Chromatographic separations of some elements on papers impregnated with a liquid cation exchanger

Summary The use of papers impregnated with the liquid cation exchanger dinonyl naphthalene sulphonic acid for separation of some metal ions is reported.

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Zusammenfassung Zur papierchromatograpischen Trennung einiger Metallionen wird ein Papier benutzt, das mit dem flüssigen Kationenaustauscher Dinonyl-naphthalin-sulfonsäure impägniert ist.

     

Extraction and spectrophotometric determination of iron as o-phenanthroline-azide mixed ligand complex

Summary The mixed ligand complex, [Fe(Phen)₂(N₃)₂] can be extracted into nitrobenzene giving a molar absorptivity of 16750 at 510 nm. This is the basis of a photometric method for iron which may be either in the trivalent or bivalent state. The new method is free from interference from a number of substances and is more sensitive than the ferroin method.

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Zusammenfassung Der Eisen-Phenanthrolin-Azid-Mischkomplex [Fe(Phen)₂(N₃)₂] ist mit Nitrobenzol extrahierbar und gibt bei 510 nm eine molare Absorption von 16750. Darauf läßt sich eine photometrische Bestimmungsmethode für zweioder dreiwertiges Eisen begründen. Diese wird von vielen Stoffen nicht gestört und ist empfindlicher als die Ferroinmethode.

     

High surface area silicon carbide from rice husk: A support material for catalysts

Ultrafine -SiC with high surface area (150 m² g^–1) has been synthesized by inflight processing of charred rice husk in a r.f. plasma reactor operating at atmospheric pressure. The plasma-synthesized particles were doped with platinum (1%) and tested as a catalytic support material. The catalyst (1% Pt doped -SiC) showed 100% conversion of CO to CO₂ at a temperature as low as 175°C.     

Preparation and thermal decomposition study of pyridinedicarboxylate intercalated layered double hydroxides

Supramolecular 2,3- and 2,5-pyridinedicarboxylate (PDC) intercalated ZnAl-layered double hydroxides (2,3- and 2,5-PDC–ZnAl–LDHs) have been prepared by ion exchange method. The structure and composition of the intercalated materials have been studied by X-ray diffraction (XRD) and inductively coupled plasma emission spectroscopy (ICP). The study indicates that the 2,3-PDC and 2,5-PDC anions are accommodated as interdigitated bilayer and monolayer arrangement respectively between the sheets of LDHs. Furthermore, their thermal decomposition processes were studied by the use of in situ high temperature X-ray diffraction (HT-XRD), and the combined technique of thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS) under N2 atmosphere. Based on the comparison study on the temperatures of both decarboxylation and complete decomposition of interlayer PDC, it can be concluded that 2,5-PDC–ZnAl–LDHs has higher thermal stability than that of 2,3-PDC–ZnAl–LDHs.     

Synthesis of some new metal-containing polyurethanes

Some new metal-containing polyurethanes were synthesized from manganese and lead salts of mono(hydroxyethyl)phthalate by condensing them with hexamethylene diisocyanate and toluene diisocyanate in dimethylformamide as solvent. The polymers were characterized by viscometry, infrared spectroscopy and thermal analysis. The decomposition temperatures of these polymers were found to be significantly lower than those of metal-free polymers of similar structure. However, the rates of decomposition of metal-containing polyurethanes were lower than those of polyurethanes having no metal. Inherent viscosities in DMSO at 30° of these polyurethanes were low, ranging from 0.043 to 0.067.     

A new oxidimetric reagent: potassium dichromate in a strong phosphoric acid medium—I Titrimetr1c determination of manganese

A new method has been developed for the direct titrimetric determination of manganese^II, depending on its oxidation to manganese^III with potassium dichromate at room temperature in a strong phosphoric acid medium using a potentiometric or photometric endpoint. Oxygen of the air does not interfere. The potentiometric method gives results to an accuracy within ± 0.3% for 20–150 mg of manganese/50 ml of titration solution; with the photometric method 5–17 mg of manganese/40 ml of titration solution can be determined with an error of 0.3–1.0% depending on the amount present. Potassium dichromate in 12.0M phosphoric acid has a formal redox potential of about 1.5 V and this reagent appears to have great possibilities in titrimetric analysis.     

L3/L2 white-line intensity ratios in the electron energy-loss spectra of 3d transition-metal oxides

The L₃/L₂ white-line intensity ratio in transition-metal oxides deviates widely from the statistical value of 2 : 1 but shows interesting systematics. In a series of oxides of a given metal, the ratio reaches a maximum for the d⁵ configuration (e.g. MnO) and a minimum for the d⁰ configuration (e.g. KMnO₄). In a series of monoxides, sesquioxides and dioxides of different metals, the ratio is again a maximum at the d⁵ configuration and decreases as the configuration changes towards d⁰ or d¹⁰. Our results, obtained by electron energy-loss spectroscopy, carried out in an electron microscope, are interpreted on an atomic mechanism involving spin-spin coupling. According to this model, the L₂ transition probability decreases in the progression d⁰ to d⁵ whereas the L₃ transition probability decreases beyond d⁵.     

Colorimetric determination of iron (III) with 1,10-phenanthroline

Summary A new procedure has been developed for the colorimetric determination of iron(III). It consists in the reduction of iron (III) in dilute sulphuric acid medium (0.1 to 1.0 N) with an excess of hypophosphite (1100) at room temperature using one or two drops of 0.1% PdCl₂ solution as catalyst, and then complexing the reduced iron with 1.10-phenanthroline.Iron (III) can also be reduced with phosphite using the PdCl₂ catalyst and boiling for 5 to 10 min on a hot plate. The molar concentration of phosphite is preferably kept 500 times that of ferric ion.

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Zusammenfassung Es wurde ein neues Verfahren zur colorimetrischen Bestimmung von Eisen(III) ausgearbeitet. Dabei wird das Eisen in verd. Schwefelsäure (0,1–1,0 n) mit einem Überschuß von Hypophosphit (1100) bei Zimmertemperatur unter Verwendung von ein oder zwei Tropfen 0,1%iger PdCl₂-Lösung als Katalysator reduziert und anschließend das zweiwertige Eisen mit 1,10-Phenanthrolin umgesetzt.Eisen(III) kann auch mit Phosphit reduziert werden, wenn man ebenfalls PdCl₂ als Katalysator verwendet und 5–10 min erhitzt. Die molare Konzentration des Phosphits soll dabei das 500fache von der des Eisens betragen.

     

Titrimetric determination of arsenic(III) with potassium dichromate, using redox indicators

Experimental conditions have been established for the accurate direct titrimetric determination of arsenic(III) with potassium dichromate, using ferroin and N-pnenylanthranilic acid as redox indicators. Interferences have been considered.     

Enzymatic kinetic resolution of racemic 4-tetrahydropyranols by Candida rugosa lipase

Enzymatic kinetic resolution of (±)-hydroxytetrahydropyrans has been achieved for the first time by means of lipase-mediated transesterification to afford optically active (2S,4R)-tetrahydropyranyl acetates and (2R,4S)-tetrahydropyranols in excellent yields with high enantioselectivity. Absolute configurations of the tetrahydropyranyl acetates were assigned as (S) by chemical correlation.