Multivariate curve resolution-alternating least squares (MCR-ALS) and central composite experimental design for monitoring and optimization of simultaneous removal of some organic dyes

In this work, multivariate curve resolution-alternating least squares (MCR-ALS) has been applied to resolve and study the simultaneous degradation of three toxic organic dyes using Fenton reaction. Second-order kinetic-spectrophotometric data in the simultaneous degradation of malachite green, crystal violet and methylene blue were analyzed by MCR analysis to get their concentration profiles and calculate their degradation factors. The effect of three parameters (Fe²⁺, H₂O₂ concentration and initial pH) and their possible interaction in the simultaneous degradation of mentioned dyes were studied and optimized using experimental design and response surface method. Acquiring second-order data makes possible the analysis and study of the studied dyes in the gray systems which is termed as second-order advantage in the literatures. The prominent point of this work is the combination of second-order data and response surface methodology.     

Rank analysis and simultaneous determination of acetylsalicylic acid,paracetamol, and caffeine in pharmaceuticals using second-order data and multivariate curve resolution-alternating least squares (MCR-ALS)

Mixtures of acetylsalicylic acid (ASA), paracetamol (PAR), and caffeine (CAF) have been successfully analyzed by constrained multivariate curve resolution-alternating least squares (MCR-ALS). The MCR-ALS methodology adequately exploits the second-order advantage which enables quantitation of analyte in the presence of unknown and uncalibrated interferences. The procedure simultaneously takes into account the spectroscopic and pH-dependent properties of the compounds, which leads to a higher selectivity. Specially, for CAF determination fully protonated or deprotonated forms of CAF are not dominant in the pH range of data acquisition but spectral changes with pH were recorded and used for accurate determination of CAF. Furthermore, quantitative determination of an analyte in a complex mixture is performed using a synthetic solution as standard containing only the analyte of interest. Even in the presence of the rank deficiencies, in most cases accurate quantitation with relative errors in prediction lower than 5 % was obtained. The procedure was successfully applied to the analysis of real samples (pharmaceuticals) using synthetic external standards. Percent relative errors of 4.03, 3.26, and 5.85 were obtained for ASA, PAR, and CAF, respectively, in A.C.A tablets and 4.49 and 2.75 for PAR and CAF, respectively in Novafen capsules.     

One-pot, three-component synthesis of novel δ-sultam scaffolds via N-sulfonylation—intramolecular Michael sequences

The synthesis of novel δ-sultam scaffolds utilizing one-pot, three-component reactions of 1,3-dicarbonyl compounds, primary aliphatic amines and substituted styrenesulfonyl chlorides is reported. A variety of six-membered sultams are obtained in moderate to good yields presumably via N-sulfonylation—intramolecular Michael addition sequences.     

Solvent-dependent reactions for the synthesis of β-keto-benzo-δ-sultone scaffolds via DBU-catalyzed O-sulfonylation/intramolecular Baylis-Hillman/1,3-H shift or dehydration tandem sequences

We have developed a solvent-dependent method for the synthesis of novel benzo-δ-sultone scaffolds. A variety of benzylbenzo[e][1,2]oxathiin-4(3H)-one-2,2-dioxides were obtained in high yields in DMF using a one-pot, DBU-catalyzed condensation of 2-hydroxybenzaldehydes with a number of (E)-2-phenylethenesulfonyl chlorides. On the other hand, the initially prepared 2-formylphenyl-(E)-2-phenylethenesulfonate derivatives underwent DBU-catalyzed reactions to a series of 3-[methoxy(phenyl)methyl]benzo[e][1,2]oxathiine-2,2-dioxides in moderate to good yields in MeOH. These reactions presumably proceed via DBU-catalyzed O-sulfonylation/intramolecular Baylis-Hillman/1,3-H shift or dehydration tandem sequences, respectively.     

Sheep ovarian tissue vitrification by two different dehydration protocols and needle immersing methods

The present research investigated the effects of two vitrification methods on sheep ovarian tissue. The base medium (BM) of the vitrification solutions contains 60% HEPES tissue culture medium (HTCM), 15% ethylene glycol (EG) and 15% dimethyl sulfoxide (DMSO). Ovarian cortex pieces were dehydrated by two different regimens, the 2-step which consisted of 50% BM and a 90% solution of 0.25 mol/L sucrose in BM for 10 minutes each at 4 degree C and the 4-step method which utilized: a) 25% BM, b) 50% BM, c) 75% BM and d) a 90% solution of 0.25 mol/L sucrose in BM for 5 minutes each at 4 degree C. After warming, the proportion of intact antral follicles in the control (non-vitrified) and 2-step vitrification groups was significantly higher than in the 4-step vitrification group. The number of apoptotic follicles in the ovarian pieces was significantly different between the control and 4-step vitrification groups. These results indicated that sheep ovarian tissue vitrification by the 2-step method was simpler and more effective than the 4-step method.     

Self-crosslinking of 2-hydroxypropyl-N-methylmorpholinium chloride cellulose fibres

Crosslinking of cellulose fibres was obtained by inducing a substitution reaction in a cationic cellulose ether (NMM-cellulose) prepared by action of N-oxiranylmethyl-N-methylmorpholinium chloride. During the reaction the N-methylmorpholine moiety of the cellulosic ether acts as a leaving group facilitating a covalent bond formation between the ether substituent and a hydroxyl or other nucleophilic group present in the cellulose chain. In order to provide additional evidence of the suggested crosslinking route and investigate its possibilities, different reaction conditions have been investigated and assessed in terms of the obtained fibre properties. The crosslinked fibres were characterized by means of elemental analysis and structure accessibility studies, including accessibility to water, anions and nitrogen gas. According to these investigations heating at 105 °C induces a significant crosslinking. Pre-treatment with acetone restricts it mainly to formation of intra-fibre crosslinks, whereas heating from water suppresses the reactivity but results nevertheless in highly crosslinked structure with both intra- and inter-fibre crosslinks involved.     

Lattice Boltzmann simulation for hydrothermal analysis of free convection within dumbbell-shaped heat exchanger

The lattice Boltzmann simulation of nanofluid flow and heat transfer during natural convection within a dumbbell-shaped heat exchanger is carried out. The heat exchanger is filled with CuO–water. The KKL model is employed to predict the thermo-physical properties of nanofluid. In order to perform a comprehensive hydrothermal investigation, different post-processing approaches such as heatline visualization, total entropy generation, local entropy generation based on local fluid friction irreversibility and heat transfer irreversibility, average and local Nusselt variation are employed. In the present investigation, it is tried to present the impact of different influential parameters like Rayleigh number, solid volume fraction of nanofluid and thermal arrangement of internal fins-bodies on the fluid flow, heat transfer rate and entropy generation.     

Spectrophotometric study of interaction of iodine with 4'-aminobenzo-15-crown-5 in chloroform, dichloromethane and 1,2-dichloroethane solutions

The formation of charge transfer complex between 4'-aminobenzo-15-crown-5 (AB15C5) and iodine is investigated spectrophotometrically in chloroform, dichloromethane (DCM) and 1,2-dichloroethane (DCE) solutions at 25 degrees C. The continuous variation method clearly revealed the formation of 1:1 charge transfer complex in solution. The observed time dependence of the charge transfer band and subsequent formation of I 3- in solution were related to the slow transformation of the initially formed 1:1 AB15C5.I2 outer complex to an inner electron donor-acceptor (EDA) complex, followed by fast reaction of the inner complex with iodine to form a triiodide ion. The pseudo-first-order rate constants for the transformation process were evaluated from the absorbance-time data and found to vary in the order of 1,2-DCE>DCM>CHCl3. The values of the formation constant, KDA, for each complex are evaluated from Benesi-Hilebrand equation. Stability of the resulting complex in three solvents was also found to vary in the order of 1,2-DCE>DCM>CHCl3.     

The Growth of Ce,Nd:YAG Single Crystal Under New Atmosphere Condition

Crystallography Reports - Ce3+,Nd3+:YAG single crystal was grown by Czochralski method without using any reduction gas. The growth was done in the atmosphere of pure nitrogen. The limited-flow of...