Investigation of the Declared Value of Selenium in Food Supplements by HG-AFS

The method of hydride generation atomic fluorescence spectrometry (HG-AFS) was optimised for determination of selenium in food supplements. Due to the high and varied content of Cu, Mg and Zn in the samples, the standard addition method was found to be the most appropriate. The reliability of the method was checked by the independent method of radiochemical neutron activation analysis, and good agreement was found between the two methods. HG-AFS is simple and rapid for Se determination in food supplements based on minerals. Agreement between the selenium values found and declared was worse than 10% in 9 out of 13 supplements. Furthermore, 2 of the 14 supplements did not comply with the recommendations stated in the 27^th edition of the U.S. Pharmacopoeia, which states that minerals and vitamins in food supplements should be in the range of 90 and 200% of the declared value.     

Study of isotope exchange reactions by double labelling

This paper presents the method of double labelling in the study of the kinetics of homogeneous isotope exchange reactions. This method was tested by the determination of the Sn(II)−Sn(IV) exchange rate in hydrochloric acid medium. The system was labelled by the tracer^119mSn [initially in the Sn(IV) state]; when the isotope equilibrium was established, Sn(IV) was again labelled by tracer¹¹³Sn. The separation of Sn(II) and Sn(IV) in the given time of exchange was performed by the extraction of Sn(IV)-hydroxyquinolate into chloroform. The specific activities of the separated components were determined from the ratio of¹¹³Sn and^119mSn activities. The exchange rate was calculated from the time dependence of specific activities. The advantage and possibilities of the method of double labelling in the study of isotope exchange are discussed.     

A viscometric study of poly(methyl methacrylate) in 2-alkoxyethanols

θ-Conditions, the temperature coefficient of unperturbed dimensions of the macromolecules and the thermodynamic interaction parameters ψ and κ were determined for solutions of poly(methyl methacrylate) in 2-alkoxyethanols (methoxy, ethoxy and butoxy). The results for this series of solvents fit the data reported for other solvents and dln $\text{r}{}_0{}^2\text{/}\text{d}\text{T = 2.6 × 10}{}^{\mathrm{?3}}\text{K}{}^{\mathrm{?1}}$. The dependence of parameters ψ and κ exhibited deviations from the theoretical dependence, mainly near the limiting value ψ = 0.5.     

Cadmium and zinc determination by neutron activation analysis and biochemical tests in tissues of workers professionally exposed to cadmium

Cadmium and zinc levels in urine, serum, hair obtained from workers professionally exposed to cadmium oxide dust and from a control, nonoccupationally exposed group were determined by neutron activation analysis. The study was completed by biochemical monitoring tests such as the ₂ (₂-MG) determination in urine and serum and the -aminolevulinic acid dehydratase (ALAD) determination in blood. Significantly increased levels of cadmium in urine, serum, and hair, ₂-MG in urine and serum, ALAD in blood and decreased levels of zinc in serum were found in the exposed group compared to the control group. The most distinct differences of the parameters studied were observed for cadmium in hair. Correlations among the parameters were preliminary evaluated, too. For quality assurance purposes, the cadmium and zinc concentrations were determined in biological (standard) reference materials NBS SRM-1577 Bovine Liver, Bowen's Kale, IAEA A-11 Milk Powder, and IAEA H-8 Horse Kidney.     

On distribution of molecular weight in anionic polymerizates of caprolactam

Measurement has been made of the dependence of the molecular weight distribution on the ratio of the catalytic system components and on the polymerization time for polycaprolactam obtained by anionic polymerization. A bimodal character of the curves was observed for products made using molar ratios of activator (N-benzoylcaprolactam) to initiator (sodium dihydro-bis(methoxyethoxy)aluminate) of 1:1 and 1:3, when the polymerization times were less than 1 hr. This course is explained by the influence of fast side-reactions, mainly condensations. For a ratio of 3:1 of the components of the catalytic system, smooth integral distribution curves are obtained, accounting for a very fast decrease in the strong base concentration in the initial stages of the polymerization.     

Flow injection analysis : Part VI. The determination of phosphate and chloride in blood serum by dialysis and sample dilution

The rapid determination of chloride and inorganic phosphate in blood serum based on continuous flow spectrophotometry was adapted to Flow Injection Analysis by applying dialysis as well as differential dilution of the injected samples. In addition to the manual injection procedure, an automated microsampling unit was developed and used. By continuous dialysis, chloride could be determined reproducibly at a sampling rate of 125 samples per hour at sample volumes of 60 μl or less. A similar sampling rate and high precision were obtained for the determination of inorganic phosphate by using differential dilution.     

Flow injection analysis. principles,applications and trends

The basic principles of Flow Injection Analysis are outlined. The parameters governing the dispersion of the injected sample zone in the system are discussed, and it is demonstrated how these parameters can be manipulated in order to suit the requirements of an individual analytical procedure. A number of examples illustrating the practical application of f.i.a. are described, comprising the use of automated, stopped-flow, merging-zones, extraction techniques as well as f.i.a. scanning and methods based on intermittent pumping. Updated lists on f.i.a. procedures published and species that can be determined by f.i.a. are included.     

Spectral and electrochemical study of coordination molecules Cu4OX6L4: 3-Methylpyridine and 4-Methylpyridine Cu4OBrnCl(6−n)L4 complexes

The tetranuclear Cu₄OBr_nCl_(6-n)L₄ complexes, where L = 3-methylpyridine (3-Mepy), 4-methylpyridine (4-Mepy) and n=0–6 with trigonal bipyramidal coordination of copper(II) were prepared and their infrared and electronic absorption spectra as well as cyclic voltammograms in nitromethane solutions were measured. The polyhedra in Cu₄OBr_nCl_(6−n) (3-Mepy)₄ molecules are less distorted comparing with those of 4-Mepy analogues as indicated by infrared Cu₄O absorptions, far infrared Cu—Br, Cu—Cl, and Cu—N absorptions, d—d bands in electronic spectra and potentials, measured by cyclic voltammetry. The 3-Mepy complexes exhibit strong single infrared Cu₄O absorptions, while for related 4-Mepy complexes doubly split Cu₄O bands were observed. Two strongly overlapped d—d bands in electronic absorption spectra of the 3-and 4-Mepy complexes in nitromethane were resolved by Gaussian fitting. The 4-Mepy ligand produces slightly stronger ligand field than its 3-Mepy analogue. The maxima of high-energy d—d bands are in a linear correlation with the number of bromide ligands. The correlations for corresponding low-energy bands are considerably deviated from linearity. The halfwave potentials of the complexes in nitromethane correlate with both the number of bromides and the data of electronic absorption spectra suggesting that the reducing electron at the electrode process enters the half-filled d _{z 2} orbital of the copper(II) atom. The origin of a difference between the 3-and 4-Mepy complexes in their spectral and electrochemical properties is also discussed.     

Determination of boron in boron-alloyed steels by inductively coupled plasma atomic emission spectrometry

An inductively coupled plasma atomic emission spectrometry (ICP-AES) procedure has been developed and examined for the determination of boron content (0.01 up to about 2% B) in boron-alloyed steels such as POLDI ATA BOR (65% Fe, 19%Cr, 12% Ni, 1.5% Mn, 1% B), POLDI ATA BOR EXTRA (62% Fe, 18% Cr, 13% Ni, 2.5% Mo, 1.5% Mn, 1% B) and POLDI ATA BOR-R (75% Fe, 18% Cr, 3.5% Ti, 1.8% B). The steel sample is dissolved with a mixture of hydrochloric, nitric, sulfuric and phosphoric acids in a quartz vessel. Borides of alloyed metals, especially of iron and chromium, are quantitatively decomposed. The presence of phosphoric acid in a sample solution reduces the volatility of boric acid with water vapour.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

Pulse plating effect on microstructure and corrosion properties of Zn–Ni alloy coatings

The influence of pulse plating parameters on the surface morphology, grain size, lattice imperfection and corrosion properties of Zn–Ni alloy has been studied. The coatings were electrodeposited in an alkaline cyanide-free solution. AFM was applied for surface morphology examination, XRD measurements were carried out for phase composition and texture analysis, electron probe microanalysis was used for alloy chemical composition studies, while electrochemical techniques were applied for corrosion performance evaluation. The pulse plated Zn–Ni coatings appeared to consist of the γ-Zn₂₁Ni₅ phase and the composition of the alloy depended on the plating parameters. The grain size, lattice imperfection and homogeneity of grain distribution were established to be the main factors determining corrosion behaviour of the coating. Presented at the 4th Baltic Conference on Electrochemistry, Greifswald, March 13–16, 2005