Electrochemical detection for Hg 2+ ion based on hydrazine-montmorillonite intercalation compound as potentiometric electrode

doi:10.21203/rs.3.rs-4179563/v1

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Electrochemical detection for Hg 2+ ion based on hydrazine-montmorillonite intercalation compound as potentiometric electrode

https://doi.org/10.21203/rs.3.rs-4179563/v1

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Hydrazine-montmorillonite (HYD-MMT), intercalation compound was prepared to construct potentiometric electrode for the determination of Hg²⁺ ion. The results of X-ray diffraction spectrometry (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) mapping techniques revealed that the hydrazine was completely intercalated in the interlayer space of montmorillonite. This intercalation compound (HYD-MMT) was used to construct as potentiometric electrode and compositions were optimized. The composition of the hydrazine-montmorillonite (HYD-MMT) intercalation compound: graphite: epoxy resin of 20:20:60 % wt gave compatible slope with the Nernstian theory for Hg²⁺ ion. Potentiometric results of electrode provided the slope with 29.431.49 mV decade^-1, LOD 5.26x10^-6 M within linear concentration range 10^-6-0.1 M. The selectivity coefficient was performed by separate solution method and results presented that this electrode provided good selectivity for Hg²⁺ ion. Electrochemical impedance spectroscopy (EIS) was used to study electron transfer and behavior at the surface of electrodes, the results indicated that hydrazine in montmorillonite structure could help increase electron transfer at the surface electrode during performing Hg²⁺ ion solution. This electrode was successful to determine Hg²⁺ ion in real soil sample from rice field.

montmorillonite

intercalation compound

hydrazine

potentiometric electrode

Hg2+ detection

Montmorillonite is a clay mineral belonging to smectite family. Structure of montmorillonite consists of three layers silicate which is 2:1 ratio of alumina octahedral sheet one layer between two layers of silica tetrahedral sheets. Montmorillonite has flake like sheet shape and compose of interlayer space in structure due to substitution by other ions such as Al³⁺ for Si⁴⁺ and Mg²⁺ for Al³⁺, then charges are imbalance with negative charge. The negative charge is balanced by interlayer exchangeable cations or it is called a cation exchange capacity (CEC) of clay minerals and very important properties. CEC of montmorillonite can be used to exchange with other cations or molecules due to they are usually utilize to control some physical and chemical properties of clay minerals [1, 2].

Hydrazine is an inorganic compound which has chemical formula N₂H₄. Hydrazine is found to use as starting materials or main composition in various industries such as explosion, propulsion, insecticides, emulsifiers and pharmaceutical additives [3, 4]. Due to properties of hydrazine such as high energy density low cost, CO₂ emission and unlimited sourcing of N₂ and H₂, is used for fuel cells producing and development [5–8]. Moreover, some hydrazine’s derivative is used to apply for preventing corrosion as previous reported [9–10] and fabrication for electrochemical sensors to detect heavy metals, biomolecules, toxic substance as previous studied. [11–14].

According to previous studied [15–18], montmorillonite have been prepared as nanocomposite or intercalation compound due to important characteristic of montmorillonite such as, high specific surface area, swelling behavior, good adsorptive and ion exchange properties. Modification of montmorillonite is usually used to apply for various electrochemical sensors construction, for example to detect colorants in food industry, trace cadmium, antibiotic cefoxtaime and bioactive magiferin have been reported. [19–23]. The aim of this work is prepare and characterize hydrazine-montmorillonite intercalation compound to construct as potentiometric electrode for detection of Hg²⁺ ion in solution. Potentiometric parameters are optimized and EIS technique is used to observe electron transfer and behavior at the surface electrode.

2.1 Reagents and instrument

Na⁺-montmorillonite from BYK-Chemie GmBH Germany which has cation exchange capacity at 92.6/100 g [24]. All chemical reagents were used as analytical grade from Ajax fine chemical and Univar. Graphite (Acris Organics), hydrochloric acid (HCl, Merck), nitric acid (HNO₃, Merck). Soil sample was collected from rice field in Thapya Subdistrict, Inburi District, Sinhburi Province, Thailand The Transform 800, Aurora Microwave digestion was used to digested soil sample.

2.2 Preparation of hydrazine-montmorillonite intercalation compound

Hydrazine intercalated montmorillonite (HYD-MMT) was prepared by following [25]. The mixture was mixed by magnetic stirrer for 12 h, then separated by using centrifuge and dried at 50 $\text{℃}$. The resulting solid of hydrazine intercalated montmorillonite (HYD-MMT) was obtained as pale yellow.

2.3 Characterization

Na⁺-montmorillonite and hydrazine-montmorillonite intercalation compound (HYD-MMT) were characterized by X-ray diffractometer, smart lab SE, Rigaku by Cu-K$\text{β}$ as X-ray generator with tube voltage 40 kV at 30 mA ($\text{λ}$ = 1.54 nm) in order to observe crystalline structure of samples. The diffraction angle were scans from 5$\text{°}$ − 40$\text{°}$ with rate /min. All of clay samples were studied functional groups by performing on fourier transform infrared spectrometer, Spectrum Two, PerkinElmer, in attenuated total reflectance (ATR) mode within wave number range 4,000-500 cm⁻¹. Scanning electron microscope with energy-dispersive X-ray spectrometer mapping was employed to study morphology and surface composition of samples.

2.4 Electrode construction

Electrode was constructed at ratio of HYD-MMT : graphite : epoxy resin, 20:20:60% wt. HYD-MMT was mixed with graphite in agate mortar and ground manually about 15 minutes. Epoxy resin was used as binder then mixed entirely together with HYD-MMT graphite composite. The HYD-MMT graphite mixture was transferred to syringed with copper wire electrical contacted. The schematic diagram of electrode construction was shown in Fig. 1.

2.5 Electrochemical Apparatus

Electrochemical measurements were performed by using potentiostat /galvanostat, VIONIC, Metrohm Autolab. Electrode configuration was setup for potentiometric measurement which consists of working electrode (HYD-MMT), reference electrode Ag/AgCl and analyte solution with magnetic stirrer. Three electrodes cell configuration, HYD-MMT as working electrode, Ag/AgCl reference electrode and platinum rod counter electrode was used to perform electrochemical impedance spectroscopy (EIS) with the INTELLO 1.4 software. Frequency range was applied to electrochemical cell from 5 MHz – 0.1 Hz.

3.1 Characterization of hydrazine-montmorillonite intercalation compound

XRD patterns showed d-spacing of d₍₀₀₁₎ which response to silicate layer in montmorillonite structure, changed after mixing with hydrazine. Due to Bragg’s equation, the basal spacing of montmorillonite was found 9.72 $\AA$ at 2$\text{θ}$ of 9.10$\text{°}$. After mixing with hydrazine, it shifted to 12.09 $\text{Å}$ at 2$\text{θ}$ of 7.305$\text{°}$ ($\text{∆}$d = 2.37). The results indicated that hydrazine was successfully intercalated in montmorillonite structure.

FT-IR spectrum of Na⁺-montmorillonite (MMT), hydrazine-montmorillonite (HYD-MMT) and hydrazine (HYD) were shown in Fig. 3. The OH-stretching vibration band of water molecules were observed at 3,611 and 3,618 cm^− 1 for HYD-MMT and MMT, in addition OH deformation vibration of water molecule due to weakly bond with Si-O and Al-O in silicate layer was found at 1,633 1,627 and 1,612 cm^− 1 for MMT, HYD-MMT and HYD, respectively. The adsorption band was appeared at 3,362 and 3,345 cm^− 1 for HYD-MMT and HYD which attributed to NH stretching vibration of of amine group in hydrazine (N₂H₄) molecule, this adsorption peak was not observed for untreated MMT which conformed with previous work [25, 26]. Si-O-Si stretching vibration strong peaks was found at 1,006 and 981 cm^− 1 and the adsorption peak at 909, 520 and 508 cm^− 1 were assigned to Al-OH and Si-O-Si bending of montmorillonite which consistent with [27]. This could be concluded that hydrazine is completely attended in the structure of montmorillonite.

(blue).

Table 1

FT-IR adsorption peaks assignments of Na⁺-montmorillonite (MMT), hydrazine montmorillonite (HYD-MMT) and hydrazine (HYD).
Functional groups	Wavenumber (cm^− 1)
Functional groups	MMT	HYD-MMT	HYD
-OH stretching of water molecule in montmorillonite	3,618	3,611	-
-NH stretching of amine	-	3,362	3345
-OH deformation of water molecules bonded with Si-O and Al-O	1,633	1,627	-
Si-O-Si stretching vibration of montmorillonite	1,066	981	-
Al-OH of montmorillonite	909	909	-
Si-O-Si bending of montmorillonite	520	508	-

The morphologies of Na⁺-montmorillonite (MMT) and hydrazine-montmorillonite (HYD-MMT) are shown in Fig. 4 (a) and (b). SEM images and revealed that Na⁺-montmorillonite and hydrazine-montmorillonite exhibited flake like sheet shape and homogeneous. After treated with hydrazine, the morphology of hydrazine-montmorillonite did not change when compared with Na⁺-montmorillonite. The composition of clay samples were determined by using energy dispersive X-ray spectroscopy (EDS) technique as shown in Figs. 5 and 6, also EDS elemental mapping was shown in Fig. 7. The resulting exhibited O, Si and Al atoms as main composition and homogeneous. N atom was found at 1.37% for HYD-MMT and did not observe in Na⁺-montmorillonite (MMT) in Fig. 5. This implied that hydrazine molecule could be successfully intercalated in the interlayer sheet of montmorillonite.

Table 2

Elemental composition results of Na⁺-montmorillonite (MMT) and hydrazine montmorillonite (HYD-MMT).
Samples	Elemental (atomic %)
	O	Na	Mg	Al	Si	S	Ca	Fe	N
MMT	72.47	2.20	1.02	6.74	16.67	0.05	0.08	0.76	-
HYD-MMT	56.85	1.92	1.03	9.68	25.96	0.43	0.51	2.25	1.37

compound (e-h).

3.2 Electrochemical results

3.2.1 Potentiometric study and electrode optimization

In this research, we attempt to study of electrode response for heavy metals determination by potentiometric method. Heavy metal ions solution were prepared within concentration range 10^− 6-0.1 M. A 20:20:60% wt of HYD-MMT:graphite:epoxy resin composition was constructed as working electrode and Ag/AgCl as reference electrode. They were used to measure the potential in heavy metals ion solution (n = 4) and equipped with VIONIC PGSTAT, Metrohm Autolab. Potentiometric response results were shown in Fig. 8 and Table 3.

Table 3

Slope, R² and concentration range of 20:20:60% wt electrode composition.
Metal ions solution	Slope (mV decade^− 1)	R²	Concentration range (mol dm^− 3)
Cu²⁺	12.73	0.9430	10^− 5 − 0.1
Co²⁺	-14.15	0.8589	10^− 5 − 10^− 2
Ni²⁺	nd	nd	nd
Pb²⁺	20.40	0.9911	10^− 6 -10^− 2
Cd²⁺	nd	nd	nd
Fe³⁺	58.25	0.9692	10^− 4 − 10^− 2
Mn²⁺	nd	nd	nd
Zn²⁺	nd	nd	nd
Hg²⁺	31.60	0.9968	10^− 6 − 0.1

*nd = non detection

From Table 3, potentiometric measurement of Hg²⁺ ion exhibited good slope and linearity with 31.60$\text{±}$0.79 mV decade⁻¹ which correspond to Nernst’s theory (29.5 mV decade^− 1). The linear concentration was found in range 10⁻⁶-0.1 M, then we selected Hg²⁺ to study potentiometric response and composition of electrodes were optimized. Four compositions of electrode were prepared and used to measure potential in Hg²⁺ solution. Slope value, R² and concentration range were presented as following Table 4. Slope value of the composition of 20:20:60% wt gave slope with 29.43$\text{±}$1.49 mV decade⁻¹ (R ² = 0.9923) within linear concentration range 10⁻⁶ − 0.1 M. This study, we used 20:20:60% wt for Hg²⁺ ion determination. Plot of potential vs. log [Hg²⁺] was displayed in Fig. 9.

Table 4

Slope, R² and concentration range of four electrode compositions.
Electrode composition (% wt)	Hg²⁺ ion
Electrode composition (% wt)	Slope	R²	Concentration range (mol dm^− 3)
10:30:60	84.86	0.9892	10^− 6 – 10^− 3
20:20:60	29.43	0.9923	10^− 6 – 0.1
30:10:60	98.73	0.9063	10^− 4 – 0.1
35:5:60	nd	nd	nd

*nd = non detection

Figure 9 Plot of potential vs. log [Hg²⁺].

3.2.2 Reproducibility and durability

To examine reproducibility of electrode, 9 electrodes of the composition 20:20:60% wt were constructed and performed for Hg²⁺ ions response. Slope average values was determined at 30.53 $\text{±}$1.70 mV decade⁻¹ which far from theorical value (29.5 mV decade^− 1) only 3.49% for Hg²⁺ ion. After 6 months, the sensitivity of electrode loss 10.94% and slope was changed from 30.53 to 27.19.

3.2.3 Dynamics response time

According to IUPAC recommendation [28], response time is necessary parameter to evaluate for ion selective electrodes (ISE). To examine response time, Hg²⁺ solutions were prepared within concentration range from 10^− 6-0.1 M. HYD-MMT working electrode and Ag/AgCl reference electrode were immersed in ion solution. The resulting presented that potential exhibited constant and fast potentiometric response about 8 s as shown in Fig. 10.

3.2.4 Effect of pH

To determine an appropriate pH range for using this electrode, Hg²⁺ ion solution of 0.001 and 0.01 M were prepared and adjusted pH 2–12 with NaOH and HCl. Plot of potential vs pH was shown in Fig. 11. The results presented that potential of this electrode composition of 20:20:60% wt was slightly changed in pH range 4–9. The potential of electrode at above pH 9 were significantly changed may be due to hydroxide precipitation. In acidic solution, the potentials were increased, it might be due to the high presence of H⁺ at the surface electrode [29]. The pH range 4–9 could be taken as suitable working pH range for this electrode.

3.2.5 Selectivity of electrodes

The selectivity coefficient is one of important parameter for ion selective electrodes, ISEs. Separate solution method (SSM) was used to evaluate selectivity coefficient of electrode, the potential of potentiometric cell setup is measured in separate solution between analyte ion (A) and interfering ions (B) at same activity of a_A equal a_B. Potential of E_A and E_B are measured in according to [30], then selectivity coefficient is calculated by using Nicolsky Eisenman as following Eq. (1)

$$\text{log}{\text{K}}_{\text{A,B}}^{\text{pot}}\text{=} \frac{{\text{(E}}_{\text{B}}\text{-}{\text{E)}}_{\text{A }}{\text{z}}_{\text{A}}\text{F}}{\text{2.303RT}}\text{+}\left(\text{1-}\frac{{\text{z}}_{\text{A}}}{{\text{z}}_{\text{B}}}\right)\text{log} {\text{a}}_{\text{A}}$$

where $\text{log}{\text{K}}_{\text{A,B}}^{\text{pot}}$ is selectivity coefficient, E_A and E_B are potential of primary and interfering ion Z_A is charge number which is integrated with sign of primary ion. Z_B is charge number including with sign of interfering ions, F is the Faraday constant equal to 96,485 C mol^− 1, R is the gas constant 8.3145 J K^− 1 mol^− 1 and log a_A is logarithm concentration corresponding to primary. Selectivity coefficient of HYD-MMT electrode was shown in Table 4.

Table 4

Selectivity coefficient ($\text{log}{\text{K}}_{\text{A,B}}^{\text{pot}}$) of HYD-MMT potentiometric electrode composition of 20:20:60% wt
Interfering ions	$\text{log}{\text{K}}_{\text{A,B}}^{\text{pot}}$	Interfering ions	$\text{log}{\text{K}}_{\text{A,B}}^{\text{pot}}$
Cu²⁺	-1.13	Na⁺	-1.94
Co²⁺	-1.20	K⁺	-0.91
Cd²⁺	-0.92	F⁻	-10.45
Ni²⁺	-1.27	Cl⁻	-10.18
Cr³⁺	-2.21	Br⁻	-10.32
Mn²⁺	-1.22	I⁻	-10.33
Zn²⁺	-1.26	N${\text{O}}_{\text{3}}^{\text{-}}$	-10.41
Ca²⁺	-1.29	$\text{S}{\text{O}}_{\text{4}}^{\text{2-}}$	-7.45
Pb²⁺	-1.27

The resulting exhibited that selectivity coefficient values of electrode for divalent metal ions gave larger values than other ions. However, Nernstian slope of each ion was small and not compatible with theoretical value. This result indicated that electrode composition of 20:20:60% wt showed good selectivity to Hg²⁺ ion.

3.2.6 EIS

Electrochemical impedance spectroscopy is used to study electron transfer and electrochemical behavior at the surface electrode. Montmorillonite bare electrode (MMT) and HYD-MMT working electrode were used to perform EIS measurement in deionized water (DI) and Hg²⁺ ion solution with Ag/AgCl reference and Pt rod counter electrode by three electrochemical cell configuration. Frequency range was applied from 5 MHz − 0.1 Hz. Nyquist plots were recorded by software 1.4 INTELLO, VIONIC potentiostat/galvanostat, Metrohm Autolab as shown in Fig. 12

EIS results presented that Nyquist plots exhibited semicircle at high frequency during use of MMT (bare) and HYD-MMT as working electrode which correspond to electron transfer at the surface electrode and also Warburg diffusion was observed due to mass transfer at low frequency. Impedance values of HYD-MMT electrode was smaller than when compared with MMT (bare) electrode during performed in 0.001 M Hg²⁺ ion solution. The propose of electrode behavior could be due to hydrazine in montmorillonite structure could help increasing of electron transfer at the surface electrode.

3.2.7 Analytical application

HYD-MMT potentiometric electrode was undertaken to apply for the determination of Hg²⁺ ion in real soil sample. Due to the amount of Hg²⁺ ion in environmental was low, then this studied was attempted to determine Hg²⁺ ion in real soil sample by standard addition method. Before potentiometric performing, soil sample was mixed with aqua regia and digested by using Transform 800, Aurora, microwave digestion at 200 $\text{℃}$ with time 1,800 second. Soil digested sample was diluted with DI water by 1:100 ratio. The amount of Hg²⁺ ion in real soil sample was found at 7.71x10^− 3 M as following in Table 5.

Table 5

The amount of Hg²⁺ ion in real soil sample.
Sample	Hg²⁺ ion concentration (mol dm^− 3), (n = 5)	%RSD
Soil	7.71x10^− 3	0.84

Hydrazine intercalated montmorillonite was prepared and characterized. XRD, FT-IR and SEM-EDS mapping results revealed that hydrazine was completely intercalated in montmorillonite structure and homogeneous. This intercalation compound was used to construct potentiometric electrode for electron of Hg²⁺ ion. Potentiometric response results exhibited that the compositions of hydrazine-montmorillonite (HYD-MMT) intercalation compound: graphite: epoxy resin of 20:20:60% wt conformed with Nernstian theory when performed measuring potential in Hg²⁺ ion solution. Potentiometric results provided with good slope, low limit of detection and wide linear concentration range. This electrode showed good reproducibility, selectivity, fast respond and durability. EIS results indicated that hydrazine molecule in montmorillonite could help enhancing an electron transfer at the surface electrode. This electrode could be applied to determine Hg²⁺ ion in real soil sample from rice field.

Declarations

Conflict of interest:

There are no conflicts to declare.

Author Contribution

Kemawade Udomhan: conceptualization, methodology, data collection, formal analysis and manuscript draft writing. Thanawat Phongsak: data collection and formal analysis. Pranitda Inchomrit: data collection and formal analysisAll authors reviewed the manuscript. This work is supported full funding by Research and Development Institute, Thepsatri Rajabhat University.

Acknowledgment

This work is supported full funding by Research and Development Institute, Thepsatri Rajabhat University. The authors would like to express our special thank you to Science Program, Faculty of Science and Technology for providing scientific instruments laboratory facilities.

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Electrochemical detection for Hg 2+ ion based on hydrazine-montmorillonite intercalation compound as potentiometric electrode

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Abstract

Figures

1. Introduction

2. Material and Methods

2.1 Reagents and instrument

2.2 Preparation of hydrazine-montmorillonite intercalation compound

2.3 Characterization

2.4 Electrode construction

2.5 Electrochemical Apparatus

3. Results and discussion

3.1 Characterization of hydrazine-montmorillonite intercalation compound

3.2 Electrochemical results

3.2.1 Potentiometric study and electrode optimization

3.2.2 Reproducibility and durability

3.2.3 Dynamics response time

3.2.4 Effect of pH

3.2.5 Selectivity of electrodes

3.2.6 EIS

3.2.7 Analytical application

4. Conclusion

Declarations

Declarations

Author Contribution

Acknowledgment

References

Additional Declarations

Supplementary Files

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