In situ analysis of copper electrodeposition reaction using unilateral NMR sensor

Autor(es)

Gomes, B. F. ^[1] ; Nunes, L. M. S. ^[1] ; Lobo, C. M. S. ^[1] ; Carvalho, A. S. ^[1] ; Cabeca, L. F. ^[2] ; Colnago, L. A. ^[3]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Inst Quim Sao Carlos, BR-13560070 Sao Carlos, SP - Brazil

^[2] Univ Tecnol Fed Parana UTFPR, Londrina, PR - Brazil

^[3] Embrapa Instrumentacao, BR-13560970 Sao Carlos, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: JOURNAL OF MAGNETIC RESONANCE; v. 261, p. 83-86, DEC 2015.
• Citações Web of Science: 10

Resumo

The uses of high-resolution NMR spectroscopy and imaging (MRI) to study electrochemical reactions in situ have greatly increased in the last decade. However, most of these applications are limited to specialized NMR laboratories and not feasible for routine analysis. Recently we have shown that a bench top, time domain NMR spectrometer can be used to monitor in situ copper electrodeposition reaction and the effect of Lorentz force in the reaction rate. However these spectrometers limit the cell size to the magnet gap and cannot be used with standard electrochemical cells. In this paper we are demonstrating that unilateral NMR sensor (UNMR), which does not limit sample size/volume, can be used to monitor electrodeposition of paramagnetic ions in situ. The copper electrodeposition reaction was monitored remotely and in situ, placing the electrochemical cell on top of the UNMR sensor. The Cu2+ concentration was measured during three hours of the electrodeposition reactions, by using the transverse relaxation rate (R-2) determined with the Carr-Purcell-Meiboom-Gill pulse sequence. The reaction rate increased fourfold when the reaction was performed in the presence of a magnetic field (in situ), in comparison to the reactions in the absence of the magnetic field (ex situ). The increase of reaction rate, in the presence of the UNMR magnet, was related to the magneto hydrodynamic force (F-B) and magnetic field gradient force (F-del B). F-del B was calculated to be one order of magnitude stronger than F-B. The UNMR sensor has several advantages for in situ measurements when compared to standard NMR spectrometers. It is a low cost, portable, open system, which does not limit sample size/volume and can be easily be adapted to standard electrochemical cells or large industrial reactors. (C) 2015 Elsevier Inc. All rights reserved. (AU)

• Processo FAPESP: 07/07436-8 - Desenvolvimento da técnica de rmn-ssfp para aumento da razão sinal ruído em experimentos de rmn-eletroquímica in situ
• Beneficiário: Luiza Maria da Silva Nunes
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 12/22281-9 - Estudo por RMN do fenômeno magneto-convectivo sobre íons paramagnéticos durante eletrodeposição
• Beneficiário: Bruna Ferreira Gomes Lobo
• Modalidade de apoio: Bolsas no Brasil - Doutorado Direto