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This paper discusses silica surface modification by a process involving a two-step reaction: anchoring of a silylating agent, followed by an attachment of a 4-amino-2-mercaptopyrimidine molecule. The modified material (Si-BP) was successfully characterized by the FTIR spectra, which revealed amine absorption bands, and through 13C and 29Si NMR spectra, which confirm the proposed structure of the modified silica (Si-BP). Si-BP was used to extract cadmium and lead from an aqueous medium at 298 K. The Si-BP kinetics towards metal ions was very fast, i.e., about 10 minutes, although extraction was significantly impaired at pH 3. The series of adsorption isotherms were adjusted to a modified Langmuir equation and the maximum extraction capacity was 0.193 and 0.387 mmol g-1 for Cd(II) and Pb(II), respectively. An analysis of the Ø values lead to the inference that the resulting metal ligand complex was type 1:1.
This paper proposes a method to determine selenium in samples of fish muscle and liver tissue using ultrasound assisted extraction process, and analysed by graphite furnace atomic absorption spectrometry (GFAAS). The selenium content was extracted by 0.10 M HCl at the optimal extraction conditions which were established as follows: sample mass of 100 mg; granulometry of the sample <60 µm; sonication time of five 40 s cycles; and sonication power of 136 W. The selenium determinations were performed by GFAAS, at a drying temperature of 120°C/250°C, pyrolysis temperature of 1300°C, atomization temperature of 2300°C, and cleaning temperature of 2800°C. Palladium nitrate was used as a chemical modifier coinjected with the samples, and tungsten as a permanent modifier. The concentration of selenium determined in the pool of fish muscle and liver tissue were 280.4±4.2 e 592.3±6.7 μg kg−1, respectively. The accuracy and precision of the proposed extraction method were evaluated using certified standard Bovine Muscle - NIST 8414. The results obtained by the ultrasonic extraction method were equivalent to those obtained by the method of acid mineralization of samples in a microwave oven
A method was developed to attach 2,2-bipyridine (BP) onto a silica gel surface by a two-step reaction. The first step consisted of a reaction between the matrix and a silylating agent, 3-chloropropyltrimethoxysilane. In the second step of the reaction, a ligand molecule was attached onto Si-CPTS, yielding the product Si-BP. The modified material contained 0.431±0.01 mmol of 2,2-bipyridine per gram of modified silica, as confirmed by FT-IR spectra of the proposed structure. The surface modification was characterized by the BET technique, which revealed a decrease in the surface area from 614 to 450 m2 g-1. The series of adsorption isotherms for the metal ions were adjusted to fit a modified Langmuir equation. The maximum number of moles of copper, cadmium and lead ions adsorbed was 0.64, 0.53, and 0.54 mmol g-1, respectively. The surface saturation was calculated as φ fraction and the values obtained, Cu(II) = 1.160, Cd(II) = 1.044 and Pb(II) = 0.997, suggest a type 1:1 metal-ligand complex.
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