Study of linearity and stability of Pb(II)-1,10-phenanthroline complex with the presence of Fe (II) dan Mg (II) matrix ions using UV-Vis spectrophotometry

An analytical method for the spectrophotometric determination of some phenolic compounds, i.e.: pyrocathecol and pyrogallol based on their redox reaction with iron(III)-phenanthroline complex has been developed. These two compounds, in appropriate conditions, reduce iron(III)-phenanthroline complex to yield very stable and color-intense complex of iron(II)-phenanthroline, [Fe(phen)2]2+, whose concentration is equivalent to the amount of pyrocathecol or pyrogallol in the solution, and is easily detected by spectrophotometric method. Some parameters influencing the sensitivity of the determination were optimized. These included maximum absorption wavelength, pH of the solution, time and temperature of heatingand reagent to analyte minimum mole-ratio. Using the optimum conditions obtained, the analytical performance of the method was examined and the developed method was then applied to analyzed pyrocathecol and pyrogallol contents in several river water of Yogyakarta, Indonesia. Result of the study showed that the optimum conditions for the determination of pyrocathecol are as follows: maximum absorption wavelength (lmax) at 510 nm, pH of the solution = 4, heating time = 120 min, heating temperature = 70 0C and the minimum mole ratio of reagent to analyte is 8. On the other hand, the optimum conditions for the determination of pyrogallol are as follows: maximum absorption wavelength (lmax) at 510 nm, pH of the solution = 5, heating time = 90 min, heating temperature = 90 0C and the minimum mole ratio of reagent to analyte is 7. At the corresponding conditions of analysis, calibration curves for pyrocathecol and pyrogallol are linear in the range concentration of 0.00 - 0.16 ppm and 0.00 - 0.24 ppm, respectively. The correlation coefficients for both compounds were found to be higher than 0.998 and the detection limits went down below 0.07 ppm. It has been demonstrated that the developed method can be applied for the determination of pyrocathecol and pyrogallol contents in natural samples. Keywords: Spectrophotometry, phenolic compounds, 1,10-phenanthroline, redox reaction

Download Full-text

Nickel-phenanthroline Complex Supported on Mesoporous Carbon as a Catalyst for Carboxylation under CO2 Atmosphere

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.16.1.9733.111-119 ◽

2021 ◽

Vol 16 (1) ◽

pp. 111-119

Author(s):

Iman Abdullah ◽

Riri Andriyanti ◽

Dita Arifa Nurani ◽

Yuni Krisyuningsih Krisnandi

Keyword(s):

Mesoporous Carbon ◽

Nickel Complex ◽

Solid Support ◽

Soft Template ◽

X Ray Diffraction ◽

X Ray ◽

Ft Ir ◽

Phenanthroline Complex ◽

Temperature Time ◽

Open Access Article

Carbon dioxide is a highly potential renewable C1 source for synthesis of fine chemicals. Utilization of CO2 in carboxylation reactions requires catalysts, such as: nickel complex for CO2 activation. However, the use of homogeneous catalysts in the reaction is still less efficient due to the difficulty of separating the product and catalyst from reaction mixture. Therefore, it is necessary to heterogenize the nickel complex in a solid support such as mesoporous carbon. In this report, mesoporous carbon (MC) prepared from phloroglucinol and formaldehyde through soft template method was used as a solid support for Ni-phenanthroline complex (Ni-phen). The catalyst was characterized by Fourier Transform Infra Red (FT-IR), X-Ray Diffraction (XRD), Scanning Electron Microscope - Energy Dispersive X-Ray (SEM-EDX), and Surface Area Analyzer (SAA). The result of SAA characterization showed that the pore diameter of MC was 6.7 nm and Ni-phen/MC was 5.1 nm which indicates that the materials have meso-size pores. Ni-phen/MC material was then used as a heterogeneous catalyst in the carboxylation reaction of phenylacetylene under an ambient CO2 pressure. The reactions were carried out in several variations of conditions such as temperature, time and catalyst types. Based on the results of the reaction, the best conditions were obtained at 25 °C for 8 h of reaction time using Ni-phen/MC catalyst. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0).

Download Full-text