Practical exercises from Medical Chemistry Volumetric analysis

Volumetric analysis

Contents
Introduction ....................................................................................................................................................... 1
1. Iodine determination in Lugol solution ......................................................................................................... 2

Introduction
Volumetric analysis (titration) is a quantitative method of the chemical analysis. Amount of
substance of the analysed component of a solution is determined based on the used volume of the
reagent with a known concentration (titrant). During titration the titrant (B) is added to the analysed
sample (A) until the reaction proceeds quantitatively (in stoichiometric ratio) and the equivalence
point is reached. At the equivalence point the amounts of the analysed substance (nA) and the titrant
(nB) divided by corresponding stoichiometric coefficients (νA a νB) are equal:

nA nB
=
νA νB

The chemical reactions which are often used for volumetric analysis proceed in stoichiometric ratio
1:1, for which following formula can be applied at equivalence point:

nA = nB

In this case, based on the known volume of the solution containing analysed substance (VA) and the
volume of the titrant (VB) with a known concentration (cB) used to reach the equivalence point, the
concentration of the analysed substance (cA) can be calculated according to the formula:

cB VB
cA =
VA

Indicators are substances which can detect the endpoint of the reaction between analysed substance
and titrant (equivalence point) by the change of their colour.
According to the character of reaction which proceed between analysed substance and titrant,
volumetric analysis can be divided into following types:
1. Acid-base – involving exchange of protons (H+)
2. Oxidation-reduction – involving exchange of electrons
3. Precipitation – involving formation of insoluble products
4. Complexometric – involving formation of coordination compounds

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Practical exercises from Medical Chemistry Volumetric analysis

1. Iodine determination in Lugol solution

Iodine forms nonpolar molecules I2, which are sparingly soluble in water. Therefore, for the most
applications, it is used in form of an ethanolic solution (iodine tincture) or dissolved in a solution of
−
potassium iodide (Lugol solution). In the Lugol solution, the reaction between I2 a I produces
−
triiodide anions I3 , which are responsible for its dark yellow colour:

I2 + KI → KI3

Total content of iodine in the Lugol solution can be determined by an oxidation-reduction titration
with sodium thiosulphate, during which the iodine is reduced into iodide anions while simultaneous
oxidation of sodium thiosulphate into sodium tetrathionate takes place. Iodine is usually written in
the reaction in its molecular form for simplification:

I2 + 2 Na2S2O3 → NaI + Na2S4O6

Starch can be used as an indicator for the detection of the equivalence point, while it forms a
characteristic blue-violet colour in presence of triiodide anions. Concentration of atomic iodine in
the solution can be calculated based of the used volume of the thiosulphate according to the formula:

c(Na2 S2 O3 ) V(Na2 S2 O3 )
c(I)=
V(I)

Materials
pipettes, volumetric cylinder, stand, clamps, holders, burette, titration flasks, Lugol solution,
Na2S2O3 (c = 0.01 mol/L), starch

Procedure
1. Pipette 10 mL of the Lugol solution (unknown concentration) into a titration flask.
2. Add 10 mL of distilled water to the solution.
3. Add 3 drops of starch and stir the content of the flask.
4. Titrate the mixture with the solution of sodium thiosulphate until the colour changes from dark
blue-violet to transparent.
5. Record the used volume of Na2S2O3 into the table in observation.
6. Repeat the whole procedure (2-times in total) and calculate the average volume. Calculate the
concentration of iodine according to the formula (see above) using the average volume.
7. Write the determined iodine concentration to the conclusions (take the dilution into account!)

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Practical exercises from Medical Chemistry Volumetric analysis

Observation:

Titration flask Volume of Na2S2O3 (mL) Average (mL)

1
2

Conclusions: