In this study, we report a novel procedure for fabricating internally tapered capillary columns suitable for the coupling of capillary electrochromatography (CEC) to electrospray mass spectrometry (ESI-MS). The internal tapers were prepared by slowly heating the capillary end in a methane/O2 flame. Due to continuous self-shrinking of the inner channel of the capillary, the inside diameter of the opening was reduced to 7-10 microm. The procedure is easy to handle, with no requirement for expensive equipment as well as elimination of problematic grinding of the tip. Several advantages of these new internal tapers, as compared to using externally tapered columns, are described. First, the problems of poor durability and tip breakage associated with external tapering were successfully overcome with the internal taper. A comparison of the online CEC/ESI-MS between external versus internal tapers showed that the latter provides enhanced electrospray stability, resulting in significantly lower short-term noise and very short-term noise values. In turn, the more rugged design of internal tapers allows performing CEC/MS utilizing a harsh polar organic mobile phase, which was not previously successful using an external taper due to higher operating current and electrospray arcing. Next, data on the reproducibility of the internally tapered CEC/MS column using warfarin and beta-blockers as model analytes are presented. For example, when comparing the reproducibility for separation of warfarin under reversed-phase conditions, the internal taper demonstrated superior intraday % RSD (1.6-3.4) as compared to the external taper intraday % RSD (5-6). Last, the applicability of performing quantitative CEC/MS with internally tapered capillaries is demonstrated for simultaneous enantioseparation of beta-blockers. Impressive quantitative results include good linearity of calibration curves (e.g., R2 = 0.9940-0.9988) and limit of detection as low as 30 nM. The sensitive detection of a minor impurity of one enantiomer at the 0.1% level in a major chiral entity buttresses the suitability of compliance with FDA guidelines. 相似文献
The aim of this study was to evaluate the effect of cavitation and electroporation on enzymolysis extraction of sunflower oil. The optimum extraction conditions during 2 h under enzyme-assisted extraction (EAE) with a maximum oil yield of ≈23.70 ± 0.11% were as follows: cellulase/pectinase ratio 2:1, enzyme concentration 2%, pH 4.5, liquid/solid ratio 6:1 ml/g, and extraction temperature 40°C. Under the optimized enzymatic conditions, the application of ultrasound- (250 W) and pulsed electric field- (1.2 kV/cm; 52.4 kJ/kg) assisted enzymatic extraction for 30 min significantly increased the oil extraction yield by 91.1% and 18.6%, respectively, as compared with EAE. 相似文献
Journal of Mechanical Science and Technology - Natural fiber composites have great potential for reducing the product cost, lowering weight and enhancing renewability. Functionality and performance... 相似文献
Despite many efforts into the study of fluids interaction in low salinity water flooding, they are not probing the basics of transport phenomena between the involved phases. This work is aimed to bring new understanding of fluid–fluid interaction during low salinity water flooding through a series of organized experiments in which a crude oil sample with known properties was kept in contact with different brine solutions of various ionic strengths. Measuring brine pH, conductivity and crude oil viscosity and density for a period of 45 days illustrates the strong effect of the contact time and ionic strength on the dissociation of polar components and physical properties of the crude oil and brine. Besides, the interfacial tension (IFT) measurements show that the interfacial interactions are affected by several competitive interfacial processes. By decreasing the ionic strength of the brine, the solubility of naphthenic acids in the aqueous solution increases, and hence, the conductivity and the pH of the aqueous phase decrease. To verify this important finding, UV–Vis spectroscopy and 1H NMR analysis were also performed on aged brine samples. Notably, there is an ionic strength of brine in which the lowest IFT is observed, while the other physical properties are remained relatively unchanged. 相似文献
As a first attempt, Fourier series expansion (FSE), particle swarm optimization (PSO), and genetic algorithm (GA) methods are coupled for analysis of the static–dynamic performance and propagated waves in the magneto-electro-elastic (MEE) nanoplate. The FSE method is presented for solving the motion equations of the MEE nanoplate. For increasing the performance of genetic algorithms for solving the problem, the particle swarm optimization technique is added as an operator of the GA. Accuracy, convergence, and applicability of the proposed mixed approach are shown in the results section. Also, we prove that for obtaining the convergence results of the PSO and GA, we should consider more than 16 iterations. Finally, it is shown that if designers consider the presented algorithm in their model, the results of phase velocity of the nanosystem will be increased by 27%. A useful suggestion is that there is a region the same as a trapezium in which there are no effects from magnetic and electric potential of the MEE face sheet on the phase velocity of the smart nanoplate, and the region will be bigger by increasing the wavenumber.
In this study, a microchannel reactor was designed, its catalytic performance in dry methane reforming (DRM) was assessed, and the results were compared with those observed in a conventional fixed bed reactor. The catalyst was prepared in two forms, including catalyst pellets and catalyst-coated plate. The microchannel reactor had thin films of Ni/Al2O3 coated on stainless steel substrate via radio frequency (RF) magnetron sputtering method in various sputtering times. The fall-off rate of the catalyst-coated plates can be neglected after putting the plates under the high-temperature DRM reaction, due to the formation of firm active catalyst coatings. The performance of the samples was evaluated at different temperatures from 700 to 800 °C, at P = 1 atm, with a CH4:CO2 ratio of 1. The results of XRD showed that with increasing the sputtering time, there was an increase in crystallinity. As observed in FESEM images, the sample prepared with 5 min of sputtering was dense and uniform. The results of EDX not only proved the dispersion of the samples observed in XRD and FESEM analysis, but also verified the presence of the utilized elements. The temperature of 800 °C and the sample with 5 min sputtering time were selected as the optimum condition that provided the best performance. Catalytic performance was investigated in fixed bed reactor at the same GHSV; based on the results there were no significant conversions in the fixed bed reactor. The results of the stability test in the microchannel reactor showed a good performance during 30 h on stream. Therefore, Ni/Al2O3 thin films had a satisfactory performance in the designed microchannel. Our study shows that this type of reactor has many advantages in terms of performance, compactness, and economic concerns. 相似文献
For the fast uptake into industrial applications, the further development of robust methods of nanomaterials, which are inexpensive and simultaneously technologically feasible, is one of the major key factors. A newly introduced atmospheric pulsed laser deposition method, based on a flowing gas approach, was used for plasmonic metal nanoparticle (NP) film of silver. Contrary to vacuum, in this method, the ambient air restricts expansion of the ablation plume within 1 to 3 mm above the target surface. These sets constrain on the formation of NP film close to the ablation spot. For deposition on a widely spaced surface, ablation material was entrained in a flow of argon, supplied at ~32 ms−1, and effectively delivered to the substrate at ~20 ms−1. The films produced were crystalline and particulate in nature, showing spectral plasmonic feature of surface plasmon resonance in the visible region. The film was directly tested in surface-enhanced Raman spectroscopy for chemical detection of crystal violet; the film with large particulates and aggregated crystallites was well-performed, showing enhanced Raman signals and detection sensitivity. Certainly, flowing gas atmospheric pulsed laser deposition seems a fast alternative to vacuum-pulsed laser deposition but needs further investigations to bring it in the industry for applications in sensor, catalysis, solar cell, and coating technology. 相似文献
Catalysis Letters - Nitro-aromatic pollution in industrial waste streams threat wellbeing of water resources. This study investigates the performance of a copper-based nano catalyst to reduce... 相似文献