Neutron activation analysis of microgram amounts of thorium in uranium ores and process liquors by means of thorium-233

A method is described for neutron activation analysis of thorium by employing thorium-233. Decontamination steps include anion exchange in 12.5 N HCL, precipitation of fluoride, extraction with mesityl oxide and thorium oxalate precipitation. The time spent is less than 1 h; spurious activities in counting samples amount only to 2% and can easily be corrected for. The sensitivity of the method is ca. 0.02 μg of thorium in a neutron flux of 10¹²n/cm²/sec with an irradiation time of 5 min.     

The potentiometric and amperometric determination of silver with mercaptophenylthiothiadiazolone and mercaptobenzthiazole

Summary The previously described gravimetric determinations of silver were used for the potentiometric and amperometric determinations of silver in the presence of interfering cations. The potentiometric titration of silver with MFTD (MBT) is a simple matter, if enough complexone is present, in both ammoniacal and neutral solutions. The amperometric determination of silver with MFTD (MBT) is carried out in neutral solution, containing complexone, with rotated platinum electrode and mercury-mercuric iodide half-cell, short-circuited through a microammeter. The only interfering elements are mercury, gold, and some of the platinum metals.     

Synthetische Versuche in der Gruppe hypotensiv wirksamer Alkaloide, 13. Mitt.: Synthese vondl-10-Methyldeserpidin,dl-10-Äthoxydeserpidin unddl-10-Methylmercapto-deserpidin

Zusammenfassung Die durch Umsetzung von 5-Methyltryptamin, 5-Äthoxytryptamin und 5-Methylmercapto-tryptamin (I, R=CH₃, OC₂H₅ bzw. SCH₃) mit dem racemischen Aldehyd-Ester II entstandenenSchiffschen Basen wurden durch Natriumborhydrid-Reduktion in Methanol unter gleichzeitiger Cyclisierung und Desacetylierung in die entsprechenden 10-substituiertendl-Methyl-2,3-seco-3-oxodeserpidate (IV) übergeführt. Die bei der Einwirkung von 3,4,5-Trimethoxybenzoylchlorid in Pyridin erhaltenen Ester V wurden weiter mit Phosphoroxychlorid cyclisiert und die Produkte als Perchlorate (VI) mit Zink in sauerer Lösung zu den entsprechenden 10-substituiertendl-Deserpidinen (VII, R=CH₃, OC₂H₅ bzw. SCH₃) reduziert. Mit Hilfe der Chromatographie gelang es in zwei Fällen, aus den Rohprodukten auch die entsprechendendl-3-Isodeserpidine (VIII, R=CH₃ bzw. OC₂H₅) zu isolieren. Zum Unterscheiden der Produkte der normalen Reihe (VII) und der 3-Iso-Reihe (VIII) wurden IR-Spektren und die Papierchromatographie angewendet.Mit 2 Abbildungen     

On-line filtration system for determining total chromium and chromium in the soluble fraction of industrial effluents by flow injection flame atomic absorption spectrometry

Two manifolds were assessed for the purpose of determining both the total chromium content and that present as a soluble form in industrial effluents by flow injection flame atomic absorption spectrometry (FI-FAAS). To determine the chromium content in the soluble fraction the samples were used without additional treatment, a 0.45 microm filter being included in the FI system. To determine the total chromium content, the samples were acidified with nitric acid 20% (v/v) and heated for 30 s in a microwave oven (temperatures of about 70 degrees C were reached). The problem posed by the very different concentration range in which total and soluble chromium are present was overcome by using programmed flow rate methodology and by only partially emptying the sample loop. A personal computer controlled both the rotation speed of a peristaltic pump and the volume of sample injected into the system, thus obtaining the dispersion degree required. Using the manifold proposed, the chromium content in the soluble fraction can be determined in the 0.5-20 microg mL(-1) range using a 10 microg mL(-1) single standard for calibration. To determine the total chromium content, a calibration line in the 20-200 microg mL(-1) range was obtained using a single 50 microg mL(-1) chromium standard solution. The reliability of the semi-automatic devices was verified by comparing the results obtained with those found by treating the samples and using both FAAS in a conventional way and a spectrophotometric method using diphenylcarbazide at the 95% confidence level (ANOVA test). The proposed procedures showed a RSD lower than +/-3%.     

Electrodeposition of cobalt on stainless steel foils. Preparation of57Co sources for Mössbauer experiments

Conditions for the electrodeposition of⁵⁹Co and⁵⁷Co on stainless steel foils have been studied. A set of electrolytic parameters has been determined to get a reasonably good electrodeposited sample. The⁵⁷Co electrodeposited foil was then introduced in a quartz tube to be annealed in an argon flow. The final product was a 11 Ci Mössbauer source for college experiments which was succesfully tested by obtaining spectra of stainless steel and sodium nitroprusside.     

Effects of genesis and ionizing radiation on the kinetics of reduction of NiO-CeO2 mixed oxides with hydrogen

The reduction of mixed oxides NiO-CeO₂ of various composition with hydrogen was studied at 290–470° by means of thermogravimetry. Some physicochemical properties of the system were also investigated and compared with earlier studied analogous samples of different “origin”. The degree of mutual interaction of the two components, the reduction kinetics and the sensitivity to the different sorts of radiation (gamma-rays, fast neutrons and electrons), applied in different doses, are strongly affected by the “pre-history” and by the composition in both compared series of mixed oxides.     

Studies on the conversions of diols and cyclic ethers—49: Stereochemistry of cyclodehydration of 1,4-diols on the action of brönsted and lewis acids: a comprehensive study

The stereochemistry of the cyclodehydration of (±)- and meso-2,5-hexanediol on the action of various dehydrating agents was investigated. The earlier assumed and confirmed intramolecular S_N2 mechanism for acid-catalysed ring-closure was found to hold in most cases. Various extents of racemisation can be observed on the action of certain Lewis acids, and the solvents concentrated H₂SO₄ and HMPT (hexamethyl phosporic acid triamide) under previously unexamined reaction conditions.     

Relationships for determining the rate constant of the polymerization growth reaction by means of the emulsion polymerization method

Some simple equations for the emulsion polymerization system were derived on the basis of the Smith-Ewart theory. These are used in calculating the molar monomer concentration and rate of polymerization in units of moles per liter per second for the zero-order region with respect to the monomer as well as in calculating the rate constant of the growth reaction.     

Determination of iron at ng/ml level by solid phase spectrophotometry after preconcentration on cation exchange filters

A cationic exchanger paper is used to retain analytes in solution and, after drying, to analyze directly by measuring the UV-Vis absorbance of the paper. The method was applied to determination of iron using its known 1,10-phenanthroline complex. Using 100 ml of sample the applicable concentration range was between 1.0 and 10.0 ng/ml with a detection limit of 0.2 ng/ml and a RSD around 2%. The method was applied to determination of iron total in snow, human serum and wine.     

Microdynamics of solid anilinium chloride

Intraionic C₃ reorientation of the anilinium NH⁺₃ group was evidenced by measurements of the temperature dependence of the proton spin—lattice relaxation time, by rotating frame experiments and cw NMR data. Analysis of the results yielded a rotor hindering potential E = 33.6 kJ/mole and τ_o = 4 × 10⁻¹³ s.