Semiquantitative determination of thirty cations by circular thin-layer chromatography

Summary A comprehensive scheme for the semiquantitative determination of 30 metal ions (Ag⁺, Pb²⁺, W⁶⁺, Tl⁺, Fe³⁺, Au³⁺, Mo⁶⁺, Ga³⁺, Sb⁵⁺, Ge⁴⁺, Te⁴⁺, Pt⁴⁺, Pd²⁺, Ru³⁺, Rh³⁺, Cu²⁺, Co²⁺, Ni²⁺, Zn²⁺, Cd²⁺, Cr⁶⁺, Mn²⁺, U⁶⁺, V⁵⁺, Sn⁴⁺, Bi³⁺, Hg²⁺, Ti⁴⁺, Se⁴⁺ and As³⁺) is described. It is based on circular thin-layer chromatographic technique. The error is ± 5% and 16 other metal ions, not included in the analysis scheme because of the non-availability of spray reagents, do not interfere. The determination of each cation has been made with different spray reagents separately and the mean error has been calculated. The analysis of the same cation with different spray reagents provides a useful check on the results. The method holds an excellent promise for the study of airborne particulates and for the determination of trace elements from blood, tissue and bone.

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Zusammenfassung Ein umfassender Analysengang für die halb quantitative Bestimmung von 30 Metallionen wurde beschrieben. Die Ringchromatographie auf Dünnschichten wurde hierzu verwendet. Der Fehler beträgt ±5%. 16 weitere Metallionen, die in Ermangelung geeigneter Sprühreagenzien in den Analysengang nicht aufgenommen wurden, stören nicht. Die Bestimmung jedes einzelnen Kations wurde mit verschiedenen Sprühmitteln vorgenommen; der mittlere Fehler wurde dann berechnet. So ist eine gute Überprüfung der Ergebnisse möglich. Das Verfahren dürfte sich für die Untersuchung der Luftverschmutzung sowie für die Bestimmung von Spurenelementen in Blut, Gewebe und Knochen eignen.

     

Volumetric determination of Pt(IV) in the presence of Ir,Pd, and Rh with ferrous ammonium sulfate in alkaline mannitol medium

A potentiometric reductimetric method for the determination of platinum (Pt(IV)Pt(II)) with a standard Fe(II) solution in an alkaline medium of mannitol is described. The method, the error of which does not exceed 2%, can be used in the presence of palladium, iridium, and rhodium.     

Stereospecific synthesis of 1,2-cis glycosides by vinyl-mediated IAD

[reaction: see text] Stereospecific 1,2-cis glycosylation of 2-O-vinyl thioglycosides, synthesized from the corresponding alcohols by Ir-catalyzed transvinylation with vinyl acetate, is achieved by iodine-mediated tethering of a range of primary and secondary carbohydrate acceptors, followed by intramolecular aglycon delivery (IAD). The use of such an intramolecular glycosylation strategy furnishes the desired alpha-gluco and beta-manno disaccharides in an entirely stereoselective manner.     

Semiquantitative determination of thiourea,thiocyanate, and sulfide by circular thin layer chromatography

Summary A method for semiquantitative determination of thiourea, thiocyanate, and sulfide is described. It involves making circular spots or rings on chromatoplates using the circular thin layer Chromatographic apparatus. The method is based on sensitivity and specificity of spot reactions and comparison of the color intensity of a circular spot with that of sensitivity standards. The accuracy of the method is ± 5% and the procedure is rapid, simple and economical.

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Zusammenfassung Ein Verfahren zur halbquantitativen Bestimmung von Thioharnstoff, Thiocyanat und Sulfid wurde beschrieben. Es beruht auf der chromatographischen Herstellung kreisförmiger Flecken oder Ringe auf Dünnschichtplatten. Mit empfindlichen und spezifischen Tüpfelreaktionen wurden die Flecken gefärbt und die Farbintensität mit Standardproben verglichen. Die Genauigkeit beträgt ± 5%.

     

Optical and Electrical Properties of Polymerizing Plasmas and Their Correlation with DLC Film Properties

Diamond-like carbon (DLC) films were grown from radiofrequency plasmas of acetylene-argon mixtures, at different excitation powers, P. The effects of this parameter on the plasma potential, electron density, electron temperature, and plasma activity were investigated using a Langmuir probe. The mean electron temperature increased from about 0.5 to about 7.0 eV while the mean electron density decreased from about 1.2 × 10⁹ to about 0.2 × 10⁹ cm^–3 as P was increased from 25 to 150 W. Both the plasma potential and the plasma activity were found to increase with increasing P. Through actinometric optical emission spectrometry, the relative concentrations of CH, [CH], and H, [H], in the discharge were mapped as a function of the applied power. A rise in [H] and a fall in [CH] with increasing P were observed and are discussed in relation to the plasma characteristics and the subimplantation model. The optical properties of the films were calculated from ultraviolet-visible spectroscopic data; the surface resistivity was measured by the two-point probe method. The optical gap, E _G, and the surface resistivity, _s, fall with increasing P. E _G and _s are in the ranges of about 2.0–1.3 eV and 10¹⁴–10¹⁶ /, respectively. The plasma power also influences the film self-bias, V _b, via a linear dependence, and the effect of V _b on ion bombardment during growth is addressed together with variation in the relative densities of sp² and sp³ bonds in the films as determined by Raman spectroscopy.     

Co-thickness and oxidation states effect on magnetic anisotropy in Co/MgO heterostructure

Interfacial magnetism and magnetic anisotropy constant ($K_i$) in Co/MgO heterostructure have been studied using ab-initio density functional calculations. It is found that interfacial Co spin magnetic moment shows a strong interdependence on Co-O bond lengths and a reasonable spin-polarization of ～80% is established as a function of Co layers. Our results revealed a saturated positive (out-of-plane) $K_i$ of +2.80 mJ/m² at ≥12 Co layers (～1.6 nm Co thickness), which is associated with orbital magnetic moment difference in [100] and [001] direction along with a strong hybridization between $d_{xy}$ and $d_{x^2?y^2}$ orbitals through orbital angular momentum operator $\stackrel{?}{L_z}$. Furthermore, it is shown that the $K_i$ magnitude almost remains constant and weakens in the case of under- and over-oxidations in the interfacial MgO and Co layers, respectively. Interestingly, $K_i$ improved for oxygen migrated interface due to enhanced $d_{xy}$ and $d_{x^2?y^2}$ orbitals coupling. The disordered interfaces stability is checked by analyzing the formation energy. Hence, the present findings disclose that the higher Co thickness in ordered Co/MgO structure supports to out-of-plane [001] (positive) $K_i$, which could be useful for its technological implementation in high-density magnetic data storage devices with high thermal stability.     

A study of heat and mass transfer of Non-Newtonian fluid with surface chemical reaction

Considering the significance of non-Newtonian fluid usage in manufacturing such as molten plastics, polymeric materials, pulps, and so on, significant efforts have been made to investigate the phenomenon of non-Newtonian fluids. In this article the influences of heat and mass transfer on non-Newtonian Walter's B fluid flow over uppermost catalytic surface of a paraboloid is encountered. An elasticity of the fluid layer is considered in the freestream together with heat source/sink and has the tendency to cause heat flow in the fluid saturated domain. The flow problem of two-dimensional Walter's B fluid is represented using Law of conservation of mass, momentum, heat, and concentration along with thermal and solutal chemical reactive boundary conditions. The governing equations are non-linear partial differential equation and are non-dimensionalized by employing stream function and similarity transformation. The final dimensionless equations yielded are coupled non-linear ordinary differential equations. Furthermore, shooting technique along with RK-4th order method is used to get the numerical results. Graphs and tables are modeled by using MATLAB software to check the effects of Walter's B parameter, Chemical reaction parameter and Thickness parameter on temperature, velocity, and concentration profiles. Tabular analysis shows the results of some physical parameters like skin friction coefficient, Nusselt number and Sherwood number due to the variation of Walter's B parameter, thickness parameter and chemical reactive parameter.     

Synthesis and inverse virtual screening of new bi-cyclic structures towards cancer-relevant cellular targets

Structural Chemistry - We report here synthetic approaches to access new classes of small molecules based on three heterocyclic scaffolds, i.e. 3,7-dihydropyrimido[4,5-d]pyridazine-4,8-dione,...     

Methoxy-Substituted Tyramine Derivatives Synthesis,Computational Studies and Tyrosinase Inhibitory Kinetics

Targeting tyrosinase for melanogenesis disorders is an established strategy. Hydroxyl-substituted benzoic and cinnamic acid scaffolds were incorporated into new chemotypes that displayed in vitro inhibitory effects against mushroom and human tyrosinase for the purpose of identifying anti-melanogenic ingredients. The most active compound 2-((4-methoxyphenethyl)amino)-2-oxoethyl (E)-3-(2,4-dihydroxyphenyl) acrylate (Ph9), inhibited mushroom tyrosinase with an IC₅₀ of 0.059 nM, while 2-((4-methoxyphenethyl)amino)-2-oxoethyl cinnamate (Ph6) had an IC₅₀ of 2.1 nM compared to the positive control, kojic acid IC₅₀ 16700 nM. Results of human tyrosinase inhibitory activity in A375 human melanoma cells showed that compound (Ph9) and Ph6 exhibited 94.6% and 92.2% inhibitory activity respectively while the positive control kojic acid showed 72.9% inhibition. Enzyme kinetics reflected a mixed type of inhibition for inhibitor Ph9 (K_i 0.093 nM) and non-competitive inhibition for Ph6 (K_i 2.3 nM) revealed from Lineweaver–Burk plots. In silico docking studies with mushroom tyrosinase (PDB ID:2Y9X) predicted possible binding modes in the catalytic site for these active compounds. Ph9 displayed no PAINS (pan-assay interference compounds) alerts. Our results showed that compound Ph9 is a potential candidate for further development of tyrosinase inhibitors.     

Spin‐polarized electron gas in Co2M Si/SrTiO3 (M = Ti,V, Cr,Mn, and Fe) heterostructures

Spin‐polarized density functional theory is used to study the TiO₂ terminated interfaces between the magnetic Heusler alloys Co₂Si (M = Ti, V, Cr, Mn, and Fe) and the non‐polar band insulator SrTiO₃. The structural relaxation at the interface turns out to depend systematically on the lattice mis‐ match. Charge transfer from the Heusler alloys (mainly the M 3d orbitals) to the Ti d_xy orbitals of the TiO₂ interface layer is found to gradually grow from M = Ti to Fe, resulting in an electron gas with increasing density of spin‐polarized charge carriers. (© 2016 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)