CHM026.

2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

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Activity No. 2
Voltammetry

Determination of Heavy Metals in Herbal Food Supplements using Bismuth/Multi-walled Carbon

Nanotubes/Nafion modified Graphite Electrodes sourced from Waste Batteries

Background of the Study (content should include heavy metal, glass electrode and the modification, herbal
supplements) 10 pts
Heavy metals have been introduced in substantial amounts in many environmental compartments
due to anthropogenic activities resulting in pollution. They are harmful to humans and the
environment, thus, concentrations must be monitored in different compartments. Analytical
methods for detecting trace amounts of heavy metals in samples have been developed; however,
they are not an ideal because they are costly, time-consuming, and involve complex processes and
instruments. The electrochemical method, on the other hand, is a quick and efficient method of
determining the amounts of heavy metals in samples due to its simplicity, high sensitivity, good
stability, and low cost.
The glassy carbon electrode (GCE) is the most common working electrode in voltammetry because it
is chemically and electrochemically inert and relatively reproducible. However, it is quite expensive
(Ravenna, et al., 2013). The graphite electrode (GE) is an alternative electrode suited for
electrochemical analysis of heavy metals. Graphite is abundant in dry-cell batteries and rods taken
from AA batteries are ideal for fabricating a suitable working electrode. Bare graphite electrodes
have low sensitivity due to their large activation potential. Graphite electrodes, on the other hand,
have a distinct, structure that may be easily adjusted with various materials to improve sensitivity.
Bismuth nanoparticles(BiNP) are the most often used working electrode modifiers  in
electrochemical analysis due to their low toxicity and broad electrochemical scope. Study shows that
bismuth nanoparticles for electrodes have excellent sensing properties. (Jeromiyas, N., et.al. (2019)
Multi-walled carbon nanotubes (MWCNT) modification can also improve the electrode's electrical
conductivity, reduce the likelihood of surface fouling, and speed up electrochemical reactions.
Nafion is another electrode enhancer that has excellent properties such as antifouling capacity,
chemical inertness, and high cation permeability. As a result, using BiNP, MWCNT, and Nafion as
electrode modifiers would have a synergistic effect, considerably enhancing the bare electrode's
selectivity and sensitivity.
Herbal Food Supplements(HFS) have been utilized for ages since they are thought to have
medicinal effects. It comes in a variety of forms that can be used both internally and externally,
including liquid extracts, tea, tablets, capsules, and more. However, public health concerns have
metals. As a result, it's crucial to assess possible heavy metal contamination in HFS.
surfaced, such as product contains heavy
CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

Objective of the Study:

 To develop a cost-effective and environment-friendly electrochemical sensor based on graphite rod

extracted from waste zinc-carbon battery. The extracted rods were modified with BiNP, MWCNT and
Nafion and were used as the working electrode in ASV to detect trace amounts of cadmium (Cd 2+) and lead
(Pb2+). To demonstrate the utility of the modified electrodes in sensing applications, real sample analysis
using the modified graphite electrode was done on commercially available herbal food supplements.

Procedure (Make a schematic flow using arrows and bullets) 10 pts

CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

Results and Discussion

A. Graphite electrode optimization

Refer to Figure No. 2, 3, 4. Why are these conditions optimized? Connect the optimized conditions in
operating the instrument. (5 pts)
CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

B. Calibration plot for bare Glass Electrode

Refer to Figure No. 5, 6, 7. What is the sensitivity, limit of detection and dynamic range? (5 pts)
CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

C. Modified Glass Electrode Optimization

What is the composition of the modified glass electrode? (3 pts)

CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

What instrument conditions were optimized based on Figure No. 9, 10, 11? (3 pts)

D. Calibration plot of optimized modified Glass Electrode

CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

Compare the sensitivity between the bare (Figure No. 5, 6, 7) and modified graphite electrodes (Figure No. 12,
13, 14) (4 pts)

E. Real Sample Analysis

In Table 1 above, voltammetric data (ASV) were compared to AAS. How will you evaluate the performance
of the modified glass electrode? Give your assessment and future direction. (10 pts)
CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory
CHM026.2 Analytical Chemistry for Engineering and Applied Sciences 2 Laboratory

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