Calorimetric determination of the effect of additives on cement hydration process

Possibilities of a multicell isoperibolic-semiadiabatic calorimeter application for the measurement of hydration heat and maximum temperature reached in mixtures of various compositions during their setting and early stages of hardening are presented. Measurements were aimed to determine the impact of selected components?? content on the course of ordinary Portland cement (OPC) hydration. The following components were selected for the determination of the hydration behaviour in mixtures: very finely ground granulated blast furnace slag (GBFS), silica fume (microsilica, SF), finely ground quartz sand (FGQ), and calcined bauxite (CB). A commercial polycarboxylate type superplasticizer was also added to the selected mixtures. All maximum temperatures measured for selected mineral components were lower than that reached for cement. The maximum temperature increased with the decreasing amount of components in the mixture for all components except for silica fume. For all components, except for CB, the values of total released heat were higher than those for pure Portland cement samples.     

Role of reaction atmosphere in preparation of potassium tantalate through sol–gel method

Potassium tantalate (KT) thin films and powders of both K₂Ta₂O₆ (KT pyrochlore) and KTaO₃ (KT perovskite) structures were prepared by means of chemical solution deposition method using Si(111) with ZnO and MgO buffer layers as a substrate. The influence of reaction atmosphere on reaction pathway and phase composition for both KT powders, and KT thin films has been studied mainly by means of powder diffraction and infrared spectroscopy. When an oxygen flow instead of static air atmosphere has been used the process of pyrolysis in oxygen runs over much narrower temperature interval (200–300 °C), relatively to air atmosphere (200–600 °C) and almost no (in case of powders), or no (in case of thin films) pyrochlore intermediate phase has been detected in comparison with treatment in air, where the pyrochlore phase is stable at temperatures 500–600 °C (powders). KT perovskite phase starts to crystallize at temperatures 50° and 150 °C lower compared to air atmosphere in case of powders and thin films, respectively. Microstructure formed by near-columnar grains and small grains of equiaxed shape was observed in films treated in oxygen and air atmosphere, respectively.     

Dispersion measurements using time-of-flight remote detection MRI

Remote detection nuclear magnetic resonance and magnetic resonance imaging can be used to study fluid flow and dispersion in a porous medium from a purely Eulerian point of view (i.e., in a laboratory frame of reference). Information about fluid displacement is obtained on a macroscopic scale in a long-time regime, while local velocity distributions are averaged out. It is shown how these experiments can be described using the common flow propagator formalism and how experimental data can be analyzed to obtain effective porosity, flow velocity inside the porous medium, fluid dispersion and flow tracing of fluid.     

Determination of mercury species using thermal desorption analysis in AAS

Analytical aspects of the determination of inorganic mercury (Hg) species by thermal desorption followed by atomic absorption spectrometry (AAS) detection were investigated in this work. Characteristic Hg release curves of the following species were observed: Hg⁰, HgCl₂, HgO, HgSO₄, HgS, and the Hg bound to humic acids. Particular attention was dedicated to the thermal stability and change of bond of Hg⁰ in the following matrices: sand, kaolinite, granite, peat, power plant ash, and soil. The bond of elemental Hg in environmental materials was described on basis of this experiment. Contaminated soil samples from two locations in the Czech Republic were investigated by thermal desorption analysis. Afterwards, the contents of volatile and plant-available Hg in the studied samples were determined. The determination of Hg⁰ using the thermal method was related to the results of liquid sequential extraction. The development of Hg speciation and the stability of Hg were assessed on basis of the data obtained. Thus, the analytical procedure used is a suitable tool for the study of inorganic Hg species in contaminated soils.     

Rare-earth Metal Borosilicides R9Si15–xB3 (R = Tb,Yb): New Ordered Structures Derived from the AlB2 Structure Type

Two novel ternary borosilicides R₉Si_15–xB₃ (R = Tb, x = 1.80, R = Yb, x = 1.17) were synthesized from the initial elements using tin flux method. Their crystal structures were determined by means of X-ray single crystal diffraction. Both refer to space group R32, Z = 1: a = 6.668(2) Å, c = 12.405(4) Å [R₁ = 0.027, wR₂ = 0.031 for 1832 reflections with I_o > 2σ (I_o)] for Tb₉Si_15–xB₃, and a = 6.5796(3) Å, c = 12.2599(5) Å [R_F = 0.052, wR = 0.090 for 1369 reflections with I_o > 2σ (I_o)] for Yb₉Si_15–xB₃. The structures represent a new structure type, derived from that of AlB₂, with ordering in the metalloid sublattice resulting in distorted [Si₅B] hexagons. The presence or absence of boron in this ordered structure is discussed on the basis of difference Fourier syntheses, interatomic distances, structural analysis, and theoretical calculations in relation with the parent structures of the binaries AlB₂ and Yb₃Si₅ (Th₃Pd₅ type of structure). Theoretical calculations show substantial covalent interactions between the metal and nonmetal elements. The small percentage of silicon atoms, which are missing in these nonstoichiometric compounds, probably allows strengthening boron-metal and boron-silicon bonding.     

An Enzymatic N-Acylation Step Enables the Biocatalytic Synthesis of Unnatural Sialosides

Chitin is one of the most abundant and cheaply available biopolymers in Nature. Chitin has become a valuable starting material for many biotechnological products through manipulation of its N-acetyl functionality, which can be cleaved under mild conditions using the enzyme family of de-N-acetylases. However, the chemoselective enzymatic re-acylation of glucosamine derivatives, which can introduce new stable functionalities into chitin derivatives, is much less explored. Herein we describe an acylase (CmCDA from Cyclobacterium marinum) that catalyzes the N-acylation of glycosamine with a range of carboxylic acids under physiological reaction conditions. This biocatalyst closes an important gap in allowing the conversion of chitin into complex glycosides, such as C5-modified sialosides, through the use of highly selective enzyme cascades.