SIC2022

LAB REPORT ANALYTICAL CHEMISTRY 1

EXPERIMENT 7

TITLE DIRECT POTENTIOMETRY USING ION SELECTIVE ELECTRODE

NAME SITI SARAH BINTI ABD SAMAD

ID NUMBER 23005996
DATE OF EXPERIMENT 11 DECEMBER 2024
INSTRUCTOR AP DR MUGGUNDHA RAOOV
PARTNER’S NAME NUR ALIAH BINTI ABDUL JALIL
Experiment 7

DIRECT POTENTIOMETRY USING ION SELECTIVE ELECTRODE

TITLE

Determina�on of fluoride in unknown sample A and tap water using specific ion electrode

OBJECTIVE

To determine the concentra�on of fluoride ion in water sample and an unknown sample A by
measuring its concentra�on from the poten�al of ion-selec�ve membrane electrode via
poten�ometric method.

RESULT AND DISCUSSION

Table 1 shows the concentra�on of fluoride standard solu�on and the volume used

Concentra�on of fluoride standard solu�on Volume used of fluoride standard solu�on to

(ppm) dilute (mL)
0.2 1.0
0.4 2.0
0.8 4.0
1.2 6.0
1.6 8.0
2.0 10.0

The volume of fluoride used to dilute the solu�on was obtained from the equa�on of;

M1V1 = M2V2

The concentra�on of fluoride stock solu�on, M1 = 10 mg dm-3 = 10 ppm

The volume of fluoride standard solu�on, V2 = 50 mL

Table 2 shows the table of log[F-], electrode reading in mV and poten�al mV

Concentration of Potential
Sample fluoride ion (ppm) log F- Reading Electrode reading (mV) (mV)
1 175.9 175.9
2 164.3 164.3
3 144.8 144.8
blank
1 134.6 -41.3
2 108.1 -56.2
3 122.4 -22.4
1 0.2 -0.69897 average = 121.7 -40.0
 1 115.6 -60.3
2 85.4 -78.9
3 111.1 -33.7
2 0.4 -0.39794 average = 104.03 -57.6
1 98.5 -77.4
2 70.1 -94.2
3 97 -47.8
3 0.8 -0.09691 average = 88.53 -73.1
1 89.7 -86.2
2 60.3 -104
3 87.5 -57.3
4 1.2 0.07918 average = 79.17 -82.5
1 80.3 -95.6
2 50.8 -113.5
3 79.5 -65.3
5 1.6 0.20412 average = 70.2 -91.5
1 74.9 -101
2 45.3 -119
3 73.6 -71.2
6 2 0.30130 average = 64.6 -97.1

In this experiment, calibra�on method which is a process that relates the measured analy�cal signal
to the concentra�on of the analyte was used to determine the fluoride concentra�on in the unknown
sample and in the tap water. Six standard fluoride solu�ons with different concentra�ons which are
0.2 mg/dm3, 0.4 mg/dm3, 0.8 mg/dm3, 1.2 mg/dm3, 1.6 mg/dm3 and 2.0 mg/dm3 were prepared. Then,
TISAB was added to each of the standard solu�on. TISAB was added to adjust the pH to a constant
value and to provide a background of constant ionic strength. Then, the fluoride concentra�ons of
these solu�ons were converted into electrical poten�al by an ISE meter. The poten�als obtained from
this experiment were -40.0 mV, -57.6 mV, -73.1 mV, -82.5 mV, -91.5 mV, -97.1 mV respec�vely.
 Figure 1 shows the graph of average poten�al (mV) against log [F-]

Graph of average potential (mV) against log [F-]

0
-0.80000 -0.60000 -0.40000 -0.20000 0.00000 0.20000 0.40000
-20
average potential (mV)

-40

-60

-80
y = -56.395x - 79.354
R² = 0.9984 -100

-120
log [F-]

The results gained from the standard fluoride solu�ons then used to plot a graph poten�al against the
log of fluoride concentra�on to determine the fluoride concentra�on of the unknown sample and tap
water. The graph ploted was a straight line graph with the equa�on, y = -56.395x - 79.354 and it has
a nega�ve slope. This is because the poten�al measured by the ISE is directly propor�onal to the
fluoride concentra�on in the solu�on which means the higher the concentra�on of fluoride ion, the
higher the poten�al obtained and the higher the ionic strength.

Table 3 shows the electrode reading for unknown sample with TISAB

Electrode reading
Sample Reading (mV) Potential (mV)
1 91.5 -84.4
2 93.0 -71.3
Unknown 3 90.5 -54.3

Table 4 shows the electrode reading for sample of tap water with TISAB

Electrode reading
Sample Reading (mV) Potential (mV)
1 111.6 -64.3
Tap 2 111.1 -53.2
water 3 109.4 -35.4
Calcula�on

1. Average poten�al of unknown sample + TISAB

(−84.4) + (−71.3) + (−54.3)
𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝 = = −70.0 𝑚𝑚𝑚𝑚
3

2. Average poten�al of tap water + TISAB

(−64.3) + (−53.2) + (−35.4)
𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝 = = −51.0 𝑚𝑚𝑚𝑚
3

3. Concentra�on of fluoride ion in

a) Unknown sample
y = -56.395x - 79.354
-70 = -56.395x - 79.354
x = -0.1659
log [F-] = -0.1659
[F-] = 0.68 mg/dm3

∴ The fluoride concentra�on in unknown sample is 0.68 mg/dm3

b) Tap water
y = -56.395x - 79.354
-51 = -56.395x - 79.354
x = -0.5028
log [F-] = -0.5028
[F-] = 0.31 mg/dm3

∴ The fluoride concentra�on in tap water is 0.31 mg/dm3

A blank sample containing no fluoride ion was also prepared by adding TISAB to dis�lled water with
equal volume. Next, the average poten�als of the unknown sample and the tap water obtained were
-70 mV and -51 mV respec�vely. By using this straight line equa�on, the fluoride concentra�on of the
unknown sample and the tap water obtained were 0.68 mg/dm3 and 0.31 mg/dm3 respec�vely as
shown in the calcula�on above.

The concentra�on of fluoride in tap water obtained from this experiment was slightly lower than the
actual concentra�on. This is because the minimum concentra�on of fluoride in tap water should be
approximately 0.5 mg/dm3. Fluoride in tap water help to promote our health especially dental health.
A fluoride content of 0.7 mg/dm3 is considered best for dental health. The fluoride concentra�on in
tap water shouldn’t be too high or too low because this will lead to various health problems. Even in
drinking-water, the concentra�on of fluoride should be in between 0.5 mg/dm3 and 1.2 mg/dm3. The
exposure to high concentra�on of fluoride for a long �me will cause the accumula�on of fluoride in
bones called skeletal fluorosis which will result in joint pain and also leads to weak bones in elderly.

In order to get more accurate result, some of the precau�on steps must be followed. First, always
transfer the solu�on to a beaker before pipe�ng and never pipet the solu�on straight from the
solu�on to avoid contamina�on of the solu�on. Moreover, do not immerse the �p of the pipete too
deep or too shallow and the �p should not be above the water level to avoid any mishap during the
suc�on of the water into the pipete via the pipete filler or pipete bulb. Next, the eyes level must be
perpendicular to the meniscus of the solu�on to ensure the accuracy. Other than that, rinse the ISE
before immerse into a solu�on for every measurement and dry it with a so� �ssue paper to get an
accurate poten�al. A magne�c s�rrer must be put into the solu�on to distribute the fluoride ion
throughout the whole solu�on and make sure that the s�rrer does not touch the ISE during the
measurement. Lastly, the stock sodium fluoride solu�on must be kept or store in polyethylene rather
than glass botles to prevent the glass corroded by hydrogen fluoride, HF. Equa�on below shows the
reac�on between the HF and the glass;

4HF + SiO2 → 2H2O + SiF4

CONCLUSION

The fluoride concentra�on in unknown sample and tap water are 0.68 mg/dm3 and 0.31 mg/dm3
respec�vely and lies in the calibra�on curve.

REFERENCES

1. SIC2022 Basic Analy�cal Chemistry I, Laboratory Manual, Faculty of Science, Universi�

Malaya.

2. Mar�nez-Acuña, M.I., Mercado-Reyes, M., Alegría-Torres, J.A. et al. Preliminary human

health risk assessment of arsenic and fluoride in tap water from Zacatecas, México. Environ
Monit Assess 188, 476 (2016).

3. Azrina A, Khoo HE, Idris MA, Amin I & Razman MR, Major Inorganic Elements in Tap Water
Samples in Peninsular Malaysia, 17(2): 271 – 276, 2011.

4. Interna�onal Journal of Electrochemical Science, Volume 7, Issue 2, February 2012.

htps://www.sciencedirect.com/science/ar�cle/pii/S1452398123134043