Investigation of C3 S hydration mechanism by transmission electron microscope (TEM) with integrated Super-XTM EDS system.

Tricalciumsilicate (C3 S, Alite) is the major component of the Portland cement clinker. Hydration of Alite is decisive in influencing the properties of the resulting material. This is due to its high content in cement. The mechanism of the hydration of C3 S is very complicated and not yet fully understood. There are different models describing the hydration of C3 S in various ways. In this work for a better understanding of hydration mechanism, the hydrated C3 S was investigated by using the transmission electron microscope (TEM) and for the first time, the samples for the investigations were prepared by using of focused ion beam from sintered pellets of C3 S. Also, an FEI Talos F200x with an integrated Super-X EDS system was used for the investigations. FEI Talos F200X combines outstanding high-resolution S/TEM and TEM imaging with energy dispersive X-ray spectroscopy signal detection, and 3D chemical characterization with compositional mapping. TEM is a very powerful tool for material science. A high energy beam of electrons passes through a very thin sample, and the interactions between the electrons and the atoms can be used to observe the structure of the material and other features in the structure. TEM can be used to study the growth of layers and their composition. TEM produces high-resolution, two-dimensional images and will be used for a wide range of educational, science and industry applications. Chemical analysis can also be performed. The purpose of these investigations was to get the information about the composition of the C-S-H phases and some details of the nanostructure of the C-S-H phases.

Investigation of C3S hydration by environmental scanning electron microscope.

Tricalciumsilicate (C(3)S, Alite) is the major component of the Portland cement clinker, The hydration of the Alite is decisive for the properties of the resulting material due to the high content in cement. The mechanism of the hydration of C(3)S is very complicated and not yet fully understood. There are some models that describe the hydration of C(3)S in various ways. The Environmental Scanning Electron Microscopy (ESEM) working in gaseous atmosphere enables high-resolution dynamic observations of structure of materials, from micrometre to nanometre scale. This provides a new perspective in material research. ESEM significantly allows imaging of specimen in their natural state without the need for special preparation (coating, drying, etc.) that can alter the physical properties. This paper presents the results of our experimental studies of hydration of C(3)S using ESEM. The ESEM turned out to be an important extension of the conventional scanning microscopy. The purpose of these investigations is to gain insight of hydration mechanism to determine which hydration products are formed and to analyze if there are any differences in the composition of the hydration products.

Evaluation of the sulfate dynamics in groundwater by means of environmental isotopes.

Elevated sulfate concentrations and their heterogeneous distribution in the drinking water catchment area Torgau-Mockritz (Germany) were investigated by means of multiple isotope signatures such as 834S, delta18O-H2O, deltaD, tritium, and 85K5r. delta34S values of the groundwater sulfate vary between -19...+ 37 per thousand CDT. No simple correlation exists between sulfate concentrations and delta34S. Superimposition of different sulfur sources and mobilization processes combined with a complicated groundwater movement create a complex distribution pattern. The oxidation of reduced sedimentary sulfur has to be regarded as a main source of dissolved sulfate at least regionally. Tritium and 14C data revealed that old groundwater can be excluded as source for high sulfate contents. Correlated temporal variations in the concentrations of tritium and sulfate are observed in deeper sampling positions. Highly variable delta18O and 8D, as detected in parts of the catchment area, indicate local influences of surface water infiltration into the aquifer. The spatial distribution of isotope signatures enables the identification of zones with descending younger water or hindered groundwater movement and hence provides useful hints for flow modeling.

Vibrational analysis of iron and zinc phosphate conversion coating constituents.

The FT-MIR/FT-FIR and NIR-FT-Raman spectra of orthorhombic alpha-Zn3(PO4)2 x 4H2O (alpha-hopeite) and monoclinic Zn2Fe(PO4)2 x 4H2O (phosphophyllite), including deuterated samples, have been measured in the polycrystalline state at room temperature and below. The distribution of vibrational levels was related to the results of complete unit-cell group analyses. The number of uncoupled OD stretching modes of alpha-hopeite (isotopically dilute samples) strongly exceeds that expected from the number of hydrogen positions of the structure reported. In contrast, unequivocal assignment of the four hydrogen bonds of phosphophyllite has been performed. The distortion of the phosphate tetrahedra, as revealed from both site group and unit-cell group splitting of the PO stretching modes, is found to be almost equal in both compounds, in accordance with the identical tetrahedral linkage scheme.

[Determining the size of the specific surface of bone substitutes with gas adsorption]. / Bestimmung der Grösse der spezifischen Oberfläche von Knochenersatzmaterialien mittels Gasadsorption.

The surface area and the microporosity of bone regeneration materials influence their chemical and biological properties. Therefore, the size of the specific surface area and the distribution of the pore diameters (pores < 1 micron) of bone regeneration materials were analyzed within this study. The analyzed hydroxyapatites were of synthetic, bovine, and phytotroph origin. The tricalcium phosphates and the bioglasses included only synthetic materials. The gas adsorption of each specimen was analyzed using a volumetric N2/Kr system (ASAP 2010, Micromeritics). Additionally, for materials with a specific surface area (> 2 m2/g) the pore size distribution was evaluated by the BJH-method. Two of the materials evaluated astonishingly large dimensions of the specific surface area (BioOss 79.7 m2/g, Algipore new 14.6 m2/g). A medium surface area was found for Algipore old (4.9 m2/g) and Interpore200 (2.64 m2/g). All other included materials showed only small sizes of the specific surface area (Ceros80 1.8 m2/g, Ceros82 1.31 m2/g, Cerasorb 1.2 m2/g, Biobase 0.7 m2/g, Endobone 0.7 m2/g, Perioglas 0.6 m2/g, Allotropat50 0.23 m2/g, Biogran 0.2 m2/g). The materials with large and medium sizes of the specific surface area evaluated the following pore diameters: BioOss 2-50 nm, Algipore new 2-100 nm, Algipore old 5-50 nm, Interpore200 2-100 nm. Pore sizes less than 2 nm were not found in relevant numbers. The materials BioOss, old and new Algipore, and Interpore200 contain a large interconnecting mesopore system (diameter < 1 micron). For the materials Biobase, Endobone, Perioglas, Allotropat 50, and Biogran this cannot be assumed. The materials Ceros80, Ceros82, and Cerasorb evaluated a specific surface area between those and might include only a small part of these interconnecting pores. An influence of the interconnecting porosity and the different sizes of the specific surface areas on the biological behavior of the bone regeneration materials can be suggested.

[Roentgen spectrometry comparison of currently available bone substitutes]. / Röntgenspektrometrischer Vergleich der aktuell verfügbaren Knochenersatzmaterialien.

INTRODUCTION: The crystalline structure of hydroxyapatite (HA) and tricalciumphosphate (TCP) used as bone regeneration materials affects their physical and probably also their biological properties. Varying velocities of the HA solution process seem to be correlated to different results in powder diffraction analysis (RDX) [1], a validated, routine procedure in minerology [2, 6] to analyse crystallized materials. As far we know there are no comparative RDX analyses for the TCP materials in clinical use. GOALS: The dimension and quality of the crystallization of several bone regeneration materials are analysed by RDX. MATERIAL AND METHODS: The materials analysed were divided in different groups: hydroxyapatite, tricalciumphosphate and bioglass. The materials are characterized by the specific intensity curve measurements. RESULTS: The HA products, with the exception of Algipore, seem to be monophasic. Ceros80 and Endobone were the only ones which seem to be totally crystallized. The TCP products Biobase and Cerasorb are nearly monophasic, whereas Ceros82 seems to contain a mixture of 30% HA and 70% beta-TCP. All TCPs show a high crystallization. The bioglasses did--as suspected--not show crystalline structures. DISCUSSION: There are many possible causes for inhomogeneous crystallization of the investigated materials, as they are composites of different foreign ions, extremely small crystals or abnormal (deficient) apatites. How this affects the biological behaviour is not known. SUMMARY: We found differences between the examined materials; how this affects the biological behaviour is unknown. Further investigations are necessary to correlate the characteristics of the materials to the clinical outcome.

Mineral- und heilwässer in sachsen - eine isotopenanalytische charakterisierung.

Abstract The groundwaters studied and labelled as mineral water were "natural mineral waters" for bottled waters and "natural curative waters" for heal therapeutical applications. They were characterized either by a specific mineralization or their suitability for balneology. To reveal the actual hydrological situation isotope investigations using (2)H, (18)O, (3)H, (12)C and (14)C (DIC) and (34)S (sulphate) were included in a study describing samples of 24 mineral water deposits in Saxonia. The water was classified into 4 hydrochemical types of genesis. Due to different hydrogeological and hydrochemical situations widely scattered isotope ratios were measured. Most of the investigated mineral waters are containing at least parts of younger waters (with residence times less than about 40 years). Correlations between chemical composition and the tritium content could be observed within different springs from the areas Bad Brambach, Bad Elster and Burkhardswalde. Strong variations in δ(34)S were found in samples with low sulphate content, showing different sulphur sources, as well as microbiological reactions. On the other hand mineral waters from Bad Brambach and Bad Elster show nearly the same δ(34)S value of about 6‰ CDT despite beeing of a different chemical type. The δ(13)C values between -22 and -2.2y PDB are related to different sources of CO(2).

[Reports and clarification of "critical incidents" as promoting factors in psychotherapy. A process-efficiency study between psychodynamic and client-centered treatment of patients]. / Berichte über und Klärung von "kritischen Ereignissen" als Wirkfaktoren in der Psychotherapie. Eine Prozess-Effizienz-Studie zwischen psychodynamisch und klientzentriert behandelten Patienten.

Our investigation assays if (i) the patient's thematization of and (ii) the attained degree of psychological clarification of "critical incidents" (sensu Rice & Saperia) covariate with favourable outcomes of psychotherapies. The sample consisted of 16 short psychotherapies (maximum 30 sessions), half of which treated with client centered (= CC) and the other half with psychodynamic (= PT) psychotherapy. These had been classified in a previous investigation (on the basis of questionnaire scores in 5 points in time, covering 12 years) into 8 differing time courses. Significant results are: "Critical incidents" were more often found in PT than in CC, reciprocally "psychological clarification" was higher in CC. In sessions rated "good" and in the 10 "ameliorating" time courses "critical incidents" were more frequent than in their respective countergroup. A crass exception was furnished by the "deteriorating" subgroup's quite high frequencies.