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  • 1. Acharya, Shravan S.
    et al.
    Easton, Christopher D.
    McCoy, Thomas M.
    Spiccia, Leone
    Ohlin, C. André
    Umeå University, Faculty of Science and Technology, Department of Chemistry. School of Chemistry, Monash University, Clayton, Australia.
    Winther-Jensen, Bjorn
    Diverse composites of metal-complexes and PEDOT facilitated by metal-free vapour phase polymerization2017In: Reactive & functional polymers, ISSN 1381-5148, E-ISSN 1873-166X, Vol. 116, p. 101-106Article in journal (Refereed)
    Abstract [en]

    Abstract Oxidative polymerization for the manufacture of conducting polymers such as poly(3,4-ethylenedioxy-thiophene) has traditionally employed iron(III) salts. Demonstrated in this study is vapour phase polymerization of 3,4-ethylenedio- xythiophene using a metal-free oxidant, ammonium persulfate, leading to films with an estimated conductivity of 75 S/cm. Additionally, a route for embedding active transition metal complexes into these poly(3,4-ethylenedioxythiophene)/-poly(styrene-4-sulfonate) (PEDOT/PSS) films via vapour assisted complexation is outlined. Here, the vapour pressure of solid ligands around their melting temperatures was exploited to ensure complexation to metal ions added into the oxidant mixture prior to polymerization of PEDOT. Four composite systems are discussed, viz. PEDOT/PSS embedded with tris(8-hydroxyquinolinato)cobalt(III), tris(2,2-bipyridine)cobalt(II), tris(1,10- phenanthroline)cobalt(II) and tris(8-hyd-roxyquinolinato)aluminium(III). Using these composites, electrochemical reduction of nitrite to ammonia with a faradaic efficiency of 61% was reported.

  • 2. Acharya, Shravan
    et al.
    Winther-Jensen, Bjorn
    Spiccia, Leone
    Ohlin, André C.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Rates of water exchange in 2,2'-bipyridine and 1,10-phenanthroline complexes of CoII and MnII2017In: Australian journal of chemistry (Print), ISSN 0004-9425, E-ISSN 1445-0038, Vol. 70, no 6, p. 751-754Article in journal (Refereed)
    Abstract [en]

    The rates and activation parameters of water exchange at pH 3.0 have been determined using variable temperature 17O NMR spectroscopy for four CoII complexes and one MnII complex: [Co(bpy)(H2O)4]2+, [Co(bpy)2 (H2O)2]2+, [Co(phen)-(H2O)4]2+, [Co(phen)2 (H2O)2]2+, and [Mn(bpy)(H2O)4]2+ (bpy = 2,2′-bipyridyl and phen = 1,10-phenanthroline). Substitution of aquo ligands with 1,10-phenanthroline or 2,2′-bipyridyl leads to an increase in the rate of exchange in the manganese complexes, from k298 (1.8 ± 0.1) × 107 s-1 for [Mn(H2O)6]2+ to (7.2 ± 0.3) × 107 s-1 for [Mn(phen)2 (H2O)2]2+, whereas the trends are more complex for the cobalt complexes. We have used the new data in conjunction with literature data for similar complexes to analyse the effect of M–OH2 distance and degree of substitution.

  • 3.
    Adediran, Gbotemi A.
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Liem-Nguyen, Van
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Song, Yu
    Schaefer, Jeffra K.
    Slcyllberg, Ulf
    Björn, Erik
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Microbial Biosynthesis of Thiol Compounds: Implications for Speciation, Cellular Uptake, and Methylation of Hg(II)2019In: Environmental Science and Technology, ISSN 0013-936X, E-ISSN 1520-5851, Vol. 53, no 14, p. 8187-8196Article in journal (Refereed)
    Abstract [en]

    Cellular uptake of inorganic divalent mercury (Hg(II)) is a key step in microbial formation of neurotoxic methylmercury (MeHg), but the mechanisms remain largely unidentified. We show that the iron reducing bacterium Geobacter sulfurreducens produces and exports appreciable amounts of low molecular mass thiol (LMM-RSH) compounds reaching concentrations of about 100 nM in the assay medium. These compounds largely control the chemical speciation and bioavailability of Hg(II) by the formation of Hg(LMM-RS)<INF><INF><INF>2</INF></INF> </INF>complexes (primarily with cysteine) in assays without added thiols. By characterizing these effects, we show that the thermodynamic stability of Hg(II)-complexes is a principal controlling factor for Hg(II) methylation by this bacterium such that less stable complexes with mixed ligation involving LMM-RSH, OH-, and Cl- are methylated at higher rates than the more stable Hg(LMM-RS)<INF>2</INF> complexes. The Hg(II) methylation rate across different Hg(LMM-RS)<INF>2</INF> compounds is also influenced by the chemical structure of the complexes. In contrast to the current perception of microbial uptake of Hg, our results adhere to generalized theories for metal biouptake based on metal complexation with cell surface ligands and refine the mechanistic understanding of Hg(II) availability for microbial methylation.

  • 4.
    Adranno, Brando
    et al.
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden.
    Renier, Olivier
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden.
    Bousrez, Guillaume
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden.
    Paterlini, Veronica
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden.
    Baryshnikov, Glib V.
    Department of Science and Technology, Laboratory of Organic Electronics, Linköping University, SE-60174 Norrköping, Sweden.
    Smetana, Volodymyr
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden.
    Tang, Shi
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Ågren, Hans
    Department of Physics and Astronomy, Uppsala University, Box 516, SE-751 20 Uppsala, Sweden.
    Metlen, Andreas
    The QUILL Research Centre and School of Chemistry and Chemical Engineering The Queen’s University of Belfast Belfast, Northern Ireland BT9 5AG, UK.
    Edman, Ludvig
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Anja-Verena, Mudring
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden; Intelligent Advanced Materials (iAM), Department of Biological and Chemical Engineering and iNANO, Aarhus University, 8000 Aarhus C, Denmark.
    Rogers, Robin D.
    Department of Materials and Environmental Chemistry, Stockholm University, Svante Arrhenius väg 16C, SE-10691 Stockholm, Sweden; The QUILL Research Centre and School of Chemistry and Chemical Engineering The Queen’s University of Belfast Belfast, Northern Ireland BT9 5AG, UK.
    The 8-hydroxyquinolinium cation as a lead structure for efficient color-tunable ionic small molecule emitting materials2023In: Advanced Photonics Research, ISSN 2699-9293, Vol. 4, no 3, article id 2200279Article in journal (Refereed)
    Abstract [en]

    Albeit tris(8-hydroxyquinolinato) aluminum (Alq3) and its derivatives are prominent emitter materials for organic lighting devices, and the optical transitions occur among ligand-centered states, the use of metal-free 8-hydroxyquinoline is impractical as it suffers from strong nonradiative quenching, mainly through fast proton transfer. Herein, it is shown that the problem of rapid proton exchange and vibration quenching of light emission can be overcome not only by complexation, but also by organization of the 8-hydroxyquinolinium cations into a solid rigid network with appropriate counter-anions (here bis(trifluoromethanesulfonyl)imide). The resulting structure is stiffened by secondary bonding interactions such as pi-stacking and hydrogen bonds, which efficiently block rapid proton transfer quenching and reduce vibrational deactivation. Additionally, the optical properties are tuned through methyl substitution from deep blue (455 nm) to blue-green (488 nm). Time-dependent density functional theory (TDFT) calculations reveal the emission to occur from which an unexpectedly long-lived S-1 level, unusual for organic fluorophores. All compounds show comparable, even superior photoluminescence compared to Alq3 and related materials, both as solids and thin films with quantum yields (QYs) up to 40-50%. In addition, all compounds show appreciable thermal stability with decomposition temperatures above 310 °C.

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  • 5.
    Akhtar, Sohel
    et al.
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    Bala, Sukhen
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    De, Avik
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    Das, Krishna Sundar
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    Adhikary, Amit
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    Jyotsna, Shubhra
    Physical & Materials Chemistry Division, CSIR-National Chemical Laboratory, Pune, India.
    Poddar, Pankaj
    Physical & Materials Chemistry Division, CSIR-National Chemical Laboratory, Pune, India.
    Mondal, Raju
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    Designing Multifunctional MOFs Using the Inorganic Motif [Cu33-OH)(μ-Pyz)] as an SBU and Their Properties2018In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 19, no 2, p. 992-1004Article in journal (Refereed)
    Abstract [en]

    In a continuation of our interest in pyrazole-based multifunctional metal–organic frameworks (MOFs), we report herein the construction of a series of Cu(II) MOFs using pyrazole and various 5-substituted isophthalic acids. The central theme is to generate MOFs using the crystal engineering strategy of spacer and node; however, for the node we have introduced a well-known inorganic motif, a [Cu3(μ3-OH)(μ-Pyz)3] unit. The appearance of the SBU in five MOFs confirms the robustness and reproducibility of the motif with some interesting structures of various dimensionality ranging from 1D helical and 2D herringbone grid to a complex 3D framework. The deployment of bent acids brings chirality via helicity in the system, as further confirmed by solid-state CD spectra. A detailed investigation of the porous MOFs reveals their importance as zeolite analogues for environment remediation. MOF-1–MOF-5 show some interesting photodegradation of harmful organic dyes. MOF-4 and MOF-5 show impressive selective CO2 gas sorption properties. Furthermore, magnetic properties associated with the trinuclear and hexanuclear SBUs of MOF-1 and MOF-3–MOF-5 have also been investigated.

  • 6.
    Andersson, Kristoffer
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Selective detection of TNT withmodified SERS-surfaces: Investigation of TNT adsorption and detection using goldand silver nano structured surfaces modified by cysteineand cysteamine2010Independent thesis Advanced level (degree of Master (One Year)), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    In the search for trace amounts of explosives in various environmental samples, the

    analytical procedure is in need of improvements. If it is for national security or for

    environmental purposes the detection of trace amounts of for example 2,4,6-

    trinitrotoluene (TNT) is a costly and time consuming procedure. The use of Raman

    spectrometry for trace amounts detection is one of the research areas that are in the

    advancement and mainly because of the discovery of Surface-Enhanced Raman

    spectroscopy (SERS). Raman spectrometry detects the inelastically scattered light

    from molecules giving a fingerprint spectrum that can be interpreted and species can

    be detected. The inelastically scattering of light only occurs in a small amount of the

    molecules making the signal low and sensitive for interferences. SERS enhances the

    signal from the molecules making it possible to detect very low concentrations. The

    surfaces used in SERS need to be selective for the wanted species to be useful for the

    analysis of environmental samples that often contains a wide variety of compounds.

    This project’s aim was to investigate the possibility of modifying gold- and silvercoated

    SERS surfaces (provided by DTU Nanotech) to get a selective detection of

    trace amounts of TNT in water and air samples.

    The results from the modification indicated some problems with the surfaces. The

    modification molecules were cysteine or cysteamine. The hypothesis was that both of

    them should bind to the surface by sulphur bond. But for cysteine this was not the

    case. The results indicated a binding of the carboxyl group making the use of the

    modification for the selective detection of TNT impossible. The modification by

    cysteamine was more successful but the detection of TNT in water samples was hard

    to get clear results from. The detection of TNT in air samples was carried out by a

    method never tested before using a so-called Linkam cell in conjunction with a TNT

    treated GC-column which together create a controlled environment. The results from

    this experiment were very positive where a clear SERS-signal from TNT could be

    detected.

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  • 7. Andrew, Rhiann E.
    et al.
    Ferdani, Dominic W.
    Ohlin, C. Andre
    Chaplin, Adrian B.
    Coordination Induced Atropisomerism in an NHC-Based Rhodium Macrocycle2015In: Organometallics, ISSN 0276-7333, E-ISSN 1520-6041, Vol. 34, no 5, p. 913-917Article in journal (Refereed)
    Abstract [en]

    Reversible interaction with carbon monoxide results in the onset of dynamic atropisomerism at 298 K in an otherwise static NHC-based rhodium pincer complex, [Rh(C boolean AND N boolean AND C-(CH2)(12))(CO)][BArF4] (1, ArF = 3,5-C6H3(CF3)(2)). The mechanism of this process has been comprehensively interrogated by a combination of variable-temperature NMR spectroscopy, IR spectroscopy, and computational modeling. In addition, a structural analogue of a high-energy symmetrical intermediate species-invoked in the process but not directly observed spectroscopically-has been prepared and characterized in solution and the solid-state.

  • 8. Artemenko, A.
    et al.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Štenclová, P.
    Wågberg, Thomas
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Segervald, Jonas
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Jia, X.
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Kromka, A.
    Reference XPS spectra of amino acids2021Conference paper (Refereed)
    Abstract [en]

    In this report we present XPS data for five amino acids (AAs) (tryptophan, methionine, glutamine, glutamic acid, and arginine) with different side chain groups measured in solid state (powder form). The theoretically and experimentally obtained chemical structure of AAs are compared. Here, we analyse and discuss C 1 s, N 1 s, O 1s and S 2p core level binding energies, FWHMs, atomic concentrations of the functional groups in AAs. The experimentally obtained and theoretically calculated ratio of atomic concentrations are compared. The zwitterionic nature of methionine and glutamine in solid state was determined from protonated amino groups in N 1s peak and deprotonated carboxylic groups in the C 1s spectrum. The obtained XPS results for AAs well correspond with previously reported data.

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  • 9. Aureliano, M.
    et al.
    Ohlin, C. Andre
    Decavanadate in vitro and in vivo effects: facts and opinions2014In: Journal of Inorganic Biochemistry, ISSN 0162-0134, E-ISSN 1873-3344, Vol. 137, p. 123-130Article in journal (Refereed)
    Abstract [en]

    This review covers recent advances in the understanding of the in vitro and in vivo effects of decavanadate, (V10O28)(6-), particularly in mitochondria. In vivo toxicological studies involving vanadium rarely account for the fact that under physiological conditions some vanadium may be present in the form of the decavanadate ion, which may behave differently from ortho- and metavanadates. It has for example been demonstrated that vanadium levels in heart or liver mitochondria are increased upon decavanadate exposure. Additionally, in vitro studies have shown that mitochondrial depolarization (IC50, 40 nM) and oxygen consumption (IC50, 99 nM) are strongly affected by decavanadate, which causes reduction of cytochrome b (complex III). We review these recent findings which together suggest that the observed cellular targets, metabolic pathway and toxicological effects differ according to the species of vanadium present. Finally, the toxicological effects of decavanadate depend on several factors such as the mode of administration, exposure time and type of tissue. (C) 2014 Elsevier Inc. All rights reserved.

  • 10. Aureliano, Manuel
    et al.
    Fraqueza, Gil
    Ohlin, C. Andre
    Ion pumps as biological targets for decavanadate2013In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 42, no 33, p. 11770-11777Article in journal (Refereed)
    Abstract [en]

    The putative applications of poly-, oligo-and mono-oxometalates in biochemistry, biology, pharmacology and medicine are rapidly attracting interest. In particular, these compounds may act as potent ion pump inhibitors and have the potential to play a role in the treatment of e. g. ulcers, cancer and ischemic heart disease. However, the mechanism of action is not completely understood in most cases, and even remains largely unknown in other cases. In the present review we discuss the most recent insights into the interaction between mono-and polyoxometalate ions with ion pumps, with particular focus on the interaction of decavanadate with Ca2+-ATPase. We also compare the proposed mode of action with those of established ion pump inhibitors which are currently in therapeutic use. Of the 18 classes of compounds which are known to act as ion pump inhibitors, the complete mechanism of inhibition is only known for a handful. It has, however, been established that most ion pump inhibitors bind mainly to the E2 ion pump conformation within the membrane domain from the extracellular side and block the cation release. Polyoxometalates such as decavanadate, in contrast, interact with Ca2+-ATPase near the nucleotide binding site domain or at a pocket involving several cytoplasmic domains, and therefore need to cross through the membrane bilayer. In contrast to monomeric vanadate, which only binds to the E2 conformation, decavanadate binds to all protein conformations, i.e. E1, E1P, E2 and E2P. Moreover, the specific interaction of decavanadate with sarcoplasmic reticulum Ca2+-ATPase has been shown to be non-competitive with respect to ATP and induces protein cysteine oxidation with concomitant vanadium reduction which might explain the high inhibitory capacity of V-10 (IC50 = 15 mu M) which is quite similar to the majority of the established therapeutic drugs.

  • 11. Aureliano, Manuel
    et al.
    Ohlin, C. André
    Vieira, Michele O.
    Marques, M. Paula M.
    Casey, William H.
    Batista de Carvalho, Luis A. E.
    Characterization of decavanadate and decaniobate solutions by Raman spectroscopy2016In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 45, no 17, p. 7391-7399Article in journal (Refereed)
    Abstract [en]

    The decaniobate ion, (Nb-10 = [Nb10O28](6-)) being isoelectronic and isostructural with the decavanadate ion (V-10 = [V10O28](6-)), but chemically and electrochemically more inert, has been useful in advancing the understanding of V-10 toxicology and pharmacological activities. In the present study, the solution chemistry of Nb-10 and V-10 between pH 4 and 12 is studied by Raman spectroscopy. The Raman spectra of V-10 show that this vanadate species dominates up to pH 6.45 whereas it remains detectable until pH 8.59, which is an important range for biochemistry. Similarly, Nb-10 is present between pH 5.49 and 9.90 and this species remains detectable in solution up to pH 10.80. V-10 dissociates at most pH values into smaller tetrahedral vanadate oligomers such as V-1 and V-2, whereas Nb-10 dissociates into Nb-6 under mildly (10 > pH > 7.6) or highly alkaline conditions. Solutions of V-10 and Nb-10 are both kinetically stable under basic pH conditions for at least two weeks and at moderate temperature. The Raman method provides a means of establishing speciation in the difficult niobate system and these findings have important consequences for toxicology activities and pharmacological applications of vanadate and niobate polyoxometalates.

  • 12.
    Backman, Rainer
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    MALIbase: Termodynamisk data för föreningar i systemet CaO-K2O-P2O52015Other (Other (popular science, discussion, etc.))
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  • 13.
    Bala, Sukhen
    et al.
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, India; Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry, Sun Yat-Sen University, Guangzhou, P. R. China.
    De, Avik
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, India.
    Adhikary, Amit
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, West Bengal, India.
    Saha, Sayan
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, India.
    Akhtar, Sohel
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, India.
    Das, Krishna Sundar
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, India.
    Tong, Ming-Liang
    Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry, Sun Yat-Sen University, Guangzhou, P. R. China.
    Mondal, Raju
    School of Chemical Science, Indian Association for the Cultivation of Science, Kolkata, India.
    Influence of Semirigidity and Diverse Binding Modes of an Asymmetric Pyridine-pyrazole Based Bis-Chelating Ligand in Controlling Molecular Architectures and Their Properties2020In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 20, no 9, p. 5698-5708Article in journal (Refereed)
  • 14. Barišić, Antun
    et al.
    Lützenkirchen, Johannes
    Bebić, Nikol
    Li, Qinzhi
    Hanna, Khalil
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Begović, Tajana
    Experimental Data Contributing to the Elusive Surface Charge of Inert Materials in Contact with Aqueous Media2021In: Colloids and interfaces, E-ISSN 2504-5377, Vol. 5, no 1, article id 6Article in journal (Other academic)
    Abstract [en]

    We studied the charging of inert surfaces (polytetrafluoroethylene, i.e., PTFE; graphite; graphene; and hydrophobic silica) using classical colloid chemistry approaches. Potentiometric titrations showed that these surfaces acquired less charge from proton-related reactions than oxide minerals. The data from batch-type titrations for PTFE powder did not show an effect of ionic strength, which was also in contrast with results for classical colloids. In agreement with classical colloids, the electrokinetic results for inert surfaces showed the typical salt level dependence. In some cases, the point of zero net proton charge as determined from mass and tentatively from acid&ndash;base titration differed from isoelectric points, which has also been previously observed, for example by Chibowski and co-workers for ice electrolyte interfaces. Finally, we found no evidence for surface contaminations of our PTFE particles before and after immersion in aqueous solutions. Only in the presence of NaCl-containing solutions did cryo-XPS detect oxygen from water. We believe that our low isoelectric points for PTFE were not due to impurities. Moreover, the measured buffering at pH 3 could not be explained by sub-micromolar concentrations of contaminants. The most comprehensive explanation for the various sets of data is that hydroxide ion accumulation occurred at the interfaces between inert surfaces and aqueous solutions.

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  • 15. Behravesh, Erfan
    et al.
    Kumar, Narendra
    Balme, Quentin
    Roine, Jorma
    Salonen, Jarno
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Process Chemistry Centre, Åbo Akademi University, FI-20500 Turku/Åbo, Finland.
    Peurla, Markus
    Aho, Atte
    Eränen, Kari
    Murzin, Dmitry Yu.
    Salmi, Tapio
    Synthesis and characterization of Au nano particles supported catalysts for partial oxidation of ethanol: Influence of solution pH, Au nanoparticle size, support structure and acidity2017In: Journal of Catalysis, ISSN 0021-9517, E-ISSN 1090-2694, Vol. 353, p. 223-238Article in journal (Refereed)
    Abstract [en]

    Partial oxidation of ethanol to acetaldehyde was carried out over gold catalysts supported on various oxides and zeolites by deposition precipitation. The special focus of this work was on the influence of H-Y zeolite surface charge on Au cluster size and loading linking it to activity and selectivity in ethanol oxidation and comparing with other studied catalysts. The catalysts were characterized by nitrogen physisorption, transmission electron microscopy (TEM), scanning electron microscopy/energy dispersive X-ray analysis (SEM/EDXA), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and zeta potential measurements. pH of the solution governed the Au NPs size within the range of 5.8–13.2 nm with less negatively charged surfaces leading to formation of smaller clusters. Au loading on H-Y zeolite with silica to alumina ratio of 80 was increased by raising the pH. In fact, H-Y-12 and H-Beta-25 were selective towards diethyl ether while acetaldehyde was the prevalent product on less acidic H-Y-80. The results demonstrated strong dependency of the catalytic activity on the Au cluster size. Namely turn over frequency (TOF) decreased with an increase in metal size from 6.3 to 9.3 nm on H-Y-80. Selectivity towards acetaldehyde and ethyl acetate did not change significantly on H-Y-80 within 6.3–9.3 nm Au particle size range. On Al2O3 support, however, selectivity towards acetaldehyde increased considerably upon diminishing Au average particle size from 3.7 to 2.1 nm.

  • 16.
    Bertrand, Sebastien
    et al.
    Renard Centre of Marine Geology, Ghent University, Gent, Belgium; GEOPS, Paris-Saclay University, Orsay, France.
    Tjallingii, Rik
    Section Climate Dynamics and Landscape Evolution, GFZ German Research Centre for Geosciences, Potsdam, Germany.
    Kylander, Malin E.
    Department of Geological Sciences and the Bolin Centre for Climate Research, Stockholm University, Sweden.
    Wilhelm, Bruno
    Université Grenoble Alpes, Grenoble, France.
    Roberts, Stephen J.
    British Antarctic Survey, Cambridge, United Kingdom.
    Arnaud, Fabien
    EDYTEM, Université Savoie Mont Blanc, Le Bourget du Lac, France.
    Brown, Erik
    University of Minnesota Duluth, Duluth, United States.
    Bindler, Richard
    Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences.
    Inorganic geochemistry of lake sediments: a review of analytical techniques and guidelines for data interpretation2024In: Earth-Science Reviews, ISSN 0012-8252, E-ISSN 1872-6828, Vol. 249, article id 104639Article, review/survey (Refereed)
    Abstract [en]

    Inorganic geochemistry is a powerful tool in paleolimnology. It has become one of the most commonly used techniques to analyze lake sediments, particularly due to the development and increasing availability of XRF core scanners during the last two decades. It allows for the reconstruction of the continuous processes that occur in lakes and their watersheds, and it is ideally suited to identify event deposits. How earth surface processes and limnological conditions are recorded in the inorganic geochemical composition of lake sediments is, however, relatively complex. Here, we review the main techniques used for the inorganic geochemical analysis of lake sediments and we offer guidance on sample preparation and instrument selection. We then summarize the best practices to process and interpret bulk inorganic geochemical data. In particular, we emphasize that log-ratio transformation is critical for the rigorous statistical analysis of geochemical datasets, whether they are obtained by XRF core scanning or more traditional techniques. In addition, we show that accurately interpreting inorganic geochemical data requires a sound understanding of the main components of the sediment (organic matter, biogenic silica, carbonates, lithogenic particles) and mineral assemblages. Finally, we provide a series of examples illustrating the potential and limits of inorganic geochemistry in paleolimnology. Although the examples presented in this paper focus on lake and fjord sediments, the principles presented here also apply to other sedimentary environments.

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  • 17.
    Björnberg, Arne
    Umeå University, Faculty of Science and Technology.
    Crystal structure studies of a new series of molybdovanadate polyanions and some related vanadates1980Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    The determination of complexes formed in weakly acidic aqueous solutions containing pentavalent vanadium as well as hexavalent molybdenum has proved diffi cui t due to slow equilibria and 1 imi ted sol ubi 1 i ty of especially the vanadium species. The formation of several different polynuclear complexes with a very varied molybdenum/vanadium ratio also complicates the interpretation of Potentiometrie data. In order to clarify the picture of complexes formed and provide starting points for equilibrium calculations single-crystal X-ray studies were made on crystals obtained from âqueous solutions. In addition, these studies can provide information on bonding conditions and possibly formation mechanisms for molybdovanadate polyanions. Crystals were synthesized by slow evaporation of aqueous solutions. Solutions with varied molybdenum/vanadium ratios and also varied pH values were prepared and used in the synthesis experiments. The X-ray measurements were performed with Philips PAILRED, Syntex P21 and Syntex R3 automatic diffractometers. All data sets were corrected for absorption. Five of the structures were solved with heavy-atom methods and one by direct methods. The structures were refined by computer-performed least-squares methods. The following crystals were obtained and structurally determined: NaV03•1.89H2O, which contains chains of VO5 trigonal bipyramids. Na4V2O7 (H2O)18 , containing discrete V2O74- anions which are completely surrounded by sodium-coordinated water molecules. Discrete molybdovanadate polyanions were found in the structures of the compounds Na6Mo6\/2O26 (H2O)16 , K7Mo8V5O40 • 8H2O, K8Mo4,V8O36 - 12H20 and K6 (V2 , Mo10) VO40 • 13H20. The last substance belongs to a class of compounds named 'heteropoly blues', which contain metal atoms in mixed-valence states, and has one unpaired electron on the polyanion. This compound was also investigated with electron spin resonance spectroscopy. The bonding configurations of oxygen atoms coordinated to molybdenum or vanadium are described and discussed. As the Mo4V8O368-, Mo8V5O407- (which is an isomer of the Keggin anion but has a quite different structure) and Mo6V2O266- anions all contain remnants of mononuclear molybdate and vanadate anions, it seems likely that these polyanions are formed mainly through the condensation of mononuclear species.An electrostatic model for the simulation of bond distances in polyions, starting with perfectly regular idealized models, is presented.

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    Crystal structure studies of a new series of molybdovanadate polyanions and some related vanadates
  • 18.
    Boily, Jean-Francois
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kozin, Philipp A.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Particle Morphological and Roughness Controls on Mineral Surface Charge Development2014In: Geochimica et Cosmochimica Acta, ISSN 0016-7037, E-ISSN 1872-9533, Vol. 141, no 15 September, p. 567-578Article in journal (Other academic)
    Abstract [en]

    Effects of mineral particle morphology and roughness on potential determining ion (p.d.i.; H+, OH) loadings achieved at synthetic lepidocrocite (γ-FeOOH) surfaces were predominantly investigated by potentiometry and thermodynamic modeling. Nanosized rod- (RL) and lath-shaped (LL) particles exhibiting different proportions of the same predominant crystallographic faces acquired largely comparable pH, ionic strength and counterion (NaCl, NaClO4) dependencies on p.d.i. loadings. These results supported previous claims that faces ideally containing proton silent sites only, are likely populated by additional proton active sites. This concept was supported further by results of roughened LL-like particles (LLR) also showing highly congruent pH-, ionic strength- and composition-dependent p.d.i. loadings with those of LL and RL. These loadings thereby correspond to maximal levels allowed by net attractive and repulsive forces at each solution composition, irrespective of particle morphology. Contrasting equilibration times required to achieve these loadings revealed considerably slower exchange of p.d.i. and electrolyte ions near the point of zero charge in the rough LLR than in the more idealized LL and RL particles.

    Thermodynamic modeling was used to test various concepts accounting for these results. The model made use of a novel framework capable of isolating electrostatic contributions from different faces, and of accounting for ion-specific double-layer properties within a single crystallographic face. These efforts made use of capacitance values for each electrolyte ions within the framework of a recently developed Variable Capacitance Model. Attempts at modeling all three particle types were used to suggest that the (0 1 0) face contains ∼0.9 site nm−2 of proton active sites, a value notably constrained by recently published Na+, Cl, and ClO4 loadings derived by cryogenic X-ray photoelectron spectroscopy. The model presented in this work thus provides a means to predict p.d.i. loadings on multifaceted mineral particle surfaces, and can therefore be used to constrain further our understanding of mineral/water interface reactivity.

  • 19.
    Boily, Jean-François
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ilton, Eugene S.
    An independent confirmation of the correlation of Uf4 primary peaks and satellite structures of UVI, UV and UIV in mixed valence uranium oxides by two-dimensional correlation spectroscopy2008In: Surface Science, ISSN 0039-6028, E-ISSN 1879-2758, Vol. 602, no 24, p. 3637-46Article in journal (Refereed)
    Abstract [en]

    Two-dimensional (2D) correlation spectroscopy was used to resolve the positions and correlations among U4f primary peaks and satellite structures of UIV, UV and UVI components on a dry mica surface. These different species resulted from the reduction of UVI, initially sorbed/precipitated from solution, upon exposure to a high flux of monochromatic Al Kα X-rays during X-ray photoelectron spectroscopy. Synchronous and asynchronous 2D maps of these results are consistent with previous assignments to UIV, UV and UVI components of the solid. The synchronous spectra confirmed the negative correlation between UVI and UIV components and the asynchronous spectra confirmed the role of UV as a reactive intermediate in the reduction reaction of UVI to UIV. Simulations of 2D correlation maps using synthetic spectra of the primary peaks showed that the presence of highly overlapped peaks centered within 2 eV of each other cannot be distinguished without the presence of additional cross-peaks. The maps have therefore confirmed the existence of three dominant oxidation states, and identified positions of UIV, UV and UVI U4f primary peaks and satellite structures that are consistent with previous peak-fitting efforts. Satellite structures also showed out-of-phase correlations among the different oxidation states, further confirming their use as reliable indicators of oxidation state.

  • 20. Boniolo, Manuel
    et al.
    Chernev, Petko
    Cheah, Mun Hon
    Heizmann, Philipp A.
    Huang, Ping
    Shylin, Sergii, I
    Salhi, Nessima
    Hossain, Md Kamal
    Gupta, Arvind K.
    Messinger, Johannes
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Molecular Biomimetics, Department of Chemistry – Ångström Laboratory, Uppsala University, Sweden.
    Thapper, Anders
    Lundberg, Marcus
    Electronic and geometric structure effects on one-electron oxidation of first-row transition metals in the same ligand framework2021In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 50, no 2, p. 660-674Article in journal (Refereed)
    Abstract [en]

    Developing new transition metal catalysts requires understanding of how both metal and ligand properties determine reactivity. Since metal complexes bearing ligands of the Py5 family (2,6-bis-[(2-pyridyl)methyl] pyridine) have been employed in many fields in the past 20 years, we set out here to understand their redox properties by studying a series of base metal ions (M = Mn, Fe, Co, and Ni) within the Py5OH (pyridine-2,6-diylbis[di-(pyridin-2-yl)methanol]) variant. Both reduced (M-II) and the one-electron oxidized (M-III) species were carefully characterized using a combination of X-ray crystallography, X-ray absorption spectroscopy, cyclic voltammetry, and density-functional theory calculations. The observed metal-ligand interactions and electrochemical properties do not always follow consistent trends along the periodic table. We demonstrate that this observation cannot be explained by only considering orbital and geometric relaxation, and that spin multiplicity changes needed to be included into the DFT calculations to reproduce and understand these trends. In addition, exchange reactions of the sixth ligand coordinated to the metal, were analysed. Finally, by including published data of the extensively characterised Py5OMe (pyridine-2,6-diylbis[di-(pyridin-2-yl)methoxymethane])complexes, the special characteristics of the less common Py5OH ligand were extracted. This comparison highlights the non-innocent effect of the distal OH functionalization on the geometry, and consequently on the electronic structure of the metal complexes. Together, this gives a complete analysis of metal and ligand degrees of freedom for these base metal complexes, while also providing general insights into how to control electrochemical processes of transition metal complexes.

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  • 21.
    Boniolo, Manuel
    et al.
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Hossain, Md Kamal
    Synthetic Molecular Chemistry, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Chernev, Petko
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Suremann, Nina F.
    Synthetic Molecular Chemistry, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Heizmann, Philipp A.
    Synthetic Molecular Chemistry, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Lyvik, Amanda S.L.
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Beyer, Paul
    Physics Department, Freie Universität Berlin, Berlin, Germany.
    Haumann, Michael
    Physics Department, Freie Universität Berlin, Berlin, Germany.
    Huang, Ping
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Salhi, Nessima
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Cheah, Mun Hon
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Shylin, Sergii I.
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Lundberg, Marcus
    Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Thapper, Anders
    Synthetic Molecular Chemistry, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Messinger, Johannes
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Molecular Biomimetics, Department of Chemistry, Ångström Laboratory, Uppsala University, Uppsala, Sweden.
    Water Oxidation by Pentapyridyl Base Metal Complexes? A Case Study2022In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 61, no 24, p. 9104-9118Article in journal (Refereed)
    Abstract [en]

    The design of molecular water oxidation catalysts (WOCs) requires a rational approach that considers the intermediate steps of the catalytic cycle, including water binding, deprotonation, storage of oxidizing equivalents, O-O bond formation, and O2 release. We investigated several of these properties for a series of base metal complexes (M = Mn, Fe, Co, Ni) bearing two variants of a pentapyridyl ligand framework, of which some were reported previously to be active WOCs. We found that only [Fe(Py5OMe)Cl]+ (Py5OMe = pyridine-2,6-diylbis[di-(pyridin-2-yl)methoxymethane]) showed an appreciable catalytic activity with a turnover number (TON) = 130 in light-driven experiments using the [Ru(bpy)3]2+/S2O82- system at pH 8.0, but that activity is demonstrated to arise from the rapid degradation in the buffered solution leading to the formation of catalytically active amorphous iron oxide/hydroxide (FeOOH), which subsequently lost the catalytic activity by forming more extensive and structured FeOOH species. The detailed analysis of the redox and water-binding properties employing electrochemistry, X-ray absorption spectroscopy (XAS), UV-vis spectroscopy, and density-functional theory (DFT) showed that all complexes were able to undergo the MIII/MII oxidation, but none was able to yield a detectable amount of a MIV state in our potential window (up to +2 V vs SHE). This inability was traced to (i) the preference for binding Cl- or acetonitrile instead of water-derived species in the apical position, which excludes redox leveling via proton coupled electron transfer, and (ii) the lack of sigma donor ligands that would stabilize oxidation states beyond MIII. On that basis, design features for next-generation molecular WOCs are suggested.

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  • 22.
    Boström, Dan
    et al.
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Broström, Markus
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Skoglund, Nils
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Boman, Christoffer
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Backman, Rainer
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Öhman, Marcus
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Engineering.
    Grimm, Alejandro
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Engineering.
    Ash transformation chemistry during energy conversion of biomass2010In: Impacts of Fuel Quality on Power Production & Environment: 29/08/2010 - 03/09/2010, Impacts of Fuel Quality , 2010Conference paper (Refereed)
    Abstract [en]

    There is relatively extensive knowledge available concerning ash transformation reactions during energy conversion of woody biomass. Traditionally, these assortments have constituted the main resources for heating in Sweden. In recent decades the utilization of these energy carriers has increased, from a low technology residential small scale level to industrial scale (e.g. CHP plants). Along this evolution ash-chemical related phenomena for woody biomass has been observed and studied. So, presently the understanding for these are, if not complete, fairly good. Briefly, from a chemical point of view the ash from woody biomass could be characterized as a silicate dominated systems with varying content of basic oxides and with relatively high degree of volatilization of alkali sulfates and chlorides. Thus, the main ash transformation mechanisms in these systems have been outlined. Here, an attempt to give a general description of the ash transformation reactions of biomass fuels is presented, with the intention to provide guidance in the understanding of ash matter behavior in the utilization of any biomass fuel, primarily from knowledge of the concentrations of ash forming elements but also by considering the physical condition in the specific combustion appliance and the physical characteristic of the biomass fuel. Furthermore, since the demand for CO2-neutral energy resources has increased the last years and will continue to do so in the foreseeable future, other biomasses as for instance agricultural crops has become highly interesting. Globally, the availability of these shows large variation. In Sweden, for instance, which is a relatively spare populated country with large forests, these bio-masses will play a secondary role, although not insignificant. In other parts of the world, more densely populated and with a large agricultural sector, such bio-masses may constitute the main energy bio-mass resource in the future. However, the content of ash forming matter in agricultural bio-mass is rather different in comparison to woody biomass. Firstly, the content is much higher; from being about 0.3 – 0.5% (wt) in stem wood, it can amount to between 2 and 10 %(wt) in agricultural biomass. In addition, the composition of the ash forming matter is different. Shortly, the main difference is due to a much higher content of phosphorus (occasionally also silicon) which has major consequences on the ash-transformation reactions. In many crops, the concentration of phosphorus and silicon is equivalent, which (depending on the concentration levels of basic oxides) may result in a phosphate dominated ash. The properties of this ash are in several aspects different from the silicate dominated woody biomass ash and will consequently behave differently in various types of energy conversion systems. The knowledge about phosphate dominated ash systems has so far been scarce. We have been working with these systems, both with basic and applied research, for about a decade know. Some general experiences and conclusions as well as some specific examples of our research will be presented.

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  • 23.
    Boulanger, Nicolas
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Nano-Engineered Materials and Organic Electronics Laboratory.
    Yu, Victor
    Hilke, Michael
    Toney, Michael F.
    Barbero, David R.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Nano-Engineered Materials and Organic Electronics Laboratory.
    In situ probing of the crystallization kinetics of rr-P3HT on single layer graphene as a function of temperature2017In: Physical Chemistry, Chemical Physics - PCCP, ISSN 1463-9076, E-ISSN 1463-9084, Vol. 19, no 12, p. 8496-8503Article in journal (Refereed)
    Abstract [en]

    We studied the molecular packing and crystallization of a highly regio-regular semiconducting polymer poly(3-hexylthiophene) (P3HT) on both single layer graphene and silicon as a function of temperature, during cooling from the melt. The onset of crystallization, crystallites' size, orientation, and kinetics of formation were measured in situ by synchrotron grazing incidence X-ray diffraction (GIXD) during cooling and revealed a very different crystallization process on each surface. A favored crystalline orientation with out of plane pi-pi stacking formed at a temperature of 200 degrees C on graphene, whereas the first crystallites formed with an edge-on orientation at 185 degrees C on silicon. The crystallization of face-on lamellae revealed two surprising effects during cooling: (a) a constant low value of the pi-pi spacing below 60 degrees C; and (b) a reduction by half in the coherence length of face-on lamellae from 100 to 30 degrees C, which corresponded with the weakening of the 2nd or 3rd order of the in-plane (k00) diffraction peak. The final ratio of face-on to edge-on orientations was 40% on graphene, and 2% on silicon, revealing the very different crystallization mechanisms. These results provide a better understanding of how surfaces with different chemistries and intermolecular interactions with the polythiophene polymer chains lead to different crystallization processes and crystallites orientations for specific electronic applications.

  • 24. Bányai, István
    et al.
    Conte, Valeria
    Pettersson, Lage
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Silvagni, Adriano
    On the Nature of VV Species in Hydrophilic Ionic Liquids: A Spectroscopic Approach2008In: European Journal of Inorganic Chemistry, ISSN 1434-1948, E-ISSN 1099-1948, no 34, p. 5373-81Article in journal (Refereed)
    Abstract [en]

    Heteronuclear NMR experiments, in particular 51V, wereperformed with the aim to elucidate the nature of vanadates and peroxovanadates in hydrophilic ionic liquids (i.e., [bmim][BF4], [bmim][TfO] and [bdmim][BF4]). The data so far reported clearly indicate that ionic liquids have a strong influence on the solution chemistry of vanadate in water both for the formation of the aggregates (with and without H2O2) and for the rate of peroxide consumption catalyzed by vanadium. In BF4- containing ionic liquids, formation of vanadate-fluoride adducts is suggested. The obtained results are also discussed in the light of the reactivity data of peroxovanadates in ionic liquids.

  • 25. Carlsson, Per
    et al.
    Ma, Charlie
    Luleå University of Technology, Energy Engineering, Division of Energy Science, SE-971 87, Luleå, Sweden.
    Molinder, Roger
    Weiland, Fredrik
    Wiinikka, Henrik
    Öhman, Marcus
    Öhrman, Olov
    Slag Formation During Oxygen Blown Entrained-Flow Gasification of Stem Wood2014In: Energy & Fuels, ISSN 0887-0624, E-ISSN 1520-5029, Vol. 28, no 11, p. 6941-6952Article in journal (Refereed)
    Abstract [en]

    Stem wood powders were fired in a mullite-lined pilot-scale oxygen-blown pressurized entrained-flow gasifier. During repeated campaigns involving increases in fuel load and process temperature, slag formations that eventuated in the blockage of the gasifier outlet were observed. These slags were retrieved for visual and chemical characterization. It was found that the slags had very high contents of Al and, in particular, high Al/Si ratios that suggest likely dissolution of the mullite-based refractory of the gasifier lining due to interactions with the fuel ash. Possible causes for the slag formation and behavior are proposed, and practical implications for the design of future stem wood entrained-flow gasifiers are also discussed

  • 26. Carvalho, Paulo H. B. Brant
    et al.
    Mace, Amber
    Andersson, Ove
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Tulk, Chris A.
    Molaison, Jamie
    Haussermann, Ulrich
    Elucidating the guest disorder in structure II argon hydrate: A neutron diffraction isotopic substitution study2020In: Journal of Solid State Chemistry, ISSN 0022-4596, E-ISSN 1095-726X, Vol. 285, article id 121220Article in journal (Refereed)
    Abstract [en]

    Clathrate hydrates with the cubic structure II (CS-II) form typically with large guest molecules, such as tetrahydrofuran, trimethylamine oxide, or propane. However, CS-II is also realized for argon hydrate despite the comparatively small van der Waals diameter of the guest (around 3.8 angstrom). Here, the structure of deuterated argon hydrate was studied at ambient pressure in the temperature range 20-95 K using neutron diffraction and comparing natural Ar with Ar-36, which scatters neutrons more than 13 times more efficiently. The procedure allowed to unambiguously establish the positional disorder within the large cages of CS-H, while simultaneously refining host and guest structures. These cages are singly occupied and off-centered argon atoms distribute on two tetrahedron-shaped split positions with a ratio 3:1. Molecular dynamics (MD) simulations revealed that the crystallographic positional disorder structure is due to mobile argon atoms even at 20 K. The MD potential energy distribution confirmed the diffraction model. It is noted that the unit cell volumes of argon hydrate in the investigated temperature range are virtually identical to N-2 hydrate, which has a similar composition at ambient pressure, indicating a very similar (slightly attractive) host-guest interaction.

  • 27.
    Cheng, Wei
    et al.
    College of Resources and Environmental Science, South-Central Minzu University, Wuhan, China.
    Li, Jiabin
    College of Resources and Environmental Science, South-Central Minzu University, Wuhan, China.
    Sun, Jie
    College of Resources and Environmental Science, South-Central Minzu University, Wuhan, China.
    Luo, Tao
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Université de Rennes, Ecole Nationale Supérieure de Chimie de Rennes, CNRS, ISCR-UMR 6226, Rennes, France.
    Marsac, Rémi
    Université de Rennes, CNRS, Géosciences Rennes─UMR 6118, Rennes, France.
    Boily, Jean-Francois
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Hanna, Khalil
    Université de Rennes, Ecole Nationale Supérieure de Chimie de Rennes, CNRS, ISCR-UMR 6226, Rennes, France.
    Nalidixic acid and Fe(II)/Cu(II) coadsorption at Goethite and Akaganéite surfaces2023In: Environmental Science and Technology, ISSN 0013-936X, E-ISSN 1520-5851, Vol. 57, no 41, p. 15680-15692Article in journal (Refereed)
    Abstract [en]

    Interactions between aqueous Fe(II) and solid Fe(III) oxy(hydr)oxide surfaces play determining roles in the fate of organic contaminants in nature. In this study, the adsorption of nalidixic acid (NA), a representative redox-inactive quinolone antibiotic, on synthetic goethite (α-FeOOH) and akaganéite (β-FeOOH) was examined under varying conditions of pH and cation type and concentration, by means of adsorption experiments, attenuated total reflectance-Fourier transform infrared spectroscopy, surface complexation modeling (SCM), and powder X-ray diffraction. Batch adsorption experiments showed that Fe(II) had marginal effects on NA adsorption onto akaganéite but enhanced NA adsorption on goethite. This enhancement is attributed to the formation of goethite-Fe(II)-NA ternary complexes, without the need for heterogeneous Fe(II)-Fe(III) electron transfer at low Fe(II) loadings (2 Fe/nm2), as confirmed by SCM. However, higher Fe(II) loadings required a goethite-magnetite composite in the SCM to explain Fe(II)-driven recrystallization and its impact on NA binding. The use of a surface ternary complex by SCM was supported further in experiments involving Cu(II), a prevalent environmental metal incapable of transforming Fe(III) oxy(hydr)oxides, which was observed to enhance NA loadings on goethite. However, Cu(II)-NA aqueous complexation and potential Cu(OH)2 precipitates counteracted the formation of ternary surface complexes, leading to decreased NA loadings on akaganéite. These results have direct implications for the fate of organic contaminants, especially those at oxic-anoxic boundaries.

  • 28.
    Chorell, Erik
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Bengtsson, Christoffer
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Sainte-Luce Banchelin, Thomas
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Das, Pralay
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Uvell, Hanna
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Sinha, Arun K
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Pinkner, Jerome S
    Department of Molecular Microbiology, Washington University, School of Medicine, St. Louis, Missouri 63110, USA.
    Hultgren, Scott J
    Department of Molecular Microbiology, Washington University, School of Medicine, St. Louis, Missouri 63110, USA.
    Almqvist, Fredrik
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Synthesis and application of a bromomethyl substituted scaffold to be used for efficient optimization of anti-virulence activity2011In: European Journal of Medicinal Chemistry, ISSN 0223-5234, E-ISSN 1768-3254, Vol. 46, no 4, p. 1103-1116Article in journal (Refereed)
    Abstract [en]

    Pilicides are a class of compounds that attenuate virulence in Gram negative bacteria by blocking the chaperone/usher pathway in Escherichia coli. It has also been shown that compounds derived from the peptidomimetic scaffold that the pilicides are based on can prevent both Aβ aggregation and curli formation. To facilitate optimizations towards the different targets, a new synthetic platform has been developed that enables fast and simple introduction of various substituents in position C-7 on the peptidomimetic scaffold. Importantly, this strategy also enables introduction of previously unattainable heteroatoms in this position. Pivotal to the synthetic strategy is the synthesis of a C-7 bromomethyl substituted derivative of the ring-fused dihydrothiazolo 2-pyridone pilicide scaffold. From this versatile and reactive intermediate various heteroatom-linked substituents could be introduced on the scaffold including amines, ethers, amides and sulfonamides. In addition, carbon-carbon bonds could be introduced to the sp(3)-hybridized bromomethyl substituted scaffold by Suzuki-Miyaura cross couplings. Evaluation of the 24 C-7 substituted compounds in whole-bacterial assays provided important structure-activity data and resulted in the identification of a number of new pilicides with activity as good or better than those developed previously.

  • 29.
    Das, Krishna Sundar
    et al.
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, India.
    Pal, Baishakhi
    Department of Physics, Jadavpur University, Jadavpur, Kolkata, India.
    Saha, Sayan
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, India.
    Akhtar, Sohel
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, India.
    De, Avik
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, India.
    Ray, Partha Pratim
    Department of Physics, Jadavpur University, Jadavpur, Kolkata, India.
    Mondal, Raju
    School of Chemical Sciences, Indian Association for the Cultivation of Science, Kolkata, India.
    Utilization of counter anions for charge transportation in the electrical device fabrication of Zn(ii) metal–organic frameworks2020In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 49, no 46, p. 17005-17016Article in journal (Refereed)
    Abstract [en]

    The present work reports the fabrication of anion-induced electrical devices with Zn(II) metal–organic frameworks. The essence of our electronic device fabrication is to utilize the anionic species entrapped inside of the three-dimensional network of the MOFs for charge transportation. The idea is to generate MOFs as a host–guest system with encapsulated anions or anion–solvent clusters as guests and a cationic yet insulating three-dimensional framework as the host. Accordingly, we have synthesized two Zn(II) MOFs using a neutral bispyrazole-based ligand, which results in a cationic chassis with substantial void space and porous channels inside the network. For both MOFs, the porous channels are occupied by infinitely hydrogen bonded networks of anions and anion–solvent clusters. This provides an excellent platform for anionic species-induced charge transportation and improved electrical conductivity. Indeed, the impedance spectroscopy data and current density–voltage (J–V) characteristics of the fabricated electrical devices further vindicate our idea. The current–voltage measurements clearly indicate the usefulness of modified host–guest-type MOFs for electronic device fabrication with corroborating conductivity values of 8.71 × 10−5 S m−1 and 5.79 × 10−4 S m−1 for compound 1 and compound 2, respectively.

  • 30.
    De, Avik
    et al.
    School of Chemical Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Bala, Sukhen
    Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education;School of Chemistry;Sun Yat-Sen University;Guangzhou 510275;P. R. China.
    Saha, Sayan
    School of Chemical Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Das, Krishna Sundar
    School of Chemical Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Akhtar, Sohel
    School of Chemical Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Adhikary, Amit
    School of Chemical Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Ghosh, Arijit
    Laboratory of Molecular Biology;School of Biological Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Huang, Guo-Zhang
    Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education;School of Chemistry;Sun Yat-Sen University;Guangzhou 510275;P. R. China.
    Chowdhuri, Srijita Paul
    Laboratory of Molecular Biology;School of Biological Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Das, Benu Brata
    Laboratory of Molecular Biology;School of Biological Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Tong, Ming-Liang
    Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education;School of Chemistry;Sun Yat-Sen University;Guangzhou 510275;P. R. China.
    Mondal, Raju
    School of Chemical Sciences;Indian Association for the Cultivation of Science;Kolkata 700032;India.
    Lanthanide clusters of phenanthroline containing a pyridine–pyrazole based ligand: magnetism and cell imaging2021In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 50, no 10, p. 3593-3609Article in journal (Refereed)
    Abstract [en]

    In this contribution, we report the synthesis, characterization and luminescence-magnetic properties of Ln-clusters (Ln = Gd3+, Eu3+and Tb3+) using a new pyridine-pyrazole functionalized ligand fitted with a chromophoric phenanthroline backbone. The unorthodox N-rich ligand forms isostructural trinuclear lanthanide complexes with a topology that closely resembles two interdigitating hairpins. The clusters crystallize in chiral space groups and also exhibit chirality for bulk samples, which were further confirmed using solid state CD spectra. Magnetic studies on the complexes reveal their interesting features while the Gd cluster shows a significant cryogenic magnetic cooling behaviour with a moderately high magnetic entropy change of −23.42 J kg−1K−1at 7 T and 2 K. On the other hand, Eu and Tb complexes exhibit interesting fluorescence properties. The compounds were subsequently used as fluorescent probes for the imaging of human breast adenocarcinoma (MCF7) cells. Live cell confocal microscopy images show that the complexes penetrate beyond the usual cytoplasm region and can be useful in imaging the nucleus region of MCF7 cells.

  • 31.
    De, Avik
    et al.
    Department of Inorganic Chemistry, Indian Association for the Cultivation of Science, Kolkata, India.
    Mondal, Raju
    Department of Inorganic Chemistry, Indian Association for the Cultivation of Science, Kolkata, India.
    Toxic Metal Sequestration Exploiting a Unprecedented Low-Molecular-Weight Hydrogel-to-Metallogel Transformation2018In: ACS Omega, E-ISSN 2470-1343, Vol. 3, no 6, p. 6022-6030Article in journal (Refereed)
    Abstract [en]

    We report herein the development of a unique low-molecular-weight gelator-induced technique for environmental remediation. The motive of this work is wastewater purification using a gel-based toxic heavy metal sequestration. The essence of this technique was to bring two different functionalities, one capable of multiple coordination and another with gel-forming ability, arranged in tandem within a single ligand molecule. Naturally, the success of the approach depends on whether the two tandem-arrayed functionalities are indeed working in tandem. Our results show that the ligand molecule is an excellent example of concomitant hydrogelator and metallogelator. The most interesting aspects of this study involve the toxic metal sequestration of Pb, Cd, and Hg which was further studied in detail with spectroscopic, microscopic, and diffraction techniques. We also report here a rare property of pure organic hydrogel-to-metallogel transformation which could open up a new avenue on wastewater purification. In essence, the hydrogels can be envisaged as a unique class of metal-free zeolite analogue for environmental remediation not by just absorbance but through absorbance cum coordination, which are further corroborated by the inductively coupled plasma-optical emission spectroscopy results.

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  • 32.
    Ding, Xiangbin
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Identity of Fluoride and Phosphate-Binding Sites at FeOOH Surfaces2012Independent thesis Advanced level (degree of Master (Two Years)), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Iron oxyhydroxides are of widespread occurrence in nature and play essential roles in both environmental as well as industrial processes. Due to their high reactivity, these minerals can act as sinks and/or transformation centers for a variety of inorganic and organic ions. These reactions are often mediated by various surface hydroxyl groups that are in turn singly-, doubly- or triply-coordinated with respect to underlying Fe atoms. In an effort to follow the reactivity of these different groups, attenuated total reflectance (ATR) - Fourier transform infrared (FTIR) spectroscopy was used to monitor adsorption reactions of on iron oxyhydroxide minerals.

    This work was specifically focused on synthetic submicron-sized lepidocrocite and goethite particles reacted to aqueous solutions of sodium fluoride and sodium phosphate. Langmuir-Freundlich adsorption isotherms were calibrated on adsorption data at various pH values to provide independent clues to the maximum sorption density achieved by these ions. When compared to theoretical site densities, these values suggested that although singly-coordinated groups are by far the more reactive groups on all surfaces, doubly-coordinated groups could be substituted by fluoride ions. FTIR measurements of dry mineral samples equilibrated with fluoride and phosphate confirmed these findings and also showed that triply-coordinated groups cannot be exchanged.

    Key words

    : goethite, lepidocrocite, FTIR, surface, adsorption, isotherm, modeling

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  • 33. Domashevskaya, EP
    et al.
    Ryabtsev, SV
    Turishchev, S Yu
    Kashkarov, VM
    Yurakov, Yu A
    Chuvenkova, OA
    Shchukarev, Andrey V
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    XPS and XANES studies of SnOx nanolayers2008In: Journal of Structural Chemistry, ISSN 0022-4766, E-ISSN 1573-8779, Vol. 49, no Suppl 1, p. 80-91Article in journal (Refereed)
    Abstract [en]

    This paper presents the results of our XPS (X-ray photoelectron spectroscopy) and XANES (X-ray absorption near edge structure) Studies of tin oxide nanolayers obtained by magnetron spraying of the metal and its further oxidation in air at different temperatures. It was shown that at 240 degrees C (annealing temperature), tin monoxide was dominant in the surface layer of the samples. When the temperature was increased to 450 degrees C, the phase composition corresponded to tin dioxide. Increased sorption ability was found for the samples oxidized at 450 degrees C. The band structure model of SnOx nanolayers obtained by superposition of the XANES and XPS data revealed cross transitions with energy similar to 3.7 eV in the presence of the SnO and SnO, phases. Surface doping of nanolayers with palladium gave the Pd, PdO, and PdO2 components, among which PdO was most intense. Alternate treatments with O-2 and H-2 gases led to the disappearance of palladium dioxide and the reduction of PdO to the Pd metal. After the volume doping of nanoplayers with palladium, the surface layer contained PdO and PdO2; the latter was represented by two types of particles with different sizes.

  • 34.
    Ekspong, Joakim
    et al.
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Sharifi, Tiva
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Klechikov, Alexey
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Wågberg, Thomas
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Gracia-Espino, Eduardo
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Stabilizing Active Edge Sites in Semicrystalline Molybdenum Sulfide by Anchorage on Nitrogen-Doped Carbon Nanotubes for Hydrogen Evolution Reaction2016In: Advanced Functional Materials, ISSN 1616-301X, E-ISSN 1616-3028, Vol. 26, no 37, p. 6766-6776Article in journal (Refereed)
    Abstract [en]

    Finding an abundant and cost-effective electrocatalyst for the hydrogen evolu-tion reaction (HER) is crucial for a global production of hydrogen from water electrolysis. This work reports an exceptionally large surface area hybrid catalyst electrode comprising semicrystalline molybdenum sulfi de (MoS 2+ x) catalystattached on a substrate based on nitrogen-doped carbon nanotubes (N-CNTs), which are directly grown on carbon fiber paper (CP). It is shown here that nitrogen-doping of the carbon nanotubes improves the anchoring of MoS 2+ xcatalyst compared to undoped carbon nanotubes and concurrently stabilizes a semicrystalline structure of MoS 2+ x with a high exposure of active sites for HER. The well-connected constituents of the hybrid catalyst are shown to facilitate electron transport and as a result of the good attributes, the MoS 2+ x/N-CNT/CPelectrode exhibits an onset potential of −135 mV for HER in 0.5 M H2SO4, a Tafel slope of 36 mV dec −1, and high stability at a current density of −10 mA cm −2.

  • 35.
    Elbashir, Sana
    et al.
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Ramstedt, Madeleine
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Thyrel, Mikael
    Sveriges Lantbruksuniversitet, Institutionen för skogens biomaterial och teknologi.
    Broström, Markus
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Skoglund, Nils
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Structural Study On The Chemical Environment Surrounding Phosphorus In Ash Fractions Suitable For Nutrient Recovery2022In: ESPC4 & PERM5 2022 – Book of Abstracts, 2022Conference paper (Refereed)
    Abstract [sv]

    Nutrient recovery is an integral part of sustainable clean energy production where one of the most important nutrients is phosphorus (P). Phosphorus recovery from biomass and waste ashes has been a hot topic for research and development activities for decades. However, the chemical speciation of heavy metals (HM) that may be included in recovered phosphates is yet to be resolved. Numerous trial and error approachs have been applied to lower the amount of HM content by fuel design and/or additives. Nevertheless, the connection between P and HM is theses complex phosphate systems on the atomic level is not fully understood. Therefore, exploring if HM are associated with phosphates is paramount for creating a naturallink between sustainable energy production and primary production of biomass.

    This study aims to examine the formation of different phosphates found in ashes and the potential inclusion of HM in their structures. The inclusion of Zn and Cu in whitlockite phosphates is investigated by powder X-ray diffraction and FTIR/RAMAN spectroscopy to identify possibilities and challenges with direct application of P-rich ash fractions as a nutrient source for plants. These measurements will be complemented by synchrotron-based X-rayabsorption spectroscopy analysis in future work.

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  • 36. Fan, Mei-Cen
    et al.
    Zhao, Yun
    Kang, Yu-Qiong
    Wozny, John
    Liang, Zheng
    Wang, Jun-Xiong
    Zhou, Guang-Min
    Li, Bao-Hua
    Tavajohi Hassan Kiadeh, Naser
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kang, Fei-Yu
    Room-temperature extraction of individual elements from charged spent LiFePO4 batteries2022In: Rare Metals, ISSN 1001-0521, E-ISSN 1867-7185Article in journal (Refereed)
    Abstract [en]

    Recycling millions of metric tons of spent LiFePO4 batteries would benefit human health while reducing resource depletion and environmental pollution. However, recovering individual elements from the spent batteries without generating waste is challenging. Here, we present a distinctive approach for recycling spent LiFePO4 batteries at room temperature, where water is the only leaching agent consumed. FePO4 and lithium intercalated graphite act as a precursor material for selectively extracting lithium, iron, and phosphorus through charging the LiFePO4 batteries to the delithiated state. NaOH solution extracted Fe from FePO4 within 30 min and regenerated without consumption, similar to a catalyst. Under the optimal leaching conditions (1 mol·L−1 NaOH, 0.5 h, NaOH/Fe molar ratio of 4.5), Fe and P leaching efficiencies achieved 89.1% and 99.2%, respectively. The methodology reflected in this research reduced the material cost per kg cathode material to a fraction of previously published reports, only occupies 6.13% of previous reports. In addition, the method improved the battery recycling revenue calculated by the EverBatt model by 2.31 times and 1.94 times over pyrometallurgical and hydrometallurgical methods. The proposed method allows for the convenient recovery of the elemental components of spent LiFePO4 batteries.

  • 37.
    Faust, Robin
    et al.
    Department of Chemistry and Chemical Engineering, Chalmers University of Technology, Kemigården 4, 412 96 Gothenburg, Sweden.
    Fürsatz, Katharina
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics. BEST – Bioenergy and Sustainable Technologies GmbH, Inffeldgasse 21b, Graz, Austria; TU Wien, Institute of Chemical, Environmental and Bioscience Engineering (ICEBE), Getreidemarkt 9/166, Vienna, Austria.
    Aonsamang, Panida
    Department of Chemistry and Chemical Engineering, Chalmers University of Technology, Kemigården 4, 412 96 Gothenburg, Sweden.
    Sandberg, Marcus
    Department of Chemistry and Chemical Engineering, Chalmers University of Technology, Kemigården 4, 412 96 Gothenburg, Sweden.
    Kuba, Matthias
    BEST – Bioenergy and Sustainable Technologies GmbH, Inffeldgasse 21b, Graz, Austria; TU Wien, Institute of Chemical, Environmental and Bioscience Engineering (ICEBE), Getreidemarkt 9/166, Vienna, Austria.
    Skoglund, Nils
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Knutsson, Pavleta
    Department of Chemistry and Chemical Engineering, Chalmers University of Technology, Kemigården 4, 412 96 Gothenburg, Sweden.
    Early layer formation on K-feldspar during fluidized bed combustion with phosphorus-rich fuel2023In: Fuel, ISSN 0016-2361, E-ISSN 1873-7153, Vol. 331, article id 125595Article in journal (Refereed)
    Abstract [en]

    K-feldspar was utilized as bed material for fluidized bed combustion of bark, chicken manure, and their mixture. Bed samples were extracted after 4 and 8 h and the samples were analyzed with scanning electron microscopy to study the impact of P-rich chicken manure on the bed material. The results were compared to fixed bed exposures with different orthophosphates to investigate their influence in detail. The fresh bed material used for this study exhibited an uneven surface with many cavities which facilitated the deposition and retention of the fuel ash. Utilizing pure chicken manure as fuel led to the formation of Ca- and P-rich particles which accumulated in these cavities. At the same time, larger ash particles were formed which consisted of the elements found in chicken manure ash. The co-combustion of bark and chicken manure led to the interaction of the two ash fractions and the formation of a thicker ash layer, which consisted of elements from both fuel ashes, namely Ca, P, Si, K and S. The layer appeared to be partially molten which could be favorable for the deposition of ash particles and thereby the formation of a mixed Ca/K-phosphate. Fixed bed exposures of the K-feldspar particles with Na3PO4 or K3PO4 caused particle agglomeration which means presence of alkali-phosphates should be limited. The co-combustion of bark with chicken manure showed promising results both regarding a shift from Ca-phosphates to more bioavailable Ca/K-phosphates and an acceleration in ash layer formation. The formation of an ash layer after only 4 h of exposure with the mixture of bark and chicken manure could be advantageous for catalytic activation of the bed material.

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  • 38. Filinchuk, Yaroslav
    et al.
    Talyzin, Alexandr V.
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Hagemann, Hans
    Dmitriev, Vladimir
    Chernyshov, Dmitry
    Sundqvist, Bertil
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Cation Size and Anion Anisotropy in Structural Chemistry of Metal Borohydrides. The Peculiar Pressure Evolution of RbBH42010In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 49, no 11, p. 5285-5292Article in journal (Refereed)
    Abstract [en]

    The pressure evolution of RbBH4 has been characterized by synchrotron powder X-ray diffraction and Raman spectroscopy up to 23 GPa. Diffraction experiments at ambient temperature reveal three phase transitions, at 3.0, 10.4, and 18 GPa (at 2.6, 7.8, and 20 GPa from Raman data), at which the space group symmetry changes in the order Fm-3m(Z=4) → P4/nmm(2) → C222(2) → I-42m(4). Crystal structures and equations of state are reported for all four phases. The three high-pressure structure types are new in the crystal chemistry of borohydrides. RbBH4 polymorphs reveal high coordination numbers (CNs) for cation and anion sites, increasing with pressure from 6 to 8, via an intermediate 4 + 4 coordination. Different arrangements of the tetrahedral BH4 group in the Rb environment define the crystal symmetries of the RbBH4 polymorphs. The structural evolution in the MBH4 series is determined by the cation’s size, as it differs drastically for M = Li (CNs = 4, 6), Na (CN = 6), and Rb. The only structure common to the whole MBH4 family is the cubic one. Its bulk modulus linearly decreases as the ionic radius of M increases, indicating that the compressibility of the material is mainly determined by the repulsive BH4···BH4 interactions.

  • 39. Fischer, A I
    et al.
    Kuznetsov, V A
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Belyaev, A N
    Crystal and molecular structures of mixedvalence octanuclear cobalt(II,III) propionate and butyrate with an etagerelike core2012In: Russian chemical bulletin, ISSN 1066-5285, E-ISSN 1573-9171, Vol. 61, no 4, p. 821-827Article in journal (Refereed)
    Abstract [en]

    The new mixed-valence octanuclear cobalt carboxylate complexes [CoII4CoIII4(μ4-O)4-(μ3-OMe)4(μ-O2CR)6(O2CR)2(H2O)6]·4H2O, where R = Et (3) or n-Pr (4), were investigated by X-ray diffraction analysis. Complexes 3 and 4 have a molecular octanuclear structure, and they are valence trapped, and contain four cobalt atoms Co3+ in the central cubane fragment with four cobalt atoms Co2+ at the periphery of the molecules. The molecules of the complexes are stabilized by four intramolecular hydrogen bonds and are linked, together with water solvent molecules, by intermolecular hydrogen bonds to form a three-dimensional supramolecular system.

  • 40. Fraqueza, G.
    et al.
    Carvalho, L.
    Marques, P.
    Ohlin, C. Andre
    Casey, W.
    Aureliano, M.
    Functional and structural interactions of Nb, V, Mo and W oxometalates with the sarcoplasmic reticulum Ca2(+) -ATPase reveal new insights into inhibition processes: a combination of NMR, Raman, AA and EPR spectroscopie with kinetic studies2012In: The FEBS Journal, ISSN 1742-464X, E-ISSN 1742-4658, Vol. 279, no 1, SIArticle in journal (Refereed)
  • 41. Fraqueza, Gil
    et al.
    Batista de Carvalho, Luis A. E.
    Marques, M. Paula M.
    Maia, Luisa
    Ohlin, C. Andre
    Casey, William H.
    Aureliano, Manuel
    Decavanadate, decaniobate, tungstate and molybdate interactions with sarcoplasmic reticulum Ca2+-ATPase: quercetin prevents cysteine oxidation by vanadate but does not reverse ATPase inhibition2012In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 41, no 41, p. 12749-12758Article in journal (Refereed)
    Abstract [en]

    Recently we demonstrated that the decavanadate (V-10) ion is a stronger Ca2+-ATPase inhibitor than other oxometalates, such as the isoelectronic and isostructural decaniobate ion, and the tungstate and molybdate monomer ions, and that it binds to this protein with a 1 : 1 stoichiometry. The V-10 interaction is not affected by any of the protein conformations that occur during the process of calcium translocation (i.e. E1, E1P, E2 and E2P) (Fraqueza et al., J. Inorg. Biochem., 2012). In the present study, we further explore this subject, and we can now show that the decaniobate ion, [Nb-10 = Nb10O28](6-), is a useful tool in deducing the interaction and the non-competitive Ca2+-ATPase inhibition by the decavanadate ion [V-10 = V10O28](6-). Moreover, decavanadate and vanadate induce protein cysteine oxidation whereas no effects were detected for the decaniobate, tungstate or molybdate ions. The presence of the antioxidant quercetin prevents cysteine oxidation, but not ATPase inhibition, by vanadate or decavanadate. Definitive V(IV) EPR spectra were observed for decavanadate in the presence of sarcoplasmic reticulum Ca2+-ATPase, indicating a vanadate reduction at some stage of the protein interaction. Raman spectroscopy clearly shows that the protein conformation changes that are induced by V-10, Nb-10 and vanadate are different from the ones induced by molybdate and tungstate monomer ions. Here, Mo and W cause changes similar to those by phosphate, yielding changes similar to the E1P protein conformation. The putative reduction of vanadium(V) to vanadium(IV) and the non-competitive binding of the V-10 and Nb-10 decametalates may explain the differences in the Raman spectra compared to those seen in the presence of molybdate or tungstate. Putting it all together, we suggest that the ability of V-10 to inhibit the Ca2+-ATPase may be at least in part due to the process of vanadate reduction and associated protein cysteine oxidation. These results contribute to the understanding and application of these families of mono-and polyoxometalates as effective modulators of many biological processes, particularly those associated with calcium homeostasis.

  • 42. Fraqueza, Gil
    et al.
    Ohlin, C. Andre
    Casey, William H.
    Aureliano, Manuel
    Sarcoplasmic reticulum calcium ATPase interactions with decaniobate, decavanadate, vanadate, tungstate and molybdate2012In: Journal of Inorganic Biochemistry, ISSN 0162-0134, E-ISSN 1873-3344, Vol. 107, no 1, p. 82-89Article in journal (Refereed)
    Abstract [en]

    Over the last few decades there has been increasing interest in oxometalate and polyoxometalate applications to medicine and pharmacology. This interest arose, at least in part, due to the properties of these classes of compounds as anti-cancer, anti-diabetic agents, and also for treatment of neurodegenerative diseases, among others. However, our understanding of the mechanism of action would be improved if biological models could be used to clarify potential toxicological effects in main cellular processes. Sarcoplasmic reticulum (SR) vesicles, containing a large amount of Ca(2+)-ATPase, an enzyme that accumulates calcium by active transport using ATP, have been suggested as a useful model to study the effects of oxometalates on calcium homeostasis. In the present article, it is shown that decavanadate, decaniobate, vanadate, tungstate and molybdate, all inhibited SR Ca(2+)-ATPase, with the following IC(50) values: 15, 35, 50, 400 mu M and 45 mM, respectively. Decaniobate (Nb(10)), is the strongest P-type enzyme inhibitor, after decavanadate (V(10)). Atomic-absorption spectroscopy (AAS) analysis, indicates that decavanadate binds to the protein with a 1:1 decavanadate:Ca(2+)-ATPase stoichiometry. Furthermore, V10 binds with similar extension to all the protein conformations, which occur during calcium translocation by active transport, namely El, El P, E2 and E2P, as analysed by MS. In contrast, it was confirmed that the binding of monomeric vanadate (H(2)VO(4)(2-):V(1)) to the calcium pump is favoured only for the E2 and E2P conformations of the ATPase, whereas no significant amount of vanadate is bound to the E1 and E1P conformations. Scatchard plot analysis, confirmed a 1:1 ratio for decavanadate-Ca(2+)-ATPase, with a dissociation constant, k(d) of 1 mu M(-1). The interaction of decavanadate V(10)O(28)(6-) (V(10)) with Ca(2+)-ATPase is prevented by the isostructural and isoelectronic decaniobate Nb(10)O(28)(6-) (Nb(10)), whereas no significant effects were detected with ATP or with heparin, a known competitive ATP binding molecule, suggesting that V(10) binds non-competitively, with respect to ATP, to the protein. Finally, it was shown that decaniobate inhibits SR Ca(2+)-ATPase activity in a non competitive type of inhibition, with respect to ATP. Taken together, these data demonstrate that decameric niobate and vanadate species are stronger inhibitors of the SR calcium ATPase than simple monomeric vanadate, tungstate and molybdate oxometalates, thus affecting calcium homeostasis, cell signalling and cell bioenergetics, as well many other cellular processes. The ability of these oxometalates to act either as phosphate analogues, as a transition-state analogue in enzyme-catalysed phosphoryl group transfer processes and as potentially nucleotide-dependent enzymes modulators or inhibitors, suggests that different oxometalates may reveal different mechanistic preferences in these classes of enzymes. (C) 2011 Elsevier Inc. All rights reserved.

  • 43. Gordeeva, Alisa
    et al.
    Hsu, Ying-Jui
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Jenei, Istvan Z.
    Carvalho, Paulo H. B. Brant
    Simak, Sergei, I
    Andersson, Ove
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Haussermann, Ulrich
    Layered Zinc Hydroxide Dihydrate, Zn5(OH)10·2H2O, from Hydrothermal Conversion of ε-Zn(OH)2 at Gigapascal Pressures and its Transformation to Nanocrystalline ZnO2020In: ACS Omega, E-ISSN 2470-1343, Vol. 5, no 28, p. 17617-17627Article in journal (Refereed)
    Abstract [en]

    Layered zinc hydroxides (LZHs) with the general formula (Zn2+)x(OH)2xmy(Am)y·nH2O (Am = Cl, NO3, ac, SO42–, etc) are considered as useful precursors for the fabrication of functional ZnO nanostructures. Here, we report the synthesis and structure characterization of the hitherto unknown “binary” representative of the LZH compound family, Zn5(OH)10·2H2O, with Am = OH, x = 5, y = 2, and n = 2. Zn5(OH)10·2H2O was afforded quantitatively by pressurizing mixtures of ε-Zn(OH)2 (wulfingite) and water to 1–2 GPa and applying slightly elevated temperatures, 100–200 °C. The monoclinic crystal structure was characterized from powder X-ray diffraction data (space group C2/c, a = 15.342(7) Å, b = 6.244(6) Å, c = 10.989(7) Å, β = 100.86(1)°). It features neutral zinc hydroxide layers, composed of octahedrally and tetrahedrally coordinated Zn ions with a 3:2 ratio, in which H2O is intercalated. The interlayer d(200) distance is 7.53 Å. The H-bond structure of Zn5(OH)10·2H2O was analyzed by a combination of infrared/Raman spectroscopy, computational modeling, and neutron powder diffraction. Interlayer H2O molecules are strongly H-bonded to five surrounding OH groups and appear orientationally disordered. The decomposition of Zn5(OH)10·2H2O, which occurs thermally between 70 and 100 °C, was followed in an in situ transmission electron microscopy study and ex situ annealing experiments. It yields initially 5–15 nm sized hexagonal w-ZnO crystals, which, depending on the conditions, may intergrow to several hundred nm-large two-dimensional, flakelike crystals within the boundary of original Zn5(OH)10·2H2O particles.

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  • 44. Gordon, C M
    et al.
    Ohlin, C A
    Ritchie, C
    Ionic liquids: Clean solvents for organic synthesis.2001Other (Refereed)
  • 45.
    Gorzsás, András
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Vanadate and Peroxovanadate Complexes of Biomedical Relevance: A speciation approach with focus on diabetes2005Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Diabetes mellitus is one of the most threatening epidemics of modern times with rapidly increasing incidence. Vanadium and peroxovanadium compounds have been shown to exert insulin–like actions and, in contrast to insulin, are orally applicable. However, problems with side–effects and toxicity remain. The exact mechanism(s) by which these compounds act are not yet fully known. Thus, a better understanding of the aqueous chemistry of vanadates and peroxovanadates in the presence of various (bio)ligands is needed.

    The present thesis summarises six papers dealing mainly with aqueous speciation in different vanadate – and peroxovanadate – ligand systems of biological and medical relevance. Altogether, five ligands have been studied, including important blood constituents (lactate, citrate and phosphate), a potential drug candidate (picolinic acid), and a dipeptide (alanyl serine) to model the interaction of (peroxo)vanadate in the active site of enzymes. Since all five ligands have been studied both with vanadates and peroxovanadates, the number of systems described in the present work is eleven, including the vanadate – citrate – lactate mixed ligand system. The pH–independent formation constants have been determined for 33 ternary vanadate – ligand, 41 quaternary peroxovanadate – ligand and two vanadate – mixed ligand species in addition to the pKa values of all five ligands. These constants have been used to model physiological conditions, and the biomedical relevance of the different species is discussed.

    The studies have been performed at 25 ºC in the physiological medium of 0.150 M Na(Cl), i.e. the ionic strength of human blood. No buffers have been used, and wide pH–ranges have usually been covered. The applied experimental techniques comprise mostly 51V NMR and potentiometry, but 31P, 13C, 1H and 14N NMR as well as EPR and ESI–MS have also been used to gain additional information. Multimethod data have been treated by the least–squares program LAKE and modelling has been carried out by the software package WinSGW.

    Whenever possible, solution structures of the species have been proposed. In addition, simple biological tests have been carried out to determine the stability of the formed peroxovanadate complexes in the presence of human catalase. A brief comparison is given of the different vanadate – ligand and peroxovanadate – ligand systems with emphasis on observed trends and general features.

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  • 46.
    Grimm, Alejandro
    et al.
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science.
    Skoglund, Nils
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Boström, Dan
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Öhman, Marcus
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science.
    Bed agglomeration characteristics in fluidized quartz bed combustion of phosphorus-rich biomass fuels2011In: Energy & Fuels, ISSN 0887-0624, E-ISSN 1520-5029, Vol. 25, no 3, p. 937-947Article in journal (Refereed)
    Abstract [en]

    The bed agglomeration characteristics during combustion of phosphorus-rich biomass fuels and fuel mixtures were determined in a fluidized (quartz) bed reactor (5 kW). The fuels studied (separately and in mixtures) included logging residues, bark, willow, wheat straw, and phosphorus-rich fuels, like rapeseed meal (RM) and wheat distillers dried grain with solubles (DDGS). Phosphoric acid was used as a fuel additive. Bed material samples and agglomerates were studied by means of scanning electron microscopy (SEM) in combination with energy-dispersive X-ray spectroscopy (EDX), in order to analyze the morphological and compositional changes of coating/reaction layers and necks between agglomerated bed particles. Furthermore, bed ash particles were separated by sieving from the bed material samples and analyzed with SEM/EDS and powder X-ray diffraction (XRD). For logging residues, bark, and willow, with fuel ash rich in Ca and K but with low contents of P and organically bound Si, the bed layer formation is initiated by reactions of gaseous or liquid K compounds with the surface of the bed material grains, resulting in the formation of a potassium silicate melt. The last process is accompanied by the diffusion/dissolving of Ca into the melt and consequent viscous flow sintering and agglomeration. The addition of high enough phosphorus content to convert the available fuel ash basic oxides into phosphates reduced the amount of K available for the reaction with the quartz bed material grains, thus preventing the formation of an inner bed particle layer in the combustion of logging residues, bark, and willow. Some of the phosphate-rich ash particles, formed during the fuel conversion, adhered and reacted with the bed material grains to form noncontinuous phosphate−silicate coating layers, which were found responsible for the agglomeration process. Adding phosphorus-rich fuels/additives to fuels rich in K and Si (e.g., wheat straw) leads to the formation of alkali-rich phosphate−silicate ash particles that also adhered to the bed particles and caused agglomeration. The melting behavior of the bed particle layers/coatings formed during combustion of phosphorus-rich fuels and fuel mixtures is an important controlling factor behind the agglomeration tendency of the fuel and is heavily dependent on the content of alkaline earth metals in the fuel. A general observation is that phosphorus is the controlling element in ash transformation reactions during biomass combustion in fluidized quartz beds because of the high stability of phosphate compounds.

  • 47. Grivel, J-C
    et al.
    Pitillas, A.
    Namazkar, S.
    Umeå University, Faculty of Science and Technology, Department of Plant Physiology. Department of Energy Conversion and Storage, Technical University of Denmark, 4000-Roskilde, Denmark.
    Alexiou, A.
    Holte, O. J.
    Preparation and characterization of MgB2 with Pd, Pt and Re doping2016In: Physica. C, Superconductivity, ISSN 0921-4534, E-ISSN 1873-2143, Vol. 520, p. 37-41Article in journal (Refereed)
    Abstract [en]

    Samples with Mg1-xDxB2.04 (D = Pt, Pd or Re) nominal compositions have been synthesised by a solid-state route. None of these doping elements can be substituted for Mg in a detectable amount and their presence in the samples has no influence on the critical temperature and on the lattice parameters of the MgB2 superconductor. Impurity phases are formed by reaction mostly with Mg. The microstructure of the Pt, Pd and Re-based phases depends on the elements. Re-rich particles with large sizes up to 8 mu m form, whereas Pt- and Pd-containing impurities are finely dispersed with a particle size that does not exceed 1 mu m. The field dependence of the normalised critical current density is improved when Pt, Pd or Re are present in the samples. (C) 2015 Elsevier B.V. All rights reserved.

  • 48. Gumerova, Nadiia I.
    et al.
    Caldera Fraile, Tania
    Roller, Alexander
    Giester, Gerald
    Pascual-Borràs, Magda
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ohlin, C. André
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Rompel, Annette
    Direct Single- and Double-Side Triol-Functionalization of the Mixed Type Anderson Polyoxotungstate [Cr(OH)3W6O21]6–2019In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 58, p. 106-113Article in journal (Refereed)
    Abstract [en]

    Since the first successful triol-functionalization of the Anderson polyoxometalates, the six protons of their central octahedron X(OH)6 (X—heteroatom, p- or d-element) have been considered as a prerequisite for their functionalization with tripodal alcohols, and therefore, the functionalization of Anderson structures from the unprotonated sides have never been reported. Here, we describe the triol-functionalization of [Cr(OH)3W6O21]6– leading to the single-side grafted anions [Cr(OCH2)3CRW6O21]6– (CrW6-tris-R, R = −C2H5, −NH2, −CH2OH) and the unprecedented double-side functionalized anion [Cr((OCH2)3CC2H5)2W6O18]3– (CrW6-(tris-C2H5)2), despite the lack of protons in the parent anion in the solid state. CrW6-(tris-C2H5)2 demonstrates the first example of double-side functionalized Anderson POT with the partially one-side protonated corresponding parent anion. The new heteropolytungstates were characterized by single-crystal X-ray diffraction, elemental analysis, Fourier-transform infrared spectroscopy, thermal gravimetric analysis, cyclic voltammetry, and electrospray ionization mass spectrometry. Density functional theory calculations were performed to investigate and compare the stability among the different isomers of the parent anion [Cr(OH)3W6O21]6–.

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  • 49. Gumerova, Nadiia I.
    et al.
    Prado-Roller, Alexander
    Rambaran, Mark
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ohlin, C. André
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Rompel, Annette
    The Smallest Polyoxotungstate Retained by TRIS-Stabilization2021In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 60, no 17, p. 12671-12675Article in journal (Refereed)
    Abstract [en]

    A polycondensation reaction of the orthotungstate anion WO42–, buffered at pH 7.5 in a TRIS-HCl (0.15 M) solution, results in the first example of a discrete polyoxotungstate anion, with just two W ions stabilized with TRIS ligands. It was isolated and characterized as Na2[WVI2O6(C4O3NH10)2]·6H2O by single-crystal and powder X-ray diffraction, FT-IR spectroscopy, thermogravimetrical analysis (TGA), and elemental analysis in solid state and by electro-spray ionization mass spectrometry (ESI-MS), 13C, and 183W NMR, as well as Raman spectroscopy in solution. This synthesis demonstrates the crucial and new role of the added tris-alkoxy ligand in the development of a new hybrid TRIS-isopolytungstate with the lowest known nuclearity (so far) and the terminal oxygens substituted with two nitrogen atoms arising from amines of the TRIS ligands.

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  • 50.
    Gustafsson, Tomas
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Saxin, Maria
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kihlberg, Jan
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Synthesis of a C-glycoside analogue of β-D -galactosyl threonine2003In: Journal of Organic Chemistry, ISSN 0022-3263, E-ISSN 1520-6904, Vol. 68, no 6, p. 2506-2509Article in journal (Refereed)
    Abstract [en]

    C-linked analogue of β-d-galactosylthreonine has been prepared from 2,3,4,6-tetra-O-benzyl-d-galactopyranolactone (1) in 14 steps. Three stereogenic centers were created during the synthesis, with the anomeric center of the C-glycoside being generated first by addition of a Grignard reagent to 1 and subsequent reduction of the intermediate hemiacetal with triethylsilane. The two stereogenic centers in the threonine moiety were both established by alkylation of Evans' chiral N-acyloxazolidinone enolates.

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