Combination of three analytical techniques for speciation of Al in environmental samples

An analytical scheme is proposed which combines three speciation techniques for determination of particular Al species in soil extracts and percolating waters. A cation-exchange fast protein liquid chromatography — inductively coupled plasma atomic emission spectrometry (FPLC-ICP-AES) procedure, a microcolumn chelating ion-exchange chromatography- atomic absorption spectrometry (MCC-ETAAS) technique and the 8-hydroxyquinoline spectrophotometric method (8HQ-spectrophotometry) were employed. The FPLC-ICP-AES procedure offers determination of Al³⁺ (retention time 4.5 min) and Al(OH)²⁺ species (retention time 4.0 min) which are separated from Al(OH)⁺ ₂ (retention time 1.5min). AlF²⁺ coelutes with Al(OH)²⁺ species, while Al(SO₄)⁺, AlF⁺ ₂ and negatively charged Al organic complexes coelute with Al(OH)⁺ ₂ species. The MCC-ETAAS technique enables determination of the sum of positively charged monomeric aqua- and hydroxy-Al species plus sulphate- and fluoro-Al complexes. Employing the 8HQ-spectrophotometry the sum of positively charged monomeric aqua- and hydroxy-Al species plus sulphato- and most of the labile organic Al species are determined. The sensitivities of these selected techniques were adequate for speciation of Al in the samples analyzed. On the basis of the specific selectivity of a particular technique various groups of Al species may be determined. Thus, the comparison of analytical data from complementary procedures provides more comprehensive information on Al species present in soil extracts and percolating waters.     

Nonordered quantum logic and its YES-NO representation

It is shown that an orthomodular lattice is an ortholattice in which aunique operation of bi-implication corresponds to the equality relation and that the ordering relation in the binary formulation of quantum logic as well as the operation of implication (conditional) in quantum logic are completely irrelevant for their axiomatization. The soundness and completeness theorems for the corresponding algebraic unified quantum logic are proved. A proper semantics, i.e., a representation of quantum logic, is given by means of a new YES-NO relation which might enable a proof of the finite model property and the decidability of quantum logic. A statistical YES-NO physical interpretation of the quantum logical propositions is provided.     

Radon and gamma-radiation measurements in schools on the territory of the abandoned uranium mine “Žirovski vrhl”

On the territory of the abandoned uranium mine irovski vrh, Slovenia, indoor radon and gamma dose rate measurements were carried out in nineteen schools from February 10 to May 10, 1995, using scintillation cells and etched track detectors for radon and thermoluminescence dosimeters for gamma-ray detection. In five schools indoor radon levels exceeded 400 Bq·m^-3, which is the proposed Slovene action level. The maximum average radon value of 1600 Bq·m^-3 and the maximum gamma-dose rate of 172 Sv·month^-1 were found in the same school. According to the ICRP 65 methodology, annual effective doses from radon decay products ranged from 0.05 to 6.10 mSv for pupils and from 0.04 to 4.90 mSv for teachers. Gamma dose rates ranged from 0.05 to 0.19 mSv·y^-1 for pupils and from 0.07 to 0.27 mSv·y^-1 for teachers.     

Structural characterization of chondroitin/dermatan sulfate oligosaccharides from bovine aorta by capillary electrophoresis and electrospray ionization quadrupole time-of-flight tandem mass spectrometry

An analytical approach based on high-performance capillary electrophoresis (CE) in conjunction with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) has been developed for providing the basis to obtain new insights into the domain structure of the glycosaminoglycan (GAG) moiety of proteoglycans. The feasibility and performance of the off-line CE/ESI-QTOF-MS approach in GAG oligosaccharide analysis were assessed by screening a chondroitin/dermatan sulfate (DS) oligosaccharide mixture obtained from bovine aorta by enzymatic depolymerization by chondroitin B lyase. The CS/DS mixture was analyzed by CE using 50 mM ammonium acetate, pH 12.0, dissolved in aqueous methanol (2:3; v/v), as a CE carrier. Structural identification of the GAG components was achieved using off-line CE/nanoESI-QTOF-MS and-MS/MS experiments. ESI-QTOF instrumental parameters were found to play an important role in the MS screening of the CE-separated GAG species. By optimizing the ESI conditions, oligosaccharides differing in chain length and degree of sulfation could be detected. The building block composition, the size of the carbohydrate chain, as well as structural features of the repeating HexA-GalNAc, HexA-GalNAc(S) units, have been determined using MS/MS by applying collision-induced dissociation at low energies. Cleavage of GAG chains by chondroitin B lyase occurs with formation of structural markers useful for identification of IdoA-containing domains.     

Kinetic determination of codeine in pharmaceutical preparations

A kinetic method for the determination of codeine, based on its inhibitor action on the catalytic decomposition of hydrogen peroxide by cobalt(II), is presented. It has been found that the effect of codeine is most pronounced in the presence of 5% v/v ethylene glycol. The reaction is followed photometrically. Codeine can be determined in concentrations ranging from 0.80×10^–5 M to 2.4×10^–5 M. The method has been applied to the determination of codeine in pharmaceutical preparations.     

Electrochemical oxidation of formic acid at noble metals: Catalytic effects of foreign metal monolayers

The catalytic effects of a submonolayer of lead on noble metals have been shown and discussed in terms of a previously published model. A theoretical analysis of these effects is presented. It was demonstrated that foreign metal monolayers allow a determination of the true catalytic activity of electrodes in the case of self-poisoning reactions. A volcano-shaped curve for oxidation of formic acid on noble metal electrodes was obtained.     

Determination of diamine oxidase by a kinetic method with 2,2''-azino-di(3-ethylbenzthiazoline-6-sulfonate)

Hydrogen peroxide, the product of diamine oxidase-catalyzed putrescine or cadaverine oxidation, formed in proportion to the enzyme activity, is measured spectrophotometrically by using the above sulfonate (ABTS) and peroxidase. Only one reagent solution containing 3 mmol of putrescine or 10 mmol of cadaverine, 4 mmol of ABTS and 3000 U of peroxidase per litre of 0.2 mol l^-1 Tris—0.1 mol l^-1 HCl buffer pH 7.5 is needed. Absorbance changes are measured at 410 nm over the first 3 min of the reaction. This initial oxidation rate of the chromogen enables diamine oxidase activity up to 230 U l^-1 to be determined.