119Sn chemical shifts in seven-coordinate organotin compounds

The FT NMR studies revealed that ¹¹⁹Sn chemical shifts in seven-coordinate organotin compounds are more than 100 ppm upfield from those in six-coordinate analogues.     

Simultaneous determination of iron(II), iron(III), and titanium(IV) by flow injection analysis using kinetic spectrophotometry with Tiron

Summary Two flow injection analysis systems have been worked out for the simultaneous determination of Fe(III), Fe(II), and Ti(IV) based on the kinetic spectrophotometry with Tiron. The first system uses a silver reductor column and a single detector with two flow cells aligned in the same optical path to yield two peaks corresponding to (a) Ti(IV)-Tiron and (b) Ti(IV) plus total iron(III)-Tiron complexes. An another sample injection without the silver column yields a single peak which corresponds to Ti(IV) plus Fe(III)-Tiron complexes. With the two sample aliquot injections the system permits simultaneous determinations with throughput of 30 samples/h in the g to several tens g range of each species. The second system is a multidetection system with or without the silver reductor column using the same spectrophotometry with Tiron, in which the entrapment of the sample plug into a closed system allows its repetitive passage through a single detector. With the advantage of much simpler instrumentation, the system permits 6 samples/h to be analyzed for the three metal species with somewhat lower precisions than the first system.     

Anion-exchange system in magnesium nitrate media. Application to chemical analysis of manganese nodules for thorium and uranium

Summary The adsorption behaviour of 26 metal ions on the strongly basic anion-exchange resin Bio Rad AG-1, X-8 has been examined in magnesium nitrate media. The salt concentration range from 0.50-3.0 M is covered in the presence of 0.1 M free nitric acid. The distribution coefficients of bismuth(III), thorium(IV) and uranium(VI) rise to the order of 1,000 in media of 0.1 M nitric acid with high salt strength, while most other elements are only weakly adsorbed as is also the case in pure nitric acid media. The system allows thorium(IV) and uranium(VI) to be concentrated simultaneously from 2.5 M nitrate media, so that it can be applied successfully to the determination of thorium and uranium in manganese nodules with consecutive Chromatographic elution from a single small resin column. The subsequent determination is carried out spectrophotometrically with Arsenazo III.

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Anionenaustausch in Magnesiumnitratlösung. Anwendung zur Thorium- und Uranbestimmung in Manganknollen

Zusammenfassung Das Adsorptionsverhalten von 26 Metallionen wurde aus Magnesiumnitratlösung an dem stark basischen Anionenaustauscher Bio-Rad AG-1, X-8, untersucht. Die Salzkonzentration reichte von 0,5-3,0 M bei Gegenwart von 0,1 M freier Salpetersäure. Die Verteilungskoeffizienten von Bismut(III), Thorium(IV) und Uran(VI) reichen bei hoher Salzkonzentration bis zur Größenordnung von 1000, wogegen die meisten anderen Elemente nur schwach adsorbiert werden, was auch in reiner salpetersaurer Lösung der Fall ist. Dadurch können Th(IV) und U(VI) gleichzeitig aus 2,5 M Nitratlösung angereichert und mit gutem Erfolg in Manganknollen bestimmt werden, wobei nur eine einzige Elution von einer kleinen Harzsäule erforderlich ist. Die anschließende Bestimmung erfolgt spektralphotometrisch mit Arsenazo III.

     

Determination of traces of gallium and indium in ores by electrothermal-atomization atomic absorption spectrometry with matrix modifications

Methods were developed for the determination of gallium and indium in complex ores by electrothermal-atomization atomic absorption Spectrometry using matrix modifications. Nickel and nickel-ammonium sulfate as matrix modifier has enhanced the absorption signals for gallium and indium, respectively, eliminating the matrix interferences to allow their solutions in nitric acid to be used as calibration standards. No matrix separations are necessary. Results are quoted for a variety of black ore samples (Kuroko). The RSDs are 7.0% for gallium and 5.3% for indium at their 10 g/g levels, and the inverse sensitivities are 20 pg of gallium and 38 pg of indium for respective 1% absorption.     

Determination of rhenium by neutron activation

A neutron activation method is proposed for the determination of rhenium in rocks and ores. After the irradiation, the radiochemical separation consists of a one-step anion exchange; β-activities of radiochemically pure ¹⁸⁸Re or ¹⁸⁶Re are counted. The chemical yield averaged 75% and there was a considerable saving of time in the radiochemical work. Results are quoted for the rhenium contents of the standard rock W-1, several molybdenites and pyrolusites.     

Determination of five trace elements in sea water after separation by anion-exchange chromatography

Summary A preconcentration technique involving anion-exchange in a thiocyanate medium has been developed for the determination of traces of vanadium, cobalt, copper, zinc, and cadmium in sea water. A conventional, small column containing a strongly basic anionexchange resin Amberlite CG 400 in the thiocyanate form allows the five trace metals to be concentrated from a 11 of sea water sample adjusted to 0.1M in thiocyanate and 0.1M in hydrochloric acid. Sorbed metals can be recovered simultaneously by elution with 140 ml of 2M perchloric acid. A stepwise elution technique is also developed, which permits removal of vanadium-copper-cobalt as a group, zinc, and cadmium to improve the selectivity of the separation. A simple scheme of separation for vanadium, copper, and cobalt is given, so that spectrophotometric determinations of these metals even with nonselective reagents may be feasible. Results are quoted on the preconcentration and subsequent spectrophotometric determination of the five metals in brine and sea waters.     

Dry-column chromatography of uranium. Application to chemical analysis of monazite and phosphate rock for uranium

Summary A dry-column Chromatographic technique has been applied to the separation of uranium from complicated matrices. It has been demonstrated that operating parameters of thin-layer chromatography on silanized silica gel in isopropyl ether-tetrahydrofuran-nitric acid (65203) can be transferred to this technique. Chromatograms are thus easily developed on dry packed column with the solvent system of the type used in the TLC. Uranium is eluted off the column and determined with Arsenazo III spectrophotometrically. The technique is successfully applied to the determination of uranium in monazite and phosphate rock samples with good precision and accuracy.

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Trockensäulenchromatographie des Urans. Anwendung zur chemischen Analyse von Monazit und Phosphorit

Zusammenfassung Zur Abtrennung des Urans aus komplizierten Matrices wurde die Trockensäulenchromatographie verwendet. Wie gezeigt werden konnte, lassen sich die Bedingungen der Dünnschichtchromatographie (DSC) auf silanisiertem Silikagel mit Isopropylether-Tetrahydrofuran-Salpetersäure (65203) auf das genannte Verfahren übertragen. Chromatogramme sind daher auf trocken geschichteten Säulen mit Lösungsmittelsystemen der DSC herstellbar. Uran wird eluiert und mit Arsenazo III spektrophotometrisch bestimmt. Das Verfahren wurde zur Uranbestimmung in Monazit und Phosphorit erfolgreich angewendet.