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.

     

Beta-N-cyanoethyl acyl hydrazide derivatives: a new class of beta-glucuronidase inhibitors

Eight new beta-N-substituted acyl hydrazides along with their corresponding acyl derivatives were synthesized and screened for in vitro beta-glucuronidase inhibition and found to be active against the enzyme. All of these compounds were found to be noncompetitive inhibitors except for N'-(2-cyanoethyl)-4-hydroxy benzohydrazide (10), which was found to be an uncompetitive inhibitor. Structure-activity relationship studies indicated that the benzyloxy group present in compounds 12 and 13 is responsible for the beta-glucuronidase inhibition activity.     

Characterization of ion irradiated silicon surfaces ablated by laser-induced breakdown spectroscopy

Low energy metallic ions,generated by a Q-switched Nd:YAG laser(1064-nm wavelength,10-mJ energy,9-nm～12-ns-pulse width,10~(11)W/cm~2intensity)irradiated on a silicon substrate to modify various properties,such as electrical,morphological,and structural modifications.Thomson parabola technique is used to calculate the energy of these metallic ions whereas the electrical conductivity is calculated with the help of Four-point probe.Interestingly circular tracks forming chain like damage trails are produced via these energetic ions which are carefully examined by optical microscopy.It is observed that excitation,ionization,and cascade collisions are responsible for surface modifications of irradiated samples.Four-point probe analysis revealed that the electrical conductivity of substrate has reduced with increasing trend of atomic number of irradiated metallic ions(Al,Ti,Cu,and Au).The x-ray diffraction analysis elucidated the crystallographic changes leading to reduction of grain size of N-type silicon substrate,which is also associated with the metallic ions used.The decreasing trend of conductivity and grain size is due to thermal stresses,scattering effect,structural imperfections,and non-uniform conduction of energy absorbed by substrate atoms after the ion irradiation.     

Spectroscopic and morphological study of laser ablated Titanium

The optical characteristics of biological tissues sampled from the anterior abdominal wall of laboratory rats are for the first time experimentally studied in a wide wavelength range (350-2500 nm). The experiments have been performed in vitro using a LAMBDA 950 (PerkinElmer, United States) spectrophotometer. Inverse Monte Carlo simulation is used to restore the spectral dependences for scattering and absorption coefficients, as well as the scattering anisotropy factor for biological tissue based on the recorded spectra of diffuse reflection and total and collimated transmissions.     

Mixed convection unsteady stagnation point flow over a stretching sheet with heat transfer in the presence of variable free stream

An analysis is performed for the unsteady mixed convection flow of an incompressible viscous fluid about a stagnation point on a stretching sheet in the presence of a variable free stream. The equations of motion and energy are transformed into the ordinary differential equations by using similarity transformations. Homotopy analysis method is used for the solution of the governing problem. The results have been discussed by plots. The present values of the function are shown very close to the previous limiting solutions. Copyright © 2011 John Wiley & Sons, Ltd.     

THE STRUCTURE OF myo-INOSITOL HEXAPHOSPHATE IN SOLUTION: 31P N.M.R. INVESTIGATION

Abstract

Changes in the ³¹P n.m.r. spectrum of myo-inositol hexaphosphate at different pH reveal that the conformation of this molecule varies with its degree of protonation. Above pH 12 it has the equatorial structure (Ie), below it has the axial conformation (Ia) which it retains to pH 5 when it reverts to le on the addition of a seventh proton. These changes are explained by strong hydrogen bonding between phosphate groups. There is also evidence that at low pH (2) the molecule again reverts to la.     

Purification of Bioactive Lipopeptides Produced by Bacillus subtilis Strain BIA

Bacillus subtilis strain BIA was used for the production of bioactive lipopeptides. Different extraction and purification methods were assayed as liquid–liquid extraction, and acid and ammonium sulfate precipitation followed by TLC, SPE, and gel filtration. Active fractions were further purified using RP-HPLC. The molecular mass of the purified product from HPLC was determined through Tris-Tricine SDS-PAGE and MALDI–TOF-MS. The results revealed that Bacillus subtilis strain BIA produced surfactin and iturin like compounds. Coproduction of surfactin and iturin like compounds by this strain is a remarkable trait for a potential biocontrol agent. This paper also includeds techniques that have been developed for the optimal and convenient extraction of bioactive lipopeptides from microbial origin.

     

On-line spectrophotometric determination of scandium after preconcentration on XAD-4 resin impregnated with nalidixic acid

An on-line scandium preconcentration and determination method was developed with spectrophotometer associated with flow injection. Scandium from aqueous sample solution of pH 4.5 was selectively retained in the minicolumn containing XAD-4 resin impregnated with nalidixic acid at a flow rate of 11.8 mL min^?1 as scandium–nalidixic acid complex. The scandium complex was desorbed from the resin by 0.1 mol L^?1 HCl at a flow rate of 3.2 mL min^?1 and mixed with arsenazo-III solution (0.05 % solution in 0.1 mol L^?1 HCl, 3.2 mL min^?1) and taken to the flow through cell of spectrophotometer where its absorbance was measured at 640 nm. The preconcentration factors obtained were 35 and 155; detection limits of 1.4 and 0.32 μg L^?1 and sample throughputs of 40 and 11 were obtained for preconcentration time of 60 and 300 s, respectively. The tolerance limits of many interfering cations like Th(IV), U (VI), rare-earths and anions like tartrate, citrate, oxalate and fluoride were improved. The method was successfully applied to the determination of scandium from mock seawater samples and good recovery was obtained. The method was also validated on certified reference material IAEA-SL-1 (lake sediment) and the result was in good agreement with the reported value.