activities against Gram-positive bacteria (Bacillus subtilis, Staphylococcus aureus, Streptococcus pyogenes and Enterococcus faecalis) and Gram-negative bacteria (Escherichia coli and Pseudomonas aeruginosa) and anti-yeast activity (Candida glabrata, Candida parapsilosis and Candida albicans) were investigated. This exhibited some promising results towards testing organism. Among all the compounds, Ni(L1)2 complex showed high activity against Bacillus subtilis with MIC values at 7.81 μg/mL.

  3. Synthesis, characterization, antimicrobial and anthelmentic activities of some metal complexes with a new Schiff base 3-[(Z)-5-amino-1,3,3-trimethyl cyclohexylmethylimino]-1,3-dihydroindol-2-one

    International Nuclear Information System (INIS)

    Reddy, K. R. K; Mahendra, K.N.

    2008-01-01

    The complexes of Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II), dioxouranium(VI), and Th(IV) with a new Schiff base, 3-[(Z)-5-amino-1,3,3-trimethyl cyclohexylmethylimino]-1,3-dihydroindol-2-one formed by the condensation of isatin (Indole-2.3-dione) with isophoronediamine(5-amino-1,3,3-trimethyl-cyclohexane methylamine) were synthesized and characterized by microanalysis, conductivity, UV-visible, FT-IR, 1 H NMR, TGA, and magnetic susceptibility measurements. All the complexes exhibit 1: 1 metal to ligand ratio except for the dioxouranium(VI) and thorium(IV) complexes, where the metal: ligand stoichiometry is 1: 2. The spectral data revealed that the ligand acts as monobasic bidentate, coordinating to the metal ion through the azomethine nitrogen and carbonyl oxygen of the isatin moiety. Tetrahedral geometry for Co(II), Ni(II), Zn(II), Cd(II), and Hg(II) complexes, square planar geometry for Cu(II) complexes, and the coordination numbers 6 and 8 for UO 2 (VI) and Th(IV) complexes, respectively, are proposed. Both the ligand and the metal complexes were screened for their antibacterial activity against Bacillus subtilis, Staphylococcus aureus (S. aureus), Escherichia coli (E. coli), and Pseudomonas aeruginosa, and the complexes are more potent bactericides than the ligand. The anthelmintic activity of the ligand and its complexes against earthworms was also investigated [ru

  4. A study of the removal of heavy metals from aqueous solutions by Moringa oleifera seeds and amine-based ligand 1,4-bis[N,N-bis(2-picoyl)amino]butane

    Energy Technology Data Exchange (ETDEWEB)

    Obuseng, Veronica; Nareetsile, Florence [Department of Chemistry, University of Botswana, Private Bag UB 00704, Gaborone (Botswana); Kwaambwa, Habauka M., E-mail: hmkwaambwa@yahoo.com [Department of Chemistry, University of Botswana, Private Bag UB 00704, Gaborone (Botswana)

    2012-06-12

    Highlights: Black-Right-Pointing-Pointer Materials are effective and selective in simultaneous removal of heavy metal ions. Black-Right-Pointing-Pointer Use of composite adsorbent of both materials may result in more effective material. Black-Right-Pointing-Pointer Seeds biomass has various functional groups involves in metal removal. Black-Right-Pointing-Pointer Attainment of sorption equilibrium is rapid for the seeds biomass. Black-Right-Pointing-Pointer Seeds biomass effectiveness is not affected over wide effective pH range. - Abstract: Uptake for lead, copper, cadmium, nickel and manganese from aqueous solution using the Moringa oleifera seeds biomass (MOSB) and amine-based ligand (ABL) was investigated. Experiments on two synthetic multi-solute systems revealed that MOSB performed well in the biosorption and followed the decreasing orders Pb(II) > Cu(II) > Cd(II) > Ni(II) > Mn(II) and Zn(II) > Cu(II) > Ni(II). The general trend of the heavy metal ions uptake by the amine-based ligand followed decreased in the order Mn > Cd > Cu > Ni > Pb, which is the reverse trend for what was observed for MOSB. Comparing the single- and multi-metal solutions, there was no clear effect in the biosorption capacity of MOSB suggesting the presence of sufficient active binding sites for all metal ions studied. The MOSB performance is also not affected by pH in the range 3.5-8.

  5. Transition metal complexes of 5-bromosalicylidene-4-amino-3-mercapto-1,2,4-triazine-5-one: Synthesis, characterization, catalytic and antibacterial studies

    Directory of Open Access Journals (Sweden)

    AYALOOR SUBRAMANIAN RAMASUBRAMANIAN

    2011-01-01

    Full Text Available Transition metal complexes of 5-bromosalicylidene-4-amino-3-mercapto-1,2,4-triazine-5-one with metal precursors, such as Cu(II, Ni(II, Co(II and Pd(II, were synthesized and characterized by physico–chemical and spectroscopic techniques. All the complexes are of the ML type. Based on analytical, spectral data and magnetic moments, the Co(II and Ni(II complexes were assigned octahedral geometries, while the Cu (II and Pd(II complexes square planar. A study on the catalytic oxidation of benzyl alcohol, cyclohexanol, cinnamyl alcohol, 2-propanol and 2-methyl-1-propanol was performed with N-methylmorpholine-N-oxide (NMO as co-oxidant. All the complexes and their parent organic moiety were screened for their biological activity on several pathogenic bacteria and were found to possess appreciable bactericidal properties.

  6. New Mn(II, Ni(II, Cd(II, Pb(II complexes with 2-methylbenzimidazole and other ligands. Synthesis, spectroscopic characterization, crystal structure, magnetic susceptibility and biological activity studies

    Directory of Open Access Journals (Sweden)

    Shayma A. Shaker

    2016-11-01

    Full Text Available Synthesis and characterization of Mn(II, Ni(II, Cd(II and Pb(II mixed ligand complexes of 2-methylbenzimidazole with other ligands have been reported. The structure of the ligands and their complexes was investigated using elemental analysis, IR, UV–Vis, (1H, 13C NMR spectroscopy, molar conductivity and magnetic susceptibility measurements. In all the studies of complexes, the 2-methylbenzimidazole behaves as a neutral monodentate ligand which is coordinated with the metal ions through the N atom. While benzotriazole behaves as a neutral bidentate ligand which is coordinated with the Ni(II ion through the two N atoms. Moreover, the N-acetylglycine behaves as a bidentate ligand which is coordinated with the Mn(II, Ni(II and Pb(II ions through the N atom and the terminal carboxyl oxygen atom. The magnetic and spectral data indicate the tetrahedral geometry for Mn(II complex, irregular tetrahedral geometry for Pb(II complex and octahedral geometry for Ni(II complex. The X-ray single crystal diffraction method was used to confirm a centrosymmetric dinuclear Cd(II complex as each two metal ions are linked by a pair of thiocyanate N = S bridge. Two 2-methylbenzimidazole N-atom donors and one terminal thiocyanate N atom complete a highly distorted square pyramid geometry around the Cd atom. Besides, different cell types were used to determine the inhibitory effect of Mn(II, Ni(II, Cd(II and Pb(II complexes on cell growth using MTT assay. Cd(II complex showed cytotoxic effect on various types of cancer cell lines with different EC50 values.

  7. Interactions of nickel(II) with histones: enhancement of 2'-deoxyguanosine oxidation by Ni(II) complexes with CH3CO-Cys-Ala-Ile-His-NH2, a putative metal binding sequence of histone H3.

    Science.gov (United States)

    Bal, W; Lukszo, J; Kasprazak, K S

    1996-03-01

    Studies of 2'-deoxyguanosine oxidation by hydrogen peroxide in the presence of CH3CO-Cys-Ala-Ile-His-NH2 (CAIH) and/or NiCl2 have been carried out in 100 mM phosphate buffer (pH 7.4) at 37 degrees C. The dimeric CAIH oxidation product, CAIH disulfide, and its weak, octahedral Ni(II) complex, rather than the monomeric CAIH and its strong, square-planar Ni(II) complex, were found to be major catalysts of 8-oxo-2'-deoxyguanosine (8-oxo-dG) formation. The presence of Ni(II) largely enhanced 8-oxo-dG yield, especially at submillimolar concentrations of H2O2. The reaction was found not to involve detectable amounts of free radicals or Ni(III). These results, together with those published previously [Bal, W. et al. (1995) Chem. Res. Toxicol. 8, 683-692], lay a framework for the detailed investigations of the interactions of histone octamer with Ni(II) and other metal ions. They also suggest that molecular mechanisms of nickel carcinogenesis may involve oxidative damage processes catalyzed by weak Ni(II) complexes with cellular components.

  8. Nuevos receptores heteroditópicos derivados de urea con potencial aplicación en el reconocimiento selectivo de aniones y metabolitos fosfatados

    OpenAIRE

    Carreira Barral, Israel

    2016-01-01

    [Resumen]En la presente Tesis Doctoral se han desarrollado nuevas plataformas estructurales basadas en complejos de metales del bloque d (CoII, NiII, CuII y ZnII) con potencial aplicación en el reconocimiento selectivo de aniones y metabolitos con actividad biológica. Los sistemas diseñados se pueden clasificar como receptores heteroditópicos que incorporan, por un lado, una zona de reconocimiento catiónico [1,7-dioxa-4,10-diazaciclododecano, 1,4,7,10-tetraazaciclododecano (...

  9. Adsorption characteristics of Pb(II) and Cu(II) ions by domestic clays

    International Nuclear Information System (INIS)

    Kwon, Ee Yol; Noh, Hea Ran

    1990-01-01

    This investigation was carried out to study the adsorption characteristics of Pb(II) and Cu(II) ions in aqueous solution by using clays of Gampo 35, Bentonite (chulwon) and Mangwoon 95 which were dug in the country. As the results, the adsorption of metal ions clays were reached equilibrium by shaking for about 40-60 minutes. In acidic solution, the adsorptivity of clays was increased as pH increased, however, Gampo 35 showed the high adsorptivity over 90% even at pH2-3. Pb(II) ion showed better removal efficiency than Cu(II) ion. The adsorptivities of adsorbents showed following order: Gampo 35>Bentonite> Mangwoon 95. The adsorption isotherms of Pb(II) ion on clays were well fitted in Freundlich's equation. Freundlich constantstion isotherms of Pb(II) ion on clays were well fitted in Freundlich's equation. Freundlich constants (1/n) of Gampo 35, Bentonite and Mangwoon 95 were 0.195, 0.271 and 0.314, respectively.(Author)

  10. Thermodynamics of the Cu(II) adsorption on thin vanillin-modified chitosan membranes

    International Nuclear Information System (INIS)

    Cestari, Antonio R.; Vieira, Eunice F.S.; Mattos, Charlene R.S.

    2006-01-01

    In this work, low-density vanillin-modified thin chitosan membranes were synthesized and characterized. The membranes were utilized as adsorbent for the removal of Cu(II) from aqueous solutions. The experimental data obtained in batch experiments at different temperatures were fitted to the Langmuir and Freundlich isotherms to obtain the characteristic parameters of each model. The adsorption equilibrium data fitted well with the Langmuir model (average R 2 > 0.99). Interactions thermodynamic parameters (Δ int H, Δ int G, and Δ int S), as well as the interaction thermal effects (Q int ) were determined from T = (298 to 333) K. The thermodynamic parameters, the Dubinin-Radushkevick equation and the comparative values of Δ int H for some Cu(II)-adsorbent interactions suggested that the adsorption of Cu(II) ions to vanillin-chitosan membranes show average results for both the diffusional (endothermic) and chemical bonding (exothermic) processes in relation to the temperature range studied

  11. Structural and thermal characterization of ternary complexes of piroxicam and alanine with transition metals: Uranyl binary and ternary complexes of piroxicam. Spectroscopic characterization and properties of metal complexes

    Science.gov (United States)

    Mohamed, Gehad G.

    2005-12-01

    Ternary Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and UO 2(II) complexes with piroxicam (Pir) drug (H 2L 1) and dl-alanine (Ala) (HL 2) and also the binary UO 2(II) complex with Pir were studied. The structures of the complexes were elucidated using elemental, IR, molar conductance, magnetic moment, diffused reflectance and thermal analyses. The UO 2(II) binary complex was isolated in 1:2 ratio with the formula [UO 2(H 2L) 2](NO 3) 2. The ternary complexes were isolated in 1:1:1 (M:H 2L 1:L 2) ratios. The solid complexes were isolated in the general formulae [M(H 2L)(L 2)(Cl) n(H 2O) m]· yH 2O (M = Fe(III) ( n = 2, m = 0, y = 1), Co(II) ( n = 1, m = 1, y = 2) and Ni(II) ( n = 1, m = 1, y = 0)); [M(H 2L)(L 2)](X) z· yH 2O (M = Cu(II) (X = AcO, z = 1, y = 0), Zn(II) (X = AcO, z = 1, y = 3) and UO 2(II) (X = NO 3, z = 1, y = 2)). Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl-O groups, while Ala behaves as a uninegatively bidentate ligand coordinated to the metal ions via the deprotonated carboxylate-O and amino-N. The magnetic and reflectance spectral data show that the complexes have octahedral geometry except Cu(II) and Zn(II) complexes have tetrahedral structures. The thermal decomposition of the complexes was discussed in relation to structure, and the thermodynamic parameters of the decomposition stages were evaluated.

  12. Investigation of irradiated rats DNA in the presence of Cu(II) chelates of amino acids Schiff bases.

    Science.gov (United States)

    Karapetyan, N H; Torosyan, A L; Malakyan, M; Bajinyan, S A; Haroutiunian, S G

    2016-01-01

    The new synthesized Cu(II) chelates of amino acids Schiff bases were studied as a potential radioprotectors. Male albino rats of Wistar strain were exposed to X-ray whole-body irradiation at 4.8 Gy. This dose caused 30% mortality of the animals (LD30). The survival of animals exposed to radiation after preliminary administration of 10 mg/kg Cu(II)(Nicotinyl-L-Tyrosinate)2 or Cu(II)(Nicotinyl-L-Tryptophanate)2 prior to irradiation was registered about 80 and 100% correspondingly. Using spectrophotometric melting and agarose gel electrophoresis methods, the differences between the DNA isolated from irradiated rats and rats pretreated with Cu(II) chelates were studied. The fragments of DNA with different breaks were revealed in DNA samples isolated from irradiated animals. While, the repair of the DNA structure was observed for animals pretreated with the Cu(II) chelates. The results suggested that pretreatment of the irradiated rats with Cu(II)(Nicotinyl-L-Tyrosinate)2 and Cu(II)(Nicotinyl-L-Tryptophanate)2 compounds improves the liver DNA characteristics.

  13. Fabrication, characterization and sensing properties of Cu(II) ion imprinted sol–gel thin film on QCM

    International Nuclear Information System (INIS)

    Su, Pi-Guey; Hung, Fang-Chieh; Lin, Po-Hung

    2012-01-01

    Cu(II)-molecularly imprinted sol–gel films (Cu(II)-MISGF), coated on a quartz crystal microbalance (QCM) chip, were fabricated using a sol–gel procedure. Co-hydrolysis and co-condensation of Cu(II) (templates), 3-aminopropyltrimethoxysilane (APTS, functional monomer) and tetraethoxysilane (TEOS, cross-linking agent) were performed with acid and base catalysis. The properties of the Cu(II)-MISGF were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and the electrochemical methods of cyclic voltammetry (CV). Microstructural observations revealed that the acid-catalyzed system yielded more mechanically stable thin films. A combined Cu(II)-MISGF-QCM with flow injection analysis (FIA) method was utilized to investigate the sensing performance of the Cu(II)-MISGF, with special emphasis on the most important properties of sensitivity, selectivity and response time. The Cu(II)-MISGF-QCM sensor, at a TEOS/APTS molar ratio of 10, exhibited excellent selectivity and rapidly responded to Cu(II) ions. - Highlights: ► A Cu(II)-molecularly imprinted sol–gel thin film on chip was fabricated. ► The thin film had mechanical stability using acidic catalyst. ► The thin film had good selectivity and response time for Cu(II) ions.

  14. Adsorption and thermodynamic studies of Cu(II) and Zn(II) on organofunctionalized-kaolinite

    International Nuclear Information System (INIS)

    Guerra, Denis Lima; Airoldi, Claudio; Sousa, Kaline S. de

    2008-01-01

    Kaolinite-bearing clay samples from Perus, Sao Paulo state, Brazil, were used for chemical modification process with dimethyl sulfoxide and organofunctionalized with the silyating agent (RO) 3 Si(CH 2 ) 3 NH(CH 2 ) 2 NH 2 in the present study. The resulting material and natural kaolinite were subjected adsorpion process with Cu(II) and Zn(II) from aqueous solution at pH 6.0 and controlated temperature of 298 K. The Langmuir adsorption isotherm model has been applied to fit the experimental data. The results showed that the chemical modification process increases the basal spacing of the natural kaolinite from 0.711 to 0.955 nm. The energetic effects caused by Cu(II) and Zn(II) interactions were determined through calorimetric titration at the solid-liquid interface and gave a net thermal effect that enabled the calculation of the exothermic values and the equilibrium constant

  15. EPR interpretation, magnetism and biological study of a Cu(II) dinuclear complex assisted by a schiff base precursor.

    Science.gov (United States)

    Das, Kuheli; Patra, Chiranjit; Sen, Chandana; Datta, Amitabha; Massera, Chiara; Garribba, Eugenio; El Fallah, Mohamed Salah; Beyene, Belete B; Hung, Chen-Hsiung; Sinha, Chittaranjan; Askun, Tulin; Celikboyun, Pinar; Escudero, Daniel; Frontera, Antonio

    2017-06-01

    A new Cu(II) dinuclear complex, Cu 2 L 2 (1) was afforded employing the potentially pentatentate Schiff base precursor H 2 L, a refluxed product of o-vanillin and diethylenetriamine in methanol. Complex 1 was systematically characterized by FTIR, UV-Vis, emission and EPR spectrometry. The single crystal X-ray diffraction analysis of 1 reveals that the copper atom exhibits a distorted square planar geometry, comprising two pairs of phenolato-O and imine-N donors from two different H 2 L ligands. The temperature dependent magnetic interpretation agrees with the existence of weak antiferromagnetic interactions between the bridging dinuclear Cu(II) ions. A considerable body of experimental evidence has been accumulated to elucidate the magneto-structural relationship in this dinuclear Cu(II) complex by DFT computation. Both the ligand and complex 1 exhibit anti-mycobacterial activity and considerable efficacy on M. tuberculosis H 37 Ra (ATCC 25177) and M. tuberculosis H 37 Rv (ATCC 25618) strains. The practical applicability of the ligand and complex 1 has been examined in living cells (African Monkey Vero Cells). The MTT assay proves the non-toxicity of the probe up to 100 mg mL -1 . A new homometallic dinuclear Cu(II) complex is afforded with a tetradentate Schiff base precursor. EPR interpretation and temperature dependent magnetic studies show that complex 1 has weak antiferromagnetic coupling and DFT computation is governed to explain the magneto-structural correlation.

  16. Speciation of Co(II) and Ni(II) in anaerobic bioreactors measured by competitive ligand exchange - adsorptive stripping voltammetry

    NARCIS (Netherlands)

    Jansen, S.; Steffen, F.; Threels, W.F.; Leeuwen, van H.P.

    2005-01-01

    Competitive ligand exchange-adsorptive stripping voltammetry is applied to speciation analysis of dissolved Ni(II) and Co(II) in an anaerobic bioreactor and similar batch media. Co and Ni speciation in these media can be measured down to concentration levels of ca. 1 nM. Sulfide interference is

  17. H2S Sensing by Hybrids Based on Nanocrystalline SnO2 Functionalized with Cu(II Organometallic Complexes: The Role of the Ligand Platform

    Directory of Open Access Journals (Sweden)

    Marina Rumyantseva

    2017-11-01

    Full Text Available This paper deals with the functionalization of nanocrystalline SnO2 with Cu(II complexes with organic ligands, aimed at the improvement of sensor selectivity towards gas molecules. For the synthesis of metalorganic/SnO2 hybrid material complexes of Cu(II with phthalocyanine, porphyrinines, bipyridine and azadithiacrown etherwere used. The analysis of gas sensor properties showed the possibility of increasing the sensitivity and selectivity of hybrid materials in H2S detection due to the electron transfer from SnO2 to an adsorbed organic molecule, which changes during the interaction between H2S and Cu(II ions.

  18. Stability Studies of Transition Metal Chelates of 5-Bromosalicylidene-4-methoxyaniline andSalicylidene-2,3-dimethylaniline as Ligands

    Directory of Open Access Journals (Sweden)

    N. G. Nadkarni

    2011-01-01

    Full Text Available Binary and ternary complexes of the type M-Y and M-X-Y [M = Mn(II, Ni(II, Cu(II and Zn(II; X = 5-bromosalicylidene-4-methoxyaniline and Y = salicylidene-2,3-dimethylaniline] have been examined pH-metrically at 27±0.5 °C and at constant ionic strength, μ = 0.1 M (KCl in 75 : 25(v/v 1,4-dioxne-water medium. The stability constants for binary (M-Y and ternary (M-X-Y systems were calculated.

  19. Separación electrodialítica de Cu(II y As(V en electrolitos ácidos

    Directory of Open Access Journals (Sweden)

    Ibáñez, J. P.

    2007-02-01

    Full Text Available The separation of copper and arsenic from acidic electrolytes by electrodialysis was investigated at room temperature. The effect of current density and pH was studied in a batch cell during 3 hours. The kinetic parameters showed that Cu(II transport rate was 0.75 mol/m2/h and the As(V transport rate was 0.002 mol/m2/h. An efficient separation between Cu(II and As(V was achieved; generating a concentrated solution of copper with no arsenic, which was obtained independently of the electrolyte acidity and current density used. The effect of the arsenic speciation with pH is discussed as well.

    Se investigó el uso de la electrodiálisis para separar cobre y arsénico desde soluciones ácidas a temperatura ambiente. Se estudió el efecto de la densidad de corriente y grado de
    acidez del electrolito en la separación a través de experimentos en celda batch de 5 compartimientos durante 3 h. Los parámetros cinéticos indican que la velocidad de transporte de Cu(II fue de 0,75 mol/h/m2 y de As(V fue de 0,002 mol/h/m2 a una densidad de corriente de 225 A/m2. Se logró obtener una eficiente separación de Cu(II y As(V, con la generación de una solución concentrada de cobre sin presencia de arsénico, lo cual fue independiente del grado de acidez de la operación y de la densidad de corriente. El efecto de la distribución de las especies iónicas de As(V con el pH también se discute.

  20. Novel adsorptive ultrafiltration membranes derived from polyvinyltetrazole-co-polyacrylonitrile for Cu(II) ions removal

    KAUST Repository

    Kumar, Mahendra; Shevate, Rahul; Hilke, Roland; Peinemann, Klaus-Viktor

    2016-01-01

    Novel adsorptive ultrafiltration membranes were manufactured from synthesized polyvinyltetrazole−co−polyacrylonitrile (PVT−co−PAN) by nonsolvent induced phase separation (NIPS). PVT−co−PAN with various degree of functionalization (DF) was synthesized via a [3+2] cycloaddition reaction at 60°C using a commercial PAN. PVT−co−PAN with varied DF was then explored to prepare adsorptive membranes. The membranes were characterized by surface zeta potential and static water contact angle measurements, scanning electron microscopy as well as atomic force microscopy (AFM) techniques. It was shown that PVT segments contributed to alter the pore size, charge and hydrophilic behavior of the membranes. The membranes became more negatively charged and hydrophilic after addition of PVT segments. The PVT segments in the membranes served as the major binding sites for adsorption of Cu(II) ions from aqueous solution. The maximum adsorption of Cu(II) ions by the membranes in static condition and in a continuous ultrafiltration of 10 ppm solution was attained at pH = 5. The adsorption data suggest that the Freundlich isotherm model describes well Cu(II) ions adsorption on the membranes from aqueous solution. The adsorption capacity obtained from the Freundlich isotherm model was 44.3 mg g−1; this value is higher than other membrane adsorption data reported in the literature. Overall, the membranes fabricated from PVT−co−PAN are attractive for efficient removal of heavy metal ions under the optimized conditions.

  1. Novel adsorptive ultrafiltration membranes derived from polyvinyltetrazole-co-polyacrylonitrile for Cu(II) ions removal

    KAUST Repository

    Kumar, Mahendra

    2016-05-04

    Novel adsorptive ultrafiltration membranes were manufactured from synthesized polyvinyltetrazole−co−polyacrylonitrile (PVT−co−PAN) by nonsolvent induced phase separation (NIPS). PVT−co−PAN with various degree of functionalization (DF) was synthesized via a [3+2] cycloaddition reaction at 60°C using a commercial PAN. PVT−co−PAN with varied DF was then explored to prepare adsorptive membranes. The membranes were characterized by surface zeta potential and static water contact angle measurements, scanning electron microscopy as well as atomic force microscopy (AFM) techniques. It was shown that PVT segments contributed to alter the pore size, charge and hydrophilic behavior of the membranes. The membranes became more negatively charged and hydrophilic after addition of PVT segments. The PVT segments in the membranes served as the major binding sites for adsorption of Cu(II) ions from aqueous solution. The maximum adsorption of Cu(II) ions by the membranes in static condition and in a continuous ultrafiltration of 10 ppm solution was attained at pH = 5. The adsorption data suggest that the Freundlich isotherm model describes well Cu(II) ions adsorption on the membranes from aqueous solution. The adsorption capacity obtained from the Freundlich isotherm model was 44.3 mg g−1; this value is higher than other membrane adsorption data reported in the literature. Overall, the membranes fabricated from PVT−co−PAN are attractive for efficient removal of heavy metal ions under the optimized conditions.

  2. A novel Schiff-base as a Cu(II) ion fluorescent sensor in aqueous solution

    Science.gov (United States)

    Gündüz, Z. Yurtman; Gündüz, C.; Özpınar, C.; Urucu, O. Aydın

    2015-02-01

    A new fluorescent Cu(II) sensor (L) obtained from the Schiff base of 5,5‧-methylene-bis-salicylaldehyde with amidol (2,4-diaminophenol) was synthesized and characterized by FT-IR, MS, 1H NMR, 13C NMR techniques. In the presence of pH 6.5 (KHPO4-Na2HPO4) buffer solutions, copper reacted with L to form a stable 2:1 complex. Fluorescence spectroscopic study showed that Schiff base is highly sensitive towards Cu(II) over other metal ions (K+, Na+, Al3+, Ni2+, Co2+, Fe3+, Zn2+, Pb2+) in DMSO/H2O (30%, v/v). The sensor L was successfully applied to the determination of copper in standard reference material. The structural properties and molecular orbitals of the complex formed between L and Cu2+ ions were also investigated using quantum chemical computations.

  3. Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

    International Nuclear Information System (INIS)

    Saraji, Mohammad; Yousefi, Hamideh

    2009-01-01

    A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (α r ) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 μg L -1 using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

  4. Efficient removal of cobalt(II) and strontium(II) metals from water using ethylene diamine tetra-acetic acid functionalized graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Amer, Hany; Moustafa, Wafaa M. [Nuclar Fuel Cycle Department, Nuclear and Radiological Regulatory Authority (NRRA), Naser City, Cairo (Egypt); Farghali, Ahmed A.; El Rouby, Waleed M.A. [Materials Science and Nanotechnology Department, Faculty of Postgraduate Studies for Advanced Sciences (PASA), Beni-Suef University (Egypt); Khalil, Waleed F. [Nuclar Fuel Cycle Department, Nuclear and Radiological Regulatory Authority (NRRA), Naser City, Cairo (Egypt); Materials Science and Nanotechnology Department, Faculty of Postgraduate Studies for Advanced Sciences (PASA), Beni-Suef University (Egypt)

    2017-12-04

    Graphene oxide (GO) with high specific surface area was prepared and functionalized with ethylene diamine tetra-acetic acid (EDTA). The as-prepared GO and the functionalized one (GO-EDTA) were characterized using high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and Raman spectroscopy. The as-prepared and EDTA functionalized GO were applied as adsorbent to remove strontium(II) and cobalt(II) from water. The results indicated that the prepared materials are efficient adsorbents for strontium(II) and cobalt(II) removal. The adsorption of Co{sup II} and Sr{sup II} under effects of contact time, temperature, and pH was investigated It is concluded that the maximum adsorption capacities of GO for Co{sup II} and Sr{sup II} were about 168 and 140 mg.g{sup -1}, whereas of GO-EDTA the values were about 197 and 158 mg.g{sup -1}, respectively. It is indicated that pH 6 and temperature 40 C are the best condition for Co{sup II} and Sr{sup II} removal from water. The application of Langmuir and Freundlich isotherms indicated that Langmuir isotherm is best fit for Co{sup II} and Sr{sup II} equilibrium adsorption. Adsorption kinetics were studied by applying pseudo first-order, pseudo second-order, and intraparticle diffusion models on the experimental data. The results proved that pseudo second-order model is the best represented adsorption kinetics. Appling the intraparticle diffusion regressions on the experimental data indicated that intraparticle diffusion involved in adsorption process, which was not the only rate-controlling step. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. EPR-study of reversible oxygenation process of coordination compounds of cobalt(II) with S-substituted N/sup 1/,N/sup 4/-di(salicylidene)-isothiosemicarbazides

    Energy Technology Data Exchange (ETDEWEB)

    Gerbeleu, N.V.; Revenko, M.D.; Rusu, V.G.; Shames, A.T.

    1987-09-01

    The reaction between molecular oxygen and coordination compounds of cobalt(II) with S-substituted N/sup 1/,N/sup 4/-di(salicylidene)isothiosemicarbazides in dimethyl sulfoxide solution was studied by the EPR method. It was found that paramagnetic monomeric adducts and diamagnetic ..mu..-peroxo-dimers are formed. The spin-Hamiltonian parameters of the EPR spectra of the initial cobalt complexes, as well as of the paramagnetic adducts were determined. The nature of the Co-O/sub 2/ bond is discussed.

  6. Radiative parameters for some transitions in Cu(II) and Ag(II) spectrum

    International Nuclear Information System (INIS)

    Biemont, E.; Blagoev, K.; Campos, J.; Mayo, R.; Malcheva, G.; Ortiz, M.; Quinet, P.

    2005-01-01

    Radiative parameters for transitions depopulating the levels belonging to the 3d 8 4s 2 configuration of Cu(II) and 4d 9 6s and 4d 9 5d configurations of Ag(II) have been obtained both theoretically and experimentally. On the experimental side, a laser-produced plasma was used as a source of Cu(II) and Ag(II) spectra. The light emitted by the plasma was focused on the input slit of a grating monochromator coupled with a time-resolved optical multichannel analyzer system. Spectral response calibration of the experimental system was made using a deuterium lamp in the wavelength range extending from 200 to 400-bar nm, and a standard tungsten lamp in the range from 350 to 600-bar nm. The transition probabilities were obtained using measured branching fractions and available radiative lifetimes of the corresponding states. On the theoretical side, a relativistic Hartree-Fock (HFR) approach, including core-polarization effects, has been used for the calculations. A reasonable agreement theory-experiment has been observed

  7. Sorption of Pb(II and Cu(II by low-cost magnetic eggshells-Fe3O4 powder

    Directory of Open Access Journals (Sweden)

    Ren Jianwei

    2012-01-01

    Full Text Available This study explored the feasibility of using magnetic eggshell-Fe3O4 powder as adsorbent for the removal of Pb(II and Cu(II ions from aqueous solution. The metal ionsadsorption media interaction was characterized using XRD and FTIR. The effects of contact time, initial concentrations, temperature, solution pH and reusability of the adsorption media were investigated. The metal ions adsorption was fast and the amount of metal ions adsorbed increased with an increase in temperature, suggesting an endothermic adsorption. The kinetic data showed that the adsorption process followed the pseudo-second-order kinetic model. The optimal adsorption pH value was around 5.5 at which condition the equilibrium capacity was 263.2 mg/g for Pb(II and 250.0 for Cu(II. The adsorption equilibrium data fitted very well to the Langmuir and Freundlich adsorption isotherm models. The thermodynamics of Pb(II and Cu(II adsorption onto the magnetic eggshell-Fe3O4 powder indicated that the adsorption was spontaneous. The reusability study has proven that magnetic eggshell-Fe3O4 powder can be employed as a low-cost and easy to separate adsorbent.

  8. Molecular, crystal, and electronic structure of the cobalt(II) complex with 10-(2-benzothiazolylazo)-9-phenanthrol

    Energy Technology Data Exchange (ETDEWEB)

    Linko, R. V., E-mail: rlinko@mail.ru [Peoples' Friendship University of Russia (Russian Federation); Sokol, V. I. [Russian Academy of Sciences, Kurnakov Institute of General and Inorganic Chemistry (Russian Federation); Polyanskaya, N. A.; Ryabov, M. A.; Strashnov, P. V.; Davydov, V. V. [Peoples' Friendship University of Russia (Russian Federation); Sergienko, V. S. [Russian Academy of Sciences, Kurnakov Institute of General and Inorganic Chemistry (Russian Federation)

    2013-05-15

    The reaction of 10-(2-benzothiazolylazo)-9-phenanthrol (HL) with cobalt(II) acetate gives the coordination compound [CoL{sub 2}] {center_dot} CHCl{sub 3} (I). The molecular and crystal structure of I is determined by X-ray diffraction. The coordination polyhedron of the Co atom in complex I is an octahedron. The anion L acts as a tridentate chelating ligand and is coordinated to the Co atom through the phenanthrenequinone O1 atom and the benzothiazole N1 atom of the moieties L and the N3 atom of the azo group to form two five-membered metallocycles. The molecular and electronic structures of the compounds HL, L, and CoL{sub 2} are studied at the density functional theory level. The results of the quantum-chemical calculations are in good agreement with the values determined by X-ray diffraction.

  9. Molecular, crystal, and electronic structure of the cobalt(II) complex with 10-(2-benzothiazolylazo)-9-phenanthrol

    International Nuclear Information System (INIS)

    Linko, R. V.; Sokol, V. I.; Polyanskaya, N. A.; Ryabov, M. A.; Strashnov, P. V.; Davydov, V. V.; Sergienko, V. S.

    2013-01-01

    The reaction of 10-(2-benzothiazolylazo)-9-phenanthrol (HL) with cobalt(II) acetate gives the coordination compound [CoL 2 ] · CHCl 3 (I). The molecular and crystal structure of I is determined by X-ray diffraction. The coordination polyhedron of the Co atom in complex I is an octahedron. The anion L acts as a tridentate chelating ligand and is coordinated to the Co atom through the phenanthrenequinone O1 atom and the benzothiazole N1 atom of the moieties L and the N3 atom of the azo group to form two five-membered metallocycles. The molecular and electronic structures of the compounds HL, L, and CoL 2 are studied at the density functional theory level. The results of the quantum-chemical calculations are in good agreement with the values determined by X-ray diffraction.

  10. The Cu(II) affinity of the N-terminus of human copper transporter CTR1: Comparison of human and mouse sequences.

    Science.gov (United States)

    Bossak, Karolina; Drew, Simon C; Stefaniak, Ewelina; Płonka, Dawid; Bonna, Arkadiusz; Bal, Wojciech

    2018-05-01

    Copper Transporter 1 (CTR1) is a homotrimeric membrane protein providing the main route of copper transport into eukaryotic cells from the extracellular milieu. Its N-terminal extracellular domain, rich in His and Met residues, is considered responsible for directing copper into the transmembrane channel. Most of vertebrate CTR1 proteins contain the His residue in position three from N-terminus, creating a well-known Amino Terminal Cu(II)- and Ni(II)-Binding (ATCUN) site. CTR1 from humans, primates and many other species contains the Met-Asp-His (MDH) sequence, while some rodents including mouse have the Met-Asn-His (MNH) N-terminal sequence. CTR1 is thought to collect Cu(II) ions from blood copper transport proteins, including albumin, but previous reports indicated that the affinity of N-terminal peptide/domain of CTR1 is significantly lower than that of albumin, casting serious doubt on this aspect of CTR1 function. Using potentiometry and spectroscopic techniques we demonstrated that MDH-amide, a tripeptide model of human CTR1 N-terminus, binds Cu(II) with K of 1.3 × 10 13  M -1 at pH 7.4, ~13 times stronger than Human Serum Albumin (HSA), and MNH-amide is even stronger, K of 3.2 × 10 14  M -1 at pH 7.4. These results indicate that the N-terminus of CTR1 may serve as intermediate binding site during Cu(II) transfer from blood copper carriers to the transporter. MDH-amide, but not MNH-amide also forms a low abundance complex with non-ATCUN coordination involving the Met amine, His imidazole and Asp carboxylate. This species might assist Cu(II) relay down the peptide chain or its reduction to Cu(I), both steps necessary for the CTR1 function. Copyright © 2018 Elsevier Inc. All rights reserved.

  11. Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

    Science.gov (United States)

    Mandal, B; Roy, U S; Datta, D; Ghosh, N

    2011-08-19

    A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Stability constants of salicylate of zinc(II), cobalt(II), uranyl(II) and thorium(IV) by paper electrophoresis

    International Nuclear Information System (INIS)

    Singh, R.K.P.; Yadava, J.R.; Yadava, P.C.; Yadava, K.L.

    1983-01-01

    Stability constants of zinc(II), cobalt(II), uranyl(II) and thorium(IV) have been determined by paper electrophoresis. Salicylic acid (0.005 mol dm - 3 ) was added to the background electrolyte: 0.1 mol dm - 3 HClO 4 . The proportions of C 6 H 4 OHCOO - and C 6 H 4 OCOO/sup =/ were varied by changing the pH of the electrolyte. These anions yielded the complexes, ZnC 6 H 4 OHCOO + , CoC 6 H 4 OHCOO + , Th(C 6 H 4 OHCOO) 4 and UO 2 (C 6 H 4 OCOO) 2 /sup =/ whose stability constants are found to be 10/sup 3.1/, 10/sup 3.2/, 10/sup 11.6/ and 10/sup 22.2/, respectively (μ = 0.1, temp. 40 0 C). (author)

  13. Tetradentate-arm Schiff base derived from the condensation reaction of 3,3′-dihydroxybenzidine, glyoxal/diacetyl and 2-aminophenol: Designing, structural elucidation and properties of their binuclear metal(II complexes

    Directory of Open Access Journals (Sweden)

    E. Akila

    2017-05-01

    Full Text Available The novel binuclear Schiff base complexes were prepared by the reaction of 3,3′-dihydroxybenzidine, glyoxal/diacetyl and 2-aminophenol in 1:2:2 M ratio. The binucleating Schiff base ligand and its complexes of Cu(II, Ni(II and VO(II ions were characterized by elemental analysis, molar conductance, 1H NMR, infrared, electronic spectra, cyclic voltammetry, thermal, magnetic and EPR studies. The low molar conductance values of the complexes support the non-electrolytic in nature. In IR spectra, the comparison of shift in frequency of the complexes with the ligand reveals the coordination of donor atom to the metal atom. The binuclear nature of the complexes is assessed from their magnetic susceptibility values. The electronic and EPR spectra of the metal complexes provide information about the geometry of the complexes and are in good agreement with the proposed square planar geometry for Cu(II, Ni(II and square pyramidal for VO(II complexes. Molecular modeling has been used to suggest the structure of the complexes. The DNA cleavage ability of the complexes was monitored by gel electrophoresis using supercoiled pUC18 DNA. The metal complexes were screened for their antibacterial activities against pathogenic bacteria like Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae and Bacillus subtilis. The activity data show that the metal complexes are more potent activity than the parent Schiff base ligand against microorganisms.

  14. Assessment of heavy metal tolerance and hexavalent chromium reducing potential of Corynebacterium paurometabolum SKPD 1204 isolated from chromite mine seepage

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    Amal Kanti Paul

    2016-07-01

    Full Text Available Corynebacterium paurometabolum SKPD 1204 (MTCC 8730, a heavy metal tolerant and chromate reducing bacterium isolated from chromite mine seepage of Odisha, India has been evaluated for chromate reduction under batch culture. The isolate was found to tolerate metals like Co(II, Cu(II, Ni(II, Mn(II, Zn(II, Fe(III and Hg(II along with Cr(VI and was resistant to different antibiotics as evaluated by disc-diffusion method. The isolate, SKPD 1204 was found to reduce 62.5% of 2 mM Cr(VI in Vogel Bonner broth within 8 days of incubation. Chromate reduction capability of SKPD 1204 decreased with increase in Cr(VI concentration, but increased with increase in cell density and attained its maximum at 1010 cells/mL. Chromate reducing efficiency of SKPD 1204 was promoted in the presence of glycerol and glucose, while the highest reduction was recorded at pH 7.0 and 35 °C. The reduction process was inhibited by divalent cations Zn(II, Cd(II, Cu(II, and Ni(II, but not by Mn(II. Anions like nitrate, phosphate, sulphate and sulphite was found to be inhibitory to the process of Cr(VI reduction. Similarly, sodium fluoride, carbonyl cyanide m-chlorophenylhydrazone, sodium azide and N, N,-Di cyclohexyl carboiimide were inhibitory to chromate reduction, while 2,4-dinitrophenol appeared to be neither promotive nor inhibitory to the process.

  15. Impregnation of chelating agent 3,3-bis-N,N bis-(carboxymethylaminomethyl-o-cresolsulfonephthalein in biopolymer chitosan: adsorption equilibrium of Cu(II in aqueous medium

    Directory of Open Access Journals (Sweden)

    Luciano Vitali

    2006-06-01

    Full Text Available The aim of this study was to impregnate the chelating agent 3,3-bis-N,N,bis-(carboxymethylaminomethyl-o-cresolsulfonephthalein in chitosan and to investigate the adsorption of Cu(II ions. The chemical modification was confirmed by FTIR spectrometry, thermogravimetric analysis (TGA and energy dispersive x-ray spectroscopy (EDX. The adsorption studies were carried out with Cu(II ions in a batch process and were shown to be dependent on pH. The adsorption kinetics was tested using three models: pseudo first-order, pseudo second order and intraparticle diffusion. The experimental kinetics data were best fitted with the pseudo second-order model (R² = 0.999, which provided a rate constant, k2, of 1.21 x 10-3 g mg-1 min-1. The adsorption rate depended on the concentration of Cu(II ions on the adsorbent surface and on the quantity of Cu(II ions adsorbed at equilibrium. The Langmuir isotherm model provided the best fit for the equilibrium data in the concentration range investigated, with the maximum adsorption capacity being 81.0 mg of Cu(II per gram of adsorbent, as obtained from the linear equation of the isotherm. Desorption tests revealed that around 90% of the adsorbed metal was removed, using EDTA solution as the eluent. This result suggests that the polymeric matrix can be reused.

  16. Synthesis, Structural Characterization and Catalytic Activity of A Cu(II Coordination Polymer Constructed from 1,4-Phenylenediacetic Acid and 2,2’-Bipyridine

    Directory of Open Access Journals (Sweden)

    Wang Li-Hua

    2017-04-01

    Full Text Available In order to study the catalytic activity of Cu(II coordination polymer material, a novel 1D chained Cu(II coordination polymer material, [CuL(bipy(H2O5]n (A1 (H2L = 1,4-phenylenediacetic acid, bipy = 2,2’-bipyridine, has been prepared by the reaction of 1,4-phenylenediacetic acid, 2,2’-bipyridine, Cu(CH3COO2·H2O and NaOH. The composition of A1 was determined by elemental analysis, IR spectra and single crystal X-ray diffraction. The results of characterization show that each Cu(II atom adopts six-coordination and forms a distorted octahedral configuration. The catalytic activity and reusability of A1 catalyst for A3 coupling reaction of benzaldehyde, piperidine, and phenylacetylene have been investigated. And the results show that the Cu(II complex catalyst has good catalytic activity with a maximum yield of 54.3% and stability. Copyright © 2017 BCREC GROUP. All rights reserved Received: 21st October 2016; Revised: 17th November 2016; Accepted: 22nd November 2016 How to Cite: Li-Hua, W., Lei, L., Xin, W. (2017. Synthesis, Structural Characterization and Catalytic Activity of A Cu(II Coordination Polymer Constructed from 1,4-Phenylenediacetic Acid and 2,2’-Bipyridine. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (1: 113-118 (doi:10.9767/bcrec.12.1.735.113-118 Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.1.735.113-118

  17. Synthesis and Crystal Structures of Luminescent Mononuclear Ni(ii and Cd(ii Complexes with 1,10-phenanthroline

    Directory of Open Access Journals (Sweden)

    Ecaterina Tocana

    2017-12-01

    Full Text Available New supramolecular systems of Ni(II and Cd(II with 1,10-phenanthroline constructed by non-covalent interactions have been synthesized and characterized by single-crystal X-ray diffractometry. The smaller nickel(II ion forms a cis complex with outer-sphere perchlorates, while the cadmium(II ion forms a trans complex involving inner-sphere perchlorates. Both compoundsrevealintraligand-basedluminescentproperties.

  18. A treatise on benzimidazole based Schiff base metal(II) complexes accentuating their biological efficacy: Spectroscopic evaluation of DNA interactions, DNA cleavage and antimicrobial screening

    Energy Technology Data Exchange (ETDEWEB)

    Kumaravel, Ganesan; Raman, Natarajan, E-mail: ramchem1964@gmail.com

    2017-01-01

    Two novel imidazole derived Schiff bases, (Z)-1-(1H-benzo[d]imidazol-2-yl)-N-benzylidenemethanamine (L{sup 1}) and 1-(1H-benzo[d]imidazol-2-yl)-N-(4-nitrobenzylidene) methanamine, and a series of their transition metal complexes of the types [M(L{sup 1}){sub 2}]Cl{sub 2} and [M(L{sup 2}){sub 2}]Cl{sub 2} where, M = Cu(II), Ni(II), Co(II) and Zn(II) have been designed and synthesized. These compounds were characterized by various spectral and physicochemical data. UV–Vis, magnetic susceptibility and molar conductivity data indicate that all the complexes adopt square planar geometry. The EPR spectral data of the Cu(II) complexes have provided supportive evidence to the conclusion derived on the basis of electronic absorption and magnetic moment values. Moreover, the interaction of complexes with DNA via intercalation has been explored by absorption, fluorescence spectroscopy, cyclic voltammetry, viscosity and circular dichroism. Agarose gel electrophoresis technique reveals that the complexes are good metallonucleases. All the compounds have relatively high antibacterial and antifungal potencies. Among the metal complexes, Cu(II) complexes exhibit higher efficacy against all the pathogens. - Highlights: • Synthesis of new and efficient benzimidazole based DNA targeting complexes • Synthesis of efficient metallointercalators • Excellent DNA exploiting ability of Cu(II) complexes • Efficient antimicrobial agents against various pathogens.

  19. Cu(II) Binding to the Peptide Ala-His-His, a Chimera of the Canonical Cu(II)-Binding Motifs Xxx-His and Xxx-Zzz-His.

    Science.gov (United States)

    Gonzalez, Paulina; Vileno, Bertrand; Bossak, Karolina; El Khoury, Youssef; Hellwig, Petra; Bal, Wojciech; Hureau, Christelle; Faller, Peter

    2017-12-18

    Peptides and proteins with the N-terminal motifs NH 2 -Xxx-His and NH 2 -Xxx-Zzz-His form well-established Cu(II) complexes. The canonical peptides are Gly-His-Lys and Asp-Ala-His-Lys (from the wound healing factor and human serum albumin, respectively). Cu(II) is bound to NH 2 -Xxx-His via three nitrogens from the peptide and an external ligand in the equatorial plane (called 3N form here). In contrast, Cu(II) is bound to NH 2 -Xxx-Zzz-His via four nitrogens from the peptide in the equatorial plane (called 4N form here). These two motifs are not mutually exclusive, as the peptides with the sequence NH 2 -Xxx-His-His contain both of them. However, this chimera has never been fully explored. In this work, we use a multispectroscopic approach to analyze the Cu(II) binding to the chimeric peptide Ala-His-His (AHH). AHH is capable of forming the 3N- and 4N-type complexes in a pH dependent manner. The 3N form predominates at pH ∼ 4-6.5 and the 4N form at ∼ pH 6.5-10. NMR experiments showed that at pH 8.5, where Cu(II) is almost exclusively bound in the 4N form, the Cu(II)-exchange between AHH or the amidated AHH-NH 2 is fast, in comparison to the nonchimeric 4N form (AAH). Together, the results show that the chimeric AHH can access both Cu(II) coordination types, that minor changes in the second (or further) coordination sphere can impact considerably the equilibrium between the forms, and that Cu kinetic exchange is fast even when Cu-AHH is mainly in the 4N form.

  20. Nickel removal from exhausted electroplatting baths by using vegetable wastes

    OpenAIRE

    Martínez Martínez, María del Rosario; Villaescusa Gil, Isabel; Fiol Santalo, Núria; Miralles Esteban, Núria; Florido Pérez, Antonio

    2014-01-01

    During the last years our research group has been studying the use of industrial vegetable wastes as grape stalks and exhausted coffee to remove metals ions such as Ni(II), Cu(II), Pb(II), Zn(II), Cd(II) or Cr(VI) and Cr(III) in aqueous solution from the point of view to use these wastes as biosorbents in a low cost alternative to activated carbon for wastewater treatment. The optimal experimental conditions for the removal of each of these metal ions in synthetic solutions by using both bio...

  1. Stability Constants of Mixed Ligand Complexes of Transition Metal(II Ions with N-(2-Hydroxy-1-naphthylidene-2,6-diisopropylaniline as Primary Ligand and N-(2-Hydroxybenzylidene-2,3-dimethylaniline as Secondary Ligand

    Directory of Open Access Journals (Sweden)

    A. K. Mapari

    2011-01-01

    Full Text Available Binary and ternary complexes of the type M-Y and M-X-Y [M = Co(II, Ni(II, Cu(II and Zn(II; X = N-(2-hydroxy-1-naphthylidene-2,6-diisopropylaniline and Y = N-(2-hydroxybenzylidene-2,3-dimethylaniline] have been examined pH-metrically at 27±0.5 °C and µ = 0.1 M in 75: 25% (v/v 1,4-dioxne-water medium. The logarithms of the values of stability constants for binary (M-Y and for ternary (M-X-Y systems were calculated.

  2. Structural information on the coordination compounds formed by manganese(II), cobalt(II), nickel(II), zinc(II), cadmium(II) and mercury(II) thiocyanates with 4-cyanopyridine N-oxide from their magnetic moments, electronic and infrared spectra

    Science.gov (United States)

    Ahuja, I. S.; Yadava, C. L.; Singh, Raghuvir

    1982-05-01

    Coordination compounds formed by the interaction of 4-cyanopyridine. N-oxide (4-CPO), a potentially bidentate ligand, with manganese(II), cobalt(II), nickel(II), zinc(II), cadmium(II) and rnercury(II) thiocyanates have been prepared and characterized from their elemental analyses, magnetic susceptibilities, electronic and infrared spectral studies down to 200 cm -1 in the solid state. The compounds isolated are: Mn(4-CPO) 2(NCS) 2, Co(4-CPO) 2(NCS) 2,Ni(4-CPO) 2(NCS) 2,Zn(4-CPO) 2(NCS) 2, Cd(4-CPO)(NCS) 2 and Hg(4-CPO) 2(SCN) 2. It is shown that 4-CPO acts as a terminal N-oxide oxygen bonded monodentate ligand in all the metal(II) thiocyanate complexes studied. Tentative stereochemistries of the complexes in the solid state are discussed. The ligand field parameters 10 Dq, B, β and λ calculated for the manganese(II), cobalt(II) and nickel(II) complexes are consistent with their proposed stereochemistries.

  3. Syntheses, structures, and magnetic properties of cobalt(II) and nickel(II) coordination polymers based on a V-shaped ligand

    Energy Technology Data Exchange (ETDEWEB)

    Yao, Shuang [State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun 130022 (China); Yi, Fei-Yan [The School of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211 (China); Li, Guanghua [State Key Laboratory of Inorganic Synthesis & Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 (China); Yu, Yang [State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun 130022 (China); Wang, Jing-yuan, E-mail: jywang@mail.ipc.ac.cn [Technical Institute of Physics and Chemistry of the Chinese Academy of Sciences, 29 Zhongguancun East Road, Haidian District, Beijing 100190 (China); Liu, Dan, E-mail: liudan2007@ciac.ac.cn [State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun 130022 (China); Song, Shu-Yan [State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun 130022 (China)

    2017-06-15

    Two coordination polymers [Co{sub 2}(TA)(4,4′-bipy){sub 2}(H{sub 2}O){sub 2}]·H{sub 2}O (1) and [Ni{sub 2}(TA)(4,4′-bipy){sub 2}(H{sub 2}O){sub 4}]·3H{sub 2}O (2) were prepared by hydrothermal reactions of MCl{sub 2}·6H{sub 2}O (M = Co, Ni) with a V-shaped ligand TDPA (3,3′,4,4′-thiodiphthalic anhydride) and a I-shaped N-donor co-ligand (4,4′-bipy). They were characterized by elemental analyses, thermogravinetric analyses, and magnetic behavior. As is expected, TDPA hydrolyzes into the corresponding tetra-carboxylate acid H{sub 4}TA (3,3′,4,4′-thiodiphthalic acid) during the reactions. Co{sub 2} dimer and Ni mononuclear center are connected into two-dimensional (2D) layers by H{sub 4}TA and 4,4′-bipy bridge in 1 and 2, respectively. The most amazing feature is that 1 and 2 exhibit interesting spin-canting metamagnetism and weak ferromagnetic behavior, respectively, with the critical Néel temperature of T{sub N} =4 K for 1 and T{sub N} =13 K for 2, based on variable temperature magnetic susceptibility measurements. In low mono- or dinuclear metal system, such magnetic behaviors have rare been observed. Furthermore, complex 1 will be a potential metamagnet material. - Graphical abstract: Two Co(II) and Ni(II) coordination polymers were synthesized by hydrothermal reactions from a V-shape ligand (3,3′,4,4′-thiodiphthalic anhydride) and a I-shape ligand (4,4′-bipy), which were characterized by single crystal X-ray diffraction, elemental analyses, thermogravinetric analyses, and magnetic behavior, and exhibit interesting spin-canting metamagnetism and weak ferromagnetic behavior, respectively. - Highlights: • Two Co(II) and Ni(II) coordination polymers were successfully synthesized. • Co(II) coordination polymer shows an interesting spin-canting metamagnetism. • Ni(II) coordination polymer exhibits a weak ferromagnetic behavior.

  4. Separation and preconcentration of lead(II), cobalt(II), and nickel(II) on EDTA immobilized activated carbon cloth prior to flame atomic absorption spectrometric determination in environmental samples

    OpenAIRE

    ALOTHMAN, ZEID ABDULLAH; YILMAZ, ERKAN; HABİLA, MOHAMED; SOYLAK, MUSTAFA

    2015-01-01

    The synthesis and characterization of ethylenediaminetetraacetic acid immobilized activated carbon cloth was performed in the present work. It was used for preconcentration-separation of lead(II), cobalt(II), and nickel(II) at trace levels as an adsorbent. Factors including pH, concentration and volume of eluent, sample and eluent flow rates, sample volume, and effect of coexisting ions on the solid phase extraction of analytes were examined. The preconcentration factor was 50. The detection ...

  5. Cu(II Complexes of Isoniazid Schiff Bases: DNA/BSA Binding and Cytotoxicity Studies on A549 Cell Line

    Directory of Open Access Journals (Sweden)

    Pulipaka Ramadevi

    2014-01-01

    Full Text Available A series of isonicotinoyl hydrazones have been synthesized via template method and were complexed to Cu(II. The ligands are coordinated to Cu(II ion through the enolic oxygen and azomethine nitrogen resulting in a square planar geometry. The CT-DNA and bovine serum albumin binding propensities of the compounds were determined spectrophotometrically, the results of which indicate good binding propensity of complexes to DNA and BSA with high binding constant values. Furthermore, the compounds have been investigated for their cytotoxicities on A549 human lung cancer cell. Also the mode of cell death was examined employing various staining techniques and was found to be apoptotic.

  6. Cu(II complexes of an ionic liquid-based Schiff base [1-{2-(2-hydroxy benzylidene amino ethyl}-3-methyl­imidazolium]Pf6: Synthesis, characterization and biological activities

    Directory of Open Access Journals (Sweden)

    Saha Sanjoy

    2015-01-01

    Full Text Available Two Cu(II complexes of an ionic liquid based Schiff base 1-{2-(2-hydroxybenzylideneamino ethyl}-3-methylimidazolium hexaflurophosphate, were prepared and characterized by different analytical and spectroscopic methods such as elemental analysis, magnetic susceptibility, UV-Vis, IR, NMR and mass spectroscopy. The Schiff base ligand was found to act as a potential bidentate chelating ligand with N, O donor sites and formed 1:2 metal chelates with Cu(II salts. The synthesized Cu(II complexes were tested for biological activity.

  7. Spectroscopic, thermal, catalytic and biological studies of Cu(II) azo dye complexes

    Science.gov (United States)

    El-Sonbati, A. Z.; Diab, M. A.; El-Bindary, A. A.; Shoair, A. F.; Hussein, M. A.; El-Boz, R. A.

    2017-08-01

    New complexes of copper(II) with azo compounds of 5-amino-2-(aryl diazenyl)phenol (HLn) are prepared and investigated by elemental analyses, molar conductance, IR, 1H NMR, UV-Visible, mass, ESR spectra, magnetic susceptibility measurements and thermal analyses. The complexes have a square planar structure and general formula [Cu(Ln)(OAc)]H2O. Study the catalytic activities of Cu(II) complexes toward oxidation of benzyl alcohol derivatives to carbonyl compounds were tested using H2O2 as the oxidant. The intrinsic binding constants (Kb) of the ligands (HLn) and Cu(II) complexes (1-4) with CT-DNA are determined. The formed compounds have been tested for biological activity of antioxidants, antibacterial against Gram-positive (Staphylococcus aureus) and Gram-negative (Escherichia coli) bacteria and yeast Candida albicans. Antibiotic (Ampicillin) and antifungal against (Colitrimazole) and cytotoxic compounds HL1, HL2, HL3 and complex (1) showed moderate to good activity against S. aureus, E. coli and Candida albicans, and also to be moderate on antioxidants and toxic substances. Molecular docking is used to predict the binding between the ligands with the receptor of breast cancer (2a91).

  8. High-sensitivity determination of Zn(II) and Cu(II) in vitro by fluorescence polarization

    Science.gov (United States)

    Thompson, Richard B.; Maliwal, Badri P.; Feliccia, Vincent; Fierke, Carol A.

    1998-04-01

    Recent work has suggested that free Cu(II) may play a role in syndromes such as Crohn's and Wilson's diseases, as well as being a pollutant toxic at low levels to shellfish and sheep. Similarly, Zn(II) has been implicated in some neural damage in the brain resulting from epilepsy and ischemia. Several high sensitivity methods exist for determining these ions in solution, including GFAAS, ICP-MS, ICP-ES, and electrochemical techniques. However, these techniques are generally slow and costly, require pretreatment of the sample, require complex instruments and skilled personnel, and are incapable of imaging at the cellular and subcellular level. To address these shortcomings we developed fluorescence polarization (anisotropy) biosensing methods for these ions which are very sensitivity, highly selective, require simple instrumentation and little pretreatment, and are inexpensive. Thus free Cu(II) or Zn(II) can be determined at picomolar levels by changes in fluorescence polarization, lifetime, or wavelength ratio using these methods; these techniques may be adapted to microscopy.

  9. Electron paramagnetic resonance of Cu(II) and vibrational spectrum of chalcanthite

    International Nuclear Information System (INIS)

    Reddy, B.J.; Sreeramulu, P.; Ramesh, K.; Reddy, Y.P.; Botto, I.L.

    1988-01-01

    The EPR spectrum of Cu(II) in Chalcanthite has the characteristic features of D 4h symmetry. Optical and EPR results are correlated. The parameters g parallel, g perpendicular, k parallel and k perpendicular are evaluated. The nature of the bonding between the metal ion and the ligand environment is analized. On the other hand, the vibrational spectrum confirms the information about the site symmetry of the SO 4 group in the lattice. (Author) [es

  10. Stability constants of glutarate complexes of copper(II), zinc(II), cobalt(II) and uranyl(II) by paper electrophoresis

    International Nuclear Information System (INIS)

    Singh, R.K.P.; Yadava, J.R.; Yadava, K.L.

    1981-01-01

    Stability constants of Copper(II), Zinc(II), Cobalt(II) and Uranyl(II) glutarates have been determined by paper electrophoresis. Glutaric acid (0.005 mol dmsup(-3)) was added to the background electrolyte : 0.1 mol dmsup(-3) HClO 4 . The proportions of (CH 2 ) 3 COOH COO - and (CH 2 ) 3 C 2 O 4 2- were varied by changing the pH of the electrolyte. These anions yielded the complexes Cu(CH 2 ) 3 C 2 O 4 , [Zn(CH 2 ) 3 COOH COO] + [Co(CH 2 ) 3 COOH COO] + and UO 2 (CH 2 ) 3 C 2 O 4 whose stability constants are found to be 10sup(3.9), 10sup(2.9), 10sup(2.7) and 10sup(13.5) respectively. (author)

  11. Synthesis, crystallographic and spectral studies of homochiral cobalt(II) and nickel(II) complexes of a new terpyridylaminoacid ligand

    Science.gov (United States)

    Wang, Xing; Gao, Chang-Qing; Gao, Zhi-Yang; Wu, Ben-Lai; Niu, Yun-Yin

    2018-04-01

    Based on a chiral terpyridylaminoacid ligand, a series of homochiral Co(II) and Ni(II) complexes, namely, [Co(H2L)(HL)]·Cl·(PF6)2·2H2O (1), [Ni(H2L)(HL)]·Cl·(PF6)2 (2), [Co2(L)2(CH3OH)(H2O)]·(PF6)2·CH3OH (3), [Ni2(L)2(CH3OH)2]·(PF6)2·2CH3OH (4), [Co2(L)2(N3)2]·3H2O (5), and [Ni2(L)2(SCN)2]·4H2O (6) have been successfully synthesized and characterized by elemental analysis, TGA, spectroscopic methods (IR, CD and electronic absorption spectra) and single-crystal X-ray diffraction structural analysis (HL = (S)-2-((4-([2,2':6‧,2″-terpyridin]-4‧-yl)benzyl)amino)-4-methylpentanoic acid). In the acidic reaction conditions, one protonated (H2L)+ and one zwitterionic HL only used their terpyridyl groups to chelate one metal ion Co(II) or Ni(II), forming chiral mononuclear cationic complexes 1 or 2. But in the basic and hydro(solvo)thermal reaction conditions, deprotonated ligands (L)‒ acting as bridges used their terpyridyl and amino acid groups to link with two Co(II) or Ni(II) ions, fabricating chiral dinuclear metallocyclic complexes 3-6. Those chiral mononuclear and dinuclear complexes whose chirality originates in the homochiral ligand HL further self-assemble into higher-dimensional homochiral supramolecular frameworks through intermolecular hydrogen-bonding and π···π interactions. Notably, the coordination mode, hydrogen-bonding site, and existence form of HL ligand can be controlled by the protonation of its amino group, and the architectural diversity of those supramolecular frameworks is adjusted by pH and counter anions. Very interestingly, the 3D porous supramolecular frameworks built up from the huge chiral mononuclear cationic complexes 1 and 2 have novel helical layers only formed through every right-handed helical chain intertwining with two adjacent same helical chains, and the 2D supramolecular helicate 5 consists of two types of left-handed helical chains.

  12. Low-cost route for synthesis of mesoporous silica materials with high silanol groups and their application for Cu(II) removal

    International Nuclear Information System (INIS)

    Wang Yangang; Huang Sujun; Kang Shifei; Zhang Chengli; Li Xi

    2012-01-01

    Graphical abstract: A simple and low-cost route to synthesize mesoporous silica materials with high silanol groups has been demonstrated by means of a sol–gel process using citric acid as the template and acid catalyst, further studies on the adsorption of Cu(II) onto the representative amine-functionalized mesoporous silica showed that it had a high Cu(II) removal efficiency. Highlights: ► A low-cost route to synthesize mesoporous silica with high silanol groups was demonstrated. ► Citric acid as the template and acid catalyst for the reaction of tetraethylorthosilicate. ► Water extraction method was an effective technique to remove template which can be recycled. ► The mesoporous silica with high silanol groups was easily modified by functional groups. ► A high Cu(II) removal efficiency on the amine-functionalized mesoporous silica. - Abstract: We report a simple and low-cost route for the synthesis of mesoporous silica materials with high silanol groups by means of a sol–gel process using citric acid as the template, tetraethylorthosilicate (TEOS) as the silica source under aqueous solution system. The citric acid can directly work as an acid catalyst for the hydrolysis of TEOS besides the function as a pore-forming agent in the synthesis. It was found that by using a water extraction method the citric acid template in as-prepared mesoporous silica composite can be easily removed and a high degree of silanol groups were retained in the mesopores, moreover, the citric acid template in the filtrate can be recycled after being dried. The structural properties of the obtained mesoporous silica materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), and nitrogen adsorption–desorption analysis. Furthermore, an adsorption of Cu(II) from aqueous solution on the representative amine-functionalized mesoporous silica was investigated

  13. EPR of Cu(II) in sarcosine cadmium chloride: probe into dopant site - symmetry and copper-sarcosine interaction

    CERN Document Server

    Pathinettam-Padiyan, D; Murugesan, R

    2000-01-01

    The electron paramagnetic resonance spectra of Cu(II) doped sarcosine cadmium chloride single crystals have been investigated at room temperature. Experimental results reveal that the Cu(II) ion enters the lattice interstitially. The observed superhyperfine lines indicate the superposition of two sets of quintet structure with interaction of nitrogen atoms and the two isotopes of copper. The spin Hamiltonian parameters are evaluated by Schonland method and the electric field symmetry around the copper ion is rhombic. An admixture of d sub z sup 2 orbital with the d sub x sub sup 2 sub - sub y sub sup 2 ground state is observed. Evaluation of MO coefficients reveals that the in-plane interaction between copper and nitrogen is strong in this lattice.

  14. Enhanced selective removal of Cu(II) from aqueous solution by novel polyethylenimine-functionalized ion imprinted hydrogel: Behaviors and mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jingjing [State Key Laboratory of Pollutant Control and Resource Reuse, Nanjing 210023 (China); School of the Environment, Nanjing University, Nanjing 210023 (China); Li, Zhengkui, E-mail: zhkuili@nju.edu.cn [State Key Laboratory of Pollutant Control and Resource Reuse, Nanjing 210023 (China); School of the Environment, Nanjing University, Nanjing 210023 (China)

    2015-12-30

    Highlights: • A novel ion-imprinted poly(polyethylenimine/hydroxyethyl acrylate) hydrogel was synthesized. • The prepared hydrogel enhanced the selectivity of Cu(II) removal. • The material had high adsorption capacity and excellent regeneration property for copper. • The adsorption mechanism was the chelate interaction between functional groups and Cu(II) ions. - Abstract: A novel polyethylenimine-functionalized ion-imprinted hydrogel (Cu(II)-p(PEI/HEA)) was newly synthesized by {sup 60}Co-γ-induced polymerization for the selective removal of Cu(II) from aqueous solution. The adsorption performances including the adsorption capacity and selectivity of the novel hydrogel were much better than those of similar adsorbents reported. The hydrogel was characterized via scanning electron microscope, transmission electron microscopy, Fourier transform infrared spectra, thermal gravimetric analysis and X-ray photoelectron spectroscopy to determine the structure and mechanisms. The adsorption process was pH and temperature sensitive, better fitted to pseudo-second-order equation, and was Langmuir monolayer adsorption. The maximum adsorption capacity for Cu(II) was 40.00 mg/g. The selectivity coefficients of ion-imprinted hydrogel for Cu(II)/Pb(II), Cu(II)/Cd(II) and Cu(II)/Ni(II) were 55.09, 107.47 and 63.12, respectively, which were 3.93, 4.25 and 3.53 times greater than those of non-imprinted hydrogel, respectively. Moreover, the adsorption capacity of Cu(II)-p(PEI/HEA) could still keep more than 85% after four adsorption–desorption cycles. Because of such enhanced selective removal performance and excellent regeneration property, Cu(II)-p(PEI/HEA) is a promising adsorbent for the selective removal of copper ions from wastewater.

  15. On the biosorption, by brown seaweed, Lobophora variegata, of Ni(II) from aqueous solutions: equilibrium and thermodynamic studies.

    Science.gov (United States)

    Basha, Shaik; Jaiswar, Santlal; Jha, Bhavanath

    2010-09-01

    The biosorption equilibrium isotherms of Ni(II) onto marine brown algae Lobophora variegata, which was chemically-modified by CaCl(2) were studied and modeled. To predict the biosorption isotherms and to determine the characteristic parameters for process design, twenty-three one-, two-, three-, four- and five-parameter isotherm models were applied to experimental data. The interaction among biosorbed molecules is attractive and biosorption is carried out on energetically different sites and is an endothermic process. The five-parameter Fritz-Schluender model gives the most accurate fit with high regression coefficient, R (2) (0.9911-0.9975) and F-ratio (118.03-179.96), and low standard error, SE (0.0902-0.0.1556) and the residual or sum of square error, SSE (0.0012-0.1789) values to all experimental data in comparison to other models. The biosorption isotherm models fitted the experimental data in the order: Fritz-Schluender (five-parameter) > Freundlich (two-parameter) > Langmuir (two-parameter) > Khan (three-parameter) > Fritz-Schluender (four-parameter). The thermodynamic parameters such as DeltaG (0), DeltaH (0) and DeltaS (0) have been determined, which indicates the sorption of Ni(II) onto L. variegata was spontaneous and endothermic in nature.

  16. Fe3O4@SiO2@CS-TETA functionalized graphene oxide for the adsorption of methylene blue (MB) and Cu(II)

    Science.gov (United States)

    Wang, Fan; Zhang, Lijuan; Wang, Yeying; Liu, Xijian; Rohani, Sohrab; Lu, Jie

    2017-10-01

    The graphene oxide (GO) functionalized by Fe3O4@SiO2@CS-TETA nanoparticles, Fe3O4@SiO2@CS-TETA-GO, was firstly fabricated in a mild way as a novel adsorbent for the removal of Cu(II) ions and methylene blue (MB) from aqueous solutions. The magnetic composites showed a good dispersity in water and can be conveniently collected for reuse through magnetic separation due to its excellent magnetism. When the Fe3O4@SiO2@CS- TETA-GO was used as an absorbent for the absorption of MB and Cu(II), the adsorption kinetics and isotherms data well fitted the pseudo-second-order model and the Langmuir model, respectively. Under the optimized pH and initial concentration, the maximum adsorption capacity was about 529.1 mg g-1 for MB in 20 min and 324.7 mg g-1 for Cu(II) in 16 min, respectively, exhibiting a better adsorption performance than other GO-based adsorbents reported recently. More importantly, the synthesized adsorbent could be effectively regenerated and repeatedly utilized without significant capacity loss after six times cycles. All the results demonstrated that Fe3O4@SiO2@CS-TETA-GO could be used as an excellent adsorbent for the adsorption of Cu(II) and MB in many fields.

  17. Quantum chemical calculations and experimental investigations on 2-aminobenzoic acid-cyclodiphosph(V)azane derivative and its homo-binuclear Cu(II) complex

    Science.gov (United States)

    El-Gogary, Tarek M.; Alaghaz, Abdel-Nasser M. A.; Ammar, Reda A. A.

    2012-03-01

    A novel 2-aminobenzoic acid-cyclodiphosph(V)azane ligand H4L and its homo-binuclear Cu(II) complex of the type [Cu2L(H2O)2].2.5 H2O in which L is 1,3-di(-o-pyridyl)-2,4-(dioxo)-2',4'-bis-(2-iminobenzoic acid) cyclodiphosph(V)azane, were synthesized and characterized by different physical techniques. Infrared spectra of the complex indicate deprotonation and coordination of the imine NH and carboxyl COOH groups. It also confirms that nitrogen atom of the pyridine ring contribute to the complexation. Electronic spectra and magnetic susceptibility measurements reveal square-planar geometry for the Cu(II) complex. The elemental analyses and thermogravimetric results have justified the [Cu2L(H2O)2]·2.5H2O composition of the complex. Quantum chemical calculations were utilized to explore the electronic structure and stability of the H4L as well as the binuclear Cu(II) complex. Computational studies have been carried out at the DFT-B3LYP/6-31G(d) level of theory on the structural and spectroscopic properties of H4L and its binuclear Cu(II) complex. Different tautomers and geometrical isomers of the ligand were optimized at the ab initio DFT level. Simulated IR frequencies were scaled and compared with that experimentally measured. TD-DFT method was used to compute the UV-VIS spectra which show good agreement with measured electronic spectra.

  18. Equilibrium modeling of mono and binary sorption of Cu(II and Zn(II onto chitosan gel beads

    Directory of Open Access Journals (Sweden)

    Nastaj Józef

    2016-12-01

    Full Text Available The objective of the work are in-depth experimental studies of Cu(II and Zn(II ion removal on chitosan gel beads from both one- and two-component water solutions at the temperature of 303 K. The optimal process conditions such as: pH value, dose of sorbent and contact time were determined. Based on the optimal process conditions, equilibrium and kinetic studies were carried out. The maximum sorption capacities equaled: 191.25 mg/g and 142.88 mg/g for Cu(II and Zn(II ions respectively, when the sorbent dose was 10 g/L and the pH of a solution was 5.0 for both heavy metal ions. One-component sorption equilibrium data were successfully presented for six of the most useful three-parameter equilibrium models: Langmuir-Freundlich, Redlich-Peterson, Sips, Koble-Corrigan, Hill and Toth. Extended forms of Langmuir-Freundlich, Koble-Corrigan and Sips models were also well fitted to the two-component equilibrium data obtained for different ratios of concentrations of Cu(II and Zn(II ions (1:1, 1:2, 2:1. Experimental sorption data were described by two kinetic models of the pseudo-first and pseudo-second order. Furthermore, an attempt to explain the mechanisms of the divalent metal ion sorption process on chitosan gel beads was undertaken.

  19. Adsorption of Cd(II) and Cu(II) from aqueous solution by carbonate hydroxylapatite derived from eggshell waste

    International Nuclear Information System (INIS)

    Zheng Wei; Li Xiaoming; Yang Qi; Zeng Guangming; Shen Xiangxin; Zhang Ying; Liu Jingjin

    2007-01-01

    Carbonate hydroxylapatite (CHAP) synthesized by using eggshell waste as raw material has been investigated as metal adsorption for Cd(II) and Cu(II) from aqueous solutions. The effect of various parameters on adsorption process such as contact time, solution pH, amount of CHAP and initial concentration of metal ions was studied at room temperature to optimize the conditions for maximum adsorption. The results showed that the removal efficiency of Cd(II) and Cu(II) by CHAP could reach 94 and 93.17%, respectively, when the initial Cd(II) concentration 80 mg/L and Cu(II) 60 mg/L and the liquid/solid ratio was 2.5 g/L. The equilibrium sorption data for single metal systems at room temperature could be described by the Langmuir and Freundlich isotherm models. The highest value of Langmuir maximum uptake, (b), was found for cadmium (111.1 mg/g) and copper (142.86 mg/g). Similar Freundlich empirical constants, K, were obtained for cadmium (2.224) and copper (7.925). Ion exchange and surface adsorption might be involved in the adsorption process of cadmium and copper. Desorption experiments showed that CaCl 2 , NaCl, acetic acid and ultrasonic were not efficient enough to desorb substantial amount of metal ions from the CHAP. The results obtained show that CHAP has a high affinity to cadmium and copper

  20. Optical properties of 3d transition metal ion-doped sodium borosilicate glass

    International Nuclear Information System (INIS)

    Wen, Hongli; Tanner, Peter A.

    2015-01-01

    Graphical abstract: Photographs of undoped (SiO 2 ) 50 (Na 2 O) 25 (B 2 O 3 ) 25 (SiNaB) glass and transition metal ion-doped (TM) 0.5 (SiO 2 ) 49.5 (Na 2 O) 25 (B 2 O 3 ) 25 glass samples. - Highlights: • 3d transition metal ion (from Ti to Zn) doped SiO 2 -Na 2 O-B 2 O 3 glasses. • Optical properties of doped glasses investigated. • V(IV,V); Cr(III, VI); Mn(II,III); Fe(II,III); Co(II); Ni(II); Cu(II) by XANES, DRS. • Strong visible absorption but only vanadium ion gives strong emission in glass. - Abstract: SiO 2 -Na 2 O-B 2 O 3 glasses doped with 3d-transition metal species from Ti to Zn were prepared by the melting-quenching technique and their optical properties were investigated. The X-ray absorption near edge spectra of V, Cr, and Mn-doped glasses indicate that the oxidation states of V(IV, V), Cr(III, VI) and Mn(II, III) exist in the studied glasses. The oxidation states revealed from the diffuse reflectance spectra of the glasses are V(IV, V), Cr(III, VI), Mn(III), Fe(II, III), Co(II), Ni(II), and Cu(II). Most of the 3d transition element ions exhibit strong absorption in the visible spectral region in the glass. Under ultraviolet excitation, the undoped sodium borosilicate glass produces weak and broad emission, while doping of vanadium introduces strong and broad emission due to the V(V) charge transfer transition. Only weak emission is observed from Ti(IV), Mn(II), Fe(III) and Cu(II), partly resulting from the strong electron–phonon coupling of the 3d-electrons and the relatively high phonon energy of the studied glass host, with the former leading to dominant nonradiative relaxation based on multiphonon processes for most of the 3d excited states

  1. Controlling the oxidation of bis-tridentate cobalt(ii) complexes having bis(2-pyridylalkyl)amines: ligand vs. metal oxidation.

    Science.gov (United States)

    Anjana, S; Donring, S; Sanjib, P; Varghese, B; Murthy, Narasimha N

    2017-08-22

    Two bis-tridentate chelated cobalt(ii) complexes, which differ in the ligand structure by a methylene group, activate molecular oxygen (O 2 ), and give different oxidation products. The O 2 reaction of [Co II (pepma) 2 ] 2+ (1) with unsymmetrical 2-(2-pyridyl)-N-(2-pyridylmethyl)ethanamine (pepma) results in ligand oxidation, to the corresponding Co(ii) imine complex [Co II (pepmi) 2 ] 2+ (2). Contrastingly, the Co(ii) complex [Co II (bpma) 2 ] 2+ (3) of similar symmetrical bis(2-pyridylmethyl)amine (bpma), undergoes metal oxidation, yielding a cobalt(iii) complex, [Co III (bpma) 2 ] 2+ (4). The reversibility of the amine to imine conversion and the stability of the Co(ii) imine complex (2) are investigated. Furthermore, the solution dynamics of Co(ii) complexes are highlighted with the help of paramagnetic 1 H-NMR spectroscopy.

  2. Template synthesis, characterization and antimicrobial activity of some new complexes with isonicotinoyl hydrazone ligands

    Directory of Open Access Journals (Sweden)

    LIVIU MITU

    2009-09-01

    Full Text Available Complexes of Cu(II, Ni(II, Co(II with the 9-anthraldehyde iso-nicotinoyl hydrazone ligand (HL1 and the 3,5-di-tert-butyl-4-hydroxy-benzaldehyde isonicotinoyl hydrazone ligand (H2L2 were synthesized by the template method. The complexes were characterized by analytical analysis, IR, UV-Vis and ESR spectroscopy, magnetic measurements, conductometry and thermal analysis and the two ligands by 1H-NMR spectroscopy. From the elemental analysis, 1:2 (metal:ligand stoichiometry for the complexes of Cu(II, Ni(II with the ligands HL1 and H2L2 and 1:1 (metal:ligand stoichiometry for the complex of Co(II with the ligand HL1 are proposed. The molar conductance data showed that the complexes are non-electrolytes. The magnetic susceptibility results coupled with the electronic and ESR spectra suggested a distorted octahedral geometry for the complexes Ni(II/HL1, Ni(II/H2L2 and Cu(II/H2L2, a tetrahedral stereochemistry for the complex Cu/HL1 and a square-planar geometry for the complex Co/HL1. The IR spectra demonstrated the bidentate coordination of the ligands HL1 and H2L2 by the O=C amide oxygen and the azomethine nitrogen, as well as monodentate coordination of the ligand HL1 by the azomethine nitrogen in the Cu(IIcomplex. The antibacterial activity of the ligands and their metallic complexes were tested against Staphylococcus aureus, Escherichia coli and Klebsiella pneumoniae.

  3. Synthesis, structural, spectroscopic and biological studies of Schiff base complexes

    Science.gov (United States)

    Diab, M. A.; El-Sonbati, A. Z.; Shoair, A. F.; Eldesoky, A. M.; El-Far, N. M.

    2017-08-01

    Schiff base ligand 4-((pyridin-2- yl)methyleneamino)-1,2-dihydro-2,3-dimethyl-1-phenylpyrazol-5-one (PDMP) and its complexes were prepared and characterized on the basis of elemental analysis, IR, mass spectra and thermogravimetric analysis. All results confirm that the complexes have 1:1 (M: PMDP) stoichiometric formula [M(PMDP)Cl2H2O ] (M = Cu(II), Co(II), Ni(II) and Mn(II)), [Cd(PMDP)Cl2] and the ligand behaves as a bi/tridentate forming five-membered chelating ring towards the metal ions, bonding through azomethine nitrogen/exocyclic carbonyl oxygen, azomethine pyridine nitrogen and exocyclic carbonyl oxygen. The shift in the band positions of the groups involved in coordination has been utilized to estimate the metal-nitrogen and/or oxygen bond lengths. The complexes of Co(II), Ni(II) and Cu(II) are paramagnetic and the magnetic as well as spectral data suggest octahedral geometry, whereas the Cd(II) complex is tetrahedral. The XRD studies show that both the ligand and its metal complexes (1 and 3) show polycrystalline with crystal structure. Molecular docking was used to predict the binding between PMDP ligand and the receptors. The corrosion inhibition of mild steel in 2 M HCl solution by PDMP was explored utilizing potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and (EFM) electrochemical frequency modulation method. Potentiodynamic polarization demonstrated that PDMP compound is mixed-type inhibitor. EIS spectra exhibit one capacitive loop and confirm the protective ability. The percentage of inhibition efficiency was found to increase with increasing the inhibitor concentration.

  4. A study on adsorption of Pb(II), Cr(Ш) and Cu(II) from aqueous ...

    African Journals Online (AJOL)

    Peanut husk has been used in this work for removing Pb(II), Cr(Ш) and Cu(II) from aqueous solution. Batch adsorption studies were carried out under different pH, initial concentration of metal ions, interfering metal ions, time and temperature. Adsorption was poor in strongly acidic solution but was improved in alkaline ...

  5. Straightforward grafting approach for cyclam-functionalized screen-printed electrodes for selective Cu(II) determination

    International Nuclear Information System (INIS)

    Jasmin, Jean-Philippe; Ouhenia-Ouadahi, Karima; Miserque, Frédéric; Dumas, Eddy; Cannizzo, Caroline; Chaussé, Annie

    2016-01-01

    We report in this paper an original way to covalently bind the macrocyclic ligand, 1,4,8,11-tetraazacyclotetradecane (cyclam), through diazonium salt chemistry, on the surface of carbon screen-printed electrodes (SPEs). The in situ synthesis of the diazonium salt obtained from the amine precursor derived from the cyclam and its electrografting are described. X-ray Photoelectron Spectroscopy was used to characterize this functionalized surface. Owing to the strong cyclam–Cu(II) affinity, the so called SPE-cyclam can be used as electrochemical sensors for Cu(II) determination at trace levels. The influence of electroanalysis parameters such as the accumulation time and the pH of the medium were investigated. An interference study was carried out with numerous metallic cations and few interference was found for Cu(II) quantification. The described method provided a limit of detection and a limit of quantification of 1.3 × 10"−"8 M and 4.0 × 10"−"8 M, respectively. Interference study and performances show that SPE-cyclam could be considered as efficient sensors for environmental analysis.

  6. FORMATION OF BINARY COMPLEXES OF Co(II), Ni(II) AND Cu(II ...

    African Journals Online (AJOL)

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    adverse effects and decreasing the availability of dopamine to the CNS; so it is the ... Cobalt is essential for the production of red blood cells and cobalamin and it acts as the substrate for the final enzymatic reaction that yields the active coenzyme ..... competition between hydrogen and metal ion for this second donor site.

  7. Metal chelates of some transition and non-transition metal ions with Schiff base derived from isatin with o-phenylenediamine

    International Nuclear Information System (INIS)

    Hassaan, A.M.A.; Khalifa, M.A.

    1993-01-01

    New Cr(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II) chelates of the Schiff base derived from isatin with o-phenylenediamine have been synthesized and characterized on the basis of elemental analyses, electronic, IR and 1 H NMR spectra, and also by aid of molar conductivity and magnetic moment measurements. It has been found that the Schiff base behaves as ONNO tetradentate dibasic ligand forming chelates with 1:1 (metal:ligand) stoichiometry. Square planar environment is suggested for nickel(II) chelate. All the metal chelates show non-electrolytic behaviour

  8. Transition metal M(II complexes with isonicotinoylhydrazone-9-anthraldehyde

    Directory of Open Access Journals (Sweden)

    Dianu M.L.

    2010-01-01

    Full Text Available New complexes of isonicotinoylhydrazone-9-anthraldehyde with Cu(II, Co(II and Ni(II have been prepared and characterized by analytical and physico-chemical techniques, such as elemental and thermal analyses, magnetic susceptibility and conductivity measurements, and electronic, EPR and IR spectral studies. The infrared spectral studies revealed the bidentate or monodentate nature of the Schiff base in the complexes; the pyridine nitrogen does not participate in the coordination. A tetrahedral geometry is suggested for the nitrate-complexes and an octahedral geometry for the others. Thermal studies support the chemical formulation of these complexes.

  9. Electrochemical behavior of free-radical derivatives of tetra(4hydroxyl-3,5-di-tert-butylphenyl) porphyrin

    Energy Technology Data Exchange (ETDEWEB)

    Pokhodenko, V.D.; Melezhik, A.V.; Platonova, E.P.; Vovk, D.N.

    1984-08-01

    The electrochemical behavior of free-radical derivatives of tetra(4hydroxyl-3,5-di-tert-butylphenyl) porphyrins and their complexes with Mg(II), Zn(II), Ni(II), CU(II), and Pd(II) ions was studied by the methods of voltamperometry, ESR, and spectrophotometry. It was shown that the introduction of free-radical substituents into the porphin macrocycle leads to a substantial decrease in the oxidation and reduction potentials of the complexes. The degree of conjunction of substituents with the porphin macrocycle is estimated according to the difference of the redox potentials of free-radical and quinoid derivatives of metalloporphyrins.

  10. Study of the relationship between chemical structure and antimicrobial activity in a series of hydrazine-based coordination compounds.

    Science.gov (United States)

    Dobrova, B N; Dimoglo, A S; Chumakov, Y M

    2000-08-01

    The dependence of antimicrobial activity on the structure of compounds is studied in a series of compounds based on hydrazine coordinated with ions of Cu(II), Ni(II) and Pd(II). The study has been carried out by means of the original electron-topological method developed earlier. A molecular fragment has been found that is only characteristic of biologically active compounds. Its spatial and electron parameters have been used for the quantitative assessment of the activity in view. The results obtained can be used for the antimicrobial activity prediction in a series of compounds with similar structures.

  11. IR, UV-Vis, magnetic and thermal characterization of chelates of some catecholamines and 4-aminoantipyrine with Fe(III) and Cu(II)

    Science.gov (United States)

    Mohamed, Gehad G.; Zayed, M. A.; El-Dien, F. A. Nour; El-Nahas, Reham G.

    2004-07-01

    The dopamine derivatives participate in the regulation of wide variety of physiological functions in the human body and in medication life. Increase and/or decrease in the concentration of dopamine in human body reflect an indication for diseases such as Schizophrenia and/or Parkinson diseases. α-Methyldopa (α-MD) in tablets is used in medication of hypertension. The Fe(III) and Cu(II) chelates with coupled products of adrenaline hydrogen tartarate (AHT), levodopa (LD), α-MD and carbidopa (CD) with 4-aminoantipyrine (4-AAP) are prepared and characterized. Different physico-chemical methods like IR, magnetic and UV-Vis spectra are used to investigate the structure of these chelates. Fe(III) form 1:2 (M:catecholamines) chelates while Cu(II) form 1:1 chelates. Catecholamines behave as a bidentate mono- or dibasic ligands in binding to the metal ions. IR spectra show that the catecholamines are coordinated to the metal ions in a bidentate manner with O,O donor sites of the phenolic - OH. Magnetic moment measurements reveal the presence of Fe(III) chelates in octahedral geometry while the Cu(II) chelates are square planar. The thermal decomposition of Fe(III) and Cu(II) complexes is studied using thermogravimetric (TGA) and differential thermal analysis (DTA) techniques. The water molecules are removed in the first step followed immediately by decomposition of the ligand molecules. The activation thermodynamic parameters, such as, energy of activation, enthalpy, entropy and free energy change of the complexes are evaluated and the relative thermal stability of the complexes are discussed.

  12. Adsorption of tetracycline on soil and sediment: Effects of pH and the presence of Cu(II)

    International Nuclear Information System (INIS)

    Zhang Zheyun; Sun Ke; Gao Bo; Zhang Guixiang; Liu Xitao; Zhao Ye

    2011-01-01

    Tetracycline (TC) is frequently detected in the environment, however, knowledge on the environmental fate and transport of TC is still limited. Batch adsorption experiments of TC by soil and sediment samples were conducted. The distribution of charge and electrostatic potential of individual atoms of various TC species in the aqueous solution were determined using MOPAC version 0.034 W program in ChemBio3D Ultra software. Most of the adsorption isotherms on the soil, river and marine sediments were well fitted with the Freundlich and Polanyi-Manes (PMM) models. The single point organic carbon (OC)-normalized adsorption distribution coefficients (K OC ) and PMM saturated adsorption capacity (Q OC 0 ) values of TC were associated with the mesopore volume and clay content to a greater extent, indicating the mesopore volume of the soil and sediments and their clay content possibly influenced the fate and transport of TC in the natural environment. The adsorption of TC on soil and sediments strongly depended on the pH and presence of Cu(II). The presence of Cu(II) facilitated TC adsorption on soil and sediments at low pH (pH < 5), possibly due to the metallic complexation and surface-bridging mechanism by Cu(II) adsorption on soil and sediments. The cation exchange interaction, metallic complexation and Coulombic interaction of mechanisms for adsorption of TC to soils and sediments were further supported by quantum chemical calculation of various TC species in different pH.

  13. Preparation and characterization of trihydroxamic acid functionalized carbon materials for the removal of Cu(II) ions from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Godino-Salido, M. Luz, E-mail: mlgodino@ujaen.es [Departamento de Química Inorgánica y Orgánica, Facultad de Ciencias Experimentales, Universidad de Jaén, 23071, Jaén (Spain); Santiago-Medina, Antonio; López-Garzón, Rafael; Gutiérrez-Valero, María D.; Arranz-Mascarós, Paloma; López de la Torre, M. Dolores [Departamento de Química Inorgánica y Orgánica, Facultad de Ciencias Experimentales, Universidad de Jaén, 23071, Jaén (Spain); Domingo-García, María; López-Garzón, F. Javier [Departamento de Química Inorgánica, Facultad de Ciencias, Universidad de Granada, 18071, Granada (Spain)

    2016-11-30

    Highlights: • Hybrid materials made by irreversible adsorption of a deferoxamine derivative on ACs. • The surface trihydroxamate groups are the active functions of the hybrid materials. • Great adsorption capacity for Cu(II) of novel trihydroxamic acid functionalized ACs. • Desorption of Cu(II) from the loaded hybrid materials regenerates the parent hybrids. - Abstract: The main objective of this study is to prepare and characterize two functionalizated carbon materials with enhanced adsorptive properties for Cu(II). Thus, two novel hybrid materials have been prepared by a non-covalent functionalization method based on the adsorption of a pyrimidine-desferrioxamine-B conjugate compound (H{sub 4}L) on two activated carbons, ACs (labelled Merck and F). The adsorption of H{sub 4}L on the ACs is pH-dependent and highly irreversible. This is due to strong π-π interactions between the arene centers of the ACs and the pyrimidine moiety of H{sub 4}L. The textural characterization of the AC/H{sub 4}L hybrids shows large decreases of their surface areas. Thus the values of Merck and F are 1031 and 1426 m{sup 2}/g respectively, while these of Merck/H{sub 4}L and F/H{sub 4}L hybrids are 200 and 322 m{sup 2}/g. An important decrease in the micropore volumes is also found, due to the blockage of narrow porosity produced by the adsorption of H{sub 4}L molecules. The ACs/H{sub 4}L hybrids show larger adsorption capacities for Cu(II) (0.105(4) and 0.13(2) mmol/g, at pH 2.0, and 0.20(3) and 0.242(9) mmol/g, at pH 5.5, for Merck/H{sub 4}L and F/H{sub 4}L, respectively) than those of the ACs (0.024(6) and 0.096(9) mmol/g, at pH 2.0, and 0.10(2) and 0.177(8) mmol/g, at pH 5.5, for Merck and F respectively), which is explained on the basis of the complexing ability of the trihydroxamic acid functions. The desorption of Cu(II) from the ACs/H{sub 4}L/Cu(II) materials in acid solution allows the regeneration of most active sites (78.5% in the case of Merck/H{sub 4}L/Cu(II) and 83

  14. Contact angle study on the activation mechanisms of sphalerite with Cu(II) and Pb(II); Estudio de los mecanismos de activacion de la esfalerita con Cu(II) y Pb(II)

    Energy Technology Data Exchange (ETDEWEB)

    Davila Pulido, G. I.; Uribe Salas, A.

    2011-07-01

    This article presents results of an experimental study on the sphalerite activation with Cu(II) and Pb(II), whose main objective was to investigate the activation mechanisms and to evaluate the magnitude of the hydrophobization achieved with both chemical species. The hydrophobicity acquired by the mineral due to the interaction with the activator and collector (sodium isopropyl xanthate) is characterized making use of the contact angle technique. The results show that Cu(II) replaces the Zn of the external layers of the mineral, promoting the sulfide (S{sup 2}-) oxidation to produce a mixture of CuS, Cu{sub 2}S and S{sup o}, of hydrophobic nature. The subsequent interaction with xanthate increases the hydrophobicity of the mineral surface. In turn, Pb(II) activation of sphalerite is due to the formation of a PbS layer that reacts with xanthate to produce hydrophobic species (e.g., PbX{sub 2}). It is also observed that the hydrophobicity of sphalerite activated with Pb(II) is favored under air atmospheres, as compared to that obtained under nitrogen atmospheres. It is concluded that the hydrophobicity achieved by lead activation may be of the same order of magnitude to that deliverately induced by copper activation. (Author) 11 refs.

  15. Removal of Pb(II), Cu(II) and Cd(II) from aqueous solution by some fungi and natural adsorbents in single and multiple metal systems

    International Nuclear Information System (INIS)

    Shoaib, A.; Badar, T.; Aslam, N.

    2011-01-01

    Six fungal and 10 natural biosorbents were analyzed for their Cu(II), Cd(II) and Pb(II) uptake capacity from single, binary and ternary metal ion system. Preliminary screening biosorption of assays revealed 2 fungi (Aspergillus niger and Cunninghamella echinulata) and three natural [Cicer arietinum husk, Moringa oleifera flower and soil (clay)] adsorbents hold considerable high adsorption efficiency and capacity for 3 meta l ions amongst the adsorbents. Further biosorption trials with five elected adsorbents showed a considerable reduction in metal uptake capability of adsorbents in binary- and ternary systems as compared to singly metal system. Cd(II) manifested the highest inhibitory effect on the biosorption of other metal ions, followed by Pb(II) and Cu(II). On account of metal preference, the selectivity order for metal ion towards the studied biomass matrices was Pb(II) (40-90%) > Cd(II) (2-53%) > Cu(II) (2-30%). (author)

  16. Removal of Ni(II), Zn(II) and Pb(II) ions from single metal aqueous solution using rice husk-based activated carbon

    Energy Technology Data Exchange (ETDEWEB)

    Taha, Mohd F., E-mail: faisalt@petronas.com.my; Shaharun, Maizatul S. [Fundamental and Applied Sciences Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750, Perak Darul Ridzuan (Malaysia); Shuib, Anis Suhaila, E-mail: anisuha@petronas.com.my; Borhan, Azry [Chemical Engineering Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750, Perak Darul Ridzuan (Malaysia)

    2014-10-24

    An attempt was made to investigate the potential of rice husk-based activated carbon as an alternative low-cost adsorbent for the removal of Ni(II), Zn(II) and Pb(II) ions from single aqueous solution. Rice husk-based activated carbon was prepared via treatment of rice husk with NaOH followed by the carbonization process at 400°C for 2 hours. Three samples, i.e. raw rice husk, rice husk treated with NaOH and rice husk-based activated carbon, were analyzed for their morphological characteristics using field-emission scanning electron microscope/energy dispersive X-ray (FESEM/EDX). These samples were also analyzed for their carbon, hydrogen, nitrogen, oxygen and silica contents using CHN elemental analyzer and FESEM/EDX. The porous properties of rice husk-based activated carbon were determined by Brunauer-Emmett-Teller (BET) surface area analyzer, and its surface area and pore volume were 255 m{sup 2}/g and 0.17 cm{sup 2}/g, respectively. The adsorption studies for the removal of Ni(II), Zn(II) and Pb(II) ions from single metal aqueous solution were carried out at a fixed initial concentration of metal ion (150 ppm) with variation amount of adsorbent (rice husk-based activated carbon) as a function of varied contact time at room temperature. The concentration of each metal ion was analyzed using atomic absorption spectrophotometer (AAS). The results obtained from adsorption studies indicate the potential of rice husk as an economically promising precursor for the preparation of activated carbon for removal of Ni(II), Zn(II) and Pb(II) ions from single aqueous solution. Isotherm and kinetic model analyses suggested that the experimental data of adsorption studies fitted well with Langmuir, Freundlich and second-order kinetic models.

  17. Pecan nutshell as biosorbent to remove Cu(II), Mn(II) and Pb(II) from aqueous solutions.

    Science.gov (United States)

    Vaghetti, Julio C P; Lima, Eder C; Royer, Betina; da Cunha, Bruna M; Cardoso, Natali F; Brasil, Jorge L; Dias, Silvio L P

    2009-02-15

    In the present study we reported for the first time the feasibility of pecan nutshell (PNS, Carya illinoensis) as an alternative biosorbent to remove Cu(II), Mn(II) and Pb(II) metallic ions from aqueous solutions. The ability of PNS to remove the metallic ions was investigated by using batch biosorption procedure. The effects such as, pH, biosorbent dosage on the adsorption capacities of PNS were studied. Four kinetic models were tested, being the adsorption kinetics better fitted to fractionary-order kinetic model. Besides that, the kinetic data were also fitted to intra-particle diffusion model, presenting three linear regions, indicating that the kinetics of adsorption should follow multiple sorption rates. The equilibrium data were fitted to Langmuir, Freundlich, Sips and Redlich-Peterson isotherm models. Taking into account a statistical error function, the data were best fitted to Sips isotherm model. The maximum biosorption capacities of PNS were 1.35, 1.78 and 0.946mmolg(-1) for Cu(II), Mn(II) and Pb(II), respectively.

  18. Complex Formation in a Liquid-Liquid Extraction System Containing Cobalt(II, 4-(2-Pyridylazoresorcinol, and Nitron

    Directory of Open Access Journals (Sweden)

    Petya Vassileva Racheva

    2013-01-01

    Full Text Available Complex formation and liquid-liquid extraction were studied in a system containing cobalt(II, 4-(2-pyridylazoresorcinol (PAR, 1,4-diphenyl-3-(phenylamino-1H-1,2,4-triazole (Nitron, Nt, water, and chloroform. The effect of some experimental parameters (pH, shaking time, concentration of PAR, and concentration of Nt was systematically investigated, and the optimum conditions for cobalt extraction as an ion-association complex, (NtH+[Co3+(PAR2], were found. The following key equilibrium constants were calculated: constant of association (Log β=4.77±0.06, constant of distribution (LogKD=1.34±0.01, and constant of extraction (LogKex=6.11±0.07. Beer’s law was obeyed for Co concentrations up to 1.7 μg mL−1 with a molar absorptivity of 6.0×104 L mol−1 cm−1 at λmax=520 nm. Some additional characteristics, such as limit of detection, limit of quantification, and Sandell’s sensitivity, were estimated as well.

  19. Highly luminescent colloidal Eu(3)+-doped KZnF(3) nanoparticles for the selective and sensitive detection of Cu(II) ions.

    Science.gov (United States)

    Sarkar, Shyam; Chatti, Manjunath; Mahalingam, Venkataramanan

    2014-03-17

    This article describes a green synthetic approach to prepare water dispersible perovskite-type Eu3+-doped KZnF3 nanoparticles, carried out using environmentally friendly microwave irradiation at low temperature (85 8C) with water as a solvent. Incorporation of Eu3+ ions into the KZnF3 matrix is confirmed by strong red emission upon ultraviolet (UV) excitation of the nanoparticles. The nanoparticles are coated with poly(acrylic acid) (PAA), which enhances the dispersibility of the nanoparticles in hydrophilic solvents. The strong red emission from Eu3+ ions is selectively quenched upon addition of CuII ions, thus making the nanoparticles a potential CuII sensing material. This sensing ability is highly reversible by the addition of ethylenediaminetetraacetic acid (EDTA), with recovery of almost 90% of the luminescence. If the nanoparticles are strongly attached to a positively charged surface, dipping the surface in a CuII solution leads to the quenching of Eu3+ luminescence, which can be recovered after dipping in an EDTA solution. This process can be repeated for more than five cycles with only a slight decrease in the sensing ability. In addition to sensing, the strong luminescence from Eu3+-doped KZnF3 nanoparticles could be used as a tool for bioimaging.

  20. Synthesis and characterization of nickel(II), cobalt(II), copper(II), manganese(II), zinc(II), zirconium(IV), dioxouranium(VI) and dioxomolybdenum(VI) complexes of a new Schiff base derived from salicylaldehyde and 5-methylpyrazole-3-carbohydrazide

    International Nuclear Information System (INIS)

    Syamal, A.; Maurya, M.R.

    1986-01-01

    Synthesis of a new Schiff base derived from salicylaldehyde and 5-methylpyrazole-3-carbohydrazide, and its coordination compounds with nickel(II), cobalt(II), copper(II), manganese(II), zinc(II), zirconium(IV), dioxouranium(VI) and dioxomolybdenum(VI) are described. The ligand and the complexes have been characterized on the basis of analytical, conductance, molecular weight, i.r., electronic and n.m.r. spectra and magnetic susceptibility measurements. The stoichiometries of the complexes are represented as NiL . 3H 2 O, CoL . 2H 2 O, CuL, MnL . 2H 2 O, ZnL . H 2 O, Zr(OH) 2 (LH) 2 , Zr(OH) 2 L . 2MeOH, UO 2 L . MeOH and MoO 2 L . MeOH (where LH 2 =Schiff base). The copper(II) complex shows a subnormal magnetic moment due to antiferromagnetic exchange interaction while the nickel(II), cobalt(II) and manganese(II) complexes show normal magnetic moments at room temperature. The i.r. and n.m.r. spectral studies show that the Schiff base behaves as a dibasic and tridentate ligand coordinating through the deprotonated phenolic oxygen, enolic oxygen and azomethine nitrogen. (orig.)

  1. Chemically modified activated carbon with 1-acylthiosemicarbazide for selective solid-phase extraction and preconcentration of trace Cu(II), Hg(II) and Pb(II) from water samples.

    Science.gov (United States)

    Gao, Ru; Hu, Zheng; Chang, Xijun; He, Qun; Zhang, Lijun; Tu, Zhifeng; Shi, Jianping

    2009-12-15

    A new sorbent 1-acylthiosemicarbazide-modified activated carbon (AC-ATSC) was prepared as a solid-phase extractant and applied for removing of trace Cu(II), Hg(II) and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 3, the maximum static adsorption capacity of Cu(II), Hg(II) and Pb(II) onto the AC-ATSC were 78.20, 67.80 and 48.56 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 3.0 mL of 2% CS(NH2)2 and 2.0 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3sigma) of this method for Cu(II), Hg(II) and Pb(II) were 0.20, 0.12 and 0.45 ng mL(-1), respectively. The relative standard deviation under optimum conditions is less than 4.0% (n=8). The prepared sorbent was applied for the preconcentration of trace Cu(II), Hg(II) and Pb(II) in certified and water samples with satisfactory results.

  2. Cu(II) and Co(II) complexes of benzimidazole derivative: Structures, catecholase like activities and interaction studies with hydrogen peroxide

    Science.gov (United States)

    Kumari, Babli; Adhikari, Sangita; Matalobos, Jesús Sanmartín; Das, Debasis

    2018-01-01

    Present study describes the synthesis and single crystal X-ray structures of two metal complexes of benzimidazole derivative (PBI), viz. the Cu(II) complex, [Cu(PBI)2(NCS)]ClO4 (1) and a Co(II) complex, [Co(PBI)2(NCS)1.75Cl0.25] (2). The Cu(II) complex (1) shows catecholase like activity having Kcat = 1.84 × 104 h-1. Moreover, interactions of the complexes with hydrogen peroxide have been investigated using fluorescence spectroscopy. The interaction constant of 1 and 2 for H2O2 are 6.67 × 102 M-1 and 1.049 × 103 M-1 while their detection limits for H2O2 are 3.37 × 10-7 M and 2.46 × 10-7 M respectively.

  3. Removal of Ni(II from aqueous solution using leaf, bark and seed of Moringa stenopetala adsorbents

    Directory of Open Access Journals (Sweden)

    A. A. Mengistie

    2013-04-01

    Full Text Available The present study investigates the possibility of using leaf, bark and seed of Moringa stenopetala as alternative adsorbents for removal of Ni(II from aqueous solutions. The optimum adsorption conditions for removal of Ni(II were found to be 30, 20 and 50 mg/L initial concentration, 1.5, 2 and 2.5 g adsorbent dose, 250, 250 and 300 rpm agitation speed, 90, 120 and 90 min contact time, 40, 30 and 23 oC temperature and pH of 5, 6 and 6 using leaf, bark and seed as adsorbent, respectively. At optimum experimental conditions the percent adsorption of synthetic wastewater sample was found to be 93.90, 96.25 and 97.50 for leaf, bark and seed, respectively. The tested experimental data best fits to pseudo-second order (R2 > 0.98 than pseudo-first order, Elovich and intraparticle diffusion kinetic models indicating rate limiting step to be chemisorption. It also fits to Langmuir (R2 > 0.895 using adsorbate variation and also R2 > 0.998 using both time and temperature variation data than Freundlich, Temkin and D-R isotherm models. D-R isotherm and thermodynamic study reveals formation of physical adsorption. Hence the adsorption mechanism could be regarded as physico-chemical adsorption process. The adsorption results of industrial wastewater also reveal that for removal of nickel 83% and 85% was obtained using bark and seed adsorbents, respectively. The new method of adsorption developed in this study is cheap, fast and environmental friendly.DOI: http://dx.doi.org/10.4314/bcse.v27i1.4

  4. Synthesis, Characterization and Antimicrobial Studies of a New Mannich Base N-[Morpholino(phenylmethyl]acetamide and Its Cobalt(II, Nickel(II and Copper(II Metal Complexes

    Directory of Open Access Journals (Sweden)

    L. Muruganandam

    2012-01-01

    Full Text Available A new Mannich base N-[morpholino(phenylmethyl]acetamide (MBA, was synthesized and characterized by spectral studies. Chelates of MBA with cobalt(II, nickel(II and copper(II ions were prepared and characterized by elemental analyses, IR and UV spectral studies. MBA was found to act as a bidentate ligand, bonding through the carbonyl oxygen of acetamide group and CNC nitrogen of morpholine moiety in all the complexes. Based on the magnetic moment values and UV-Visible spectral data, tetracoordinate geometry for nitrato complexes and hexacoordinate geometry for sulphato complexes were assigned. The antimicrobial studies show that the Co(II nitrato complex is more active than the other complexes.

  5. Synthesis, Physical Characterization and Biological Activity of Some Schiff Base Complexes

    Directory of Open Access Journals (Sweden)

    R. Rajavel

    2008-01-01

    Full Text Available Structural modification of organic molecule has considerable biological relevance. Further, coordination of a biomolecules to the metal ions significantly alters the effectiveness of the biomolecules. In view of the antimicrobial activity ligand [bis-(2-aminobenzaldehyde] malonoyl dihydrazone], metal complexes with Cu(II, Ni(II, Zn(II and oxovanadium(IV have been synthesized and found to be potential antimicrobial agents. An attempt is also made to correlate the biological activities with geometry of the complexes. The complexes have been characterized by elemental analysis, molar conductance, spectra and cyclicvoltammetric measurements. The structural assessment of the complexes has been carried out based on electronic, infrared and molar conductivity values.

  6. Synthesis of Two Potentially Heptadentate (N4O3 Schiff-base Ligands Derived from Condensation of Tris(3-aminopropyl-amine and Salicylaldehyde or 4-Hydroxysalicylaldehyde. Nickel(II and Copper(II Complexes of the Former Ligand

    Directory of Open Access Journals (Sweden)

    R. V. Parish

    2002-02-01

    Full Text Available Two potentially heptadentate (N4O3 tripodal Schiff-base ligands: tris(3-(salicylideneiminopropylamine (H3L1 and tris(3-(4’-hydroxysalicylideneimino-propylamine (H3L2 have been prepared and characterized by various spectroscopic methods (IR, FAB-MS, NMR. They are derived from the condensation reactions of tris(3-aminopropylamine (tpt, with 3 equivalents of either salicylaldehyde or the ringsubstituted salicylaldehyde, 4-hydroxysalicylaldehyde. The nickel(II and copper(II complexes of H3L1 were obtained from the its reactions Ni(II and Cu(II salts in absolute methanol. These complexes were studied by IR and FAB-Mass spectrometry.

  7. Spectral, magnetic, and thermal properties of some thiazolylazo complexes

    International Nuclear Information System (INIS)

    Masoud, M. S.; Mohamed, G. B.; Abdulrazek, Y. H.; Ali, A. E.; Khairy, F. N.

    2002-01-01

    The thiazolylazo compounds and their Co(II), Ni(II) and Cu(II) complexes of barbituric acid, uracil, thiouracil, citrazinic acid, chromotropic acid, gallic acid, pyrogallol and salicylic acid were prepared and characterized by 1 H NMR, IR and the effect of pH on the electronic absorption spectra. The mode of ionization, the electronic transitions and the dissociation constants were discussed. The stoichiometries of the complexed were of 1:1, 2:1 and 3:2 (M:L). The copper complexes are of isotropic ESR spectra (except that of gallic acid which showed a complicated one) and are of magnetically diluted behavior with orbital contribution. Detailed DTA data were obtained and discussed

  8. Preparation and characterisation of biodegradable pollen-chitosan microcapsules and its application in heavy metal removal.

    Science.gov (United States)

    Sargın, İdris; Kaya, Murat; Arslan, Gulsin; Baran, Talat; Ceter, Talip

    2015-02-01

    Biosorbents have been widely used in heavy metal removal. New resources should be exploited to develop more efficient biosorbents. This study reports the preparation of three novel chitosan microcapsules from pollens of three common, wind-pollinated plants (Acer negundo, Cupressus sempervirens and Populus nigra). The microcapsules were characterized (Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy and elemental analysis) and used in removal of heavy metal ions: Cd(II), Cr(III), Cu(II), Ni(II) and Zn(II). Their sorption capacities were compared to those of cross-linked chitosan beads without pollen grains. C. sempervirens-chitosan microcapsules exhibited better performance (Cd(II): 65.98; Cu(II): 67.10 and Zn(II): 49.55 mg g(-1)) than the other microcapsules and the cross-linked beads. A. negundo-chitosan microcapsules were more efficient in Cr(III) (70.40 mg g(-1)) removal. P. nigra-chitosan microcapsules were found to be less efficient. Chitosan-pollen microcapsules (except P. nigra-chitosan microcapsules) can be used in heavy metal removal. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Synthesis, Characterization and Biological Evaluation of Transition Metal Complexes Derived from N, S Bidentate Ligands

    Directory of Open Access Journals (Sweden)

    Enis Nadia Md Yusof

    2015-05-01

    Full Text Available Two bidentate NS ligands were synthesized by the condensation reaction of S-2-methylbenzyldithiocarbazate (S2MBDTC with 2-methoxybenzaldehyde (2MB and 3-methoxybenzaldehyde (3MB. The ligands were reacted separately with acetates of Cu(II, Ni(II and Zn(II yielding 1:2 (metal:ligand complexes. The metal complexes formed were expected to have a general formula of [M(NS2] where M = Cu2+, Ni2+, and Zn2+. These compounds were characterized by elemental analysis, molar conductivity, magnetic susceptibility and various spectroscopic techniques. The magnetic susceptibility measurements and spectral results supported the predicted coordination geometry in which the Schiff bases behaved as bidentate NS donor ligands coordinating via the azomethine nitrogen and thiolate sulfur. The molecular structures of the isomeric S2M2MBH (1 and S2M3MBH (2 were established by X-ray crystallography to have very similar l-shaped structures. The Schiff bases and their metal complexes were evaluated for their biological activities against estrogen receptor-positive (MCF-7 and estrogen receptor-negative (MDA-MB-231 breast cancer cell lines. Only the Cu(II complexes showed marked cytotoxicity against the cancer cell lines. Both Schiff bases and other metal complexes were found to be inactive. In concordance with the cytotoxicity studies, the DNA binding studies indicated that Cu(II complexes have a strong DNA binding affinity.

  10. Synthesis, characterization, X-ray crystal structure and conductometry studying of a number of new Schiff base complexes; a new example of binuclear square pyramidal geometry of Cu(II) complex bridged with an oxo group

    Science.gov (United States)

    Golbedaghi, Reza; Alavipour, Ehsan

    2015-11-01

    Three new binuclear Cu(II), Mn(II), Co(II) complexes [Cu2(L) (ClO4)](ClO4)2 (1), [Mn2(L) (ClO4)](ClO4)2 (2), and [Co2(L) (ClO4)](ClO4)2 (3), {L = 1,3-bis(2-((Z)-(2-aminopropylimino)methyl)phenoxy)propan-2-ol} have been synthesized. Single crystal X-ray structure analysis of complex 1 showed that the complex is binuclear and all nitrogen and oxygen atoms of ligand (N4O3) are coordinated to two Cu(II) center ions. In addition, the crystal structure studying shows, a perchlorate ion has been bridged to the Cu(II) metal centers. However, two distorted square pyramidal Cu(II) ions are bridged asymmetrically by a perchlorate ion and oxygen of hydroxyl group of Schiff base ligand. In addition, the conductometry behaviors of all complexes were studied in acetonitrile solution.

  11. Synthesis and Characterization of a New Coordinative Compound of Cu(II with 1-(3 Bromo, 2 Hydroxy, 4 Methylphenyl- 2-(4 Bromo-Phenyl-Sulphanyl- Etanone

    Directory of Open Access Journals (Sweden)

    Antighin Simona

    2015-07-01

    Full Text Available Continuing the research in the field of complex compounds, the authors present in this paper the synthesis and characterization of a new compound of Cu(II with the ligand 1-(3 bromo, 2 hydroxy, 4 methyl-phenyl-2-(4 bromophenyl- sulphanyl-etanone. Different methods were used, such as chemical elemental analysis, thermal-gravimetry, infrared absorption spectroscopy and electronic spin resonance (ESR. From chemical analysis resulted that the combination ratio ligand-central atom is 2:1. The new compound can also be used for gravimetric determination of Cu(II.

  12. Speciation of Co(II), Ni(II) and Cu(II) Complexes with L-Glutamic ...

    African Journals Online (AJOL)

    NICO

    2011-08-10

    Aug 10, 2011 ... Cobalt in the form of vitamin B12 or one of the cobinamides is essential for the ... proteins10–12 and catalyzes the hydrolysis of urea to yield ammonia and carbamate. ... oxygenation, oxidation, reduction and disproportionation. The ..... cosolvent content depends upon electrostatic and non-electro-.

  13. A metal-organic framework nanocomposite made from functionalized magnetite nanoparticles and HKUST-1 (MOF-199) for preconcentration of Cd(II), Pb(II), and Ni(II)

    International Nuclear Information System (INIS)

    Ghorbani-Kalhor, Ebrahim

    2016-01-01

    The author describes the preparation of a magnetic metal organic framework of type MOF-199 containing magnetite (Fe 3 O 4 ) nanoparticles carrying covalently immobilized 4-(thiazolylazo) resorcinol (Fe 3 O 4 -TAR). This material is shown to represent a viable sorbent for separation and preconcentration of Cd(II), Pb(II), and Ni(II) ions. Box-Behnken design was applied to optimize the parameters affecting preconcentration. Following elution with 0.6 mol L −1 EDTA, the ions were quantified by FAAS. The capacity of the sorbent ranged between 185 and 210 mg g −1 . The limits of detection are 0.15, 0.40, and 0.8 ng mL −1 for Cd(II), Ni(II), and Pb(II) ions, respectively. The relative standard deviations are <8.5 %. The method was successfully applied to the rapid extraction of trace amounts of these ions from sea food and agri food. (author)

  14. Ising-type magnetic anisotropy in a cobalt(II) nitronyl nitroxide compound: a key to understanding the formation of molecular magnetic nanowires.

    Science.gov (United States)

    Caneschi, A; Gatteschi, Dante; Lalioti, N; Sessoli, R; Sorace, L; Tangoulis, V; Vindigni, A

    2002-01-04

    The compound [Co(hfac)2-(NITPhOMe)2] (2) (hfac = hexafluoroacetylacetonate, NITPhOMe = 4'-methoxyphenyl-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) crystallizes in the triclinic P1 space group, a= 10.870(5), b = 11.520(5), c = 19.749(5) A, alpha = 78.05(5), beta = 84.20(5), gamma = 64.51(5) degrees, Z = 2. It can be considered a model system for studying the nature of the magnetic anisotropy of [Co(hfac)2(NITPhOMe)] (1), which was recently reported to behave as a molecular magnetic wire. The magnetic anisotropy of 2 was investigated by EPR spectroscopy and SQUID magnetometry both in the polycrystalline powder and in a single crystal. The experimental magnetic anisotropy was related to the anisotropy of the central ion and to the exchange interaction between the cobalt(II) ion and the radicals.

  15. Competitive adsorption of Pb(II), Cu(II), and Zn(II) ions onto hydroxyapatite-biochar nanocomposite in aqueous solutions

    Science.gov (United States)

    Wang, Yu-Ying; Liu, Yu-Xue; Lu, Hao-Hao; Yang, Rui-Qin; Yang, Sheng-Mao

    2018-05-01

    A hydroxyapatite-biochar nanocomposite (HAP-BC) was successfully fabricated and its physicochemical properties characterized. The analyses showed that HAP nanoparticles were successfully loaded on the biochar surface. The adsorption of Pb(II), Cu(II), and Zn(II) by HAP-BC was systematically studied in single and ternary metal systems. The results demonstrated that pH affects the adsorption of heavy metals onto HAP-BC. Regarding the adsorption kinetics, the pseudo-second-order model showed the best fit for all three heavy metal ions on HAP-BC. In both single and ternary metal ion systems, the adsorption isotherm of Pb(II) by HAP-BC followed Langmuir model, while those of Cu(II) and Zn(II) fitted well with Freundlich model. The maximum adsorption capacity for each tested metal by HAP-BC was higher than that of pristine rice straw biochar (especially for Pb(II)) or those of other reported adsorbents. Therefore, HAP-BC could explore as a new material for future application in heavy metal removal.

  16. Preliminary screening of Ni(II metal tolerance and dye-decolorizing by Nocardiopsis sp. SD8

    Directory of Open Access Journals (Sweden)

    Ramasamy Thangaraj

    2016-04-01

    Full Text Available Objective: To reveal the screening of metal tolerance and dye-decolorizing of Nocardiopsis sp. Methods: NiSO4 and Congo red dye were used for evaluating the metal tolerance and dyedecolorizing of the randomly selected actinobacterial isolates. Results: Nocardiopsis sp. SD8 showed a better efficiency in Ni(II tolerance, though a longer lag phase was observed for this microorganism grown for 7 days in integrated mismatch negativity. Interestingly, we also found that Nocardiopsis sp. SD8 had dye-decolorizing, hemolytic, lipase and protease activity. Conclusions: The present results revealed the bioremediation of metal resistant and diverse properties of Nocardiopsis sp. SD8 and further investigations are needed to extract and identify the potent molecule.

  17. Cassava root husks powder as green adsorbent for the removal of Cu(II) from natural river water

    Energy Technology Data Exchange (ETDEWEB)

    Jorgetto, A.O.; Silva, R.I.V.; Saeki, M.J.; Barbosa, R.C. [IB-UNESP, Dept. Química e Bioquímica, C.P. 510, 18618-000 Botucatu, SP (Brazil); Martines, M.A.U. [UFMS – Dept. Química, 79074-460 Campo Grande, MS (Brazil); Jorge, S.M.A.; Silva, A.C.P. [IB-UNESP, Dept. Química e Bioquímica, C.P. 510, 18618-000 Botucatu, SP (Brazil); Schneider, J.F. [USP – Instituto de Física de São Carlos, 13566-590 São Carlos, SP (Brazil); Castro, G.R., E-mail: castrogr@ibb.unesp.br [IB-UNESP, Dept. Química e Bioquímica, C.P. 510, 18618-000 Botucatu, SP (Brazil)

    2014-01-01

    Through a series of simple processes, cassava root husks were turned into a fine powder of controlled particle size (63–75 μm). FTIR spectrum demonstrated the existence of alcohol, amine and carboxylic groups; and elemental analysis confirmed the presence of elements of interest such as sulphur, nitrogen and oxygen. Cross-polarized {"1H}-{sup 13}C NMR technique indicated the existence of methionine and thiamine through the signals observed at 55 ppm and 54 ppm, respectively, and the point of zero charge (pH{sub pzc}) was achieved at pH 5.2. The material was applied in solid-phase extraction of Cu(II) via batch experiments. Optimum adsorption pH was found to be in range of 3–6 and in the kinetic experiment the equilibrium was attained in 1 min. The highest adsorption capacity was 0.14 mmol g{sup −1}. The adsorption data were fit to the modified Langmuir equation, and the maximum amount of metal species extracted from the solution, N{sub s}, was determined to be ∼0.14 mmol g{sup −1}, which is an indicative that the main adsorption mechanism is through chemisorption. Under optimized conditions, the material was utilized in preconcentration experiments, which culminated in an enrichment factor of 41.3-fold. With the aid of the enrichment factor, experiments were carried out to determine the Cu(II) content in tap water and natural water. Preconcentration method was also applied to a certified reference material (1643e) and the concentration found was 23.03 ± 0.79 μg L{sup −1}, whereas the specified Cu(II) concentration was 22.7 ± 0.31 μg L{sup −1}.

  18. Characterization of a meso-chiral isomer of a hexanuclear Cu(II) cage from racemization of the L-alanine Schiff base.

    Science.gov (United States)

    Rajesh, Chinnaiyan Mahalingam; Ray, Manabendra

    2014-09-14

    We are reporting structural characterization of two new hexanuclear cages (H3O)2[Cu3(μ3-OH)(μ3-NH3)(0.5)(L)3]2·8H2O (1) and (H3O)2[Cu3(μ3-OH)(μ3-H2O)(0.5)(L)3]2·8H2O (1a) where L(2-) is the dianionic form of the Schiff base of L-alanine and salicylaldehyde. The complex 1 has two C3 symmetric hydroxo bridged trinuclear halves joined by an ammonia or water molecule at the center through H-bonding. Each of the trinuclear halves is enantiopure but of opposite chirality to the other half, making the hexanuclear unit a meso isomer. Temperature dependent magnetic measurements showed the presence of ferromagnetic interactions among trinuclear Cu(II) units, a rare occurrence among trinuclear Cu(II) complexes. Characterization of the LiHL showed it to be enantiopure. Addition of a base, monitored using optical rotation, showed that racemization occurs as a result of base addition. The racemization depends on the base as well as the temperature. Base or Cu(II) induced racemization of amino acid derivatives has been indicated in a number of cases in the past but structural characterization of the products or formation of this type of chiral hexanuclear architecture was never reported. Structures of the complex and the ligand have a number of interesting H-bonding situations.

  19. A novel adsorbent TEMPO-mediated oxidized cellulose nanofibrils modified with PEI: Preparation, characterization, and application for Cu(II) removal

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Nan; Zang, Guo-Long; Shi, Chen; Yu, Han-Qing; Sheng, Guo-Ping, E-mail: gpsheng@ustc.edu.cn

    2016-10-05

    Highlights: • A cellulose nanofibril based adsorbent with abundant carboxyl/amino was prepared. • After modification by PEI, the Cu adsorption capacity of nanofibril increased. • TOCN-PEI has good Cu(II) removal ability and its maximum capacity was 52.32 mg g{sup −1}. • Results show Cu adsorption on TOCN-PEI is an exothermic and enthalpy-driven process. • Sorption-desorption tests reveal that TOCN-PEI has good stability for Cu removal. - Abstract: This study describes the preparation of a novel adsorbent based on cellulose nanofibrils by first TEMPO mediated oxidation and then PEI grafting (TOCN-PEI) for heavy metal removal. FTIR results demonstrated the successful introduction of the adsorption functional groups (carboxyl and amino groups), and the elemental analysis and acid base titration were used to quantify the contents of these introduced groups. The kinetics curve suited the pseudo-second-order model better and the equilibrium data well fitted the Langmuir model, with the maximum Cu(II) uptake of 52.32 mg g{sup −1}. Kinetic study showed that the PEI grafting increased the initial adsorption rate of the TOCN-PEI compared with the adsorbents without PEI. Thermodynamic study was carried out through isothermal titration calorimetry (ITC) measurement and the binding reaction was found to be exothermic and driven by enthalpy change. The adsorption process by TOCN-PEI was pH dependent, and decreasing pH would lead to desorption of Cu(II) ions, thus make the reuse of the absorbent more convenient through adsorption-desorption cycles.

  20. A novel sensitive Cu(II) and Cd(II) nanosensor platform: Graphene oxide terminated p-aminophenyl modified glassy carbon surface

    International Nuclear Information System (INIS)

    Gupta, Vinod Kumar; Yola, Mehmet Lütfi; Atar, Necip; Ustundag, Zafer; Solak, Ali Osman

    2013-01-01

    Graphical abstract: - Highlights: • We electrochemically prepared sensor based on graphene oxide. • The prepared electrode was characterized by using various techniques. • The proposed nanosensor showed good stability, selectivity and high sensitivity. • The proposed nanosensor electrode was used for the analysis of Cd(II) and Cu(II). - Abstract: Graphene oxide (GO) based glassy carbon (GC) electrode has been prepared. Firstly, p-nitrophenyl (NP) modified GC (NP/GC) electrode was prepared via the electrochemical reduction of its tetraflouroborate diazonium salt. After the formation of NP/GC electrode, the negative potential was applied to NP/GC electrode to reduce the nitro groups to amine. p-Aminophenyl (AP) modified GC (AP/GC) electrode was immersed into a graphene oxide solution containing 1-ethyl-3(3-(dimethlyamino)propyl)-carbodiimide. Hence, we constructed GO terminated AP modified GC (GO/AP/GC) electrode. NP/GC, AP/GC and GO/AP/GC electrodes were characterized sequentially using cyclic voltammetry (CV) in the presence of 1.0 mM of potassium ferricyanide in 0.1 M KCl. In addition, GO and GO/AP/GC surfaces were characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The GO/AP/GC electrode was used for the analysis of Cd(II) and Cu(II) ions by adsorptive stripping voltammetry. The linearity range and the detection limit of Cd(II) and Cu(II) ions were 1.0 × 10 −11 –5.0 × 10 −10 M and 3.3 × 10 −12 M (S/N = 3), respectively

  1. Ni(II) complexes of arginine Schiff-bases and its interaction with DNA

    Energy Technology Data Exchange (ETDEWEB)

    Sallam, S.A., E-mail: shehabsallam@yahoo.com [Chemistry Department, Faculty of Science, Suez Canal University, Isamilia (Egypt); Abbas, A.M. [Chemistry Department, Faculty of Science, Suez Canal University, Isamilia (Egypt)

    2013-04-15

    Ni(II) complexes with Schiff-bases obtained by condensation of arginine with salicylaldehyde; 2,3-; 2,4-; 2,5-dihydroxybenzaldehyde and o-hydroxynaphthaldehyde have been synthesized using the template method in ethanol or ammonia media. They were characterized by elemental analyses, conductivity measurements, magnetic moment, UV, IR and {sup 1}H NMR spectra as well as thermal analysis (TG, DTG and DTA). The Schiff-bases are dibasic tridentate donors and the complexes have diamagnetic square planar and octahedral structures. The complexes decompose in three steps where kinetic and thermodynamic parameters of the decomposition steps were computed. The interactions of the formed complexes with FM-DNA were monitored by UV and fluorescence spectroscopy. -- Highlights: ► Arginine Schiff-bases and their nickel(II) complexes have been synthesized. ► Magnetic and spectral data show diamagnetic square planar and octahedral complexes. ► The complexes thermally decompose in three stages. Interaction with FM-DNA shows hyperchromism with blue shift.

  2. Ni(II) complexes of arginine Schiff-bases and its interaction with DNA

    International Nuclear Information System (INIS)

    Sallam, S.A.; Abbas, A.M.

    2013-01-01

    Ni(II) complexes with Schiff-bases obtained by condensation of arginine with salicylaldehyde; 2,3-; 2,4-; 2,5-dihydroxybenzaldehyde and o-hydroxynaphthaldehyde have been synthesized using the template method in ethanol or ammonia media. They were characterized by elemental analyses, conductivity measurements, magnetic moment, UV, IR and 1 H NMR spectra as well as thermal analysis (TG, DTG and DTA). The Schiff-bases are dibasic tridentate donors and the complexes have diamagnetic square planar and octahedral structures. The complexes decompose in three steps where kinetic and thermodynamic parameters of the decomposition steps were computed. The interactions of the formed complexes with FM-DNA were monitored by UV and fluorescence spectroscopy. -- Highlights: ► Arginine Schiff-bases and their nickel(II) complexes have been synthesized. ► Magnetic and spectral data show diamagnetic square planar and octahedral complexes. ► The complexes thermally decompose in three stages. Interaction with FM-DNA shows hyperchromism with blue shift

  3. Column dynamic studies and breakthrough curve analysis for Cd(II) and Cu(II) ions adsorption onto palm oil boiler mill fly ash (POFA).

    Science.gov (United States)

    Aziz, Abdul Shukor Abdul; Manaf, Latifah Abd; Man, Hasfalina Che; Kumar, Nadavala Siva

    2014-01-01

    This paper investigates the adsorption characteristics of palm oil boiler mill fly ash (POFA) derived from an agricultural waste material in removing Cd(II) and Cu(II) from aqueous solution via column studies. The performance of the study is described through the breakthrough curves concept under relevant operating conditions such as column bed depths (1, 1.5, and 2 cm) and influent metal concentrations (5, 10, and 20 mg/L). The Cd(II) and Cu(II) uptake mechanism is particularly bed depth- and concentration-dependant, favoring higher bed depth and lower influent metal concentration. The highest bed capacity of 34.91 mg Cd(II)/g and 21.93 mg Cu(II)/g of POFA was achieved at 20 mg/L of influent metal concentrations, column bed depth of 2 cm, and flow rate of 5 mL/min. The whole breakthrough curve simulation for both metal ions were best described using the Thomas and Yoon–Nelson models, but it is apparent that the initial region of the breakthrough for Cd(II) was better described using the BDST model. The results illustrate that POFA could be utilized effectively for the removal of Cd(II) and Cu(II) ions from aqueous solution in a fixed-bed column system.

  4. Experimental study of mixed additive of Ni(II) and piperazine on ammonia escape in CO2 capture using ammonia solution

    International Nuclear Information System (INIS)

    Ma, Shuangchen; Chen, Gongda; Zhu, Sijie; Wen, Jiaqi; Gao, Ran; Ma, Lan; Chai, Jin

    2016-01-01

    Highlights: • Compound additive was used to obtain high CO 2 absorption efficiency and low NH 3 escape. • Both organic material and metal ion were applied as compound additive. • Influences of additives on CO 2 absorption and NH 3 escape were investigated. • Possible mechanism and products were analyzed by XRD and UV–visible spectrophotometer. - Abstract: In order to obtain high CO 2 absorption efficiency and low ammonia escape rate, mixed additives of piperazine and Ni(II) were used as absorbent in bubbling reactor. The effects of mixed additive on CO 2 absorption efficiency and ammonia escape rate were investigated; the performances of mixed additive in removal process were compared with that of pure ammonia solution. The proposed mechanism was analyzed by XRD and UV–visible spectrophotometer. The mixed additive has well effect on CO 2 absorption efficiency and ammonia escape reduction. The CO 2 absorption efficiency was 72% when 2 wt% ammonia solution mixed with 0.025 mol/L piperazine and 0.05 mol/L Ni(II), higher than that achieved by 3 wt% ammonia solution without additive, and the amount of ammonia loss was nearly 1/3 compared with 3 wt% pure ammonia solution. This paper provided one feasible method which is beneficial to the balance between CO 2 absorption and ammonia escape in CO 2 capture process.

  5. Preparation, spectral, X-ray powder diffraction and computational studies and genotoxic properties of new azo-azomethine metal chelates

    Science.gov (United States)

    Bitmez, Şirin; Sayin, Koray; Avar, Bariş; Köse, Muhammet; Kayraldız, Ahmet; Kurtoğlu, Mükerrem

    2014-11-01

    A new tridentate azo-azomethine ligand, N‧-[{2-hydroxy-5-[(4-nitrophenyl)diazenyl]phenyl}methylidene]benzohydrazidemonohydrate, (sbH·H2O) (1), is prepared by condensation of benzohydrazide and 2-hydroxy-5-[(4-nitrophenyl)diazenyl]benzaldehyde (a) with treatment of a solution of diazonium salt of p-nitroaniline and 2-hydroxybenzaldehyde in EtOH. The five coordination compounds, [Co(sb)2]·4H2O (2), [Ni(sb)2]·H2O (3), [Cu(sb)2]·4H2O (4), [Zn(sb)2]·H2O (5) and [Cd(sb)2]·H2O (6) are prepared by reacting the Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) ions with the ligand. The structures of the compounds are elucidated from the elemental analyses data and spectroscopic studies. It is found the ligand acts as a tridentate bending through phenolic and carbonyl oxygens and nitrogen atom of the Cdbnd Nsbnd group similar to the most of salicylaldimines. Comparison of the infrared spectra of the ligand and its metal complexes confirm that azo-Schiff base behaves as a monobasic tridentate ligand towards the central metal ion with an ONO donor sequence. Upon complexation with the ligand, the Cd(II), and Zn(II) ions form monoclinic structures, while Co(II), Cu(II) and Ni(II) ions form orthorhombic structures. Quantum chemical calculations are performed on tautomers and its metal chelates by using DFT/B3LYP method. Most stable tautomer is determined as tautomer (1a). The geometrical parameters of its metal chelates are obtained as theoretically. The NLO properties of tautomer (1a) and its metal complexes are investigated. Finally, the ligand and its metal complexes are assessed for their genotoxicity.

  6. Adsorption performances and mechanisms of the newly synthesized N,N'-di (carboxymethyl) dithiocarbamate chelating resin toward divalent heavy metal ions from aqueous media

    International Nuclear Information System (INIS)

    Jing Xiaosheng; Liu Fuqiang; Yang Xin; Ling Panpan; Li Lanjuan; Long Chao; Li Aimin

    2009-01-01

    N,N'-di (carboxymethyl) dithiocarbamate chelating resin (PSDC) was synthesized by anchoring the chelating agent of N,N'-di (carboxymethyl) dithiocarbamate to the chloromethylated PS-DVB (Cl-PS-DVB) matrix, as a new adsorbent for removing divalent heavy metal ions from waste-stream. The physicochemical structures of Cl-PS-DVB and PSDC were elaborately characterized using Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), and were further morphologically characterized using BET and BJH methods. The adsorption performances of PSDC towards heavy metals such as Cu(II), Pb(II) and Ni(II) were systematically investigated, based upon which the adsorption mechanisms were deeply exploited. For the above target, the classic batch adsorption experiments were conducted to explore the kinetics and isotherms of the removal processes with pH-value, initial concentration, temperature, and contact time as the controlling parameters. The kinetic and isotherm data could be well elucidated with Lagergren-second-order equation and Langmuir model respectively. The strong affinity of PSDC toward these target soft acids could be well demonstrated with the electrostatic attraction and chelating interaction caused by IDA moiety and sulphur which were namely soft bases on the concept of hard and soft acids and bases (HASB). Thermodynamic parameters, involving ΔH o , ΔS o and ΔG o were also calculated from graphical interpretation of the experimental data. The standard heats of adsorption (ΔH o ) were found to be endothermic and the entropy change values (ΔS o ) were calculated to be positive for the adsorption of Cu(II), Pb(II) and Ni(II) ions onto the tested adsorbents. Negative values of ΔG o indicated that adsorption processes for all tested metal ions onto PSDC were spontaneous.

  7. Competition from Cu(II), Zn(II) and Cd(II) in Pb(II) binding to Suwannee River Fulvic Acid

    NARCIS (Netherlands)

    Chakraborty, P.; Chakrabarti, C.L.

    2008-01-01

    This is a study of trace metal competition in the complexation of Pb(II) by well-characterized humic substances, namely Suwannee River Fulvic Acid (SRFA) in model solutions. It was found that Cu(II) seems to compete with Pb(II) for strong binding sites of SRFA when present at the same concentration

  8. Solid Phase Extraction of Trace Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) Ions in Beverages on Functionalized Polymer Microspheres Prior to Flame Atomic Absorption Spectrometric Determinations.

    Science.gov (United States)

    Berber, Hale; Alpdogan, Güzin

    2017-01-01

    In this study, poly(glycidyl methacrylate-methyl methacrylate-divinylbenzene) was synthesized in the form of microspheres, and then functionalized by 2-aminobenzothiazole ligand. The sorption properties of these functionalized microspheres were investigated for separation, preconcentration and determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions using flame atomic absorption spectrometry. The optimum pH values for quantitative sorption were 2 - 4, 5 - 8, 6 - 8, 4 - 6, 2 - 6 and 2 - 3 for Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II), respectively, and also the highest sorption capacity of the functionalized microspheres was found to be for Cu(II) with the value of 1.87 mmol g -1 . The detection limits (3σ; N = 6) obtained for the studied metals in the optimal conditions were observed in the range of 0.26 - 2.20 μg L -1 . The proposed method was successfully applied to different beverage samples for the determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions, with the relative standard deviation of <3.7%.

  9. Preparation and Spectral Properties of Mixed-Ligand Complexes of VO(IV, Ni(II, Zn(II, Pd(II, Cd(II and Pb(II with Dimethylglyoxime and N-acetylglycine

    Directory of Open Access Journals (Sweden)

    Shayma A. Shaker

    2010-01-01

    Full Text Available A number of mixed-ligand complexes of the general formula [M(D(G] where D=dimethylglyoximato monoanion, G=N-acetylglycinato and M=VO(IV, Ni(II, Zn(II, Pd(II, Cd(II and Pb(II were prepared. Each complex was characterized by elemental analysis, determination of metal, infrared spectra, electronic spectra, (1H and 13C NMR spectra, conductivity and magnetic moments. All these complexes were not soluble in some of the organic solvent but highly soluble in dimethylformamide. The conductivity data showed the non-electrolytic nature of the complexes. The electronic spectra exhibited absorption bands in the visible region caused by the d-d electronic transition such as VO(IV, Ni(II and Pd(II. The IR and (1H, 13C NMR spectra which have indicate that the dimethylglyoxime was coordinated with the metal ions through the N and O atoms of the oxime group and N-acetylglycine was coordinated with metal ions through the N atom and terminal carboxyl oxygen atom.

  10. Application of EDTA-functionalized bamboo activated carbon (BAC) for Pb(II) and Cu(II) removal from aqueous solutions

    Science.gov (United States)

    Lv, Dan; Liu, Yu; Zhou, Jiasheng; Yang, Kunlun; Lou, Zimo; Baig, Shams Ali; Xu, Xinhua

    2018-01-01

    In this study, a novel bamboo activated carbon (BAC) with ethylene diamine tetraacetic acid (EDTA) functionality was prepared by direct grafting in the presence of tetraethyl orthosilicate (TEOS) as a crosslinking agent. The BAC@SiO2-EDTA was characterized by SEM, TEM, TGA, FTIR, XPS and its adsorption property for removal of Pb(II) and Cu(II) under various experimental conditions was also investigated. The characterization results reflected that EDTA was successfully assembled on the surface of the BAC and average pore size increased from 4.10 to 4.83 nm as BAC grafted with EDTA. Adsorption data fitted very well in Langmuir isotherm model and pseudo-second-order kinetic model. As compared with the raw BAC, the maximum adsorption capacities of BAC@SiO2-EDTA for the Pb(II) and Cu(II) increased from 45.45 to 123.45 mg g-1 and from 6.85 to 42.19 mg g-1, since the existence of EDTA on modified BAC promoted the formation of chemical complex. The removal of heavy metal ions mainly depended on the complexation with EDTA and the electrostatic attractions with negatively charged surface of BAC@SiO2-EDTA. The adsorption of Pb(II)/Cu(II) on the BAC@SiO2-EDTA was pH dependent and pH 5-6 was considered an optimum. However, lower temperature favored the adsorption and the maximum adsorption was recorded at 20 °C. In addition, BAC@SiO2-EDTA had an excellent reusability with about 40% decline in the adsorption capacity for Pb(II) after fifth reuse. Insignificant influences of co-existing cations and natural organic matter (NOM) were found on the adsorption of Pb(II) and Cu(II). All the results demonstrate that BAC@SiO2-EDTA is a potential adsorbent for metal ions in wastewater.

  11. Cr(III,Mn(II,Fe(III,Co(II,Ni(II,Cu(II and Zn(II Complexes with Diisobutyldithiocarbamato Ligand

    Directory of Open Access Journals (Sweden)

    Mohammad Tarique

    2011-01-01

    Full Text Available The synthesis of sulphur and nitrogen containing dithiocarbamato ligand derived from diisobutylamine as well as its coordination compounds with 3d series transition metals is presented. These synthesized compounds were characterized on the basis of elemental analysis, conductometric measurements and IR spectral studies. The analytical data showed the stoichiometry 1:2 and 1:3 for the compounds of the types ML2 {M=Mn(II, Co(II, Ni(II, Cu(II and Zn(II} and M'L3{M'=Cr(III and Fe(III} respectively. The conductometric measurements proved the non-electrolytic behaviour of all the compounds. The bidentate nature of dithiocarbamato moiety was confirmed on the basis of IR spectral data.

  12. Removal of heavy metals from industrial wastewaters using amine-functionalized nanoporous carbon as a novel sorbent

    International Nuclear Information System (INIS)

    Sayar, O.; Khan, S.J.; Amini, M.M.; Moghadamzadeh, H.; Sadeghi, O.

    2013-01-01

    Nano-porous carbon (NPC) was synthesized by hydrothermal condensation of fructose and characterized by X-ray powder diffraction and also nitrogen adsorption analysis. It was then modified with amino groups and used as a sorbent for the removal of heavy metal ions. The formation of amino-modified NPC was confirmed by X-ray powder diffraction, infrared spectroscopy, thermogravimetric and elemental analysis. NPC was applied for removal of Pb(II), Cd(II), Ni(II) and Cu(II) ions. The effects of sample pH and the adsorption kinetics were studied, and the adsorption capacity was determined. The sorbent was applied to the removal of heavy metal ions in industrial waste water samples. (author)

  13. Spectral, magnetic, and thermal properties of some thiazolylazo complexes

    Energy Technology Data Exchange (ETDEWEB)

    Masoud, M. S.; Mohamed, G. B.; Abdulrazek, Y. H.; Ali, A. E. [Alexandria Univ., Alexandria (Egypt); Khairy, F. N. [Ahfad Univ. for Women, Omderman (Sudan)

    2002-04-01

    The thiazolylazo compounds and their Co(II), Ni(II) and Cu(II) complexes of barbituric acid, uracil, thiouracil, citrazinic acid, chromotropic acid, gallic acid, pyrogallol and salicylic acid were prepared and characterized by {sup 1}H NMR, IR and the effect of pH on the electronic absorption spectra. The mode of ionization, the electronic transitions and the dissociation constants were discussed. The stoichiometries of the complexed were of 1:1, 2:1 and 3:2 (M:L). The copper complexes are of isotropic ESR spectra (except that of gallic acid which showed a complicated one) and are of magnetically diluted behavior with orbital contribution. Detailed DTA data were obtained and discussed.

  14. Preparation Characterization and Antibacterial Studies of Chelates of Schiff Base Derived from4-Aminoantipyrine, Furfural and o-phenylenediamine

    Directory of Open Access Journals (Sweden)

    M. S. Suresh

    2011-01-01

    Full Text Available A new series of transition metal complexes of Mn(II, Co(II, Ni(II, Cu(II and Zn(II were synthesized from the Schiff base ligand derived from 4-aminoantipyrine, furfural and o-phenylenediamine. The structural features were derived from their elemental analyses, infrared, UV-visible spectroscopy, NMR spectroscopy, thermal gravimetric analyses, ESR spectral analyses and conductivity measurements. The data of the complexes suggested square planar geometry for the metals with primary valency two. Antimicrobial screening tests were performed against bacteria. The comparative study of the MIC values of the Schiff base and its metal complexes indicate that the metal complexes exhibit greater antibacterial activity than the free ligand.

  15. Metalloantibiotic Mn(II)-bacitracin complex mimicking manganese superoxide dismutase

    International Nuclear Information System (INIS)

    Piacham, Theeraphon; Isarankura-Na-Ayudhya, Chartchalerm; Nantasenamat, Chanin; Yainoy, Sakda; Ye Lei; Buelow, Leif; Prachayasittikul, Virapong

    2006-01-01

    Superoxide dismutase (SOD) activities of various metallobacitracin complexes were evaluated using the riboflavin-methionine-nitro blue tetrazolium assay. The radical scavenging activity of various metallobacitracin complexes was shown to be higher than those of the negative controls, e.g., free transition metal ions and metal-free bacitracin. The SOD activity of the complex was found to be in the order of Mn(II) > Cu(II) > Co(II) > Ni(II). Furthermore, the effect of bacitracin and their complexation to metals on various microorganisms was assessed by antibiotic susceptibility testing. Moreover, molecular modeling and quantum chemical calculation of the metallobacitracin complex was performed to evaluate the correlation of electrostatic charge of transition metal ions on the SOD activity

  16. Can Cu(II) ions be doped into the crystal structure of potassium hydrogen tartrate?

    OpenAIRE

    Srinivasan, Bikshandarkoil R.; Remesh, H.

    2015-01-01

    The differing binding preferences of the hydrogen tartrate ligand (HC4H4O6)- namely {\\mu}7-octadentate mode for potassium ion and bidentate mode for cupric ion rules out the doping (incorporation) of any Cu(II) ion into the crystal structure of potassium hydrogen tartrate. Hence, the claim of growth of copper doped potassium hydrogen tartrate viz. K0.96Cu0.04C4H5O6 by Mathivanan and Haris, Indian J Pure App Phys 51 (2013) 851-859 is untenable.

  17. New Mononuclear Cu(II Complexes and 1D Chains with 4-Amino-4H-1,2,4-triazole

    Directory of Open Access Journals (Sweden)

    Marinela M. Dîrtu

    2013-12-01

    Full Text Available The crystal structures of two mononuclear Cu(II NH2trz complexes [Cu(NH2trz4(H2O](AsF62 (I and [Cu(NH2trz4(H2O](PF62 (II as well as two coordination polymers [Cu(μ2-NH2trz2Cl]Cl∙H2O (III and [Cu(μ2-NH2trz2Cl] (SiF60.5∙1.5H2O (IV are presented. Cationic 1D chains with bridging bis-monodentate μ2-coordinated NH2trz and bridging μ2-coordinated chloride ligands are present in III and IV. In these coordination polymers, the Cu(II ions are strongly antiferromagnetically coupled with J = −128.4 cm−1 for III and J = −143 cm−1 for IV (H = −JΣSiSi+1, due to the nature of the bridges between spin centers. Inter-chain interactions present in the crystal structures were taken into consideration, as well as g factors, which were determined experimentally, for the quantitative modeling of their magnetic properties.

  18. 1D Cu(II) coordination polymer derived from 2-(2-(2,4-dioxopentan-3-ylidene)hydrazinyl)benzenesulfonate chelator and pyrazine spacer

    Science.gov (United States)

    Mahmudov, Kamran T.; Haukka, Matti; Sutradhar, Manas; Mizar, Archana; Kopylovich, Maximilian N.; Pombeiro, Armando J. L.

    2013-02-01

    Reaction of 2-(2-(2,4-dioxopentan-3-ylidene)hydrazinyl)benzenesulfonic acid (H2L) with copper(II) nitrate hydrate in the presence of pyrazine (pz) in methanol affords the coordination polymer [Cu2(μ-L)2(H2O)2(μ-pz)]n (1), where the bidentate pz molecule links two Cu(II) centres of two different dimeric units, giving rise to a one-dimensional chain. The dimeric unit [Cu2(μ-L)2(H2O)2] consists of two distorted octahedral Cu(II) centres connected via oxygen atoms of the sulfo group of the bridging L2- ligand. The extensive hydrogen bonding between the coordinated water and pz molecules leads to the formation of a supramolecular 3D associate. Compound 1 has been characterized by elemental analysis, ESI-MS, IR spectroscopy and single-crystal X-ray diffraction analysis.

  19. A new Ni(II complex as a novel and efficient recyclable catalyst for the synthesis of pyrano[2,3-d]pyrimidines

    Directory of Open Access Journals (Sweden)

    M. Habibi Kheirabadi

    2016-12-01

    Full Text Available A simple and highly efficient one-pot three-component synthesis of a series of pyrido[2,3-d]pyrimidines from the condensation of barbituric acid, malononitrile and aromatic aldehydes using catalytic amount of a new Ni(II complex based on 5-nitro-N1-((pyridin-2-ylmethylene benzene-1,2-diamine (NiL is reported. This new heterogeneous catalyst has the advantages of being environmentally friendly, simple work-up and high yields character.

  20. Polymerization of Methyl Methacrylate Catalyzed by Co(II), Cu(II), and Zn(II) Complexes Bearing N-Methyl-N-((pyridin-2-yl)methyl) cyclohexanamine

    Energy Technology Data Exchange (ETDEWEB)

    Ahn, Seoung Hyun; Lee, Hyosun [Kyungpook National University, Daegu (Korea, Republic of); Shin, Jongwon [POSTECH, Pohang (Korea, Republic of); Nayab, Saira [Shaheed Benazir Bhutto University, Sheringal (Pakistan)

    2016-05-15

    We demonstrated the synthesis and characterization of Co(II), Cu(II), and Zn(II) complexes ligated to N-methyl-N-((pyridin-2-yl)methyl)cyclohexanamine. The complex [Co(nmpc)Cl{sub 2}] in the presence of MMAO showed the highest catalytic activity for MMA polymerization at 60 °C compared with its Zn(II) and Cu(II) analogs. The metal center showed an obvious influence on the catalytic activity, although this appeared to have no effect on the stereo-regularity of the resultant PMMA. X-ray diffraction analysis revealed that [Co(nmpc)Cl{sub 2}] and [Zn(nmpc)Cl{sub 2}] crystallized in the monoclinic system with space group P2{sub 1}/c and existed as monomeric and solvent-free complexes.

  1. Effectively simultaneous naked-eye detection of Cu(II), Pb(II), Al(III) and Fe(III) using cyanidin extracted from red cabbage as chelating agent

    Science.gov (United States)

    Khaodee, Warangkhana; Aeungmaitrepirom, Wanlapa; Tuntulani, Thawatchai

    Simultaneous determination of Cu(II), Pb(II), Al(III) and Fe(III) using cyanidin as a chelating agent was investigated in terms of both quantitative and qualitative detections. Cyanidin was extracted and purified from red cabbage which is a local plant in Thailand. The selectivity of this method was examined by regulating the pH of cyanidin solution operated together with masking agents. It was found that Cu(II), Pb(II), Al(III) and Fe(III) simultaneously responded with the color change at pH 7, pH 6, pH 5 and pH 4, respectively. KF, DMG and the mixture of KF and DMG were used as masking agents for the determination of Fe(III), Al(III) and Pb(II), respectively. Results from naked-eye detection were evaluated by comparing with those of inductively coupled plasma (ICP), and there was no significant difference noticed. Cyanidin using as a multianalyte reagent could be employed for simultaneous determination of Cu(II), Pb(II), Al(III) and Fe(III) at the lowest concentration at 50, 80, 50 and 200 μM, respectively, by slightly varying pHs. Moreover, the proposed method could be potentially applied for real water samples with simplicity, rapidity, low cost and environmental safety.

  2. Electrospray ionization mass spectrometric investigations of the complexation behavior of macrocyclic thiacrown ethers with bivalent transitional metals (Cu, Co, Ni and Zn).

    Science.gov (United States)

    Tsybizova, Alexandra; Tarábek, Ján; Buchta, Michal; Holý, Petr; Schröder, Detlef

    2012-10-15

    Heavy metals are both a problem for the environment and an important resource for industry. Their selective extraction by means of organic ligands therefore is an attractive topic. The coordination of three thiacrown ethers to late 3d-metal ions was investigated by a combination of electrospray ionization mass spectrometry (ESI-MS) and electron paramagnetic resonance (EPR). The mass spectrometric experiments were carried out in an ion trap mass spectrometer with an ESI source. Absolute binding constants were estimated by comparison with data for 18-crown-6/Na(+). EPR spectroscopy was used as a complementary method for investigating the Cu(I) /Cu(II) redox couple. The study found that thiacrown ethers preferentially bind traces of copper even at an excess of other metal ions (Co(II), Ni(II), and Zn(II)). The absolute association constants of the Cu(I) complexes were about 10(8) M(-1), and about two orders of magnitude lower for the other 3d-metal cations. The EPR spectra demonstrated that the reduction from Cu(II) to Cu(I) upon formation of the [(thiacrown)Cu](+) species takes place in solution. ESI-MS demonstrated that the three thiacrown ligands examined had high binding constants as well as good selectivities for copper(I) at low concentrations, and in the presence of other metal ions. By a combination of ESI-MS and EPR spectrometry it was shown that the reduction from Cu(II) to Cu(I) occurred in solution. Copyright © 2012 John Wiley & Sons, Ltd.

  3. Synthesis, structural studies and antimicrobial activity of N'-((2Z, 3E)-3-(hydroxyimino)butan-2-ylidene)-2-phenylacetohydrazide and its Co(II), Ni(II) complexes

    Science.gov (United States)

    Karadeniz, Şeyma; Ataol, Cigdem Yuksektepe; Şahin, Onur; İdil, Önder; Bati, Hümeyra

    2018-06-01

    A new aroylhydrazoneoxime, N'-((2Z, 3E)-3-(hydroxyimino)butan-2-ylidene)-2-phenylacetohydrazide ligand (LH2) and its Ni(II) and Co(II) complexes, have been synthesized and characterized by elemental and thermal analyses, IR and UV-vis spectroscopy, magnetic moment and X-ray diffraction. The antimicrobial activities of these compounds were tested by using minimal inhibitory concentration method (MIC). The ligand-containing aroylhydrazone and oxime groups and its Ni complex crystallize in the triclinic system and P 1 - space group, while its Co complex crystallizes in the monoclinic system and the C 2/c space group. X-ray results show that the ligand in the keto form is transformed into enolic form when it forms coordination. From elemental analysis data, the stoichiometry of Co(II) complex was found to be 1:2 (metal/ligand), but 1:1 for Ni(II). IR spectra indicate that the ligand acts as monoanionic NNO- tridentate and coordination takes place form through the oxime nitrogen, imine nitrogen, and enolate oxygen atoms.

  4. Asymmetric synthesis of α-amino acids via homologation of Ni(II) complexes of glycine Schiff bases. Part 2: aldol, Mannich addition reactions, deracemization and (S) to (R) interconversion of α-amino acids.

    Science.gov (United States)

    Sorochinsky, Alexander E; Aceña, José Luis; Moriwaki, Hiroki; Sato, Tatsunori; Soloshonok, Vadim

    2013-11-01

    This review provides a comprehensive treatment of literature data dealing with asymmetric synthesis of α-amino-β-hydroxy and α,β-diamino acids via homologation of chiral Ni(II) complexes of glycine Schiff bases using aldol and Mannich-type reactions. These reactions proceed with synthetically useful chemical yields and thermodynamically controlled stereoselectivity and allow direct introduction of two stereogenic centers in a single operation with predictable stereochemical outcome. Furthermore, new application of Ni(II) complexes of α-amino acids Schiff bases for deracemization of racemic α-amino acids and (S) to (R) interconversion providing additional synthetic opportunities for preparation of enantiomerically pure α-amino acids, is also reviewed. Origin of observed diastereo-/enantioselectivity in the aldol, Mannich-type and deracemization reactions, generality and limitations of these methodologies are critically discussed.

  5. Efficient simultaneous removal of U(VI) and Cu(II) from aqueous solution using core-shell nZVI@SA/CMC-Ca beads

    International Nuclear Information System (INIS)

    Shuhong Hu; Xiaoyan Lin; Wenhui Zhao; Ministry of Education, Sichuan; Xuegang Luo

    2018-01-01

    Core-shell nanoscale zero-valent iron@alginate/carboxymethyl cellulose sodium composite loaded with calcium (nZVI@SA/CMC-Ca) beads were synthesized in this study using coaxial electronic injection method. The adsorbent structure was characterized via FT-IR, SEM, EDX and XPS. The adsorption behavior of U(VI) and Cu(II) on core-shell nZVI@SA/CMC-Ca beads was studied under various experimental parameters like pH, contact time and temperature. The isotherm and the kinetic data, pertaining to the adsorption of U(VI) and Cu(II) by core-shell nZVI@SA/CMC-Ca beads obeyed both the Langmuir and Freundlich isotherms model and the pseudo-second-order kinetics model, respectively. The thermodynamic parameters revealed the spontaneous and endothermic nature of the adsorption. The experiment of regeneration and reusability suggested core-shell nZVI@SA/CMC-Ca bead was a regenerated material. (author)

  6. Adsorption of heavy metal ions on molybdenum and molybdenum trioxide from dilute aqueous solution

    International Nuclear Information System (INIS)

    Utsunomiya, Taizo; Hoshino, Yoshio; Sakabe, Ken-ichi

    1984-01-01

    The adsorption of heavy metal ions such as Co(II), Cu(II) and Pb(II) on molybdenum powder has been investigated by the batch technique as a function of soaking time, concentration of heavy metal ions and coexisting salts, pH etc. Molybdenum trioxide was also used as an adsorbent for a comparison to discuss the adsorption mechanism. The amount of these heavy metal ions adsorbed was highly pH and coexisting salts dependent. These adsorbents have features of selective adsorption for Pb(II) and large adsorption rate. The adsorption of heavy metal ions on these adsorbents proceeds independently or concurrently by following complex mechanism; (1) cation exchange reaction by hydroxyl radical on the surface of Mo and MoO 3 is predominant for most of heavy metal ions except Pb(II) [Co(II), Mn(II), Fe(III), Ni(II), Zn(II), Cd(II) and Sr(II)], (2) reduction (electron exchange reaction) to low ionic or metallic state after cation exchange reaction [Cu(II) and Ag(I) on Mo] and (3) formation of a compound [Pb(II) on both Mo and MoO 3 ]. (author)

  7. Tetra-, Penta- and Hexa-Coordinated Transition Metal Complexes Constructed from Coumarin-Containing N2O2 Ligand

    Directory of Open Access Journals (Sweden)

    Lei Gao

    2018-02-01

    Full Text Available Three newly designed complexes, [Cu(L]·CHCl3 (1, [Co(L(MeOH]·CHCl3 (2 and [{Ni(L(MeOH(PhCOO}2Ni] (3 a coumarin-containing Salamo-type chelating ligand (H2L have been synthesized and characterized by elemental analyses, IR and UV-VIS spectra, and X-ray crystallography. Complex 1 includes one Cu(II atom, one completely deprotonated (L2− unit and one crystalling chloroform molecule, the Cu(II atom shows a square-planar geometry. Complex 2 includes one Co(II atom, one completely deprotonated (L2− unit, one coordinated methanol molecule and one crystalling chloroform molecule. The Co(II atom is a distorted trigonal-bipyramidal geometry. While complex 3 includes three Ni(II atoms, two completely deprotonated (L2− units, two benzoates and two coordinated methanol molecules. The complexes 1 and 2 are both possess three-dimensional supra-molecular structures by abundant noncovalent interactions. But, complex 3 formed a two-dimensional supra-molecular structure by intra-molecular hydrogen bonds. In addition, the antimicrobial and fluorescence properties of H2L and its complexes 1, 2 and 3 were also investigated.

  8. Development of a Novel Cu(II Complex Modified Electrode and a Portable Electrochemical Analyzer for the Determination of Dissolved Oxygen (DO in Water

    Directory of Open Access Journals (Sweden)

    Salvatore Gianluca Leonardi

    2016-04-01

    Full Text Available The development of an electrochemical dissolved oxygen (DO sensor based on a novel Cu(II complex-modified screen printed carbon electrode is reported. The voltammetric behavior of the modified electrode was investigated at different scan rates and oxygen concentrations in PBS (pH = 7. An increase of cathodic current (at about −0.4 vs. Ag/AgCl with the addition of oxygen was observed. The modified Cu(II complex electrode was demonstrated for the determination of DO in water using chronoamperometry. A small size and low power consumption home-made portable electrochemical analyzer based on custom electronics for sensor interfacing and operating in voltammetry and amperometry modes has been also designed and fabricated. Its performances in the monitoring of DO in water were compared with a commercial one.

  9. Formation of binary complexes of Co(II), Ni(II) and Cu(II) with L ...

    African Journals Online (AJOL)

    The trend in the variation of stability constants with change in the mole fraction of the medium was explained based on electrostatic and non-electrostatic forces. Distribution of the species with pH at different compositions of dioxan-water mixtures was also presented. KEY WORDS: Binary species, Stability constants, Metal, ...

  10. Mass-spectrometric study of phosphorous amides and their Co(O), Mo(O), Ni(II), and Cu(I) complexes

    International Nuclear Information System (INIS)

    Nifant'ev, E.E.; Blokhin, Y.I.; Chikishev, Y.G.; Rozynov, B.V.; Teleshev, A.T.

    1985-01-01

    This article examines the performance of the mass-spectroscopic method in investigating allied comounds and original kigands. Apart from Cu(I) complexes, Co(O), Mo(O), and Ni(II) derivatives. The nature of the organophosphorus ligand is shown as having a substantial indluence on the structure of the cobalt complexes formed. The breakdown of the original ligands is accompanied by the initial breakage of the P-N bond. In the halide complexes first the metal is eliminated with the formation of the XhaL fragment, and the halogen is eliminated subsequently, but in the carbonyl derivatives the stagewise elimination of CO groups occurs with the subsequent elimination of the metal

  11. Characterization of Ni(II) complexes of Schiff bases of amino acids and (S)-N-(2-benzoylphenyl)-1-benzylpyrrolidine-2-carboxamide using ion trap and QqTOF electrospray ionization tandem mass spectrometry

    NARCIS (Netherlands)

    Jirasko, Robert; Holcapek, Michal; Kolarova, Lenka; Nadvornik, Milan; Popkov, Alexander

    This work demonstrates the application of electrospray ionization mass spectrometry (ESI-MS) using two different mass analyzers, ion trap and hybrid quadrupole time-of-flight (QqTOF) mass analyzer, for the structural characterization of Ni(II) complexes of Schiff bases of

  12. Insolubilization of Chestnut Shell Pigment for Cu(II Adsorption from Water

    Directory of Open Access Journals (Sweden)

    Zeng-Yu Yao

    2016-03-01

    Full Text Available Chestnut shell pigment (CSP is melanin from an agricultural waste. It has potential as an adsorbent for wastewater treatment but cannot be used in its original state because of its solubility in water. We developed a new method to convert CSP to insolubilized chestnut shell pigment (ICSP by heating, and the Cu(II adsorption performance of ICSP was evaluated. The conversion was characterized, and the thermal treatment caused dehydration and loss of carboxyl groups and aliphatic structures in CSP. The kinetic adsorption behavior obeyed the pseudo-second-order rate law, and the equilibrium adsorption data were well described with both the Langmuir and the Freundlich isotherms. ICSP can be used as a renewable, readily-available, easily-producible, environmentally-friendly, inexpensive and effective adsorbent to remove heavy-metal from aquatic environments.

  13. Base Catalytic Approach: A Promising Technique for the Activation of Biochar for Equilibrium Sorption Studies of Copper, Cu(II Ions in Single Solute System

    Directory of Open Access Journals (Sweden)

    Sharifah Bee Abdul Hamid

    2014-04-01

    Full Text Available This study examines the feasibility of catalytically pretreated biochar derived from the dried exocarp or fruit peel of mangostene with Group I alkali metal hydroxide (KOH. The pretreated char was activated in the presence of carbon dioxide gas flow at high temperature to upgrade its physiochemical properties for the removal of copper, Cu(II cations in single solute system. The effect of three independent variables, including temperature, agitation time and concentration, on sorption performance were carried out. Reaction kinetics parameters were determined by using linear regression analysis of the pseudo first, pseudo second, Elovich and intra-particle diffusion models. The regression co-efficient, R2 values were best for the pseudo second order kinetic model for all the concentration ranges under investigation. This implied that Cu(II cations were adsorbed mainly by chemical interactions with the surface active sites of the activated biochar. Langmuir, Freundlich and Temkin isotherm models were used to interpret the equilibrium data at different temperature. Thermodynamic studies revealed that the sorption process was spontaneous and endothermic. The surface area of the activated sample was 367.10 m2/g, whereas before base activation, it was only 1.22 m2/g. The results elucidated that the base pretreatment was efficient enough to yield porous carbon with an enlarged surface area, which can successfully eliminate Cu(II cations from waste water.

  14. Synthesis and structural characterization of nickel(II), cobalt(II), Zinc(II), manganese(II), cadmium(II) and uranium(VI) complexes of α-oximinoacetoacet-o/p-anisidide thiosemicarbazone

    International Nuclear Information System (INIS)

    Patel, P.S.; Patel, M.M.; Ray, R.M.

    1993-01-01

    A few metal complexes of α-oximinoacetoacet-o/p-anisidide thiosemicarbazones (OAOATS)/(OAPATS) with Ni(II), Co(II), Zn(II), Mn(II), Hg(II), Cd(II) and UO 2 (II) have been prepared and characterized by elemental analyses, conductivity, differential scanning calorimetry study, thermogravimetric analyses and infrared and electronic spectral measurements in conjunction with magnetic susceptibility measurements at room temperature. They have also been tested for their antimicrobial activities. (author). 24 refs., 2 tabs

  15. The Influence of Pyrolytic Temperature on Sorption Ability of Carbon Xerogel Based on 3-Aminophenol-formaldehyde Polymer for Cu(II) Ions and Phenol.

    Czech Academy of Sciences Publication Activity Database

    Veselá, P.; Slovák, V.; Zelenka, T.; Koštejn, Martin; Mucha, M.

    2016-01-01

    Roč. 121, SEP (2016), s. 29-40 ISSN 0165-2370 Institutional support: RVO:67985858 Keywords : temperature of pyrolysis * sorption mechanism * Cu(II) ions Subject RIV: CI - Industrial Chemistry , Chemical Engineering Impact factor: 3.471, year: 2016

  16. CFA-13 - a bifunctional perfluorinated metal-organic framework featuring active Cu(i) and Cu(ii) sites.

    Science.gov (United States)

    Fritzsche, J; Denysenko, D; Grzywa, M; Volkmer, D

    2017-11-07

    The synthesis and crystal structure of the mixed-valent perfluorinated metal-organic framework (Me 2 NH 2 )[CFA-13] (Coordination Framework Augsburg University-13), (Me 2 NH 2 )[CuCu(tfpc) 4 ] (H 2 -tfpc = 3,5-bis(trifluoromethyl)-1H-pyrazole-4-carboxylic acid) is described. The copper-containing MOF crystallizes in the monoclinic crystal system within the space group P2 1 /n (no. 14) and the unit cell parameters are as follows: a = 22.3887(19), b = 13.6888(8), c = 21.1804(13) Å, β = 90.495(3)°, V = 6491.0(8) Å 3 . (Me 2 NH 2 )[CFA-13] features a porous 3-D structure constructed from two types of secondary building units (SBUs). Besides novel trinuclear [Cu(pz) 4 ] - coordination units, the network also exhibits Cu(ii) paddle-wheel SBUs. (Me 2 NH 2 )[CFA-13] is fully characterized by single crystal X-ray diffraction, thermogravimetric analysis, variable temperature powder X-ray diffraction, IR spectroscopy, photoluminescence, gas sorption measurements and pulse chemisorption experiments. M[CFA-13] (M = K + , Cs + ) frameworks were prepared by postsynthetic exchange of interchannel dimethylammonium cations. Moreover, it was shown that CO molecules can be selectively bound at Cu(i) sites of [Cu(pz) 4 ] - units, whereas Cu(ii) paddle-wheel units bind selectively NH 3 molecules.

  17. Modeling of solvent extraction equilibrium of Cu(II from sulphuric Acid solution with MOC-55TD

    Directory of Open Access Journals (Sweden)

    Alguacil, F. J.

    1999-06-01

    Full Text Available The extraction of Cu(II from acidic sulphate aqueous solutions using the commercial MOC-55TD extractant is studied. A predictive model, which consists in a set of non-linear mass action and mass balance equations is proposed. The model was solved using a tailor-made equation-solving program. The extraction of copper can be described by the formation of CuR2 species (log Kext= 0.717 ± 0.03 in the organic phase. The copper equilibrium isotherm was also obtained at 20°C.

    Se estudia la extracción de Cu(II de disoluciones acuosas acidas, en medio sulfato, mediante la oxima comercial MOC-55TD. Se propone un modelo para predecir la extracción del metal; este modelo consiste en una serie de ecuaciones no lineales de acción de masas y balance de masas. El modelo se resolvió empleando un programa de ordenador específicamente definido para este tipo de equilibrios. La extracción de cobre se describe por la formación de la especie CuR2 (log Kext= 0,717 ± 0,03 en la fase orgánica. Se ha obtenido la isoterma de extracción de cobre a 20 °C.

  18. Chelation of Cu(II, Zn(II, and Fe(II by Tannin Constituents of Selected Edible Nuts

    Directory of Open Access Journals (Sweden)

    Magdalena Karamać

    2009-12-01

    Full Text Available The tannin fractions isolated from hazelnuts, walnuts and almonds were characterised by colorimetric assays and by an SE-HPLC technique. The complexation of Cu(II and Zn(II was determined by the reaction with tetramethylmurexide, whereas for Fe(II, ferrozine was employed. The walnut tannins exhibited a significantly weaker reaction with the vanillin/HCl reagent than hazelnut and almond tannins, but the protein precipitation capacity of the walnut fraction was high. The SE-HPLC chromatogram of the tannin fraction from hazelnuts revealed the presence of oligomers with higher molecular weights compared to that of almonds. Copper ions were most effectively chelated by the constituents of the tannin fractions of hazelnuts, walnuts and almonds. At a 0.2 mg/assay addition level, the walnut tannins complexed almost 100% Cu(II. The Fe(II complexation capacities of the tannin fractions of walnuts and hazelnuts were weaker in comparison to that of the almond tannin fraction, which at a 2.5 mg/assay addition level, bound Fe(II by ~90%. The capacity to chelate Zn(II was quite varied for the different nut tannin fractions: almond tannins bound as much as 84% Zn(II, whereas the value for walnut tannins was only 8.7%; and for hazelnut tannins, no Zn(II chelation took place at the levels tested.

  19. Characterization and application of expanded graphite modified with phosphoric acid and glucose for the removal of Ni(II) from aqueous solution

    Science.gov (United States)

    Jiang, Li; Zhang, Jian; Xu, Xiaoli; Zhang, Jie; Liu, Hai; Guo, Zizhang; Kang, Yan; Li, Yiran; Xu, Jingtao

    2015-12-01

    Three kinds of modified expanded graphite (EG), impregnated with phosphoric acid (H3PO4) (P-EG), impregnated with glucose (G-EG), and impregnated with H3PO4 and glucose (G-P-EG), were prepared under a low temperature (150 °C). The adsorption capacity of G-P-EG (Qm = 7.016 mg/g) is much higher than original expanded graphite (EG Qm = 0.423 mg/g) and other two kinds of modified expanded graphite (P-EG Qm = 0.770 mg/g; G-EG Qm = 0.507 mg/g). The physicochemical properties of EG and G-P-EG were characterized by N2 adsorption/desorption, Boehm's titration and X-ray photoelectron spectroscopy (XPS). EG exhibited higher values of BET surface area (11.357 m2/g) and total pore volume (0.0303 cm3/g) than that of G-P-EG (4.808 m3/g and 0.0109 cm3/g). However, the results of Bohm's titration and XPS showed that G-P-EG contained more surface oxygen-containing functional groups. The Ni(II) adsorption equilibrium data agreed well with the Langmuir model. And the experimental data of EG and G-P-EG fitted better by pseudo-second order model. Based on the results of batch adsorption experiments and XPS analysis, there were several possible mechanisms for Ni(II) adsorption on the G-P-EG, including chemical adsorption, cation exchange, electrostatic attraction and surface complication.

  20. Kinetic studies of the impact of thiocyanate moiety on the catalytic properties of Cu(II) and Fe(III) complexes of a new Mannich base

    Science.gov (United States)

    Ayeni, Ayowole O.; Watkins, Gareth M.

    2018-04-01

    Four new metal complexes of a novel Mannich base 5-methyl-2-((4-(pyridin-2-yl)piperazin-1-yl)methyl)phenol (HL) have been prepared. The compounds were characterized by an array of analytical and spectroscopic methods including Nuclear Magnetic Resonance, Infra-red and UV-Visible spectroscopy. Compounds 1-4 behaved as effective catalysts towards the oxidation of 3,5-di-tert-butylcatechol (3,5-DTBC) to its corresponding quinone in the presence of molecular oxygen in DMF solution while compound 4 proved to be the best catalyst with a turnover rate of 17.93 ± 1.10 h-1 as other complexes showed lower rates of oxidation. Also with the exception of dinuclear iron complex (4); thiocyanate containing Cu(II) complex exhibited lower catecholase activity compared to the Cu(II) complex without it.

  1. Structurally flexible and solution stable [Ln4TM8(OH)8(L)8(O2CR)8(MeOH)y](ClO4)4

    DEFF Research Database (Denmark)

    Hooper, Thomas N.; Inglis, Ross; Lorusso, Giulia

    2016-01-01

    the predominant antiferromagnetic interactions in 2a yield an inverse magnetocaloric effect; that is, the temperature increases on lowering the applied field, under the proper experimental conditions. In spite of increasing the magnetic density by adding ions that bring in antiferromagnetic interactions (2a...... effect evolves by introducing either antiferromagnetic or ferromagnetic interactions, or magnetic anisotropy, by substituting the nonmagnetic ZnII (1a) with CuII (2a), NiII (6a) or CoII (7a), respectively. The largest magnetocaloric effect is found for the ferromagnetically coupled complex 6a, while......) or magnetic anisotropy (7a), the magnetocaloric effect is overall smaller in 2a and 7a than in 1a, where only four GdIII spins per molecule contribute to the magnetocaloric properties....

  2. Liquid membrane ion-selective electrodes for potentiometric dosage of coper and nickel

    Directory of Open Access Journals (Sweden)

    MARIA PLENICEANY

    2005-02-01

    Full Text Available This paper presents experimental and theoretical data regarding the preparation and characterization of three liquid-membrane electrodes, which have not been mentioned in the specialized literature so far. The active substances, the solutions of which in nitrobenzene formed the membranes on a graphite rod, are simple complex combinations of Cu(II and Ni(II ions with an organic ligand belonging to the Schiff base class: N-[2-thienylmethilidene]-2-aminoethanol (TNAHE. The Cu2+ -selective and Ni2+ -selective electrodes were used to determine the copper and nickel ions in aqueous solutions, both by direct potentiometry and by potentiometric titration with EDTA. They were also used for the determination of Cu2+ and Ni2+ ions in industrial waters by direct potentiometry.

  3. Synthesis, spectroscopic, biological activity and thermal characterization of ceftazidime with transition metals

    Science.gov (United States)

    Masoud, Mamdouh S.; Ali, Alaa E.; Elasala, Gehan S.; Kolkaila, Sherif A.

    2018-03-01

    Synthesis, physicochemical characterization and thermal analysis of ceftazidime complexes with transition metals (Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II)) were discussed. It's obtained that ceftazidime act as bidentate ligand. From magnetic measurement and spectral data, octahedral structures were proposed for all complexes except for cobalt, nickel and mercury had tetrahedral structural. Hyper chemistry program confirmed binding sites of ceftazidime. Ceftazidime complexes show higher activity than ceftazidime for some strains. From TG and DTA curves the thermal decomposition mechanisms of ceftazidime and their metal complexes were suggested. The thermal decomposition of the complexes ended with the formation of metal oxides as a final product except in case of Hg complex.

  4. Evaluating Design Parameters for Breakthrough Curve Analysis and Kinetics of Fixed Bed Columns for Cu(II Cations Using Lignocellulosic Wastes

    Directory of Open Access Journals (Sweden)

    Zaira Zaman Chowdhury

    2014-12-01

    Full Text Available A continuous adsorption study for removal of Cu(II cations from wastewater using a fixed-bed column was conducted. A granular carbonaceous activated adsorbent produced by carbonization of the outer rind, or exocarp, of mangostene fruit shell was used for column packing. The effects of feed flow rate, influent cation concentration, and bed depth on the breakthrough curve were investigated at pH 5.5. Experimental analysis confirmed that the breakthrough curves were dependent on flow rate, initial concentration of Cu(II cations, and bed height related to the amount of activated carbon used for column packing. Thomas, Yoon–Nelson, and Adams–Bohart models were applied to analyze the breakthrough curves at different conditions. Linear regression analysis of experimental data demonstrated that Thomas and Yoon–Nelson models were appropriate to explain the breakthrough curve, while the Adams–Bohart model was only applicable to predict the initial part of the dynamic process. It was concluded that the column packed with fruit rind based activated carbon can be used to treat Cu(II-enriched wastewater.

  5. Estudio de los mecanismos de activación de la esfalerita con Cu(II y Pb(II

    Directory of Open Access Journals (Sweden)

    Dávila Pulido, G. I.

    2011-08-01

    Full Text Available This article presents results of an experimental study on the sphalerite activation with Cu(II and Pb(II, whose main objective was to investigate the activation mechanisms and to evaluate the magnitude of the hydrophobization achieved with both chemical species. The hydrophobicity acquired by the mineral due to the interaction with the activator and collector (sodium isopropyl xanthate is characterized making use of the contact angle technique. The results show that Cu(II replaces the Zn of the external layers of the mineral, promoting the sulfide (S2– oxidation to produce a mixture of CuS, Cu2S and S°, of hydrophobic nature. The subsequent interaction with xanthate increases the hydrophobicity of the mineral surface. In turn, Pb(II activation of sphalerite is due to the formation of a PbS layer that reacts with xanthate to produce hydrophobic species (e.g., PbX2. It is also observed that the hydrophobicity of sphalerite activated with Pb(II is favored under air atmospheres, as compared to that obtained under nitrogen atmospheres. It is concluded that the hydrophobicity achieved by lead activation may be of the same order of magnitude to that deliverately induced by copper activation.

    Este artículo presenta los resultados de un estudio experimental sobre la activación de esfalerita (ZnS con Cu(II y Pb(II, cuyo objetivo principal consistió en investigar los mecanismos de activación y en evaluar la magnitud relativa de la hidrofobización alcanzada con ambas especies químicas. La hidrofobicidad que la superficie mineral adquiere como resultado de la interacción con los activadores y colectores tipo xantato (ditiocarbonatos alquílicos, R-O-CS2 –, se caracteriza mediante la técnica del ángulo de contacto. Los resultados muestran que el Cu(II es intercambiado por el Zn de las capas exteriores del cristal, promoviendo la oxidación de sulfuro (S2– para producir una mezcla de

  6. Zone-refining of beryllium(II) acetylacetonate

    International Nuclear Information System (INIS)

    Yoshida, Isao; Kobayashi, Hiroshi; Ueno, Keihei

    1975-01-01

    Zone melting was applied to bis (acetylacetonato) beryllium(II), Be(AA) 2 , to remove trace metal constiutents. The effective distribution coefficient, k, of a minor component measured in a binary mixture with the majority of Be(AA) 2 , fell in the range of 0.4 to 0.8, while the value obtained in a multiple component mixture fell in the range of 0.8 to 0.9 except Zn(II)- and Ni(II) chelates. Cr(AA) 3 was concentrated upward in the direction of the zone travelling, and similar results were obtained with Cu(II)-, Co(III)- Fe(III)- and Al(III) acetylacetonates, while Zn(II)-, Ni(II)- and Mn(III) chelates were fractionated in the both ends of the column. On the other hand, when the zone was moved downward, the minor components were concentrated in the lower end of a column. Efficiency in zone refining was compared to each other between the upward- and downward zone travelling modes on the crude beryllium acetylacetonates obtained from a commercial reagent of beryllium nitrate, and the latter mode was found more effective in the concentration of trace components. Discussion was given on possible mechanisms resulting in the difference in the refining efficiency. (author)

  7. A colorimetric and luminescent dual-modal assay for Cu(II ion detection using an iridium(III complex.

    Directory of Open Access Journals (Sweden)

    Dik-Lung Ma

    Full Text Available A novel iridium(III complex-based chemosensor bearing the 5,6-bis(salicylideneimino-1,10-phenanthroline ligand receptor was developed, which exhibited a highly sensitive and selective color change from colorless to yellow and a visible turn-off luminescence response upon the addition of Cu(II ions. The interactions of this iridium(III complex with Cu2+ ions and thirteen other cations have been investigated by UV-Vis absorption titration, emission titration, and 1H NMR titration.

  8. Sorption Behavior of Cu(II From Acidic SolutionUsing Weathered Basalt Andesite Products

    Directory of Open Access Journals (Sweden)

    Rajesh Singh

    2007-01-01

    Full Text Available Wastewater discharged from electroplating industry pose a serioushazard due to their heavy metal load. The objective of this work is to evaluatethe removal of Cu(II from acidic solution by sorption onto Weathered BasaltAndesite Products (WBAP. WBAP has been characterized and utilized forremoval of copper from aqueous solution over wide range of initial metal ionconcentration (25 mg/L to 500 mg/L, contact duration (0-8 h, sorbent dose(5-35 g/L, pH (1.0 to 6.0, and temperature (276 K to 333 K. The sorptionpattern of Cu ions onto WBAP followed Langmuir, Freundlich, and Dubinin-Kaganer-Radushkevich isotherms. The thermodynamic parameters (∆H0, ∆S0,and ∆G0 for Cu sorption onto WBAP were also determined.

  9. Effect of pre-pyrolysis mode on simultaneous introduction of nitrogen/oxygen-containing functional groups into the structure of bagasse-based mesoporous carbon and its influence on Cu(II) adsorption.

    Science.gov (United States)

    Wan, Zeqing; Li, Kunquan

    2018-03-01

    A convenient effective microwave pre-pyrolysis treatment to synthesize biomass-based mesoporous carbon with higher nitrogen/oxygen-chelating adsorption for Cu(II) is reported here, in which phosphoric acid impregnated bagasse was used as a microwave absorber and porogen. For comparison, conventional electric-heating pyrolyzed carbon was prepared and doped with nitrogen/oxygen groups. Nitrogen adsorption, scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy (XPS) and batch adsorption were employed to investigate the effects of the two pre-pyrolysis modes on the sample physicochemical and Cu(II) adsorptive properties. The 22-min-microwave-pyrolyzed bagasse mesoporous activated carbon (MBAC, 85.32% mesoporosity) contained 10.52% O, which is 3.94% more than electric-heating pyrolyzed mesoporous activated carbon (89.52% mesoporosity). After electrophilic aromatic substitutions of N/O doping, the former possessed more N (5.83%) and more O (21.40%), confirming that time-saving energy-efficient microwave pyrolysis favors the formation of defective C/O atoms in or at the edges of the graphite layer of MBAC, which are highly active and tend to act as preferred reactive positions for the doping of N/O-containing groups simultaneously compared with conventional electric-heating pyrolysis. These N and O species existed mainly as COOH, OH, NH and NH 2 functional groups, and were confirmed by XPS to be active sites for metal binding via electrostatic attraction, hydrogen bonding, a chelate effect and complexation, resulting in the great enhancement of Cu(II) adsorption. Langmuir isotherm and pseudo-second-order kinetic fitting further proved that Cu(II) adsorption by N/O-doped MBAC is ascribed mainly to chemisorption. Therefore, rapid microwave pre-pyrolysis provides a promising route to prepare excellent-performance N/O-doped carbon adsorbents. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Silica gel modified with N-(3-propyl)-O-phenylenediamine: functionalization, metal sorption equilibrium studies and application to metal enrichment prior to determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Akl, Magda Ali Abd-elAziz; Kenawy, Ibraheim Mohamed; Lasheen, Rabab Ramadan

    2005-08-01

    The use of the chemically modified silica gel N-(3-propyl)-O-phenylenediamine (SiG-NPPDA) adsorbent, for the preconcentration and separation of trace heavy metals, was described. SiG-NPPDA sorbs quantitatively (90-100% recovery) trace amounts of nine heavy metals, viz., Cd(II), Zn(II), Fe(III), Cu(II), Pb(II), Mn(II), Cr(III), Co(II) and Ni(II) at pH 7-8. The sorption capacity varies from 350 to 450 micromol g(-1). Desorption was found to be quantitative with 1-2 M HNO3 or 0.05 M Na2EDTA. The distribution coefficient, Kd and the percentage concentration of the investigated metal ions on the adsorbent at equilibrium, C(M,eqm)% (Recovery, R%), were studied as a function of experimental parameters. The logarithmic values of the distribution coefficient, log Kd, ranges between 4.0 and 6.4. Some foreign ions caused little interference in the preconcentration and determination of the investigated nine metals by flame atomic absorption spectrometry (AAS). The adsorbent and its formed metal chelates were characterized by IR (absorbance and/or reflectance), potentiometric titrations and thermogravimetric analysis (TGA and DTG). The mode of chelation between the SiG-NPPDA adsorbent and the investigated metal ions is proposed to be due to the reaction of the investigated metal ions with the two nitrogen atoms of the SiG-NPPDA adsorbent. The present adsorbent coupled with flame AAS has been used to enrich and determine the nine metal ions in natural aqueous systems and in certified reference materials (RSD < or = 5%). The copper, iron, manganese and zinc present in some pharmaceutical vitamin samples were also preconcentrated on SiG-NPPDA adsorbent and determined by flame AAS (RSD < or = 4.2%). Nanogram concentrations (0.07-0.14 ng ml(-1)) of Cd(II), Zn(II), Fe(III), Pb(II), Cr(III), Mn(II), Cu(II), Co(II) and Ni(II) can be determined reliably with a preconcentration factor of 100.

  11. Adsorption of some metal complexes derived from acetyl acetone on activated carbon and purolite S-930

    Directory of Open Access Journals (Sweden)

    Salam A.H. Al-Ameri

    2014-12-01

    Full Text Available A new Schiff base (HL derived from condensation of p-anisidine and acetyl acetone has been prepared and used as a chelating ligand to prepare Cr(III, Mn(II, Co(II, Ni(II and Cu(II complexes. The study of the nature of these complexes formed in ethanol solution following the mole ratio method (2:1, L:M gave results which were compared successfully with these obtained from isolated solid state studies. These studies revealed that the complexes having square planner geometry of the type (ML2, M = Co(II, Ni(II and Cu(II, and octahedral geometry of the type [CrIIIL2(H2O2]Cl and [MNIIL2(H2O2]. The adsorption studies of three complexes Cr(III, Mn(II, and Co(II on activated carbon, H and Na-forms of purolite S-930 resin show high adsorption percentage for Cr(III on purolite S-930 due to ion exchange interaction compared with high adsorption of neutral Mn(II, Co(II complexes on activated charcoal. Linear plot of log Qe versus log Ce showed that the adsorption isotherm of these three complexes on activated carbon, H and Na-forms of purolite S-930 surface obeys Freundlich isotherm and was similar to S-curve type according to Giles classification which investigates heterogeneous adsorption. The regression values indicate that the adsorption data for these complexes fitted well within the Freundlich isothermal plots for the concentration studied. The accuracy and precision of the concentration measurements of these complexes were determined by preparing standard laboratory samples, the results show relative error ranging from ±1.08 to 5.31, ±1.04 to 4.82 and ±0.28 to 3.09 and the relative standard deviation did not exceed ±6.23, ±2.77 and ±4.38% for A1, A2 and A3 complexes, respectively.

  12. Semi-interpenetrating hybrid membranes containing ADOGEN{sup ®} 364 for Cd(II) transport from HCl media

    Energy Technology Data Exchange (ETDEWEB)

    Mora-Tamez, Lucía; Rodríguez de San Miguel, Eduardo; Briones-Guerash, Ulrich; Munguía-Acevedo, Nadia M.; Gyves, Josefina de, E-mail: degyves@unam.mx

    2014-09-15

    Graphical abstract: - Highlights: • Semi-interpenetrating hybrid membranes are used for quantitative cadmium(II) recovery. • Optimization of membrane and solutions compositions is performed. • Membranes present increased stability respect to polymer inclusion membranes. • Models for cadmium (II) extraction and transport are proposed. • Excellent selectivity for Cd(II) over Ni(II), Cu(II) and Pb(II) was achieved. - Abstract: Cd(II) transport from 1 mol dm{sup −3} HCl media was investigated across semi-interpenetrating hybrid membranes (SIHMs) that were prepared by mixing an organic matrix composed of ADOGEN{sup ®} 364 as an extracting agent, cellulose triacetate as a polymeric support and nitrophenyloctyl ether as a plasticizer with an organic/inorganic network (silane phase, SP) composed of polydimethylsiloxane and a crosslinking agent. The stripping phase used was a 10{sup −2} mol dm{sup −3} ethanesulfonic acid solution. The effects of tetraorthoethoxysilane, phenyltrimethoxysilane and N′,N′-bis[3-tri(methoxysilyl)propyl]ethylendiamine as crosslinking agents on the transport were studied. H{sub 3}PO{sub 4} was used as an acid catalyst during the SP synthesis and optimized for transport performance. Solid–liquid extraction experiments were performed to determine the model that describe the transport of Cd(II) via ADOGEN{sup ®} 364. The transport was found to be chained-carrier controlled with a percolation threshold of 0.094 mmol g{sup −1}. The selective recovery of Cd(II) was studied with respect to Ni(II), Zn(II), Cu(II), and Pb(II) at a 1:1 molar ratio, and the optimized membrane system was applied for the recovery of Cd(II) from a real sample consisting of a Ni/Cd battery with satisfactory results. Finally, stability experiments were performed using the same membrane for 14 cycles. The results obtained showed that SIHMs had excellent stability and selectivity, with permeabilities comparable to those of PIMs.

  13. Microencapsulated Aliivibrio fischeri in Alginate Microspheres for Monitoring Heavy Metal Toxicity in Environmental Waters

    Directory of Open Access Journals (Sweden)

    Dedi Futra

    2014-12-01

    Full Text Available In this article a luminescence fiber optic biosensor for the microdetection of heavy metal toxicity in waters based on the marine bacterium Aliivibrio fischeri (A. fischeri encapsulated in alginate microspheres is described. Cu(II, Cd(II, Pb(II, Zn(II, Cr(VI, Co(II, Ni(II, Ag(I and Fe(II were selected as sample toxic heavy metal ions for evaluation of the performance of this toxicity microbiosensor. The loss of bioluminescence response from immobilized A. fischeri bacterial cells corresponds to changes in the toxicity levels. The inhibition of the luminescent biosensor response collected at excitation and emission wavelengths of 287 ± 2 nm and 487 ± 2 nm, respectively, was found to be reproducible and repeatable within the relative standard deviation (RSD range of 2.4–5.7% (n = 8. The toxicity biosensor based on alginate micropsheres exhibited a lower limit of detection (LOD for Cu(II (6.40 μg/L, Cd(II (1.56 μg/L, Pb(II (47 μg/L, Ag(I (18 μg/L than Zn(II (320 μg/L, Cr(VI (1,000 μg/L, Co(II (1700 μg/L, Ni(II (2800 μg/L, and Fe(III (3100 μg/L. Such LOD values are lower when compared with other previous reported whole cell toxicity biosensors using agar gel, agarose gel and cellulose membrane biomatrices used for the immobilization of bacterial cells. The A. fischeri bacteria microencapsulated in alginate biopolymer could maintain their metabolic activity for a prolonged period of up to six weeks without any noticeable changes in the bioluminescence response. The bioluminescent biosensor could also be used for the determination of antagonistic toxicity levels for toxicant mixtures. A comparison of the results obtained by atomic absorption spectroscopy (AAS and using the proposed luminescent A. fischeri-based biosensor suggests that the optical toxicity biosensor can be used for quantitative microdetermination of heavy metal toxicity in environmental water samples.

  14. Synthesis, characterization and biological activity of some transition metals with Schiff base derived from 2-thiophene carboxaldehyde and aminobenzoic acid

    Science.gov (United States)

    Mohamed, Gehad G.; Omar, M. M.; Hindy, Ahmed M. M.

    2005-12-01

    Metal complexes of Schiff base derived from 2-thiophene carboxaldehyde and 2-aminobenzoic acid (HL) are reported and characterized based on elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance and thermal analysis (TGA). The ligand dissociation as well as the metal-ligand stability constants were calculated pH metrically at 25 °C and ionic strength μ = 0.1 (1 M NaCl). The complexes are found to have the formulae [M(HL) 2](X) n· yH 2O (where M = Fe(III) (X = Cl, n = 3, y = 3), Co(II) (X = Cl, n = 2, y = 1.5), Ni(II) (X = Cl, n = 2, y = 1) and UO 2(II) (X = NO 3, n = 2, y = 0)) and [M(L) 2] (where M = Cu(II) (X = Cl) and Zn(II) (X = AcO)). The molar conductance data reveal that Fe(III) and Co(II), Ni(II) and UO 2(II) chelates are ionic in nature and are of the type 3:1 and 2:1 electrolytes, respectively, while Cu(II) and Zn(II) complexes are non-electrolytes. IR spectra show that HL is coordinated to the metal ions in a terdentate manner with ONS donor sites of the carboxylate O, azomethine N and thiophene S. From the magnetic and solid reflectance spectra, it is found that the geometrical structure of these complexes are octahedral. The thermal behaviour of these chelates shows that the hydrated complexes losses water molecules of hydration in the first step followed immediately by decomposition of the anions and ligand molecules in the subsequent steps. The activation thermodynamic parameters, such as, E*, Δ H*, Δ S* and Δ G* are calculated from the DrTG curves using Coats-Redfern method. The synthesized ligands, in comparison to their metal complexes also were screened for their antibacterial activity against bacterial species, Escherichia coli, Pseudomonas aeruginosa, Staphylococcus pyogones and Fungi (Candida). The activity data show that the metal complexes to be more potent/antibacterial than the parent Schiff base ligand against one or more bacterial species.

  15. Sorption studies of heavy metal ions by salicylic acid–formaldehyde–catechol terpolymeric resin: Isotherm, kinetic and thermodynamics

    Directory of Open Access Journals (Sweden)

    Riddhish R. Bhatt

    2015-05-01

    Full Text Available Terpolymeric resin has been synthesized by condensing salicylic acid with catechol employing formaldehyde as a cross linking agent at 80 ± 5 °C using DMF as a solvent. The resin was characterized by elemental analysis, FTIR, XRD and thermal analysis (TGA, DTA and DTG. The morphology of the resin was studied by optical photographs and scanning electron micrographs (SEM at different magnifications. The physico-chemical properties have been studied. The uptake behavior of various metal ions viz. Ni(II, Cu(II, Zn(II, Cd(II and Pb(II towards synthesized resin has been studied depending on contact time, pH and temperature. The selectivity order found is: Cu(II > Zn(II > Pb(II > Ni(II > Cd(II. The sorption data obtained at optimized conditions were analyzed by six two parameter isotherm models like Langmuir, Freundlich, Temkin, Dubinin–Radushkevich (D–R, Halsey and Harkins–Jura. The Langmuir, Freundlich and Dubinin–Radushkevich (D–R isotherms were found better to describe the sorption data with high correlation for the adsorption with a low SSE value for all the metals under study. The adsorption capacities of the SFC resin for removal of Ni(II, Cu(II, Zn(II, Cd(II and Pb(II were determined with the Langmuir equation and found to be 0.815, 1.104, 1.215, 0.498, and 0.931 mmol/g respectively. The adsorption process follows first order kinetics and specific rate constant Kr was obtained by the application of Lagergren equation. Thermodynamic parameters viz. ΔGads, ΔSads and ΔHads have also been calculated for the metal-resin systems. The external diffusion rate constant (Ks and intra-particle diffusion rate constant (Kid were calculated by Spahn–Schlunder and Weber–Morris models respectively. Desorption studies were done using various desorbing agents viz. de-ionized water, boiled water, various concentrations of HCl, ammonia, thiourea, citric acid and tartaric acid.

  16. Selective and Efficient Solvent Extraction of Copper(II Ions from Chloride Solutions by Oxime Extractants

    Directory of Open Access Journals (Sweden)

    Zahra Kaboli Tanha

    2016-06-01

    Full Text Available Oxime extractants 3-tert-butyl-2-hydroxy-5-methyl benzaldehyde oxime (HL1 and 3-tert-butyl-2-hydroxy-5-methoxy benzaldehyde oxime (HL2 were synthesized and characterized by conventional spectroscopic methods. Suitable lipophilic nature of the prepared extractants allowed examining the ability of these molecules for extraction-separation of copper from its mixture with normally associated metal ions by performing competitive extraction experiments of Cu(II, Co(II, Ni(II, Zn(II, Cd(II and Pb(II ions from chloride solutions. Both ligands transfer selectively the copper ions into dichloromethane by a cation exchange mechanism. Conventional log-log analysis and isotherm curves showed that Cu(II ions are extracted as the complexes with 1:2 metal to ligand ratio by both extractants. Verification of the effect of the organic diluent used in the extraction of copper ions by HL1 and HL2 demonstrated that the extraction efficiency varies as: dichloromethane ~ dichloroethane > toluene > xylene > ethylacetate. Time dependency investigation of the extraction processes revealed that the kinetics of the extraction of copper by HL2 is more rapid than that of HL1. The application of the ligands for extraction-separation of copper ions from leach solutions of cobalt and nickel-cadmium filter-cakes of a zinc production plants was evaluated.

  17. Synthesis, spectral, thermal and biological studies of transition metal complexes of 4-hydroxy-3-[3-(4-hydroxyphenyl-acryloyl]-6-methyl-2H-pyran-2-one

    Directory of Open Access Journals (Sweden)

    BALASAHEB R. ARBAD

    2011-09-01

    Full Text Available The solid complexes of Mn(II, Fe(III, Co(II, Ni(II, and Cu(II with 4-hydroxy-3-[(2E-3-(4-hydroxyphenylprop-2-enoyl]-6-methyl-2H-pyran-2-one, derived from 3-acetyl-6-methyl-2H-pyran-2,4(3H-dione (dehydroacetic acid and 4-hydroxybenzaldehyde, were synthesized and characterized by elemental analysis, conductometry, thermal analysis, magnetic measurements, IR, 1H-NMR and UV–Vis spectroscopy and a biological study. From the analytical and spectral data, the stoichiometry of the complexes was found to be 1:2 (metal:ligand. The physico–chemical data suggest a distorted octahedral geometry for the Cu(II complexes and an octahedral geometry for all the other complexes. The thermal decomposition of all the complexes was studied by the TG–DTA method. The synthesized ligand and its metal complexes were screened for their in vitro antibacterial activity against Gram-negative (Escherichia coli and Gram-positive (Staphylococcus aureus bacterial strains and for in vitro antifungal activity against Aspergillus flavus, Curvularia lunata and Penicillium notatum. The results of these studies showed the metal complexes to be more antibacterial/antifungal against one or more species as compared with the non-complexed ligand.

  18. Potentiometric and spectroscopic study of the interaction of 3d transition metal ions with inositol hexakisphosphate

    Science.gov (United States)

    Veiga, Nicolás; Macho, Israel; Gómez, Kerman; González, Gabriel; Kremer, Carlos; Torres, Julia

    2015-10-01

    Among myo-inositol phosphates, the most abundant in nature is the myo-inositol hexakisphosphate, InsP6. Although it is known to be vital to cell functioning, the biochemical research into its metabolism needs chemical and structural analysis of all the protonation, complexation and precipitation processes that it undergoes in the biological media. In view of its high negative charge at physiological level, our group has been leading a thorough research into the InsP6 chemical and structural behavior in the presence of the alkali and alkaline earth metal ions essential for life. The aim of this article is to extend these studies, dealing with the chemical and structural features of the InsP6 interaction with biologically relevant 3d transition metal ions (Fe(II), Fe(III), Mn(II), Co(II), Ni(II), Cu(II) and Zn(II)), in a non-interacting medium and under simulated physiological conditions. The metal-complex stability constants were determined by potentiometry, showing under ligand-excess conditions the formation of mononuclear species in different protonation states. Under metal ion excess, polymetallic species were detected for Fe(II), Fe(III), Zn(II) and Cu(II). Additionally, the 31P NMR and UV-vis spectroscopic studies provided interesting structural aspects of the strong metal ion-InsP6 interaction.

  19. Highly stable acyclic bifunctional chelator for {sup 64}Cu PET imaging

    Energy Technology Data Exchange (ETDEWEB)

    Abada, S.; Lecointre, A.; Christine, C.; Charbonniere, L. [CNRS/UDS, EPCM, Strasbourg (France). Lab. d' Ingenierie Appliquee a l' Analyse; Dechamps-Olivier, I. [Univ. de Reims Champagne Ardenne, Reims (France). Group Chimie de Coordination; Platas-Iglesias, C. [Univ. da Coruna (Spain). Dept. de Quimica Fundamental; Elhabiri, M. [CNRS/UDS, EPCM, Strasbourg (France). Lab. de Physico-Chimie Bioinorganique

    2011-07-01

    Ligand L{sup 1}, based on a pyridine scaffold, functionalized by two bis(methane phosphonate)aminomethyl groups, was shown to display a very high affinity towards Cu(II) (log K{sub CuL}=22.7) and selectivity over Ni(II), Co(II), Zn(II) and Ga(III) ({delta} log K{sub ML}>4) as shown by the values of the stability constants obtained from potentiometric measurements. Insights into the coordination mode of the ligand around Cu(II) cation were obtained by UV-Vis absorption and EPR spectroscopies as well as density functional theory (DFT) calculations (B3LYP model) performed in aqueous solution. The results point to a pentacoordination pattern of the metal ion in the fully deprotonated [CuL{sup 1}]{sup 6-} species. Considering the beneficial thermodynamic parameters of this ligand, kinetic experiments were run to follow the formation of the copper(II) complexes, indicating a very rapid formation of the complex, appropriate for {sup 64}Cu complexation. As L{sup 1} represents a particularly interesting target within the frame of {sup 64}Cu PET imaging, a synthetic protocol was developed to introduce a labeling function on the pyridyl moiety of L{sup 1}, thereby affording L{sup 2}, a potential bifunctional chelator (BFC) for PET imaging.

  20. Transition metal complexes of a new 15-membered [N5] penta-azamacrocyclic ligand with their spectral and anticancer studies

    Science.gov (United States)

    El-Boraey, Hanaa A.; Serag El-Din, Azza A.

    2014-11-01

    Novel penta-azamacrocyclic 15-membered [N5] ligand [L] i.e. 1,5,8,12-tetetraaza-3,4: 9,10-dibenzo-6-ethyl-7-methyl-1,12-(2,6-pyrido)cyclopentadecan-5,7 diene-2,11-dione and its transition metal complexes with Co(II), Ni(II), Cu(II), Ru(III) and Pd(II) have been synthesized and structurally characterized by elemental analysis, spectral, thermal as well as magnetic and molar conductivity measurements. On basis of IR, MS, UV-Vis 1H NMR and EPR spectral studies an octahedral geometry has been proposed for all complexes except Co(II), Cu(II) nitrate complexes and Pd(II) chloride complex that adopt tetrahedral, square pyramidal and square planar geometries, respectively. The antitumor activity of the synthesized ligand and some complexes against human breast cancer cell lines (MCF-7) and human hepatocarcinoma cell lines (HepG2) has been studied. The complexes (IC50 = 2.04-9.7, 2.5-3.7 μg/mL) showed potent antitumor activity comparable with their ligand (IC50 = 11.7, 3.45 μg/mL) against the above mentioned cell lines, respectively. The results evidently show that the activity of the ligand becomes more pronounced and significant when coordinated to the metal ion.

  1. Biosorption of copper(II), lead(II), iron(III) and cobalt(II) on Bacillus sphaericus-loaded Diaion SP-850 resin

    International Nuclear Information System (INIS)

    Tuzen, Mustafa; Uluozlu, Ozgur Dogan; Usta, Canan; Soylak, Mustafa

    2007-01-01

    The biosorption of copper(II), lead(II), iron(III) and cobalt(II) on Bacillus sphaericus-loaded Diaion SP-850 resin for preconcentration-separation of them have been investigated. The sorbed analytes on biosorbent were eluted by using 1 mol L -1 HCl and analytes were determined by flame atomic absorption spectrometry. The influences of analytical parameters including amounts of pH, B. sphaericus, sample volume etc. on the quantitative recoveries of analytes were investigated. The effects of alkaline, earth alkaline ions and some metal ions on the retentions of the analytes on the biosorbent were also examined. Separation and preconcentration of Cu, Pb, Fe and Co ions from real samples was achieved quantitatively. The detection limits by 3 sigma for analyte ions were in the range of 0.20-0.75 μg L -1 for aqueous samples and in the range of 2.5-9.4 ng g -1 for solid samples. The validation of the procedure was performed by the analysis of the certified standard reference materials (NRCC-SLRS 4 Riverine Water, SRM 2711 Montana soil and GBW 07605 Tea). The presented method was applied to the determination of analyte ions in green tea, black tea, cultivated mushroom, boiled wheat, rice and soil samples with successfully results

  2. Effect of Cu(II), Cd(II) and Zn(II) on Pb(II) biosorption by algae Gelidium-derived materials.

    Science.gov (United States)

    Vilar, Vítor J P; Botelho, Cidália M S; Boaventura, Rui A R

    2008-06-15

    Biosorption of Pb(II), Cu(II), Cd(II) and Zn(II) from binary metal solutions onto the algae Gelidium sesquipedale, an algal industrial waste and a waste-based composite material was investigated at pH 5.3, in a batch system. Binary Pb(II)/Cu(II), Pb(II)/Cd(II) and Pb(II)/Zn(II) solutions have been tested. For the same equilibrium concentrations of both metal ions (1 mmol l(-1)), approximately 66, 85 and 86% of the total uptake capacity of the biosorbents is taken by lead ions in the systems Pb(II)/Cu(II), Pb(II)/Cd(II) and Pb(II)/Zn(II), respectively. Two-metal results were fitted to a discrete and a continuous model, showing the inhibition of the primary metal biosorption by the co-cation. The model parameters suggest that Cd(II) and Zn(II) have the same decreasing effect on the Pb(II) uptake capacity. The uptake of Pb(II) was highly sensitive to the presence of Cu(II). From the discrete model it was possible to obtain the Langmuir affinity constant for Pb(II) biosorption. The presence of the co-cations decreases the apparent affinity of Pb(II). The experimental results were successfully fitted by the continuous model, at different pH values, for each biosorbent. The following sequence for the equilibrium affinity constants was found: Pb>Cu>Cd approximately Zn.

  3. Preparation and characterisation of some transition metal complexes of niacinamide (vitamin b3)

    International Nuclear Information System (INIS)

    Hasan, M.M.; Hossain, M.E.; Halim, M.E.

    2015-01-01

    Niacinamide forms metal complexes of general formula (M(C/sub 6/H/sub 6/N/sub 2/O)2)Cl/sub 2/; where M = Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) in the aqueous medium. The complexes were formulated by comparing the experimental and calculated data for C, H, N and metal. The prepared complexes were characterized by different physicochemical methods. The UV-vis, FTIR spectral analysis and thermo gravimetric analysis (TGA). TGA of these complexes have been discussed. Magnetic susceptibility values indicate that all complexes except Zn complex are paramagnetic in nature. The redox properties of the metal ions in the Mn, Cu and Zn complexes have been discussed from the cyclic voltammetric studies. In all cases the systems are quasi reversible. (author)

  4. Cloud point extraction for the determination of heavy metals by nonionic surfactant Triton X-100 and PAN

    International Nuclear Information System (INIS)

    Cabrera Puig, I.; Perez Gramatges, A.

    2006-01-01

    A novel methodology for extraction and preconcentration of trace metals based on cloud point phenomenon was applied to the analysis of Co(II), Cu(II), Cd(II), Pb(II) y Ni(II) in a certified reference material (CRM), using Triton X-100 as nonionic surfactant, and AAS for the determination. Different parameters that can influence the extraction efficiency were studied, such as pH and ionic strength of the solution. The precision, accuracy and detection limits of the method were determined using a CRM from the Environmental Analysis Laboratory of InSTEC. We applied our methodology to the detection of the metals in naturals waters (Almendares river and tap water) . The data obtained presented in this work is part of the validation file of the proposed analytical procedure for the determination of heavy metals

  5. Synthesis, characterization and spectroscopic studies of the dihydrobis(1,2,3-benzotriazolylborate anion and its complexes with MCl2·py2

    Directory of Open Access Journals (Sweden)

    KHWAJA S. SIDDIQI

    2006-11-01

    Full Text Available The preparation of sodium dihydrobis(1,2,3-benzotriazolylborate was realised by refluxing one mole of sodium borohydride with two moles of 1,2,3-benzotriazole in toluene over a period of 12 h. Its complexes with MCl2·py2 [whereM=Mn(II, Fe(II, Co(II, Ni(II, Cu(II and py=pyridine] were characterized by elemental analysis as well as magnetic, spectroscopic and conductivity measurements. On the basis of these studies, it is proposed that the geometry of all the complexes is octahedral. The ligand field parameters 10 Dq, B and b show extensive overlap between the M–L orbital. The molar conductance of 10-3 M solutions of the complexes in DMSO suggest them to be non-ionic in nature.

  6. Magnetic exchange couplings from noncollinear perturbation theory: dinuclear CuII complexes.

    Science.gov (United States)

    Phillips, Jordan J; Peralta, Juan E

    2014-08-07

    To benchmark the performance of a new method based on noncollinear coupled-perturbed density functional theory [J. Chem. Phys. 138, 174115 (2013)], we calculate the magnetic exchange couplings in a series of triply bridged ferromagnetic dinuclear Cu(II) complexes that have been recently synthesized [Phys. Chem. Chem. Phys. 15, 1966 (2013)]. We find that for any basis-set the couplings from our noncollinear coupled-perturbed methodology are practically identical to those of spin-projected energy-differences when a hybrid density functional approximation is employed. This demonstrates that our methodology properly recovers a Heisenberg description for these systems, and is robust in its predictive power of magnetic couplings. Furthermore, this indicates that the failure of density functional theory to capture the subtle variation of the exchange couplings in these complexes is not simply an artifact of broken-symmetry methods, but rather a fundamental weakness of current approximate density functionals for the description of magnetic couplings.

  7. In situ ligand generation for novel Mn(II) and Ni(II) coordination polymers with disulfide ligand: Solvothermal syntheses, structures and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Han, Yinfeng, E-mail: hanyinfeng@gmail.com; Wang, Chang' an; Zheng, Zebao; Sun, Jiafeng; Nie, Kun; Zuo, Jian; Zhang, Jianping

    2015-07-15

    Two coordination polymers, ([Mn{sub 2}(L1){sub 2}(μ{sub 2}-H{sub 2}O)(H{sub 2}O){sub 4}]·5H{sub 2}O){sub n}1 and ([Ni(L1)(H{sub 2}O){sub 2}]·2H{sub 2}O){sub n}2 (H{sub 2}L1=2,2′-dithiobisnicotinic acid), were prepared by the solvothermal reactions of the Mn(II) or Ni(II) ions with 2-mercaptonanicotinic acid. In 1, the [Mn{sub 2}(COO){sub 4}] units are connected by the 2,2′-dithiobisnicotinic dianion to form a two-dimensional (4,4)-connected network. In 2, the adjacent Ni(II) ions are connected by the carboxyl groups of the 2,2′-dithiobisnicotinic dianion to form an one-dimensional inorganic rod-shaped chain [Ni(COO){sub 2}]{sub n}, which are further interconnected by the 2,2′-dithiobisnicotinic ligand, giving rise to a two-dimensional framework. Variable-temperature magnetic susceptibilities of 1 and 2 exhibit overall weak antiferromagnetic coupling between the adjacent metal ions. - Graphical abstract: Two 2D coordination polymers were synthesized by transition-metal/in-situ oxidation of 2-mercaptonicotinic acid. The compounds pack into 2D frameworks by the carboxyl groups of 2,2′-dithiobisnicotinic dianion and exhibit overall weak antiferromagnetic coupling. - Highlights: • Two 2D coordination polymers containing 2,2′-dithiobisnicotinic dianion. • In situ oxidation and dehydro coupling reaction of 2-mercaptonbenzoic acid. • Two compounds display weak antiferromagnetic exchanges.

  8. Enhancement strategies for Cu(II), Cr(III) and Cr(VI) remediation by a variety of seaweed species.

    Science.gov (United States)

    Murphy, V; Hughes, H; McLoughlin, P

    2009-07-15

    Various chemical treatments have been applied to six brown, red and green seaweed species with a view to enhancing their metal removal for Cu(II), Cr(III) and Cr(VI). Treatment with acetone resulted in the greatest enhancement for both cationic and anionic species with relatively low mass losses (15-35%), indicating its low risk to biomass operational stability. Cation binding was increased by 69%, while the total Cr removal was augmented by 15%. Cr(VI) binding was shown to be an adsorption-coupled reduction, whereby Cr(VI) was bound to the biomass surface at pH 2 and subsequently reduced to Cr(III). Acetone treatment also resulted in biomasses that were capable of converting up to 83% of Cr(VI) in solution to Cr(III). Blocking of carboxyl and amino functionalities had significant negative effects both on total Cr removal as well as percentage conversion of Cr(VI) to Cr(III). Results therefore indicated the significant role played by these moieties in metal binding to these seaweeds. Potentiometric titrations displayed agreement between the degree of esterification and the decrease in Cu(II) removal for Ulva spp. and Polysiphonia lanosa. FTIR analysis identified changes in biomass functionality and availability after chemical modification, the results of which were in agreement with metal removal studies. In conclusion, these biosorbents represent suitable candidates to replace conventional removal technologies for metal bearing wastewaters, in particular for the detoxification of hazardous Cr(VI) waste streams.

  9. Gamma radiolysis of Cu(II) complex of metronidazole

    International Nuclear Information System (INIS)

    Mandal, P.C.; Bardhan, D.K.; Bhattacharyya, S.N.

    1990-01-01

    Aqueous solutions of Cu(II)Metronidazole (Cu(II)M) at neutral pH were irradiated with 60 Co γ-rays under different conditions of radiolysis. The radiolytic formation of HNO 2 and Cu(I) was followed. The radiolytic yields of chromophore loss of Cu(II)M were also determined under different conditions. The OH radicals attack the metal complex to give the OH adducts of the ligand at C 2 , C 4 , and C 5 either directly or through the formation of Cu(III) species. The C 5 -OH adduct, however, undergoes oxidative denitration and as a result the metal complex is decomposed. The OH adducts also undergo electron transfer to Cu(II) ion to give reduced complex. No denitration was observed due to the reaction of e eq - with the metal complex. On the other hand, the nitro group of the ligand in the complex undergoes successive 4-electron reduction to give hydroxylamino derivative. From the competition kinetics using t-butyl alcohol as the scavenger of OH in N 2 O saturated solution of the metal complex, the rate constant for the reaction of OH with complex was evaluated to be ca. 2.1x10 9 dm 3 mol -1 s -1 which is of the same order as that observed in the case of free metronidazole. (author)

  10. Removal of Cu(II) and Pb(II) from Aqueous Solutions Using Nanoporous Materials

    Science.gov (United States)

    Dutta, Debajani; Roy, Sushanta Kumar; Das, Bodhaditya; Talukdar, Anup K.

    2018-05-01

    The present work deals with the adsorption of Cu2+ and Pb2+ on zeolites (ZSM-5, mordenite) and mesoporous materials (MCM-48, MCM-41). The characterization of the synthesized samples was performed by means of XRD, SEM, and thermogravimetric analysis. The batch method was employed to study the influence of adsorbent nature, contact time, initial metal ion concentration, and adsorbent load. The adsorption on MCM-48 follows a pseudo-second-order kinetic model. This material was found to be more effective for the removal of lead in a batch process as compared to the other adsorbents and the removal efficiency of the materials for Pb(II) followed the order MCM-48 > mordenite > ZSM-5 > MCM-41 and that for Cu(II) followed the order ZSM-5 > mordenite > MCM-41 > MCM-48.

  11. Crystal structure of bis(azido-κNbis[2,5-bis(pyridin-2-yl-1,3,4-thiadiazole-κ2N2,N3]cobalt(II

    Directory of Open Access Journals (Sweden)

    Abdelhakim Laachir

    2015-05-01

    Full Text Available In the mononuclear title complex, [Co(N32(C12H8N4S2], the cobalt(II atom is located on an inversion centre and displays an axially weakly compressed octahedral coordination geometry. The equatorial positions are occupied by the N atoms of two 2,5-bis(pyridin-2-yl-1,3,4-thiadiazole ligands, whereas the axial positions are occupied by N atoms of the azide anions. The thiadiazole and pyridine rings linked to the metal are almost coplanar, with a maximum deviation from the mean plane of 0.0273 (16 Å. The cohesion of the crystal is ensured by weak C—H...N hydrogen bonds and by π–π interactions between pyridine rings [intercentroid distance = 3.6356 (11 Å], forming a layered arrangement parallel to (001. The structure of the title compound is isotypic with that of the analogous nickel(II complex [Laachir et al. (2013. Acta Cryst. E69, m351–m352].

  12. INFLUENCIA DEL pH SOBRE LA ADSORCIÓN EN CARBÓN ACTIVADO DE Cd(II) Y Ni(II) DESDE SOLUCIONES ACUOSAS

    OpenAIRE

    Paola Rodríguez; Liliana Giraldo; Juan Carlos Moreno

    2011-01-01

    La adsorción de iones Cd(II) y Ni(II) desde soluciones acuosas sobre carbón activado se estudia con diferentes valores de pH. La adsorción de los iones se realiza en dos condiciones de pH de la solución: en la primera el pH varía en el transcurso del proceso a medida que los iones se adsorben y en la segunda el pH se mantiene fijo durante la adsorción. Cuando no se realiza un control en el pH de la solución se observan incrementos en la concentración de los io...

  13. The hierarchical porous structure bio-char assessments produced by co-pyrolysis of municipal sewage sludge and hazelnut shell and Cu(II) adsorption kinetics.

    Science.gov (United States)

    Zhao, Bing; Xu, Xinyang; Zeng, Fanqiang; Li, Haibo; Chen, Xi

    2018-05-04

    The co-pyrolysis technology was applied to municipal sewage sludge (MSS) and hazelnut shell with alkaline activating agent K 2 CO 3 under N 2 atmosphere. The innovative bio-char produced by co-pyrolysis had significant physical and chemical characteristics. The specific surface area reached 1990.23 m 2 /g, and the iodine absorption number was 1068.22 mg/g after co-pyrolysis at 850 °C. Although hazelnut shell was a kind of solid waste, it also had abundant cellulose resource, which could contribute to porous structure of bio-char during co-pyrolysis with MSS and decrease total heavy metals contents of raw material to increase security of bio-chars. Meanwhile, the residual fractions of heavy metals in bio-char were above 92.95% after co-pyrolysis at 900 °C except Cd to prevent heavy metals digestion, and the bio-char presented significant immobilization behavior from co-pyrolysis technology. Moreover, the yield and the iodine absorption number of bio-chars under different process variables were analyzed, and it was confirmed that appropriate process variables could contribute the yield and the iodine absorption number of bio-char and prevent to etch pore structure excessively to collapse. The changes of surface functional groups and crystallographic structure before and after co-pyrolysis were analyzed by FTIR and XRD, respectively. The hierarchical porous structure of bio-char was presented by SEM and N 2 adsorption-desorption isotherm. The Cu(II) adsorption capacity of the bio-char was 42.28 mg/g after 24 h, and surface functional groups acted as active binding sites for Cu(II) adsorption. Langmuir model and pseudo-second-order model can describe process of Cu(II) adsorption well.

  14. Characterization of L-cysteine capped CdTe quantum dots and application to test Cu(II) deficiency in biological samples from critically ill patients

    Energy Technology Data Exchange (ETDEWEB)

    Sáez, Laura; Molina, Jorge; Florea, Daniela I.; Planells, Elena M. [Institute of Nutrition and Food Technology and Department of Physiology, Faculty of Pharmacy, Campus Cartuja, University of Granada, E-18071 Granada (Spain); Cabeza, M. Carmen [Department of Physical Chemistry, Faculty of Pharmacy, University of Granada, E-18071 Granada (Spain); Quintero, Bartolomé, E-mail: bqosso@ugr.es [Department of Physical Chemistry, Faculty of Pharmacy, University of Granada, E-18071 Granada (Spain)

    2013-06-27

    Graphical abstract: -- Highlights: •We examinate stability of L-cysteine capped CdTe QD. •Factors influence QD fluorescence response are controlled. •Application in copper deficiency analysis is made. •We report comparison with other techniques. -- Abstract: The catalytic activity of copper ion gives, from the physiological point of view, a central role in many biological processes. Variations in the composition and location of cellular copper have been addressed given their physiological and pathological consequences. In this paper L-cysteine capped CdTe quantum dots is used for the fluorimetric determination of Cu(II) in biological samples from healthy individuals and patients admitted to the Intensive Care Units (ICU). An acceptable homogeneity in the CdTe QDs size has been obtained with an average value of 3 nm. No significant alterations in the spectral properties were observed for 2 months when stored in vacutainers at 6 °C and a concentration of approximately 2 μM. Data from oxidative stress markers such superoxide dismutase, total antioxidant capacity and DNA damage can be correlated with a Cu(II) deficiency for the ICU patients as measured by flame-atomic absorption spectroscopy (FAAS) and inductively coupled plasma source mass spectrometry (ICP-MS). Aqueous solutions 0.3 μM of L-cysteine capped CdTe QDs in MOPS buffer (6 mM, pH 7.4) used at 21 °C in the range 15–60 min after preparation of the sample for the measurements of fluorescence gives contents in Cu(II) for erythrocytes in good agreement with those obtained in FAAS and ICP-MS but the comparative ease of use makes the fluorimetric technique more suitable than the other two techniques for routine analysis.

  15. Kinetic and isotherm studies of Cu(II) biosorption onto valonia tannin resin

    Energy Technology Data Exchange (ETDEWEB)

    Sengil, I. Ayhan [Department of Environmental Engineering, Engineering Faculty, Sakarya University, 54100 Sakarya (Turkey)], E-mail: asengil@sakarya.edu.tr; Ozacar, Mahmut [Department of Chemistry, Science and Arts Faculty, Sakarya University, 54100 Sakarya (Turkey); Tuerkmenler, Harun [Institute of Sciences and Technology, Sakarya University, 54040 Sakarya (Turkey)

    2009-03-15

    The biosorption of Cu(II) from aqueous solutions by valonia tannin resin was investigated as a function of particle size, initial pH, contact time and initial metal ion concentration. The aim of this study was to understand the mechanisms that govern copper removal and find a suitable equilibrium isotherm and kinetic model for the copper removal in a batch reactor. The experimental isotherm data were analysed using the Langmuir, Freundlich and Temkin equations. The equilibrium data fit well in the Langmuir isotherm. The experimental data were analysed using four sorption kinetic models - the pseudo-first- and second-order equations, the Elovich and the intraparticle diffusion model equation - to determine the best fit equation for the biosorption of copper ions onto valonia tannin resin. Results show that the pseudo-second-order equation provides the best correlation for the biosorption process, whereas the Elovich equation also fits the experimental data well.

  16. Thermodynamic Modeling of Poorly Complexing Metals in Concentrated Electrolyte Solutions: An X-Ray Absorption and UV-Vis Spectroscopic Study of Ni(II) in the NiCl2-MgCl2-H2O System

    Science.gov (United States)

    Zhang, Ning; Brugger, Joël; Etschmann, Barbara; Ngothai, Yung; Zeng, Dewen

    2015-01-01

    Knowledge of the structure and speciation of aqueous Ni(II)-chloride complexes is important for understanding Ni behavior in hydrometallurgical extraction. The effect of concentration on the first-shell structure of Ni(II) in aqueous NiCl2 and NiCl2-MgCl2 solutions was investigated by Ni K edge X-ray absorption (XAS) and UV-Vis spectroscopy at ambient conditions. Both techniques show that no large structural change (e.g., transition from octahedral to tetrahedral-like configuration) occurs. Both methods confirm that the Ni(II) aqua ion (with six coordinated water molecules at R Ni-O = 2.07(2) Å) is the dominant species over the whole NiCl2 concentration range. However, XANES, EXAFS and UV-Vis data show subtle changes at high salinity (> 2 mol∙kg-1 NiCl2), which are consistent with the formation of small amounts of the NiCl+ complex (up to 0.44(23) Cl at a Ni-Cl distance of 2.35(2) Å in 5.05 mol∙kg-1 NiCl2) in the pure NiCl2 solutions. At high Cl:Ni ratio in the NiCl2-MgCl2-H2O solutions, small amounts of [NiCl2]0 are also present. We developed a speciation-based mixed-solvent electrolyte (MSE) model to describe activity-composition relationships in NiCl2-MgCl2-H2O solutions, and at the same time predict Ni(II) speciation that is consistent with our XAS and UV-Vis data and with existing literature data up to the solubility limit, resolving a long-standing uncertainty about the role of chloride complexing in this system. PMID:25885410

  17. Effects of 12 metal ions on iron regulatory protein 1 (IRP-1) and hypoxia-inducible factor-1 alpha (HIF-1α) and HIF-regulated genes

    International Nuclear Information System (INIS)

    Li Qin; Chen Haobin; Huang Xi; Costa, Max

    2006-01-01

    Several metal ions that are carcinogenic affect cellular iron homeostasis by competing with iron transporters or iron-regulated enzymes. Some metal ions can mimic a hypoxia response in cells under normal oxygen tension, and induce expression of HIF-1α-regulated genes. This study investigated whether 12 metal ions altered iron homeostasis in human lung carcinoma A549 cells as measured by an activation of IRP-1 and ferritin level. We also studied hypoxia signaling by measuring HIF-1α protein levels, hypoxia response element (HRE)-driven luciferase reporter activity, and Cap43 protein level (an HIF-1α responsive gene). Our results show the following: (i) Ni(II), Co(II), V(V), Mn(II), and to a lesser extent As(III) and Cu(II) activated the binding of IRP-1 to IRE after 24 h, while the other metal ions had no effect; (ii) 10 of 12 metal ions induced HIF-1α protein but to strikingly different degrees. Two of these metal ions, Al(III) and Cd(II), did not induce HIF-1α protein; however, as indicated below, only Ni(II), Co (II), and to lesser extent Mn(II) and V(V) activated HIF-1α-dependent transcription. The combined effects of both [Ni(II) + As(III)] and [Ni(II) + Cr(VI)] on HIF-1α protein were synergistic; (iii) Addition of Fe(II) with Ni(II), Co(II), and Cr(VI) attenuated the induction of HIF-1α after 4 h treatment; (iv) Ni(II), Co(II), and Mn(II) significantly decrease ferritin level after 24 h exposure; (v) Ni(II), Co(II), V(V), and Mn(II) activated HRE reporter gene after 20 h treatment; (vi) Ni(II), Co(II), V(V), and Mn(II) increased the HIF-1-dependent Cap43 protein level after 24 h treatment. In conclusion, only Ni (II), Co (II), and to a lesser extent Mn(II) and V(V) significantly stabilized HIF-1α protein, activated IRP, decreased the levels of ferritin, induced the transcription of HIF-dependent reporter, and increased the expression of Cap43 protein levels (HIF-dependent gene). The mechanism for the significant stabilization and elevation of HIF-1

  18. The characteristics of dissolved organic matter (DOM) in storm sewer sediments and the binding interaction with Cu(II) in four typical regions in Beijing, China.

    Science.gov (United States)

    Zhang, Ziyang; Li, Kun; Zhang, Xiaoran; Li, Haiyan

    2017-07-01

    In this work, dissolved organic matter (DOM) was extracted from storm sewer sediments collected in four typical regions (residential, campus, traffic and business regions) in Beijing, China. The basic characteristics of DOM were analyzed by UV-visible spectroscopy (UV-Vis), excitation-emission matrix Fluorescence Spectroscopy and Fourier Transform Infrared Spectroscopy. Furthermore, the complexation between DOM and Cu(II) were investigated. The results showed that there were large amount of aromatic structure in the DOM extracted from storm sewer sediments. The microbial activities had also made a contribution to the DOM in storm sewer sediments. The composition of DOM influenced the complexing capacity of Cu(II) greatly, which may be attributed to the protein-like and humic-like substances in storm sewer sediments. This study demonstrated valuable information on the structure present in the DOM of storm sewer sediments and provided new insight for exploring the relationship between DOM and co-existing heavy metals in storm sewer sediments.

  19. Enhanced selective removal of Cu(II) from aqueous solution by novel polyethylenimine-functionalized ion imprinted hydrogel: Behaviors and mechanisms.

    Science.gov (United States)

    Wang, Jingjing; Li, Zhengkui

    2015-12-30

    A novel polyethylenimine-functionalized ion-imprinted hydrogel (Cu(II)-p(PEI/HEA)) was newly synthesized by (60)Co-γ-induced polymerization for the selective removal of Cu(II) from aqueous solution. The adsorption performances including the adsorption capacity and selectivity of the novel hydrogel were much better than those of similar adsorbents reported. The hydrogel was characterized via scanning electron microscope, transmission electron microscopy, Fourier transform infrared spectra, thermal gravimetric analysis and X-ray photoelectron spectroscopy to determine the structure and mechanisms. The adsorption process was pH and temperature sensitive, better fitted to pseudo-second-order equation, and was Langmuir monolayer adsorption. The maximum adsorption capacity for Cu(II) was 40.00 mg/g. The selectivity coefficients of ion-imprinted hydrogel for Cu(II)/Pb(II), Cu(II)/Cd(II) and Cu(II)/Ni(II) were 55.09, 107.47 and 63.12, respectively, which were 3.93, 4.25 and 3.53 times greater than those of non-imprinted hydrogel, respectively. Moreover, the adsorption capacity of Cu(II)-p(PEI/HEA) could still keep more than 85% after four adsorption-desorption cycles. Because of such enhanced selective removal performance and excellent regeneration property, Cu(II)-p(PEI/HEA) is a promising adsorbent for the selective removal of copper ions from wastewater. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Adsorption of Pb(II and Cu(II by Ginkgo-Leaf-Derived Biochar Produced under Various Carbonization Temperatures and Times

    Directory of Open Access Journals (Sweden)

    Myoung-Eun Lee

    2017-12-01

    Full Text Available Ginkgo trees are common street trees in Korea, and the large amounts of leaves that fall onto the streets annually need to be cleaned and treated. Therefore, fallen gingko leaves have been used as a raw material to produce biochar for the removal of heavy metals from solutions. Gingko-leaf-derived biochar was produced under various carbonization temperatures and times. This study evaluated the physicochemical properties and adsorption characteristics of gingko-leaf-derived biochar samples produced under different carbonization conditions regarding Pb(II and Cu(II. The biochar samples that were produced at 800 °C for 90 and 120 min contained the highest oxygen- and nitrogen-substituted carbons, which might contribute to a high metal-adsorption rate. The intensity of the phosphate bond was increased with the increasing of the carbonization temperature up to 800 °C and after 90 min of carbonization. The Pb(II and Cu(II adsorption capacities were the highest when the gingko-leaf-derived biochar was produced at 800 °C, and the removal rates were 99.2% and 34.2%, respectively. The highest removal rate was achieved when the intensity of the phosphate functional group in the biochar was the highest. Therefore, the gingko-leaf-derived biochar produced at 800 °C for 90 min can be used as an effective bio-adsorbent in the removal of metals from solutions.

  1. Analytical application of aminohydroxamic acids

    International Nuclear Information System (INIS)

    Fadl Elmoula, Abd ELfatah Abdella

    2000-11-01

    Anthranilic hydroxamic acid was prepared by coupling of methylanthranilate (prepared by esterification of anthranilic acid with methyl alcohol using the fisher-speir method) with freshly prepared hydroxylamine. The lignad was characterized by the usual reaction of hydroxamic acid with acidic V(V) and Fe(III) solutions that gives blood-red colour in amyl alcohol and deep-violet colour in aqueous solution, respectively. The absorbance of Fe(III)-hydroxamic acids complexes increases with increase of pH. In this study, the effect of pH on the absorbance of Fe(III)-anthranilic hydroxamic acid was in accordance with this trend. The maximum absorbance was obtained at pH 5.0 at maximum wavelength of 482 nm. For Cu(II)-anthranilic hydroxamic acid complex, the use of acidic basic pH lead to precipitation of Cu(II)-ligand complex. But when using buffer pH (acetic acid/sodium acetate) a clear green colour of Cu(II)-ligand complex was obtained. The maximum wavelength of 390 nm. V(V)-anthranilic hydroxamic acid complex was extracted in acidic medium in amyl alcohol at pH 2.0 because in aqueous solution V(V)-anthranilic hydroxamic acid complex has not clear colour. It was observed the the maximum extraction in acidic medium decrease sharply with the increasing of pH value. The maximum wavelength for maximum absorbance was recorded at 472 nm. V(V) interfered with determination of Fe(III)) above concentration of 2 ppm, whereas Cu(II) interferes slightly with the determination of Fe(III) ions even at a high concentration of the Cu(II) ions. Both Cu(II) and Ni(II) do not interfere with the determination of V(V) ions even at high concentrations, Fe(III) ion produced slight interference, while Mo(VI) ions have a pronounced interference. Both V(V) and Fe(III) ions interfered markedly with the determination of Cu(II) ions, and made impractical under conditions. However, the calibration curves for the three metal ions produced a practical linear dynamic range.(Author)

  2. Reaction of Non-Symmetric Schiff Base Metallo-Ligand Complexes Possessing an Oxime Function with Ln Ions

    Directory of Open Access Journals (Sweden)

    Jean-Pierre Costes

    2018-03-01

    Full Text Available The preparation of non-symmetric Schiff base ligands possessing one oxime function that is associated to a second function such as pyrrole or phenol function is first described. These ligands, which possess inner N4 or N3O coordination sites, allow formation of cationic or neutral non-symmetric CuII or NiII metallo-ligand complexes under their mono- or di-deprotonated forms. In presence of Lanthanide ions the neutral complexes do not coordinate to the LnIII ions, the oxygen atom of the oxime function being only hydrogen-bonded to a water molecule that is linked to the LnIII ion. This surprising behavior allows for the isolation of LnIII ions by non-interacting metal complexes. Reaction of cationic NiII complexes possessing a protonated oxime function with LnIII ions leads to the formation of original and dianionic (Gd(NO352− entities that are well separated from each other. This work highlights the preparation of well isolated mononuclear LnIII entities into a matrix of diamagnetic metal complexes. These new complexes complete our previous work dealing with the complexing ability of the oxime function toward Lanthanide ions. It could open the way to the synthesis of new entities with interesting properties, such as single-ion magnets for example.

  3. Characterization and application of expanded graphite modified with phosphoric acid and glucose for the removal of Ni(II) from aqueous solution

    International Nuclear Information System (INIS)

    Jiang, Li; Zhang, Jian; Xu, Xiaoli; Zhang, Jie; Liu, Hai; Guo, Zizhang; Kang, Yan; Li, Yiran; Xu, Jingtao

    2015-01-01

    Highlights: • Glucose and H 3 PO 4 , single or together, were used to modify expanded graphite. • The modified condition was at a low temperature (150 °C). • The properties of EG and the highest adsorption ability modified EG were compared. • G-P-EG has the highest adsorption ability, which is much higher than that of EG. - Abstract: Three kinds of modified expanded graphite (EG), impregnated with phosphoric acid (H 3 PO 4 ) (P-EG), impregnated with glucose (G-EG), and impregnated with H 3 PO 4 and glucose (G-P-EG), were prepared under a low temperature (150 °C). The adsorption capacity of G-P-EG (Q m = 7.016 mg/g) is much higher than original expanded graphite (EG Q m = 0.423 mg/g) and other two kinds of modified expanded graphite (P-EG Q m = 0.770 mg/g; G-EG Q m = 0.507 mg/g). The physicochemical properties of EG and G-P-EG were characterized by N 2 adsorption/desorption, Boehm's titration and X-ray photoelectron spectroscopy (XPS). EG exhibited higher values of BET surface area (11.357 m 2 /g) and total pore volume (0.0303 cm 3 /g) than that of G-P-EG (4.808 m 3 /g and 0.0109 cm 3 /g). However, the results of Bohm's titration and XPS showed that G-P-EG contained more surface oxygen-containing functional groups. The Ni(II) adsorption equilibrium data agreed well with the Langmuir model. And the experimental data of EG and G-P-EG fitted better by pseudo-second order model. Based on the results of batch adsorption experiments and XPS analysis, there were several possible mechanisms for Ni(II) adsorption on the G-P-EG, including chemical adsorption, cation exchange, electrostatic attraction and surface complication.

  4. Influencia del ph sobre la adsorción en carbón activado de cd(ii) y ni(ii) desde soluciones acuosas

    OpenAIRE

    Rodríguez, Paola; Giraldo, Liliana; Moreno, Juan Carlos

    2011-01-01

    La adsorción de iones Cd(II) y Ni(II) desde soluciones acuosas sobre carbón activado se estudia con diferentes valores de pH. La adsorción de los iones se realiza en dos condiciones de pH de la solución: en la primera el pH varía en el transcurso del proceso a medida que los iones se adsorben y en la segunda el pH se mantiene fijo durante la adsorción. Cuando no se realiza un control en el pH de la solución se observan incrementos en la concentración de los io...

  5. Synthesis, spectral and theoretical studies of Ni(II), Pd(II) and Pt(II) complexes of 5-mercapto-1,2,4-triazole-3-imine-2'-hydroxynaphthaline.

    Science.gov (United States)

    Gaber, Mohamed; El-Ghamry, Hoda; Atlam, Faten; Fathalla, Shaimaa

    2015-02-25

    Ni(II), Pd(II) and Pt(II) complexes of 5-mercapto-1,2,4-triazole-3-imine-2'-hydroxynaphthaline have been isolated and characterized by elemental analysis, IR, (1)H NMR, EI-mass, UV-vis, molar conductance, magnetic moment measurements and thermogravimetric analysis. The molar conductance values indicated that the complexes are non-electrolytes. The magnetic moment values of the complexes displayed diamagnetic behavior for Pd(II) and Pt(II) complexes and tetrahedral geometrical structure for Ni(II) complex. From the bioinorganic applications point of view, the interaction of the ligand and its metal complexes with CT-DNA was investigated using absorption and viscosity titration techniques. The Schiff-base ligand and its metal complexes have also been screened for their antimicrobial and antitumor activities. Also, theoretical investigation of molecular and electronic structures of the studied ligand and its metal complexes has been carried out. Molecular orbital calculations were performed using DFT (density functional theory) at B3LYP level with standard 6-31G(d,p) and LANL2DZ basis sets to access reliable results to the experimental values. The calculations were performed to obtain the optimized molecular geometry, charge density distribution, extent of distortion from regular geometry, the highest occupied molecular orbital (HOMO), the lowest unoccupied molecular orbital (LUMO), Mulliken atomic charges, reactivity index (ΔE), dipole moment (D), global hardness (η), softness (σ), electrophilicity index (ω), chemical potential and Mulliken electronegativity (χ). Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Cobalt(II) complexes with azole-pyridine type ligands for non-aqueous redox-flow batteries: Tunable electrochemistry via structural modification

    Science.gov (United States)

    Armstrong, Craig G.; Toghill, Kathryn E.

    2017-05-01

    A single species redox flow battery employing a new class of cobalt(II) complexes with 'tunable' tridentate azole-pyridine type ligands is reported. Four structures were synthesised and their electrochemical, physical and battery characteristics were investigated as a function of successive substitution of the ligand terminal pyridyl donors. The Co(II/I) and Co(III/II) couples are stable and quasi-reversible on gold and glassy carbon electrodes, however redox potentials are tunable allowing the cobalt potential difference to be preferentially increased from 1.07 to 1.91 V via pyridine substitution with weaker σ-donating/π-accepting 3,5-dimethylpyrazole groups. The charge-discharge properties of the system were evaluated using an H-type glass cell and graphite rod electrodes. The complexes delivered high Coulombic efficiencies of 89.7-99.8% and very good voltaic efficiencies of 70.3-81.0%. Consequently, energy efficiencies are high at 63.1-80.8%, marking an improvement on other similar non-aqueous systems. Modification of the ligands also improved solubility from 0.18 M to 0.50 M via pyridyl substitution with 3,5-dimethylpyrazole, though the low solubility of the complexes limits the overall energy capacity to between 2.58 and 12.80 W h L-1. Preliminary flow cell studies in a prototype flow cell are also demonstrated.

  7. Optimization of simultaneous electrochemical determination of Cd(II), Pb(II), Cu(II) and Hg(II) at carbon nanotube-modified graphite electrodes.

    Science.gov (United States)

    Pikna, L'ubomír; Heželová, Mária; Kováčová, Zuzana

    2015-01-01

    The health of the environment is worsening every day. Monitoring of potentially toxic elements and remediation of environmental pollution are necessary. Therefore, the research and development of simple, inexpensive, portable and effective sensors is important. Electrochemistry is a useful component of the field of environment monitoring. The present study focuses on evaluating and comparing three types of electrodes (PIGE, PIGE/MWCNT/HNO3 and PIGE/MWCNT/EDTA/HNO3) employed for the simultaneous electrochemical determination of four potentially toxic elements: Cd(II), Pb(II), Cu(II) and Hg(II). Cyclic voltammograms were measured in an acetate buffer. The LOD, LOQ, the standard and relative precisions of the method and a prediction intervals were calculated (according to the technical procedure DIN 32 645) for the three electrodes and for each measured element. The LOD for PIGE/CNT/HNO3 (the electrode with narrowest calculated prediction intervals) was 2.98 × 10(-7) mol L(-1) for Cd(II), 4.83 × 10(-7) mol L(-1) for Pb(II), 3.81 × 10(-7) mol L(-1) for Cu(II), 6.79 × 10(-7) mol L(-1) for Hg(II). One of the benefits of this study was the determination of the amount of Hg(II) in the mixture of other elements.

  8. Ni(ii) ions cleave and inactivate human alpha-1 antitrypsin hydrolytically, implicating nickel exposure as a contributing factor in pathologies related to antitrypsin deficiency.

    Science.gov (United States)

    Wezynfeld, Nina Ewa; Bonna, Arkadiusz; Bal, Wojciech; Frączyk, Tomasz

    2015-04-01

    Human alpha-1 antitrypsin (AAT) is an abundant serum protein present at a concentration of 1.0-1.5 g L(-1). AAT deficiency is a genetic disease that manifests with emphysema and liver cirrhosis due to the accumulation of a misfolded AAT mutant in hepatocytes. Lung AAT amount is inversely correlated with chronic obstructive pulmonary disease (COPD), a serious and often deadly condition, with increasing frequency in the aging population. Exposure to cigarette smoke and products of fossil fuel combustion aggravates AAT deficiency and COPD according to mechanisms that are not fully understood. Taking into account that these fumes contain particles that can release nickel to human airways and skin, we decided to investigate interactions of AAT with Ni(ii) ions within the paradigm of Ni(ii)-dependent peptide bond hydrolysis. We studied AAT protein derived from human blood using HPLC, SDS-PAGE, and mass spectrometry. These studies were aided by spectroscopic experiments on model peptides. As a result, we identified three hydrolysis sites in AAT. Two of them are present in the N-terminal part of the molecule next to each other (before Thr-13 and Ser-14 residues) and effectively form one N-terminal cleavage site. The single C-terminal cleavage site is located before Ser-285. The N-terminal hydrolysis was more efficient than the C-terminal one, but both abolished the ability of AAT to inhibit trypsin in an additive manner. Nickel ions bound to hydrolysis products demonstrated an ability to generate ROS. These results implicate Ni(ii) exposure as a contributing factor in AAT-related pathologies.

  9. Effect of process parameters on removal and recovery of Cd(II) and Cu(II) from electroplating wastewater by fixed-bed column of nano-dimensional titanium (IV) oxide agglomerates

    CSIR Research Space (South Africa)

    Debnath, S

    2014-01-01

    Full Text Available Removal performances of Cd(II) and Cu(II) from water was investigated using agglomerated nanoparticle of hydrous titanium(IV) oxide (NTO) packed fixed bed. The parameters varied were the bed depth, flow rate and feed solution concentrations...

  10. Synthesis and characterization of ligational behavior of curcumin drug towards some transition metal ions: Chelation effect on their thermal stability and biological activity

    Science.gov (United States)

    Refat, Moamen S.

    2013-03-01

    Complexes of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with curcumin ligand as antitumor activity were synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-Vis, IR, Raman, ESR, 1H-NMR spectroscopy, X-ray diffraction analysis of powdered samples and thermal analysis, and screened for antimicrobial activity. The IR spectral data suggested that the ligand behaves as a monobasic bidentate ligand towards the central metal ion with an oxygen's donor atoms sequence of both sbnd OH and Cdbnd O groups under keto-enol structure. From the microanalytical data, the stoichiometry of the complexes 1:2 (metal:ligand) was found. The ligand and their metal complexes were screened for antibacterial activity against Escherichia Coli, Staphylococcus aureus, Bacillus subtilis and Pseudomonas aeruginosa and fungicidal activity against Aspergillus flavus and Candida albicans.

  11. Coordination chemistry and bioactivity of Ni2+, Cu2+, and Zn2+ complexes containing a bidentate NS ligand, β-N-phenyldithiocarbazic acid, and the crystal structure of β-hydroxy-β-phenylmethylene α-phenylimine

    International Nuclear Information System (INIS)

    Tarafder, M.T.H.; Ahmed Faizal Shamsuddin; Grouse, Karen A.; Yamin, B.M.; Ali, A.M.; Fun, H.-K.

    2003-07-01

    A bidentate ligand (PhDTCH) with NS donor sequence was prepared from the reaction between carbon disulfide and phenylhydrazine in ethanol. Complexes of this ligand with Ni(II), Cu(II) and Zn(II) were synthesized and characterized by elemental analyses, and various physicochemical techniques. The metal complexes were all four coordinated. In an attempt to resolve the crystal structure of PhDTCH, an ethanolic solution, after leaving for a few days gave bright crystals of PhD6, β-hydroxy-β-phenylmethylene α-phenylimine, the crystal structure of which has been resolved. The crystal packing indicated that it is monoclinic with a space group of P21/n. All of the compounds were tested against different bacteria and fungi, and also against leukemic cell lines. All of the compounds showed weak biological properties compared to standard drugs. (author)

  12. "Periodic-table-style" paper device for monitoring heavy metals in water.

    Science.gov (United States)

    Li, Miaosi; Cao, Rong; Nilghaz, Azadeh; Guan, Liyun; Zhang, Xiwang; Shen, Wei

    2015-03-03

    If a paper-based analytical device (μ-PAD) could be made by printing indicators for detection of heavy metals in chemical symbols of the metals in a style of the periodic table of elements, it could be possible for such μ-PAD to report the presence and the safety level of heavy metal ions in water simultaneously and by text message. This device would be able to provide easy solutions to field-based monitoring of heavy metals in industrial wastewater discharges and in irrigating and drinking water. Text-reporting could promptly inform even nonprofessional users of the water quality. This work presents a proof of concept study of this idea. Cu(II), Ni(II), and Cr(VI) were chosen to demonstrate the feasibility, specificity, and reliability of paper-based text-reporting devices for monitoring heavy metals in water.

  13. Coordination Polymers of N, Nʼ-di-(8-Hydroxyquinolinolyl- 5-methyl-N, N-diethyl-1,3-propane diamine (QEPD

    Directory of Open Access Journals (Sweden)

    Asha D. Patel

    2010-01-01

    Full Text Available Coordination polymers containing a novel bis(oxine bidentate ligand, namely N,Nʼ-di(8-hydroxyquinolinolyl-5-methyl-N,Nʼ-diethyl-1,3-propane diamine (QEPD have been prepared with the metal ions Zn(II, Cu(II, Ni(II, Co(II and Mn(II. The novel bis-(bidentate ligand was synthesized by condensation of 5-chloromethyl-8-hydroxyquinoline hydrochloride with N,Nʼ-diethyl-1,2- propane diamine in the presence of a base catalyses. All of these coordination polymers and the parent ligand were characterized by elemental analyses, IR spectral and diffuse reflectance spectral studies. The thermal stability and number- average molecular weights (Mn¯ of all of the coordination polymers were determined by thermogravimetric analyses and non-aqueous conductometric titrations, respectively. In addition, all of the coordination polymers have been characterized by their magnetic susceptibilities.

  14. Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes

    Science.gov (United States)

    Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M. Arif

    2016-05-01

    We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica.

  15. Mandelazo I as a reagent for Zr(IV) determination

    International Nuclear Information System (INIS)

    Rakha, T.H.; Filip, P.; Stefan, N.

    1984-01-01

    A spectrometric study of the reaction of the Zr(IV) ions with Mandelazo I was carried out. Absorption spectra revealed that the maximum absorption of the zirconium compound appears at a wavelength (316 nm) different from the maxima of the reagent (253 and 390 nm). Beer-Lambert law is followed for zirconium concentrations of the order of 8.8 x 10 -5 M (i.e. 8 μg Zr(IV)/mL). Possible interferences of ions such as Be(II), Cu(II), Zn(II), Al(III), Th(IV), U(VI), Mn(II), Fe(III), Co(II) and Ni(II) were investigated in connection with some masking agents such as SO 4 2- and C 2 O 4 2- . Also, the solid state Zr(IV)- Mandelazo I compound was prepared and characterized by nitrogen and thermogravimetric analyses

  16. Characterization and use of in natura and calcined rice husks for biosorption of heavy metals ions from aqueous effluents

    Directory of Open Access Journals (Sweden)

    M. G. A. Vieira

    2012-09-01

    Full Text Available Heavy metal removal by adsorption using rice husks as a bioadsorbent was evaluated as an alternative for wastewater treatment. Batch equilibrium experiments and kinetic sorption studies were performed using monocomponent solutions of Ni(II, Cd(II, Zn(II, Pb(II and Cu(II in surface samples of in natura(RH and calcined rice husks (RHA. RHA showed higher potential for removing lead and copper. Experimental data for adsorption isotherms of lead and copper were adjusted by Langmuir, Freundlich and Dubinin-Radushkevick (D-R models, being better represented by the Langmuir model. The calcination of RH increased its surface area, improving its adsorption properties. From a morphological analysis obtained by SEM and diffraction patterns (XRD, a longitudinal fibrous and amorphous structure was observed for RH. TGA resultsindicated a total mass loss of around 60% for RH and 24.5% for RHA.

  17. Recovery of Cu(II from diluted aqueous solutions by non-dispersive solvent extraction

    Directory of Open Access Journals (Sweden)

    Alguacil, E. J.

    2002-08-01

    Full Text Available The removal of copper from diluted aqueous solutions with ACORGA M5640 extractant using non-dispersive solvent extraction technology was studied. It was possible to remove Cu(II below the international standars from solutions having initially as low concentration as 0,01 g/l under various experimental conditions, i.e aqueous pH 4.0, 10 % v/v ACORGA M5640 in Exxol D100, an organic flow of 100 ml/min, and an aqueous flow 50ml/min. Since the removal occurs by chelating ion exchange between copper from solution and protons from the extractant, the former was stripped by using a 180 g/l sulphuric acid solution which flowed (50 ml/min through the tube side organic was passed (400 ml/min through the shell side of the fibers of the module

    Se estudia la eliminación del cobre presente en disoluciones acuosas diluidas empleando el agente de extracción ACORGA M5640 y la tecnología de extracción con disolventes no dispersiva. Bajo las condiciones experimentales estudiadas, pH de la fase acuosa 4,0 ±0,1, 10 % v/v ACORGA M5640 en Exxsol D100, flujo de la fase orgánica 100 ml/min, flujo de la fase acuosa 50 ml/min, es posible eliminar el Cu(II, por debajo de los límites marcados internacionalmente, en disoluciones con un contenido tan bajo como 0,01 g/1 del metal. Debido a que la extracción transcurre mediante un intercambio catiónico (y formación de un compuesto tipo quelato entre el cobre presente en el medio acuoso y los protones del agente de extracción, el metal se puede reextraer mediante la utilización de una disolución de 180 g/1 de ácido sulfúrico que fluye (50 ml/min a través de la parte interior de las fibras del módulo, mientras que la fase orgánica fluye (400 ml/min por la parte exterior de las mismas fibras.

  18. Synthesis, structure and magnetic properties of cobalt(II) and copper(II) coordination polymers assembled by phthalate and 4-methylimidazole

    International Nuclear Information System (INIS)

    Baca, S.G.; Malinovskii, S.T.; Franz, Patrick; Ambrus, Christina; Stoeckli-Evans, Helen; Gerbeleu, Nicolae; Decurtins, Silvio

    2004-01-01

    New coordination polymers [M(Pht)(4-MeIm) 2 (H 2 O)] n (M=Co (1), Cu (2); Pht 2- =dianion of o-phthalic acid; 4-MeIm=4-methylimidazole) have been synthesized and characterized by IR spectroscopy, X-ray crystallography, thermogravimetric analysis and magnetic measurements. The crystal structures of 1 and 2 are isostructural and consist of [M(4-MeIm) 2 (H 2 O)] building units linked in infinite 1D helical chains by 1,6-bridging phthalate ions which also act as chelating ligands through two O atoms from one carboxylate group in the case of 1. In complex 1, each Co(II) atom adopts a distorted octahedral N 2 O 4 geometry being coordinated by two N atoms from two 4-MeIm, three O atoms of two phthalate residues and one O atom of a water molecule, whereas the square-pyramidal N 2 O 3 coordination of the Cu(II) atom in 2 includes two N atoms of N-containing ligands, two O atoms of two carboxylate groups from different Pht, and a water molecule. An additional strong O-H↑··O hydrogen bond between a carboxylate group of the phthalate ligand and a coordinated water molecule join the 1D helical chains to form a 2D network in both compounds. The thermal dependences of the magnetic susceptibilities of the polymeric helical Co(II) chain compound 1 were simulated within the temperature range 20-300 K as a single ion case, whereas for the Cu(II) compound 2, the simulations between 25 and 300 K, were made for a linear chain using the Bonner-Fisher approximation. Modelling the experimental data of compound 1 with MAGPACK resulted in: g=2.6, vertical bar D vertical bar=62 cm -1 . Calculations using the Bonner-Fisher approximation gave the following result for compound 2: g=2.18, J=-0.4 cm -1

  19. Selective enrichment and determination of monoamine neurotransmitters by CU(II) immobilized magnetic solid phase extraction coupled with high-performance liquid chromatography-fluorescence detection.

    Science.gov (United States)

    He, Maofang; Wang, Chaozhan; Wei, Yinmao

    2016-01-15

    In this paper, iminodiacetic acid-Cu(II) functionalized Fe3O4@SiO2 magnetic nanoparticles were prepared and used as new adsorbents for magnetic solid phase extraction (MSPE) of six monoamine neurotransmitters (MNTs) from rabbit plasma. The selective enrichment of MNTs at pH 5.0 was motivated by the specific coordination interaction between amino groups of MNTs and the immobilized Cu(II). The employed weak acidic extraction condition avoided the oxidation of MNTs, and thus facilitated operation and ensured higher recoveries. Under optimal conditions, the recoveries of six MNTs from rabbit plasma were in the range of 83.9-109.4%, with RSD of 2.0-10.0%. When coupled the Cu(II) immobilized MSPE with high-performance liquid chromatography-fluorescence detection, the method exhibited relatively lower detection limits than the previously reported methods, and the method was successfully used to determine the endogenous MNTs in rabbit plasma. The proposed method has potential application for the determination of MNTs in biological samples. Also, the utilization of coordination interaction to improve the selectivity might open another way to selectively enrich small alkaloids from complex samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Sulfonated Magnetic Nanocomposite Based on Reactive PGMA-MAn Copolymer@Fe3O4 Nanoparticles: Effective Removal of Cu(II Ions from Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Reza Hasanzadeh

    2016-01-01

    Full Text Available Chelating magnetic nanocomposites have been considered as suitable materials for removal of heavy metal ions for water treatment. In this work poly(glycidyl methacrylate-maleic anhydride copolymer (PGMA-MAn is modified with 4-aminobenzenesulfonic acid (ABSAc and subsequently the product reacted with modified Fe3O4 nanoparticles and 1,2-ethanedithiol (EDT in the presence of ultrasonic irradiation for preparation of tridimensional chelating magnetic nanocomposite. Synthesized magnetic nanocomposite was characterized by Fourier transform infrared spectroscopy (FT-IR, scanning electron microscopy (SEM, X-ray diffraction analysis (XRD, vibrating sample magnetometer (VSM, energy dispersive X-ray analysis (EDX, elemental mapping analysis (EMA, Brunauer-Emmett-Teller (BET, and thermal gravimetric analysis (TGA. The adsorption behavior of Cu(II ions was investigated by synthesized nanocomposite in various parameters such as pH, contact time, metal ion concentration, and adsorbent dosage. The equilibrium distribution coefficient (kd was determined and the findings prove that the kd value is approximately high in the case of all selected metal ions. The synthesized nanocomposite exhibited good tendency for removing Cu(II ions from aqueous solutions even at an acidic pH.

  1. Synthesis and complexation of acyclic dithiolate ligands

    International Nuclear Information System (INIS)

    Ashford, L.

    1999-11-01

    Four approaches to ring substituted and unsubstituted N,N'-bis(o-mercaptobenzyliden)propylenediaminate ligands are described using N,N-dimethylcarbamate as a thiolate protecting group. Of the four basic methods, substitution, reduction, rearrangement and oxidation, the latter two successfully synthesise the aldehyde precursor. Rearrangement of the thiocarbamoyl group to the protected thiophenol is shown to be facilitated by a para-nitro substiuent. Ni(II) and Cu(II) complexes of N,N'-bis(p-nitro-o-mercaptobenzyliden)-propylenediaminate are synthesised by reaction of 2-formyl-4-nitro-N,N-dimethylcarbamoyI thiophenol, [Ni(OAc) 2 ].4(H 2 O) and 1,3-diaminopropane. The para-unsubstituted Ni(II) complex, Nickel-[N,N'-bis(o-mercaptobenzyliden) propylenediaminate] is prepared via reaction of the aldehyde, 2-formyl-N,N-dimethylcarbamoyl thiophenol with [Ni(OAc) 2 ].4(H 2 O) and 1,3-diaminopropane. The analogous carbamoyl-protected amine ligands, N,N'-dimethyl-N.N'-di[2-(N'',N''-dimethylcarbamyl)mercapto] benzyl-1,3-propane-diamine and N,N'-dimethyl-N,N'-di[2-(N'',N''-dimethylcarbamyl)mercapto] benzyl-1,2-ethane-diamine are also studied. The tertiary-butyl-protected diimine ligand, N,N'-bis-(o-mercaptobenzylidene)-propylenediaminate is prepared from 2-(tert-butylsulfanyl)benzaldehyde and 1,3-diaminopropane. Reaction with [Ni(H 2 O) 6 ]Cl 2 gives Nickel-[N,N'-bis(o-mercaptobenzyliden)-propylenediaminate], the crystal structure showing a distorted square-planar Ni(II) centre. Reaction with ZnCl 2 gives Zinc-[N,N'-bis(o-mercaptobenzyliden)propylenediaminate]dichloride. The crystal structure shows the thiolate donors remain protected and uncoordinated. The Zn(II) ion is coordinated by two imine donors and two chloride ions in a tetrahedral environment. In reactions with Ag(I) and Hg(II), N,N'-bis-(o-mercaptobenzylidene)-propylenediaminate acts as a reductant giving the free metals. Structural data and NMR and IR spectroscopic data for Nickel

  2. Synthesis, spectral and theoretical studies of Ni(II), Pd(II) and Pt(II) complexes of 5-mercapto-1,2,4-triazole-3-imine-2‧-hydroxynaphyhaline

    Science.gov (United States)

    Gaber, Mohamed; El-Ghamry, Hoda; Atlam, Faten; Fathalla, Shaimaa

    2015-02-01

    Ni(II), Pd(II) and Pt(II) complexes of 5-mercapto-1,2,4-triazole-3-imine-2‧-hydroxynaphthaline have been isolated and characterized by elemental analysis, IR, 1H NMR, EI-mass, UV-vis, molar conductance, magnetic moment measurements and thermogravimetric analysis. The molar conductance values indicated that the complexes are non-electrolytes. The magnetic moment values of the complexes displayed diamagnetic behavior for Pd(II) and Pt(II) complexes and tetrahedral geometrical structure for Ni(II) complex. From the bioinorganic applications point of view, the interaction of the ligand and its metal complexes with CT-DNA was investigated using absorption and viscosity titration techniques. The Schiff-base ligand and its metal complexes have also been screened for their antimicrobial and antitumor activities. Also, theoretical investigation of molecular and electronic structures of the studied ligand and its metal complexes has been carried out. Molecular orbital calculations were performed using DFT (density functional theory) at B3LYP level with standard 6-31G(d,p) and LANL2DZ basis sets to access reliable results to the experimental values. The calculations were performed to obtain the optimized molecular geometry, charge density distribution, extent of distortion from regular geometry, the highest occupied molecular orbital (HOMO), the lowest unoccupied molecular orbital (LUMO), Mulliken atomic charges, reactivity index (ΔE), dipole moment (D), global hardness (η), softness (σ), electrophilicity index (ω), chemical potential and Mulliken electronegativity (χ).

  3. Syntheses, structural elucidation, thermal properties, theoretical quantum chemical studies (DFT and biological studies of barbituric–hydrazone complexes

    Directory of Open Access Journals (Sweden)

    Amina A. Soayed

    2015-03-01

    Full Text Available Condensation of barbituric acid with hydrazine hydrate yielded barbiturichydrazone (L which was characterized using IR, 1H NMR and mass spectra. The Co(II, Ni(II and Cu(II complexes derived from this ligand have been synthesized and structurally characterized by elemental analyses, spectroscopic methods (IR, UV–Vis and ESR and thermal analyses (TGA, DTG and DTA and the structures were further elucidated using quantum chemical density functional theory. Complexes of L were found to have the ML.nH2O stoichiometry with either tetrahedral or octahedral geometry. The ESR data showed the Cu(II complex to be in a tetragonal geometry. Theoretical investigation of the electronic structure of metal complexes at the TD-DFT/B3LYP level of theory has been carried out and discussed. The fundamental vibrational wavenumbers were calculated and a good agreement between observed and scaled calculated wavenumbers was achieved. Thermal studies were performed to deduce the stabilities of the ligand and complexes. Thermodynamic parameters, such as the order of reactions (n, activation energy ΔE∗, enthalpy of reaction ΔH∗ and entropy ΔS∗ were calculated from DTA curves using Horowitz–Metzger method. The ligand L and its complexes have been screened for their antifungal and antibacterial activities and were found to possess better biological activities compared to those of unsubstituted barbituric acid complexes.

  4. Synthesis and characterization of monomeric and polymeric Cu(II) complexes of 3,4-ethylenedioxythiophene-functionalized with cyclam ligand

    International Nuclear Information System (INIS)

    Velauthamurty, Kuhamoorthy; Higgins, Simon J.; Rajapakse, R.M. Gamini; Bandara, H.M.N.; Shimomura, Masaru

    2010-01-01

    A functionalized EDOT derivative with 1,4,8,11-tetraazacyclotetradecane (cyclam) ligand pendant to the ethylene bridge (4) and its complexes [M(4)(BF 4 ) 2 ], where M(II) = Cu(II), was prepared and characterized. Their electrochemical copolymerization with EDOT was studied. The electro-co-polymerized films were characterized by electrochemical methods, X-ray photoelectron spectroscopy and by X-ray fluorescence spectroscopy. The co-polymerization method was found to afford a good control of the metal concentration in the polymer matrix and represents a good technique for preparing electronically conductive polymers containing redox-active metal complexes.

  5. Utilization of ICP/OES for the determination of trace metal binding to different humic fractions.

    Science.gov (United States)

    de la Rosa, G; Peralta-Videa, J R; Gardea-Torresdey, J L

    2003-02-28

    In this study, the use of inductively coupled plasma/optical emission spectrometry (ICP/OES) to determine multi-metal binding to three biomasses, Sphagnum peat moss, humin and humic acids is reported. All the investigations were performed under part per billion (ppb) concentrations. Batch pH profile experiments were performed using multi-metal solutions of Cd(II), Cu(II), Pb(II), Ni(II), Cr(III) and Cr(VI). The results showed that at pH 2 and 3, the metal affinity of the three biomasses exposed to the multi-metal solution that included Cr(III) presented the following order: Cu(II), Pb(II)>Ni(II)>Cr(III)>Cd(II). On the other hand, when Cr(VI) was in the heavy metal mixture, Sphagnum peat moss and humin showed the following affinity: Cu(II), Pb(II)>Ni(II)>Cr(VI)>Cd(II); however, the affinity of the humic acids was: Cu(II)>Pb(II), Cr(VI)>Ni(II)>Cd(II). The results demonstrated that pH values of 4 and 5 were the most favorable for the heavy metal binding process. At pH 5, all the metals, except for Cr(VI), were bound between 90 and 100% to the three biomasses. However, the binding capacity of humic acids decreased at pH 6 in the presence of Cr(VI). The results showed that the ICP/OES permits the determination of heavy metal binding to organic matter at ppb concentration. These results will be very useful in understanding the role of humic substances in the fate and transport of heavy metals, and thus could provide information to develop new methodologies for the removal of low concentrations of toxic heavy metals from contaminated waters.

  6. Batch removal and optimization of Cu(II) ions from aqueous solution by biosorption on to native and pretreated mangifera indica seeds

    International Nuclear Information System (INIS)

    Noreen, A.; Ali, G.; Jabeen, M.

    2011-01-01

    Biosorption is a process that utilizes biomass to sequester toxic heavy metals and is particularly useful for the removal of contaminants from industrial effluents. Present study involved batch experiments for the sorption of Cu(II) onto Mangifera indica seeds kernel particles in order to optimize the biosorbent dose, agitation rate, pH, contact time and initial metal ion concentration. The effect of citric acid pretreatment was also studied. Maximum uptake was observed at pH 5, biosorbent dose 0.5 g and agitation rate 150 rpm. A direct correlation was found to exist between adsorbed Cu(II) ion concentration and initial metal concentration upto a certain level then it reached a saturation value at about 250 mg/L. Biosorption equilibrium was established by 60 min. The maximum metal uptake capacity was 13.2 mg/g at optimized conditions. The uptake capacity of the biomass was increased by chemical pretreatment with citric acid (15.2 mg/g) when compared with the raw biomass (13.2 mg/g). Equilibrium data was fitted to Freundlich and Langmuir isotherm equations and the data was found to well represented by Langmuir isotherm equation with r/sup 2/ = 0.9981 and q/sub max/ = 17.939 mg/g for raw biomass and with r/sup 2/ = 0.9984 and qmax 18.57 mg/g for modified biomass. (author)

  7. Synthesis of a new ONNO donor tetradentate schiff base ligand and binuclear Cu(II) complex: Quantum chemical, spectroscopic and photoluminescence investigations

    International Nuclear Information System (INIS)

    Sarıoğlu, Ahmet Oral; Ceylan, Ümit; Yalçın, Şerife Pınar; Sönmez, Mehmet; Ceyhan, Gökhan; Aygün, Muhittin

    2016-01-01

    The Schiff base compound 3,3′-(1,4-phenylimino)-bis-[1,3-bis-(4-methoxyphenyl) propan-1-one)], formulated as C 40 H 36 N 2 O 6, and its Cu(II) complex were synthesized and characterized by analytical analysis, various spectral techniques such as FT-IR, NMR, UV–vis, magnetic measurements and molar conductivity. Thermo gravimetric analysis (TGA and DTA) carried out to obtain information about its thermal stability. The molecular structure and spectroscopic properties of the ligand were obtained with FT-IR, 1 H and 13 C NMR, UV–vis investigations as experimentally and compared with theoretical results obtained from DFT/B3LYP/6-311++G(d,p) basis set. In addition to molecular calculations of the title compound, molecular electrostatic potential (MEP), dipole moments, atomic charges, HOMO–LUMO, NLO and NBO analysis were computed. The calculated results show that the optimized geometry can well reproduce the crystal structure parameters, and the theoretical vibrational frequencies, 1 H and 13 C NMR chemical shifts show good agreement with experimental values. Photoluminescence properties of the ligand and its Cu(II) complex were examined. - Highlights: • FT-IR and 1 H– 13 C NMR spectra were recorded and compared with the theoretical results. • The photoluminescence properties were studied. • NLO, NBO analysis of the molecule were studied. • HOMO and LUMO energies, MEP distribution of the molecule were calculated.

  8. 3,4-Dimethyl diphenyldithiophosphate of mononuclear cobalt(II) with N-donor ligands: Synthesis, structural characterization, DFT and antibacterial studies

    Science.gov (United States)

    Kumar, Sandeep; Kour, Gurpreet; Schreckenbach, Georg; Andotra, Savit; Hundal, Geeta; Sharma, Vishal; Jaglan, Sundeep; Pandey, Sushil K.

    2017-08-01

    3,4-Dimethyl diphenyldithiophosphate of cobalt(II) with N-donor ligands [{(ArO)2PS2}2CoL2] [Ar = 3,4-(CH3)2C6H3 (1-3); L = C5H5N (1), 3,4-(CH3)2C5H3N (2) and 4-(C2H5)C5H4N (3)] have been synthesized and characterized by elemental analyses, infrared spectroscopy (IR), powder X-ray diffraction (PXRD) and single crystal X-ray analysis. Complex 1 crystallizes in the monoclinic space group P21/n whereas complexes 2 and 3 crystallize in the triclinic space group Pbar1. The crystal structures of complexes 1-3 reveal mononuclear units with the Co(II) center chelated in bidentate fashion by four S atoms of the two diphenyldithiophosphate ligands. The N atoms from two donor ligands are axially coordinated, leading to distorted octahedral geometry around Co(II). The complexes have been optimized using density functional theory (DFT), structural parameters have been calculated, and the energy gaps of the frontier orbitals (HOMO-LUMO) have been predicted. Mayer bond orders have also been calculated. Structural parameters from the crystallographic and DFT studies are in good agreement with each other. To explore the biological potential, complexes were evaluated for their antibacterial activity against three bacterial strains. The bacterial growth inhibition capacity of the ligand and complexes followed the order of 3 > 2 > 1 > L1.

  9. Biosorption of Cu(II) from aqueous solutions by mimosa tannin gel

    Energy Technology Data Exchange (ETDEWEB)

    Sengil, I. Ayhan [Department of Environmental Engineering, Engineering Faculty, Sakarya University, 54100 Sakarya (Turkey)], E-mail: asengil@sakarya.edu.tr; Ozacar, Mahmut [Department of Chemistry, Science and Arts Faculty, Sakarya University, 54100 Sakarya (Turkey)

    2008-09-15

    The biosorption of Cu(II) from aqueous solutions by mimosa tannin resin (MTR) was investigated as a function of particle size, initial pH, contact time and initial metal ion concentration. The aim of this study was to understand the mechanisms that govern copper removal and find a suitable equilibrium isotherm and kinetic model for the copper removal in a batch reactor. The experimental isotherm data were analysed using the Langmuir, Freundlich and Temkin equations. The equilibrium data fit well in the Langmiur isotherm. The experimental data were analysed using four sorption kinetic models - the pseudo-first- and second-order equations, and the Elovich and the intraparticle diffusion equation - to determine the best fit equation for the biosorption of copper ions onto mimosa tannin resin. Results show that the pseudo-second-order equation provides the best correlation for the biosorption process, whereas the Elovich equation also fits the experimental data well. Thermodynamic parameters such as the entropy change, enthalpy change and Gibb's free energy change were found out to be 153.0 J mol{sup -1} K{sup -1}, 42.09 kJ mol{sup -1} and -2.47 kJ mol{sup -1}, respectively.

  10. The adsorption of Tl(I), Au(III), Cu(II) and the separation of 199Tl from alpha bombardment of gold target with PDB-18C6

    International Nuclear Information System (INIS)

    Zhou Dehai; Zhou Jimeng

    1989-01-01

    The adsorptive behavior of polymer of methyl aldehyde of dibenzo-18-crown-6 (PDB-18C6) in hydrochloric acid medium is studied and it is shown that the adsorption of T1(I), Au(III), and Cu(II) depends on the particle size of the crown ether resins, hydrochloric acid concentration and amount of the crown ether resins used. The difference in the adsorption behavior of different particle sizes of crown ether resins may be used for separating Tl(I), Au(III), and Cu(II) ions. The best eluant of Tl(I) and Au(III) is 0.4 mol/l perchloric acid and 2-ethoxy-ethanol. The recovery for Tl(I) is 82-98.8%. The gold target is bombarded in a 1.2 m cyclotron with 25-27 MeV α-particle with a cumulative beam intensities of 27μA·h, and 199 Tl is separated from the gold target with PDB-18C6. γ-spectrometry has shown that the Tl obtained is 199 Tl of high purity containing only about 0.50% 200 Tl

  11. Schiff bases derived from L-Tyrosine L-Tryptophan and their Cu(II) chelates as effective means for preventive-treatment of radiation injuries

    International Nuclear Information System (INIS)

    Malakyan, M.H.; Bajinyan, S.A.; Matosyan, V.H.; Tonoyan, V.J.; Babayan, K.N.; Boyajyan, A.S.; Yeghiazaryan, D.E.; Vardevanyan, L.A.; Sorenson, J.R.J.

    2008-01-01

    Full text: Study on essential metallo element chelates as radioprotectors presents a promising direction in a search for and development of novel anti-radiation agents and offers a new approach to overcome the pathological effects of ionizing radiation. The key idea elucidating the radioprotective effects of metallo element-containing chelates of amino acid derivatives is their role in stimulation of de novo synthesis of metallo element-dependent enzymes required for recovery of hemopoietic activity and immuno competency lost as a consequence of radiation damage. Aimed to develop novel anti-radiation remedies of less toxicity and high efficacy, Schiff bases derived from L-Tyrosine and L-Tryptophan and their Cu(II) chelates were synthesized. In experiments in vitro and in vivo biological and pharmacological properties of the mentioned Schiff Bases and their copper complexes are under study. According to the results obtained, L-Tyrosinate and L-Tryptophanate Schiff bases are low toxic compounds with a weak antioxidant activity and exert radioprotective effects in case of animal X-ray irradiation at a dose level equal or less than LD 50/30 . Unlike Schiff Bases, their appropriate Cu(II) chelates possess high anti radical/antioxidant activity and manifest expressed radio-protective action at LD 100/30 dose of ionizing radiation. Anti-radiation effects of amino acid Schiff bases and their metallo chelates are manifested in case of both subcutaneous and oral single administration to the animal organism at 10, 20, or 40 mg/kg 1, 3, 6, or 24 hours prior to radiation exposure. Conclusions are drawn basing on determinations of survival and average life-span indices of irradiated animals, as well as on studies for their hematological, biochemical, immunological, biophysical indices. It is revealed that on the background of preliminary administration of the compounds studied to the animal organism the characteristics of DNA are significantly improved, the immune status

  12. Characterization and application of expanded graphite modified with phosphoric acid and glucose for the removal of Ni(II) from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Li [Shandong Key Laboratory of Water Pollution Control and Resource Reuse, School of Environmental Science and Engineering, Shandong University, Jinan 250100 (China); Zhang, Jian, E-mail: zhangjian00@sdu.edu.cn [Shandong Key Laboratory of Water Pollution Control and Resource Reuse, School of Environmental Science and Engineering, Shandong University, Jinan 250100 (China); Xu, Xiaoli [Shandong Key Laboratory of Water Pollution Control and Resource Reuse, School of Environmental Science and Engineering, Shandong University, Jinan 250100 (China); Zhang, Jie [Shandong Experimental High School, Jinan 250100 (China); Liu, Hai; Guo, Zizhang; Kang, Yan; Li, Yiran [Shandong Key Laboratory of Water Pollution Control and Resource Reuse, School of Environmental Science and Engineering, Shandong University, Jinan 250100 (China); Xu, Jingtao [School of Municipal and Environmental Engineering, Shandong Jianzhu University, Jinan 250100 (China)

    2015-12-01

    Highlights: • Glucose and H{sub 3}PO{sub 4}, single or together, were used to modify expanded graphite. • The modified condition was at a low temperature (150 °C). • The properties of EG and the highest adsorption ability modified EG were compared. • G-P-EG has the highest adsorption ability, which is much higher than that of EG. - Abstract: Three kinds of modified expanded graphite (EG), impregnated with phosphoric acid (H{sub 3}PO{sub 4}) (P-EG), impregnated with glucose (G-EG), and impregnated with H{sub 3}PO{sub 4} and glucose (G-P-EG), were prepared under a low temperature (150 °C). The adsorption capacity of G-P-EG (Q{sub m} = 7.016 mg/g) is much higher than original expanded graphite (EG Q{sub m} = 0.423 mg/g) and other two kinds of modified expanded graphite (P-EG Q{sub m} = 0.770 mg/g; G-EG Q{sub m} = 0.507 mg/g). The physicochemical properties of EG and G-P-EG were characterized by N{sub 2} adsorption/desorption, Boehm's titration and X-ray photoelectron spectroscopy (XPS). EG exhibited higher values of BET surface area (11.357 m{sup 2}/g) and total pore volume (0.0303 cm{sup 3}/g) than that of G-P-EG (4.808 m{sup 3}/g and 0.0109 cm{sup 3}/g). However, the results of Bohm's titration and XPS showed that G-P-EG contained more surface oxygen-containing functional groups. The Ni(II) adsorption equilibrium data agreed well with the Langmuir model. And the experimental data of EG and G-P-EG fitted better by pseudo-second order model. Based on the results of batch adsorption experiments and XPS analysis, there were several possible mechanisms for Ni(II) adsorption on the G-P-EG, including chemical adsorption, cation exchange, electrostatic attraction and surface complication.

  13. Complexation of nitrogen and sulphur donor Schiff's base ligand to Cr(III) and Ni(II) metal ions: Synthesis, spectroscopic and antipathogenic studies

    Science.gov (United States)

    Sharma, Amit Kumar; Chandra, Sulekh

    2011-01-01

    2,6-Diacetyl pyridine based ligand was synthesized by the reaction of 2,6-diacetyl pyridine with thiocarbohydrazide in presence of acetic acid. The coordination compounds with Cr(III) and Ni(II) metal ions having [Cr(L)X]X 2 and [Ni(L)X]X compositions (where L = ligand and X = NO 3-, Cl - and CH 3COO -) were synthesized and characterized by physicochemical and spectral studies. The studies like elemental analyses, molar conductance measurements, magnetic susceptibility measurements, IR, UV-Vis, NMR, mass and EPR reveal that the complexes are octahedral. The compounds were examined against the pathogenic fungal and bacterial strains like Alternaria brassicae, Aspergillus niger, Fusarium oxysporum, Xanthomonas compestris and Pseudomonas aeruginosa. A. niger causes the diseases Apergillosis and Otomycosis in humans.

  14. Spectrophotometric Determination of Iron(II and Cobalt(II by Direct, Derivative, and Simultaneous Methods Using 2-Hydroxy-1-Naphthaldehyde-p-Hydroxybenzoichydrazone

    Directory of Open Access Journals (Sweden)

    V. S. Anusuya Devi

    2012-01-01

    Full Text Available Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH reacts with iron(II and cobalt(II to form reddish-brown and yellow-coloured [Fe(II-HNAHBH] and [Co(II-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II-HNAHBH], Beer’s law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II-HNAHBH] complex obeys Beer’s law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content.

  15. Cobalt(II), nickel(II), copper(II), zinc(II) and hafnium(IV) complexes of N'-(furan-3-ylmethylene)-2-(4-methoxyphenylamino)acetohydrazide.

    Science.gov (United States)

    Emam, Sanaa M; El-Saied, Fathy A; Abou El-Enein, Saeyda A; El-Shater, Heba A

    2009-03-01

    Cobalt(II), nickel(II), copper(II), zinc(II) and hafnium(IV) complexes of furan-2-carbaldehyde 4-methoxy-N-anilinoacetohydrazone were synthesized and characterized by elemental and thermal (TG and DTA) analyses, IR, UV-vis and (1)H NMR spectra as well as magnetic moment and molar conductivity. Mononuclear complexes are obtained with 1:1 molar ratio except complexes 3 and 9 which are obtained with 1:2 molar ratios. The IR spectra of ligand and metal complexes reveal various modes of chelation. The ligand behaves as a neutral bidentate one and coordination occurs via the carbonyl oxygen atom and azomethine nitrogen atom. The ligand behaves also as a monobasic tridentate one and coordination occurs through the enolic oxygen atom, azomethine nitrogen atom and the oxygen atom of furan ring. Moreover, the ligand behaves as a neutral tridentate and coordination occurs via the carbonyl oxygen, azomethine nitrogen and furan oxygen atoms as well as a monobasic bidentate and coordination occurs via the enolic oxygen atom and azomethine nitrogen atom. The electronic spectra and magnetic moment measurements reveal that all complexes possess octahedral geometry except the copper complex 10 possesses a square planar geometry. The thermal studies showed the type of water molecules involved in metal complexes as well as the thermal decomposition of some metal complexes.

  16. Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes.

    Science.gov (United States)

    Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M Arif

    2016-05-15

    We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Effect on the Inhibitory Activity of Potential Microbes on the Complexation of Methyl Anthranilate Derived Hydrazide with Cu, Ni and Zn (II) Metal Ions

    International Nuclear Information System (INIS)

    Ikram, M.; Rehman, S.; Khan, K.

    2013-01-01

    The hydrazide ligand 2-amino-(N-aminobezoyl)benzohydrazide (ABH) have been synthesized and characterized by 1H-NMR, 13C-NMR, ES+-MS, elemental analyses and infrared studies. The ligand was complexed with Ni(II), Cu(II) and Zn(II) metal ions and were characterized by analytical and spectroscopic methods including elemental analyses, ES+-MS, conductance, infrared, UV-Visible and magnetic susceptibilities studies. Infrared spectra show that the ligand form complexes through -NH2 and carbonyl moieties, the elemental studies suggested the M(ABH)X2 composition of the coordination compounds. The synthesized complexes were studied for their biological activities against gram negative bacteria including Escherichia coli, Salmonella typhi, Enterobacter aerogenes, Proteus vulgaris, Pseudomonas aeruginosa, Gram positive bacterial strains like Staphylococcus aureus and fungus like Candida albican. These activities show that the metal complexes are more active to the tested microbes as compared to neat ligand. (author)

  18. Determination of trace impurities in high-purity iron using salting-out of polyoxyethylene-type surfactants

    Energy Technology Data Exchange (ETDEWEB)

    Matsumiya, Hiroaki, E-mail: h-matsu@numse.nagoya-u.ac.jp [Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan); Sakane, Yuto; Hiraide, Masataka [Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan)

    2009-10-19

    To an iron sample solution was added polyoxyethylene-4-isononylphenoxy ether (PONPE, nonionic surfactant, average number of ethylene oxides 7.5) and the surfactant was aggregated by the addition of lithium chloride. The iron(III) matrix was collected into the condensed surfactant phase in >99.9% yields, leaving trace metals [e.g., Ti(IV), Cr(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Pb(II), and Bi(III)] in the aqueous phase. After removing the surfactant phase by centrifugation, the remaining trace metals were concentrated onto an iminodiacetic acid-type chelating resin. The trace metals were desorbed with dilute nitric acid for the determination by inductively coupled plasma-mass spectrometry or graphite-furnace atomic absorption spectrometry. The proposed separation method allowed the analysis of high-purity iron metals for trace impurities at low {mu}g g{sup -1} to ng g{sup -1} levels.

  19. Potentiometric studies on the complexes of tetracycline (TC) and oxytetracycline (OTC) with some metal ions

    International Nuclear Information System (INIS)

    Ghandour, M.A.; Azab, H.A.; Hassan, A.; Ali, A.M.

    1992-01-01

    The interaction of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Zn(II), Cd(II), Hg(II), Pb(II), Al(III), and UO 2 (II) ions with tetracycline (TC) were studied by potentiometric pH titrations. The formation constants of the different binary complexes formed in such systems have been determined at 25±0.1 deg C and μ=0.1 moll -1 (NaNO 3 ). Potentiometric pH equilibrium measurements have been made under the same conditions for the interaction of oxytetracycline (OTC) and Cu(II), Cd(II), Pb(II), and UO 2 (II). The formation of (1:1) binary complexes are inferred from the potentiometric pH titration curves. The protonation constants of TC and OTC were also determined under the same conditions and refined (ESAB2M computer program). The transition metal stability constants are consistent with the Irving-Williams series. (authors)

  20. Potentiometric studies on the complexes of tetracycline (TC) and oxytetracycline (OTC) with some metal ions. Potentiometrische Untersuchungen der Komplexe von Tetracyclin (TC) und Oxytetracyclin (OTC) mit einigen Metall-Ionen

    Energy Technology Data Exchange (ETDEWEB)

    Ghandour, M A; Azab, H A; Hassan, A; Ali, A M [Assiut Univ. (Egypt)

    1992-01-01

    The interaction of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Zn(II), Cd(II), Hg(II), Pb(II), Al(III), and UO[sub 2](II) ions with tetracycline (TC) were studied by potentiometric pH titrations. The formation constants of the different binary complexes formed in such systems have been determined at 25[+-]0.1 deg C and [mu]=0.1 moll[sup -1] (NaNO[sub 3]). Potentiometric pH equilibrium measurements have been made under the same conditions for the interaction of oxytetracycline (OTC) and Cu(II), Cd(II), Pb(II), and UO[sub 2](II). The formation of (1:1) binary complexes are inferred from the potentiometric pH titration curves. The protonation constants of TC and OTC were also determined under the same conditions and refined (ESAB2M computer program). The transition metal stability constants are consistent with the Irving-Williams series. (authors).

  1. Extraction of metal cations by polyterephthalamide microcapsules containing a poly(acrylic acid) gel.

    Science.gov (United States)

    Laguecir, A; Ernst, B; Frère, Y; Danicher, L; Burgard, M

    2002-01-01

    Polyterephthalamide microcapsules containing a poly(acrylic acid) gel as a macromolecular ligand (PAA-CAPS) were prepared using an original two step polymerization process in a water-in-oil inverse emulsion system. A polyamide microcapsule containing acrylic acid, initiator and cross-linking agent, is formed by interfacial polycondensation of terephthaloyl dichloride with hexamethylenediamine. In situ radical polymerization of the microcapsule core acrylic acid is initiated to obtain encapsulated poly(acrylic acid) gel. Reference polyamide microcapsules, i.e. without ligand (CAPS), were also synthesized. The mean diameter of synthesized microcapsules was 210 microm, and the microcapsule wall thickness was evaluated by SEM and TEM observations of microcapsule cross-section cuts. The microcapsule water content was determined by thermogravimetric experiments. The extractabilities of Cu(II), Ni(II), Co(II) and Zn(II) into PAA-CAPS were examined. The stripping of the various cations can be promoted in diluted hydrochloric acid solutions.

  2. Heavy metal adsorption by modified oak sawdust: Thermodynamics and kinetics

    International Nuclear Information System (INIS)

    Argun, Mehmet Emin; Dursun, Sukru; Ozdemir, Celalettin; Karatas, Mustafa

    2007-01-01

    This paper describes the adsorption of heavy metal ions from aqueous solutions by oak (Quercus coccifera) sawdust modified by means of HCl treatment. Our study tested the removal of three heavy metals: Cu, Ni, and Cr. The optimum shaking speed, adsorbent mass, contact time, and pH were determined, and adsorption isotherms were obtained using concentrations of the metal ions ranging from 0.1 to 100 mg L -1 . The adsorption process follows pseudo-second-order reaction kinetics, as well as Langmuir and D-R adsorption isotherms. The paper discusses the thermodynamic parameters of the adsorption (the Gibbs free energy, entropy, and enthalpy). Our results demonstrate that the adsorption process was spontaneous and endothermic under natural conditions. The maximum removal efficiencies were 93% for Cu(II) at pH 4, 82% for Ni(II) at pH 8, and 84% for Cr(VI) at pH 3

  3. Effect of Gamma Radiation on the Chemical and Physical Properties of Plasticised Carboxymethyl Cellulose (Cc) / Poly (vinyl alcohol)(Pva) Polymer Blend

    International Nuclear Information System (INIS)

    El-Salmawi, M.K.; Abu Zaid, M.M.; Ibraheim, M.S.; El-Nagger Abdel Wahab, M.; Zahran Abdel Hamid, H.

    2000-01-01

    The chemical and physical properties of plasticizer carboxymethyl cellulose (CMC)/ poly (vinylalcohol)(PVA) polymer blend before and after exposure to gamma ray were investigated by means of mechanical properties, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and scanning electron microscope (SEM). It was found that addition of plasticizer causes a significant increase in elongation at break and causes a marked drop in thermal stability. Thus, the addition of glycerol cause a significant decrease in glass transition temperature(Tg) of about 24 degree from the initial value. The morphological structure of plasticised blend was investigated by observation of fracture surfaces using SEM. The plasticised blend was used for recovery of some heavy metals from their salts such as Cu(II), Co(II) and Ni(II). It was found that plasticised blend have a great ability for absorbing these metals and it is measured by compleximetric titration and colour strength measurements

  4. Spectrophotometric Determination of Metoprolol Tartrate in Pharmaceutical Dosage Forms on Complex Formation with Cu(II

    Directory of Open Access Journals (Sweden)

    Mustafa Cesme

    2011-06-01

    Full Text Available A new, simple, sensitive and accurate spectrophotometric method has been developed for the assay of metoprolol tartrate (MPT, which is based on the complexation of drug with copper(II [Cu(II] at pH 6.0, using Britton-Robinson buffer solution, to produce a blue adduct. The latter has a maximum absorbance at 675 nm and obeys Beer’s law within the concentration range 8.5-70 mg/mL. Regression analysis of the calibration data showed a good correlation coefficient (r = 0.998 with a limit of detection of 5.56 mg/mL. The proposed procedure has been successfully applied to the determination of this drug in its tablets. In addition, the spectral data and stability constant for the binuclear copper(II complex of MPT (Cu2MPT2Cl2 have been reported.

  5. Influence of Ni(II) and Fe(III) complexes of 1,2 dihydroxy 9,10 anthraquinone on the modification in calf thymus DNA upon gamma irradiation

    International Nuclear Information System (INIS)

    Das, Saurabh; Mandal, Parikshit C.

    2009-01-01

    Ionizing radiation when allowed to fall upon cells or DNA, the radicals produced modify the base-pair region of the double strands. Radiation-induced double-strand modifications in calf thymus DNA were detected using Ni(II) and Fe(III) complexes of 1,2 dihydroxy 9,10 anthraquinone (DHA). 60 Co was used as the source for γ-radiation and ethidium bromide (EB) as the fluorescent dye for detecting double-strand modifications caused in DNA. Results show that the Fe(III)-DHA complex is more efficient in modifying the base-pair region in double-stranded DNA in comparison to DHA or the Ni(II)-DHA complex

  6. Synthesis of amino functionalized magnetic graphenes composite material and its application to remove Cr(VI), Pb(II), Hg(II), Cd(II) and Ni(II) from contaminated water

    International Nuclear Information System (INIS)

    Guo, Xiaoyao; Du, Bin; Wei, Qin; Yang, Jian; Hu, Lihua; Yan, Liangguo; Xu, Weiying

    2014-01-01

    Highlights: • Graphenes magnetic composite nanoparticles (Fe 3 O 4 -GS) were used to adsorb metal ions. • The adsorption of metal ions onto Fe 3 O 4 -GS could be well interpreted by the Freundlich equation. • The adsorption of metal ions onto Fe 3 O 4 -GS fit pseudo-second order kinetic model. • Thermodynamic studies illustrated that the adsorption process was endothermic and spontaneous in nature. - Abstract: In the present study, a kind of graphenes magnetic material (Fe 3 O 4 -GS) was prepared by compositing graphene sheet with ferroferric oxide, and shown to be effictive for removing Cr(VI), Pb(II), Hg(II), Cd(II) and Ni(II) ions from aqueous solution. The synthesized sorbent was characterized by SEM, TEM, FTIR, XRD, XPS and BET, respectively. The pH ZPC value of the sorbent was estimated to be 3.5 by alkaline-titration methods. Fe 3 O 4 -GS can be simply recovered from water with magnetic separation at low magnetic field within one minute. The sorption capacities of the metals were 17.29, 27.95, 23.03, 27.83 and 22.07 mg g −1 for Cr(VI), Pb(II), Hg(II), Cd(II) and Ni(II), respectively. Kinetic data showed good correlation with pseudo-second-order equation and the Freundlich model was found to fit for the isotherm data of all the heavy metal ions. It was found that the metals sorption was accomplished mainly via chelation or ion exchange. The results of thermodynamic studies illustrate that the adsorption process was endothermic and spontaneous in nature

  7. Biosorption of Cd(II), Ni(II) and Pb(II) from aqueous solution by dried biomass of aspergillus niger: application of response surface methodology to the optimization of process parameters

    Energy Technology Data Exchange (ETDEWEB)

    Amini, Malihe; Younesi, Habibollah [Department of Environmental Science, Faculty of Natural Resources and Marine Sciences, Tarbiat Modares University, Noor (Iran)

    2009-10-15

    In this study, the biosorption of Cd(II), Ni(II) and Pb(II) on Aspergillus niger in a batch system was investigated, and optimal condition determined by means of central composite design (CCD) under response surface methodology (RSM). Biomass inactivated by heat and pretreated by alkali solution was used in the determination of optimal conditions. The effect of initial solution pH, biomass dose and initial ion concentration on the removal efficiency of metal ions by A. niger was optimized using a design of experiment (DOE) method. Experimental results indicated that the optimal conditions for biosorption were 5.22 g/L, 89.93 mg/L and 6.01 for biomass dose, initial ion concentration and solution pH, respectively. Enhancement of metal biosorption capacity of the dried biomass by pretreatment with sodium hydroxide was observed. Maximal removal efficiencies for Cd(II), Ni(III) and Pb(II) ions of 98, 80 and 99% were achieved, respectively. The biosorption capacity of A. niger biomass obtained for Cd(II), Ni(II) and Pb(II) ions was 2.2, 1.6 and 4.7 mg/g, respectively. According to these observations the fungal biomass of A. niger is a suitable biosorbent for the removal of heavy metals from aqueous solutions. Multiple response optimization was applied to the experimental data to discover the optimal conditions for a set of responses, simultaneously, by using a desirability function. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  8. Synthesis and thermal characterization of new ternary chelates of piroxicam and tenoxicam with glycine and DL-phenylalanine and some transition metals

    Science.gov (United States)

    Zayed, M. A.; El-Dien, F. A. Nour; Mohamed, Gehad G.; El-Gamel, Nadia E. A.

    2006-05-01

    The ternary chelates of piroxicam (Pir) and tenoxicam (Ten) with Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) in the presence of various amino acids such as glycine (Gly) or DL-phenylalanine (PhA) were prepared and characterized with different physicochemical methods. IR spectra confirm that Pir and Ten behave as a neutral bidentate ligand coordinated to the metal ions via the pyridine- N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its deprotonated carboxylic group. In addition, PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its deprotonated carboxylic and amino groups. The solid reflectance spectra and magnetic moment measurements confirm that all the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. Thermal behaviour of the complexes is extensively studied using TG and DTA techniques. TG results show that water molecules (hydrated and coordinated) and anions are removed in the first and second steps while Gly, PhA, Pir and Ten are decomposed in the next and subsequent steps. The pyrolyses of the chelates into different gases are observed in the DTA curves as exo- or endothermic peaks. Also, phase transition states are observed in some chelates. Different thermodynamic parameters are calculated using Coats-Redfern method and the results are interpreted.

  9. Dynamics of ligand exchange mechanism at Cu(II) in water: an ab initio quantum mechanical charge field molecular dynamics study with extended quantum mechanical region.

    Science.gov (United States)

    Moin, Syed Tarique; Hofer, Thomas S; Weiss, Alexander K H; Rode, Bernd M

    2013-07-07

    Ab initio quantum mechanical charge field molecular dynamics (QMCF-MD) were successfully applied to Cu(II) embedded in water to elucidate structure and to understand dynamics of ligand exchange mechanism. From the simulation studies, it was found that using an extended large quantum mechanical region including two shells of hydration is required for a better description of the dynamics of exchanging water molecules. The structural features characterized by radial distribution function, angular distribution function and other analytical parameters were consistent with experimental data. The major outcome of this study was the dynamics of exchange mechanism and reactions in the first hydration shell that could not be studied so far. The dynamical data such as mean residence time of the first shell water molecules and other relevant data from the simulations are close to the results determined experimentally. Another major characteristic of hydrated Cu(II) is the Jahn-Teller distortion which was also successfully reproduced, leading to the final conclusion that the dominating aqua complex is a 6-coordinated species. The ab initio QMCF-MD formalism proved again its capabilities of unraveling even ambiguous properties of hydrated species that are far difficult to explore by any conventional quantum mechanics/molecular mechanics (QM/MM) approach or experiment.

  10. Dynamics of ligand exchange mechanism at Cu(II) in water: An ab initio quantum mechanical charge field molecular dynamics study with extended quantum mechanical region

    International Nuclear Information System (INIS)

    Moin, Syed Tarique; Hofer, Thomas S.; Weiss, Alexander K. H.; Rode, Bernd M.

    2013-01-01

    Ab initio quantum mechanical charge field molecular dynamics (QMCF-MD) were successfully applied to Cu(II) embedded in water to elucidate structure and to understand dynamics of ligand exchange mechanism. From the simulation studies, it was found that using an extended large quantum mechanical region including two shells of hydration is required for a better description of the dynamics of exchanging water molecules. The structural features characterized by radial distribution function, angular distribution function and other analytical parameters were consistent with experimental data. The major outcome of this study was the dynamics of exchange mechanism and reactions in the first hydration shell that could not be studied so far. The dynamical data such as mean residence time of the first shell water molecules and other relevant data from the simulations are close to the results determined experimentally. Another major characteristic of hydrated Cu(II) is the Jahn-Teller distortion which was also successfully reproduced, leading to the final conclusion that the dominating aqua complex is a 6-coordinated species. The ab initio QMCF-MD formalism proved again its capabilities of unraveling even ambiguous properties of hydrated species that are far difficult to explore by any conventional quantum mechanics/molecular mechanics (QM/MM) approach or experiment

  11. The preparation and characterization of Cu(II complexes with N,N’,N”,N’”-tetrakis(2-pyridylmethyl-1,4,8,11-tetraazacyclotetradecane and 2,6-diacetylpyridine bis(semi/thiosemicarbazones

    Directory of Open Access Journals (Sweden)

    GORDANA VUCKOVIC

    2004-03-01

    Full Text Available Two new Cu(II mixed-ligand complexes with octadentate N,N’,N”,N’”-tetrakis(2-pyridylmethyl-1,4,8,11-tetraazacyclotetradecane (tpmc and potentially pentadentate ligands 2,6-diacetylpyridine bis(semicarbazone (DAPsc2 or 2,6-diacetylpyridine bis(thiosemicarbazone (DAPtsc2 were prepared. The general formulas: [Cu4 DAPsc2(tpmc2]ClO48·5CH3COCH3·H2O and [Cu2 DAPtsc2(tpmc](ClO44·7C2H5OH were proposed on the basis of elemental analyses and conductometric measurements. The complexes were characterized by magnetic measurement, electronic absorption and IR spectroscopy. For the dinuclear complex, an exo coordination of Cu(II with four nitrogens from tpmc and m-bonded DAPtsc2 through sulfurs and possibly terminal hydrazinic (azomethine nitrogens is assumed. For the tetranuclear complex, it is supposed that one DAPsc2 bridges two [Cu2 tpmc]4+ units using oxygens and terminal hydrazinic nitrogens as ligators. Finally, some antibacterial activity of the complexes was found.

  12. Adsorption of heavy metals from aqueous solutions by Mg-Al-Zn mingled oxides adsorbent.

    Science.gov (United States)

    El-Sayed, Mona; Eshaq, Gh; ElMetwally, A E

    2016-10-01

    In our study, Mg-Al-Zn mingled oxides were prepared by the co-precipitation method. The structure, composition, morphology and thermal stability of the synthesized Mg-Al-Zn mingled oxides were analyzed by powder X-ray diffraction, Fourier transform infrared spectrometry, N 2 physisorption, scanning electron microscopy, differential scanning calorimetry and thermogravimetry. Batch experiments were performed to study the adsorption behavior of cobalt(II) and nickel(II) as a function of pH, contact time, initial metal ion concentration, and adsorbent dose. The maximum adsorption capacity of Mg-Al-Zn mingled oxides for cobalt and nickel metal ions was 116.7 mg g -1 , and 70.4 mg g -1 , respectively. The experimental data were analyzed using pseudo-first- and pseudo-second-order kinetic models in linear and nonlinear regression analysis. The kinetic studies showed that the adsorption process could be described by the pseudo-second-order kinetic model. Experimental equilibrium data were well represented by Langmuir and Freundlich isotherm models. Also, the maximum monolayer capacity, q max , obtained was 113.8 mg g -1 , and 79.4 mg g -1 for Co(II), and Ni(II), respectively. Our results showed that Mg-Al-Zn mingled oxides can be used as an efficient adsorbent material for removal of heavy metals from industrial wastewater samples.

  13. Synthesis and stereochemical assignments of diastereomeric Ni(II complexes of glycine Schiff base with (R-2-(N-{2-[N-alkyl-N-(1-phenylethylamino]acetyl}aminobenzophenone; a case of configurationally stable stereogenic nitrogen

    Directory of Open Access Journals (Sweden)

    Hiroki Moriwaki

    2014-02-01

    Full Text Available A family of chiral ligands derived from α-phenylethylamine and 2-aminobenzophenone were prepared by alkylation of the nitrogen atom. Upon reaction with glycine and a Ni(II salt, these ligands were transformed into diastereomeric complexes, as a result of the configurational stability of the stereogenic nitrogen atom. Different diastereomeric ratios were observed depending on the substituent R introduced in the starting ligand, and stereochemical assignments were based on X-ray analysis, along with NMR studies and optical rotation measurements.

  14. Studies on chelation properties of ampicillin with trace metal ions and comparison with penicillin complexes

    International Nuclear Information System (INIS)

    Rehmani, F.S.; Hameed, W.

    2003-01-01

    The penicillin is highly effective antibiotic with extremely wide margin of safety. Ampicillin e is the penicillin group of antibiotic in which side chain is phenyl group i.e. D-amino benzyl penicillin. The side chain determines many of anti bacterial and pharmacological characteristics. They inhibit the protein synthesis in bacterial cell wall. The chelating properties of the antibiotic may be used in the metal transport across the membrane. The present investigations are helpful in drug metabolism and their effects on minerals contents of the body. The complex formation between Ampicillin and penicillin with trace metal ions such as Fe(III), Cr(III), Al(III), Mn(II), Ni(II), Co(II), Ca(II), Mg(II), Cu(III) and Zn(II) were studied by potentiometric titrations and spectrophotometric methods. Stoichiometry of these complexes were studied by mole ratio method. It was found that the Fe(III) and Cu(II) ions form most stable complexes near physiological pH and the mole ratio was 1:1. (author)

  15. Microwave synthesis, spectral, thermal, and antimicrobial activities of some transition metal complexes involving 5-bromosalicylaldehyde moiety

    Directory of Open Access Journals (Sweden)

    Rajendra K. Jain

    2012-07-01

    Full Text Available The coordination complexes of Co(II, Ni(II and Cu(II derived from 5-bromosalicylidene-3,4-dimethylaniline (BSMA and 5-bromosalicylidene-3,4-dichloroaniline (BSCA have been synthesized by conventional as well as microwave methods. These compounds have been characterized by elemental analysis, FT-IR, molar conductance, electronic spectra, 1H-NMR, FAB-mass, ESR, magnetic susceptibility, electrical conductivity and thermal analysis. The complexes are coloured and stable in air. Analytical data revealed that all the complexes exhibited 1:2 (metal: ligand ratio with coordination number 4 or 6. IR data shows that the ligand coordinates with the metal ions in a bidentate manner through the phenolic oxygen and azomethine nitrogen. FAB-mass and thermal data show degradation pattern of the complexes. Solid state electrical conductivity studies reflect semiconducting nature of the complexes. The Schiff base and metal complexes show a good activity against the Gram-positive bacteria; Staphylococcus aureus and Gram-negative bacteria; Escherichia coli and fungi Aspergillus niger and Candida albicans.

  16. Photochemical activation and reactivity of polynuclear transition metal complex molecules. Final report

    International Nuclear Information System (INIS)

    Endicott, J.F.; Lintvedt, R.L.

    1982-06-01

    Several bi- and trinuclear metal complexes containing ligands from β-polyketonates have been synthesized and characterized including homo- and hetero-polynuclear complexes. New synthetic approaches to the preparation of heterobi- and trinuclear complexes have been developed that allow the preparation of a large number of molecules containing heavy-metal ions such as Pd 2+ or UO 2 2+ and a first-row transition-metal ion. The electrochemical properties of these complexes have been investigated and many exhibit the ability to transfer two electrons at very nearly the same potential. Photochemical studies on binuclear Cu(II) and Ni(II) showed that these compounds yielded reduced metal species and decomposition upon irradiation. Luminescence of hetero-complexes of uranyl polyketonates is observed at 77 0 K with the UO 2 2+ moiety functioning as an isolated chromophore in which emission is observed only on direct excitation of UO 2 2+ and energy transfer to lower states in the molecule is not observed

  17. Biosorption of heavy metals from wastewater by biosolids

    Energy Technology Data Exchange (ETDEWEB)

    Orhan, Y.; Bueyuekguengoer, H. [Ondokuz Mayis University, Engineering Faculty, Environmental Engineering Department, 55139 Samsun (Turkey); Hrenovic, J. [University of Zagreb, Faculty of Science, Department of Biology, Rooseveltov trg 6, 10000 Zagreb (Croatia)

    2006-08-15

    In a study where the removal of heavy metals from wastewater is the primary aim, the biosorption of heavy metals onto biosolids prepared as Pseudomonas aeruginosa immobilized onto granular activated carbon was investigated in batch and column systems. In the batch system, adsorption equilibriums of heavy metals were reached between 20 and 50 min, and the optimal dosage of biosolids was 0.3 g/L. The biosorption efficiencies were 84, 80, 79, 59 and 42 % for Cr(VI), Ni(II), Cu(II), Zn(II) and Cd(II) ions, respectively. The rate constants of biosorption and pore diffusion of heavy metals were 0.013-0.089 min{sup -1} and 0.026-0.690 min{sup -0.5}. In the column systems, the biosorption efficiencies for all heavy metals increased up to 81-100 %. The affinity of biosorption for various metal ions towards biosolids was decreased in the order: Cr = Ni > Cu > Zn > Cd. (Abstract Copyright [2006], Wiley Periodicals, Inc.)

  18. Multiple heavy metal removal using an entomopathogenic fungi Beauveria bassiana.

    Science.gov (United States)

    Gola, Deepak; Dey, Priyadarshini; Bhattacharya, Arghya; Mishra, Abhishek; Malik, Anushree; Namburath, Maneesh; Ahammad, Shaikh Ziauddin

    2016-10-01

    Towards the development of a potential remediation technology for multiple heavy metals [Zn(II), Cu(II), Cd(II), Cr(VI) and Ni(II)] from contaminated water, present study examined the growth kinetics and heavy metal removal ability of Beauveria bassiana in individual and multi metals. The specific growth rate of B. bassiana varied from 0.025h(-1) to 0.039h(-1) in presence of individual/multi heavy metals. FTIR analysis indicated the involvement of different surface functional groups in biosorption of different metals, while cellular changes in fungus was reflected by various microscopic (SEM, AFM and TEM) analysis. TEM studies proved removal of heavy metals via sorption and accumulation processes, whereas AFM studies revealed increase in cell surface roughness in fungal cells exposed to heavy metals. Present study delivers first report on the mechanism of bioremediation of heavy metals when present individually as well as multi metal mixture by entomopathogenic fungi. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. The use of sugar and alcohol industry waste in the adsorption of potentially toxic metals.

    Science.gov (United States)

    Santos, Oseas Silva; Mendonça, André Gustavo Ribeiro; Santos, Josué Carinhanha Caldas; Silva, Amanda Paulina Bezerra; Costa, Silvanio Silverio Lopes; Oliveira, Luciana Camargo; Carmo, Janaina Braga; Botero, Wander Gustavo

    2016-01-01

    One of the waste products of the industrial process of the sugar and alcohol agribusiness is filter cake (FC). This waste product has high levels of organic matter, mainly proteins and lipids, and is rich in calcium, nitrogen, potassium and phosphorous. In this work we characterized samples of FC from sugar and alcohol industries located in sugarcane-producing regions in Brazil and assessed the adsorption of potentially toxic metals (Cu(II), Cd(II), Pb(II), Ni(II) and Cr(III)) by this waste in mono- and multi-elemental systems, seeking to use FC as an adsorbent in contaminated environments. The characterization of FCs showed significant differences between the samples and the adsorption studies showed retention of over 90% of potentially toxic metals. In a competitive environment (multi-metallic solution), the FC was effective in adsorbing all metals except lead, but less effective compared to the mono-metallic solution. These results show the potential for use of this residue as an adsorbent in contaminated environments.

  20. Spectral, optical and cytotoxicity studies on 2-isonicotinoyl-N-phenylhydrazine-1-carboxamide(H3L) and some of its metal complexes

    Science.gov (United States)

    Hosny, Nasser M.; Hassan, Nader Y.; Mahmoud, Heba M.; Abdel-Rhman, Mohamed H.

    2018-03-01

    The ligand 2-isonicotinoyl-N-phenylhydrazine-1-carboxamide (H3L) and its metal complexes with Co(II), Ni(II), Cu(II) and Zn(II) acetates have been synthesized. The isolated compounds have been characterized by elemental analyses, FT-IR, 1H NMR, 13C NMR, ESR, mass, electronic spectra, electrical conductivity, effective magnetic moments and thermal analyses. The free organic ligand exists in the keto form, but in the metal complexes, it coordinates in the enol form. Four coordinated species were suggested for all the isolated metal complexes. The measured optical band gap values confirmed the presence of direct electronic transition and the semi-conductivity of the compounds. The ligand and its Zn(II) complex were examined as cytotoxic agent against HCT-116 and HePG-2. The ligand showed very strong cytotoxic effect against HePG-2, but moderate cytotoxicity against HCT-116. Zn(II) complex showed weak cytotoxicity against the two cell lines.