Electrochemical Activation of Graphite Nanosheets Decorated with Palladium Nanoparticles for High Performance Amperometric Hydrazine Sensor

Abstract

Herein, we have demonstrated a preparation of palladium nanoparticles on electroactivated graphite nanosheets modified screen printed carbon electrode (PdNPs‐EGNS/SPCE) by a simple electrochemical method. The well‐prepared electrocatalyst was potentially applied to the high performance electrocatalytic oxidation of hydrazine in neutral medium. The PdNPs‐EGNS novel composite was characterized by scanning electron microscope (SEM) and the average diameter and thickness of PdNPs and EGNS were found to be ∼38 nm and 85 nm, respectively. The high performance electrocatalytic determination of hydrazine was performed by the amperometric i‐t method. The fabricated sensor displayed irreversible electrocatalytic oxidation of hydrazine with diffusion‐controlled electrode process. The oxidation of hydrazine at PdNPs‐EGNS/SPCE showed wider linear range 0.05–1415 µM and high sensitivity 4.382 µA µM−1 cm−2. The as‐prepared electrocatalyst achieved quick response towards hydrazine with a lower detection limit 4 nM.

Screen-Printed Electrodes Modified with Metal Nanoparticles for Small Molecule Sensing

“…The parameters usually optimized are separated in two main groups: The ones related to the precursor solution where the salt type and concentration are involved, and the conditions of electrochemical deposition. A list of usual salts employed are AgNO 3 [30][31][32][33][34] for silver NPs; HAuCl 4 [31,35,36] and AuCl 3 [37] for gold NPs; Bi(NO 3 ) 3 [16,38,39] for bismuth NPs; CoCl 2 [40] for cobalt NPs; CuCl 2 [41], CuSO 4 [42], and CuNO 3 [43,44] for copper NPs; NiCl 2 [40,45] and NiSO 4 [46,47] for nickel NPs; PdCl 2 [48][49][50] [30,[52][53][54][55][56], and PtCl 2 [37] for platinum NPs; RhCl 3 [57] for rhodium NPs, etc. Although higher concentrations of precursor allow bigger particles to be obtained, the size and shape are usually controlled electrochemically; so, the precursor concentration usually tends to be high enough to have sufficient material susceptible to be deposited and it is not often optimized [33].…”

“…Cyclic voltammetry is also employed for electrodeposition, but control is more difficult because more parameters need to be optimized, such as the scan rate, scan cycles, and potential window. Published works that use this technique with noble metals are mainly focused on the novelty of the substrates employed like graphite nanosheets [49], carbon nanotubes [55], fullerenes [48], graphene [46], and graphene oxide [59] than electrodeposition itself.…”

“…In addition, hydrogen was also tested in a proof-of-concept assay, making possible the application of palladium-based SPE sensors as gas detectors [12]. Although no real samples were assayed in this work, subsequent publications based on carbon nanomaterial substrates were successfully applied to monitor dopamine in pharmaceuticals [48] and hydrazine in wastewater samples [49]. Electrodeposition of rhodium NPs also gives rise to a good platform to detect bromide in seawater and pharmaceuticals [57].…”

Functionalization of Reduced Graphene Oxide with β‐cyclodextrin Modified Palladium Nanoparticles for the Detection of Hydrazine in Environmental Water Samples

“…Our hydrazine sensor achieved a wider linear sensing range from 0.05 to 1600 μM, which is higher than the other PdNPs/carbon or other materials based hydrazine sensors. For instance, PdNPs/rGO; 0.1–1000 μM , nano Pd/MWCNT; 0.1–10 μM , Pd/CILE; 5–800 μM , PdNPs/EGNS; 0.05–1415 μM , PdNPs/MWCNT‐Nafion; 2.5–700 μM , AuPd/GR; 2–185 μM , PdNPs‐EDAC; 5–150 μM , and AuPdCu/MWCNT; 0.1–306 μM have shown lower linear range than PdNPs‐β‐CD/rGO hybrid based sensor. On the other hand, some PdNPs based composite modified hydrazine sensors showed very high linear range and lower detection limit than our proposed sensor; however, these sensors also displayed some limitation such as poor sensitivity, detection limit and critical synthesis procedure (high temperature and strong reducing agent has been used) .…”

“…Numerous methods were extensively studied to detect the hydrazine such as high‐performance liquid chromatography, spectrophotometry, gas chromatography‐mass spectrometry, coulometry and electrochemical method . Among these techniques, electrochemical method is suitable platform for the determination of hydrazine owing to their portability, low‐cost, simple and rapid detection with high sensitivity and reproducibility . On the other hand, direct oxidation of hydrazine is difficult on commercially available electrodes due to their poor electron transfer behavior and higher oxidation potential .…”