Ultrasensitive Electroanalytical Detection of Pb2+ and H2O2 Using Bi and Fe—Based Nanoparticles Embedded into Porous Carbon Xerogel—The Influence of Nanocomposite Pyrolysis Temperatures
Abstract
:1. Introduction
2. Results and Discussion
2.1. Morphological and Structural Characterization
2.1.1. Pyrolysis-Induced Changes in the Crystalline Structure
2.1.2. Effects Induced at Micro- and Nano-Scales
2.2. Electrochemical Behavior of GC/Chi-(CXBiFe-T) Modified Electrodes
2.2.1. EIS Measurements
2.2.2. Square Wave Voltammetry Measurements for H2O2 Detection
2.2.3. Square Wave Anodic Stripping Voltammetry Measurements for Pb2+ Detection
2.2.4. Correlations between the Morphological and Structural Characteristics and the Electroanalytical Behavior of BiFe-Carbon Xerogel Nanocomposites Modified Electrodes
Conductivity and Porosity
Nanoparticle Activation and Spatial Statistics of Diffusion Domains
2.2.5. Sensor—Long-Term Stability and Repeatability
2.2.6. Real Sample Analysis
3. Conclusions
4. Materials and Methods
4.1. Reagents
4.2. Synthesis and Temperature Program for CXBiFe-T Xerogel Ternary Composite
4.3. Characterization Methods
4.4. Preparation of the GC/Chi-(CXBiFe-T) Electrodes
4.5. Electrochemical Measurements
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Sample | dXRD (nm) | ID1/IG1 | SBET (m2/g) | DDLS (nm) | C/O/Bi/Fe (at%) | dnp (nm) | DV (nm) | |||
---|---|---|---|---|---|---|---|---|---|---|
Bi2O3 | Bi | Fe2O3/Fe3O4 | γ-Fe | |||||||
OXBiFe | - | - | - | - | 0.86 | 10 | - | 74.0/25.5/0.2/0.2 | - | - |
CXBiFe-600 | 33 | - | - | - | 0.72 | 229 | 1400 | 93.6/5.6/0.4/0.5 | 18 | 119 |
CXBiFe-750 | 45 | - | 14 | - | 0.97 | 146 | 740 | 95.2/3.8/0.5/0.5 | 21 | 128 |
CXBiFe-900 | - | 18 | 13 | 13 | 1.46 | 91 | 655 | 92.3/7.1/0.3/0.3 | 29 | 129 |
CXBiFe-1050 | - | 22 | 18 | 13 | 1.70 | 16 | 570 | 94.4/4.8/0.1/0.7 | 33 | 154 |
Electrode Type | GC | GC/Chi-CXBiFe-600 | GC/Chi-CXBiFe-750 | GC/Chi-CXBiFe-900 | GC/Chi-CXBiFe-1050 |
---|---|---|---|---|---|
Rel (Ω cm2) * | 5.98 ± 3 | 7.98 ± 0.9 | 22.6 ± 2.5 | 6.65 ± 1.5 | 12.2 ± 2.6 |
CPE (µS sn/cm2) * n * | 25.2 ± 6 0.87 ± 1.0 | 84.1 ± 1 0.74 ± 0.22 | 58.2 ± 11 0.76 ± 2.1 | 50.2 ± 4 0.75 ± 0.79 | 40.9 ± 8 0.78 ± 1.4 |
Rct (kΩ cm2) * | 6.2 ± 2 | 3.93 ± 1.6 | 1.5 ± 15.6 | 1.25 ± 5.4 | 0.91 ± 4.3 |
W (mS s1/2/cm2) * | 4.89 ± 5 | 0.38 ± 1 | 0.30 ± 6.7 | 0.76 ± 3.6 | 1.05 ± 3.7 |
C (µF/cm2) | 13.3 | 56.6 | 26.4 | 19.5 | 16.5 |
χ2 | 0.003716 | 0.0002446 | 0.007471 | 0.002048 | 0.005647 |
Electrode Type | Peak Potential (V*) | Linear Range (mM) | Sensitivity (µA/mM) | Detection Limit (µM) | Ref. |
---|---|---|---|---|---|
(Fe-CA)-CPE | −0.3 | 1–50 | 1.78 | 500.0 | [9] |
α-Fe2O3NP|FePO4 | −0.3 | 1.66–4.95 | 225.00 | 3.4 | [28] |
Fe3C/NG | −0.6 | 0.05–15 | 9.44 | 35.0 | [29] |
Fe-NGCs | −0.3 | 0.001–5 | 13.30 | 0.5 | [30] |
GC/Chi-BiFeCX | −0.3 | 0.005–0.05 | 1860.00 | 4.8 | [19] |
GC/Chi-CXBiFe1.2 | −0.3 | 0.003–0.03 | 2350.00 | 0.2 | [18] |
GC/Chi-(CXBiFe-900) | −0.50 | 0.05–1 | 2.10 | 5.7 | This work |
GC/Chi-(CXBiFe-1050) | −0.46 | 0.05–1 | 4.55 | 2.5 |
Electrode Type | Peak Potential (V*) | Linear Range | Sensitivity (µA/µM) | Detection Limit (pM) | Ref. | |
---|---|---|---|---|---|---|
µM | pM | |||||
GC/AlOOH-rGO | −0.6 | 0.2–0.8 | 3.5 | 93.20 | [31] | |
Au/[Ru(bpy)3]2+-GO | −0.38 | 0.1–1.5 | 24.1 | 35.00 | [32] | |
Fe3O4/Bi2O3/C3N4/GC | −0.5 | 0.01–3 | 82.5 | 103 | [33] | |
NiO/rGO/GCE | 0.03–0.6 | 92.8 | 104 | [34] | ||
GC/Chi-(BiCX)Imp | −0.55 | 1–10 | 1.1 × 06 | 0.36 | [15] | |
GC/Chi-(BiCX)Cos | −0.56 | 1–10 | 1.3 × 106 | 0.28 | [16] | |
GC/Chi-(BiCA)Cos | −0.44 | 1–10 | 2.3 × 105 | 0.48 | [16] | |
GC/Chi-(CXBiFe0.01) | −0.58 | 1–10 | 1.0 × 106 | 0.56 | [18] | |
GC/Chi-(CXBiFe-600) | −0.53 | 10–90 | 2 × 104 | 6.19 | This work | |
GC/Chi-(CXBiFe-750) | −0.48 | 10–110 | 4.9 × 104 | 5.67 | ||
GC/Chi-(CXBiFe-900) | −0.44 | 1–12 | 2.5 × 105 | 0.30 | ||
GC/Chi-(CXBiFe-1050) | −0.40 | 0.5–10 | 9.2 × 105 | 0.09 |
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Rusu, M.M.; Fort, C.I.; Vulpoi, A.; Barbu-Tudoran, L.; Baia, M.; Cotet, L.C.; Baia, L. Ultrasensitive Electroanalytical Detection of Pb2+ and H2O2 Using Bi and Fe—Based Nanoparticles Embedded into Porous Carbon Xerogel—The Influence of Nanocomposite Pyrolysis Temperatures. Gels 2023, 9, 868. https://doi.org/10.3390/gels9110868
Rusu MM, Fort CI, Vulpoi A, Barbu-Tudoran L, Baia M, Cotet LC, Baia L. Ultrasensitive Electroanalytical Detection of Pb2+ and H2O2 Using Bi and Fe—Based Nanoparticles Embedded into Porous Carbon Xerogel—The Influence of Nanocomposite Pyrolysis Temperatures. Gels. 2023; 9(11):868. https://doi.org/10.3390/gels9110868
Chicago/Turabian StyleRusu, Mihai M., Carmen I. Fort, Adriana Vulpoi, Lucian Barbu-Tudoran, Monica Baia, Liviu C. Cotet, and Lucian Baia. 2023. "Ultrasensitive Electroanalytical Detection of Pb2+ and H2O2 Using Bi and Fe—Based Nanoparticles Embedded into Porous Carbon Xerogel—The Influence of Nanocomposite Pyrolysis Temperatures" Gels 9, no. 11: 868. https://doi.org/10.3390/gels9110868