Optimization of the solid phase extraction method for determination of Cu(II) in natural waters by using response surface methodology

A solid-phase extraction method was proposed for the preconcentration of Cu(II) in different samples in a mini-column packed with functionalized multi-walled carbon nanotubes (MWCNTs-COOH) as an effective sorbent, without using any complexing reagent, prior to its determination by flame atomic absorption spectrometry using response surface methodology. The experimental optimization step was performed by both a two-level full factorial design, with a center point, and a Box-Behnken design combined with response surface methodology. Three variables (pH, amount of Cu(II), and sample volume) were regarded as factors in the optimization. It was found that pH is the most significant factor affecting the preconcentration of Cu(II). The preconcentration factor was obtained as 100. The linear range was 1-5 mg L(-1) (R(2) = 0.999). Under the optimized experimental conditions, the detection limit (3s) of the proposed method followed by FAAS was found to be 0.27 μg L(-1). The relative standard deviation for 10 replicate measurements of 50 and 100 μg L(-1) Cu(II) was 2.39% and 0.98%, respectively. The response surface methodology was successfully applied to the determination of Cu(II) in water samples and mussel samples, and in a certified standard reference material (BCR-320R, Channel sediment).     

Study of the Thermal Decompositions on N,N-Dialkyl-N'-Benzoylthiourea Complexes of Cu(II), Ni(II), Pd(II), Pt(II), Cd(II), Ru(III) and Fe(III)

The thermal decompositions of the complexes of N,N-dialkyl-N'-benzoylthioureas with Cu(II), Ni(II), Pd(II), Pt(II), Cd(II), Ru(III) and Fe(III) were studied by TG and DTA techniques. These metal complexes decompose in two stages: elimination of dialkylbenzamide, and total decomposition to metal sulphides or metals. The influence of the alkyl substituents in these benzoylthiourea chelates on the thermal behaviour of the metal complexes was investigated.This revised version was published online in November 2005 with corrections to the Cover Date.     

An investigation of decomposition stages of a ruthenium polypridyl complex by non-isothermal methods

Thermal properties of [cis-(dithiocyanato)(4,5-diazafluoren-9-one)(4,4??-dicarboxy-2,2??-bipyridyl)ruthenium(II)], [Ru(L ₁)(L ₂)(NCS)₂] (where the ligands L ₁?=?4,5-diazafluoren-9-one, L ₂?=?4,4??-dicarboxy-2,2??-bipyridyl) have been investigated by DTA/TG/DTG measurements under inert atmosphere in the temperature range of 30?C1155?°C. The mass spectroscopy technique has been used to identify the products during pyrolytic decomposition. The pyrolytic final products have been analyzed by X-ray powder diffraction technique. A decomposition mechanism has been also suggested for the cis-[Ru(L ₁)(L ₂)(NCS)₂] complex based on the results of thermogravimetrical and mass analysis. The values of the activation energy, E* have been obtained by using model-free Kissenger?CAkahira?CSunose and Flyn?CWall?COzawa non-isothermal methods for all decomposition stages. Thirteen kinetic model equations have been tested for selecting the best reaction models. The best model equations have been determined as A2, A3, D1, and D2 which correspond to nucleation and growth mechanism for A2 and A3 and diffusion mechanism for D1 and D2. The optimized average values of E* are 31.35, 58.48, 120.85, and 120.56?kJ?mol^?1 calculated by using the best model equations for four decomposition stages, respectively. Also, the average Arrhenius factor, A, has been obtained as 2.21, 2.61, 2.52, and 2.21?kJ?mol^?1 using the best model equation for four decomposition stages, respectively. The ??H*, ??S*, and ??G* functions have been calculated using the optimized values.     

The thermoluminescence properties of CdS films under nitrogen atmosphere

Chemically deposited cadmium sulphide (CdS) films have been grown on glass at 60 °C and annealed at nitrogen atmosphere at different temperatures. The as-deposited film shows a mix phase of cubic and hexagonal. Once the film subjected to annealing the hexagonal phase becomes dominant and the crystal size increases due to these changes optical band gap energy decreases from 2.44 to 2.28 eV. The electrical conductivity increases depending on temperature and the film annealed at 423 K shows the highest conductivity. Thermoluminescence (TL) intensity of the films was measured after irradiating the films with ⁹⁰Sr/⁹⁰Y β-source and the trap depths were calculated after the TL curves deconvoluted by using the computer glow curve deconvolution (CGCD) method. It is observed that the as-deposited film has three different trap depths, at around 0.257, 0.372, and 0.752 eV corresponding to 383, 473, and 608 K, respectively.