Internal standardization for the determination of cadmium,cobalt, chromium and manganese in saline produced water from petroleum industry by inductively coupled plasma optical emission spectrometry after cloud point extraction

In the present paper a procedure is proposed for the determination of traces of Cd, Co, Mn and Cr in petroleum industry produced water by inductively coupled plasma optical emission spectrometry. The procedure is based on cloud point extraction of these metals, as their dithizonate complexes, into the surfactant-rich phase of octylphenoxypolyethoxyethanol surfactant (Triton X-114). Extractions were carried out in solutions with salinities between 10‰ and 70‰. Since residual salinity in the surfactant-rich phase caused differences in its transport to the plasma, yttrium was used as an internal standard to correct for this effect. The simultaneous metal extraction procedure was optimized by response surface methodology using a Doehlert design and desirability function. Enhancement factors of 21, 21, 9 and 19, along with limits of quantification of 0.093, 0.20, 0.73 and 1.2 μg L^− 1, and precision expressed as relative standard deviation (n = 8, 20.0 μg L^− 1) of 5.8, 1.2, 1.7 and 5.7% were obtained for Cd, Co, Mn and Cr, respectively. The accuracy was evaluated by spike recovery tests on the high salinity water samples with salinity of 40 and 63‰.     

Development of a so-called hour method for analysis of plutonium in soil samples

A short overview of HPLC column packings is presented. The properties of chromatographic carriers and the possibilities to combine the solid matrices with organic polymeric stationary phases are elucidated in detail. The latest achievements and anticipated future developments in the area are outlined.     

Estimates for the Poisson kernel and Hardy spaces on compact manifolds

We study Hardy spaces on the boundary of a smooth open subset or Rn and prove that they can be defined either through the intrinsic maximal function or through Poisson integrals, yielding identical spaces. This extends to any smooth open subset of Rn results already known for the unit ball. As an application, a characterization of the weak boundary values of functions that belong to holomorphic Hardy spaces is given, which implies an F. and M. Riesz type theorem.     

Large-scale production of cellulose-binding domains. Adsorption studies using CBD-FITC conjugates

A method for the gram-scale production of cellulose-binding domains (CBD) through the proteolytic digestion of a commercial enzymatic preparation (Celluclast) was developed. The CBD obtained, isolated from Trichoderma reesei cellobiohydrolase I, is highly pure and heavily glycosylated. The purified peptide has a molecular weight of 8.43 kDa, comprising the binding module, a part of the linker, and about 30% glycosidic moiety. Its properties may thus be different from recombinant ones expressed in bacteria. CBD-fluorescein isothiocyanate conjugates were used to study the CBD-cellulose interaction. The presence of fluorescent peptides adsorbed on crystalline and amorphous cellulose fibers suggests that amorphous regions have a higher concentration of binding sites. The adsorption is reversible, but desorption is a very slow process.     

Comparison of the performance of graphitized carbon black and poly(styrene-divinylbenzene) cartridges for the determination of pesticides and industrial phosphates in environmental waters

The determination of polar and nonpolar organophosphorus compounds, triazines and their metabolites, molinate and chlorothalonil in 1 l water samples was investigated using off-line solid-phase extraction followed by gas chromatography with nitrogen-phosphorus and flame photometric detection. The ethylvinylbenzene-divinylbenzene copolymer (LiChrolut EN) and the commercial graphitized carbon black (GCB) of Envi-Carb were tested as solid-phase sorbents. The matrix effect was studied by extracting the compounds spiked in water samples of different types (Milli-Q, tap, salted tap water, river and sea water). The polymeric sorbent LiChrolut EN allowed the determination at low ng/l of all 40 compounds tested, except the very polar atrazine-desethyl-deisopropyl (DDA). Recoveries of compounds from the Envi-Carb sorbent are comparable to those obtained for LiChrolut EN with the exception of chlorothalonil and the more hydrophobic organophosphorus compounds (coumaphos, leptophos), which were strongly sorbed in the Envi-Carb cartridges. Envi-Carb, however, enabled the determination of DDA with a limit of detection of 14 ng/l.     

Molecular weight effect on the photoinduced birefringence and surface relief gratings formation of a methacrylate azopolymer

Samples of a methacrylic side-chain azopolymer were synthesized by a radical copolymerization of methyl-methacrylate with the methacrylic derivative of the commercial dye Disperse Red-13 (DR13). Copolymers with different molecular weight were obtained by varying the reaction time and the concentration of initiator. Samples with molecular weight averages (M_w) from 3 to 8 × 10⁴ g/mol and 1.4-1.7 polydispersity were obtained. The glass transition temperature of the samples increased linearly from the lower to the highest molecular weight. Optical quality cast films were prepared for all samples and photoinduced birefringence was successfully carried out in all samples as well as surface relief gratings could be inscribed in the cast films.     

Direct determination of gallium on polyurethane foam by X-ray fluorescence

Gallium chloride is easily extracted from 6M HCl by comminuted polyether-type polyurethane foam. After the extraction step, the gallium absorbed by the PU foam can be quantitatively determined by X-ray fluorescence. A procedure for the direct determination of gallium absorbed by PU foam by XRFS is thus described. Gallium is determined at levels as low as 60 ng/ml (C(L)), with a calibration sensitivity of 424 cps ml/mug, within a linear range 0.1-2.30 mug/ml. The procedure investigated was successfully applied to determination of gallium in aluminum alloys, bauxite and industrial residue samples.     

Determination of volatile corrosion inhibitors by capillary electrophoresis

In this work, a capillary electrophoresis (CE) method using indirect UV detection (214nm) for the simultaneous determination of monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), diethylethanolamine (DEEA), monocyclohexylamine (MCHA) and dicyclohexylamine (DCHA) in water/ethanol extracts of wrapping materials containing volatile corrosion inhibitors (VCIs) was described. A running buffer consisting of 0.010 molL(-1) imidazole, 0.010 molL(-1) 2-hydroxyisobutyric acid (HIBA) and 0.010 molL(-1) 18-crown-6 ether enabled separation of the analytes in less than 7 min. A few method validation parameters were determined revealing good migration time repeatability (<0.7% RSD) and area repeatability (< 1.8% RSD). Limits of detection were in the range of 0.52-1.54 mg L(-1). Recovery values were in the range of 94.8-100.9%. The methodology was successfully applied to the analysis of three commercial products (VCI treated paper, foam and plastic). The concentration of amines in these materials varied from 0.050 to 22.3% (w/w).     

Trace and major elements in serum of patients with chronic myelogenous leukemia

Summary Major and trace elements were determined in serum of patients with chronic myelogenous leukemia (CML) using total reflection X-ray fluorescence induced by synchrotron radiation (SRTXRF). CML affects 1 to 2 people per 100,000 and accounts for 7-20% cases of leukemia. It was possible to determine the concentrations of the following elements: P, S, Cl, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Br and Rb. Using analysis of variance (ANOVA) it was observed that the contents of the P, S, Ca, Cr, Mn, Fe, Cu and Rb elements differed significantly at a = 0.05 between groups of healthy subjects and CML patients and also genders (males and females).