Ultratrace Analysis of Dopamine Using a Combination of Imprinted Polymer-Brush-Coated SPME and Imprinted Polymer Sensor Techniques

A combination approach in solid-phase microextraction, based on a molecularly imprinted polymer-brush coating on an optical fiber coupled with a complementary molecularly imprinted polymer sensor, has been adopted for isolation, preconcentration, and analysis of dopamine at ultratrace levels in highly dilute aqueous samples. This combination enabled enhanced (up to 8.5-fold) preconcentration of the analyte, which is appropriate for achieving a stringent detection limit in clinical diagnosis of several neurodegenerative diseases. The detection limit of dopamine in biological samples was 0.018 ng mL^?1 with a relative standard deviation less than 2.1% and without any non-specific contributions.     

Preparation of electrodeless discharge lamps for emission studies of uranium isotopes at trace level

A simplified method for preparation of electrodeless discharge lamp for uranium isotopes with specific concerns for ²³²U is described. Micro-gram quantities of solid uranium oxides and aqueous solution of uranium nitrate have been used as a starting material for in situ synthesis of uranium tetraiodide. High temperature iodination reaction is carried out in the presence of inert gas neon. By careful design, the preparation time and surface area of quartz reaction tubes have been reduced considerably. The latter decreases the level of contamination which has a direct bearing on the operational lifetime of the lamps. Incorporation of steps to purify the product from an unwanted material improved the stability of the lamps. The procedure provides a safe and convenient way of handling ²³²U in particular but can be extended in general to any actinides having radioactivity similar to that of freshly separated ²³²U. Characteristic emission of uranium isotopes have been recorded by Fourier Transform Spectrometer to show the satisfactory operation of the lamps as well as their usage for studying emission spectra of the specific isotope.     

Multilayer mirror as a substrate for total reflection X-ray fluorescence spectrometry

X-ray field intensity generated over a multilayer surface during a strong Bragg reflection condition has been used to analyze the particulate matter deposited on its surface, for the average particles size distribution and detection sensitivity of various elements. The elemental detection sensitivities achieved at Bragg reflection condition are compared to those obtained at incidence angles below critical angle, under total external reflection condition. The results obtained indicate that when big size particles (> 1 μm) are distributed over a large surface area, the observed fluorescence yields deteriorate by 15–18% in the total external reflection condition, due to strong sample absorption effects. In such a case, use of a multilayer mirror as a sample carrier and fluorescence excitation under Bragg reflection condition provides better fluorescence yield and hence improved detection sensitivity for an element.     

Characterization of trace embedded impurities in thin multilayer structures using synchrotron X‐ray standing waves

X‐ray standing wave (XSW) field generated under Bragg reflection condition in a periodic Mo/Si multilayer structure has been used to determine the concentration and location of various trace element contaminants embedded in different layers of that multilayer structure. We have used intense synchrotron X rays for XSW analysis. It is observed that various trace element impurities such as Cr, Fe, Ni and W get embedded unintentionally in the multilayer structure during the deposition process. Consequences of such impurity incorporation on the optical properties of the multilayer structure are discussed in hard and soft X‐ray regions. Present measurements are important in order to optimize the deposition methods on one hand and to better correlate the measured optical properties of a multilayer structure with theoretical models on the other. Copyright © 2010 John Wiley & Sons, Ltd.     

A New Spectrophotometric Method for the Determination of Ascorbic Acid Using Leuco Malachite Green

A new simple and sensitive and selective spectrophotometric method has been developed for the determination of ascorbic acid (AA) at trace level using a new reagent, leuco malachite green (LMG). AAreacts with potassium iodide‐iodate solution under acidic conditions to liberate iodine and the liberated iodine selectively oxidizes LMG to MG dye. The colour of the dye was measured at 620 nm. Beer's law is obeyed over the concentration range of 0.8–8 iμg μAA per 25 mL of final solution (0.032–0.32 ppm). The apparent molar absorptivity and Sandell's sensitivity of the method were found to be 2.98 × 10⁵ l mol⁻¹ cm⁻¹, 0.0042 μg cm⁻², and respectively. Statistical treatment of the experimental results indicates that the method is precise and accurate. The method is free from interference of common ions and many of the ingredients commonly found in pharmaceuticals. The reliability of the method was established by parallel determination against Leucocrystal violet (LCV) method. The method described was satisfactorily applied for the determination of AA in fruit juices, pharmaceuticals and biological samples.     

Nanofibrous polyaniline thin film prepared by plasma‐induced polymerization technique for detection of NO2 gas

A nanofibrous polyaniline (PANI) thin film was fabricated using plasma‐induced polymerization method and explored its application in the fabrication of NO₂ gas sensor. The effects of substrate position, pressure, and the number of plasma pulses on the PANI film growth rate were monitored and an optimum condition for the PANI thin film preparation was established. The resulting PANI film was characterized with UV–visible spectrophotometer, FTIR, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The PANI thin film possessed nanofibers with a diameter ranging from 15 to 20 nm. The NO₂ gas sensing behavior was studied by measuring the change in electrical conductivity of PANI film with respect to NO₂ gas concentration and exposure time. The optimized sensor exhibited a sensitivity factor of 206 with a response time of 23 sec. The NO₂ gas sensor using nanofibrous PANI thin film as sensing probe showed a linear current response to the NO₂ gas concentration in the range of 10–100 ppm. Copyright © 2009 John Wiley & Sons, Ltd.     

Optical and dielectric properties of isothermally crystallized nano-KNbO3 in Er3+-doped K2O–Nb2O5–SiO2 glasses

Precursor glass of composition 25K₂O–25Nb₂O₅–50SiO₂ (mol%) doped with Er₂O₃ (0.5 wt% in excess) was isothermally crystallized at 800 °C for 0–100 h to obtain transparent KNbO₃ nanostructured glass–ceramics. XRD, FESEM, TEM, FTIRRS, dielectric constant, refractive index, absorption and fluorescence measurements were carried out to analyze the morphology, dielectric, structure and optical properties of the glass–ceramics. The crystallite size of KNbO₃ estimated from XRD and TEM is found to vary in the range 7–23 nm. A steep rise in the dielectric constant of glass–ceramics with heat-treatment time reveals the formation of ferroelectric nanocrystalline KNbO₃ phase. The measured visible photoluminescence spectra have exhibited green emission transitions of ²H_11/2, ⁴S_3/2 → ⁴I_15/2 upon excitation at 377 nm (⁴I_15/2 → ⁴G_11/2) absorption band of Er³⁺ ions. The near infrared (NIR) emission transition ⁴I_13/2 → ⁴I_15/2 is detected around 1550 nm on excitation at 980 nm (⁴I_15/2 → ⁴I_11/2) of absorption bands of Er³⁺ ions. It is observed that photoluminescent intensity at 526 nm (²H_11/2 → ⁴I_15/2), 550 nm (⁴S_3/2 → ⁴I_15/2) and 1550 nm (⁴I_13/2 → ⁴I_15/2) initially decrease and then gradually increase with increase in heat-treatment time. The measured lifetime (τ_f) of the ⁴I_13/2 → ⁴I_15/2 transition also possesses a similar trend. The measured absorption and fluorescence spectra reveal that the Er³⁺ ions gradually enter into the KNbO₃ nanocrystals.     

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.     

Thermoluminescence characteristics of inorganically and organically capped ZnS:Cu nanophosphors

ZnS:Cu nanophosphors were prepared by wet chemical methods and characterized by X-ray diffraction (XRD). The typical morphologies of the nanophosphors were investigated by scanning electron microscopy (SEM). The thermoluminescence (TL) properties of inorganically and organically passivated ZnS:Cu nanophosphors were investigated after γ-irradiation using a ⁶⁰Co source at room temperature. The TL glow curve of capped ZnS:Cu showed variation in TL peak and intensity as the capping agent was changed. Amongst the synthesized samples the TL glow curve of SiO₂ capped ZnS:Cu showed the highest TL intensity. It has been found that TL response of SiO₂ capped ZnS:Cu is linear in the range 10-550 Gy. A discussion of the obtained results is also presented.     

Resonance effects in the nonadiabatic nonlinear quantum dimer

In the presence of 1/f ^β noise, we investigate the logical stochastic resonance (LSR) in an asymmetric bistable model driven by various cycling combinations of two logic inputs. The probability of correct logic outputs is calculated according to true table of logic relationships. Two major results are presented. Firstly, it is shown that the LSR effect can be obtained by changing noise strength. Over entire range of noise variance, white noise can be considered to be better than 1/f noise or 1/f ² noise to obtain clean logic operation. At a smaller noise level, 1/f noise can realize higher output probability than white noise or 1/f ² noise. In the sense, 1/f noise can be considered to be better than white noise or 1/f ². On the other hand, the correct probability can evolves nonmonotonically as noise exponent β increases, and a kind of SR-like effect can be obtained as a result of β. At certain intermediate noise variance, the output probability is able to attain its minimum at β = 1. It is also shown that actually some finite β sometime can be better than β = 0 at small range of noise variance. The study might provide some potential complement to LSR effect in the presence of 1/f ^β noise.