Amperometric flow injection analysis as a new approach for studying disperse systems

EUSTAQUIO M. ERRO; CARLA E. GIACOMELLI; ROSARIO PEREZ; MARIA ANGELES ULIBARRI; PATRICIA I ORTIZ; RICARDO ROJAS

ELECTROCHIMICA ACTA

PERGAMON-ELSEVIER SCIENCE LTD

Año: 2009 vol. 55 p. 475 - 479

0013-4686

Fast and simple quantitative determination in dispersed systems (layered double hydroxides – LDHs – suspensions in aqueous solutions) was performed by a procedure that couplesflowinjection and amperometric detection (FI-AM). LDH dispersions are injected in a continuous flow (1mLmin−1) of 0.05 mol L−1 KNO3 solution and [Cu(H2O)6]2+, used as a probe, is detected at a glassy carbon electrode housed in a flat electrochemical cell. The  current intensity, recorded at the selected working potential (−0.25V vs Ag/AgCl/NaCl (3 mol L−1)), presents a linear relationship with [Cu(H2O)6]2+ concentration and the procedure offers high sensitivity (slope = 0.036A/(mol L−1)), a low detection limit (=0.7mol L−1) and a wide quantification range (4–200mol L−1). The method was applied to [Cu(H2O)6]2+ determination in two particular LDH-aqueous solution dispersed systems: (1) [Cu(H2O)6]2+ scavenging by etilendiammintetraacetic acid (EDTA) modified Zn-Al- LDHs, and (2) [Cu(H2O)6]2+ release from a copper doped Mg-Al-LDHs. The results obtained are comparable to those reported in previous works using different quantification techniques. FI-AM determination is applied without sample pretreatment (solid–supernatant separation) providing a high sampling rate (above 120 samples h−1) that allows a better comprehension of the processes, particularly at the initial stages.−1) of 0.05 mol L−1 KNO3 solution and [Cu(H2O)6]2+, used as a probe, is detected at a glassy carbon electrode housed in a flat electrochemical cell. The  current intensity, recorded at the selected working potential (−0.25V vs Ag/AgCl/NaCl (3 mol L−1)), presents a linear relationship with [Cu(H2O)6]2+ concentration and the procedure offers high sensitivity (slope = 0.036A/(mol L−1)), a low detection limit (=0.7mol L−1) and a wide quantification range (4–200mol L−1). The method was applied to [Cu(H2O)6]2+ determination in two particular LDH-aqueous solution dispersed systems: (1) [Cu(H2O)6]2+ scavenging by etilendiammintetraacetic acid (EDTA) modified Zn-Al- LDHs, and (2) [Cu(H2O)6]2+ release from a copper doped Mg-Al-LDHs. The results obtained are comparable to those reported in previous works using different quantification techniques. FI-AM determination is applied without sample pretreatment (solid–supernatant separation) providing a high sampling rate (above 120 samples h−1) that allows a better comprehension of the processes, particularly at the initial stages.