Instrumental Analytical Methods

Lab Report 2013

Anastazija Ristovska
Experiment 3
Colorimetric Titration
Determining the Concentration of Iron via a Colorimetric Titration with Sulfosalicylic Acid

The purpose of this experiment was to determine the concentration of iron through a
colorimetric titration. As the name suggests, we were supposed to do something nearly
impossible to measure color. But is it really that impossible? The goal of this lab was to show
that, to the human eye it is indeed impossible to determine the exact concentration based on
color, however there are sophisticated instruments that can measure the energy and wavelength
of photos and light energy at particular frequencies in order to determine the exact color and
color is just light at a particular frequency in the visible spectrum.
We were given a beaker with unknown concentration of iron and a particular pink color
obtained by having the iron react with sulfosalycilic acid C7H6O6S in a complexiometric titration.
This beaker was kept intact, and in another beaker we were attempting to reach the same color
by reacting known amounts of sulfosalycilic acid and iron. When we thought the same color was
reached, we recorded the amount of iron spent and concluded that this was the amount of iron
present in the initial (intact) beaker. We were aware though that this was most likely not the exact
amount, and the exact amount could only be determined by using sophisticated instrumentation
that will be able to capture the exact wavelengths of the colors of the two beakers, and when
these two colors are at the exact same wavelength then the pH of the solution is the same,
whereas when the intensity of the color and light of particular wavelength emitted by the two
beakers is the same, then the two solutions have iron in the same concentration.
Sulfosalycilic acid is known as an analytical reagent useful for determining iron
concentration because it gives characteristic colors due to compexation. The colors can vary as
function of pH and concentration. The pH affects the wavelength, i.e. the color shade of the
solution, and the concentration of iron affects the intensity of light. So what we were actually
trying to achieve using the naked human eye was a same intensity of light of the same
wavelength of the two solutions. The change in color at different pH indicates that different
types of complexes are forming. When acidic the solution can be violet, deep red, or rose,
whereas when alkaline the complex formed makes the solution yellow. That is over 150nm of
wavelength variation in the 750nm-600nm range. The only way this variation can be explained is
through different chemistry of the complex. Our solution was acidic and was expected to have
about pH=1, given the amount of acid dissolved: 2ml highly concentrated HCl in 200ml
solution, giving approximately 0.14M solution of HCl; pH=-log[0.14]=0.85. The color seemed to
be in the 725-750nm range, with a low intensity.
1

Figure 1 An Example of Sulfosalycilic Acid Iron Complex Formation

Titration Beaker 1
Titration Beaker 2
Titration Beaker 3

Volume Fe3+ soln.

(24g/ml) spent (ml)
8,1
4,2
5,15

Control Solution 1
Control Solution 2
Control Solution 3

Mass of Iron (in g)

194,4
100,8
123,6

The mass of iron was determined in three different control solutions. In titrating the first
solution the volume of (24 g/ml) iron solution spent was 8.1ml and the mass of iron in this
control solution was thus found to be 194.4 g. We spent 8.1ml of iron to achieve what seemed
to be the same intensity of iron as the control solution, and therefore we could only state that the
approximate mass of iron in control solution one was 194.4 g. Similarly for titrating the second
beaker 4.2ml iron solution were spent and the concentration of iron in the second control
solution was calculated to be approximately 100.8 g. The volume of iron spent in titrating the

1.

Spectrophotometric Studies on Complex Formation with Sulfosalicylic Acid. I. With Iron III.
Robert T. Foley and Robbin C. Anderson. Journal of the American Chemical Society 1948 70 (3),
1195-1197
1

third beaker was 5.15ml, and therefore the mass of iron in the third control solution was found
to be 123.6ml.
In our reaction, adding HCl and thus changing the pH of a sulfosalicylic acid solution
causes the formation of a chromophore group in the structure of the sulfosalicylic acid solution
and its complex with iron.
Both beakers used ought to be of same volume due to the need to relatively compare the
total final volume of the solutions. However due to manufacturing obstacles beakers are almost
never of the exactly precise same volume and thus same beaker volumes are needed only for
approximation of the volumes of the control solution and the titrated solution.
We conclude that the exact light intensity could only be determined through
spectrophotometric means. The human eye is simply not capable of counting photons at specific
wavelengths, or counting photons at any wavelength.