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Capillary gap flow cell as capillary-end electrochemical detector in flow-based analysis


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Islam, MA ORCID: 0000-0002-3982-5347, Lam, SC ORCID: 0000-0001-5247-8397, Li, Y, Atia, MA, Mahbub, P, Nesterenko, PN ORCID: 0000-0002-9997-0650, Paull, B ORCID: 0000-0001-6373-6582 and Macka, M ORCID: 0000-0002-6792-2574 2019 , 'Capillary gap flow cell as capillary-end electrochemical detector in flow-based analysis' , Electrochimica Acta, vol. 303 , pp. 85-93 , doi: 10.1016/j.electacta.2019.02.026.

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A gap flow cell (gap-FC) as a capillary-end electrochemical (EC) detector, incorporating exchangeable screen-printed electrodes, that facilitates adjustment of the gap distance between the capillary outlet and working electrode down to 30 μm was investigated. The analytical performance of the gap-FC was assessed in terms of detector response (current), the efficiency of EC conversion of ferrocyanide, and effective cell volume, as a function of flow rate and gap distance, within a range of 0.1-200 μL min-1 and 30-100 μm, respectively. As a result, an efficiency of EC conversion within the range of ∼1.5-11% (∼3-16 times higher than wall-jet FC), at an effective cell volume of ∼30-75 nL, was achieved. The gap-FC was applied as a liquid chromatography EC detector, coupled with standard and capillary format liquid chromatographs, where the analytical performance of gap-FC was compared with that of a UV detector. With the standard LC, the sensitivity for ascorbic acid, 2,3-dihydroxybenzoic acid and pyrocatechol, was greater than with the UV detector, with limits of detection (LODs) one order of magnitude lower for the gap-FC (0.10 μM, 0.09 μM, 0.19 μM, respectively, RSD 1.35-3.8%, n = 9, linearity r2 ∼0.99 for concentration range 1-100 μM). LODs of test electroactive solutes using the gap-FC were ∼2 times lower than LODs reported in existing literature using standard EC detectors, including wall-jet and thin-layer FCs.

Item Type: Article
Authors/Creators:Islam, MA and Lam, SC and Li, Y and Atia, MA and Mahbub, P and Nesterenko, PN and Paull, B and Macka, M
Keywords: conversion efficiency, effective cell volume, flow-based analysis, gap distance, gap flow cell
Journal or Publication Title: Electrochimica Acta
Publisher: Pergamon-Elsevier Science Ltd
ISSN: 0013-4686
DOI / ID Number: 10.1016/j.electacta.2019.02.026
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© 2019 Published by Elsevier Ltd.

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