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  • 1.
    Ahlkvist, Johan
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ajaikumar, Samikannu
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    One-pot catalytic conversion of Nordic pulp media into green platform chemicals2013In: Applied Catalysis A: General, ISSN 0926-860X, E-ISSN 1873-3875, Vol. 454, p. 21-29Article in journal (Refereed)
    Abstract [en]

    In this paper, both sulphite and sulphate (Kraft) cellulose from Nordic pulp mills were used as raw materials in the catalytic one-pot synthesis of green platform chemicals, levulinic and formic acids, respectively. The catalyst of choice was a macro-porous, cationic ion-exchange resin, Amberlyst 70. The optimal reaction conditions were determined and the influence of various gas atmospheres was investigated. The maximum yields of 53% formic acid and 57% of levulinic acid were separately obtained in a straight-forward conversion system only containing cellulose, water and the heterogeneous catalyst. The concept introduces a one-pot procedure providing a feasible route to green platform chemicals obtained via conversion of coniferous soft wood pulp to levulinic and formic acids, respectively.

  • 2.
    Ahlkvist, Johan
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Samikannu, Ajaikumar
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Wärnå, Johan
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Åbo, Finland.
    Salmi, Tapio
    Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Åbo, Finland.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Åbo, Finland.
    Reaction Network upon One-pot Catalytic Conversion of Pulp2013In: / [ed] Sauro Pierucci, Jiří J. Klemeš, AIDIC - associazione italiana di ingegneria chimica, 2013, Vol. 32, p. 649-654Conference paper (Refereed)
    Abstract [en]

    Nordic sulphite and sulphate (Kraft) cellulose originating from Nordic pulp mills were used as raw materials in the catalytic synthesis of green platform chemicals, levulinic and formic acids, respectively. The catalyst of choice used in this study was a macro-porous, cationic ion-exchange resin Amberlyst 70 for which the optimal reaction conditions leading to best yields were determined. For this system, maximum yields of 53 mol-% and 57 mol-% were obtained for formic and levulinic acid, respectively. The reaction network of the various chemical species involved was investigated and a simple mechanistic approach involving first order reaction kinetics was developed. The prototype model was able to describe the behaviour of the system in a satisfactory manner.

  • 3.
    Ajaikumar, Samikannu
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ahlkvist, Johan
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boström, Dan
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Kordas, K
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Highly active and selective bimetallic catalysts supported on transition metal oxides for the oxidation of α-pinene using molecular oxygen2010Conference paper (Other academic)
  • 4.
    Ajaikumar, Samikannu
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ahlkvist, Johan
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boström, Dan
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Kordas, K
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Synthesis and characterization of Cu and Cu-M (M=Co, Ni, Au and Zn) bimetallic catalysts supported on TiO2 modified SBA-152010Conference paper (Other academic)
  • 5.
    Ajaikumar, Samikannu
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ahlkvist, Johan
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kordas, K
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Piispankatu 8, FIN-20500, Turku/Åbo, Finland.
    Oxidation of α-pinene over gold containing bimetallic nanoparticles supported on reducible TiO2 by DPU method2011In: Applied Catalysis A: General, ISSN 0926-860X, E-ISSN 1873-3875, Vol. 392, no 1-2, p. 11-18Article in journal (Refereed)
    Abstract [en]

    A series of bimetallic catalysts Au–M (where M = Cu, Co and Ru) were supported on a reducible TiO2 oxide via deposition-precipitation (DP) method with a slow decomposition of urea as the precipitating agent. The characteristic structural features of the prepared materials were characterized by various physico-chemical techniques such as X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). XPS results indicated the formation of alloyed bimetallic particles on the TiO2 support. TEM results confirmed the fine dispersion of metal nanoparticles on the support with an average particle size in the range of 3–5 nm. An industrially important process, oxy-functionalization of α-pinene was carried out over the prepared bimetallic heterogeneous catalysts under liquid phase conditions. Reaction parameters such as the reaction time, temperature, and the effect of solvent were studied for optimal conversion of α-pinene into verbenone. The major products obtained were verbenone, verbenol, α-pinene oxide and alkyl-pinene peroxide. The activity of the catalysts followed the order; AuCu/TiO2 > AuCo/TiO2 > Cu/TiO2 > Au/TiO2 > AuRu/TiO2. Upon comparison of the various catalysts, AuCu/TiO2 was found to be an active and selective catalyst towards the formation of verbenone. The temperature, nature of the catalysts and the choice of solvents greatly influenced the reaction rate.

  • 6.
    Bodén, Ida
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Umeå University, Faculty of Medicine, Department of Surgical and Perioperative Sciences, Surgery. Umeå University, Faculty of Science and Technology, Centre for Biomedical Engineering and Physics (CMTF).
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Nilsson, David
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Forssell, Erik
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Naredi, Peter
    Umeå University, Faculty of Medicine, Department of Surgical and Perioperative Sciences, Surgery.
    Lindholm-Sethson, Britta
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Umeå University, Faculty of Science and Technology, Centre for Biomedical Engineering and Physics (CMTF).
    In vivo skin measurements with a novel probe head for simultaneous skin impedance and near-infrared spectroscopy2011In: Skin research and technology, ISSN 0909-752X, E-ISSN 1600-0846, Vol. 17, no 4, p. 494-504Article in journal (Refereed)
    Abstract [en]

    Background/purpose: Near-infrared (NIR) spectroscopy and skin impedance (IMP) measurements are useful techniques for objective diagnostics of various skin diseases. Here, we present a combined probe head for simultaneous, time-saving NIR spectroscopy and skin impedance measurements. The probe also ensures that both measurements are performed under equal conditions and at the same skin location.

    Methods: Finite element method simulations were performed for evaluation of the impedance. In vivo skin measurements were performed and combined NIR and impedance spectra were analysed by means of multivariate methods with respect to body location, age and gender. The classification rate was determined by a planar discriminant analysis. Reproducibility was investigated by calculation of scatter values and statistical significance between overlapping groups was assessed by the calculation of intra-model distances, q.

    Results: The novel probe yielded rapid reproducible results and was easy to manage. Significant differences between skin locations and to a lesser extent age groups and gender were demonstrated.

    Conclusion: With the novel probe, statistically significant differences between overlapping classes in score plots can be confirmed by calculating intra-model distances. The influence of molecular differences in the skin at different body locations is larger than the influence of gender or age and therefore relevant reference measurements are discussed.

  • 7.
    Bukhanko, Natalia
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Samikannu, Ajaikumar
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Leino, Anne-Riikka
    Microelectronics and Materials Physics Laboratories, University of Oulu, Finland.
    Kordas, Krisztian
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Microelectronics and Materials Physics Laboratories, University of Oulu, Finland.
    Wärnå, Johan
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Finland.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Finland.
    Continuous gas phase synthesis of 1-ethyl chloride from ethyl alcohol and hydrochloric acid over Al2O3-based catalysts: the ‘green’ route2013In: ACS Sustainable Chemistry & Engineering, Vol. 1, no 8, p. 883-893Article in journal (Refereed)
    Abstract [en]

    The synthesis of 1-ethyl chloride in the gas-phase mixture of ethanol and hydrochloric acid over ZnCl2/Al2O3 catalysts was studied in a continuous reactor using both commercial and tailor-made supports. The catalytic materials were characterized by the means of structural (XPS, TEM, XRD, and BET) and catalytic activity (selectivity and conversion) measurements. The reaction parameters such as temperature, pressure, and feedstock flow rates were optimized for the conversion of ethanol to ethyl chloride. The new tailor-made highly porous Al2O3-based catalyst outperformed its commercial counterpart by exhibiting high conversion and selectivity (98%) at the temperature of 325 °C. Long-term stability tests (240 h) confirmed the excellent durability of the tailor-made alumina catalysts. The process demonstrated here poses an efficient and economic “green” large-scale on-site synthesis of this industrially important reactant in industry, where bioethanol is produced and 1-ethyl chloride is necessary, e.g., for ethylation of cellulose and synthetic polymer products. On-site in situ production of ethyl chloride avoids the problems associated with the transportation and storage of toxic and flammable 1-ethyl chloride.

  • 8.
    Bukhanko, Natalia
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Department of Forest Biomaterials Technology, Swedish University of Agricultural Science, Umeå, Sweden.
    Schwarz, Christopher
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Samikannu, Ajaikumar
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Ngoc Pham, Tung
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Department of Chemistry, The University of Danang - University of Science and Technology, Nguyen Luong Bang, Lien Chieu, Da Nang, Viet Nam.
    Siljebo, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Wärnå, Johan
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Rautio, Anne-Riikka
    Kordas, Krisztian
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Gas phase synthesis of isopropyl chloride from isopropanol and HCl over alumina and flexible 3-D carbon foam supported catalysts2017In: Applied Catalysis A: General, ISSN 0926-860X, E-ISSN 1873-3875, Vol. 542, no 25, p. 212-225Article in journal (Refereed)
    Abstract [en]

    Isopropyl chloride synthesis from isopropanol and HCl in gas phase over ZnCl2 catalysts supported on Al2O3 as well as flexible carbon foam was studied in a continuous reactor. A series of catalytic materials were synthesised and characterised by BET, XPS, SEM, TEM, XRD and NH3-TPD methods. Catalytic activity tests (product selectivity and conversion of reactants) were performed for all materials and optimal reaction conditions (temperature and feedstock flow rates) were found. The results indicate that the highest yield of isopropyl chloride was obtained over 5 wt.% ZnCl2 on commercial Al2O3 (No. II) (95.3%). Determination of product mixture compositions and by-product identification were done using a GC-MS method. Carbon foam variant catalyst, 5 wt.% ZnCl2/C, was found to perform best out of the carbon-supported materials, achieving ∼75% yield of isopropyl chloride. The kinetic model describing the process in a continuous packed bed reactor was proposed and kinetic parameters were calculated. The activation energy for the formation of isopropyl chloride reaction directly from isopropanol and HCl was found to be ∼58 kJ/mol.

  • 9.
    Golets, Mikhail
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Samikannu, Ajaikumar
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Blomberg, David
    Processum Biorefinery Initiative AB, 89186, Örnsköldsvik, Sweden.
    Grundberg, H
    Aditya Birla Domsjö Fabriker AB, 89186, Örnsköldsvik, Sweden .
    Wärnå, J
    Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Turku, Finland.
    Salmi, T
    Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Turku, Finland.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Turku, Finland.
    A kinetic study of the liquid phase acetoxylation of α-pinene2012In: Topics in catalysis, ISSN 1022-5528, E-ISSN 1572-9028, Vol. 55, no 7-10, p. 649-656Article in journal (Refereed)
    Abstract [en]

    The present study introduces kinetic modeling of liquid phase α-pinene acetoxylation with acetic acid over an ion-exchange resin catalyst. The reaction was carried out in a laboratory scale high-pressure autoclave. α-terpinyl (35 wt%) and bornyl (40 wt%) acetates were the primary products. The predominant reaction pathways were identified and evaluated.

  • 10. Horáček, Jan
    et al.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Industrial Chemistry & Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Åbo-Turku, Finland.
    Ajaikumar, Samikannu
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Šťávová, Gabriela
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Hora, Lukáš
    Kubička, David
    Studies on sodium lignosulfonate depolymerization over Al2O3 supported catalysts loaded with metals and metal oxides in a continuous flow reactor2013In: Topics in catalysis, ISSN 1022-5528, E-ISSN 1572-9028, Vol. 56, no 9-10, p. 794-799Article in journal (Refereed)
    Abstract [en]

    The aim of this work was to study the how various heterogeneous catalysts perform upon lignosulfonate decomposition reactions. The main target of the study was to obtain extractable phenolic compounds as potential renewable chemicals for the production of fuel components and chemicals. The nature of the heterogeneous catalyst was found to have a great impact on the obtained product yields and the composition of the product mixture. Initially, a nickel–tungsten on alumina (NiW/Al2O3) reference catalyst was applied upon screening the influence of catalyst particle size and various reaction parameters. Significantly increasing product yields with decreasing catalyst particle size indicated that the lignosulfonate transformation takes place on the external catalyst surface due to large macromolecular structure of the feedstock. The contact time (space time velocity) and catalyst particle size were the most important factors influencing the selectivity profiles towards various products as well as the yields observed. The highest conversion to phenolics was obtained over in-house-prepared NiO/Al2O3 and NiMo/Al2O3 catalysts with various NiO and MoO3 loadings.

  • 11.
    Huang, Yang
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Siljebo, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Westlund, Per-Olof
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Water proton and deuterium spin-lattice relaxation in Zeolite ZSM-5 by fast field-cycling NMR relaxometry2015Manuscript (preprint) (Other academic)
    Abstract [en]

    The water dynamics in the confined space of the zeolite ZSM-5 has bee ninvestigated by means of the field dependence of 1H- and 2H- spin-lattice relaxation rates using a 1T Stelar FFC2000 fast field-cycling instrument. The NMRD analysis of  the experimental results indicates that the characteristic time dependence ( 50 ns to 1-2.4 μs) is due to water translational diffusion in narrow pores. The temperature dependence of the spin-lattice relaxation rates is weak.Zeolites with different counter ions( H+, NH4+ change the water hydration and the water translational diffusion in the pores drastically. The Zeolite-NH4+ slow down the water motion with a factor of 2.The NMRD profiles show somewhat stretched character and is described by two Lorenzian which indicates that the distribution of pore sizes is broaden.The water 1H and 2H spin lattice relaxation profiles give qualitatively information about water hydration in zeolites with different counter ions and is expected also to indicate structural changes of the zeolites. 

  • 12.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Chemistry.
    New approaches to moisture determination in complex matrices based on the Karl Fischer Reaction in methanolic and non-alcoholic media2008Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Moisture determination is of great importance in the production and use of many substances. For example, the moisture content can affect the efficiency of a chemical reaction or determine the shelf life of pharmaceuticals or foods. The standard method for moisture determination is Karl Fischer (KF) titration, based on either volumetry or coulometry. This thesis concerns new approaches to trace determination in complex sample matrices and is focused on oils and substances that interfere with alcoholic KF reagents.

    Moisture is frequently separated from oil matrices before titration by means of evaporation techniques. In connection with the preparation of new reference materials for moisture in oil, the National Institute of Standards and Technology (NIST) questioned the efficiency of such evaporation techniques. NIST claimed that some of the moisture was sequestered in the oil phase and that it could only be released and detected by using a modified volumetric KF method with a reagent containing at least 65% chloroform. In this thesis, an alternative KF method that meets the proposed requirement for a complete dissolution of the oil sample is presented. With this method it is shown that there is no reason to question the efficiency of the evaporation techniques and that the criticized volumetric method used by NIST is biased high.

    Ever since its introduction diaphragm-free coulometry has gained popularity due to its ease of use, with a single reagent and short conditioning times. Trace determination with this technique sets great demands on the reagent due to the resulting low current densities at the generator cathode. The performance of several commercial reagents is evaluated under such unfavorable conditions and critical titration parameters are identified. It is also shown that decanol has a favorable effect on the cathode process when using reagents modified with xylene according to standard methods for moisture determination in oils.

    For samples that are incompatible with the alcohol component in ordinary KF reagent a new reagent based on N-methylformamide is presented. It is shown that is works well for determinations of moisture in a conductive salt used in lithium-ion batteries. The concept of alcohol-free KF reagents is taken a step further in a systematic investigation, also including formamide and dimethylformamide. Advantages and disadvantages with these solvents are discussed and possible reaction paths are surveyed. It is shown that the position of the sulfur dioxide/hydrogen sulfite equilibrium is the main explanation for the large differences in the KF reaction rates in these solvents.

  • 13.
    Larsson, William
    et al.
    Umeå University, Faculty of Science and Technology, Chemistry.
    Cedergren, Anders
    Umeå University, Faculty of Science and Technology, Chemistry.
    Coulometric Karl Fischer titration of trace water in diaphragm-free cells2005In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 65, no 5, p. 1349-54Article in journal (Refereed)
    Abstract [en]

    Factors influencing the accuracy and precision for diaphragm-free Karl Fischer coulometric determinations of low mu g-amounts of water have been studied using the Metrohm 756 (pulsed current) coulometer and eight different types of commercial coulometric reagents and some modifications of these. As in the case of diaphragm-free coulometric titration of large amounts of water, the positive errors, due to the formation of oxidizable reduction products (of sulfur dioxide) in the cathode reaction (besides hydrogen), were found to be minimized by the use of highest possible pulse current (in the range 100-400 mA) in combination with the fastest possible titration rate. Most accurate (102-103%) and precise results (typical relative standard deviation 1.8%) were obtained for reagents containing very large concentrations of imidazole in combination with the presence of modifiers like hexanol, chloroform and propylene glycol (i.e. the HYDRA-POINT reagents). Similar results were obtained when this type of reagent was mixed 60/40 with xylene according to the ASTM recommendation for water determinations in petroleum products like crude and lubricating oils. Addition of decanol to this type of reagent mixture was found to reduce the influence from the oxidative reduction products significantly. A reduction of the error from 3.6% relative to 1.6% was achieved by addition of 9% (v/v) of decanol to a 60/40 reagent mixture of HYDRA-POINT Coulometric Gen (containing hexanol as modifier) and xylene. For larger concentrations of decanol the pulse current had to be lowered to 100 mA and this might explain why no further improvement was observed. An additional attempt to minimize the interference by lowering the concentration of sulfur dioxide in the reagents gave no significant effect. However. by means of a home-built computer-controlled coulometric instrumentation based on continuous instead of pulsed current (including a large cathodic current density) it was possible to achieve recovery rates close to 100% for the best reagents investigated. The reason for this improvement is discussed.

  • 14.
    Larsson, William
    et al.
    Umeå University, Faculty of Science and Technology, Chemistry.
    Cedergren, Anders
    Investigation of Amine-Buffered Amide Reagents for Coulometric Karl Fischer Titration2009In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 78, no 4-5, p. 1452-1457Article in journal (Refereed)
    Abstract [en]

    Formamide (FA), N-methylformamide (NMF), and dimethylformamide (DMF),were evaluated as solvents for coulometric Karl Fischer (KF) reagents in combination with several amine bases. Except for the effect of the iodine species (iodine or triiodide), the pH of the reagent and the position of the sulfur dioxide/ hydrogen sulfite equilibrium were found to be the main factors explaining the large difference in the observed reaction rates betweenwater and the KF reagent in these solvents. Acid–base titrations showed that hydrogen sulfite is the main sulfur reactant in these media. The results will be of great importance in finding suitable combinations of base and solvent with respect to stoichiometry, side reactions caused by active carbonyl compounds, and reagent stability.

  • 15.
    Larsson, William
    et al.
    Umeå University, Faculty of Science and Technology, Chemistry.
    Jalbert, Jocelyn
    Gilbert, Roland
    Cedergren, Anders
    Umeå University, Faculty of Science and Technology, Chemistry.
    Efficiency of methods for Karl Fischer determination of water in oils based on oven evaporation and azeotropic distillation2003In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 75, no 6, p. 1227-32Article in journal (Refereed)
    Abstract [en]

    The efficiency of azeotropic distillation and oven evaporation techniques for trace determination of water in oils has recently been questioned by the National Institute of Standards and Technology (NIST), on the basis of measurements of the residual water found after the extraction step. The results were obtained by volumetric Karl Fischer (KF) titration in a medium containing a large excess of chloroform (> or = 65%), a proposed prerequisite to ensure complete release of water from the oil matrix. In this work, the extent of this residual water was studied by means of a direct zero-current potentiometric technique using a KF medium containing more than 80% chloroform, which is well above the concentration recommended by NIST. A procedure is described that makes it possible to correct the results for dilution errors as well as for chemical interference effects caused by the oil matrix. The corrected values were found to be in the range of 0.6-1.5 ppm, which should be compared with the 12-34 ppm (uncorrected values) reported by NIST for the same oils. From this, it is concluded that the volumetric KF method used by NIST gives results that are much too high.

  • 16.
    Larsson, William
    et al.
    Umeå University, Faculty of Science and Technology, Chemistry.
    Panitz, Jan-Christoph
    Cedergren, Anders
    Umeå University, Faculty of Science and Technology, Chemistry.
    Interference-free coulometric titration of water in lithium bis(oxalato)borate using Karl Fischer reagents based on N-methylformamide2006In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 69, no 1, p. 276-280Article in journal (Refereed)
    Abstract [en]

    A non-alcoholic coulometric reagent based on N-methylformamide (NMF) was shown to eliminate the severe interference effect caused by the alcohol component of the conventional Karl Fischer (KF) reagent on the battery electrolyte lithium bis(oxalato)borate (LiBOB). For sample amounts up to 240 μg of water, the stoichiometry of the KF reaction deviated only slightly from the ideal 1:1 ratio for the best reagent composition. Both solid and dissolved (in acetonitrile, tetrahydrofuran (THF), and ethylene carbonate/ethyl methyl carbonate) LiBOB were titrated successfully using a Metrohm 756 KF Coulometer with a diaphragm cell. The detection limit was estimated to be 0.5–1 μg of water using 100 ml of reagent in this system.

  • 17.
    Lundmark, Lars
    et al.
    Umeå University, Faculty of Science and Technology, Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Chemistry.
    Improving quality and comparability of environmental parameters in transboundary waters between Russia, Lithuania, Latvia and Belarus2006Report (Other (popular science, discussion, etc.))
  • 18.
    Ngoc Pham, Tung
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Univ Danang, Univ Sci & Technol, Dept Chem, 54 Nguyen Luong Bang, Lien Chieu, Danang, Vietnam.
    Sharifi, Tiva
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Sandström, Robin
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Siljebo, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kordas, Krisztian
    Wågberg, Thomas
    Umeå University, Faculty of Science and Technology, Department of Physics.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Åbo Akad Univ, Dept Chem Engn, Proc Chem Ctr, Ind Chem & React Engn, FI-20500 Turku, Finland.
    Robust hierarchical 3D carbon foam electrode for efficient water electrolysis2017In: Scientific Reports, ISSN 2045-2322, E-ISSN 2045-2322, Vol. 7, article id 6112Article in journal (Refereed)
    Abstract [en]

    Herein we report a 3D heterostructure comprising a hierarchical macroporous carbon foam that incorporates mesoporous carbon nanotubes decorated with cobalt oxide nanoparticles as an unique and highly efficient electrode material for the oxygen evolution reaction (OER) in electrocatalytic water splitting. The best performing electrode material showed high stability after 10 h, at constant potential of 1.7 V vs. RHE (reversible hydrogen electrode) in a 0.1 M KOH solution and high electrocatalytic activity in OER with low overpotential (0.38 V vs RHE at 10 mA cm(-2)). The excellent electrocatalytic performance of the electrode is rationalized by the overall 3D macroporous structure and with the firmly integrated CNTs directly grown on the foam, resulting in a large specific surface area, good electrical conductivity, as well as an efficient electrolyte transport into the whole electrode matrix concurrent with an ability to quickly dispose oxygen bubbles into the electrolyte. The eminent properties of the three-dimensional structured carbon matrix, which can be synthesized through a simple, scalable and cost effective pyrolysis process show that it has potential to be implemented in large-scale water electrolysis systems.

  • 19. Reinik, Janek
    et al.
    Heinmaa, Ivo
    Kirso, Uuve
    Kallaste, Toivo
    Ritamäki, Johannes
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Boström, Dan
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics, Energy Technology and Thermal Process Chemistry.
    Pongrácz, Eva
    Huuhtanen, Mika
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Keiski, Riitta
    Kordás, Krisztián
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Alkaline modified oil shale fly ash: Optimal synthesis conditions and preliminary tests on CO(2) adsorption2011In: Journal of Hazardous Materials, ISSN 0304-3894, E-ISSN 1873-3336, Vol. 196, p. 180-186Article in journal (Refereed)
    Abstract [en]

    Environmentally friendly product, calcium-silica-aluminum hydrate, was synthesized from oil shale fly ash, which is rendered so far partly as an industrial waste. Reaction conditions were: temperature 130 and 160°C, NaOH concentrations 1, 3, 5 and 8M and synthesis time 24h. Optimal conditions were found to be 5M at 130°C at given parameter range. Original and activated ash samples were characterized by XRD, XRF, SEM, EFTEM, (29)Si MAS-NMR, BET and TGA. Semi-quantitative XRD and MAS-NMR showed that mainly tobermorites and katoite are formed during alkaline hydrothermal treatment. Physical adsorption of CO(2) on the surface of the original and activated ash samples was measured with thermo-gravimetric analysis. TGA showed that the physical adsorption of CO(2) on the oil shale fly ash sample increases from 0.06 to 3-4mass% after alkaline hydrothermal activation with NaOH. The activated product has a potential to be used in industrial processes for physical adsorption of CO(2) emissions.

  • 20. Reinik, Janek
    et al.
    Heinmaa, Ivo
    Ritamäki, Johannes
    Boström, Dan
    Umeå University, Faculty of Science and Technology, Department of Applied Physics and Electronics.
    Pongracz, Eva
    Huuhtanen, Mika
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Keiski, Riitta
    Kordas, Krisztian
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    DIRECT CO2 SEQUESTRATION ONTO ALKALINE MODIFIED OIL SHALE FLY ASH2014In: Gorûcie slancy, ISSN 0208-189X, E-ISSN 1736-7492, Vol. 31, no 1, p. 79-90Article in journal (Refereed)
    Abstract [en]

    The present study focuses on the direct chemical adsorption of CO2 onto alkaline hydrothermally activated oil shale fly ash (OSFA). The CO2 chemisorption experiments were conducted in a high-pressure reactor at a temperature of 150 degrees C and CO2 partial pressure of 100 bar during a 24-hour period. Original, activated and chemisorbed OSFA samples were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) coupled with energy-dispersive X-ray spectroscopy (EDS), specific surface area (BETN2) and high-resolution Si-29 magic angle spinning nuclear magnetic resonance (MAS-NMR). The results indicated moderate weight increase (max 5 wt%) and according to XRD and MAS-NMR analysis tobermorites had reacted with CO2, leading to calcite formation. The results also show that the alkaline hydrothermally activated OSFA has a potential to be used in industrial processes for direct chemical adsorption of CO2 from flue gases.

  • 21.
    Samikannu, Ajaikumar
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Golets, MikhailUmeå University, Faculty of Science and Technology, Department of Chemistry.Larsson, WilliamUmeå University, Faculty of Science and Technology, Department of Chemistry.Shchukarev, AndreyUmeå University, Faculty of Science and Technology, Department of Chemistry.Kordas, KrisztianUmeå University, Faculty of Science and Technology, Department of Chemistry. Microelectronics and Materials Physics Laboratories, University of Oulu, FIN-90570 Oulu, Finland.Leino, Anne-RiikkaMicroelectronics and Materials Physics Laboratories, University of Oulu, FIN-90570 Oulu, Finland.Mikkola, Jyri-PekkaUmeå University, Faculty of Science and Technology, Department of Chemistry. Åbo Akademi University, Åbo, Finland.
    Dehydroisomerization of α-pinene over metal supported Si-SBA-15 mesoporous molecular sieves2013Conference proceedings (editor) (Refereed)
    Abstract [en]

    The effective dispersion of active metal species on mesoporous Si-SBA-15 is acquired by means of deposition-precipitation method.  In order to achieve this, the surface of Si-SBA-15 was first modified with TiO2 via grafting method, followed by deposition-precipitation method (DP) to obtain a fine dispersion of metallic nanoparticles over TiO2 modified Si-SBA-15. The structural features of the synthesized materials were characterized by means of X-ray diffraction (XRD), nitrogen sorption (BET), XPS and HR-TEM. A valuable platform chemical, p-cymene, was produced over the prepared catalyst by dehydroisomerization of α-pinene under vapour-phase conditions. A stable catalyst for one-spot synthesis of renewable p-cymene from α-pinene was developed.

  • 22.
    Samikannu, Ajaikumar
    et al.
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Golets, Mikhail
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Kordas, Krisztian
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Microelectronics and Materials Physics Laboratories, University of Oulu, FIN-90570 Oulu, Finland.
    Leino, A-R
    Microelectronics and Materials Physics Laboratories, University of Oulu, FIN-90570 Oulu, Finland.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Effective dispersion of Au and Au-M (M = Co, Ni, Cu and Zn) bimetallic nanoparticles over TiO2 grafted SBA-15: their catalytic activity on dehydroisomerization of α-pinene2013In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 173, p. 99-111Article in journal (Refereed)
    Abstract [en]

    Mesostructured siliceous SBA-15 was synthesized via direct hydrothermal crystallization from acidic solution of poly-(ethylene glycol)-block-poly(propylene glycol)-block poly(ethylene glycol)-copolymer and tetraethyl orthosilicate. The amorphous surface of the calcined Si-SBA-15 was modified with 20wt.% of TiO2 by chemical grafting method using titanium isopropoxide as the titanium source in ethanol solution. Various metal nanoparticles Au, Au-M (M = Co, Ni, Cu and Zn) were supported on TiO2/SBA-15 by deposition-precipitation method (DP) using urea as the precipitating agent. The structural features of the synthesized materials were characterized by various physico-chemical techniques such as X-ray diffraction, nitrogen sorption, XPS and HR-TEM. BET results of Si-SBA-15 revealed the formation of mesoporous structure with an average pore size of 5.9nm, pore volume of 1.12 cm3/g and the specific surface area of 846 m2/g. HR-TEM results demonstrated that metal nanoparticles were highly dispersed over TiO2/SBA-15 and long range ordering of hexagonal mesopores of Si-SBA-15 was well retained after loading of 20 wt.% TiO2 and 3 wt.% of bimetallic nanoparticles. The catalytic performances of the prepared catalysts were studied on dehydroisomerization of α-pinene under gas phase conditions using hydrogen atmosphere. The stability and catalytic activity of Au-M-TiO2/SBA-15 (DP) catalysts upon conversion of α-pinene in to p-cymene was explored in comparison with the catalysts prepared by conventional method. AuNi-TiO2/SBA-15 catalysts prepared via DP method were found to be stable upon longer reaction time as well as superior in terms of conversion and selective towards the formation of p-cymene.

  • 23. Wu, Ming-Chung
    et al.
    Hiltunen, Jussi Tapio
    Sápi, András
    Avila, Anna
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Liao, Hsueh-Chung
    Huuhtanen, Mika
    Tóth, Géza
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Laufer, Noémi
    Kukovecz, Akos
    Konya, Zoltan
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Keiski, Riitta
    Su, Wei-Fang
    Chen, Yang-Fang
    Jantunen, Heli
    Ajayan, Pulickel M
    Vajtai, Robert
    Kordás, Krisztián
    Nitrogen-doped anatase nanofibers decorated with noble metal nanoparticles for photocatalytic production of hydrogen2011In: ACS NANO, Vol. 5, no 6, p. 5025-5030Article in journal (Refereed)
    Abstract [en]

    We report the synthesis of N-doped TiO2 nanofibers and high photocatalytic efficiency in generating hydrogen from ethanol-water mixtures under UV-A and UV-B irradiation. Titanate nanofibers synthesized by hydrothermal method are annealed in air and/or ammonia to achieve N-doped anatase fibers. Depending on the synthesis route, either interstitial N atoms or new N-Ti bonds appear in the lattice resulting in slight lattice expansion as shown by XPS and HR-TEM analyses, respectively. These nanofibers were then used as support for Pd and Pt nanoparticles deposited with wet impregnation followed by calcination and reduction. In the hydrogen generation tests the N-doped samples were clearly outperforming their un-doped counterparts showing remarkable efficiency not only under UV-B but also with UV-A illumination. Applying 100 mg catalyst (N-doped TiO2 nanofiber decorated with Pt nanoparticles) in 1 L water-ethanol mixture the H2 evolution rates were as high as 700 μmol/h (UV-A) and 2250 μmol/h (UV-B) corresponding to photo energy percentages of ~3.6% and ~12.3%, respectively.

  • 24. Wu, Ming-Chung
    et al.
    Liao, Hsueh-Chung
    Cho, Yu-Cheng
    Hsu, Che-Pu
    Lin, Ting-Han
    Su, Wei-Fang
    Sapi, Andras
    Kukovecz, Akos
    Konya, Zoltan
    Shchukarev, Andrey
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Sarkar, Anjana
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Larsson, William
    Umeå University, Faculty of Science and Technology, Department of Chemistry.
    Mikkola, Jyri-Pekka
    Umeå University, Faculty of Science and Technology, Department of Chemistry. Åbo Akademi University, Åbo-Turku, Finland.
    Mohl, Melinda
    Toth, Geza
    Jantunen, Heli
    Valtanen, Anna
    Huuhtanen, Mika
    Keiski, Riitta L.
    Kordas, Krisztian
    Photocatalytic activity of nitrogen-doped TiO2-based nanowires: a photo-assisted Kelvin probe force microscopy study2013In: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 16, no 1, p. Article Number: UNSP 2143-Article in journal (Refereed)
    Abstract [en]

    In this study, a set of nitrogen-doped TiO2-based nanomaterials demonstrating photocatalytic activity was developed by combining the efforts of lattice doping and metal nanoparticle decoration and tested for photo-degradation of methylene blue dye by applying solar simulator irradiation. The surface potential shifts of these TiO2-based photocatalytic nanomaterials measured by Kelvin probe force microscope have been used to study the degree of electron generation of the photocatalysts after irradiation and were well correlated with the photocatalytic activity. The nitrogen-doped TiO2 nanowires decorated with Pt nanoparticles can induce obvious electron accumulation and result in a large shift of surface potential. The analysis shows a clear correlation between the surface potential shift and the photodegradation activity. Furthermore, a thorough comparative photocatalytic activity study combined with X-ray photoelectron spectroscopy analysis of the materials-doped with nitrogen under various conditions-reveals that the photocatalytic efficiency of the catalysts is maintained even if the lattice doping is leached e.g., by thermal treatments after doping. By monitoring the surface potential shifts of various TiO2-based photocatalysts by photo-assisted Kelvin probe force microscopy, we obtain a useful tool for developing novel materials with high photocatalytic activity.

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