Yttrium tris(trimethylsilylmethyl) complexes grafted onto MCM-48 mesoporous silica nanoparticles

A series of tris(trimethylsilylmethyl) yttrium donor adduct complexes was synthesized and fully characterized by X-ray diffraction, 1H/13C/29Si/31P/89Y heteronuclear NMR and DRIFT spectroscopy as well as elemental analyses. Treatment of Y(CH2SiMe3)3(thf)x...

Low Temperature HCHO Detection by SnO2/TiO2@Au and SnO2/TiO2@Pt: Understanding by in-situ DRIFT Spectroscopy

In this work we analyze the effectiveness of decoration of nanocrystalline SnO2/TiO2 composites with gold nanoparticles (Au NPs) and platinum nanoparticles (Pt NPs) in enhancing gas sensor properties in low-temperature HCHO detection. Nanocrystalline SnO2/TiO2 composites were synthesized by a chemical precipitation method with following modification with Pt and Au NPs by the impregnation method. The nanocomposites were characterized by TEM, XRD, Raman and FTIR spectroscopy, DRIFTS, XPS, TPR-H2 methods. In HCHO detection, the modification of SnO2 with TiO2 leads to a shift in the optimal temperature from 150 to 100 °C. Further modification of SnO2/TiO2 nanocomposites with Au NPs increases the sensor signal at T = 100 °C, while modification with Pt NPs gives rise to the appearance of sensor responses at T = 25 °C and 50 °C. At 200 °C nanocomposites exhibited high selectivity toward formaldehyde within the sub-ppm concentration range among different VOCs. The influence of Pt and Au NPs on surface reactivity of SnO2/TiO2 composite and enhancement of the sensor response toward HCHO was studied by DRIFT spectroscopy and explained by the chemical and electronic sensitization mechanisms.

The Impact of Lanthanum and Zeolite Structure on Hydrocarbon Storage

Hydrocarbon traps can be used to bridge the temperature gap from the cold start of a vehicle until the exhaust after-treatment catalyst has reached its operating temperature. In this work, we investigate the effect of zeolite structure (ZSM-5, BEA, SSZ-13) and the effect of La addition to H-BEA and H-ZSM-5 on the hydrocarbon storage capacity by temperature-programmed desorption and DRIFT spectroscopy. The results show that the presence of La has a significant effect on the adsorption characteristics of toluene on the BEA-supported La materials. A low loading of La onto zeolite BEA (2% La-BEA) improves not only the toluene adsorption capacity but also the retention of toluene. However, a higher loading of La results in a decrease in the adsorbed amount of toluene, which likely is due to partial blocking of the pore of the support. High loadings of La in BEA result in a contraction of the unit cell of the zeolite as evidenced by XRD. A synergetic effect of having simultaneously different types of hydrocarbons (toluene, propene, and propane) in the feed is found for samples containing ZSM-5, where the desorption temperature of propane increases, and the quantity that desorbed increases by a factor of four. This is found to be due to the interaction between toluene and propane inside the structure of the zeolite.

Comparison of soil organic matter composition under different land uses by DRIFT spectroscopy

The study aimed to estimate and characterise soil organic matter under different land uses (cropland, grassland, and forest) and soil depths. The soil organic matter composition of the soil was assessed by diffuse reflectance infrared spectroscopy (DRIFT). Humic and fulvic acids (HAs, FAs) were extracted from soils and their compositions were evaluated by DRIFT. Low molecular mass organic acids content was also measured. Our result revealed that the largest differences of the spectra in the composition of organic matter were observed in the upper parts of the soil profile. The forest soil spectra had more intense aliphatic bands, carboxylic, and CH bands than spectra of grassland and cropland soils. The difference of HAs spectra was at 3 010 to 2 800/cm where the most intensive aliphatic bands were in forest soil HAs, followed by grassland and cropland soil HAs. The grassland topsoil FAs spectrum differs most from the other land uses. It has lower peaks around 1 660–1 600/cm and 1 200/cm than cropland and forest. The concentration of low molecular mass organic acid (LMMOA) was the highest in the forest soil and the most abundant acid was citrate.

Mechanochemical synthesis of a novel eutectic of the antimicrobial nitazoxanide with improved dissolution performance

Background: Nitazoxanide (NTZ) is a broad spectrum antimicrobial agent with poor aqueous solubility and low bioavailability. Thus, the generation of new solid forms of NTZ is relevant to improve its unfavorable properties. The present study deals with the application of mechanochemistry for the preparation of alternate solid forms of NTZ, using saccharine (SAC) as coformer. Methods: NTZ-SAC mixtures were prepared by neat and liquid-assisted grinding (LAG) and characterized using differential scanning calorimetry (DSC), hot stage microscopy (HSM), X-ray Powder Diffraction (XRPD), 13C Solid-state Nuclear Magnetic Resonance (SSNMR) and Diffuse Reflectance Infrared Fourier Transform (DRIFT) spectroscopy. Powder dissolution (PD) profiles were obtained with USP apparatus 2 in buffer phosphate pH 6.5 with 0.25% Tween 80 - 0.25% triethanolamine and in 0.25% sodium lauryl sulfate, at 37 ºC ± 0.5 ºC and 75 rpm. Drug release was characterized in terms of dissolution efficiency (DE). Results: XRPD, SSNMR and DRIFT indicated that NTZ and SAC did not cocrystallize but DSC and HSM revealed that they formed a binary eutectic mixture which melted near 176 °C, a melting temperature lower than those of NTZ and SAC. PD data indicated that the 1:1 NTZ-SAC sample obtained by LAG exhibited a slightly higher DE than pure NTZ in the two assayed media. Conclusion: NTZ and SAC formed a eutectic, the first reported for this drug, which improved its dissolution rate and opened the pathway for studies searching for new eutectics with better biopharmaceutical attributes than NTZ and the NTZ-SAC eutectic reported herein.

Mesoporous KIT-6 supported Cr and Co-based catalysts for microwave-assisted non-oxidative ethane dehydrogenation

In the present study, mono and bi-metallic catalysts containing Cr and Co were prepared by impregnating the hydrothermally prepared mesoporous KIT-6 support with 5–10 wt% total metal content. The well-ordered three-dimensional mesoporous structure of the KIT-6 support was confirmed by small angle X-ray diffraction (XRD) patterns. N2 adsorption-desorption analysis results showed that the mesoporous structure of KIT-6 was preserved after metal loading. Structural bonds of KIT-6 support and prepared catalysts were determined by Fourier-transform infrared (FT-IR) spectroscopy. The pyridine adsorbed diffuse reflectance FT-IR (DRIFT) spectroscopy results revealed the presence of Lewis acid sites on the surface of the catalysts. Activity experiments were carried out in a microwave-heated continuous-flow fixed bed reactor system at temperature range of 350–650 °C and feed ratios of Ethane/Argon: 1/2, 1/1, 2/1 with a gas hourly space velocity (GHSV) of 18,000 ml/h.gcat. The 5Cr@KIT-6 catalyst exhibited high ethane conversion (63.5%) while the highest ethylene/hydrogen ratio (0.98) was obtained with the 2.5Cr2.5Co@KIT-6 catalyst at 450 °C. It was concluded that high temperatures (above 450 °C) facilitate the formation of side reactions and the production of aromatic compounds. The high catalytic activities of mesoporous catalysts were thought to be due to hot spots in the microwave reactor system.