ANODIC STRIPPING

VOLTAMMETRY
SALSABILA LATIFAH
2010412046
Anodic Stripping Voltammetry
Anodic Stripping Voltammetry is a method to demonstrate the presence of
multiple metals in water. This method is usually applied to investigate the water
quality of sewage, surface or drinking water. Anodic stripping voltammetry (ASV) which
has an in situ preconcentration (electrodeposition) step can be applied directly for
simultaneous determination of cadmium and lead at trace levels

Metal ions were electrochemically deposited on a working electrode, e.g., a hanging mercury
drop electrode (HMDE), a mercury film electrode [7–9], or a more environment friendly
bismuth film electrode. the determination was done in the stripping step by scanning potential
to positive (anodic) direction, where re-oxidation of the deposited metals was occurred at a
specific potential for each metal. However, this method can detect free metal ions only and is
suffered from interferences such as surface active organic substances
Article
Backstory
Cadmium and lead are well-known toxic metals. These metals are found in glazed ceramic
surfaces and are controlled by law for permissible amounts released from some ceramic
products. Glaze is a thin layer of liquid, which is put on a piece of pottery and becomes
hard and shiny when the pottery is heated in a hot oven

In Thailand, ceramic products are mainly produced in northern provinces, e.g., Lampang,
Sukhothai and Chiang Mai. Release of cadmium and lead from ceramic ware, glass–
ceramic ware and glass dinnerware intended to be used in contact with food is tested
according to the Thai industrial standard

The method involving extraction of themetals from the glaze by 4% (v/v) acetic acid,
which is kept in the ceramic ware to be tested for 24 h in the dark, and determination of
the metals in the extracted solution by flame atomic absorption spectrophotometry (FAAS)
Chemicals and instrument
Deionized water
Stock standard solution of lead(II) (1000 mg L−1)
Stock standard solution of cadmium(II) (1000 mg L−1)
Stock standard solution of copper(II) (1000 mg L−1)
Stock standard solution of zinc(II) (1000 mg L−1)
The working standard solutions were prepared daily by diluting the stock standard solution of each metal with 4% (v/v) acetic acid
The extracted solution (4% (v/v) acetic acid) was prepared by diluting 40 mL of glacial acetic acid in water and adjusting the final
volume to 1000 mL
An oxygen free nitrogen (OFN) gas

A voltammetric analyzer
HMDE as a working electrode (WE)
a platinum rod electrode as an auxiliary electrode (AE),
a Ag/AgCl electrode (3 M KCl) as a reference electrode (RE)
Extracting
ceramic ware

cleaned to be free from grease or other matter likely to affect the test
s filled with 4% (v/v) acetic acid solution
covered the specimen and allowed to stand in the dark at 22 ± 2 ◦C for 24 ± 0.5 h

Extracted solution
collected in a polyethylene bottle
Voltametric method
An aliquot of 10 mL of the extracted solution

put in a voltammetric cell and the solution was purged with OFN for 3 min
a fixed potential of −1.20 V was applied to the WE for a period of 45 s
solution was stirred at 2000 rpm

the stirring was stopped for 5 s

anodically scanning of the potential from −1.20 to 0.15 V, employing a square wave waveform with amplitude of 40 mV, step
potential of 10 mV, and frequency of 50 Hz (stripping step)

voltammogram was recorded

Adding standard solution of each metal to the sample solution, then the deposition and stripping steps were performed (4 times)
 Effecting parameters
• A square wave waveform was employed in the stripping step, as it
provided fast scanning and good sensitivity for the reversible redox
reaction
• Effect of deposition potential was investigated in the range of
−0.90 to −1.30 V. It was found that the more negative potential
used the higher sensitivity was obtained. Deposition potential of
−1.20 V was chosen because too negative potential may lead to
deposition of some interferences or evolving of hydrogen gas at the
WE in the high acidic medium
• Peak currents of all the metals, except Cu, are linearly proportional
to deposition time up to 2 min. At too long deposition time, the
deposited metals may saturate at the HMDE so no further increase
in peak current was observed
• Acetic acid in concentration range of 1–6% (v/v) did not affect
either on peak potential or peak current of all the metals studied.
However, the higher concentration of acetic acid used, the higher
zinc content in the electrolyte solution (blank) was observed
Voltammogram
Result and conclusion
Metal LOD (g L−1 ) Relative standart deviation (%)

Cd 0,25 3,0

Pb 0,07 2,8

Cu 2,7 3,6

Zn 0,5 2,8

Standard addition method was employed for quantification in

order to account for the effect of sample matrix. Sensitivity and
detection limit could be improved by using longer deposition
time. found that the contents of cadmium, lead, copper and zinc
released from the samples were in the range of <0.013–0.16,
0.02–0.45, <0.14 and 0.28–10.36 g dm−2, respectively, which
are lower than the permissible values of the Thai industrial
standard.
THANKS
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