XRPD

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Deutsch

Mit dieser Arbeit liegt die erste grundlegende Aufarbeitung zu den Warenarten aus Essens Früh- und Hochmittelalter vor. Anhand der Materialaufnahme kann die ersten Einteilungen der Scherben in die unterschiedlichen Warenarten vorgenommen werden. Diese Einteilung wird mit Hilfe der Pulverdiffraktometrie (XRPD) bestätigt. In diesem Zuge können auch Erkenntnisse über die Brenntemperaturen und die Tonzusammensetzungen gewonnen werden. Durch die Analyse der Tonzusammensetzungen kann ebenfalls belegt werden, dass die Pingsdorfer Ware wie auch die Badorfer und Hunneschans Ware aus dem gleichen Ton gefertigt wurden, der sich jedoch deutlich von den Essener Waren unterscheidet. In diesem Zuge können einige hier vorgelegte Warenarten als einheimische Essener Ware angesprochen werden. Eine weiterführende Abgrenzung gegenüber der Duisburger Ware bleibt jedoch noch zu erbringen.

Die Keramiken lassen sich des Weiteren auch ihrem Gebrauch nach unterteilen. So sind Badorfer, Hunneschans und Pingdorfer Ware vorwiegend Trink- und Schankgefäße, die im 13.Jh.n.Chr. vom Siegburger (Fast-)Steinzeug abgelöst werden, während die einheimische Essener Ware die Funktion der Kochkeramik übernimmt.

In der Verbindung aus archäometrischen Analysen, archäologischer und keramikkundlicher Forschung, unter Berücksichtigung der wenigen historisch belegten Quellen, kann in dieser Arbeit eine Darstellung des mittelalterlichen Alltags als „menschliches Leben inmitten der materiellen Kultur“ [Goetz, 2002, 14] und damit ein Beitrag zur frühen Essener Stadtgeschichte geleistet werden.

Als Beitrag zur frühen Essener Stadtgeschichte und damit zum Forschungsbereich der Archäologie des Mittelalters kann diese Arbeit leider nur die Hälfte der hier normalerweise zu betrachtenden Paradigmen [Frommer, 2007, 89] behandeln. Die Ansprache der Befunde kann für diese Grabung wohl niemals eindeutig geklärt werden. Ebenso und genau aus diesem Grund lassen sich kaum Schlüsse siedlungsarchäologischer Natur ziehen. Jedoch sind die Paradigmen, die Funde betreffend, ergiebig. Hier kann vor allem etwas zur Alltags-, Sozial- und Wirtschaftsgeschichte beigetragen werden. Handel und Import wie auch lokale Produktion, deren Bestellung durch das Stift und der Gebrauch der unterschiedlichen Waren im Alltag können hier eingehend dargestellt werden.


Englisch

This work is the first overview over ceramic typs from Essen's early and high Middle Ages. First the material was classified into different types. This classification is confirmed using powder diffractometry (XRPD). In this process, informations about firing temperatures and clay compositions can also be obtained. Analysis of the clay compositions also show that Pingsdorfer ware as well as  Badorfer and Hunneschans ware were made from the same clay, which differs significantly from the Essen ware. In this context, some of the types presented here can be addressed as native Essen ware. However, a further demarcation from Duisburg ware remains to be achieved.

The ceramics can also be divided according to their use. Badorfer, Hunneschans and Pingdorfer ware are mainly drinking and dispensing vessels that were made in the 13th century AD. replaced by (almost-)stoneware from Siegburg, while local ware from Essen takes over the function of cooking ceramics.

In combination of archaeometric analysis, archaeological research and research in ceramic, taking into account the few historically documented sources, this work can present medival everyday life as “human life in material culture” [Goetz, 2002, 14]  and thus makes it contribution on the early history of Essen.

As a contribution to the early history of Essen and thus to research of archeology of Middle Ages, this work can unfortunately only deal with half of the paradigms [Frommer, 2007, 89] normally to be considered here. Defining of findings can probably never be clearly clarified for this excavation. Likewise and precisely for this reason, it is difficult to draw conclusions of a settlement-archaeological nature. However, the paradigms regarding to finds are productive. Above all, something can be contributed to everyday, social and economic history. Trade and import as well as local production, their ordering by the "convent" and use of different wares in everyday life can be described in detail here.

Through a combined use of experimental and theoretical approaches such as XRPD, EXAFS, IR, and UV−vis spectroscopies and ab initio periodic DFT calculations, we report a detailed characterization of structural, vibrational, and electronic properties of UiO-66 (Zr-BDC MOF) in its hydroxylated and dehydroxylated forms. The stability of the materials with respect to the most common solvents, acids, and bases is determined by combining XRPD and TGA/MS techniques. The structures of the two forms of UiO-66 are refined through an interactive XRPD/EXAFS approach and validated by ab initio calculations. Experimental and calculated IR spectra are reported and compared to enlighten the nature of vibrational modes upon dehydroxylation and to show the complete reversibility of the dehydration/hydration phenomenon. Experimental and calculated band gaps are also reported and compared. In this work, we show the necessity to combine, in a synergic way, different experimental techniques and periodic ab initio approaches to disclose and fully understand the nature of complex novel materials such as UiO-66 on structural, vibrational, and electronic grounds. The correct structure refinement could not be possible using one of these three approaches alone, in particular, XRPD data were unable to detect an important distortion of the Zr6O6 units of the dehydrated material that was, however, foreseen in the ab initio calculations and measured in the EXAFS spectra.

Naringenin is a flavonoid specific to citrus fruits and possesses anti-inflammatory, anticarcinogenic, and antitumour effects. But due to a lower half-life and rapid clearance from the body, frequent administration of the molecule is required. To improve the bioavailability and prolong its duration in body system, its phospholipid complexes were prepared by a simple and reproducible method. Naringenin was complexed with phosphatidylcholine in equimolar ratio, in presence of dichloromethane. The prepared Phytosomes (naringenin–phospholipid complex) were evaluated for various physical parameters like FT-IR spectroscopy, Differential Scanning Calorimetry (DSC), X-ray powder diffractometry (XRPD), Solubility, Scanning Electron Microscopy (SEM) and the in vitro drug release study. These phospholipid complexes of naringenin were found to be irregular and disc shaped with rough surface in SEM. Drug content was found to be 91.7% (w/w). FTIR, 1H NMR, DSC and XRPD data confirmed the formation of phospholipid complex. Water solubility of naringenin improved from 43.83 to 79.31 μg/mL in the prepared complex. Unlike the free naringenin (which showed a total of only 27% drug release at the end of 10 h), naringenin complex showed 99.80% release at the end of 10 h of dissolution study. Thus it can be concluded that the phospholipid complex of naringenin may be of potential use for improving bioavailability.

The present study deals with the characterization of a ceramic assemblage from the 17 Late Mycenaean (Late Helladic III) settlement of Kastrouli, at Desfina near Delphi, Central Greece 18 using various analytical techniques. Kastrouli is located in a strategic position supervising the Mes-19 okampos plateau and the entire peninsula and is related to other nearby coeval settlements. In total 20 40 ceramic sherds and 8 clay raw materials were analyzed through mineralogical, petrographic and 21 microstructural techniques. Experimental briquettes (DS) made from clayey raw materials collected 22 in the vicinity of Kastrouli, were fired under temperatures (900 and 1050 o C) in oxidizing conditions 23 for comparison with the ancient ceramics. The petrographic analysis performed on thin sections 24 prepared from the sherds has permitted the identification of six main fabric groups and a couple of 25 loners. The aplastic inclusions recognized in all fabric groups but one confirmed the local ...

The present study deals with the characterization of a ceramic assemblage from the Late Mycenaean (Late Helladic III) settlement of Kastrouli, at Desfina near Delphi, Central Greece using various analytical techniques. Kastrouli is located in a strategic position supervising the Mesokampos plateau and the entire peninsula and is related to other nearby coeval settlements. In total 40 ceramic sherds and 8 clay raw materials were analyzed through mineralogical, petrographic and microstructural techniques. Experimental briquettes (DS) made from clayey raw materials collected in the vicinity of Kastrouli, were fired under temperatures (900 and 1050 °C) in oxidizing conditions for comparison with the ancient ceramics. The petrographic analysis performed on thin sections prepared from the sherds has permitted the identification of six main fabric groups and a couple of loners. The aplastic inclusions recognized in all fabric groups but one confirmed the local provenance since they are rel...

The settlement of Sorgenti della Nova, dating to the Late Bronze Age, is characterized by a proto-urban spatial organization, hosting a series of complex structures, among which sub-elliptic wooden/straw huts, artificial caves, animal enclosures, warehouses and service structures. As part as this last category, 5 ovens has been found in the site, both within and nearby the huts, very likely used for food processing and cooking. This paper presents preliminary results of experimental and archeometric research. In particular the astonishing state of preservation of oven 1 provided precious data for a pilot-experiment, testing hypotheses about building techniques and the relationship between shape and materials related to the thermal behavior. XRD analyses carried out on a few samples from ovens 3 and 5 added new data about the composition of the material used for the construction.

The present study deals with the characterization of a ceramic assemblage from the Late Mycenaean (Late Helladic III) settlement of Kastrouli, at Desfina near Delphi, Central Greece using various analytical techniques. Kastrouli is located in a strategic position supervising the Mesokampos plateau and the entire peninsula and is related to other nearby coeval settlements. In total 40 ceramic sherds and 8 clay raw materials were analyzed through mineralogical, petrographic and microstructural techniques. Experimental briquettes (DS) made from clayey raw materials collected in the vicinity of Kastrouli, were fired under temperatures (900 and 1050 °C) in oxidizing conditions for comparison with the ancient ceramics. The petrographic analysis performed on thin sections prepared from the sherds has permitted the identification of six main fabric groups and a couple of loners. The aplastic inclusions recognized in all fabric groups but one confirmed the local provenance since they are rel...

Detailed analysis of the C K near-edge X-ray absorption fine structure (NEXAFS) spectra of a series of saccharides (fructose, xylose, glucose, galactose, maltose mono-hydrate, α-lactose monohydrate, anhydrous β-lactose, cellulose) indicates that the precise determination of IPs and σ* shape resonance energies is sensitive enough to distinguish different crystalline saccharides through the variations in their average C−OH bond lengths. Experimental data as well as FEFF8 calculations confirm that bond length variations in the organic solid state of 0.01 Å can be experimentally detected, opening up the possibility to use NEXAFS for obtaining incisive structural information for molecular materials, including noncrystalline systems without long-range order such as dissolved species in solutions, colloids, melts, and similar amorphous phases. The observed bond length sensitivity is as good as that originally reported for gas-phase and adsorbed molecular species. NEXAFS-derived molecular structure data for the condensed phase may therefore be used to guide molecular modeling as well as to validate computationally derived structure models for such systems. Some results indicate further analytical value in that the σ* shape resonance analysis may distinguish hemiketals from hemiacetals (i.e., derived from ketoses and aldoses) as well as α from β forms of otherwise identical saccharides.

A multi-analytical approach focus on the archaeometric characterization of plaster from temple C, and two elite houses belong to the late chalcolithic 3-4 (3800-3400 B.C), period VII in Arslantepe – Turkey, a site located in the Malatya plain, 5 km away from the city center and 15 km away from the Euphrates right bank, is done using three different methods: optical microscopy (OM) in thin section under polarizing microscopy to define petrographic features in terms of plaster fabric texture and structure as well as the type, percentage, ratio grain size and distribution of the added aggregate and inclusions Micro-morphological analysis has been carried out by Scanning Electron Microscopy coupled with Energy Dispersive Spectroscopy (SEM-EDS) to define the fabric , inclusions and the secondary product in the pores . a mineralogical analysis by X-ray powder diffraction (XRPD) has been carried out also to identify the quantitative and qualitative mineralogical composition of the samples. In a result a marly limestone has been determine as a plaster raw material which probably came from two different source (local and other imported from different part of Malatya plain). Moreover, different aggregate selection, and diffirent technological levels were also detected in the samples, that are probably related to the level or the purpose (function) of the buildings. An evidence of a re-plastering process was also detected in the two elite houses, which probably refer to a routine maintenance process.

The settlement of Sorgenti della Nova, dating to the Late Bronze Age, is characterized by a proto-urban spatial organization, hosting a series of complex structures, among which sub-elliptic wooden/straw huts, artificial caves, animal enclosures, warehouses and service structures. As part as this last category, 5 ovens has been found in the site, both within and nearby the huts, very likely used for food processing and cooking. This paper presents preliminary results of experimental and archeometric research. In particular the astonishing state of preservation of oven 1 provided precious data for a pilot-experiment, testing hypotheses about building techniques and the relationship between shape and materials related to the thermal behavior. XRD analyses carried out on a few samples from ovens 3 and 5 added new data about the composition of the material used for the construction.

Prehistoric pottery decorated with incisions or impressions filled with white and seldom coloured inlays is well documented in the archaeological literature, but the related in-depth archaeometric studies are sporadic. 43 decorated ceramic shards, dating from the Neolithic to the Bronze Age, and an Iron Age fibula from the archaeological site of Castello di Annone (Piedmont, North-Western Italy) were analysed with FTIR, Raman and XRPD for characterization of the ornamental pigments forming these inlays. Few white components were used as fillers, namely talc and bone ash (hydroxyapatite – Bone White), often as a mixture and seldom accompanied by other pigments (i.e. kaolinite and presumably secondary calcite). Comparison with freshly-heated biogenic hydroxyapatite proved that ancient Bone White pigment was calcined at about 900 °C. Such a process was kept separate from pottery firing as these white mixtures show absence of talc degradation by-products and sporadic presence of kaolini...

Different solid state and sol–gel preparations of undoped and Mn substituted cathode material LiFePO4 are investigated. Li3PO4, Fe2P2O7 and Li4P2O7 are detected and quantified by XRPD only in solid state synthesis. In addition, micro-Raman spectra reveal low amount of different iron oxides clusters. EPR data, combined with the results of magnetization measurements, evidence signals from Fe3+ ions in maghemite nanoclusters, and in Li3Fe2(PO4)3. The sol–gel synthesis, showing the lowest amount of impurity phases, seems the most suitable to obtain a promising cathode material. The structural refinement gives new insights into the cation distribution of the Mn doped triphylite structure: (i) about 85% of Mn2+ ions substitutes Fe2+, the remaining 15% being located on the Li site, thus suggesting a structural disorder also confirmed by EPR and micro-Raman results; (ii) Mn ions on the Li site are responsible for the observed slight cell volume expansion.The combined use of different spectroscopic, structural and magnetic techniques has been successfully applied to characterize structure, cation distribution and physical properties of undoped and Mn substituted triphylite and to evaluate the impurity phases formation.