Chromatographic determination of solubility of low soluble substances the physico-chemical basis

The physico-chemical basis for a direct chromatographic determination of solubility of low soluble substances by means of adsorption and partition TLC is discussed. This method is a practical consequence of the chromatographic binary solutions model, a new semi-empirical approach based on phenomenological thermodynamics.

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Chromatographische Bestimmung der Löslichkeit von schwerlöslichen Substanzen. Die physikalisch-chemische Basis (Kurze Mitteilung)

Zusammenfassung Die physikalisch-chemische Basis einer direkten chromatographischen Bestimmung der Löslichkeit von schwerlöslichen Substanzen mit Hilfe der Adsorptions- und Verteilungsdünnschichtchromatographie wird diskutiert. Die Möglichkeit einer solchen Bestimmung ist die praktische Konsequenz des chromatographischen Modells der binären Lösungen, einer neuen semiempirischen, auf der phänomenologischen Thermodynamik begründeten Methode.

     

Thermogravimetric investigation ofwastes from electrical and electronic equipment (WEEE)

Two components of electronic wastes (sample A – a mixture of three types of printed circuit boards, sample B – a mixture of electronic junctions with metal wires) were investigated using thermogravimetric analysis (TG). Thermogravimetric and derivative thermogravimetric data (TG and DTG) give information on the thermal stability of A and B samples and allows finding the correct conditions for their degradation using pyrolysis in an experimental system, built on the laboratory scale for utilization of hazardous wastes. X-ray fluorescence measurements prove that brominated flame retardant is present in sample A, whilst chlorinated flame retardant is a probable component of sample B. Preliminary liquid chromatography of oil products obtained as a result of thermal waste degradation shows that the hydrocarbons released during pyrolysis could be used as a fuel.     

Behavior of peptides and computer-assisted optimization of peptides separations in a normal-phase thin-layer chromatography system with and without the addition of ionic liquid in the eluent

The addition of an ionic liquid into the mobile phase appeared to be useful in optimization of chromatographic separation of peptides. Different behavior of peptides in thin-layer chromatography (TLC) was observed after addition of 1-ethyl-3-methylimidazolium tetra fluoroborate to the eluent in comparison to the system without the ionic liquid. Nonlinear dependence of the retention coefficient, R(M), of peptides on the volume percentage of acetonitrile in the eluent was found in normal-phase TLC with and without immidazolium tetra fluoroborate in the mobile phase. In general, R(M) increased with increasing concentration of acetonitrile. In TLC systems without the ionic liquid, R(M) can be described well with a quadratic function. On the other hand, in a TLC system with an ionic liquid as the additive to the mobile phase, the retention behavior is better described with a third-degree polynomial function. The potential usefulness of ionic liquids for optimization of separation of peptides was demonstrated. Optimization of the separation conditions was supported by a commercially available computer program.     

Thin-Layer Chromatographic and Polarimetric Investigation of the Oscillatory In-Vitro Chiral Inversion of S-(+)-Ketoprofen

JPC – Journal of Planar Chromatography – Modern TLC - Our earlier thin-layer chromatographic and polarimetric investigations enabled discovery of the spontaneous in-vitro oscillatory...     

Measurement of the spin and magnetic moment of 31Mg: evidence for a strongly deformed intruder ground state

Unambiguous values of the spin and magnetic moment of 31Mg are obtained by combining the results of a hyperfine-structure measurement and a beta-NMR measurement, both performed with an optically polarized ion beam. With a measured nuclear g factor and spin I=1/2, the magnetic moment mu(31Mg)=-0.88355(15)mu(N) is deduced. A revised level scheme of 31Mg (Z=12, N=19) with ground state spin/parity I(pi)=1/2(+) is presented, revealing the coexistence of 1p-1h and 2p-2h intruder states below 500 keV. Advanced shell-model calculations and the Nilsson model suggest that the I(pi)=1/2(+) ground state is a strongly prolate deformed intruder state. This result plays a key role for the understanding of nuclear structure changes due to the disappearance of the N=20 shell gap in neutron-rich nuclei.     

Adsorption/partition model of liquid chromatography for chemically bonded stationary phases of the aliphatic cyano, reversed-phase C8 and reversed-phase C18 types

A novel approach was introduced to modeling solute retention in the liquid chromatography systems, employing silica-based aliphatic chemically bonded stationary phases of the cyano, reversed-phase C8 and reversed-phase C18 types, and the mixed binary eluents most frequently used in the reversed-phase and normal-phase chromatography modes (i.e. using the methanol-water and the 2-propanol-n-hexane liquid mixtures, respectively). This approach takes notice of the mixed (adsorption/partition) mechanism of solute retention, in which both, the adsorptive and the dispersive forces contribute to the overall energetics of this process. Performance of our new model was compared with that of the widely recognized and on a routine basis applied Schoenmakers approach, and it was found out that both models perform with a practically equal and outstanding accuracy.     

Investigation of the association of higher fatty alcohols on a chromatographic paper

Summary An attempt was made to apply a low-activity chromatographic layer (Whatman 2) and a non-polar mobile phase (decalin) in studying the self-association of higher fatty alcohols. The obtained results showed a satisfactory, semi-quantitative agreement with IR spectroscopic data and theoretical considerations and calculations. Usefulness of the complementary paper chromatographic investigations can be considered as complementary investigations when setudying the self-association of higher fatty alcohols.     

The effects of ultrasound on chromium gels in light of their catalytic activity and electron paramagnetic resonance

Investigations into the influence of ultrasound on the catalytical properties of chromium gels are presented. The changes of the EPR spectra and surface concentration of Cr on the sixth oxidation degree of certain preparations are described. These changes are then related to the increase in the velocity in the test reaction of H₂O₂ decomposition and the increased yield of cyclohexane dehydrogenation when the insonated preparations are used as catalysts.     

A simple thermodynamic model for rationalizing the formation of self-assembled multimetallic edifices: application to triple-stranded helicates

Reaction of the bis-tridentate ligand bis[1-ethyl-2-[6'-(N,N-diethylcarbamoyl)pyridin-2'-yl]benzimidazol-5-yl]methane (L2) with Ln(CF(3)SO(3))(3).xH(2)O in acetonitrile (Ln = La-Lu) demonstrates the successive formation of three stable complexes [Ln(L2)(3)](3+), [Ln(2)(L2)(3)](6+), and [Ln(2)(L2)(2)](6+). Crystal-field independent NMR methods establish that the crystal structure of [Tb(2)(L2)(3)](6+) is a satisfying model for the helical structure observed in solution. This allows the qualitative and quantitative beta23 (bi,Ln1,Ln2)characterization of the heterobimetallic helicates [(Ln(1))(Ln(2))(L2)(3)](6+). A simple free energy thermodynamic model based on (i) an absolute affinity for each nine-coordinate lanthanide occupying a terminal N(6)O(3) site and (ii) a single intermetallic interaction between two adjacent metal ions in the complexes (DeltaE) successfully models the experimental macroscopic constants and allows the rational molecular programming of the extended trimetallic homologues [Ln(3)(L5)(3)](9+).     

Investigation of Phase Transition inLa1–xPrxGaO3 and La1–xNdxGaO3 Crystals

The solid solution crystals, La_1–xNd_xGaO₃ and La_1–xPr_xGaO₃ have been studied by differential scanning calorimetry method; the crystals exhibit the first order phase transition, the temperature of the transition linearly increases with the concentration of Pr or Nd. The structure of the crystals has been determined by X-ray diffraction. The correlation between the phase transition temperature and crystalline structure at the temperature of the phase transition in both solid solution families is discussed. This revised version was published online in July 2006 with corrections to the Cover Date.