Atomic-absorption spectrometric determination of cobalt,nickel, and copper in geological materials with matrix masking and chelation-extraction

An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO₃ and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5–1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature.     

ESR studies of the state of Ti3+ and Ti2+ in Ti?Mg catalysts for olefin polymerization

ESR studies have revealed that in Ti–Mg catalysts after interaction with organoaluminium compounds, the Ti³⁺ ions formed are present mainly as TiCl₃ associates. Isolated Ti³⁺ ions of various types are also detected. Part of titanium ions is in the divalent state and provides an ESR signal after oxidation by water to the trivalent state in the form of Ti³⁺ ordered by cooperative Jahn-Teller interaction.

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, - , Ti³⁺ TiCl₃. Ti³⁺ . Ti³⁺ - -.

     

Elemental analysis of fertilizer by fast neutron activation

A simple and accurate technique has been developed to analyse the commercial fertilizers for phosphorous, potassium, chlorine, magnesium and silicon. The method is based on the fast neutron activation.     

The oxidation state of tungsten in NaxWO3 bronzes as determined by X-ray photoelectron spectroscopy

The XPS spectrum of the 4f levels of W in Na_xWO₃ bronzes is explained by assuming the presence of three oxidation states (W⁶⁺, W⁵⁺ and W⁴⁺). Tetravalent tungsten is formed by dismutation of W⁵⁺. The partial reduction of W⁶⁺ and W⁵⁺. during the recording of XPS spectra is briefly considered.     

Effect of actin concentration on the structure of actin-containing liposomes

Liposomes encapsulating monomeric actin (G-actin) were produced via extrusion through 400 and 600 nm pore diameter polycarbonate membranes in low ionic strength buffer (G-buffer). After actin-containing liposomes were subjected to high ionic strength polymerization buffer (F-buffer), morphological changes in the structure of actin-containing liposomes were studied using asymmetric flow field-flow fractionation (AFFF) coupled with multiangle static light scattering (MASLS). The general shape of these liposomes was initially determined by fitting three form factors, which describe the angular distribution of scattered light from a spherical thin shell, thin disk, and thin rod, to the experimentally measured light scattering spectra to regress the dimensions of the liposomes corresponding to the proposed geometry. Light scattering spectra that yielded a best fit to the thin disk model were analyzed further and fit to the ellipsoidal of revolution form factor to regress both the major and minor axis dimensions. The results of this analysis showed that actin-containing liposomes extruded through 400 and 600 nm pore diameter membranes in F-buffer, at a low actin concentration (0.1 mg/mL), assumed a spherical shape, which is also the case for plain liposomes (no actin present) in G-buffer and F-buffer. When the actin concentration was increased to 1 mg/mL, the polymerizing actin filaments stretched the initially spherical liposome into a disklike shape. However, when the actin concentration was further increased to 5 mg/mL, the liposomes reverted back to a spherical shape.     

NMR experiments on acetals—XXXVII: NMR spectral study of cis-, and trans-6-methyl-4-r-1,3-oxaselenans

The NMR spectral parameters are reported for cis-, and trans-6-Me-4-alkyl-1,3-oxaselenans with the aid of the INDOR- technique. Low temperature studies show the conformational equilibrium in the trans series to be pronouncedly one-sided and a value for the inversion barrier has been obtained.     

Ladder polymers from tetraaminodiquinoxalpyrene

A new fused aromatic heterocyclic tetraamine 2,3,11,12-tetraaminodiquinoxal [2,3-e,2′,3′-1] pyrene has been prepared and polymerized with 1,4,5,8-naphthalenetetracarboxylic acid and pyromellitic dianhydride. The resulting ladder polymers with inherent viscosities ranging from 0.5 to 1.0 dl/g in methanesulfonic acid exhibited thermal stabilities near 600°C in nitrogen and near 450°C in air.     

Chemistry of acetals

Summary Optimum conditions were developed for the preparation of 3-ethoxyacrolein, 3,3-diethoxypropionaldehyde, and 3,3-diethoxy~2-methylpropionaldehyde by the hydrolysis of the diacetals of malonaldehyde and methylmalonal dehyde in presence of p-toluenesulfonic acid and phosphoric acid.     

Über die dilatometrisch indizierten Titrationen

With the help of a dilatometer which permits the continuous determination of volume changes occuring in chemical reactions in aqueous solutions, the volume change during the precipitation of BaSO₄ was followed and applied to the determination of the endpoint of the precipitation. In the case of precipitations of 1 mM BaSO₄ the end-point determination can be reproduced with a standard deviation of less than 0.2%. A strict linearity between the amount of Na₂SO₄ applied and the position of the end-point does not exist. However, a correction factor could be established, so that the absolute determination of sulphate is possible (standard deviation 0.2%). The time required to carry out a single measurement is about 1.5 min. The acid concentration does not influence the composition. On the other hand, the composition was shown to be considerably dependent on Na⁺ and NH₄ ⁺ ions. The presence of the cation N(CH₃)₄ ⁺ does not alter the composition of the precipitate. It is obviously too big to substitute the Ba²⁺ ion.