Abstract
We have synthesized metal phthalocyanine modified multiwalled carbon nanotube by a solid-phase synthesis method by heating a reaction mixture of phthalic anhydride, ammonium molybdate and MWCNT in a required molar ratio using muffle furnace. The metal phthalocyanine modified MWCNT samples collected and then washed extensively with various solvents to removal all impurities and unreacted starting materials. The resulting nanocomposite was characterized by IR, UV-Visible spectroscopy, Scanning Electron Microscopy, X-ray diffraction and Raman spectroscopy. The nanostructure of the CuPc/MWCNT assembly exhibits a homogeneous nanocomposite. The electrocatalytic study of the CuPc/MWCNT assembly towards the oxidation of nitrite was investigated. An enhanced oxidation peak current was noted with lowering oxidation over potential ranges. The proposed method can be applied for the amperometry detection of nitrite present in food samples.
Publisher
Trans Tech Publications, Ltd.
Reference27 articles.
1. An XPS spectrum corresponding to N1s peak is shown Figure 5a. De convoluted spectra show that main peak is located at 400. 1 eV, whereas the peak located at 399. 39 eV corresponds to the binding energy of nitrogen atoms in C–N=C bonds. Figure 5b shows the two strong peaks at 931. 3 and 951. 2 eV correspond to the electron states of Cu2p3/2 and Cu2p1/2, respectively. Figure 5c shows the O1s peak of 532. 9 eV as compared to the XPS spectra of O1s of AF-MWCNTs (532. 1eV), the CuPc/MWCNTs peak slightly shifted to the low binding energy. This may be attributed to the formation of hydrogen bonds. It is clear from the results that a significant shift of the main peaks of CuPc has taken place in CuPc/MWCNT sample which ensures the proper attachment of CuPc on MWCNT. The SEM analysis shows that the nanocomposite CuPc/MWCNTs displays one-dimensional nanocrystals connected by MWCNTs. The variable size of MWCNT of 94. 1, 121, 126, 149, 188, 219 and 238 nm confirms the deposition of CuPc over MWCNT and present as a nanocomposite. The morphology, dimensions and orientation of CNTs can be easily revealed by using scanning electron microscopy (shown in Figure 6a [22-24]. B A C Fig. 6 SEM image of (a) CNT, (b) CuPc/MWCNT, (c) EDAX spectrum of CuPc/MWCNT Fig. 6 (A) Cyclic voltammogram for Bare GCE (a), NO2-/GCE (b) and CuPc-MWCNTGCE(c); B) The effect of concentration on oxidation of nitrite (range 0. 13 mM to 0. 66 mM) in 0. 1M Potassium Chloride solution . (C) The effect of scan rate for nitrite oxidation from 25-100 mV s-1 in KCl solution. (D) Differential pulse voltammogram for different concentration of nitrite ranging from 0. 6 mM to2. 3 mM in Potassium Chloride solution A higher magnified image of CuPc/MWCNT is shown in Figure 6b. For the clear understanding of the attachment, a closer view of the material which shows that the walls of each individual nanotube are coated with CuPc by varying thickness [16, 19]. The CuPc attachment over MWCNT increased the wall diameter of the nanotubes are 94. 1, 121, 126, 149, 188, 219, 238. The presence of each element in the CuPc/MWCNT samples was examined by using EDAX (Fig. 6c). The electrochemical behavior of CuPc/MWCNT nanoparticles was studied using 0. 1 M potassium chloride electrolyte and the resulting catalytic response is shown in Fig. 8. An oxidation peak of nitrite ion was detected at Ep = 0. 76 V and no cathodic current is observed in this potential range during the reverse cycle. The principal product formed in the first charge transfer reaction.
2. is due to the formation of nitrate. The cyclic voltammograms was recorded at various scan rates for a fixed concentration of nitrite. A linear relationship between the peak current (Ip) and concentration of nitrite was observed which indicates the oxidation process is a diffusion controlled process. CONCLUSION The nanocomposites of CuPc/MWCNT were prepared by a solid-phase synthesis method. This method is more efficient and can be used for large-scale preparation. The morphologies feature of the CuPc/ MWCNTs nanocomposite was established from SEM and XRD results. The assembly of CuPc/MWCNTs displays one-dimensional nanocrystals interconnected by MWCNT. Such a nanocomposite film modified electrode can be utilized for the electrochemical oxidation and trace level detection of nitrite. A similar type of nanocomposites can be used for various applications and explored in future. REFERENCS.
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