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Instrumental Analytical Methods

Lab Report 2013


Anastazija Ristovska
Experiment 11
Potentiometric Titration of a Mixture of Chlorides and Iodides

The purpose of this experiment was to determine the mass of chloride and iodide in a
mixture of the two ions through titrating a known volume of their solution with a silver nitrate
solution of known concentration, recording the changes in potential of the solution as a function
of volume silver nitrate added, and eventually constructing a plot of the dependence on E/V
on the volume of titrant added. From the constructed graph the titration end points of iodides
and chlorides was found. The volumes of titrant spent at these end points were used to infer the
concentration of chloride and iodide in the unknown-concentration solution. Silver and calomel
electrodes were used in the reaction, alongside a potassium nitrate salt bridge.
Throughout these experiments weve been using several different methods of spotting
the titration endpoints. Some have been visual changes; however, other types of physical changes
have been employed as well, such as a pH change, resistance change, or a change in potential. In
the determination of the endpoints in the titration of a mixture of halides the most efficient
method of determining the titration end point is a change in potential. In fact, a pH metric
titration is likewise a method that relies on measuring the change in potential across two
electrodes, but the end results on the instrument are interpreted on the pH scale. Electric
potential is defined as the amount of work needed to move a unit charge from a reference point
to a specific point against an electric field. The units in which our results were recorded were mV
and were in the range from 10 to 400 mV. The titration end points were determined by finding
the two maximum values of /V, i.e. the largest change in potential per change in volume of
titrant added in each titrant addition.
In our titration the calomel electrode maintained a constant potential regardless of what
the concentrations of the species in the solution was and how they changed. It was the silver
electrode that was sensitive to the halides concentrations, and the voltage across the two
electrodes was a function of the concentrations of the species. The half reactions were:
2I- I2 + 2e-

E0= + 0.54V

2Cl- Cl2 + 2e-

E0= + 1.36 V

Ag+ + e- Ag

E= + 0.800 V

Since I was nitrating the mixture of chlorides and iodides with silver nitrate, as the
titration progressed the concentration of silver ions changed by several orders of magnitude. The
following precipitation reactions will take place due to the low solubility product of silver
chloride and silver iodide:
AgCl Ag+ (aq) + Cl- (aq)
AgI Ag+ (aq) + I- (aq)

Ksp = 1.6 10-10


Ksp = 1.5 10-16

Because of the fact that silver iodide has a much lower solubility product than silver
chloride, it will be silver iodide that will precipitate first. The change in potential was in no way
influenced by the chloride and iodide half reactions, only by the change in silver ion
concentration. Therefore by increasing the concentration of silver in the beginning the potential
started decreasing until at one moment it began turning negative and continued decreasing. The
points when there was a largest drop in potential are the points of precipitation of silver iodide
and silver chloride. The first point of large change in potential signified the precipitation of silver
iodide, whereas the second point of large change in potential per volume titrant added was the
precipitation point of silver chloride.

200
/V

180

10ml

160
140
120

3,5ml

100
80
60
40
20

0
0

10

12

14

In the he above plot are displayed the results of the first titration in which 0,5ml of
titrant were added at a time. There are less data points and therefore we could only locate the
narrower ranges in which there was going to be a big change in potential of the solution. At
these points of change in electric potential the iodides and then the chlorides were completely
reacted with the newly introduced silver ions from the titrant.

In the second plot are displayed the results from the second titration in which, in the
range where during the first titration it was noted that a large potential change would occur,
smaller volumes of titrant, 0,1ml at a time, were added (using a microburette that allows the
addition of such small volumes). In this plot the more precise points were detected at which the
iodides and chlorides were reacted with silver ions to form salts that almost dont dissociate nor
dissolve in water.

m(I-)=0,0033L*169,87g/mol*0,0520454mol/L*5= 0,14588g=145,88mg
m(Cl-)=0,0098L*169,87g/mol*0,0520454mol/L*5= 0,43321g=433,21mg
Therefore, the total masses of iodide and chloride in the volumetric flasks are 145,88mg
and 433,21mg respectively.

800
/V
700

3,3ml

600

/V

500
400
300

9,8ml

200
100
0
0

10

12

14

Volume 0.052M AgNO3 added (ml)

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