Anal. Methods Environ. Chem. J. 6 (1) (2023) 58-68

Research Article, Issue 1

Analytical Methods in Environmental Chemis try Journal

Journal home page: www.amecj.com/ir

AMECJ

Study of the behavior and determination of phenol Based on

with nickel oxide-nitrogen

carbon quantum dots using cyclic voltammetry

Khalil Ibrahim Alabid a,* and Hajar Naser Nasser a

aAnalytical Chemi s try - Department of Chemi s try - Faculty of Science - Tishreen University – Syria.

ABSTRACT



carbon pa s te electrode (MCPE) with nickel oxide nanoparticles doped

by nitrogen carbon quantum dots as nanoadsorbent (NiO-NCQD) and

cyclic voltammetry (CV). The MCP electrode was manufactured





Cyclic voltammetry can provide behavior

       

     trans    

trans) by increasing the

phenol concentration in the solution, and increasing of con s tant K0

when the concentration of phenol increased in the solution. Also,

the highe s t occupied molecular orbital (HOMO), lowe s t unoccupied



calculated. In this s tudy, EHOMOLUMO

were considered. The drinking water samples from Latakia city were

analyzed based on NiO-NCQD adsorbent using the MCPE method

(NiO-NCQD/MCPE). The phenol concentration in the drinking water

sample in Latakia was achieved less than the quantitative detection

limit (LOQ), and the proposed procedure was validated by spiking

samples.

Keywords:

Phenol,

Cyclic voltammetry,



Nickel oxide nanoparticles,

Nitrogen carbon quantum dots,

Kinetic

ARTICLE INFO:









*Corresponding Author: Khalil Ibrahim Alabid

Email: khalilibrahimalabid@gmail.com



------------------------

1. Introduction

Phenol is described as an aromatic organic

compound CH5OH. Phenol and its derivatives

are the main pollutants in water sources . It

is highly toxic  and enters the human body

through inge s tion, inhalation, or contact with the

skin; exposure to phenol for long periods causes

severe damage. Among these damages: Damage to

the lungs, liver, kidneys, urinary and reproductive

tracts, cardiovascular disease, shortness of breath,

neurological problems, as well as severe abdominal

pain, ga s trointe s tinal irritation, nausea, vomiting,

diarrhea, sweating, coma, and death. Inge s tion of

; phenol increases

oxidative s tress in biological materials, disrupting

endocrine metabolism and promoting cancer

; the maximum permissible level of phenol

according to the world health organization (WHO)

that its concentration does not exceed one µg L

in drinking water . Phenol and total phenol

can be e s timated spectrophotometrically in the

visible (VIS) , in the ultraviolet (UV) ,

and High-Performance Liquid Chromatography

(HPLC) .   showed the phenol

oxidation (one-electron oxidation) and reaction

process .

Cyclic voltammetry is one of the mo s t important

electrochemical techniques that help provide

information about the kinetics, mechanics, and

behavior of the s tudied material ; it is also

possible from cyclic voltammetry to know if the

reaction is subject to oxidation, reduction, or both.

It has three cases: reversible, quasi-reversible, or

irreversible . Cyclic voltammetry can provide

kinetic and mechani s tic information; as such:

   , mass transport

(mtrans) ),

, and con s tant K0 , the highe s t occupied

molecular orbital (HOMO), lowe s t unoccupied

molecular orbital (LUMO)  , Gibbs free

 and interface trap density (Dit)

.

     

Randles-Sevcik irreversible   .

The mass transport is given by.



by Equation 3 . Con s tant (k0

s tandard rate con s tant (k0) ratio to mass transfer. It

is given by Equation 4 . The HOMO-LUMO

values are given by     .

 .

The interface trap density (Dit) can be obtained by

.



Where, ip: Peak current (A), n: Number of electrons,

), A: electrode area

(cm

C: concentration (mol. cm–3), R: gas con s tant

(J. mol K     

s), v: Scan rate (V s).



(Eq.3)

       

represents a measure of the symmetry barrier in a



of electrons involved in the rate-determining s tep.

Schema 1. The oxidation and reaction of phenol

Study and Determination of Phenol by NiO-NCQD and CV Khalil Ibrahim Alabid et al

 Anal. Methods Environ. Chem. J. 6 (1) (2023) 58-68

(Eq.4)

Where: io: exchange current density (A m), in the

case where the oxidation is irreversible it mu s t be:

k0 ≪ mtrans, as for according to Nicholson, mu s t be

k0-4 × v .

EHOMO eV= [ Eox - E(Eq.5)

ELUMO = (EHOMO – Eg) 

Where: Eox     :

half-oxidation potential for peak, Eg: Optical

Bandgap (from absorption s tudies).

ox - Ered - Eg + C 

Where: Eox: Oxidation potential, Ered: Redaction

potential, Eg: the excited singlet s tate energies, C: is

the electro s tatic interaction energy for the initially

formed ion pair, generally considered negligible in

polar solvents.

(Eq.8)

A, q, Cox, V, and Eg are the gate area, electron

   

voltage shift, and bandgap.

Carbon/graphite pa s te electrodes (CPE) are

important for being chemically inert, easy to

fabricate, electrode surface renewability, low ohmic

resi s tance, low co s t, and environmentally friendly.

However, its kinetics, s tability, and selectivity are



; therefore, in



relied upon, as they are more selective and sensitive

to organic compounds. This research is one of the

critical research s tudies on the behavior of phenol

in the electrochemical cell and determines the

concentration of phenol in a drinking water sample

using a selective electrode for carbon pa s te with

nanoparticles by cyclic voltammetry.

2. Experimental

2.1. In s truments

Voltammetry sy s tem for trace analysis and education.

Complete accessories with VA Computrace software

and all electrodes for a complete measurement

sy s tem: Multi-Mode Electrode pro (MME pro),

Ag/AgCl reference electrode, and Pt auxiliary

electrode. In this s tudy, a modern voltammetric was

connected to a PC based on a USB port (Metrohm

    



Data Weighing Sy s tem Company (pH meter and

mV meter; DWS Inc., USA)

2.2. Reagents and Materials

All chemicals with high purity were purchased

from Sigma or Merck Company (Germany). Phenol

CHO purchased from Acros Organics Company

    ,

-3

The monopotassium dihydrogen phosphate

(KHPO4) was prepared from Sigma, Germany

      



Sigma).

2.3. Synthesis of NiO-NCQD nanocomposite



with 30 mL of nitrogen quantum carbon dot after

       

      

then washed three times with di s tilled water and



nanocomposite.

2.4. General procedure

2.4.1.Fabrication of selective electrode

The selective electrode is made (in the laboratory). It

consi s ts of a glass tube that is open at both ends and



upper back; it is connected to the device. A copper wire

conducting electric current is connected between the

   

carbon pa s te using NiO-NCQD nanocomposite 



Study and Determination of Phenol by NiO-NCQD and CV Khalil Ibrahim Alabid et al







the electrode body is made of glass. Symbolizes the

factory electrode (NiO-NCQD/MCPE) shown in

. Then the electrode is connected to the volt-

amperometric cell (VA), which consi s ts of a working

electrode (WE) and a comparison electrode, and it is

usually an Ag/AgCl electrode where its potential is

󰀰

2.4.2.Preparation of s tock solution and

monopotassium phosphate buer





       

prepared from KHPO4







3. Results and discussion

3.1. Eect of pH



on the current intensity I(µA) of a s tandard phenol

solution shown in .

      

values of and U(V), it is noted that it two peaks

Fig. 1. Schematic of factory electrode components (NiO-NCQD/MCPE)

Fig. 2. 



and achieves the highe s t value of peak current =

       

two values are adopted. In the case of phenol,

when used CV method, it undergoes an oxidation

process only without reduction, so the sy s tem is

irreversible, phenol concentration is s tudied with





 both of pH

       

      

(NiO-NCQD/MCPE).

Cyclic voltammetry can provide behavior

     

(D     ), the mass

transport (mtrans), and the values of each are

calculated 

3.2. Eect of phenol concentration

      

o, and mass transport

and interface trap density (Dit) are s tudied for the

phenol concentrations, as in .

      

      

concentration, probably due to increasing

phenol concentration, cause the blockage of the

electrode surface. In the case where the oxidation

is irreversible, it mu s t be: Ko<m trans, according

to Nicholson, mu s t be k0  -4× v, from

previous curves, In this research, K0<m trans and

K0-4-5, the HOMO-LUMO

values are s tudied from cyclic voltammetry

     

nanocomposite, where Eox= 0.43 V, and E



from (UV) so, EHOMO

Table 1. 



pH CµM I (µA) D×109

(m2·s-1)nα α. mtrans Ko×107(Dit)

eV−1 cm−2

 90     

      

500      

      

0 45     



  0.048443    

 99     

500      

 83     

0     

Anal. Methods Environ. Chem. J. 6 (1) (2023) 58-68



Fig. 3. 







D) mass transport,



Study and Determination of Phenol by NiO-NCQD and CV Khalil Ibrahim Alabid et al



ELUMO=         



is spontaneous in the direction with electric current.

The interface trap density (Dit) of the electrode has

) eV

cm)

eV cm      

good corresponding and, as noted, interface trap

density (Dit) decrease in value with increasing



        

initially in the pre-measurement s tage at a rate

        

compound in solution inside the electrochemical

cell are, principally three :(convection, migration,

      

homogenizing the solution in addition, s tirring



of unwanted motion (migration and convection),

        

that expresses the behavior of phenol within the

electrochemical cell; during the s tirring s tage,

nitrogen gas gurgles inside the electrochemical cell

      

behavior where the temperature of the solution was

oC.

3.3. Application on drinking water samples by

the proposed electrode (NiO-NCQD/MCPE)

A drinking water sample from Latakia city was

analyzed using the proposed method, and it was

found that the sample was less than the detection

limit (<LOD) of the method. The s tandard addition

method found that the sample does not contain

phenol, according to  and . Due

to previous curves, the results can be placed in

.

It is noted from the above that the phenol concentration

in the drinking water sample in Latakia is less than

the quantitative detection limit (LOQ) of the method,

).

4. Conclusion

This paper deals with fabricating a phenol-selective



Oxide nanoparticles (NiO) doped with Nitrogen

Carbon Quantum Dots (NCQD) using Cyclic

voltammetry. The electrode was manufactured in

a laboratory. Results be s t conditions are obtained

PO4,

and the behavior of a phenol solution is s tudied in

an electrochemical cell (Cyclic voltammetry) using

NiO-NCQD/MCPE. The phenol concentration in

Fig. 4. Determination of phenol concentration in drinking water using

the proposed electrode (NiO-NCQD/MCPE) at pH = 4

Anal. Methods Environ. Chem. J. 6 (1) (2023) 58-68



the drinking water sample in Latakia is less than the

quantitative detection limit (LOQ) of the method,

).

5. Acknowledgments



University- Syria and the Higher In s titute for

Environmental Research - Tishreen University-

Syria for their help and support during this work.

6. References

     

S. Agarwal, V.K. Gupta, Electrochemical



by a titanium oxide nanotubes/single-wall

carbon nanotubes nanocomposite-ionic

    

     



 

Dahalan, A. Khalid, S.A. Ahmad, Phenol and







       

Phenol and its toxicity: A case report, Iran. J.

http://ijt.



Fig. 5. Determination of phenol concentration in drinking water using



Table 2. 

Sample Added Phenol

(μM)

Expected Phenol

(μM)

Found phenol

(μM)

RSD

(%)

Recovery

(%)

Drinking

Water

-- -- LOQ -- -

    

Drinking

Water

--* --* LOQ * --* --*

   4.3488* 

Study and Determination of Phenol by NiO-NCQD and CV Khalil Ibrahim Alabid et al



        

Suicidal phenol inge s tion: A case report,

      

  https://www.academia.edu/



      

Phenolic compounds in water: sources,

reactivity, toxicity and treatment methods,

    http://dx.doi.



 

phenols of environmental implications:

      

  



      

     

associated with phenol, Toxicol. Ind.

     https://doi.



     

    

  



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      

      

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

    

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  

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    



       

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       

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   https://

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      

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

      

    

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    

   

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    



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        

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



 

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

     

   

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

    https://



        

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     

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

      

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    

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

 

   

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    

org/ 

     

    

Moreno, Dual descriptor analysis of

   

electrodes for ascorbic acid sensing





Anal. Methods Environ. Chem. J. 6 (1) (2023) 58-68