Microdetermination of carbonyl compounds by reduction with alkaline sodium borohydride

Summary Alkaline sodium borohydride has been employed as a reducing reagent for the titrimetric determination of compounds containing the carbonyl function. The sample is dissolved in methanol and is then reduced with alkaline sodium borohydride. After completion of the reaction, the excess sodium borohydride is back titrated against standardized hydrochloric acid solution using methyl red as indicator. The stoichiometry between the carbonyl function and sodium borohydride is 41.

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Zusammenfassung Natriumborhydrid dient als Reduktionsmittel zur Titration von Carbonylverbindungen. Die Probe wird in Methanol gelöst und dann mit alkalischem Natriumborhydrid reduziert. Nach Ablauf der Reaktion wird der Überschuß mit Salzsäure gegen Methylrot zurücktitriert. Carbonylverbindung und Natriumborhydrid reagieren im Verhältnis 41.

     

Nighttime enhancements in TEC near the crest of northern equatorial ionization anomaly during low solar activity period

Enhancement in nighttime total electron content (TEC) near the crest of equatorial ionization anomaly at Bhopal (Geog. 23.2°N, 77.4°E, and MLAT 14.2°N) has been studied for the solar minimum period March 2005- November 2006. TEC data recorded by GPS Ionospheric Scintillation and TEC Monitor (GISTM) GSV4004A receiver is used for the study and results are presented in the paper. More than 10% increase in TEC with respect to background content is considered for analysis. Out of total 138 enhancements, 65 observed during pre midnight hours and 73 during post midnight hours. It is observed that nighttime enhancement in TEC at Bhopal occurs in all seasons; it is more frequent during summer, less during equinox and least during winter months. The enhancement in nighttime TEC can be observed both in geomagnetic disturbed time and in quiet time. We found that mean peak amplitude for pre-midnight TEC enhancement are more in equinox and less in winter, while in post-midnight TEC enhancement it is highest in summer and less in winter. Post-midnight enhancements have smaller peak amplitude as compared to pre-midnight. Also the most probable values for pre- and post-midnights are 4.4 TECU and 2.17 TECU respectively. The percentage occurrence of nighttime TEC enhancement does not show any dependence on solar activity whereas the peak amplitude depends on solar activity. The percentage occurrence of nighttime TEC enhancement decreases as the magnetic activity increases whereas there is no such dependency found with peak amplitude. It is also observed that majority of nighttime TEC enhancements are occurred without scintillation. The localised nighttime TEC enhancements near the crest of equatorial ionization anomaly region have been observed most of the nights during the period of study.     

Modeling of transient electroluminescence overshoot in bilayer organic light-emitting diodes using rate equations

When a voltage pulse is applied under forward biased condition to a spin-coated bilayer organic light-emitting diode (OLED), then initially the electroluminescence (EL) intensity appearing after a delay time, increases with time and later on it attains a saturation value. At the end of the voltage pulse, the EL intensity decreases with time, attains a minimum intensity and then it again increases with time, attains a peak value and later on it decreases with time. For the OLEDs, in which the lifetime of trapped carriers is less than the decay time of the EL occurring prior to the onset of overshoot, the EL overshoot begins just after the end of voltage pulse. The overshoot in spin-coated bilayer OLEDs is caused by the presence of an interfacial layer of finite thickness between hole and electron transporting layers in which both transport molecules coexist, whereby the interfacial energy barrier impedes both hole and electron passage. When a voltage pulse is applied to a bilayer OLED, positive and negative space charges are established at the opposite faces of the interfacial layer. Subsequently, the charge recombination occurs with the incoming flux of injected carriers of opposite polarity. When the voltage is turned off, the interfacial charges recombine under the action of their mutual electric field. Thus, after switching off the external voltage the electrons stored in the interface next to the anode cell compartment experience an electric field directed from cathode to anode, and therefore, the electrons move towards the cathode, that is, towards the positive space charge, whereby electron–hole recombination gives rise to luminescence. The EL prior to onset of overshoot is caused by the movement of electrons in the electron transporting states, however, the EL in the overshoot region is caused by the movement of detrapped electrons. On the basis of the rate equations for the detrapping and recombination of charge carriers accumulated at the interface expressions are derived for the transient EL intensity I, time t_m and intensity I_m corresponding to the peak of EL overshoot, total EL intensity I_t and decay of the intensity of EL overshoot. In fact, the decay prior to the onset of EL overshoot is the decay of number of electrons moving in the electron transporting states. The ratio I_m/I_s decreases with increasing value of the applied pulse voltage because I_m increases linearly with the amplitude of applied voltage pulse and I_s increases nonlinearly and rapidly with the increasing amplitude of applied voltage pulse. The lifetime τ_t of electrons at the interface decreases with increasing temperature whereby the dependence of τ_t on temperature follows Arrhenius plot. This fact indicates that the detrapping involves thermally-assisted tunneling of electrons. Using the EL overshoot in bilayer OLEDs, the lifetime of the charge carriers at the interface, recombination time of charge carriers, decay time of the EL prior to onset of overshoot, and the time delay between the voltage pulse and onset time of the EL overshoot can be determined. The intense EL overshoot of nanosecond or shorter time duration may be useful in digital communication, and moreover, the EL overshoot gives important information about the processes involving injection, transport and recombination of charge carriers. The criteria for appearance of EL overshoot in bilayer OLEDs are explored. A good agreement is found between the theoretical and experimental results.     

Highly Selective and Sensitive Graphene Based Electrochemical Sensor for Quantification of Receptor Agonist Rizatriptan

A highly selective and sensitive electrochemical sensor has been developed by modification of a glassy carbon electrode (GCE) with graphene (GRP) for quantification of Rizatriptan. The significant increase of the peak current and the improvement of the oxidation peak potential indicate that the electrochemical sensor facilitates the electron transfer of Rizatriptan. The oxidation peak current was proportional to the Rizatriptan concentration in the range from 100 to 600 µg/mL with detection (LOD) and quantification limit (LOQ) of 36.52 and 121.73 µg/mL, respectively. The developed method was successfully employed for quantification of Rizatriptan in pharmaceutical formulations. The sensor shows great promise for simple, sensitive and quantitative detection of Rizatriptan.     

Sensitive and selective methods for determination of antipsychotic drug olanzapine in pharmaceuticals

Two simple and sensitive spectrophotometric methods have been developed for analysis of the antipsychotic drug olanzapine in pharmaceuticals. Method A is based on liberation of iodine by reaction between the drug and potassium iodate, followed by reaction with leuco crystal violet (LCV), the color of oxidized LCV being measured at 598 nm. Method B is based on oxidation of olanzapine with chloramine-T (CAT) in acidic medium, the unconsumed CAT being determined with rhodamine B, measuring the absorbance at 550 nm. Calibration graphs were linear over the ranges of 0.05–2.0 and 0.1–1.6 μg mL^?1 olanzapine for method A and B, respectively. The molar absorptivity, Sandell’s sensitivity, detection limit, and quantitation limit were found to be 1.59 × 10⁵, 0.00132, 0.038, and 0.117, respectively, for method A and 0.953 × 10⁵, 0.00221, 0.064, and 0.192, respectively, for method B. The optimum conditions and other analytical parameters were evaluated. The proposed methods have been applied successfully for analysis of olanzapine in pure form and its dosage forms, and no interference was observed from common excipients present in pharmaceutical formulations.     

Crystallographic and microstructural aspects of the superconductor YBa2Cu3O7-y —an overview

Crystal structures and structural inhomogeneities observed in YBa₂Cu₃O_7-y are reviewed. It is brought out that a proper understanding of the nature of the structural inhomogeneities is essential for exploiting the technological potential of this material. The need for an adequate characterization of specimens used for experiments is emphasized. Practical implications of the ferroelastic nature of the material are discussed.     

Transient and steady state lateral charge transport in polymeric semiconductors

The Lateral photovoltaic effect (LPE) has been used as an effective tool to probe the dynamics of photogenerated charge carriers in conjugated polymer based optoelectronic devices. In this paper, we analyze the time-dependence of LPE in a position sensing device geometry using a discrete circuit equivalent model coupled with a spreading impedance approach. We elucidate the dependence of the lateral photovoltage (LPV) on the position, intensity and the modulation frequency (ω _c ) of the light beam. Previous experimental results for the position and ω _c dependence of the LPV in the steady state are successfully reproduced within the present approach. We predict a clear knee-like feature in the transient regime of the LPV for high photocurrent values. This feature prompts us to propose that the response time of the organic position sensing device decreases sharply with increasing incident intensity.     

Various ways to strengthen the fiber‐matrix interface for enhanced composite performance

Surface treatment (ST) of carbon fibers (CF) leads to an enhancement in fiber‐matrix adhesion. However, it deteriorates the strength of a fiber which makes its reinforcing action less effective in a composite. These effects in opposite directions control the net strength of a composite, and hence, the treatment has to be judiciously applied, which would enhance the first factor and minimize the second one. Authors have recently reported on four effective techniques (using various doses) such as treatments with nanoparticles of Ytterbium fluoride (YbF₃)_, cold remote nitrogen–oxygen plasma (CRNOP), γ‐ray irradiation and nitric acid oxidation. Amongst these methods, nitric acid oxidation is studied in depth in the literature, and γ‐ray irradiation is sparingly studied. However, nano‐YbF₃ and CRNOP were first time reported in the literature by the authors. However, comparative aspects of all these methods were not addressed. In this paper, these aspects in details are discussed to lay down the right criteria for selection of a ST technique of CF to design the desired performance of a composite. The composites with polyetherimide and treated CF (including untreated) were developed and evaluated for various properties including tribological one. Treated CF based composites exhibited excellent mechanical and tribological properties (under harsh operative conditions with wear rates ≈ 1 × 10^?15 m³/Nm and μ ≈ 0.09). It was concluded that for strength and tribo‐performance, different treatments and doses are to be employed. Overall nanosized‐YbF₃ treatment of CF proved to be the most promising ST method. Copyright © 2013 John Wiley & Sons, Ltd.     

Dynamic and Equilibrium Studies on Adsorption of Cu(II) Ions onto Biopolymeric Cross-Linked Pectin and Alginate Beads

Binary biopolymeric beads of alginate and pectin were prepared and characterized by FTIR spectra. On to the surfaces of the prepared beads were performed static and dynamic adsorption studies of Cu(II) ions at fixed pH and ionic strength of the aqueous metal ion solutions. The adsorption data were applied to Langmuir and Freundlich isotherm equations and various adsorption parameters were calculated. The influence of various experimental parameters such as effect of time, pH, temperature, solid to liquid ratio, and the presence of salts were investigated on the adsorption of copper ions.     

Removal of Rhodamine-B from Aqueous Solution by Adsorption onto Crosslinked Alginate Beads

The biosorption of rhodamine-B from aqueous solution using crosslinked alginate beads was studied by contact method at fixed pH ?3 and room temperature (28 ± 0.2°C). Both the Freundlich and Langmuir isotherm models could describe the adsorption equilibrium of the rhodamine-B onto crosslinked alginate beads. The influence of various experimental parameters such as pH, temperature, effect of concentration and time were evaluated. It was observed that the adsorption capacity of rhodamine-B onto alginate beads decreased with increase in pH and temperature above room temperature.