Hydrothermal Synthesis and Structural Characterization of a Novel Organic—Inorganic Hybrid Compound {[Cu（2,2′—bpy）2]2—Mo8O26}

A novel organic-inorganic hybrid compound {[Cu(2,2′-bpy)2]2Mo8O26} has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group, Pna21,with a=2.4164(5),b=1.8281(4),c=1.1877(2)nm,V=5.247(2)nm^3,Z=4,and final R1=0.0331,wR2=0.0727.The structure consists of discrete {[Cu(2,2′-bpy)2]2Mo8O26} clusters,constructed from a β-octamolybdate subunit[Mo8O26]^4- covalently bonded to two [Cu(2,2′-bpy)2]^2 coordination complex cations via bridging oxo groups.In addition,the spectroscopic properties and thernal behavior of this compound have been investigated by spectroscopic techniques (UV-vis,IR,Raman and EPR spectra) and TG analysis.     

Extraction separation of strontium and yttrium radionuclides by hydrogen heptachlorodicarbollylcobaltate in the presence of benzo-15-crown-5

Extraction of strontium and yttrium by the nitrobenzene solution of H⁺-form of heptachloro-bis-1,2-dicarbollylcobaltate (H⁺B^–) in the presence of benzo-15-crown-5 (B15C5, L) has been investigated. The presence of B15C5 leads to a great synergistic effect for the extraction of strontium and an antagonistic effect for the extraction of yttrium. The extraction constants of Sr²⁺ complexes of B15C5 were determined. The separation factor a(Sr/Y) in the system with B15C5 presents the same order of magnitude as that for 15C5.     

Concentration effects in gel permeation chromatography : IV. Contribution of viscosity phenomena and macromolecular expansion

The changes in elution volumes with the changes in the concentration of an injected polymer solution are caused by several contributing effects. Under model conditions, it is possible to assume only the effect of a viscosity gradient in a zone moving along the column and the effect of the concentration dependence of the hydrodynamic volume of a macromolecular coil. The non-Gaussian shape of the zone and the dependence of the width of the elution curve on concentration are factors that complicate the theoretical treatment of concentration effects. The described physico-chemical model allows to evaluate the ratio of mentioned two contributions in the concentration dependence of elution volumes. According to this model, the contribution of the concentration dependence of the hydrodynamic volume does not exceed about 20% of the total change in elution volume with the varying concentration under real experimental conditions. The efficiency of the columns used and the total injected volume of the polymer solution affect this ratio only negligibly. It is obvious from a comparison with earlier results that these conclusions are not fundamentally changed even by the revised model of the concentration dependence of the swelling factor.     

Application of an ion-selective field effect transistor with a photocured polymer membrane in nephrology for determination of potassium ions in dialysis solutions and in blood plasma

Application of a potassium ion sensor based on an ion sensitive field effect transistor (ISFET) for ion control of a dialysis solution in an artificial kidney and in blood plasma of patients treated by hemodialysis is presented. Sensors and their long-term stability were characterised in constant contact with test solutions. Test results are compared to those obtained with conventional ion-selective electrodes and commercial blood ion analyser. Tested ISFET sensors showed high reliability in potassium ion measurements in the physiologically significant concentration range which, along with low cost of their production, makes them promising for cited application.     

Anomalies in thorium adsorption on manganese dioxide

In this paper the authors present a study of the adsorption of thorium on manganese dioxide by batch equilibration and cartridge experiments. Some anomalies in the use of MnO₂ to concentrate thorium have been found. So the use of this technique is limited for the determination of thorium in natural waters.     

Detection of soil pollution by hydrocarbons using headspace-mass spectrometry and identification of compounds by headspace-fast gas chromatography-mass spectrometry

The direct coupling of a headspace sampler with a mass spectrometer is proposed as a screening tool for the rapid detection of soil pollution by hydrocarbons from petroleum and derivatives. The samples are subjected to the headspace generation process, with no prior treatment, and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of the sample analysed. Suitable treatment of the signal by chemometric techniques allows unequivocal characterisation of the different types of sample. The use of fast gas chromatography with a mass spectrometer detector coupled to the headspace sampler allows identification of the major hydrocarbons present in the mineral and organic polluted samples, interpretation of the results obtained, and demonstrates the analytical potential of headspace-mass spectrometry coupling.     

Air/polymer distribution coefficients for polycyclic aromatic hydrocarbons by solid-phase microextraction sampling

Two methods to estimate distribution coefficients (K) between air and poly(dimethylsiloxane) (PDMS) coating of solid-phase microextraction (SPME) fibers for eight low molecular polycyclic aromatic hydrocarbons (PAHs) there are presented. The PDMS phases were used for determination of the coefficients according to equilibrium theory with help of a developed static calibration system (SCS). Another way to estimate the coefficients is based on the use of a linear relationship between the logarithm of the coefficients (log K) and linear temperature-programmed retention indexes (LTPRI) of the compounds without necessity to calibrate. The log K values for both of methods ranged from 5.2 (naphthalene) to 8.9 (pyrene) at 22 degrees C. Relative standard deviation (R.S.D.) of log K for each compound determined by static calibration was no more than 5.3%. R.S.D. of retention times for LTPRI indices did not exceed 0.28% for repeated injection. All experiments were implemented on a GC-MS system.     

Patterns in the precision of quantitative data from multicomponent gas chromatographic or gas chromatographic-mass spectrometric analysis

The dispersion of the quantitative results in the analysis of volatile compounds from multicomponent mixtures by different fractionation techniques (solid-phase microextraction and direct thermal desorption) followed by GC or GC-MS presents nonrandom patterns related to the existence of different factors in the fractionation process or in the chromatographic separation which affect, to a different extent, the recovery of the sample components. Statistical techniques have been used to show the relative importance of these factors. The improvement in data precision achieved by using volatile compound concentration ratios is discussed.     

Preparation and practical application of spinel pigment Co0.46Zn0.55(Ti0.064Cr0.91)2O4

Synthesis of the green spinel pigment Co_0.46Zn_0.55(Ti_0.064Cr_0.91)₂O₄ by a novel two-step method of preparation have been investigated. Inorganic pigments are almost always prepared by a solid state reaction. It is classical ceramic method which used oxides, hydroxides or carbonates as precursors. The reaction is performed at temperature higher than 1300°C and an agent of mineralization is usually present. The presented novel method of preparation decreases the calcining temperature necessary for reaching of bright and clear hue of the pigments prepared. Main attention was focused on the influence of two types of titanium raw materials on the temperature region of the spinel structure formation and on the colour properties of the pigments. The mixture of precursors with TiO₂ gives a one-phase system when calcining at 1100°C but the colour properties are more interesting at 1150°C. Thermal stability of this pigment is limited by temperature 1300°C. This temperature is connected with partial oxidation of Cr(III) to Cr(VI). Thermal analysis provided the first information about the temperature region of the pigment formation and determined the thermal stability of pigment.     

Catalytic Conversion of 2-Naphthol to 2-Hydroxy-1,4-naphthoquinone Under Mild Conditions

Introduction 2-Hydroxy-1,4-naphthoquinone (HNQ), existing in natural plants,1,2 is popularly separated and purified as dye or pigment. Recent research results show that, with the function to prevent the formation of protein coenzyme of HIV-I, HNQ can inhibit HIV virus from copying and propagating,3,4 HNQs derivatives and di-chloroallyl lawsone are also the inhibitor for RNA syn-thesis of cancer.5 It is well known that there is a rela-tionship between the side chain attached to HNQ an…