Determination of polycyclic aromatic hydrocarbons in waters by ultrasound-assisted emulsification-microextraction and gas chromatography-mass spectrometry

An ultrasound-assisted emulsification-microextraction (USAEME) procedure was developed for the extraction of US EPA 16 polycyclic aromatic hydrocarbons (PAHs) in 10 mL of water samples, with subsequent determination by gas chromatography-mass spectrometry (GC-MS). After determination of the most suitable solvent and solvent volume, several other parameters (i.e., extraction time, centrifugation time and ionic strength of the sample) were optimized using a 2³ factorial experimental design. Limits of detection ranged from 0.001 to 0.036 μg L⁻¹. The developed procedure was applied to fortified distilled water with different fortification levels (0.5, 2 and 5 μg L⁻¹). Recoveries were over 92% and relative standard deviations of the recoveries were below 8%. The efficiency of the USAEME was compared with traditional liquid-liquid extraction (LLE) and solid-phase extraction on real water samples (i.e., tap water, well water and surface (lake) water as well as domestic and industrial wastewaters). The USAEME showed comparable efficiencies especially with LLE. The developed USAEME was demonstrated to be robust, viable, simple, rapid and easy to use for the determination of PAHs in water samples by GC-MS.     

Determination of selected polychlorinated biphenyls in soil by miniaturised ultrasonic solvent extraction and gas chromatography-mass-selective detection

Miniaturised ultrasonic solvent extraction procedure was developed for the determination of selected polychlorinated biphenyls (PCBs) in soil samples by gas chromatography-mass-selective detection by using 2³ factorial experimental design. Recoveries of PCBs from fortified soil samples are over 90% for three different fortification levels between 40 and 120 μg kg⁻¹, and relative standard deviations of the recoveries are below 7%. The limits of detection (LODs) ranged from 0.003 to 0.006 μg kg⁻¹. The performance of the proposed method was compared to traditional shake flask extraction method on the spiked real soil sample and extraction methods showed comparable efficiencies. Proposed miniaturised ultrasonic solvent extraction offers several advantages, i.e., reducing sample requirement for measurement of target compound, less solvent consumption and reducing the costs associated with solvent purchase and waste disposal.     

Preparation of (99m)Tc labeled vitamin C (ascorbic acid) and biodistribution in rats

The aim of this study was to label ascorbic acid with (99m)Tc and to investigate its radiopharmaceutical potential in rats. Ascorbic acid was labeled with (99m)Tc using the stannous chloride method. The radiochemical purity of [(99m)Tc]ascorbic acid ((99m)Tc-AA) was determined by RTLC, paper electrophoresis, and RHPLC methods. The labeling yield was found to be 93+/-5.0%. The maximum labeling yield of (99m)Tc-AA was determined at pH 5 and 25 degrees C. The biodistribution studies related to (99m)Tc-AA were done in male albino Wistar rats. (99m)Tc-AA, which has a specific activity of 13.02 GBq/mmol, was administered into the tail vein of the rats. The rats were sacrificed at 15, 30, 60, and 120 min after the injection by heart puncture under ether anaesthesia. The organs were weighed after removal. Their activities were counted using a Cd(Te) detector equipped with a RAD 501 count system. The %ID/g (% of injected dose per gram of tissue weight) in each organ and in blood was calculated. Maximum uptake of (99m)Tc-AA was observed in prostate and kidneys at the 60th min. (99m)Tc-AA may be a promising radiopharmaceutical for the imaging of prostate and kidneys.     

Endogenous reference points in bargaining

We allow the reference point in (cooperative) bargaining problems with a reference point to be endogenously determined. Two loss averse agents simultaneously and strategically choose their reference points, taking into consideration that with a certain probability they will not be able to reach an agreement and will receive their disagreement point outcomes, whereas with the remaining probability an arbitrator will distribute the resource by using (an extended) Gupta–Livne bargaining solution (Gupta and Livne in Manag Sci 34:1303–1314, 1988). The model delivers intuitive equilibrium comparative statics on the breakdown probability, the loss aversion coefficients, and the disagreement point outcomes.     

A note on the non-commutative neutrix product of distributions

The distributionF(x ₊, −r) Inx₊ andF(x ₋, −s) corresponding to the functionsx ₊ ^−r lnx₊ andx ₋ ^−s respectively are defined by the equations

Synthesis and Characterization of a New (E,E)-Dioxime and its Homonuclear Complexes

N′-(4′-Benzo[15-crown-5]naphthylaminoglyoxime (H₂L) and its sodium chloride complex (H₂L·NaCl) have been prepared from 2-naphthylchloroglyoxime, 4′-aminobenzo[15-crown-5] and sodium bicarbonate or sodium bicarbonate and sodium chloride. Nickel(II), cobalt(II) and copper(II) complexes of H₂L and H₂L·NaCl have a metal–ligand ratio of 1:2 and the ligand coordinates through the two N atoms, as do most of the vic-dioximes. The BF ₂ ⁺ -capped Ni(II), Co(III) and mononuclear complexes of thevic-dioxime were prepared. The macrocyclic ligands and their transition metal complexes have been characterized on the basis of IR, ¹H NMR spectroscopy and elemental analyses data.     

Amperometric determination of bonded glucose with an MnO(2) and glucose oxidase bulk-modified screen-printed electrode using flow-injection analysis

A screen-printed amperometric biosensor based on carbon ink double bulk-modified with MnO₂ as a mediator and glucose oxidase as a biocomponent was investigated for its ability to serve as a detector for bonded glucose in different compounds, such as cellobiose, saccharose, (-)-4-nitrophenyl-β-d-glucopyranoside, as well as in beer samples by flow-injection analysis (FIA). The biosensor could be operated under physiological conditions (0.1 M phosphate buffer, pH 7.5) and exhibited good reproducibility and stability. Bonded glucose was released with glucosidase in solution, and the free glucose was detected with the modified screen-printed electrode (SPE). The release of glucose by the aid of glucosidase from cellobiose, saccharose and (-)-4-nitrophenyl-β-d-glucopyranoside in solution showed that stoichiometric quantities of free glucose could be monitored in all three cases.The linear range of the amperometric response of the biosensor in the FIA-mode flow rate 0.2 mL min⁻¹, injection volume 0.25 mL, operation potential 0.48 V versus Ag/AgCl) extends from 11 to 13,900 μmol L⁻¹ glucose in free form. The limit of detection (3σ) is 1 μmol L⁻¹ glucose. A concentration of 100 μmol L⁻¹ yields a relative standard deviation of approximately 7% with five injections. These values correspond to the same concentrations of bonded glucose supposed that it is liberated quantitatively (incubation for 2 h with glucosidase).Bonded glucose could be determined in beer samples using the same assay. The results corresponded very well with the reference procedure.     

On unsteady unidirectional flows of a second grade fluid

Some properties of unsteady unidirectional flows of a fluid of second grade are considered for flows produced by the sudden application of a constant pressure gradient or by the impulsive motion of one or two boundaries. Exact analytical solutions for these flows are obtained and the results are compared with those of a Newtonian fluid. It is found that the stress at the initial time on the stationary boundary for flows generated by the impulsive motion of a boundary is infinite for a Newtonian fluid and is finite for a second grade fluid. Furthermore, it is shown that initially the stress on the stationary boundary, for flows started from rest by sudden application of a constant pressure gradient is zero for a Newtonian fluid and is not zero for a fluid of second grade. The required time to attain the asymptotic value of a second grade fluid is longer than that for a Newtonian fluid. It should be mentioned that the expressions for the flow properties, such as velocity, obtained by the Laplace transform method are exactly the same as the ones obtained for the Couette and Poiseuille flows and those which are constructed by the Fourier method. The solution of the governing equation for flows such as the flow over a plane wall and the Couette flow is in a series form which is slowly convergent for small values of time. To overcome the difficulty in the calculation of the value of the velocity for small values of time, a practical method is given. The other property of unsteady flows of a second grade fluid is that the no-slip boundary condition is sufficient for unsteady flows, but it is not sufficient for steady flows so that an additional condition is needed. In order to discuss the properties of unsteady unidirectional flows of a second grade fluid, some illustrative examples are given.     

On unsteady motions of a second-order fluid over a plane wall

In this paper, three types of unsteady flows of second-order fluids are considered, namely, flow caused by impulsive motion of a flat plate, flow induced by a constantly accelerating plane and flow imposed by a flat plate that applies a constant tangential stress to the fluid. The previous attempts made regarding these problems, by using the Laplace transform, have failed. In this paper, the sine and the cosine transforms are used to solve these problems and exact solutions for the velocity distributions are found in terms of definite integrals. It is shown that these exact solutions satisfy the initial and the boundary conditions and the governing equation.