Annali di chimica最新文献

A new ultraviolet spectrophotometric method has been developed for the direct qualitative determination of captopril in pharmaceutical preparation and biological fluids such as human plasma and urine samples. The method was accomplished based on parallel factor analysis (PARAFAC) and partial least squares (PLS). The study was carried out in the pH range from 2.0 to 12.8 and with a concentration from 0.70 to 61.50 μg ml^-1 of captopril. Multivariate calibration models PLS at various pH and PARAFAC were elaborated from ultraviolet spectra deconvolution and captopril determination. The best models for this system were obtained with PARAFAC and PLS at pH = 2.04 (PLS-PH2). The applications of the method for the determination of real samples were evaluated by analysis of captopril in pharmaceutical preparations and biological (human plasma and urine) fluids with satisfactory results. The accuracy of the method, evaluated through the root mean square error of prediction (RMSEP), was 0.58 for captopril with PARAFAC and 0.67 for captopril with PLS-PH2 model. Acidity constant of captopril at 25 °C and ionic strength of 0.1 M have also been determined spectrophotometrically. The obtained pK_a values of captopril are 3.90 ± 0.05 and 10.03 ± 0.08 for pK_a1 and pK_a2, respectively.

An investigation on the partitioning of naphthalene and phenanthrene between water and some water-insoluble phases has been carried out by Uv-vis-NIR spectrophotometry. The analysis of the experimental results emphasized the role of intermolecular interactions and structural features of the hosting phases as driving forces of the partitioning of these polycyclic aromatic hydrocarbons. The critical comparison of the resulting distribution constants allowed to evaluate the potentials of some extracting phases to set up sensitive analytical methods and/or effective environment remediation technologies.

The interaction between man's activities and the environment is gaining world wide attention. Warri an oil producing community in Delta State of Nigeria is faced with environmental oil pollution. Since open and underground water bodies are regarded as final recipients of most environmental pollutants, this study sought to provide data on the levels of the physico-chemical parameters and contaminants in Warri metropolitan water supply. This study investigated the cadmium, lead and chromium using Atomic Absorption Spectrophotometer, physico – chemical properties such as pH, temperature, total suspended solid TSS, total dissolved solid TDS, electrical conductivity EC, biological oxygen demand BOD, dissolved oxygen DO, chemical oxygen demand COD, and total coliform count of potable water sources in Warri. Ekpan River was found to have 1.2mg/L of cadmium, 1.0mg/L of chromium, 1.20mg/L of lead and 2.0mg/L of manganese. The heavy metals levels and the pollution parameters were lowest in the borehole water samples, except pH which is more acidic in borehole water samples and conductivity which is more in well water samples in all the sampling stations. Some of the parameters were above WHO standards.

A simple and accurate spectrophotometric method for determination of trace amounts of silver ion in tap and wastewater solution and photographic solutions has been described. The spectrophotometric determination of silver ion using 2-mercaptobenzoxazole (MBO) in the presence of Triton X-100 as nonionic surfactant has been carried out. The Beer's law is obeyed over the concentration range of 0.1-9.0 μg mL^-1 of Ag⁺ ion with the detection limits of 1.6 ng mL^-1. The influence of type and amount of surfactant, pH, complexation time and amount of ligand on sensitivity of method were optimized. Finally the repeatability, accuracy and the effect of interfering ions on the determination of silver ion were evaluated. There is a good agreement between results of proposed method and atomic absorption spectrometry.

The formal redox potential of the Ti(IV, III) couple has been determined at 25 °C in 1 M HCl, 2 M NaCl aqueous medium, by emf measurements of a junction-free cell with glass and mercury electrodes. Ti(III) and Ti(IV) concentrations were changed by controlled electrolysis. The mean value of the searched formal potential, in a large range of total titanium concentration, is 9 ± 1 mV against the molar hydrogen electrode in the same ionic medium.

A new flow injection chemiluminescence (CL) system was used for the determination of noscapine. This technique is based on the reduction effect of noscapine on the Ru(phen)₃³⁺, which is produced by reaction between Ru(phen)₃²⁺ and acidic Ce(IV) solutions, and this rapid reduction produces strong CL. Calibration plots were linear over the range of 3.0×10^-7-2.0×10^-6 mol L^-1 and 2.0×10^-6-2.0×10^-4 mol L^-1. The CL intensity was so high, that it is able to produce a detection limit of 6.6×10^-8 M noscapine (3σ). The relative standard deviation of 2.0×10^-6 M noscapine was 1.0% (n=10). The proposed method was successfully applied for the flow injection determination of noscapine in cough and Tonin syrup samples. The results of real sample analyses show good recovery percentages (97.3-102.4%). The minimum sampling rate was 100 samples per hour.

The chromium, cobalt and lead removal from aqueous solution by natural and modified zeolites was examined by using a batch-type method. Clinoptilolite samples used in this study were supplied from Bigadiç, Turkey. All samples were modified with HNO₃ or NaOH to improve the adsorption capacity for heavy metals. The removal efficiencies and kinetics of heavy metals such as chromium, cobalt and lead on natural and modified zeolites were determined. The effects of the initial metal concentration on the removal percentage of heavy metal ions were studied. Freundlich and Langmuir isotherm constants and correlation coefficients were found and the equilibrium process was described by the Freundlich isotherm. The adsorption kinetic was tested and then it indicates the process to be diffusion controlled.

Equilibrium studies for the heavy metal ions La(III), Ce(III), Th(IV) and UO₂(IV) (M) complexes of the zwitterionic buffer tricine (L) in aqueous solution are investigated. Stoichiometry and stability constants for the different complexes formed as well as hydrolysis products of the metal cations are determined at 25 °C and ionic strength 0.1 M NaNO₃. The stability of the formed complexes are discussed in terms of the nature of the heavy metal cation. The solid complexes are synthesized and characterized by means of elemental analysis, FTIR, and TG analysis. The general molecular formulae of the obtained complexes is suggested to be [M(L)₂](NO₃)_n-2(H₂O)_x, where n = the charge of the metal cation, x = no. of water molecules.

Modified matrix solid-phase dispersion (MMSPD) and gas chromatography have been developed for quantitative analysis of various classes of pesticides (pirimicarb, metalaxyl, metolachlor, isopropalin and pendimethalin) in soil. MMSPD used Florisil as dispersant and acetone as solvent. Determination was carried out by gas chromatography with nitrogen-phosphorus detection (GC-NPD). The effect of the residence time of pesticides in soil on the recoveries was studied. MMSPD was compared with continuous liquid-solid extraction (LSE). MMSPD had good extraction efficiency and cleanup efficiency and the extract obtained could be directly subjected to GC analysis without further purification. The method gave recoveries ranging from 93% to 100% with relative standard deviations (RSDs) lower than 10%. The limits of detection (LODs) ranged from 0.2 to 2.0 ng g^-1.