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| 2. |
- Törnkvist, Anna, et al.
(författare)
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Interference of the electrospray voltage on chromatographic separations using porous graphitic carbon columns
- 2004
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Ingår i: Journal of Mass Spectrometry. - : Wiley. - 1076-5174 .- 1096-9888. ; 39:2, s. 216-222
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Tidskriftsartikel (refereegranskat)abstract
- The electrospray ionization (ESI) voltage is shown to interfere with liquid chromatographic separations performed with packed porous graphitic carbon (PGC) capillary columns. This interference is ascribed to the presence of an electric field over the conductive column in the absence of an earth point between the column and the ESI emitter. The current evolved alters the chromatographic behavior of the catecholamine metabolite 3-O-methyl-DOPA significantly, as both peak splitting and a dramatic decrease in the retention time were observed. Furthermore, the response from the mass spectrometer was decreased by 33% at the same time. A related compound, tyrosine, exhibited decreased retention times but no peak splitting, whereas no shifts in the retention times (or peak splitting) were seen for the less retained dopamine and noradrenaline. When the current through the PGC column was eliminated by the use of an earth point between the column and the ESI emitter, the chromatographic behavior of the column was found to return slowly to normal after hours of equilibration with 60 : 40 (v/v) methanol-ammonium formate buffer of pH 2.9. The behavior of the PGC column with and without the earth point was found to be highly reproducible during a period of 1 month. We propose that the effect of the ESI voltage on the chromatographic behavior of the PGC column is due to associated redox reactions affecting both the PGC particles and the analytes. It is concluded that (for analytical reasons), care should be taken to ensure that no current is flowing through the chromatographic system when interfacing PGC columns, and conducting parts in general, to ESI mass spectrometry.
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| 3. |
- Zettersten, Camilla, et al.
(författare)
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The influence of the thin-layer flow cell design on the mass spectra when coupling electrochemistry to electrospray ionisation mass spectrometry
- 2006
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Ingår i: Journal of Electroanalytical Chemistry. - : Elsevier BV. - 0022-0728 .- 1873-2569 .- 1572-6657. ; 590:1, s. 90-99
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Tidskriftsartikel (refereegranskat)abstract
- The influence of the flow cell configuration on the mass spectra obtained when coupling an electrochemical thin-layer flow cell to electrospray mass spectrometry (ESI-MS) has been investigated. It is shown that interferences due to the electrochemical reaction on the counter electrode and/or the absence of 100% conversion efficiency can alter the mass spectra when conventional thin-layer flow cells are used in conjunction with ESI-MS. The effects, which affect the intensities and distribution of the peaks in the mass spectra, can result in the inability to detect products formed at the working electrode. Comparisons of mass spectra, generated after the electrochemical oxidation of a dinuclear Mn complex (where bpmp = 2,6-bis[bis(2-pyridylmethyl) amino]methyl-4-methylphenol) using two different thin-layer flow cells clearly show that the potential dependence and appearance of the mass spectra depend on the flow cell configuration used. The use of a modified thin-layer flow cell, in which the counter electrode had been separated from the working electrode, gave rise to significantly increased intensities for the oxidised MnIII,IV state of the complex. With the conventional unmodified cell, the corresponding complex was only seen for considerably higher oxidation potentials. The different results can be explained by the reduced risk of redox cycling and interferences due to species generated at the counter electrode with the modified cell. As interferences due to the counter electrode reactions likewise may be expected with many coulometric flow cells, the electrochemical cell design clearly needs to be considered when using electrochemistry coupled to ESI-MS to study electrochemical reactions.
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| 4. |
- Andersen, Jesper N, et al.
(författare)
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Strong Phonon Replicas in Be 1 s Photoemission Spectra
- 2001
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Ingår i: Physical Review Letters. - 1079-7114. ; 86:19, s. 4398-4401
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Tidskriftsartikel (refereegranskat)abstract
- The Be 1s core level photoemission line from metallic Be is shown to contain unexpected internal fine structure. We argue that this fine structure is caused by intrinsic excitation of a narrow band of optical phonons in the 1s photoemission process. The general importance of the present results for high resolution core level photoemission investigations of metals is pointed out.
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| 5. |
- Andersen, J. N., et al.
(författare)
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Strong phonon replicas in Be 1s photoemission spectra
- 2001
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Ingår i: Physical Review Letters. - 0031-9007 .- 1079-7114. ; 86:19, s. 4398-4401
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Tidskriftsartikel (refereegranskat)abstract
- Strong phonon replicas in Be 1s photoemission spectra were investigated. The fine structure caused by intrinsic excitation of a narrow band of optical phonons was discussed in the 1s photoemission proces. The excitations of the optical Be phonons in the photoemission process caused fine structures. It was found that the phonon replicas in Be metal were strong due to large size misfit between neutral and core-ionized Be.
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| 6. |
- Andersson, Claes-Henrik, 1980-, et al.
(författare)
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Synthesis and characterization of a ferrocene-linked bis-fullerene[60] dumbbell
- 2012
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Ingår i: Dalton Transactions. - 1477-9226 .- 1477-9234. ; 41:8, s. 2374-2381
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Tidskriftsartikel (refereegranskat)abstract
- A new [60]fullerene dumbbell consisting of two fulleropyrrolidines connected to a central ferrocene unit by amide linkages has been prepared and fully characterized by elemental analysis, 1H NMR, UV/Vis, fluorescence and mass spectrometry. The electrochemical properties as determined by cyclic voltammetry show ground state electronic communication between the ferrocene and the fullerene units. In addition, the preparaton of a ferrocene building block for an alternative linking approach is presented.
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| 7. |
- Andersson, Matilda, et al.
(författare)
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Deposition and characterization of magnetron sputtered amorphous Cr-C films
- 2012
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Ingår i: Vacuum. - : Elsevier BV. - 0042-207X .- 1879-2715. ; 86:9, s. 1408-1416
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Tidskriftsartikel (refereegranskat)abstract
- Thin films in the Cr-C system with carbon content of 25-85 at.% have been deposited using non-reactive DC magnetron sputtering from elemental targets. Analyses with X-ray diffraction and transmission electron microscopy confirm that the films are completely amorphous. Also, annealing experiment show that the films had not crystallized at 500 degrees C. Furthermore, X-ray spectroscopy and Raman spectroscopy show that the films consist of two phases, an amorphous CrCx phase and an amorphous carbon (a-C) phase. The presence of two amorphous phases is also supported by the electrochemical analysis, which shows that oxidation of both chromium and carbon contributes to the total current in the passive region. The relative amounts of these amorphous phases influence the film properties. Typically, lower carbon content with less a-C phase leads to harder films with higher Young's modulus and lower resistivity. The results also show that both films have lower currents in the passive region compared to the uncoated 316L steel substrate. Finally, our results were compared with literature data from both reactively and non-reactively sputtered chromium carbide films. The comparison reveals that non-reactive sputtering tend to favour the formation of amorphous films and also influence e.g. the sp(2)/sp(3) ratio of the a-C phase.
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| 8. |
- Asfaw, Habtom D., et al.
(författare)
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Boosting the thermal stability of emulsion–templated polymers via sulfonation : an efficient synthetic route to hierarchically porous carbon foams
- 2016
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Ingår i: ChemistrySelect. - : Wiley. - 2365-6549. ; 1:4, s. 784-792
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Tidskriftsartikel (refereegranskat)abstract
- Hierarchically porous carbon foams with specific surface areas exceeding 600 m2 g−1 can be derived from polystyrene foams that are synthesized via water-in-oil emulsion templating. However, most styrene-based polymers lack strong crosslinks and are degraded to volatile products when heated above 400 oC. A common strategy employed to avert depolymerization is to introduce potential crosslinking sites such as sulfonic acids by sulfonating the polymers. This article unravels the thermal and chemical processes leading up to the conversion of sulfonated high internal phase emulsion polystyrenes (polyHIPEs) to sulfur containing carbon foams. During pyrolysis, the sulfonic acid groups (-SO3H) are transformed to sulfone (-C-SO2-C-) and then to thioether (-C−S-C-) crosslinks. These chemical transformations have been monitored using spectroscopic techniques: in situ IR, Raman, X-ray photoelectron and X-ray absorption near edge structure spectroscopy. Based on thermal analyses, the formation of thioether links is associated with increased thermal stability and thus a substantial decrease in volatilization of the polymers.
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| 9. |
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| 10. |
- Asfaw, Habtom Desta
(författare)
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Multifunctional Carbon Foams by Emulsion Templating : Synthesis, Microstructure, and 3D Li-ion Microbatteries
- 2017
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- Carbon foams are among the existing electrode designs proposed for use in 3D Li-ion microbatteries. For such electrodes to find applications in practical microbatteries, however, their void sizes, specific surface areas and pore volumes need be optimized. This thesis concerns the synthesis of highly porous carbon foams and their multifunctional applications in 3D microbatteries. The carbon foams are derived from polymers that are obtained by polymerizing high internal phase water-in-oil emulsions (HIPEs).In general, the carbonization of the sulfonated polymers yielded hierarchically porous structures with void sizes ranging from 2 to 35 µm and a BET specific surface area as high as 630 m2 g-1. Thermogravimetric and spectroscopic evidence indicated that the sulfonic acid groups, introduced during sulfonation, transformed above 250 oC to thioether (-C-S-) crosslinks which were responsible for the thermal stability and charring tendency of the polymer precursors. Depending on the preparation of the HIPEs, the specific surface areas and void-size distributions were observed to vary considerably. In addition, the pyrolysis temperature could also affect the microstructures, the degree of graphitization, and the surface chemistry of the carbon foams.Various potential applications were explored for the bespoke carbon foams. First, their use as freestanding active materials in 3D microbatteries was studied. The carbon foams obtained at 700 to 1500 oC suffered from significant irreversible capacity loss during the initial discharge. In an effort to alleviate this drawback, the pyrolysis temperature was raised to 2200 oC. The resulting carbon foams were observed to deliver high, stable areal capacities over several cycles. Secondly, the possibility of using these structures as 3D current collectors for various active materials was investigated in-depth. As a proof-of-concept demonstration, positive active materials like polyaniline and LiFePO4 were deposited on the 3D architectures by means of electrodeposition and sol-gel approach, respectively. In both cases, the composite electrodes exhibited reasonably high cyclability and rate performance at different current densities. The syntheses of niobium and molybdenum oxides and their potential application as electrodes in microbatteries were also studied. In such applications, the carbon foams served dual purposes as 3D scaffolds and as reducing reactants in the carbothermal reduction process. Finally, a facile method of coating carbon substrates with oxide nanosheets was developed. The approach involved the exfoliation of crystalline VO2 to prepare dispersions of hydrated V2O5, which were subsequently cast onto CNT paper to form oxide films of different thicknesses.
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