Extraction-spectrometric determination of antimony with triphenyltetrazolium chloride

Summary The optimum conditions for the antimony(V) extraction in strong hydrochloride acid medium as a ternary ion-associated complex with triphenyltetrazolium chloride have been investigated. The extraction constant has been determined with dichlorethene and chloroform (11) (K _ex =3.06×10⁴). A working procedure for the determination of antimony has been developed. Interferences are only caused by iron(III), gold(III), thallium(III) and gallium. The application of the method is demonstrated by the analysis of metallic lead, which has also been carried out with two other methods (AAS and spectrophotometry with crystal violet). The new method is superior in reliability and accuracy. The relative standard deviation of the mean is ± 7.4%.

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Extraktionsspektralphotometrische Bestimmung von Antimon mit Triphenyltetrazoliumchlorid

Zusammenfassung Die optimalen Bedingungen für die Extraktion von Antimon aus stark salzsaurer Lösung als Ionenanlagerungskomplex mit Triphenyltetrazoliumchlorid wurden bestimmt. Die Extraktionskonstante bei Extraktion mit einer Dichlorethan-Chloroform-Mischung (11) beträgt (K _ex =3,06·10⁴). Für die Antimonbestimmung wurde eine entsprechende Methode ausgearbeitet. Nur Fe(II), Au(III), Tl(III) und Ga(III) stören. Die Anwendung der Methode wurde an Hand der Analyse von metallischem Blei demonstriert, die zusätzlich auch nach zwei anderen Methoden (AAS und Spektralphotometrie mit Kristallviolett) durchgeführt wurde. Die neue Methode ist in bezug auf Zuverlässigkeit und Genauigkeit überlegen. Die relative Standardabweichung des Mittelwertes beträgt ± 7,4%.

The first of the authors dedicates this article to his teacher at the University of Saarbrücken, Prof. Dr. E. Blasius, an occasion of his 60th birthday     

Extraction-chromatographic separation of iron from cobalt, nickel, and copper using dibenzyl sulphoxide solution as the stationary phase

Summary The separation of Fe from Co, Ni, and Cu by LLC was carried out with silica gel coated with dibenzyl sulphoxide solution as stationary phase and dilute hydrochloric acid as mobile phase, saturated with the same dibenzyl sulphoxide solution. A liquid chromatograph of own construction was used, in which a corrosive mobile phase can be pumped through a glass column. By means of stepwise elution, first with 7 M HCl and then with water, it is possible to separate and to determine as little as 0.2 g of Fe in the presence of up to 655 g of Cu (saturated solution of CuCl₂) within 15 min with a rel. error of 3.5% and a rel. standard deviation of 4%. The same accuracy and precision were found for the determination of Cu (from peak height) and for Ni or Co (AAS in collected eluate fractions).Dedicated to Prof. Dr. R. Bock on the occasion of his 65th birthday     

Extraction-flame atomic absorption determination of microtraces of copper, zinc, nickel, cobalt, manganese and iron in some alkali salts

Summary The microtrace content of Cu, Zn, Ni, Co, Mn and Fe in NaClO₄, KCl, KOH and KAl(SO₄)₂ · 12 H₂O is determined by flame atomic absorption spectrometry after preceding preconcentration of the traces using the extraction system PMBP/MIBK. It is proved that the salt matrix does not affect the quantitative extraction of the traces. The method permits the determination of the traces in the concentration range of 10^–3–10^–6% with good precision (variation coefficient 2–8%) and accuracy.

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Extraktions-Flammenatomabsorptions-Bestimmung von Mikrospuren von Cu, Zn, Ni, Co, Mn und Fe in Alkali-Salzen

Zusammenfassung Der Mikrospurengehalt von Cu, Zn, Ni, Co, Mn und Fe in NaClO₄, KCl, KOH, und KAl(SO₄)₂ · 12H₂O wurde durch Flammenatomabsorption nach Extraktionsanreicherung mit einer 1-Phenyl-3-methyl-4-benzoylpyrazolon-5 (PMBP)-Lösung in MIBK bestimmt. Die Salz-Matrix weist keinen störenden Einflu\ auf die quantitative Extraktion der Elementspuren auf. Die Bestimmung der Spuren im Konzentrationsgebiet von 10^–3–10^–6% erfolgt mit guter PrÄzision (Variationskoeffizient 2–8%) und Richtigkeit.

     

A new method for separation and spectrophotometric determination of phosphate ion by the liquid-liquid extraction with benzophenone at an elevated temperature

Summary A new type of separation of phosphate ion, along with its spectrophotometric determination, was established by liquid-liquid extraction, where the yellow heteropoly acid formed by the reaction with ammonium molybdate in acid solution is quantitatively extracted into molten benzophenone at a temperature of about 60° C. When cooled down to room temperature, the benzophenone extract converts from the liquid state to the solid state. The resulting solidified extract is dissolved in methyl propionate, and the phosphate ion in the solvent is determined spectrophotometrically by the blue heteropoly acid method. Possible interference by Si, As and Ge is eliminated by the separation procedure.The authors wish to thank President Dr. Yawara Yoshitoshi and Prof. Yoshisaburo Ota of University School of Medicine, for their hospitality and encouragement.