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Sökning: swepub > Umeå universitet > Refereegranskat > (2000-2004) > Pettersson Lage

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1.
  • Gorzsás, András, et al. (författare)
  • A speciation study of the aqueous H+/H2VO4–/H2O2/L--alanyl-L-serine system
  • 2003
  • Ingår i: Dalton Transactions. ; s. 1161-7
  • Tidskriftsartikel (refereegranskat)abstract
    • A detailed study of the quaternary aqueous H+/H2VO4–/H2O2/L--alanyl-L-serine (Alaser) system has been performed at 25 °C in 0.150 M Na(Cl) medium, representing the ionic strength of human blood, using quantitative 51V NMR and potentiometric data (glass electrode). Data were evaluated with the computer program LAKE, which is able to treat combined EMF and NMR data. The pKa-values for Alaser were determined as 8.04 ± 0.01 and 3.07 ± 0.01. The errors given are 3. In the ternary H+/H2VO4–/Alaser system, two complexes, (H+)p(H2VO4–)q(Alaser)r, having (p, q, r) values (0, 1, 1) and (–1, 1, 1) with log0,1,1= 2.42 ± 0.01 and log–1,1,1=–5.80 ± 0.05 explain all data in the pH region 2.5–9.5. Equilibrium conditions are illustrated in distribution diagrams and structure proposals are given based on 1H and 13C NMR investigations. In the quaternary H+/H2VO4–/H2O2/Alaser system, six complexes could be found in addition to all binary and ternary complexes over the pH region 2.6–11.1, four with a V/X/Alaser ratio 1 1 1 and two with a ratio 1 2 1 (X = peroxo ligand). The formation of the monoperoxo vanadium species is very slow, requiring up to 10 days for complete equilibrium. Significant decomposition of peroxide occurs only in acidic solutions. Chemical shifts, compositions and formation constants for the six quaternary complexes are given, and equilibrium conditions are illustrated in distribution diagrams. The H+/H2VO4–/H2O2/Alaser/Alahis system, where Alahis denotes L--alanyl-L-histidine, was briefly investigated and no mixed ligand species were detected.
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2.
  • Gorzsás, András, et al. (författare)
  • Speciation in the aqueous H+/H2VO4–/H2O2/L-(+)-lactate system
  • 2003
  • Ingår i: Dalton Transactions. ; s. 2503-11
  • Tidskriftsartikel (refereegranskat)abstract
    • A detailed study of the quaternary aqueous H+/H2VO4–/H2O2/L-(+)-lactate (Lac–) system has been performed at 25 °C in 0.150 M Na(Cl) medium, representing the ionic strength of human blood, using quantitative 51V NMR and potentiometric data (glass electrode). Data were evaluated with the computer program LAKE, which is able to treat combined EMF and NMR data. The pKa-value for lactic acid was determined as 3.653 ± 0.002. The error given is 3. In the ternary H+/H2VO4–/Lac– system, eight complexes were found in the pH region 1.1–10.9; only half of them are mononuclear. Owing to the fast reduction of vanadium(V) in acidic solutions and to the slow equilibria of the inorganic vanadates under certain conditions, the final model of this ternary system presented in the study is limited to pH > 3.1. Solutions, in which reduction occurred to any extent, were excluded from all calculations, hence the study is limited to vanadium(V). In the quaternary H+/H2VO4–/H2O2/Lac– system, seven complexes could be found in addition to all binary and ternary complexes over the pH region 2.1–10.0, only two of which were mononuclear. Equilibrium is fast, but significant decomposition of peroxide occurs in acidic solutions over very short time, limiting the final model to pH > 4. Chemical shifts, compositions and formation constants are given, and equilibrium conditions are illustrated in distribution diagrams as well as the fit of the model to the experimental data. Simple biological tests were carried out to check the resistance of different peroxovanadate complexes (including the ones with Lac–) against human catalase and the results are being presented here.
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3.
  • Pettersson, Lage, et al. (författare)
  • 17O NMR Study of Aqueous Peroxoisopolymolybdates at lower peroxide/Mo ratios.
  • 2003
  • Ingår i: Dalton Trans. ; :1, s. 146-152
  • Tidskriftsartikel (refereegranskat)abstract
    • Aqueous peroxomolybdates have been studied using 17O NMR together with equilibrium measurements and calculations, over a wide range of conditions. Ten peroxo species are identified, mostly in more than one state of protonation. Some are already known in the solid state, or from equilibrium analysis, but structural information is also obtained for MoO3(HO2)– and the new or previously tentative species Mo2O5(O2)22–, HpMo7O23(O2)2p–6 and HpMo7O23(O2)p–6(p= 0–2). Sites of protonation are identified, as are 17O resonances from both bidentate and monodentate peroxide. Several oxygen exchange processes are also seen, including a probable dimer–tetramer exchange.
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4.
  • Taube, Fabian, et al. (författare)
  • Equilibria and Dynamics of Some Aqueous Peroxomolybdophosphate Catalysts: A Potentiometric and 31P NMR Spectroscopic Study
  • 2003
  • Ingår i: Dalton Trans.. ; :12, s. 2512-2518
  • Tidskriftsartikel (refereegranskat)abstract
    • The equilibrium speciation in the pH++qMoO42–+rH2O2+sH2PO4–+tSO42–(H+)p(MoO42–)q(H2O2)r(H2PO4–)s(SO42–)tp–2q–s–2t system in 0.300 M Na2(SO4) medium at 25 °C and [H2O2]tot/[Mo]tot > 2 has been determined from potentiometric data and 31P NMR integral and chemical shift data in the range 1.0 pH 9.0, 2.0 [MoO42–]tot/mM 293, 32 [H2O2]tot/mM 640, 2 [H2PO4–]tot/mM 60 and 200 [SO42–]tot/mM 380. Species with the following compositions were obtained: MoX2P3–(0,1,2,1,0), MoX2P2–(1,1,2,1,0), MoX2P–(2,1,2,1,0), Mo2X4P3–(2,2,4,1,0), Mo2X4P2–(3,2,4,1,0), Mo3X6P3–(4,3,6,1,0), Mo3X6P2–(5,3,6,1,0) and Mo4X8P3–(6,4,8,1,0). The numbers and charges of molybdenum (Mo), peroxide (X), phosphate (P) and sulfate (S) in each species are given in the abbreviated formula MoqXrPsStp–2q–s–2t. The numbers in parentheses refer to the values of p, q, r, s and t in the formula above. The following formation constants with 3 were obtained; log0,1,2,1,0= 5.16 ± 0.09, log1,1,2,1,0= 12.73 ± 0.02 (pKa= 7.63), log2,1,2,1,0= 16.14 ± 0.03 (pKa= 3.42), log2,2,4,1,0= 25.03 (± 0.04), log3,2,4,1,0= 29.54 ± 0.02 (pKa= 4.51), log4,3,6,1,0= 42.30 ± 0.03, log5,3,6,1,0= 44.06 ± 0.08 (pKa= 1.76), log6,4,8,1,0= 57.30 ± 0.07. pKa values for H3PO4 and H2PO4– were determined to 2.00 and 6.48, respectively. Chemical exchange processes were detected by 31P NMR 2D EXSY and selective magnetisation transfer experiments between the complexes. An averaged lifetime, (X2Mo–OP) 30 ms, can be estimated for the MoX2P and Mo2X4P species at pH = 5.5 and 5 °C.
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5.
  • Andersson, Ingegärd, et al. (författare)
  • Speciation in the aqueous H+/H2VO4–/H2O2/picolinate system relevant to diabetes research
  • 2004
  • Ingår i: Dalton Transactions. - Cambridge : Royal Society of Chemistry, Thomas Graham House. - 1477-9226. ; :3, s. 421-428
  • Tidskriftsartikel (refereegranskat)abstract
    • A detailed study of the quaternary aqueous H+/H2VO4−/H2O2/picolinate (Pi−) system has been performed at 25 °C in 0.150 M Na(Cl) medium using quantitative 51V NMR (500 MHz) and potentiometric data (glass electrode). In the ternary H+/H2VO4−/Pi− system, six complexes have been found in the pH region 1–10. In the quaternary H+/H2VO4−/H2O2/Pi−system, eight additional complexes have been found. Generally, equilibria are fast in both systems. The rate of peroxide decomposition depends on the species in solution. Chemical shifts, compositions and formation constants for the species are given. Equilibrium conditions and the fit of the model to the experimental data are illustrated in distribution diagrams. Possible formation of mixed ligand species with imidazole, lactic acid and citric acid have been investigated and ruled out under the same experimental conditions. Structural proposals are given, based on 13C NMR data and available crystal structures.
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6.
  • Andersson, Ingegärd, et al. (författare)
  • Speciation in vanadium bioinorganic systems 6. Speciation study of aqueous peroxovanadates, including complexes with imidazole
  • 2000
  • Ingår i: Journal of Inorganic Biochemistry. ; 80:1-2, s. 51-8
  • Tidskriftsartikel (refereegranskat)abstract
    • Using a combination of potentiometry (glass electrode) and quantitative 51V NMR spectroscopy, the full speciation in the vanadate–peroxide and vanadate–peroxide–imidazole systems was determined in the pH range 1–10 (0.150 M Na(Cl) medium, 25 °C). Using the computer program LAKE, the pKa value of imidazole and the formation constants for 10 peroxovanadate species and also for three more species where a single imidazole moiety is also bound, have been calculated. The experimental data show a good fit to the calculated speciation model, even for the less abundant species. The species are either monomeric or dimeric in vanadium, and four resonances of the dimeric species have been unambiguously assigned via 2D 51V NMR. Diperoxovanadates are the favoured species at pH 2–10, when sufficient peroxide is present. Imidazole is found to bind strongly to them at pH 6–9. The equilibrium conditions are illustrated in distribution diagrams.
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7.
  • Boström, Dan, et al. (författare)
  • Sodium trirubidium metavanadate monohydrate
  • 2003
  • Ingår i: Acta Crystallographica Section E : Structure Reports Online. - International Union of Crystallography. - 1600-5368. ; E59:11, s. i151-i153
  • Tidskriftsartikel (refereegranskat)abstract
    • The title compound, sodium trirubidium metavanadate monohydrate, NaRb3(VO3)4(H2O), crystallizes in the orthorhombic space group Pnma. The structure, which represents a rare type of catena-vanadate, is built up of strongly folded chains of corner-sharing [VO4] tetrahedra, running in the [010] direction with a periodicity of four. A three-dimensional framework is obtained by sodium ions linking adjacent chains in the [001] direction and by rubidium ions linking adjacent chains in the [100] direction. The single water molecule binds to the sodium ion and to two rubidium ions.
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8.
  • Gorzsás, András, et al. (författare)
  • Speciation in the aqueous H+/H2VO4–/H2O2/citrate system of biomedical interest
  • 2004
  • Ingår i: Dalton Transactions. - Cambridge : Royal Society of Chemistry, Thomas Graham House. - 1477-9226. ; :18, s. 2873-2882
  • Tidskriftsartikel (refereegranskat)abstract
    • The speciation in the quaternary aqueous H+/H2VO4–/H2O2/citrate (Cit3–) and H+/H2VO4–/Cit3–/L-(+)-lactate (Lac–) systems has been determined at 25 °C in the physiological medium of 0.150 M Na(Cl). A combination of 51V NMR integral intensities and chemical shift (Bruker AMX500) as well as potentiometric data (glass electrode) have been collected and evaluated with the computer program LAKE, which is able to treat multimethod data simultaneously. The pKa-values for citric acid have been determined as 2.94, 4.34 and 5.61. Altogether six vanadate–citrate species have been found in the ternary H+/H2VO4–/Cit3– system in the pH region 2–10, only two of which are mononuclear. Reduction of vanadium(V) becomes more pronounced at pH < 2. Solutions, in which reduction occurred to any extent, were excluded from all calculations. In the quaternary H+/H2VO4–/H2O2/Cit3– system, eight complexes have been found in addition to all binary and ternary complexes over the pH region 2–10, including three mononuclear species. Equilibria in general are fast, but the significant and rapid decomposition of peroxide in acidic solutions limited the final model to pH > 4. In the quaternary H+/H2VO4–/Cit3–/Lac– system, two mixed-ligand species have been determined, with the compositions V2CitLac2– and V2CitLac3–(pKa= 5.0). To our knowledge, this is the first time such complexes have been reported for vanadium(V). 51V NMR chemical shifts, compositions and formation constants are given, and equilibrium conditions are illustrated in distribution diagrams as well as the fit of the model to the experimental data. When suitable, structural proposals are given, based on 13C NMR measurements and available literature data of related compounds.
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9.
  • Lyxell, Dan-Göran, et al. (författare)
  • Multicomponent Polyanions. 57. Large-Angle X-ray Scattering Study of Aqueous Molybdophenylphosphonate Solutions
  • 2001
  • Ingår i: Inorganic Chemistry. ; 40:4, s. 584-92
  • Tidskriftsartikel (refereegranskat)abstract
    • The radial distribution functions are calculated from large-angle X-ray scattering (LAXS) measurements for one concentrated aqueous molybdate/heptamolybdate solution and five aqueous molybdophenylphosphonate solutions (lithium chloride medium). Besides water and hydrated lithium, chloride, and molybdate ions, five species in all, having different nuclearities, are postulated to exist in the solutions, according to equilibrium studies using potentiometry and 31P NMR spectroscopy. The structures of the three polymolybdate species Mo7O246-, Mo8O264-, and (C6H5P)2Mo5O214-, for which the structures are determined crystallographically, are confirmed to exist also in aqueous solution. The principal structures of the remaining two complexes, (C6H5P)Mo6O21(OH2)52- and (C6H5P)Mo7O25(OH2)4-, are elucidated with the use of structures of related species. Both anions have one group of four edge-sharing MoO6 octahedra and another group of two MoO6 octahedra connected by sharing corners, forming a bent unsymmetric six-membered ring, with the C6H5PO3 group placed on the crowded side of the ring. In the former, the group of two MoO6 octahedra is edge-shared, while in the latter, the group is face-shared, resulting in a ring small enough to tetrahedrally coordinate to the seventh molybdenum opposite the phenyl group.
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10.
  • Pettersson, Lage, et al. (författare)
  • Speciation in peroxovanadate systems
  • 2003
  • Ingår i: Coordination Chemistry Reviews. ; 237:1-2, s. 77-87
  • Tidskriftsartikel (refereegranskat)abstract
    • Detailed and thorough potentiometric and 51V-NMR spectroscopic investigations of H+–H2VO4−–H2O2–Ligand systems have been performed at 25 °C in 0.15 M Na(Cl) ionic medium. Extensive ranges of vanadate, hydrogen peroxide and ligand concentration and of pH have been covered. The medium was chosen to represent the physiological conditions in human blood. The computer program , designed to treat different types of data simultaneously, has been used to establish the entire speciation in the systems. Before studying systems containing the ligand (L), the complete speciation in the subsystem H+–H2VO4−–H2O2 must be known under the same experimental conditions. The formation constants in this subsystem have earlier been determined and it was found that hydrogen peroxide interacts with vanadate in the whole pH range studied (0.5–10.5). In all, 10 peroxovanadate species were identified and diperoxovanadate species were found to be exceptionally stable at physiological pH. The ligands studied so far include imidazole (Im), -α-alanyl--histidine (Ah), -α-alanyl--serine (As), picolinic acid (Pi), and -(+)-lactic acid (La). In these five systems, as many as 3, 8, 6, 8, and 5 different peroxovanadate—L species (isomers included) were identified. A feature common to all these systems is that V(H2O2)2L species are formed at physiological pH. Notably, the 51V chemical shift values of diperoxovanadate moieties are always found in the range −670 to −770 ppm, and those of monoperoxovanadate from −540 to −670 ppm. The equilibrium conditions are illustrated in distribution diagrams and the effectiveness of the different ligands as complexation agents are compared. In the case of diperoxovanadate complexes, ligands with aromatic nitrogen (Im, Pi, Ah) are the most effective, the one with both aliphatic nitrogen and oxygen (As) is less effective, and the one with oxygen only (La) is the least preferred.
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