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    Vibrational spectra of a ferrocenyl phosphine derivative chemisorbed on 3-aminopropylsilyl modified silica gel
    (Elsevier BV, 2013-11)
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    Madalska, Martyna
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    Hey-Hawkins, Evamarie
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    A direct method of quantification of maximal chemisorption of 3-aminopropylsilyl groups on silica gel using DRIFT spectroscopy
    (Elsevier BV, 2015-10-05)
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    Hey-Hawkins, Evamarie
    3-Aminopropylsilyl (APS) modified silica gel plays an important role as a precursor for further modifications, where APS acts as a spacer or bridging molecule. A monolayer of APS which is most suitable for this purpose was obtained in anhydrous conditions. The properties of the APS-modified silica gel depend on the amount of molecules chemisorbed on the surface. A direct quantitative method using Diffuse Reflectance Infrared Fourier Transform (DRIFT) spectroscopy was proposed. The obtained results were further supported by elemental analysis. The conclusion was that the proposed methodology can be used for the quantification of APS groups chemisorbed on silica gel when the grafting chemical reaction was mainly irreversible.
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    Crystal structure and spectroscopic determination of the phase transitions in methylammonium and formamidinium bismuth iodide perovskites
    (Elsevier, 2024-06-24)
    Understanding of the structural properties of hybrid organic–inorganic perovskites (HOIPs) and their behavior is crucial for their use as photovoltaics and for the design and assembly of solar cells. As part of this work, a detailed study was conducted to further understand bismuth iodide perovskites, with a specific focus on the phase transitions of methylammonium and formamidinium analogs. A detailed analysis of the temperature-dependent IR spectra was also performed in order to analyze the structural changes that occur. The presence of five phases in the methylammonium bismuth iodide (MABiI) and four phases in formamidinium bismuth iodide (FABiI) were determined. An additional confirmation of the reported results was obtained from the differential scanning calorimetry. The ambiguities concerning the crystal structure of FABiI were resolved based on the results by X- ray powder diffraction (XRPD)
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    Indirect quantitative IR assessment of maximal monomolecular deposition of 3-aminopropyltrimethoxysilane on silica gel surface
    (Society of Chemists and Technologists of Macedonia, 2014-12-01)
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    <jats:p>Quantification of the amount of maximum loaded 3-aminopropyltrimethoxysylil (APS) on a thermally pretreated silica gel (600 ºC) was performed using IR spectroscopy. A possibility to find the maximum load through a construction of a Langmuir isotherm was not possible due to the irreversibility of the chemisorption reaction. The method used in this work was based on the analysis of the toluene solution on the quantity of the non-reacted APTMS after the saturation of the silica gel surface with APS. The process of chemisorption was monitored via the increasing band intensity of CH<sub>2</sub> and NH­<sub>2</sub> modes of the adsorbent and decreasing band intensity characteristic for the free isolated OH groups of silica gel using DRIFT spectroscopy. The obtained results on maximum adsorption are in line with the previously obtained, using carbon elemental analysis and a direct DRIFT method.</jats:p>
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    Unmasking the Aliphatic Repertoire: New Polyunsaturated Metabolites in Bupleurum falcatum sensu lato Provide Chemotaxonomic Insights
    (MDPI AG, 2025-05-10)
    Nešić, Milica D.
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    Nešić, Milan S.
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    Raca, Irena Lj.
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    Radulović, Niko S.
    Bupleurum falcatum (Apiaceae) sensu lato includes multiple infraspecific taxa with longstanding taxonomic ambiguities, often resulting from incomplete morphological and chemical characterizations. Herein, diethyl ether extracts were analyzed from four Balkan populations that were tentatively identified as B. falcatum subsp. falcatum (syn. B. falcatum) and B. falcatum subsp. cernuum (syn. B. sibthorpianum). Comprehensive chro-matography and spectroscopic techniques (GC-MS and 1D/2D NMR) enabled the iso-lation of several newly identified aliphatic polyunsaturated esters, including com-pounds bearing uncommon conjugated tetraene and triyne backbones. These novel structures differ from canonical falcarinol derivatives by lacking the usual 3-hydroxylation, suggesting a divergent branch in the crepenynate pathway. The chemical profiles of each sample correlated closely with leaf morphology and infra-specific designations: for example, the Galičica Mt. population of B. falcatum featured a unique newly detected heptadecadientriyne, while the populations from Šar Planina and Suva Planina displayed distinct polyunsaturated repertoires. Extracts from B. sibthorpianum likewise contained stereoisomeric compounds that highlight metabolic divergence. Collectively, these findings demonstrate significant chemotypic variation within the Bupleurum falcatum complex and provide the first account of less-polar sec-ondary metabolites, including newly discovered polyunsaturated metabolites. Future research integrating molecular markers and bioactivity assays may elucidate how these specialized metabolites contribute to both the taxonomy and pharmacological potential of these understudied taxa.
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    Formation of WO3 thin films from RF sputtered tungsten films by air annealing: A cost-effective approach
    (National Library of Serbia, 2025)
    Jovanovski, Stefan
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    Popovic, Maja
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    Novakovic, Mirjana
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    Rajic, Vladimir
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    WO3 thin films were prepared by RF sputtering metallic tungsten onto glass substrates, followed by thermal oxidation through annealing in air. This technique is straightforward, cost-efficient, and time-effective, achieving high deposition rates of 16 nm/min on average at 200 W magnetron power for the highly homogeneous W-metallic films. SEM/EDX analysis showed that after annealing at 450ᵒC in air, the RF sputtered 269 nm thick metallic W films with a round grain morphology (~30 nm) turned into 420 nm thick nearly stoichiometric transparent WO3 (tungsten (VI) oxide) film, with a dramatically changed morphology of aggregated crystal rods approximately 1 μm long. XRD and Raman spectroscopy confirmed a biphasic crystal structure, with a dominant monoclinic phase and a minor tetragonal phase. XPS analysis revealed the characteristic W4f7/2 and W4f5/2 electron peaks associated with the W6+ oxidation state, with no evidence of W5+ species, indicating a stoichiometric nature of the WO3 films.