Rapid separation of microgram amounts of metal ions on stannic antimonate ion-exchange paper

Summary Microgram amounts of metal ions have been separated using stannic antimonate paper. Most of the separations can be accomplished within 15 minutes.

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Zusammenfassung Unter Verwendung von Zinn(IV)antimonat-Papier lassen sich Mikromengen zahlreicher Metallionen trennen. Die meisten Trennungen lassen sich innerhalb 15 min durchführen.

     

Synthesis and ion-exchange properties of zirconium antimonate

Samples of zirconium antimonate have been prepared under varying conditions of precipitation. Their properties, composition, and ion-exchange behaviour are reported. The 1g K_d vs. pH curves are given for Rb⁺, Cs⁺, Zn²⁺, Ca²⁺ and Tl³⁺ ions. The distribution coefficients of 26 metal ions have been measured and several separations of analytical and radiochemical importance achieved.     

New paper chromatographic separation of microquantities of opium alkaloids

Summary A paper Chromatographic technique on salt-buffered papers for separating the alkaloids of opium has been devised. The method has been used for determining the origin of opium samples by studying the pattern of theR _f values of the alkaloids present and the effect on it produced by the presence of various adulterants.

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Zusammenfassung Die chromatographische Trennung der Opiumalkaloide auf gepuffertem Papier wurde beschrieben. Das Verfahren wurde zur Herkunftsbestimmung von Opiumproben auf Grund desR _f -Musters der anwesenden Alkaloide benützt. Der Einfluß verschiedener Fälschungszusätze wurde untersucht.

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Résumé Mise au point d'une technique de Chromatographie sur papier pour la séparation des alcaloïdes de l'opium, oú les papiers sont imprégnés des sels tampons. Utilisation de la méthode pour déterminer l'origine des échantillons d'opium en étudiant les valeurs duR _f des alcaloïdes présents et l'effet produits sur celles-ci par la présence d'adultérants divers.

     

Structural studies on some antimonate exchangers

The possibility of simultaneous extraction of palladium and technetium from nitrate solutions was investigated using tri-n-octylamine (TOA) solutions in carbon tetrachloride as a heavy, non-flammable diluent. Conditions of technetium extraction being essentially known, the main attention was focussed on the extraction of palladium which was studied in dependence on the concentration of nitric acid, salts (nitrates, chlorides, nitrites), urea and palladium. A strong decrease of Pd extraction with 10% TOA in CCl₄ has been found above a palladium concentration of 10⁻⁴M but in the presence of chlorides and nitrites a satisfactory high distribution can be preserved. Both Tc and Pd extracted with TOA/CCl₄ can be stripped into dilute ammoniacal solutions. An extraction procedure for the simultaneous isolation of Pd (80% yield) and Tc (99%) from fission product waste solutions (0.20 g Tc and 0.17 g Pd/dm³ 0.5–1.0M HNO₃) is proposed.     

The separation of some Bi- and tervalent cations on zirconium phosphate columns

Summary On small columns filled with the inorganic cation-exchanger zirconium phosphate, Zn²⁺-Cd²⁺ were quantitatively and Ni²⁺-Co²⁺ partly separated. The exchanger was in the NH₄+ form, and 0.5–4N NH₄Cl served as eluent. With the exchanger in the H+ form, U0₂ ²⁺ was separated from bivalent cations and ferric iron by stepwise elution with 0.1, 0.5 and 4N HCl solutions.

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Zusammenfassung An kleinen Säulen des anorganischen Kationenaustauschers Zirkoniumphosphat wurden Zn²⁺ und Cd²⁺ quantitativ, Ni²⁺ und Co²⁺ teilweise getrennt. Der Austauscher lag in der NH₄+-Form vor, 0,5-bis 4-n Ammoniumchlorid diente als Eluent. Mit der H+-Form des Austauschers wurde UO₂ ²⁺ von zweiwertigen Kationen und von Fe³⁺ durch schrittweise Elution mit 0,1-, 0,5- und 4-n Salzsäure getrennt.

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Résumé On a séparé Zn²⁺-Cd²⁺ quantitativement et Ni²⁺-Co²⁺ partiellement sur de petites colonnes remplies de phosphate de zirconium comme échangeur minéral cationique. L'échangeur se trouvait sous forme NH₄+ et l'on a pris NH₄Cl 0,5-4N comme éluant. Avec l'échangeur sous forme H⁺, on a séparé UO₂ ²⁺ des cations bivalents et de l'ion ferrique par élution graduelle avec des solutions chlorhydriques 0,1, 0,5 et 4N.

     

Ion-exchange selectivity and chromatographic separation of trivalent metals on titanium antimonate

Summary The ion exchange selectivity of trivalent metal ions has been determined on titanium antimonate cation exchanger prepared by coprecipitation of antimony to titanium at different mole ratios. The selectivity sequence Al³⁺<Cr³⁺<Ga³⁺<In³⁺<Fe³⁺ was found for trivalent metal ions at an initial concentration of 10^–4 mol dm^–3 in nitric acid media. A high separation factor ^Ga/Al = Kd^Ga/Kd^Al, 4.8×10³, was observed for the Ga³⁺–Al³⁺ pair on titanium antimonate with an antimony to titanium ratio of 0.34. The effective separation of Ga³⁺ and In³⁺ from Al³⁺ was achieved using a 3 cm×0.5 cm i.d. column containing titanium antimonate with an antimony to titanium ratio of 0.34.     

Chromatography of alkaloids on titanium arsenate papers and quantitative separation of some alkaloids from nicotine on titanium arsenate columns

Columns and papers of titanium arsenate have been utilized for chromatographic studies of several alkaloids in aqueous and mixed solvent systems. The results have been compared with those obtained with plain papers. A number of separations have been achieved on papers impregnated with titanium arsenate. Distribution coefficients of these alkaloids have been determined. A number of alkaloids have been separated quantitatively from nicotine on titanium arsenate columns.     

Scheme for the microchemical separation of some toxicologically important alkaloids

Summary A scheme for the successful separation and identification of milligram quantities of twenty of the most important narcotic alkaloids has been presented. The alkaloids studied are those which are most commonly employed in general pharmacology and hence are most frequently met with. The scheme has been found useful when the total quantity of the alkaloids in 1 milliliter of aqueous solution ranges from 0,5 to 3 milligrams and not more than three of the bases are present at a time. If only one alkaloid is present, still less than one half milligram can be isolated and definitely identified. In addition, it has been found that in the case of certain alkaloids, e. g. morphine, it is possible to separate less than 0,5 milligram from a mixture of the bases studied.

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Zusammenfassung Es wird ein Verfahren für die Trennung und den anschließenden Nachweis von Milligrammengen von zwanzig der wichtigsten narkotischen Alkaloide beschrieben. Die berücksichtigten Alkaloide gehören zu denen, die in der Pharmakologie allgemein verwendet werden und denen man daher auch häufig begegnet. Der Trennungsgang hat sich bewährt, wenn die Gesamtmenge der in 1 Kubikzentimeter wäßriger Lösung enthaltenen Alkaloide zwischen 0,5 und 3 mg beträgt und im jeweiligen Falle nicht mehr als drei der berücksichtigten Basen gleichzeitig zugegen sind. Wenn nur ein einziges Alkaloid anwesend ist, so können weitaus geringere Mengen davon isoliert und einwandfrei nachgewiesen werden. Außerdem genügen von gewissen Alkaloiden, wie z. B. Morphin, weit kleinere Mengen als 0,5 mg, um die Abtrennung aus Alkaloidgemischen und den Nachweis zu gestatten.

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Résumé (L) Les auteurs proposent une méthode de séparation et d'identification de vingt des plus importants des alcaloides narcotiques, sur des quantités de l'ordre du milligramme. Les alcaloides envisagés sont les plus employés en pharmacologie et par conséquent aussi ceux que l'on rencontre le plus fréquemment.La méthode de separation s'est révélée efficace quand la quantité totale d'alcaloide contenue dans un centimètre cube de solution aqueuse est comprise entre 0,5 et 3 mg, alors que simultanément n'existent en solution tout au plus que trois des bases envisagées. Dans le cas où un seul des alcaloides existe en solution, des quantités beaucoup plus petites de celui-ci peuvent encore être mises en évidence. En outre, pour certains alcaloides, comme la morphine, des quantités très inférieures à 0,5 mg permettent encore son extraction du mélange d'alcaloides et sa caractérisation ultérieure.

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The work herein reported represents a portion of the work presented by Mr.Wood as his dissertation in partial fulfillment of the requirements for the degree of Doctor of Philosophy at the Polytechnic Institute of Brooklyn.     

Sorption and separation of some elements of nuclear importance using Chelex-100

Chelex-100, in the anionic form has been studied for its ability to perform selective separation and concentration of some metal ions of nuclear importance from mineral acid solutions. The sorption behavior of Zr(IV)–Nb(V), Mo(VI), Tc(VII), Te(IV) and U(VI) from solutions of hydrochloric and sulphuric acids on Chelex-100 has been studied under static and dynamic conditions. Mo(VI) and Tc(VII) have been concentrated on the resin from hydrochloric or sulphuric acid solutions at low acidities probably, as the anions MoO ₄ ^2– and TcO ₄ ^– , respectively. Te(IV) has been isolated from hydrochloric acid solutions of normalities 6 in the form of the anionic chloro complex TeCl ₆ ^2– . Optimum conditions for elution and separation of Mo(VI), Tc(VII), Te(IV) and U(VI) were recommended.     

Adsorption of some hazardous radionuclides on cerium (IV) antimonate

Cerium(IV) antimonate was prepared by dropwise addition of 0.6M antimony pentachloride and 0.6M cerium ammonium nitrate solutions by a molar ratio of Ce/Sb 0.75. Exchange isotherms for H⁺/Co²⁺, H⁺/Cs⁺, H⁺/Zn²⁺, H⁺/Sr²⁺ and H⁺/Eu³⁺ were determined at 25, 40 and 60°C. Besides, it was proved that europium is physically adsorped, while zinc, strontium, cobalt and cesium are chemically adsorbed. Moreover, the heat of adsorption of zinc, strontium, cobalt and cesium on cerium (IV) antimonate was calculated and indicated that cerium(IV) antimonate is of endothermic behavior towards these ions. Also the distribution coefficients of these ions were determined and it was found that the selectivity is in the order: Eu³⁺>Sr²⁺>Cs⁺>Na⁺.