Abstract

In this paper, carboxyl groups were introduced by liquid oxidation methods onto multi-walled carbon nanotubes (MWCNTs) to improve the MWCNTs’ electrocatalytic properties. A platinum wire microelectrode (ME) was corroded using aqua regia and subsequently embedded with MWCNTs to achieve more active sites, producing a so-called powder microelectrode (PME). Compared with conventional MEs, the PME has a larger specific surface area and more active sites. When PME was used to detect ascorbic acid (AA), the AA oxidation potential shifted negatively and current peak was visibly increased. The calibration curve obtained for AA was in a range of 5.00 × 10−6~9.50 × 10−4 mol·L−1: Ipa(μA) = 3.259 × 10−2 + 1.801 × 102 C (mol·L−1) under the optimum testing conditions. Moreover, the detection and quantitation limits were confirmed at 4.89 × 10−7 mol·L−1 and 1.63 × 10−7 mol·L−1, respectively. When the fabricated PME was practically applied to detect AA, it was shown a recovery rate of 94~107% with relative standard deviation (RSD) <5%. The proposed strategy thus offers a promising, rapid, selective and low-cost approach to effective analysis of AA.

Highlights

  • Ascorbic acid (AA) is an acid compound containing six carbon atoms and hydroxy groups, which is considered a natural organic acid AA has no carboxyl group [1]

  • The potential pulse excitation signal was sent to the dual-electrode sensor system via the electrochemical workstation, so that the AA-sensing electrode was in real-time controlled at Sensors 2017, 17, 1549states

  • AA, an apparent peak pattern was obtained. Compared to those of DMF/carboxyl/Multi-walled carbon nanotubes (MWCNTs)/ME, peak current increased by 5.65 times and the peak potential was shifted to −0.020 V on the powder microelectrode (PME)

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Summary

Introduction

Ascorbic acid (AA) is an acid compound containing six carbon atoms and hydroxy groups, which is considered a natural organic acid AA has no carboxyl group [1]. As an improvement on macroelectrodes, microelectrodes (MEs) were introduced into the field of electrochemical analysis because of their small time constants, large diffusion speed and other advantages. When it comes to practical applications, MEs’ sensitivity do not achieve the desired effect. MWCNTs, functionalized with carboxyl groups by pretreatment with strong mixed acid, were embedded into MEs for fabricating PMEs. a two-electrode electrochemical system was constructed to detect AA based on its direct oxidation on the electrode surface using the PME as bass electrode and a platinum plate electrode as reference electrode

Chemicals
Apparatus
Construction of Sensor System
Fabrication of PME
Working
TEM of MWCNTs
FT-IR of MWCNTs
Effect
Influence
Effect of Sweep Rates on AA Detecting
Determination of AA
Interference Study
Sample Analysis
Repeatability and Stability of the PME
Conclusions

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