High-performance liquid radiochromatography: Its application for stability study of [3H] stobadin

An HPLC method was developed for studying the stability of [³H] stobadin stored in physiological saline or buffers at various pH. Optimum conditions for the separation of degradation products were elaborated. A high-performance liquid chromatograph equipped with a radioactivity detector was used.     

FIA-fluorimetric determination of adrenaline in pharmaceutical formulations by oxidation with molecular oxygen

The fluorimetric determination of adrenaline is carried out in a continuous-flow assembly and by means of the molecular dissolved oxygen. The sample solution merges with an NaOH stream, then the resulting mixture is heated at 73 °C and led to the flow-cell of the fluorimeter. The flow-assembly is very simple and the procedure is quick (107 samples h^–1) reproducible (R.S.D. 0.6%), selective and suitable to be applied to determination of adrenaline in formulations. Calibrations graph are linear over the ranges 0.05–15 and 20–40 mgl^–1.     

Recovery and recrystallization in AISI 321 steel under static conditions

Static softening of AISI 321 steel after cold and hot deformation characterizing the industrial thermomechanical treatment was studied by means of tensile tests and TEM. The deformation temperature, the strain and the grain size were the main parameters determining the final softening. The results can be applied for optimization of the solution annealing.     

Stereospecific total synthesis of (±)-strempeliopine

The 18-methylene-1,2-dehydroaspidospermidine (III) was stereospecifically transformed into the schizozygane alkaloid strempeliopine (II) in 16,6 % overall yield.     

Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC-MIP-AES as measurement technique, were approximately 5-10 ng g(-1). Precision in the consecutive analysis of three sediment samples varied between 3 and 10%.     

Spectrophotometric study of bismuth with N-(2-acetamido)iminodiacetic acid (ADA): Determination of bismuth in pharmaceutical formulations

A new method for the Spectrophotometric determination of bismuth using N-(2-acetamido)iminodiacetic acid as complexometric agent is proposed. The complex is formed in a wide pH range, 5.5–7.5, and has a maximum absorption at 265 nm. Beer's law is obeyed in the interval 3.8–17.9 μg of bismuth(III)/ml, with a minimum photometric error of 2.3. The molar absorptivity is 9.1 × 10³ liters/cm mol. The stoichiometry of the reaction takes place in the metal-to-ligand ratio 1:2. The interferences produced by the more common ions are studied. The method has been successfully applied to the determination of bismuth in pharmaceutical formulations.     

Synthesis and stereochemical studies of 6-substituted 1H,3H,6H,7aH-3,3-dimethylimidazo-[1,5-c]thiazol-5-one-7-thiones

The reaction of (4S)-5,5-dimethyl-4-thiazolidine-carboxylic acid 1 with alkyl and aryl isothiocyanates 2 gave bicyclic thiohydantoins 3 . The (2R,4S)- and (2S,4S)-mixtures of 2-substituted 5,5-dimethyl-4-thiazolidine-carboxylic acids 4 and 8 containing two centers of chirality in the analogous reaction afforded thiohydantoins 7 and 10 , respectively, with (1R)-configuration. In some cases we managed to isolate the thioureido acid intermediates 6 and 9 or their triethylamine salts which afforded the corresponding bicycles 7 and 10 under thermal cyclization or acidification. The stereochemistry has been elucidated by high resolution ram studies, optical rotation measurements and X-ray crystallography.     

Radionuclide X-ray fluorescence analysis of drinking water using preconcentration of trace metals on chelating cellulose exchanger OSTSORB-OXIN

Determination of Cr, Fe, Cu, Zn and Pb in drinking water preconcentrated on a chelating ion exchanger of Czechoslovak production is described. The analytical system consisted of a radionuclide source²³⁸Pu, a Si/Li semiconductor detector and a multichannel analyzer. Results are compared with trehshold limit values recommended for drinking water.     

Elaboration of a programmed,semi-automated radiochemical processing system for neutron activation analysis of some volatile elements

Based on the method of SAMSAHL a programmed, semi-automated processing system has been developed and tested for the neutron activation analysis of the following elements: As, Se, Sb, Br, Sn and Te. The main characteristics of the procedure are the following: wet ashing of the sample (by means of digestion in a mixture of concentrated sulphuric acid and hydrogen peroxide), bromination, and chlorination. The procedure is controlled via the appropriate dosage of the reagents and a carefully managed thermal balance. The chemical yield and its reproducibility were determined by tracer techniques using exactly the same parameters as for the active runs. According to the results the method can be used for the routine determination of the given elements except antimony. Presented at the 4th Symposium on the Recent Developments in Neutron Activation Analysis, 1975, Cambridge.     

On the biological importance of the hydrogen bond breaking potency of fluorocarbons

Fluorocarbons containing higher halogens have the potency of breaking certain hydrogen bonds in solutions. The relative strength of this potency varies in the series F < Cl < Br < I and the presence of hydrogen atoms in the fluorocarbon increases it. There is a striking parallelism between the hydrogen bond breaking and the anaesthetic potency of these molecules. It is suggested that the breaking of hydrogen bonds is an important step in the mechanism of anaesthesia.