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Spectrometric Methods for Research of Humic Substances
Enev, Vojtěch ; Maršálek, Roman (referee) ; Sýkorová, Ivana (referee) ; Klučáková, Martina (advisor)
The main aim of doctoral thesis is the study on physicochemical properties of humic substances (HS) by modern instrumental techniques. The subject of the study were HS isolated from South Moravian lignite, South Bohemian peat, forest soil Humic Podzol and finally extract from brown sea algae Ascophyllum nodosum. With respect on determination of structure and reactivity of these unique “biocolloids”, standard samples (Leonardite HA, Elliott Soil HS and Pahokee Peat HS) were also studied. These samples were obtained from International Humic Substances Society (IHSS). All mentioned substances were characterized by elemental analysis (EA), molecular absorption spectroscopy in ultraviolet and visible region (UV/Vis), infrared spectroscopy with Fourier transformation (FTIR), nuclear magnetic resonance spectroscopy of carbon isotope 13C (LS 13C NMR), steady-state and time resolved fluorescence spectroscopy. Obtained fluorescence, UV/Vis and 13C NMR spectra were used for calculation of fluorescence and absorption indexes, values of specific absorbance and structural parameters respectively, which were used for fundamental characterization of these “biocolloidal” compounds. Infrared spectroscopy with Fourier transformation was utilized for the identification of functional groups and structural units of HS. Evaluation of infrared spectra is quiet complicated by overlapping of absorption bands especially in fingerprint region. This problem was overcome by Fourier self-deconvolution (FSD). Steady-state fluorescence spectroscopy was used for deeper characterization of HS with respect to origin, structural units, amount of substituents with electron-donor and electron-acceptor effects, content of reactive functional groups, “molecular” heterogeneity, the degree of humification, etc. Parameters of complexation of samples Elliott Soil with heavy metal ions (Cu2+, Pb2+ and Hg2+) were obtained by using modified Stern-Volmer equation. These ions were chosen purposefully, because the interaction of HS with these ions is one of the fundamental criteria for the assessment of the reactivity of HS. Key part of the whole doctoral thesis is time-resolved fluorescence spectroscopy. It is able to determine the origin of emission of HS by method Time-Resolved Area Normalized Emission Spectra (TRANES). The viscosity of micro medium about excited fluorophores of HS was determined by Time-Resolved Emission Spectra (TRES).
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Anthracology and NMR spectroscopy in Palaeoecological Research of Chernozems
Danková, Lenka ; Šefrna, Luděk (advisor) ; Chuman, Tomáš (referee)
This thesis deals with black carbon, its characteristic features and with its occurrence in chernozemic soils. In particular, this thesis deals with methods, which can study presence of black carbon in soils. The presence of black carbon and the whole composition of soil organic matter of three chernozemic soils in Czechia (Zeměchy, Tursko, Syrovice) is examined by 13 C NMR spectroscopy. Anthracological analysis of charcoal from fossil chernozems of Zemechy loess ravine deals with pedogenesis of chernozems and development of Quaternary vegetation in Central Europe. Coniferous tree species of Pinus sp., Pinus cf. cembra, Larix/Picea, Juniperus a Vaccicium, i.e. cold- and drought-tolerant taxa, were identified by anthracological analysis of soils of Zemechy loess ravine. The identified species suggest that the landscape around Zemechy was probably formed by parkland taiga. According to 13 C NMR spectroscopy, soil organic matter of fossil chernozem of Zemechy loess ravine consists particularly of alkyl and O-alkyl carbon. Aromatic carbon is also significant. O-alkyl carbon is the most important in the recent chernozems of Tursko and Syrovice. Aromatic carbon has the smallest proportion in both chernozems. The presence of aromatic carbon in chernozem of Tursko is the smallest of all analyzed soils. The...
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Anthracology and NMR spectroscopy in Palaeoecological Research of Chernozems
Danková, Lenka ; Šefrna, Luděk (advisor) ; Chuman, Tomáš (referee)
This thesis deals with black carbon, its characteristic features and with its occurrence in chernozemic soils. In particular, this thesis deals with methods, which can study presence of black carbon in soils. The presence of black carbon and the whole composition of soil organic matter of three chernozemic soils in Czechia (Zeměchy, Tursko, Syrovice) is examined by 13 C NMR spectroscopy. Anthracological analysis of charcoal from fossil chernozems of Zemechy loess ravine deals with pedogenesis of chernozems and development of Quaternary vegetation in Central Europe. Coniferous tree species of Pinus sp., Pinus cf. cembra, Larix/Picea, Juniperus a Vaccicium, i.e. cold- and drought-tolerant taxa, were identified by anthracological analysis of soils of Zemechy loess ravine. The identified species suggest that the landscape around Zemechy was probably formed by parkland taiga. According to 13 C NMR spectroscopy, soil organic matter of fossil chernozem of Zemechy loess ravine consists particularly of alkyl and O-alkyl carbon. Aromatic carbon is also significant. O-alkyl carbon is the most important in the recent chernozems of Tursko and Syrovice. Aromatic carbon has the smallest proportion in both chernozems. The presence of aromatic carbon in chernozem of Tursko is the smallest of all analyzed soils. The...
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Spectrometric Methods for Research of Humic Substances
Enev, Vojtěch ; Maršálek, Roman (referee) ; Sýkorová, Ivana (referee) ; Klučáková, Martina (advisor)
The main aim of doctoral thesis is the study on physicochemical properties of humic substances (HS) by modern instrumental techniques. The subject of the study were HS isolated from South Moravian lignite, South Bohemian peat, forest soil Humic Podzol and finally extract from brown sea algae Ascophyllum nodosum. With respect on determination of structure and reactivity of these unique “biocolloids”, standard samples (Leonardite HA, Elliott Soil HS and Pahokee Peat HS) were also studied. These samples were obtained from International Humic Substances Society (IHSS). All mentioned substances were characterized by elemental analysis (EA), molecular absorption spectroscopy in ultraviolet and visible region (UV/Vis), infrared spectroscopy with Fourier transformation (FTIR), nuclear magnetic resonance spectroscopy of carbon isotope 13C (LS 13C NMR), steady-state and time resolved fluorescence spectroscopy. Obtained fluorescence, UV/Vis and 13C NMR spectra were used for calculation of fluorescence and absorption indexes, values of specific absorbance and structural parameters respectively, which were used for fundamental characterization of these “biocolloidal” compounds. Infrared spectroscopy with Fourier transformation was utilized for the identification of functional groups and structural units of HS. Evaluation of infrared spectra is quiet complicated by overlapping of absorption bands especially in fingerprint region. This problem was overcome by Fourier self-deconvolution (FSD). Steady-state fluorescence spectroscopy was used for deeper characterization of HS with respect to origin, structural units, amount of substituents with electron-donor and electron-acceptor effects, content of reactive functional groups, “molecular” heterogeneity, the degree of humification, etc. Parameters of complexation of samples Elliott Soil with heavy metal ions (Cu2+, Pb2+ and Hg2+) were obtained by using modified Stern-Volmer equation. These ions were chosen purposefully, because the interaction of HS with these ions is one of the fundamental criteria for the assessment of the reactivity of HS. Key part of the whole doctoral thesis is time-resolved fluorescence spectroscopy. It is able to determine the origin of emission of HS by method Time-Resolved Area Normalized Emission Spectra (TRANES). The viscosity of micro medium about excited fluorophores of HS was determined by Time-Resolved Emission Spectra (TRES).
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