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A simple and efficient method of preparing composites of carbon nanotubes and titania (CNT-TiO2) is reported via a microwave-assisted synthesis in an ionic liquid, [bmim][BF4]. CNT-TiO2 nanocomposites were formed by the thermal decomposition of titanium (IV) isopropoxide (Ti(OPri)4) in the presence of CNTs under microwave irradiation. The obtained product was characterized by BET surface area, XRD, SEM, and TEM. TiO2 particles with average size of 9 nm were as anatase. The surface area of the Composites increased with an increase of CNT content. Moreover, the catalytic efficiency of the composite was investigated through the photoelectrodegradation of methylene blue.
The graft polymerization of ε-caprolactone (ε-CL) onto magnetite was carried out under microwave irradiation in the presence of tin(II) 2-ethylhexanoate. The molar ratio of ε-CL to tin(II) 2-ethylhexanoate was 300, whereas the molar ratio of ε-CL to magnetite was 5. The chemical structures of the obtained poly(ε-caprolactone) coated magnetic nanoparticles were characterized by FTIR and XPS spectroscopy. These magnetic-polymer hybrid nanostructures were further investigated by X-ray diffraction and magnetization measurements. The morphology of the magnetic core-shell nanostructures were determined by TEM.
A series of phenolic-acid-based 2-oxazoline monomers with methoxysubstituted phenyl and cinnamyl side chains is synthesized and polymerized in a microwave reactor at 140 °C using methyl tosylate as the initiator. The obtained poly(2-oxazoline)s are characterized by NMR spectroscopy, MALDITOF mass spectrometry, and size-exclusion chromatography (SEC). Kinetic studies reveal that the microwave-assisted polymerization is fast and completed within less than ≈10 min for low monomer-to-initiator ratios of ≤25.
Polymers with number-average molar masses of up to 6500 g mol−1 and low dispersity (1.2–1.3) are produced. The aryl methyl ethers are successfully cleaved with aluminum triiodide/N,N′ diisopropylcarbodiimide to give a poly(2-oxazoline) with pendent catechol groups.
Ground penetrating radar (GPR) was used to characterize the frequency-dependent dielectric relaxation phenomena in ordinary Portland cement (OPC) hydration in concrete changing from fresh to hardened state. The study was experimented by measuring the changes of GPR A-scan waveforms over a period of 90 days, and processed the waveforms with short-time Fourier transform (STFT) in joint time-frequency analysis (JTFA) domain rather than a conventional time or frequency domain alone. The signals of the direct wave traveled at the concrete surface and the reflected wave from an embedded steel bar were transformed with STFT, in which the changes of peak frequency over ages were tracked. The peak frequencies were found to increase with ages and the patterns were found to match closely with primarily the well-known OPC hydration process and secondarily, the evaporation effect. The close match is contributed to the simultaneous effects converting free to bound water over time, on both conventional OPC hydration and dielectric relaxation mechanisms.
We have compared the performance of the typical Darr and CM moisture testing techniques, which are destructive with several non-destructive testing techniques on two types of floor screeds. In case of cement based screeds these destructive tests failed to deliver reliable results. Moreover, our measurements indicate significantly different drying and moisture transport behavior for the investigated cement based and calcium-sulphate based screeds. Whereas we have strong with depth decreasing moisture gradients in the CT material, we observe in the penetrated volumes of our ndt methods basically no clear moisture gradient in the CA samples. The findings with ndt methods could be supported by moisture gradient studies with nuclear magnetic resonance measurements.
Die Bestimmung der Belegreife von Estrichen erfolgt im Bauwesen meist unter Verwendung von zerstörenden Verfahren, die Probenentnahmen erfordern und nur punktuelle Daten liefern. Bei anhydritgebundenen Estrichen gelten 0,5 M% und bei zementgebundenen ca. 3,5 M% und höher als belegreifer Feuchtegehalt. Die Belegreife wird als Feuchtegehalt in Masseprozent (M%) bezogen auf die Trockenmasse des Baustoffes angegeben. Zur zerstörungsfreien Feuchtemessung existieren verschiedene einfach zu bedienende Handgeräte, die u. a. auf elektrischen, elektromagnetischen und kapazitiven Methoden beruhen. In dieser Arbeit wurden ein kapazitives (Kugelsonde), ein elektromagnetisches (Mikrowellensensoren) und ein elektrisches Messverfahren (Vierelektroden-Sonde) untersucht. Mit Ausnahme der Vierelektroden-Sonde weisen die Handgeräte keine ausreichende Sensitivität in Bereichen niedriger Feuchtegehalte unterhalb von 1 M% auf und scheinen somit nicht für anhydritgebundene Estriche geeignet zu sein. Für zementgebundene Estriche lassen sich hingegen mit allen getesteten Geräten Änderungen in dem Bereich der Belegreife erfassen. In dieser Arbeit wird zusätzlich die Wasserabgabe in g/m²/Tag als Bezugsgröße herangezogen. Die Wasserabgabe stellt ein geeigneteres Maß für die Schadensträchtigkeit dar und ermöglicht direkte Vergleiche unabhängig von der verwendeten Estrichart. Für alle getesteten Estriche konnte eine Wasserabgabe von ca. 8-10 g/m²/Tag als Belegreifegrenzwert bestimmt werden.
Moisture and salt loads of concrete can significantly change its microstructure and consequently lead to chemical and mechanical degradation. However, the non-destructive investigation of moisture and salt present in concrete is still difficult. In order to address and compare the sensitivity of different methods concrete samples with different pore systems realized by varying the w/z ratios have been fabricated. The focus of this study was put on the analysis of ultrasonic long and trans waves measured on the surface and in transmission mode. The results show clear dependencies of all applied methods. With the radar and microwave methods predominantly changes in the concrete moisture could be detected, whereas the different pore systems were not observed to alter the signals. In contrast for the ultrasound method also the ongoing hydration as well as the nature of the pore system strongly influenced the signals. As a consequence in a subsequent drying experiment it was also tried to delineate the effects of moisture and hydration. All specimens have been re-saturated under pressure and the drying experiment was repeated using the same multi-sensor approach.
In Germany there is an existing built infrastructure worth about 50 trillion Euros. The expected lifetimes of individual structures are up to 100 years. Considerable costs (annually about 35 billion Euros, the trend continues upwards) are involved in order to maintain and rehabilitate both residential as well as transportation infrastructure buildings. Most damages we observe on our built infrastructure are moisture-induced processes. Consequently reliable moisture measurement tools a highly needed for meaningful building diagnosis investigations. The optimal moisture measuring technique would be non-destructive, fast, repeatable, reliable, independent of steel in the vicinity, the surface condition or possible salt loads of the material under test. Since this is unfortunately not the case for any non-destructive method, it is often very difficult to decide for users which method to use for the particular testing problem. The only standardized methods in Germany are the “direct” and destructive Darr- and the CM tests. Although they can be highly accurate (when handled with care during the sampling), they deliver only punctual information and cannot be used for monitoring. The other, non-destructive methods are based on the change in humidity-dependent physical material properties. The underlying physics, their particular advantages and disadvantages are discussed in this paper.
Amino acid analysis is considered to be the gold standard for quantitative peptide and protein analysis. Here, we would like to propose a simple HPLC/UV method based on a reversed-phase separation of the aromatic amino acids tyrosine (Tyr), phenylalanine (Phe), and optionally tryptophan (Trp) without any derivatization. The hydrolysis of the proteins and peptides was performed by an accelerated microwave technique, which needs only 30 minutes. Two internal standard compounds, homotyrosine (HTyr) and 4-fluorophenylalanine (FPhe) were used for calibration. The limit of detection (LOD) was estimated to be 0.05 µM (~10 µg/L) for tyrosine and phenylalanine at 215 nm. The LOD for a protein determination was calculated to be below 16 mg/L (~300 ng BSA absolute). Aromatic amino acid analysis (AAAA) offers excellent accuracy and a precision of about 5% relative standard deviation, including the hydrolysis step. The method was validated with certified reference materials (CRM) of amino acids and of a pure protein (bovine serum albumin, BSA). AAAA can be used for the quantification of aromatic amino acids, isolated peptides or proteins, complex peptide or protein samples, such as serum or milk powder, and peptides or proteins immobilized on solid supports.