4,4′‐Butane‐1,4‐diylbis[3‐ethyl‐1H‐1,2,4‐triazol‐5(4H)‐one] and 4‐hydr­oxy‐3‐n‐prop­yl‐1H‐1,2,4‐triazol‐5(4H)‐one

The title compounds, C₁₂H₂₀N₆O₂, (I), and C₅H₉N₃O₂, (II), display the characteristic features of 1,2,4‐triazole derivatives. Compound (I) lies about an inversion centre which is at the mid‐point of the central C—C bond. Compound (II) also contains a planar 1,2,4‐triazole ring but differs from (I) in that it has a hydr­oxy group attached to the ring. Mol­ecules of (I) are held together in the crystal structure by inter­molecular N—H⋯O contacts and by weak π–π stacking inter­actions between the 1,2,4‐triazole moieties. Compound (II) contains inter­molecular O—H⋯O and N—H⋯O hydrogen bonds.     

Factorial design in the optimization of preconcentration procedure for lead determination by FAAS

The present paper proposes a preconcentration procedure for lead determination using flame atomic absorption spectrometry (FAAS). It is based on lead(II) ions extraction as brilliant cresyl blue (BCB) complex and its sorption onto Diaion HP-2MG, a methacrylic ester copolymer. The optimization step was carried out using factorial design and the variables studied were pH, shaking time and reagent concentration. In the established experimental conditions, lead can be determinate with a limit of detection of 3.7 μg L⁻¹ lead (N = 20) and a relative standard deviation of 7% for a lead concentration of 100 μg L⁻¹. The accuracy was confirmed by analysis of a certified reference material, the stream sediment furnished by National Research Centre for Certified Reference Materials (NRCCRM), China (GBW 07310). Effect of other ions in the procedure proposed was also studied. The method was applied for lead determination in real samples of water, tea, soil and dust. Tests of addition/recovery in the experiments for lead determination in water samples revealed that the proposed procedure could be applied satisfactorily for analysis of these samples.     

Direct determination of sulfite in food samples by a biosensor based on plant tissue homogenate

In the work described here, a biosensor was developed for the determination of sulfite in food. Malva vulgaris tissue homogenate containing sulfite oxidase enzyme was used as the biological material. M. vulgaris tissue homogenate was crosslinked with gelatin using glutaraldehyde and fixed on a pretreated Teflon membrane. Sulfite was enzymatically converted to sulfate in the presence of the dissolved oxygen, which was monitored amperometrically. Sulfite determination was carried out by standard curves, which were obtained by the measurement of consumed oxygen level related to sulfite concentration. Several operational parameters had been investigated: the amounts of plant tissue homogenate and gelatin, percentage of glutaraldehyde, optimum pH and temperature. Also, some characterization studies were done. There was linearity in the range between 0.2 and 1.8 mM at 35 °C and pH 7.5. The results of real sample analysis obtained with the biosensor agreed well with the enzymatic reference method using spectrophotometric detection.     

A flow-through microfluidic chip for continuous dielectrophoretic separation of viable and non-viable human T-cells

Effective methods for rapid sorting of cells according to their viability are critical in T cells based therapies to prevent any risk to patients. In this context, we present a novel microfluidic device that continuously separates viable and non-viable T-cells according to their dielectric properties. A dielectrophoresis (DEP) force is generated by an array of castellated microelectrodes embedded into a microfluidic channel with a single inlet and two outlets; cells subjected to positive DEP forces are drawn toward the electrodes array and leave from the top outlet, those subjected to negative DEP forces are repelled away from the electrodes and leave from the bottom outlet. Computational fluid dynamics is used to predict the device separation efficacy, according to the applied alternative current (AC) frequency, at which the cells move from/to a negative/positive DEP region and the ionic strength of the suspension medium. The model is used to support the design of the operational conditions, confirming a separation efficiency, in terms of purity, of 96% under an applied AC frequency of 1.5 × 10⁶ Hz and a flow rate of 20 μl/h. This work represents the first example of effective continuous sorting of viable and non-viable human T-cells in a single-inlet microfluidic chip, paving the way for lab-on-a-chip applications at the point of need.     

Application of microcrystalline cellulose as an efficient and cheap sorbent for the extraction of metoprolol from plasma and wastewater before HPLC–MS/MS determination

A dispersive solid-phase extraction method based on a new sorbent has been performed on plasma and wastewater samples to determine metoprolol by high-performance liquid chromatography–tandem mass spectrometry. In this study, the analyte was adsorbed from the samples onto microcrystalline cellulose as a green and efficient sorbent and then eluted for use in the determination step. In the mass spectrometer, the analyte was detected in the positive mode and selectivity of the analysis was increased by sequential mass analysis through multiple reaction monitoring. All of the effective parameters in the extraction of metoprolol from plasma and wastewater were optimized. Under optimal conditions the method was linear in the ranges of 1–1,000 and 0.1–1,000 ng/ml in plasma and wastewater samples, respectively. The detection limits of the method were 0.30 and 0.03 ng/ml in plasma and wastewater samples, respectively. The data showed that the method provides low detection limit, wide linear range, good precision and high extraction recovery. Finally several plasma and wastewater samples were successfully analyzed using the method. The use of a small amount of a green and inexpensive sorbent and a low volume of plasma without the need for further pretreatment steps are the main advantages of the method.     

Flow and thermal study of MHD Casson fluid past a moving stretching porous wedge

Journal of Thermal Analysis and Calorimetry - This research provides the analysis of an analytical method named Homotopy analysis method which is applied to examine the series solutions/results on...     

Synthesis of attapulgite-MnO2 nanocomposite from manganese complex by ultrasound for hydrogen storage

The research included the synthesis of a new complex of manganese with 3,4,5-tri-methoxybenzoic acid in the presence of triethylamine as a base to which gives the complex with formula [Mn (TMB)₂].2H₂O. This complex was characterized by FTIR, CHN, magnetic susceptibility and thermal analysis. Furthermore, this complex was used as a novel precursor of manganese in preparing the attapulgite-MnO₂ nanocomposite by one-pot addition method using ultrasound. The resulting nanocomposite was characterized by X-ray diffraction and TEM and the results prove that this composite was found as nanochannel of the diameter 45 nm decorated with 26–41 nm of MnO₂ nanoparticles. The attapulgite-MnO₂ nanocomposite was used in the application of hydrogen storage, and the results proved that attapulgite-MnO₂ nanocomposite has the ability to store 3.55 wt% of hydrogen under a pressure of 90 bar and a temperature of 77 K. Furthermore, the measurement demonstrated that increasing the pressure increased the stored hydrogen, implying that the stored gas will be liberated by altering the pressure, implying that the storage will be of the physical kind.     

Three (E)‐2‐[(bromo­phen­yl)imino­meth­yl]‐4‐methoxy­phenols

The title compounds, (E)‐2‐[(2‐bromo­phenyl)imino­methyl]‐4‐methoxy­phenol, C₁₄H₁₂BrNO₂, (I), (E)‐2‐[(3‐bromo­phenyl)­imino­methyl]‐4‐methoxy­phenol, C₁₄H₁₂BrNO₂, (II), and (E)‐2‐[(4‐bromo­phenyl)imino­methyl]‐4‐methoxy­phenol, C₁₄H₁₂BrNO₂, (III), adopt the phenol–imine tautomeric form. In all three structures, there are strong intra­molecular O—H⋯N hydrogen bonds. Compound (I) has strong inter­molecular hydrogen bonds, while compound (III) has weak inter­molecular hydrogen bonds. In addition to these inter­molecular inter­actions, C—H⋯π inter­actions in (I) and (III), and π–π inter­actions in (I), play roles in the crystal packing. The dihedral angles between the aromatic rings are 15.34 (12), 6.1 (3) and 39.2 (14)° for (I), (II) and (III), respectively.     

Unusual products in the reactions of hexachlorocyclotriphosphazatriene with sodium aryloxides

Reactions of hexachlorocyclotriphosphazatriene, N₃P₃Cl₆ 1 , with sodium aryloxides have been studied. Compound 1 was found to react by the nucleophilic substitution pathway to yield monocyclophosphazenes [N₃P₃Cl₆(OC₆H₂Bu¹₃-2,4,6) 5 and N₃P₃Cl₄(OC₆H₂Me-4-Bu¹₂-2,6)₂ 6 ] and bi(cyclophosphazenes) ([Cl₅N₃P₃-P₃N₃Cl₄(OC₆H₃Bu¹₂-2,6)] 7 and [N₃P₃(OC₆H₃Bu¹₂-2,6)₅]₂ 8 ). The unusual bi(cyclophosphazenes) 7 and 8 are the first examples of two cyclotriphosphazene rings linked by a P(SINGLE BOND)P bond [2.193 (2) Å], which have been obtained by reacting 1 with ArONa. The structures of compounds 5–8 are ascertained by elemental analyses, ¹H-, ³¹P-¹³C-NMR, IR, and MS spectra. The molecular structure of monocyclic-phosphazene 5 was determined by X-ray diffraction techniques for further structural assignment. It crystallizes in the monoclinic space group P2₁/m with a = 6.144(2), b = 17.079(9), c = 13.181(9) Å, β = 92.79(7), and Z = 2, R = 0.074. Compound 5 is on a crystallographic mirror plane, and there is only a half molecule in the asymmetric unit. © 1996 John Wiley & Sons, Inc.     

Comparative evaluation of various total antioxidant capacity assays applied to phenolic compounds with the CUPRAC assay

It would be desirable to establish and standardize methods that can measure the total antioxidant capacity level directly from vegetable extracts containing phenolics. Antioxidant capacity assays may be broadly classified as electron transfer (ET)- and hydrogen atom transfer (HAT)-based assays. The majority of HAT assays are kinetics-based, and involve a competitive reaction scheme in which antioxidant and substrate compete for peroxyl radicals thermally generated through the decomposition of azo compounds. ET-based assays measure the capacity of an antioxidant in the reduction of an oxidant, which changes colour when reduced. ET assays include the ABTS/TEAC, CUPRAC, DPPH, Folin-Ciocalteu and FRAP methods, each using different chromogenic redox reagents with different standard potentials. This review intends to offer a critical evaluation of existing antioxidant assays applied to phenolics, and reports the development by our research group of a simple and low-cost antioxidant capacity assay for dietary polyphenols, vitamins C and E, and human serum antioxidants, utilizing the copper(II)-neocuproine reagent as the chromogenic oxidizing agent, which we haved named the CUPRAC (cupric ion reducing antioxidant capacity) method. This method offers distinct advantages over other ET-based assays, namely the selection of working pH at physiological pH (as opposed to the Folin and FRAP methods, which work at alkaline and acidic pHs, respectively), applicability to both hydrophilic and lipophilic antioxidants (unlike Folin and DPPH), completion of the redox reactions for most common flavonoids (unlike FRAP), selective oxidation of antioxidant compounds without affecting sugars and citric acid commonly contained in foodstuffs and the capability to assay -SH bearing antioxidants (unlike FRAP). Other similar ET-based antioxidant assays that we have developed or modified for phenolics are the Fe(III)- and Ce(IV)-reducing capacity methods.