ABSTRACT
The thermally stable zirconium-based MOF, UiO-66, was employed for the preparation of bonded porous-layer open-tubular (PLOT) GC columns. The synthesis included the in situ growth of the UiO-66 film on the inner wall of the capillary through a one-step solvothermal procedure. SEM-EDX analysis revealed the formation of a thin, continuous, uniform, and compact layer of UiO-66 polycrystals on the functionalized inner wall of the column. The average polarity (ΔIav = 700) and the McReynolds constants reflected the polar nature of the UiO-66 stationary phase. Several mixtures of small organic compounds and real samples were used to evaluate the separation performance of the fabricated columns. Linear alkanes from n-pentane to n-decane were baseline separated within 1.35 min. Also, a series of six n-alkylbenzenes (C3-C8) were separated within 3 min with a minimum resolution of 3.09, whereas monohalobenzene mixtures were separated at 220 °C within 14s. UiO-66 PLOT columns are ideally suited for the isothermal separation of chlorobenzene structural isomers at 210 °C within 45 s with Rs ≥ 1.37. The prepared column featured outstanding thermal stability (up to 450 °C) without any observed bleeding or significant impact on its performance. This feature enabled the analysis of various petroleum-based samples.
ABSTRACT
Zinc chromium oxide (Cr/ZnO, 5wt.%) was prepared by a facile chemical co-precipitation route. The structure, composition, and chemical bonding were analyzed using X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX), and Fourier-transform infrared spectroscopy (FTIR) indicating that chromium ions were integrated the host framework to form Cr/ZnO nanocomposite. Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) micrographs showed comb-shaped nanoparticles with an average size 20 nm and large surface area. The energy gap of the thin films was estimated from T% and R% measurements which exhibit a strong optical absorption edge close to the visible spectrum. The insecticidal activity of the synthesized nanocombs against C. pipiens larvae was evaluated with LC50 (30.15 ppm) and LC90 (100.22 ppm). Besides, the nanocomposite showed high antibacterial performance against gram-positive bacteria (Bacillus subtilis) and gram-negative bacteria (Proteus vulgaris) with inhibition zones 21.9 and 19 mm, respectively.
ABSTRACT
A highly ultrasensitive sensor that relied on Cr/ZnO-NPs was developed to detect etilefrine hydrochloride (ETF) in different matrices via a particular green voltammetric technique. The X-ray diffraction pattern showed the nanomaterials of the polycrystalline hexagonal structure. The energy-dispersive X-ray spectrum approved the presence of Cr3+ inside the host zinc oxide framework. The morphological and topological characteristics were visualized using transmission electron microscopy and atomic force microscopy micrographs describing the nanoparticles in spherical-like shape with large-surface area. The energy gap (Eg) was evaluated from transmittance (T %) and reflectance (R %) spectra within the visible region. The optimization study indicated that the Cr/ZnO-NP/CPE sensor has high sensitivity, thanks to the distinctive physical and chemical properties of the fabricated electrode. A new approach showed a great selectivity for determining ETF in different matrices in the presence of other interferents like levodopa. Under optimal circumstances, the square-wave voltammetry revealed a linear response to ETF from 0.01 to 10 µmol L-1 (r = 0.9996) with quantification and detection limits of 9.11 and 2.97 nmol L-1, respectively. Finally, the proposed approach was effectively applied to estimate ETF in pharmaceutical dosage forms and biological fluids using simple, accurate, and selective electrochemical electrode. The greenness profile assessment of the developed method was performed using the Eco-Scale and green analytical procedure index. These tools indicated that the proposed method is an eco-friendly technique for the determination of ETF in different matrices.
