Thiol-functionalized nanobuilding blocks (NBBs) were synthesized from 3-mercaptopropyltrimethoxysilane by using the in situ water production (ISWP) process in which the water needed to hydrolyze the precursor was provided by means of an esterification reaction. In the present study the reaction between 1-propanol and chloroacetic acid was used. Whereas the growth of the Si oligomers was followed at room temperature and 100°C using 1D 29 Si and 2D 1 H-29 Si heteronuclear single quantum correlation (HSQC) NMR spectroscopic experiments, the amount of water delivered along the process was followed by means of 1 H NMR spectroscopy. The results show a good correlation between the evolution of the degree [a]
The first transparent silicon oxycarbide aerogel has been obtained through H2decarbonzation at 800 °C starting from an alkylene-bridged silicon alkoxide precursor.
Detailed crystallographic information provided by X-ray diffraction (XRD) is complementary to molecular information provided by Raman spectroscopy. Accordingly, the combined use of these techniques allows the identification of an unknown compound without ambiguity. However, a full combination of Raman and XRD results requires an appropriate and reliable reference database with complete information. This is already available for XRD. The main objective of this paper is to introduce and describe the recently developed Raman Open Database (ROD, http://solsa.crystallography.net/rod). It comprises a collection of high-quality uncorrected Raman spectra. The novelty of this database is its interconnectedness with other open databases like the Crystallography Open Database (http://www.crystallography.net/cod and Theoretical Crystallography Open Database (http://www.crystallography.net/tcod/). The syntax adopted to format entries in the ROD is based on the worldwide recognized and used CIF format, which offers a simple way for data exchange, writing and description. ROD also uses JCAMP-DX files as an alternative format for submitted spectra. JCAMP-DX files are compatible to varying degrees with most commercial Raman software and can be read and edited using standard text editors.
The identification of mineralogical phases in drill cores is one of the most challenging tasks in the mining activity in view of an efficient metal extraction. This process requires the analytical characterization of large volumes of material to obtain a complete set of data in a minimum of time. None of the commonly used methods in mineralogical analyses, such as IR‐based techniques, X‐rays fluorescence, and hyperspectral imaging, is capable to provide a fully satisfactory response for several reasons, the main one being the complexity of the ores. Moreover, the characterization is often conducted in remote laboratories and only on selected samples to limit the time waste. A possible alternative solution requires a multianalytical approach exploiting on‐field techniques. This strategy is currently being developed within SOLSA, a joint EU H2020 project, and consists of an automatic expert system coupling sonic drilling, imaging, profilometer, hyperspectral cameras, and a combination of Raman spectroscopy, X‐rays fluorescence, and X‐rays diffraction. In this work, the principles on which this cooperative approach is based are discussed, with application to two specific test samples, showing the potential and novelty of the method. In particular, a case is considered in which the sample characterization by the separate use of a single technique fails, whereas the combination of the three analyses (Raman spectroscopy, X‐rays fluorescence, and X‐rays diffraction) works even if the system is very complex.
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