In Situ Electrochemical SFG/DFG Study of CN− and Nitrile Adsorption at Au from 1-Butyl-1-methyl-pyrrolidinium Bis(trifluoromethylsulfonyl) Amide Ionic Liquid ([BMP][TFSA]) Containing 4-{2-[1-(2-Cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} Benzonitrile (CTDB) and K[Au(CN)2]
Abstract
:1. Introduction
2. Results and Discussion
2.1. Cyclic Voltammetry
2.2. In Situ Sum- and Difference-Frequency Generation Spectroscopy (SFG/DFG)
2.2.1. Adsorption and Cathodic Reaction of CTDB in [BMP][TFSA]
2.2.2. Electrodeposition of Au from a [BMP][TFSA]-based solution containing CTDB and K[Au(CN)2]
3. Experimental
3.1. Single-Resonance Model for SFG/DFG
3.2. N-Resonance Model for SFG/DFG
3.3. Identification of a Guess Set of Parameters by Graphical Approach and Linear Least-Squares
3.4. Recovery of the “Physical” Parameter Set from the “Minimal-Correlation” Parameter Set
- (i) Since, in the case of Au, for Au, we can take: , whence: .
- (ii) It is possible to use the approximation (i) to estimate A from β as follows:, whence: . Since physical solutions ought to be positive, it follows that: .
- (iii) At this point, it is possible to estimate a from δ:, whence:
- (iv) Once an estimate of a is available, it is possible to produce a better estimate of b by using the exact expression: . This updated value of b can, of course be used at point (ii) above and following to set up an iterative scheme.
4. Conclusions
Acknowledgements
References and Notes
- Electrodeposition from Ionic Liquids; Endres, F.; MacFarlane, D.; Abbott, A. (Eds.) Wiley-VCH: Weinheim, Germany, 2008.
- Nanbu, N.; Sasaki, Y.; Kitamura, F. In situ FT-IR spectroscopic observation of a room-temperature molten salt vertical bar gold electrode interphase. Electrochem. Commun. 2003, 5, 383–387. [Google Scholar] [CrossRef]
- Nanbu, N.; Kato, T.; Sasaki, Y.; Kitamura, F. In situ SEIRAS study of room-temperature ionic liquid vertical bar gold electrode interphase. Electrochemistry 2005, 7, 610–613. [Google Scholar]
- Santos, V.O.; Alves, M.B.; Carvalho, M.S.; Suarez, P.A.Z.; Rubim, J.C. Surface-enhanced Raman scattering at the silver electrode/ionic liquid (BMIPF6) interface. J. Phys. Chem. B 2006, 110, 20379–20385. [Google Scholar]
- Baldelli, S. Surface structure at the ionic liquid-electrified metal interface. Acc. Chem. Res. 2008, 41, 421–431. [Google Scholar] [CrossRef]
- Iwahashi, T.; Miyamae, T.; Kanai, K.; Seki, K.; Kim, D.; Ouchi, Y. Anion configuration at the air/liquid interface of ionic liquid [bmim]OTf studied by sum-frequency generation spectroscopy. J. Phys. Chem. B 2008, 112, 11936–11941. [Google Scholar] [CrossRef]
- Bozzini, B.; Bund, A.; Busson, B.; Humbert, C.; Ispas, A.; Mele, C.; Tadjeddine, A. An SFG/DFG investigation of CN− adsorption at an Au electrode in 1-butyl-1-methyl-pyrrolidinium bis(trifluoromethylsulfonyl) amide ionic liquid. Electrochem. Commun. 2010, 12, 56–60. [Google Scholar] [CrossRef]
- Bozzini, B.; Busson, B.; Humbert, C.; Mele, C.; Raffa, P.; Tadjeddine, A. Investigation of Au electrodeposition from [BMP][TFSA] room-temperature ionic liquid containing K[Au(CN)2] by in situ two-dimensional sum frequency generation spectroscopy. J. Electroanal. Chem. 2011, 661, 20–24. [Google Scholar] [CrossRef]
- Bozzini, B.; Sgura, I. Parameter functional dependence in an electro-chemical model: Theoretical and computational issues. Note Mat. 2007, 27, 39–52. [Google Scholar]
- Bozzini, B.; D’Urzo, L.; Mele, C.; Busson, B.; Humbert, C.; Tadjeddine, A. Doubly resonant sum frequency generation spectroscopy of adsorbates at an electrochemical interface. J. Phys. Chem. C 2008, 112, 11791–11795. [Google Scholar]
- Bozzini, B.; Mele, C.; Tondo, E. A SERS investigation of Cu electrodeposition in the presence of the model leveller 4-{2-[1-(2-cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} benzonitrile. Electrochim. Acta 2010, 55, 3279–3285. [Google Scholar] [CrossRef]
- Sur, U.K.; Lakshminarayanan, V. A study of the hydrophobic properties of alkanethiol self-assembled monolayers prepared in different solvents. J. Electroanal. Chem. 2004, 565, 343–350. [Google Scholar] [CrossRef]
- Zawisza, I.; Bin, X.; Lipkowski, J. Spectroelectrochemical studies of bilayers of phospholipids in gel and liquid state on Au(111) electrode surface. Bioelectrochemistry 2004, 63, 137–147. [Google Scholar] [CrossRef]
- MacFarlane, D.R.; Meakin, P.; Sun, J.; Amini, N.; Forsyth, M. Pyrrolidinium imides: A new family of molten salts and conductive plastic crystal phases. J. Phys. Chem. B 1999, 103, 4164–4170. [Google Scholar] [CrossRef]
- Lund, H. Cleavages and Deprotection. In Organic Electrochemistry; Lund, H., Hammerich, O., Eds.; Marcel Dekker Inc.: New York, NY, USA, 2001; p. 969. [Google Scholar]
- Bozzini, B.; Busson, B.; de Gaudenzi, G.P.; D’Urzo, L.; Mele, C.; Tadjeddine, A. An in situ SFG and SERS investigation into the electrodeposition of Au from Au(CN)2− and Au(CN)4− solutions. J. Electroanal. Chem. 2007, 602, 61–69. [Google Scholar] [CrossRef]
- Tadjeddine, A.; le Rille, A. Sum and Difference Frequency Generation at Electrode Surfaces. In Interfacial Electrochemistry: Theory, Experiment, and Applications; Wieckowski, A., Ed.; Marcel Dekker, Inc.: New York, NY, USA, 1999; p. 317. [Google Scholar]
- Bozzini, B.; Mele, C.; Fanigliulo, A.; Busson, B.; Vidal, F.; Tadjeddine, A. An SFG investigation of Au(111) and Au(210) electrodes in aqueous solutions containing KCN and cetylpyridinium chloride. J. Electroanal. Chem. 2004, 574, 85–94. [Google Scholar] [CrossRef]
- Bozzini, B.; D’Urzo, L.; Mele, C. Electrodeposition of Cu from cyanoalkaline solutions in the presence of CPC and PEG—An electrochemical and in situ SERS investigation. J. Electrochem. Soc. 2005, 152, C255–C264. [Google Scholar] [CrossRef]
- Bozzini, B.; D'Urzo, L.; Mele, C.; Romanello, V. A SERS investigation of cyanide adsorption and reactivity during the electrodeposition of gold, silver, and copper from aqueous cyanocomplexes solutions. J. Phys. Chem. C 2008, 112, 6352–6358. [Google Scholar] [CrossRef]
- Bozzini, B.; Giovannelli, G.; Natali, S.; Fanigliulo, A.; Cavallotti, P.L. Crystallographic structure of gold films electrodeposited at low current densities. J. Mater. Sci. 2002, 37, 3903–3913. [Google Scholar] [CrossRef]
- Humbert, C.; Busson, B.; Six, C.; Gayral, A.; Gruselle, M.; Villain, F.; Tadjeddine, A. Sum-frequency generation as a vibrational and electronic probe of the electrochemical interface and thin films. J. Electroanal. Chem. 2008, 621, 314–321. [Google Scholar] [CrossRef]
- Sgura, I.; Bozzini, B. Numerical issues related to the modelling of electrochemical impedance data by non-linear least-squares. Int. J. Non-Lin. Mech. 2005, 40, 557–570. [Google Scholar] [CrossRef]
- Sample Availability: Samples of the compounds quoted in the text are available from the mentioned vendors.
© 2012 by the authors; licensee MDPI, Basel, Switzerland. This article is an open-access article distributed under the terms and conditions of the Creative Commons Attribution license (http://creativecommons.org/licenses/by/3.0/).
Share and Cite
Bozzini, B.; Busson, B.; Gayral, A.; Humbert, C.; Mele, C.; Six, C.; Tadjeddine, A. In Situ Electrochemical SFG/DFG Study of CN− and Nitrile Adsorption at Au from 1-Butyl-1-methyl-pyrrolidinium Bis(trifluoromethylsulfonyl) Amide Ionic Liquid ([BMP][TFSA]) Containing 4-{2-[1-(2-Cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} Benzonitrile (CTDB) and K[Au(CN)2]. Molecules 2012, 17, 7722-7736. https://doi.org/10.3390/molecules17077722
Bozzini B, Busson B, Gayral A, Humbert C, Mele C, Six C, Tadjeddine A. In Situ Electrochemical SFG/DFG Study of CN− and Nitrile Adsorption at Au from 1-Butyl-1-methyl-pyrrolidinium Bis(trifluoromethylsulfonyl) Amide Ionic Liquid ([BMP][TFSA]) Containing 4-{2-[1-(2-Cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} Benzonitrile (CTDB) and K[Au(CN)2]. Molecules. 2012; 17(7):7722-7736. https://doi.org/10.3390/molecules17077722
Chicago/Turabian StyleBozzini, Benedetto, Bertrand Busson, Audrey Gayral, Christophe Humbert, Claudio Mele, Catherine Six, and Abderrahmane Tadjeddine. 2012. "In Situ Electrochemical SFG/DFG Study of CN− and Nitrile Adsorption at Au from 1-Butyl-1-methyl-pyrrolidinium Bis(trifluoromethylsulfonyl) Amide Ionic Liquid ([BMP][TFSA]) Containing 4-{2-[1-(2-Cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} Benzonitrile (CTDB) and K[Au(CN)2]" Molecules 17, no. 7: 7722-7736. https://doi.org/10.3390/molecules17077722