Neutron activation analysis for determination of metal ions in biological fluids of patients after CoCrMo arthroplasty

Determination of metals and trace elements in patients with total knee or hip arthroplasty with CoCrMo alloy was performed. Blood, urine and cerebrospinal fluid (CSF) samples were analyzed and compared with samples from healthy people. Levels of Co, Cr as well as Na, Ca, Fe, Zn, Se, Rb, Sb and Br were determined by means of neutron activation analysis. The values of Cr and Co of the blood and urine measurements were elevated in patients with replacement, and according to the statistical analysis, significant differences of the elements Zn, Br, Co and Sb were found in the CSF (p?<?0.05).

     

The exterior magnetic field for the multilayer ellipsoidal model of the brain

The magnetic induction field in the exterior of an ellipsoidallyinhomogeneous, four-conducting-layer model of the human headis obtained analytically up to its quadrupole approximation.The interior ellipsoidal core represents the homogeneous brainwhile each one of the shells represents the cerebrospinal fluid,the skull and the scalp, all characterized by different conductivities.The inhomogeneities of these four domains, together with theanisotropy imposed by the use of the ellipsoidal geometry, providethe most realistic physical and geometrical model of the brainfor which an analytic solution of the biomagnetic forward problemis possible. It is shown that in contrast to the spherical model,where shells of different conductivity are magnetically invisible,the magnetic induction field in ellipsoidal geometry is stronglydependent on the conductivity supports. The fact that sphericalshells of different conductivity are invisible has enhancedthe common belief that the biomagnetic forward solution doesnot depend on the conductivity profiles. As we demonstrate inthe present work, this is not true. Hence, the proposed multilayeredellipsoidal model provides a qualitative improvement of therealistic interpretation of magnetoencephalography (MEG) measurements.We show that the presence of the shells of different conductivitycan be incorporated in the form of the dipole vector for thehomogeneous model. Numerical investigations show that the effectsof shell inhomogeneities are almost as sound as the level ofMEG measurements themselves. The degenerate cases, where eitherthe differences of the conductivities within the shells disappear,or the ellipsoidal geometry is reduced to the spherical one,are also considered.     

Thermal analysis of PMMA/gel silica glass composites

Thermal analysis of poly-methylmethacrylate (PMMA) impregnated porous gel silica glasses confirms that the PMMA chains form hydrogen bonds with the pore surface silanol groups. The adopted conditions for the insitu polymerisation result in about 4% of residual monomers trapped in the polymer, most of them in the amorphous structure. The polymer and monomer mixture takes up the whole of the free pore volume. Most of the residual monomer polymerises during the DSC scans above the glass transition temperature providing an excellent probe for the weak glass transition. Polymerisation in the gel silica glass medium affects the glass transition temperature, the length of polymer chains, and the degree of polymerisation.     

Determination of carbendazim,thiabendazole, and<Emphasis Type="Italic"> o-</Emphasis>phenylphenol residues in lemons by HPLC following sample clean-up by ion-pairing

An efficient analytical method is presented involving effective sample clean-up with solid-phase extraction and HPLC-UV analysis for the simultaneous determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons. Sample preparation involves extraction with acetonitrile acidified with trifluoroacetic acid and an ethyl acetate/petroleum ether mixture. Purification of the crude extract was carried out with liquid–liquid partitioning after addition of an aqueous ammonia solution. Final clean-up was performed on polymeric reversed-phase cartridges pretreated with sodium dodecyl sulfate. Chromatographic analysis was performed on a reversed-phase HPLC column isocratically eluted with an acetonitrile/water/ammonia mixture and UV detection at 254 nm. The chromatographic method is repeatable, reproducible, and sensitive. Fungicide recoveries from lemon samples fortified at levels of 5 and 1 mg kg^–1 were 81–85% for carbendazim, 96–98% for thiabendazole, and 81–106% for o-phenylphenol with coefficients of variation of 2.5–7.4%. Detection limits for carbendazim, thiabendazole, and o-phenylphenol in lemons were 0.21, 0.27, and 0.51 mg kg^–1, respectively.     

Synthesis of a halo-methylphenylene periphery-functionalized triazine-based dendritic molecule with a 3,3′-dimethyl-biphenyl linker using tris(halo-methylphenylene)triazines as building blocks

A tris(bromo-methylphenylene)triazine and its corresponding phosphine oxide derivative have been synthesized; the latter compound was found to be a potent ligand for the hydroformylation reaction. Suzuki coupling of the mono-pinacolboronate derivative of the former compound with a tris(iodo-methylphenylene)triazine was possible at two of the three iodine atoms, yielding a bromo- and iodo-methylphenylene periphery-functionalized triazine-based dendritic molecule with a 3,3′-dimethyl-biphenyl linker.     

Development and validation of a rapid HPLC method for the determination of five banned fat-soluble colorants in spices using a narrow-bore monolithic column

This work reports a fast and simple liquid chromatographic method for the simultaneous determination of five banned fat-soluble synthetic colorants, namely Sudan I-IV and Para-Red, in spice samples. The analytes were successfully separated isocratically in less than 5 min on the new narrow bore monolithic column, FastGradient^® Chromolith (50 mm × 2.0 mm i.d.) using a mobile phase of 0.1% (v/v) HCOOH/acetonitrile (35/65%, v/v) at a flow rate of 1.5 mL min⁻¹. All colorants were detected at 506 nm. The main parameters (mobile phase composition, flow rate, injection volume) affecting the separation were studied. The proposed method was thoroughly validated in terms of linearity, LODs, precision and accuracy. The method was applied to the determination of the studied azo-dyes in various spices (paprika, chilli and mixed spice powders) after ultrasound-assisted extraction. Satisfactory recoveries, ranging from 92% to 109% were obtained.     

Review of analytical methods for the determination of chlorine dioxide

The present study reviews more than twenty years (1985-present) of published research on the development and application of analytical procedures for the determination of chlorine dioxide, a widely used disinfectant and bleaching agent. The review covers a variety of techniques including batch and automated spectrophotometry and fluorimetry, electroanalysis and chromatography. The analytical figures of merit to the methods are presented, while critical discussion regarding their advantages and disadvantages is addressed.      

Investigation of HEU-type zeolite crystals after interaction with Sr2+ cations in aqueous solution using nuclear and surface analytical techniques

Pure HEU-type zeolite (heulandite) crystals were allowed to interact with Sr²⁺ cations in aqueous solution. The powdered solid experimental products obtained from batch-type sorption experiments, using solutions of Sr²⁺-concentrations between 10 and 1000 mg/l, were investigated using INAA, RI-XRF and SEM-EDS. The Sr uptake by the mineral which can adequately be described with a Freundlich-type isotherm, varies from 3.14 to 6.22 mg/g. The distribution coefficients increase progressively by decreasing the solutions concentration reaching a value of 1800 ml/g. The investigated zeolite interacts with Sr²⁺ cations through ion exchange reactions and initial exchangeable Ca²⁺ cations are replaced into the structural micropores. However, in the best case, only ca. 43% of the theoretical CEC can be covered because of the limited availability of the extra framework Ca²⁺ cations that can be removed from the lattice under ambient treatment conditions. The XPS investigation of Sr-loaded single crystals indicated that adsorption of Sr²⁺ cations on the outer surface also occurs while surface precipitation phenomena must be excluded. Similar surface analyses by means of¹²C-RBS showed that the Sr depth-distribution at near-surface layers is quite homogenous in contrast to a previous relevant study revealing an intense surface Sr-accumulation on a natural Ca-zeolite of different structural characteristics (scolecite).