Analytical applications of ternary complexes-IV Titration of macro- and micro-amounts of cyanide

The use of a 1,10-phenanthroline/Bromopyrogallol Red indicator system is proposed for the visual and photometric titration of cyanide with silver nitrate in the range 10⁻¹–10⁻⁴M and 10⁻⁴–10⁻⁵M respectively. Sharp, well-defined end-points are observed and the titration succeeds at low concentrations where the Liebig-Dénigès method is inapplicable. The results obtained agree well with those of the conventional method. EDTA may be used as a mass-masking agent for most cations.     

High spin states in the nucleus150Tb

Excited states in the nucleus¹⁵⁰Tb have been investigated up to spin 39? and 13 MeV excitation energy using the¹³⁰Te(²⁷Al, 7n) reaction and the EUROGAM array. The theoretical interpretation of the observed states has been performed in the framework of the deformed independent particle model. The analysis of the decay out of the yrast superdeformed band indicates that normal-deformed states with spins between 24? and 28? are fed.     

Microwave absorption studies of MgB2 superconductor

Microwave absorption studies have been carried out on MgB₂ superconductor using a standard X-band EPR spectrometer. The modulated low-field microwave absorption signals recorded for polycrystalline (grain size ∼ 10 μm) samples suggested the absence of weak-link character. The field dependent direct microwave absorption has been found to obey a ✓H dependence with two different slopes, which indicated a transition from strongly pinned lattice to flux flow regime.     

A simple non-selective detector for gas phase chromotography, using the measurement of reflected microwave power

A non-selective detector is described which can be used in conjunction with the microwave-excited emissive argon plasma detector. The mode of operation is based on the measurement of reflected power and its use is demonstrated with respect to a range of component vapours and permanent gases. The limit of detection for nearly all the species investigated is in the nanogram range and the detector responded to all compounds examined.     

The FT-IR study of the brain tissue of Labeo rohita due to arsenic intoxication

The brain is believed to be particularly vulnerable to arsenic due to its high oxygen consumption rate and high level of polyunsaturated fatty acids and relatively high rate of oxygen free radical generate without commensurable level of arsenic. Hence, in the present work an attempt is made to study the changes in the biochemical contents in the brain tissues of edible fish Labeo rohita due to arsenic intoxication using Fourier Transform Infrared (FT-IR) spectroscopy. FT-IR spectra reveal significant differences in absorbance intensities between the control and arsenic intoxicated brain tissues, reflecting an alteration on the major biochemical constituents, such as lipids, proteins and nucleic acids of the brain tissues of L. rohita due to arsenic intoxication. Further, the administration of antidote DMSA improves the protein and lipid contents significantly in the brain tissues when compared to arsenic intoxicated tissues. The decrease in α-helix structure due to arsenic intoxication might be responsible for the increase in β-sheet secondary structures, which is consistent with the mechanism of β-sheet formation.     

Routine analysis by high precision gas chromatography/mass selective detector/isotope ratio mass spectrometry to 0.1 parts per mil

Stable isotope methods are potentially quite useful for validating natural or enhanced mineral degradation of contaminants. For this reason, a continuous flow gas chromatograph (GC), isotope ratio mass spectrometer (IRMS) has been coupled with a quadrupole mass selective detector (MSD) to allow simultaneous mass spectral and stable carbon isotope ratio data to be obtained from a single chromatographic analysis. This allows the target contaminant and any extra-cellular degradation intermediates to be both qualified and quantified. Previously acceptable limits of precision (0.3 parts per mil) are undesirable given the small fractionation observed during aerobic degradation. To further understand the fate of organic contaminants and to gain information about the metabolic degradative pathway employed by a microorganism, routine isotopic analyses on a range of analytes have been performed. Quantities of sample producing mass-44 ion beam signal (I(44)) of 2 x 10(-10) to 1 x 10(-8) A were analysed. When the IRMS was tuned for high sensitivity, ion source nonlinearities were overcome by peak height correction from an algorithm that was produced using known isotopic standards of varying concentrations. This led to sample accuracy of <0.01 per thousand and sample precision of 0.1 per thousand. Copyright 1999 John Wiley & Sons, Ltd.     

Frequency scan for the analysis of high mass ions generated by matrix-assisted laser desorption/ionization in a paul trap

An ion trap has been modified for the analysis of high mass ions generated by matrix-assisted laser desorption/ionization. Samples are deposited on a probe tip and introduced directly onto the hyperbolically shaped surface of one endcap. All three electrodes - both the endcaps and the ring electrode - are insulated so that the radio frequency (Rf) voltage may be applied to the center ring electrode and the inverted Rf voltage to the endcaps. By using low frequencies (below 100 kHz) and low amplitudes (below 200 V), high mass singly charged ions may be trapped and analyzed by a frequency sweep at constant amplitude. In the high mass range (60-160 kDa), this instrument showed good sensitivity, signal-to-noise ratios, and mass resolution. Copyright 1999 John Wiley & Sons, Ltd.     

A comparison of the known SD bands in the mass A≈80 region

The mass A≈80 region is now firmly established as the newest region of superdeformation, with up to 11 nuclei exhibiting as many as 21 superdeformed bands. The dynamic moments of inertia of these bands reveal a variety of interesting features, such as superdeformed band crossings and the first pair of identical superdeformed bands in the mass A≈80 region. Cranked shell model calculations have been performed and the bands are interpreted in terms of the number of high-N intruder orbitals occupied. The differences in dynamic moments of inertia and the proposed single particle configurations are discussed.     

Analytical applications of ternary complexes-VI Spectrophotometric determination of trace amounts of palladium

Extremely sensitive and specific colour reactions in both aqueous and organic solutions are described for the spectrophotometric determination of palladium(II) ions. The methods are based upon ternary complex formation with 1,10-phenanthroline or pyridine, and Rose Bengal Extra. Themolar absorptivities are 5 × 10⁴ (aqueous) and 1.25 × 10⁵ (organic) in the presence of a 1000-fold molar excess of EDTA as mass masking agent. Under these conditions there is negligible interference with the pyridine-Rose Bengal Extra system from the 22 cations (including silver, gold and platinum) and seven anions investigated. Both colour reactions take place within 15 min and the complexes are stable for long periods.