Simple high‐performance liquid chromatography method for formaldehyde determination in human tissue through derivatization with 2,4‐dinitrophenylhydrazine

A simple high‐performance liquid chromatography method has been developed for the determination of formaldehyde in human tissue. FA Formaldehyde was derivatized with 2,4‐dinitrophenylhydrazine. It was extracted from human tissue with ethyl acetate by liquid–liquid extraction and analyzed by high‐performance liquid chromatography. The calibration curve was linear in the concentration range of 5.0–200 μg/mL. Intra‐ and interday precision values for formaldehyde in tissue were <6.9%, and accuracy (relative error) was better than 6.5%. The extraction recoveries of formaldehyde from human tissue were between 88 and 98%. The limits of detection and quantification of formaldehyde were 1.5 and 5.0 μg/mL, respectively. Also, this assay was applied to liver samples taken from a biopsy material.     

Comparison of preconcentration methods for nontargeted analysis of natural waters using HPLC-HRMS: Large volume injection versus solid-phase extraction

Nontargeted analysis of water samples using liquid chromatography combined with high-resolution mass spectrometers is an emerging approach for surface water monitoring and evaluation of water treatment processes. In this study, sample preconcentration via direct, large volume injection with 500 μL and 1000 μL injection volumes was compared to SPE regarding analytical performance parameters in targeted and nontargeted workflows. In targeted analysis, the methods were evaluated in terms of LOD and intrabatch precision of the selected compounds, whereas in nontargeted analysis, the number of detected unknown compounds, the method's intra-batch precision, and the retention time versus molecular mass pattern of the detected unknowns were evaluated. In addition, a novel intensity drift correction method was developed that is not based on quality control samples and makes use of the signals obtained for continuously infused reference compounds, which are conventionally utilized for online mass drift correction. It could be demonstrated that the new correction method significantly reduced the bias introduced by instrumental drift and is important for the reliable intercomparison of different nontargeted methods. Intercomparison of results showed that the 1000 μL large volume injection method revealed the best performance in terms of precision under repeatability conditions of measurement as well as lower LODs for targeted compound analysis. In nontargeted analysis, the SPE method detected a higher number of unknown compounds but exhibited also a higher uncertainty of measurement caused by matrix effects.     

A New Fluorescent “Turn-Off” Coumarin-Based Chemosensor: Synthesis,Structure and Cu-Selective Fluorescent Sensing in Water Samples

We report the synthesis and characterization two coumarin-based fluorescence probes, N′-{[7-(diethylamino)-2-oxo-2H-chromen-3-yl]carbonyl}pyridine-3-carbohydrazide (3) and N′-benzoyl-7-(diethylamino)-2-oxo-2H-chromene-3-carbohydrazide (4), proposed as a novel fluorescent chemosensor. The two probes designed showed an instant turn-off fluorescence response to Cu²⁺ over other metal ions in ethanol-water mixture based on intramolecular charge transfer (ICT). It was found that pyridine-analogue coumarin is highly selective and sensitive sensor for Cu²⁺. The 3 sensor coordinates Cu²⁺ in 1:1 stoichiometry with a binding constant, K_a = 5.22 M^?1 and the detection limit was calculated 1.97 × 10^?9 M.     

Equation of state of asymmetric nuclear matter: a VMC study

A Variational Monte Carlo (VMC) method is employed to investigate the properties of symmetric and asymmetric nuclear matter. The realistic Urbana V ₁₄ twonucleon interaction potential of Lagaris and Pandharipande was used to describe the microscopic interactions. Also, many body interactions are included as a density dependent term in the potential. Total kinetic and potential energies per particle are calculated for asymmetric nuclear matter by VMC method at various densities and isospin asymmetry parameters. The results are compared with data found in literature, and it was observed that the results obtained in this study reasonably agree with the results found in the literature. Also, the symmetry energy and incompressibility factor of the nuclear matter were obtained. The results obtained are in good agreement with those obtained by various authors with different methods and techniques.     

Effect of microstructure on fracture in age hardenable Al alloys

ABSTRACT

In the present study, the fracture behaviour of AA6016 alloy was investigated during bending deformation. Wrap-bend tests were conducted and the material was subjected to different bend angles to study crack propagation. The average grain size of the as-received material is approximately 45?μm. The aspect ratio of the grains was changed from 0.53 to 0.40 during bending. The presence of deformation bands was observed during bending in both tensile and compressive regions of the sample. No orientation correlation was observed between the deformation band and its corresponding parent grain. The Schmid factor inside the deformation bands was higher than that of the parent grain, which indicates that the deformation bands accommodate strain during bending. The crystallographic texture evolved significantly during bending deformation. The strength of cube texture component decreases with increasing bend angle and new texture components formed during bending. These new texture components favour either single slip or duplex slip. A mixture of intra-granular and inter-granular fracture occurs during bending. It is observed that inter-granular crack propagation is predominantly favoured along high-angle boundaries, and grain boundary de-cohesion occurs in regions where the misorientation angle is greater than 40°. The formation of deformation-induced coincidence lattice site (CSL) boundaries is also observed during bending and it is shown that the volume fraction of CSL boundaries of Σ3 type increases with increasing bend angle. The current study shows that the formation of deformation-induced CSL boundaries of Σ3 type in AA6016 alloy can improve its inherent resistance to crack propagation during bending.     

A convenient approach directly from triglycerides toward the producing of thia-wax esters as bio- and chemical raw materials

Research on Chemical Intermediates - Practical and efficient method has been developed for the preparation of novel sulfur-containing esters from triglycerides as potential important industrial and...     

Analysis of the Electronic Structure of Aqueous Urea and Its Derivatives: A Systematic Soft X‐Ray–TD‐DFT Approach

Soft X‐ray emission (XE), absorption (XA), and resonant inelastic scattering (RIXS) experiments have been conducted at the nitrogen K‐edge of urea and its derivatives in aqueous solution and were compared with density functional theory and time‐dependent density functional theory calculations. This comprehensive study provides detailed information on the occupied and unoccupied molecular orbitals of urea, thiourea, acetamide, dimethylurea, and biuret at valence levels. By identifying the electronic transitions that contribute to the experimental spectral features, the energy gap between the highest occupied and the lowest unoccupied molecular orbital of each molecule is determined. Moreover, a theoretical approach is introduced to simulate resonant inelastic X‐ray scattering spectra by adding an extra electron to the lowest unoccupied molecular orbital, thereby mimicking the real initial state of the core‐electron absorption before the subsequent relaxation process.     

Microstructural and Radioluminescence Characteristics of Nd<Superscript>3+</Superscript> Doped Columbite-Type SrNb<Subscript>2</Subscript>O<Subscript>6</Subscript> Phosphor

Undoped and different concentration Nd³⁺ doped SrNb₂O₆ powders with columbite structure were synthesized by molten salt process using a mixture of strontium nitrate and niobium (V) oxide and NaCl-KCl salt mixture as a flux under relatively low calcining temperature. X-ray diffraction analysis results indicated that SrNb₂O₆ phases found to be orthorhombic columbite single phase for undoped, 0.5 and 3 mol% Nd³⁺ doping concentrations. Phase composition of the powders was examined by SEM-EDS analyses. Radioluminescence properties of Nd³⁺ doped samples from UV to near-IR spectral region were studied. The emissions increased with the doping concentration of up to 3 mol%, and then decreased due to concentration quenching effect. There is a sharp emission peak around 880 nm associated with ⁴F_5/2 → ⁴I_9/2 transition in the Nd³⁺ ion between 300 and 1100 nm. The broad emission band intensity was observed from 400 to 650 nm where the peak intensities increased by increasing Nd³⁺ doping concentration. All the measurements were taken under the room temperature.