A simple, rapid, sensitive and inexpensive approach is described in this work based on a combination of solid‐phase extraction of 8‐hydroxyquinoline (8HQ), for speciation and preconcentration of Cr(III) and Cr(VI) in river water, and the direct determination of these species using a flow injection system with chemiluminescence detection (FI–CL) and a 4‐diethylamino phenyl hydrazine (DEAPH)–hydrogen peroxide system. At different pH, the two forms of chromium [Cr(III) and Cr(VI)] have different exchange capacities for 8HQ, therefore two columns were constructed; the pH of column 1 was adjusted to pH 3 for retaining Cr(III) and column 2 was adjusted to pH 1 for retaining of Cr(VI). The sorbed Cr(III) and Cr(VI) species were eluted from columns using 3.0 ml of 0.1 N of HCl and 3.0 ml of 0.1 N of NaOH, respectively. The flow injection–chemiluminescence (FI–CL) method is based on light emitted due to the oxidation of DEAPH by the H2O2 in the presence of Cr(III), which catalyzes the reaction. The flow cell is a transparent coiled tube made from glass (2.0 × 4.0, inner and outer diameter) and located close to the photodetector. The flow parameters: flow rate, sample volume, flow cell length, and distance to the CL detector were studied and optimized. Under optimum flow conditions, the Cr(III) concentration can be determined over the range 5–350 μg L−1 with a limit of detection of 1.2 μg L−1, as the Cr(III) concentration is proportional to the intensity of the CL signal. The relative standard deviations (%) for 10 and 50 μg L−1 Cr(III) were 1.2% and 3.2%, respectively. The effects of Al(III), Cd(II), Zn(II), Hg(II), Pb(II), Co(II), Cu(II), Ni(II), Mn(II), Ca(II), and Fe(III) were investigated. The proposed method is highly selective and sensitive, enabling a rapid determination of the Cr(III) amount in the presence of other interfering metals. Finally, the FI–CL method was examined in five river water samples with excellent recoveries.
A simple, rapid and sensitive spectrophotometric method has been proposed for the determination of La (III) using 3-hydroxy -4-(2-hydroxy-phenyl azo) naphthalene -1- sulfonic acid as a chromogenic reagent. This method is based on the formation of a red-pink colored complex, upon the reaction of La(III) with the reagent in an alkaline medium (pH= 9.50), having a maximum absorbance at 459 nm. Beer's law is valid in the concentration range 0.512 µg.ml-1 with a Sandell's sensitivity value of 0.0188 µg.cm-2 and molar absorptivity of 7376.12 L.mol-1.cm-1. The stoichiometric composition of the chelate is 1:3. The effect of the presence of different cations as interferants in the determination of La(III) under the given optimum conditions wer
... Show MoreSamarium(III) ions react with (l-2(2-benzoinidazolyl-azo)-2-hydroxy-3-naphthoic acid in basic medium (pH = 8.0) forms a red-orange complex at A.max (550nm). The complex was found to be stable for at least 48 hrs. at the given pH. The apparent molar absorptivity is 7776.77 L.mol-1.Cm-1 and a linear calibration curve is obtained in the range (0.639x 10-5M - 6.350x 10 -5M). The stoichiometry of complex was confirmed by using mole ratio method which indicated that ratio of reagent to metal is 3:1. The effects of the presence of different cations and anions as interferences in the determination of samarium(III) under the given conditions were investigated
The complexes of the 2-hydroxy-4-Nitro phenyl piperonalidene with metal ions Cr(III), Ni(II), Pt(IV) and Zn(II) were prepared in ethanolic solution. These complexes were characterized by spectroscopic methods, conductivity, metal analyses and magnetic moment measurements. The nature of the complexes formed in ethanolic solution was study following the molar ratio method. From the spectral studies, monomer structures proposed for the nickel (II) and Zinc (II) complexes while dimeric structures for the chromium (III) and platinum (IV) were proposed. Octahedral geometry was suggested for all prepared complexes except zinc (II) has tetrahedral geometry, Structural geometries of these compounds were also suggested in gas phase by using
... Show MoreThe new organic reagent 2-[Benzo thiazolyl azo]-4,5-diphenyl imidazole was prepared and used as complexing agent for separation and spectrophotometric determination of Cu2+ ion in some samples include plants, soil, water and human blood serum. Initially determined all factors effect on extraction method and the results show optimum pH was (pHex=9), optimum concentration was 40?g/5mLCu2+ and optimum shaking time was (15min.), as well stoichiometry study appears the complex structure was 1:1 Cu2+: BTADPI. Interferences effect of cations were studied. Synergism effect shows MIBK gave increasing in distribution ratio (D). Organic solvent effect appears there is no any linear relation between dielectric constant for organic solvent used and dis
... Show MoreThe present work investigates the effect of magneto – hydrodynamic (MHD) laminar natural convection flow on a vertical cylinder in presence of heat generation and radiation. The governing equations which used are Continuity, Momentum and Energy equations. These equations are transformed to dimensionless equations using Vorticity-Stream Function method and the resulting nonlinear system
of partial differential equations are then solved numerically using finite difference approximation. A thermal boundary condition of a constant wall temperature is considered. A computer program (Fortran 90) was built to calculate the rate of heat transfer in terms of local Nusselt number, total mean Nusselt number, velocity distribution as well as te
An optoelectronic flow-through detector for active ingredients determination in pharmaceutical formulations is explained. Two consecutive compact photodetector’s devices operating according to light-emitting diodes-solar cells concept where the LEDs acting as a light source and solar cells for measuring the attenuated light of the incident light at 180˚ have been developed. The turbidimetric detector, fabricated of ten light-emitting diodes and five solar cells only, integrated with a glass flow cell has been easily adapted in flow injection analysis manifold system. For active ingredients determination, the developed detector was successfully utilized for the development and validation of an analytical method for warfarin determination
... Show MoreAn optoelectronic flow-through detector for active ingredients determination in pharmaceutical formulations is explained. Two consecutive compact photodetector’s devices operating according to light-emitting diodes-solar cells concept where the LEDs acting as a light source and solar cells for measuring the attenuated light of the incident light at 180˚ have been developed. The turbidimetric detector, fabricated of ten light-emitting diodes and five solar cells only, integrated with a glass flow cell has been easily adapted in flow injection analysis manifold system. For active ingredients determination, the developed detector was successfully utilized for the development and validation of an analytical method for warfarin determination
... Show MoreA robust and sensitive analytical method is presented for the extraction and determination of six pharmaceuticals in freshwater sediments.
