Monitoring of Alizarin Red S (an environmental toxic dye) Using Cu-Ni Bimetallic Hybrid Nanoparticles Synthesized with Various Rations

doi:10.21203/rs.3.rs-4116715/v1

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Research Article

Monitoring of Alizarin Red S (an environmental toxic dye) Using Cu-Ni Bimetallic Hybrid Nanoparticles Synthesized with Various Rations

https://doi.org/10.21203/rs.3.rs-4116715/v1

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The development of novel nanomaterials opens the windows of research in several areas. However, its optimal synthesis and characterization is a challenging task for its performance in specific fields of use. Cu-Ni bimetallic hybrid alloy nanoparticles were manufactured by reinforcing Cu with Ni using ethylene glycol as a solvent as well as a reducing agent, and polyvinyl pyrrolidon as a fabrication material, for sensing application. UV-Vis spectroscopy, steady-state fluorescence, Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and energy-dispersive spectroscopy (EDS) techniques were used for the confirmation and morphological studies of synthesized nanoparticles. Results display that Cu portrays enhanced characteristics. SEM shows outstanding topographic properties for Cu-Ni bimetallic hybrid nanoparticles. A composite electrode of Cu-Ni/PVP/GCE (Cu-Ni NPs based electrochemical sensor) is developed by coating Cu-Ni (3:1) hybrid nanoparticles embedded in polyvinyl pyrrolidone (PVP) at the surface of cleaned Glassy Carbon Electrode (GCE). The lowest possible concentration of Alzarin Red S (0.12 µM) was detected by using Cu-Ni bimetallic hybrid nanoparticles based electrochemical sensor.

Cu-Ni bimetallic nanoparticles

Poly vinyl Pyrrolidon (PVP)

ethylene glycol

electrochemical sensor

Alzarin Red S

There are plenty of uses of nanoparticles (NPs) in different domains of life. Whether they are monometallic or bimetallic, NPs exhibit useful characteristics that support our work in a variety of scientific domains. Their form and size were ascribed to these distinctive characteristics [1]. Because of their distinct physicochemical characteristics in comparison to monometallic nanoparticles, bimetallic nanoparticles (BNPs) have garnered the interest of scientists and technologists in recent years [2]. The characteristics of BNPs are dependent on their size, content, and shape [3]. By detecting other species in their surroundings, bimetallic alloy nanoparticles' (BANPs) surface physiochemical characteristics can vary, which can aid in the detection of hazardous and cancer-causing chemicals such volatile organic compounds. To monitor one of the dangerous and environmental poisons PAHs, Cu-Ni bimetallic hybrid nanoparticles (BHNPs) may be utilized [4]. As a result, Cu-Ni BHNPs-based sensors can be created.

Cu and Ni BHNPs’ unique surface has been functionalized, and this has been used in electrochemical sensors, electronics/electro-optical devices, biosensing, catalysis, and electronics/electro-optical devices [5–7]. Cu and Ni NPs and their nanoalloys are employed as sensors because of their distinctive characteristics [8–12].

Many NPs have been thoroughly investigated for their potential as electrochemical sensors. Nevertheless, there hasn't been much research done on Cu-Ni-BHNPs based electrochemical sensing applications. Additionally, because Cu and Ni NPs are less expensive than other pricey metals like gold, platinum, etc., they provide excellent candidates for the fabrication of electrochemical sensors [13, 14]. According to one publication, exposure to an open environment poses a significant obstacle to the use of Cu NPs in the manufacture of sensors. By suggesting Cu and Ni BHNPs that regulated the decomposing action, this problem was resolved [15].

Using chemical reduction methods, a variety of electrochemical sensors based on Cu-Ni bimetallic alloys are meticulously constructed in the current research work. Ultimately, CV and electrochemical impedance spectroscopy (EIS) methods were used to examine the electrochemical sensing properties of the different test samples of BHNPs. Cu-Ni (3:1) BHNPs has demonstrated the highest sensing performance among all test samples when it comes to the detection of the worst environmental pollutants and carcinogenic dye Alizarin Red S (ARS).

2.1. Method and Materials

All of the compounds used to conduct the present research work were of research standard and didn't require any additional purification. Different chemicals used during study included Nickle nitrate (NiNO₃.6H₂O), Copper (II) nitrate trihydrate (Cu(NO₃)₂.3H₂O), Polyvinylpyrrolidone (PVP) MW = 10,000g and ethylene glycol. All glassware was previously washed with HCl solution and then repeatedly rinsed with distilled water.

2.2. Cu and Ni Nanoparticles Synthesis

To prepare 10 mM copper ions in solution, 30 mL of ethylene glycol was mixed with the necessary amount of Cu(NO₃)₂.3H₂O. A 1 mM PVP solution was prepared in another flask by dissolving a precisely estimated quantity of PVP-10,000 in 30 mL of ethylene glycol and stirring the mixture for 10 minutes. 10 mL of Cu(NO₃)₂.3H₂O (10 mM) and 10 mL of PVP (1 mM) were combined for the production of Cu nanoparticles while being continuously stirred and heated to 150°C for 15 minutes.

To prepare 10 mM nickle ions in solution, 30 mL of ethylene glycol was mixed with the necessary amount of NiNO₃.6H₂O. A 1 mM PVP solution was prepared in another flask by dissolving a precisely estimated quantity of PVP-10,000 in 30 mL of ethylene glycol and stirring the mixture for 10 minutes. 10 mL of NiNO₃.6H₂O (10 mM) and 10 mL of PVP (1 mM) were combined for the production of Cu nanoparticles while being continuously stirred and heated to 150°C for 15 minutes.

2.3. Cu-Ni Nanoalloys Synthesis

5 mL of Cu(NO₃)₂.3H₂O solution (1 mM) was mixed with 5 mL of NiNO₃.6H₂O solution (10 mM) and 5 mL of PVP (1 mM) to create Cu-Ni bimetallic hybrid nanoparticles (BHNPs). For thirty minutes, the solution was stirred continuously. For thirty minutes, the colloidal mixture was heated to a steady temperature of 175°C.

3.1. UV/ Visible spectroscopy

Since Ni and Cu NPs have been reported to produce surface plasmon response (SPR) bands within that particular range, a UV-visible spectrum was obtained between 350 and 800 nm [16]. These surface charge oscillations are quantized and are caused by an external electric field. Fascinating optical characteristics are produced by SPR stimulated metal nanoparticles. With UV-Vis Spectroscopy, these resonances may be examined in bulk solution [17]. The size, shape, and kind of particles, together with the solvent used in the synthesis, all have an impact on the SPR peaks; the wider the bandwidth of an SPR band, the smaller the nanoparticle size. The UV-visible spectra may be quantitatively analyzed to get information on the structural characteristics of the NPs [18].

The UV/visible spectrum of Cu NPs' is depicted in Fig. 1A with the highest absorption peak at 580 nm, which is quite similar to the value of 575 nm reported in the literature [19]. The UV/visible spectrum of nickel NPs, with a maximum absorption at 275 nm, is displayed in Fig. 1B. According to the observed data, there is a larger absorbance peak at around 275 nm, and the distinctive peak of SPR appears in the spectrum at 365 nm as a little shoulder, revealing that the nickel salt solution has been converted to Ni NPs [20].

The UV-visible spectra of Cu-Ni BHNPs created in different ratios, such as 1:1, 2:1, and 3:1, exhibit a red shift as the content of Cu increases. Cu-Ni BHNPs have been generated as shown by Fig. 1C, as proven by the existence of a single uv/visible absorbance peak at these wave lengths, which are between 275 nm (for pure nickel) and 575 nm (for pure copper). This demonstrates that the produced NPs were alloys rather than mixtures of elemental NPs [19–20].

Figure 2a.shows the UV/visible spectra of 1:1 Cu-Ni BHNPs having maximum absorbance at 431 nm and the absorbance vs concentration plot of Cu-Ni (1:1) BHNPs which gives a straight line with slope giving molar absorptivity equal to 77.26 liters/mole.cm this shows the data is following beer lambert law.

$$A= \in Cl$$

Figure 2b shows the UV/visible spectra of 1:2 Cu-Ni BHNPs having maximum absorbance at nm. The absorbance value got decreased as the colloidal solution is diluted and get vanished at 450 concentrations. Figure 2b also shows the absorbance vs concentration plot of Cu-Ni (1:2) BHNPs which gives a straight line with slope giving molar absorptivity equal to 54.6 liters/mole.cm hence the data is obeying beer lambert law.

Figure 2c shows the UV/visible spectra of Cu-Ni 3:1 BHNPs having maximum absorbance at 500 nm. The Fig. 2C also reflects the beer lambert law plot of Cu-Ni (1:3) BHNPs which gives a straight line with slope giving molar absorptivity equal to 94.5 liters/mole.cm.

The result obtained from uv/visible spectroscopic analysis of mono and BHNPs of Cu and Ni combined in 1:1, 1:2 and 3:1 mole ratio are depicted in Table 1.

Table 1

Parameters obtained from Uv/visible spectra of Cu, Ni, and Cu-Ni alloy nanoparticles with different mole ratio.
S. No.	Nanoparticle
1	Cu	575	-----
2	Ni	275	-----
3	Cu-Ni (1:1)	500	77.26
4	Cu-Ni (2:1)	450	54.5
5	Cu-Ni (3:1)	431	94.5

Table 2

Parameters obtained from fluorescence emission spectra of Cu-Ni at different mole ratio
N		K_sv (M^− 1)		N		Kb		∆G_b (kJ.mol^− 1)
491	210		1.67		184.93		12.93

As clear from Table 1 the value of molar absorptivity is highest for Cu-Ni ratio 3:1. So Cu-Ni BHNPs are selected for farther analysis.

3.2. Fluorescence spectra of Cu-Ni BHNPs

Figure 3a graphically explain fluorescence emission spectra of Cu-Ni BHNPs at varying mole fraction of Cu. Copper and nickel nanoparticles in a physically mixed solution exhibit two different emission spectra, while the BHNPs have a single emission peak, confirming the synthetic process. The maximum intensity peaks appear at 612 to 617 with red shift and decline in fluorescence intensity with rise in the mole fraction of Cu in the Cu-Ni BHNPs samples, thus Cu acts as quencher.

The concentration of the sample and quencher influences the intensity both in the presence and absence of the quencher.

$$ln\frac{{I}_{o}}{{I}_{Q}}=\frac{\left[Q\right]N}{\left[X\right]}$$

Where quencher concentration is represented by [Q], while sample molar concentration by [X]. N is the estimated number of atoms in the nanoparticle. Io and I_Q express the emission intensity in the absence and presence of quencher. Plotting logI_o/I_Q versus [Q]/[X] is shown in Fig. 3b. The value of N is 491 calculated from the slope.

At low concentration the quenching of fluorescence in solution follow classical Stern-Volmer equation [22].

$${(I}_{o}-{I}_{Q})/{I}_{Q}={K}_{sv}[Q]$$

Where K_sv is stern-volmer constant or quenching constant. The slope of (I_o-I_Q)/IQ versus [Q] yield the quenching constant, which is computed and displayed in Fig. 3c. The value of quenching constant or stern-volmer constant obtained from plot is 210 M^-1.

To find binding constant, binding energy and approximate number of binding sites logarithmic form of modified stern-volmer equation is used given below [23].

$$\frac{\text{log}\left({I}_{o}-{I}_{Q}\right)}{{I}_{Q}}=\text{log}{K}_{b}+ \text{nlog}\left[Q\right]$$

Where n represent the total amount of binding sites estimated by the slope of $\frac{\text{log}\left({I}_{o}-{I}_{Q}\right)}{{I}_{Q}} vs \text{l}\text{o}\text{g}\left[Q\right]$, K_b is binding constant obtained from intercept of the curve. Binding energy ∆G_b is calculated from K_b using following equation.

$$\varDelta {G}_{b}= -RTln{K}_{b}$$

Figure 3d shows plot of modified stern volmer. The value of nobtained from plot is 1.67 while k_b calculated from intercept is 184.93 while binding energy calculated from intercept is 12.93 kJ/mole.

3.3. Characterizations of Cu-Ni BHNPs

Figure 4 shows SEM images of Cu-Ni BHNPs having 1:1, 2:1 and 3: 1 mole ratio. The average particle sizes calculated from SEM images are 35nm for Cu-Ni (3:1) 64nm for Cu-Ni (2:1) and 95nm for Cu-Ni (1:1). It is clear from images that Cu-Ni (3:1) show smaller and more uniform particle size [24].

Figure 5 shows EDX spectra of Cu-Ni BHNPs having 1:1, 2:1 and 3:1 composition. The existence of Ni and Cu peaks in the EDX results and lack of any other distinctive peaks indicates their presence in NPs. Therefore, these results provide strong proof that the Cu-Ni BHNPs are pure and devoid of any additional constituents [25]. As we increase the mole ratio of Cu in nanoparticles the Cu peak in spectra enhances while the Ni peaks show a corresponding decrease. Hence the outcomes of EDX analysis correspond with the mole ratios of Cu²⁺ to Ni²⁺ used in the creation of nanoparticles.

The X-ray diffraction pattern was utilized to diagnose the structural phases of Cu-Ni BHNPs. Figure 6 displays the XRD patterns of the 1:1, 2:1 and 3:1 compositions synthetic Ni-Cu BHNPs. Plot of x-rays intensity vs 2θ give sharp peaks which confirms the crystalline nature of NPs. Sharp and intense diffraction peaks at 2θ appeared at 40.9°, 49.9°, and 75.85º, corresponding to the (111), (200), and (220) planes. These peaks suggested the creation of pure cubic Cu − Ni BHNPs [24–25]. An advancing (red) shift of the Bragg peaks to lesser diffraction angles takes place as the Ni content decreases which are in accordance with result reported in literature [25]. Scherrer's formula was used to compute the average crystallite size, from the diffraction peaks was found to be 35 − 49 nm for Ni − Cu BHNPs and particle size decreases as Cu composition is increase [26, 27].

3.4. Electrochemical applications of Cu-Ni BHNPs

The CV studies indicated that dye shows irreversible cyclic voltammetric behaviour of Cu-Ni BHNPs having compositions 1:1, 2:1 and 3:1 as displayed in Fig. 7. Figure 7 shows cyclic voltamograms of bare GCE electrode, Polyvinyl pyrrolidon (PVP) modified GCE electrode, Cu-Ni (1:1, 2:1 and 3;1) BHNPs modified GCE electrode and Cu-Ni(3:1)-PVP modified GCE electrode showing well-defined peaks at 0.29 mV for BHNPs modified electrodes as shown in Table 3. The PVP-Cu-Ni framework makes easier the electron transfer of dyes, which substantially boosts the reduction current [28].

Table 3

Ip and Ep value of different electrodes obtained from cyclic voltamogram
S. No.	Nanoparticle	I_p (mA)	E_p(V)
1	PVP/GCE	0.013	0.3
2	Cu-Ni (1:1)/GCE	0.03	0.28
3	Cu-Ni (2:1)/GCE	0.045	0.285
4	Cu-Ni (3:1)/GCE	0.07	0.291
5	PPy-Cu-Ni (3:1)/GCE	0.075	0.29

It is clear from the value of Ip obtained which is highest for PVP-Cu-Ni BHNPs modified electrode (0.08 mA) hence giving best sensitivity for detection of Alizarin red S as compare to bare GCE and Cu-Ni BHNPs modified GCE electrode.

SWV was used to examine the PVP-Cu-Ni (3:1) /GCE performance under idealized circumstances. Figure 8a displays the recorded voltammograms with ARS concentrations ranging from 10 µM to 1µM. In accordance with IUPAC recommendations, the developed sensor's Alizarin red S limit of detection (LOD) was determined [29]. The blank solution's peak current data were used to compute the standard deviation for PVP-Cu-Ni(3:1)/GCE. PPy-Cu-Ni(3:1)/GCE is a promising method for microscopic level tracing of selected dye, as evidenced by the limit of detection (LOD) value of ARS of 0.2 µM. The limit of quantification (LOQ) value is also calculated which 0.12 µM.

Experiments on the reproducibility and repeatability of the developed sensor verified its validity. As seen in Fig. 8a, voltammograms were obtained under ideal circumstances after four electrodes were similarly changed for this purpose. Similar peak current readings on the ARS show that the proposed sensor has high repeatability, with an RSD of less than 5%. As seen in Fig. 8b, a repeatability experiment including several measurements on the same electrode at various time intervals revealed that the PVP-Cu-Ni/GCE was stable, with an RSD < 5%.

Electrochemical impedance spectroscopy (EIS), provides important details on the characteristics of charge transport at the sensor surface. In a 5 mM K₃[Fe(CN)₆] redox probe in 0.1 M KCl electrolyte, the EIS measurement of GCE and Cu-Ni BHNPs modified GCE was performed at 14 kHz to 1 Hz frequency range.

The bare and modified GCE's Nyquist charts are displayed in Fig. 9. However, PVP modified GCE shows smaller semicircle than bare GCE due to electron transfer facilitation offered by conducting polymer PVP. The largest semicircle diameter of bare GCE compared to Cu-Ni/GCE exhibit a rapid charge transfer process at modified electrode as compare to bare electrode. The smallest semicircle is evidenced by GCE modified by PVP as well as Cu-Ni (3:1) BHNPs called composite electrode of electrochemical sensor indicates that Cu-Ni BHNPs further improve the electron transfer mechanism and retards the resistance to electrons, and thence the target dye (Alzarin Red S was easily sensed with its lowest concentration in aqueous media. The R_ct values obtained for PVP-Cu-Ni/GCE ((2.18 kΩ) is lowest than that for bare GCE (8.51 kΩ) and GCE modified with PVP (8.1 kΩ) and Cu-Ni (3:1) BHNPs (4.75 kΩ) alone. Due to a larger electroactive surface area, the developed sensor's optimal charge transport is shown by a reduced Rct value for Cu-Ni/GCE [29]. The modifier serves as a conduit between the sensor and the substance being tested, giving the bare GCE improved electrical characteristics [30]. Rct and other EIS parameters were computed using the Randles equivalent circuit, which is depicted in Table 4. The informations resulted from EIS strongly supports the results of CV and SWV.

Table 4

Summary of Rct value of Bare GCE and GCE modified with PPy, Cu-Ni(3:1) and PPy-Cu-Ni(3:1)
S. No.	Nanoparticle	R_ct (kΩ)
1	Bare GCE	8.51
2	PPy/GCE	8.1
3	Cu-Ni(3:1)/GCE	4.75
4	PPy-Cu-Ni (3:1)/GCE	2.18

Cu-Ni BHNPs were synthesized via polyol method. Spectroscopic study of nanoparticles shows that the wave length of maximum absorbance for Cu-Ni BHNPs is between the wave length maximum of Cu and Ni monometallic NPs with red shift with increase in Cu mole ratio. Fluorescence spectra of Cu-Ni BHNPs shows that Cu act as quencher and emission intensity decreases with increase in Cu mole ratio. An environmental friendly method was developed for the detection of Alizarin red S using synthesized of Cu-Ni BHNPs. PPy was used as capping as well as sensing detector. The electrochemical catalytic behavior of Cu-Ni BHNPs was found to depend on the Cu:Ni molar ratio. Cu-Ni (3:1) BHNPs exhibited higher I_p and lower R_ct value than the other Cu-Ni BHNPs which make it best choice. It is anticipated that the designed electrochemical sensor can successfully be applied for the detection of Alizarin red S in industrial waste water with LOD value of 0.2µM. These results revealed that GCE modified with Cu-Ni (3:1) BHNPs are the best to monitor Alizarin red S at its lowest possible concentration in aqueous medium.

Author Contribution

All authors written in the list have equal contribution in this manoscript and and no one is claiming any finencial intersst.

Acknowledgments

This work was jointly supported by Institute of Chemical Sciences University of Peshawar and National Center of Excellence in Physical Chemistry University of Peshawar. The financial support of Higher Education Commission of Pakistan and Islamia College Peshawar is also acknowledged.

It is stated that the manuscript entitled Monitoring of Alizarin Red S (an environmental toxic dye) Using Cu-Ni Bimetallic Hybrid Nanoparticles Synthesized with Various Rations is a novel research. The authors declare no competing financial interest. The coauthors have contributed equally and their contributions has been highlighted by writing their names at the start. All the authors have been informed during writing and submission of this article.

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No competing interests reported.

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Monitoring of Alizarin Red S (an environmental toxic dye) Using Cu-Ni Bimetallic Hybrid Nanoparticles Synthesized with Various Rations

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Abstract

Figures

1 Introduction

2. Experimental

2.1. Method and Materials

2.2. Cu and Ni Nanoparticles Synthesis

2.3. Cu-Ni Nanoalloys Synthesis

3. Results and Discussions

3.1. UV/ Visible spectroscopy

3.2. Fluorescence spectra of Cu-Ni BHNPs

3.3. Characterizations of Cu-Ni BHNPs

3.4. Electrochemical applications of Cu-Ni BHNPs

4. Conclusions

Declarations

Author Contribution

Acknowledgments

References

Additional Declarations

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