Application of thermal desorption to the development of a gas chromatographic/mass spectrometric method for the determination of toluene,chlorinated aromatic hydrocarbons,and 2,3,7,8-tetrachlorodibenzo-p-dioxin in combustion emissions

A fast and accurate analytical method, which uses commercially available adsorbents (Tenax TA, Carbotrap B and C, and Carbosieve S-III), was developed for the sampling and determination of aromatic hydrocarbons, chloroaromatic compounds, and 2,3,7,8-tetrachlorodibenzo-p-dioxin. The breakthrough volume data show that Carbotrap C has a good capacity for compounds of high molecular weight, whereas Carbosieve S-III and Tenax TA are efficient for volatile compounds. The organic components are thermally desorbed and transferred to a gas chromatograph/mass spectrometer. Importantly, thermal desorption avoids conventional solvent extraction procedures and also allows reuse of adsorbent tubes. Preliminary results for recovery of analytes from tubes packed with single adsorbent prove that a single-adsorbent bed is not capable of sampling a wide range of compounds. The best method to obtain the desired collection and desorption properties is to use adsorbent tubes containing several different materials. The results of optimization studies are summarized.     

Spectrophotometric Determination of Prochlorperazine Maleate in Pure and Pharmaceutical Preparations

 Prochlorperazine maleate reacts with 1-naphthylamine and sodium nitrite, after heating for 110 s at 80 °C to give an orange red colour having maximum absorbance at 460 nm. The reaction is selective for prochlorperazine maleate with 0.01 mg/mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.01 mg/10 mL to 0.33 mg/10 mL of prochlorperazine maleate and the relative standard deviation is 0.68%. The quantitative assessment of tolerable amounts of other drugs is also studied. Received September 22, 2000. Revision June 19, 2001     

Electrochemical Behavior and Determination of Hyoscine‐N‐Butylbromide from Pharmaceutical Preparations

The electrooxidation of hyoscine N‐butylbromide (HBB) was investigated by rotating disk electrode voltammetry, cyclic voltammetry and controlled potential coulometry in 0.1 M HNO₃ and in 0.1 M tetrabutylammonium perchlorate (TBAP) solutions of acetonitrile at a platinum (Pt) electrode. Based on the results obtained, it is suggested that a bromide ion of HBB was oxidized in one reversible step in aqueous solutions and in two reversible steps in acetonitrile. A differential pulse voltammetric (DPV) method at a Pt electrode was developed for the determination of HBB in the concentration range of 1.0 × 10^?6‐1.0 × 10^?3 M. The procedure was applied to the determination of HBB in its formulations as well as its recovery from blood serum and urine samples.     

Influence of formation path on the CH2BrCl2+ dissociation dynamics

To get further insight into the CH2BrCl site-selective fragmentation previously observed upon inner-shell ionization, we have performed high-resolution Br 3d and Cl 2p Auger and spin-orbit resolved Br 3d Auger spectra, and studied the dissociation properties of the CH2BrCl2+ dication formed at threshold by means of threshold electron pair-ion coincidence measurements. The key point is that the origin of site-specific bond breaking is found in the Auger decay itself, as it preferentially populates selected dication states. Whereas the predominance of the C-Br bond breaking is observed in both threshold and inner-shell studies, no signature of selective C-Cl rupture is reported for the dication formed at threshold.     

Instrumental neutron activation analysis of 23 individual food articles from a high altitude region

Twenty-three individual food items commonly consumed in a high altitude region (Kashmir) have been investigated using instrumental neutron activation analysis. The concentration of Ca, Cl, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Se, Sn, and Zn is reported for these food articles. For quality assurance of our data, IAEA and NIST standard reference materials have also been studied. The dietary intake of these elements was calculated in accordance with the weekly food selection habits of the residents of this area. The dietary contribution of most of these elements was found to be in agreement to the RDA/ESadi levels. The purpose was to design a database of essential elements for this area and to study the adequacy levels of these elements in different dietary items. Fairly adequate intake of Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Se, Sn, and Zn through these foodstuffs is reported, whereas, lower intakes through these items were found for Cl, K, and Na.     

Green Oxidations. Manganese(II) Sulfate Aided Oxidations of Organic Compounds by Potassium Permanganate

Summary. The oxidation of arenes and sulfides by potassium permanganate was accomplished in good yields under solvent free and heterogeneous conditions when manganese(II) sulfate is used as a solid support. After extraction of the organic products, the inorganic products can be reoxidized to permanganate. This result is important because it provides an approach to oxidation reactions that is, in theory, infinitely sustainable.     

Separation of uranium from complex nuclear reaction product mixtures

A solvent extraction procedure for rapid separation of uranium from complex nuclear reaction product mixtures is suggested. The procedure has been tested in batch experiments with tracer amounts of representative elements. It has also been tested with fission products and uranium tracer using the continuous chemical separation system SISAK at the Mainz TRIGA reactor.     

A modified procedure for the Dakin-West reaction: an efficient and convenient method for a one-pot synthesis of β-acetamido ketones using silica sulfuric acid as catalyst

A one-pot, four-component condensation of an aryl aldehyde, an aryl ketone, acetyl chloride and acetonitrile in the presence of silica sulfuric acid as an active, inexpensive, recoverable and recyclable catalyst is disclosed for the synthesis of β-acetamido ketones.     

Synthesis of temperature-sensitive submicron-size composite polymer particles

Temperature-sensitive composite polymer particles were prepared by seeded emulsion copolymerization of dimethylaminoethyl methacrylate and ethylene glycol dimethacrylate with 0.17 m-sized monodispersed polystyrene seed particles. The adsorption and desorption behaviors of low molecular weight cationic emulsifier as well as albumin were examined to determine the variation of surface properties as a function of temperature below and above 35°C.