In situ solution-phase Raman spectroscopy under forced convection

Huanfeng Zhu, Jun Wu, Qingfang Shi, Zhenghao Wang, Daniel Alberto Scherson

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Abstract

In situ Raman spectra of solution-phase electrogenerated species have been recorded in a channel-type electrochemical cell incorporating a flat optically transparent window placed parallel to the channel plane that contains the embedded working electrode. A microscope objective with its main axis (Z) aligned normal to the direction of flow was used to focus the excitation laser beam (λexc = 532 nm) in the solution and also to collect the Raman scattered light from species present therein. Judicious adjustment of the cell position along Z allowed the depth of focus to overlap the diffusion boundary layer to achieve maximum detection sensitivity. Measurements were performed using a Au working electrode in iron hexacyanoferrate(II), [Fe(CN)6]4-, and nitrite, NO2 -, containing aqueous solutions as a function of the applied potential, E. Linear correlations were found between both the gain and the loss of the integrated Raman intensity, IR, of bands, attributed to [Fe(CN) 6]3- and [Fe(CN)6]4-, respectively, recorded downstream from the edge of the working electrode, and the current measured at the Au electrode as a function of E. The same overall trend was found for the gain in the IR of the NO3 - band in the nitrite solution. Also included in this work is a ray trace analysis of the optical system.

Original languageEnglish
Pages (from-to)8004-8009
Number of pages6
JournalAnalytical chemistry
Volume79
Issue number21
DOIs
Publication statusPublished - 2007 Nov 1
Externally publishedYes

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ASJC Scopus subject areas

  • Analytical Chemistry

Cite this

Zhu, H., Wu, J., Shi, Q., Wang, Z., & Scherson, D. A. (2007). In situ solution-phase Raman spectroscopy under forced convection. Analytical chemistry, 79(21), 8004-8009. https://doi.org/10.1021/ac070573v