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Structure of soil organic matter (SOM) is a hot topic of discussion among scientific community for several decades. The mostly discussed models, among many, are polymer model and supramolecular model. While the former considers SOM as macromolecules consisting of amorphous and crystalline domains, the latter explains SOM as a physicochemical entity dominated by weak hydrophobic and H-bond interactions in the secondary level, which holds individual molecules of primary structure together. The weak forces in secondary level impart characteristic mobility of SOM. Very important consequence of this multidimensional formulation is that physicochemical structure plays a crucial role in most biogeochemical functions of SOM, apart from the chemical composition. Recently introduced concept of cation and water molecule mediated bridges between OM molecular segments (CaB and WaMB, respectively) evolved from physicochemical understanding of SOM structure. Even though several indirect evidences were produced for CaB and WaMB during last years, no clear-cut understanding of these processes has been achieved yet. Experimental difficulty due to overlapping effects of equally important CaB-governing parameters such a pH and competing cations raises huge challenge in investigating CaB-related influences. This thesis, therefore, aims to validate an experimental set-up for inducing CaB within OM structures and assessing it from various chemical and physicochemical aspects.
The method involved removal of omnipresent cations and adjustment of pH before cation addition. This helped to separate pH effects and cation effects. Based on results obtained on two different types of organic matter, it can be deduced that multivalent cations can cross-link SOM, given that functional group density of the SOM material is enough for the functional groups to be arranged in sufficient spatial proximity to each other. Physicochemical structural reorganisation during aging causes formation of more and/or stronger CaB and WaMB. As for inducing CaB directly after cation treatment, cationic size and valency were found determinant also for aging effect. A strongly cross-linked system in the beginning is less vulnerable to structural changes and undergoes aging with lower intensity, than an initially weakly cross-linked system. Responsible for the structural changes is, the inherent mobility of SOM within its physicochemical assemblage. Thus the information on structural requirement of CaB and its consequences on OM matrix rigidity will help to obtain insight into the physicochemical SOM structure. Additionally, organic matter quality (assessed by thermal analysis) and pore structure of SOM formed in a set of artificial soils showed that mineral materials are important for the chemical nature of SOM molecules, but not for the physical structure of organo-mineral associations, at least after several months of SOM development.
Furthermore, nanothermal analysis using atomic force microscopy (AFM-nTA) was implemented in soils for the first time to reveal nanoscale thermal properties and their spatial distribution in nano- and micrometer scales. This helped to identify physicochemical processes, such as disruption of WaMB, in low-organic soils, in which bulk methods fail due to their low sensitivity. Further, various types of materials constituting in soils were distinguished with high resolution by advanced application of the method, in combination with other AFM parameters. Attempts were done to identify various materials, with the usage of defined test materials. Above all, the method is potent to reveal microspatial heterogeneity on sample surfaces, which could help understanding process-relevant hotspots, for example.
This thesis thus contributes to the scientific understanding on physicochemical structural dynamics via cross-linking by cations and via nanoscale thermal properties. Direct investigation on CaB demonstrated here will potentially help making a big leap in knowledge about the interaction. The observed aging effects add well to the understanding of supramolecular consideration of SOM. By introducing nanothermal analysis to the field of soil science, it is made possible to face the problem of heterogeneity and spatial distribution of thermal characteristics. Another important achievement of AFM-nTA is that it can be used to detect physicochemical processes, which are of low intensity.
The polysaccharide hydration phenomenon is nowadays the subject of intense research. The interaction of native and modified polysaccharides and polysaccharides-based bioconjugates with water has an important influence on their functional behaviour. Notwithstanding that the hydration phenomenon has been studied for decades, there is still a lack of awareness about the influence of hydration water on the polysaccharide´s structure and consequences for industrial or medicinal applications. The hydration of polysaccharides is often described by the existence of water layers differing in their physical properties depending on the distance from the polysaccharide. Using the differential scanning calorimetry (DSC) such water layers were categorized according their properties upon cooling in hyaluronan (HYA, sodium salt of ß-1,4-linked units of ß-1,3-linked D-glucuronic acid and N-acetyl-D-glucosamine), a model polysaccharide in the present work. The amount of non-freezing water, i.e. water in close proximity of HYA chain which does not freeze et all, was determined around 0.74gH2O/gHYA for HYA with molecular weight from 100 to 740kDa and 0.84gH2O/gHYA for molecular weight of 1390kDa. The amount of freezing-bound water, the water pool which is affected by presence of HYA but freezes, was determined in the range from 0.74 to 2gH2O/gHYA. Above this value only non-freezing and bulk water are present since melting enthalpy measured above this concentration reached the same value as for pure water. Since this approach suffers from several experimental problems, a new approach, based on the evaporation enthalpy determination, was suggested. The analysis of the evaporation enthalpies revealed an additional process associated with apparent energy release taking part below the water content of 0.34gH2O/gHYA. Existence of this phenomenon was observed also for protonated form of HYA. The existence of energy compensating process was confirmed with the Kissinger-Akahira-Sunose method which allowed determination of actual water evaporation/desorption enthalpies in all stages of the evaporation process. In fact, the apparent evaporation enthalpy value increased until water content of 0.34gH2O/gHYA, and then dropped down to lower values which were, still higher than the value of the pure water evaporation enthalpy. By the use of time domain nuclear magnetic resonance (TD-NMR) technique it was revealed that this phenomenon is the plasticisation of HYA.
Further, it was revealed that the non-freezing water determined by the use of DSC consists of two water fractions, i.e. 15% of water structurally integrated, interacting directly with polar sites, and 85% of water structurally restricted, embedded in-between the HYA chains. The occurrence of plasticisation concentration close to equilibrium moisture content provided the possibility to influence the HYA physical structure during the drying. In this way three samples of native HYA, dried under various conditions were prepared and their physical properties were analyzed. The samples differed in kinetics of rehydration, plasticisation concentration, glass transitions, and morphology. The properties of water pool were studied in solutions of 10"25mg HYA/mL as well. The fast filed cycling (FFC) NMR relaxometry showed the existence of three water fractions which correlation times spanned from 10"6 to 10"10 seconds, progressively decreasing in dependency on its distance from HYA chain. The formation of a weak and transient intramolecular water bridge between HYA chains was observed. It was shown that, unlike the inorganic electrolytes, polyelectrolytes hydration is a dynamic process which reflects not only the technique used for the analysis, experimental conditions but also the conformation of the polysaccharide and its "thermal" and "hydration" history.
It was demonstrated that some native polysaccharide structures can be easily modified by manipulation of preparation conditions, giving fractions with specific physicochemical properties without necessity of any chemical modification.
Die Wirbelsäule als tragende Säule des menschlichen Körpers ist bei vielen Bewegungsabläufen hohen Belastungen ausgesetzt. Fehl- und Überbelastungen rufen dabei oft dauerhafte Schädigungen hervor. Daher ist es von Interesse, die innerhalb der Wirbelsäule auftretenden Belastungen zu bestimmen. Eine moderne und zuverlässige Methode zur Belastungsbestimmung ist der Aufbau eines Berechnungsmodells.
In der vorliegenden Arbeit wurde ein Mehr-Körper-System (MKS) Modell der Lendenwirbelsäule erstellt. Mit Hilfe des Modells können sowohl die übertragenen Kräfte und Momente in allen inneren Strukturen berechnet als auch die Kinematik des Bewegungsablaufs simuliert werden. Die Grundstruktur des Modells bilden die als Starrkörper angenommenen knöchernen Strukturen der fünf Lendenwirbel L1 bis L5, des Os Sacrums und des Os iliums, die über die Segmentierung eines CT-Datensatzes des Abgusses der Wirbeloberflächen eines durchschnittlich großen Europäers gewonnen wurden. Die elastischen Elemente der Wirbelsäule wurden unter Berücksichtigung ihrer physikalischen Eigenschaften in das Modell implementiert. Grundlage für die Modellierung der Zwischenwirbelscheiben waren dabei eigens durchgeführte experimentelle Messungen. Das charakteristische Kraft-Deformations-Verhalten der Ligamente wurde der Literatur entnommen.
Die Umsetzung im Computermodell berücksichtigt neben dem physikalischen Verhalten eines einzelnen Ligamentes zusätzlich durch einen Gewichtungsfaktor das Zusammenspiel aller Ligamente im komplex aufgebauten Ligamentapparat. Die Facettengelenke wurden durch Kontaktmodellierung in den Knorpelschichten realisiert. Daneben wurde ein Modell eines Implantatsystems entwickelt, das zur dynamischen Stabilisierung der Lendenwirbelsäule genutzt wird. Die Validierung der erstellten Modelle erfolgte über den Vergleich mit In-Vitro erhobenen Daten. Betrachtet wurden neben der intakten Wirbelsäule zudem degenerative Schädigungen der Zwischenwirbelscheibe und deren operative Versorgung durch Nukleotomie und dynamische Stabilisierung. Die Ergebnisse der Simulationen zeigen dabei eine sehr gute Näherung an die experimentell ermittelten Messwerte. Durch Anwendung der Computermodelle konnten die Auswirkungen verschiedener operativer Eingriffe, wie Interlaminotomie, Hemilaminektomie und Laminektomie auf die unterschiedlichen Strukturen der Lendenwirbelsäule berechnet werden. Ein weiteres Anwendungsgebiet lag in der Untersuchung des momentanen Drehzentrums. Neben der Bestimmung der Drehpunktbahn bei intakter Wirbelsäule konnten die Effekte einer degenerativ geschädigten und operativ versorgten Zwischenwirbelscheibe auf den Verlauf des momentanen Drehzentrums berechnet und simuliert werden.