Search results for "Potentiometric titration"
showing 10 items of 152 documents
CO 2 Fixation and Activation by Cu II Complexes of 5,5″‐Terpyridinophane Macrocycles
2007
An aza-terpyridinophane receptor containing the polyamine 4,7,10,13-tetraazahexadecane-1,16-diamine linked through methylene groups to the 5,5″ positions of a terpyridine unit has been prepared and characterized (L). The acid-base behaviour, CuII speciation and ability to form ternary complexes (CuII-L-carbonate) have been explored by potentiometric titrations in 0.15 M NaClO4 and by UV/Vis and paramagnetic NMR spectroscopy. Comparisons are made with a previously reported terpyridinophane containing the polyamine 4,7,10-triazatridecane-1,13-diamine (L1). For this latter receptor, reductive coupling between indigo and carbon dioxide at indigo-modified electrodes produces carboxylated derivat…
Co2+ Translocation in a Terpyridine−Cyclam Ditopic Receptor
2001
The coordination behaviour of the ditopic receptor of 1-[p-(2,2′:6′,2′′-terpyrid-4′-yl)tolyl]-1,4,8,11-tetraazacyclotetradecane (L1) towards Co2+ in acetonitrile/water (70:30, v/v) has been investigated. At acidic pH values, the L1−H+−Co2+ system shows an oxidation wave at 150 mV vs. SCE, characteristic of Co2+ in a bis(terpyridine) environment. Upon addition of OH−, a reduction in the intensity of the wave at 150 mV is observed and a new oxidation wave appears at 1.30 V. This new wave is close to that found for [Co(cyclam)]2+ under similar working conditions. The electrochemical data thus suggest that there is a pH-controlled translocation of the Co2+ ion from the bis(terpyridine) to the c…
Effect of Nitrogen Methylation on Cation and Anion Coordination by Hexa- and Heptaazamacrocycles. Catalytic Properties of These Ligands in ATP Dephos…
1996
The stability constants of the complexes formed by 1,10-dimethyl-1,4,7,10,13,16-hexaazacyclooctadecane (L) and 1,4,7-trimethyl-1,4,7,10,13,16,19-heptaazacyclohenicosane (L1) with Ni(2+), Cu(2+), Zn(2+), Cd(2+), and Pb(2+), as well as that for the formation of PbL2(2+) (L2 = 1,4,7,13-tetramethyl-1,4,7,10,13,16-hexaazacyclooctadecane), were determined by means of potentiometric (pH-metric) titrations in 0.15 mol dm(-)(3) NaClO(4) at 298.1 +/- 0.1 K. The enthalpy changes for the formation of Cu(2+) complexes with L and L1 were measured by means of microcalorimetry. These thermodynamic data were compared with those previously reported for L2, 1,4,7,10,13,16-hexaazacyclooctadecane (L3), and 1,4,…
Hydrolytically active tetranuclear [NiII2]2 complexes: synthesis, structure, spectroscopy and phosphoester hydrolysis
2015
Three tetranuclear nickel(II) complexes, [Ni4(H2chdp)2(H2O)4]Br2·4CH3OH·3H2O (1), [Ni4(H2chdp)2(H2O)4](PF6)2 (2) and [Ni4(H2chdp)2(H2O)4](ClO4)2·3.2CH3OH·0.8H2O (3) have been synthesized by exploiting the flexibility, chelating ability and bridging potential of a new symmetrical μ-bis(tetradentate) ligand, H5chdp (H5chdp = N,N′-bis[2-carboxybenzomethyl]-N,N′-bis[2-hydroxyethyl]-1,3-diaminopropan-2-ol). Complexes 1, 2 and 3 have been synthesized by carrying out reaction of the ligand H5chdp with stoichiometric amounts of NiCl2·6H2O/NaBr, NiCl2·6H2O/NH4PF6, and Ni(ClO4)2·6H2O, respectively, in methanol–water in the presence of NaOH at ambient temperature. Characterizations of the complexes ha…
NMR, potentiometric and ESI-MS combined studies on the zinc(II) magnesium(II) and calcium(II) complexation by (morpholin-1-yl)methane-1,1-diphosphoni…
2012
Abstract The crystal structures of the two derivatives of aminomethane-1,1-diphosphonic acid with morpholinyl- (1) and thiomorpholinyl- (2) side chains were determined by single crystal X-ray diffraction and discussed with respect to molecular geometry and solid state organization. The protonation equilibria, solution behavior and complex-formation equilibria in solutions of 1 and 2 with the Zn(II), Mg(II) and Ca(II) ions were studied by means of NMR, pH-potentiometry and ESI-MS methods. As the p K ( NH + ) protonation constants of 1 and 2 are high (11.65 and 11.91, respectively) two different approaches were used to evaluate the pH-potentiometric data. The first approach disregarded the pr…
Evaluation of the sequestering ability of different complexones towards Ag+ ion
2014
Abstract The interaction between Ag+ cation and different ligands was evaluated as a function of temperature and ionic strength by means of potentiometric techniques. Six aminopolycarboxylic (APCs) and aminopolyphosphonic (APPs) ligands were chosen, namely four APCs: nitrilotriacetic acid (NTA), ethylene-glycol-bis(2-aminoethylether)-N,N,N’,N’-tetraacetic acid (EGTA), ethylenediamine-N,N,N’,N’-tetraacetate (EDTA) and diethylenetriamine-N,N,N’,N”,N”-pentaacetic acid (DTPA)] and two APPs: [(1-hydroxyethane-1,1-diyl)bis(phosphonic acid) (HEDP) and [[(Phosphonomethyl)imino]bis[2,1-ethanediylnitrilobis(methylene)]] tetrakis-phosphonic acid (DTPP). Different mononuclear species with general formu…
Electronic Interactions in Ferrocene‐ and Ruthenocene‐Functionalized Tetraazamacrcocyclic Ligand Complexes of Fe II/III , Co II , Ni II , Cu II and Z…
2005
The syntheses of ferrocene- and ruthenocene-functionalized tetraazamacrocyclic ligands and their corresponding transition metal complexes are described. Reaction of N,N′-bis(2-aminoethyl)-1,3-propanediamine (2,3,2-tet) with 1,1′-diformylferrocene and 1,1′-diformylruthenocene produces the ligands fcmac and rcmac in 81−85% yield. Examination of their CuII, NiII, CoII, ZnII and FeII/III complexes by IR, UV/Vis, EPR and Mossbauer spectroscopy as well as by electrochemical studies suggests electronic communication between the two metal centers of each complex. The molecular structure of [CuII(fcmac)(FBF3)]BF4, determined by X-ray structure analysis, is reported and shows that the distance betwee…
Polyaza and azaoxa macrocyclic receptors functionalised with fluorescent subunits; Hg2+ selective signalling
2000
A polyazacycloalkane containing naphthyl groups, 1,4,8,11-tetrakis(naphthylmethyl)-1,4,8,11-tetraazacyclotetradecane (L1), and the azaoxa cycloalkane receptors containing anthracenyl groups, 7,13-bis(anthracenylmethyl)-1,4,10-trioxa-7,13-diazacyclopentadecane (L2) and 10-anthracenylmethyl-1,4,7-trioxa-10-azacyclododecane (L3), have been synthesized and their activity as fluorescent chemosensors studied towards the metal cations Cu2+, Zn2+, Cd2+, Hg2+ and Pb2+ in THF–water (70∶30 v/v, 0.1 mol dm−3 tetrabutylammonium perchlorate, 25 °C) for L1 and 1,4-dioxane–water (70∶30 v/v, 0.1 mol dm−3 potassium nitrate, 25 °C) for L2 and L3. The crystal structure of the complex [Cd(L1)(Cl)][PF6] has been…
Study of the coordination of ortho-tyrosine and trans-4-hydroxyproline with aluminum(III) and iron(III)
2018
Abstract The coordination of amino acids ortho-tyrosine (o-Tyr, 1) and trans-4-hydroxyproline (HPro, 2) with the biologically important trivalent metal ions Al(III) and Fe(III) in aqueous solution was investigated by 1H and 13C high resolution NMR, Laser Desorption Mass Spectrometry (LD-MS), and MS/MS experiments. Potentiometric measurements were also carried out in 0.16 M NaCl, 37 °C, by varying the pH between 2.0 and 3.5. NMR spectra recorded on aqueous solutions of amino acids 1 or 2 in the presence of the appropriate trivalent metal chloride suggested that binding of Al(III) and Fe(III) involved the COOH and NH2 functional groups of ligands, while their phenolic and alcoholic groups whi…
Validation of a method for the determination of boron in ceramic materials by X-ray fluorescence spectrometry
2000
Abstract A method is proposed for boron determination in ceramic materials, boracic raw materials and ceramics frits of different compositions by wavelength dispersive X-ray fluorescence technique. The instrumental conditions were studied and the sample preparation procedures were optimized. The reference method used was the potentiometric titration of mannitol–boric complex acid and the technique was optimized for the determination of B 2 O 3 in each of the materials used. The samples for XRF determination were obtained as pellets and as glass discs. For the pellets different binders were studied, such as mannitol and cellullose for the samples of raw materials, and polyvinylpirrolidone an…