Related Experiment Videos
Supercritical fluid extraction and gas chromatography or electroanalysis of metal chelates from different sample
1P. Universidad Catolica de Chile, Facultad de Quimica, Departamento de Quimica Inorganica, Santiago, Chile.
Abstract:
The supercritical fluid extraction of Pb(DDC)2 and MoO2(acac)2 complexes is performed. The previously formed complexes are used in order to simplify the extraction process. In the extraction cell, 9.0 mg of Pb(DDC)2 or 30.0 mg of MoO2(acac)2 is added. With these two complexes, a study of static and dynamic extraction as a function of pressure (1000-2500 psi), temperature (40-160 degrees C), and presence of modifier (methanol) is performed. Under the best conditions, 5.6 mg of Pb(DDC)2 (2.3 mg of Pb2+) is recovered. The parameters are 2500 psi of pressure, 160 degrees C of temperature, 0.5 mL methanol (placed in a 10-mL extraction cell), 60.0 min of static extraction, and 2.0 min of dynamic extraction. It is necessary to add 3.0 mL of methanol to enhance efficiency on the MoO2(acac)2 complex recovery. Quantitative extractions of MoO2(acac)2 (9.0 mg of MoVI) are obtained when the experiments are carried out under 1000-2500 psi of pressure, 140 degrees C, and times no longer than 10.0 min. Then, the study is carried out forming the in situ complexes. For this purpose, metallic ion and ligand are added. Under these conditions, the Pb2+ recovery decreases from 2.3 to 1.9 mg, and the MoVI recovery decreases from 9.0 to 1.0 mg. When 1.9 mg of Pb2+ and 1.0 mg of MoVI or less is placed in the extraction cell, the recoveries are always 100%. The Pb2+ extracts are directly accomplished using gas chromatography-flame ionization detection (GC-FID), and the MoVI extracts are analyzed using GC-FID and catalytic adsorption voltammetry. The quantitation of pure extracts is carried out by constructing calibration curves with complex solutions and sample solutions using the standard addition method. This method is applied by determination of Pb2+ in sodium alginate extracted from algae and blood, urine, and human milk from patients with diagnosed plumbunemy. MoVI is determined in irrigation water and pasture of animal intake.