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Analytical Chemistry Laboratory 2

Direct Potentiometric Titration of Fluoride Ion

Mr. *****

Department of Chemical Engineering and Chemistry, Mapua Institute of Technology

In this experiment, the concentration of fluoride in drinking water will be determined by


a potentiometric method.. The activity of fluoride in solution can be determined with a solid-state
fluoride selective electrode. Four standard solutions were measured for its potentials, and a
straight line was obtained. An unknown sample, in this case, sample # 3 (6 mL) was analyzed
from the potential reading of 82.1 mV. The concentration of the fluoride was therefore computed
using linear regression and the result was 2.07 ppm.

Objective
parenteral administration. The systemic
The main objective of the actions of fluoride are presumably related to
experiment is to determine the concentration the inhibition of one or more enzymes
of Fluoride ion in a sample drinking water. controlling cellular glycolysis and to the
binding or precipitation of calcium as CaF2.
Discussion
Methodology
Overview
50 mL portions of water were
To measure a potential, we create a transferred to 100 mL volumetric flasks, and
voltaic cell with the indicator and reference were diluted to the mark with TISAB
electrodes. We measure the voltage of the solution.
cell, giving a reading of the indicator A 5 ppm F- solution was prepared
electrode potential relative to the reference by diluting 5 mL of the 100 ppm standard to
electrode. We can relate this to the analyte 100 mL in a volumetric flask. Aliquots of
activity or concentration using the Nernst 2.50-, 5.0-, 10.0-, 25.0-mL of the 5 ppm
equation. solution were transferred to 100 mL
The standard fluoride solution and volumetric flasks as well as 6 mL of the
the total ionic strength adjustment buffer sample, 25 mL of TISAB solution were
(TISAB) can be purchased readily from added, and diluted to the mark. (These
commercial sources. solutions corresponded to 0.5, 1.0, 2.5, and
Fluoride is a "general protoplasmic 5.0 ppm F-, respectively, in the sample.)
poison." When present as a soluble salt, it is After thorough rinsing and drying
readily absorbed from the alimentary tract. with paper tissue, the electrodes were
A 2% solution of sodium fluoride kills immersed in the 0.5 ppm standard. It was
mucosal cells, and its ingestion leads to a stirred mechanically for 3 min; the potential
severe hemorrhagic gastroenteritis; in part was then recorded. It was repeated similarly
this corrosiveness is due to a toxic action on with the remaining standards and the
mucosal capillaries and is seen even after sample.
A linear graph is derived when
concentration is in logarithmic form.
Instrumentation 120

100

The apparatus for this experiment 80

potential
consists of a solid state fluoride electrode, a 60

40
saturated calomel electrode, and a pH meter. 20

0
-0.4 -0.3 -0.2 -0.1 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
log [concentration]

In the presence of the total ionic


strength adjustment buffer, a plot of
potential vs. log [conc.] should be linear. To
determine the amount of fluoride in a
solution of unknown concentration, we must
pH measurements with an electrode first calibrate the electrode by measuring the
involve the measurement of potentials. The potential for a series of fluoride standard
pH meter acts like a voltage measuring solutions. The unknown concentration, x,
device designed for use with high-resistance was found to be 2.07 ppm from the graph.
electrodes. The effect of all the common
interferences and activity effects can be
overcome by addition of a total ionic
strength adjustment buffer (TISAB) to the
standard and sample solutions.
Sources of error include fluoride ion
activity changes due to the ionic strength of
solution, temperature, which can affect the
measured potential through the Nernst
equation which governs the electrode
potential response and through the several
The commonly used reference equilibria that fluoride may have with
electrode is the saturated calomel electrode. species present in solution, and substances
It is designed to make measurements with that complex fluoride in solution.
high-resistance electrodes. Conclusion

Interpretation Potentiometric methods relate the


potential generated at an indicator electrode
The potential data obtained from the to the concentration of an analyte in
pH meter readings is shown below with its solution. The unknown concentration of the
corresponding concentration. drinking water was obtained from the
graphical visual from the experimental data.
Potential (mV) Concentration (ppm) It was found out to be 2.07 ppm by using the
113.4 0.5 method of linear regression for accuracy.
100.9 1
84 2 References
82.1 x
60.5 5 1. Christian, G.D., Analytical Chemistry, 6th
edition, New Jersey, John Wiley, 2004.
2. Skoog, D. A., and Leary, J. J., Principles
of Instrumental Analysis, 4th edition,
Saunders, New York 1992.

3. Harris, D.C., Quantitative Chemical


Analysis, 3rd edition, Freeman, New York,
1991.