October 1st, 2010

Chemistry Laboratory 11B - The Iodine Clock Reaction

Shawn Yuan

Purpose:
The purposes of this laboratory were to:
- observe and record the effect of changing the concentration of a reactant on
the rate of reaction; and to
- observe and record the effect of changing the temperature of a system on
the rate of a reaction.

Materials and Methods:

The materials and methods for this laboratory followed the procedures laid out in Experiment
11B on pages 149~158 of Essential Experiments for Chemistry by Morrison and Scodellaro with
the following exceptions:
- only two beakers were used to make water baths instead of four;
- volumetric pipettes were used instead of dropping pipettes;
- 20 mm × 200 mm test tubes were used instead of 18 mm × 150 mm ones;
- four test tubes were used instead of eight; and
- solutions A and B were mixed by shaking the test tube slightly, instead of
pouring between both test tubes.

Observations:
Part I:
First, approximately 60 mL of solution A and 90mL of solution B were obtained from the front
of the laboratory in 100mL beakers. According to the instructor, solution A contained 0.020M
KIO3 and solution B contained 0.0020M NaHSO3, H2SO4, and starch. Solution A appeared very
clear, its appearance no different than water while solution B appeared very murky, due to the
starch in solution.
Then, four 20 mm × 200 mm test tubes were obtained from the laboratory and placed on a test
tube rack. Using a volumetric pipette, 10mL of solution A was transferred into a graduated

1
 October 1st, 2010

cylinder, then finally into one of the test tubes. In a similar fashion, with a separate graduated
cylinder and volumetric pipette, 10mL of solution B was transferred to a second test tube. The
graduated cylinders and volumetric pipettes were labelled, in order to avoid contamination of
chemicals in other parts of this laboratory.
The contents of test tube A, solution A, was poured into test tube B. From the instant both
solutions came in contact, a timer was started. One partner kept mixing the solutions by swirling
the test tube while the other kept track of the stopwatch. After exactly 11 seconds, the originally
clear mix of the two solutions flashed dark blue. This time measurement was recorded in Table 1,
and the contents of the test tube were poured down the sink, and both test tubes were washed
thoroughly as they were to be reused in future trials.
In order to observe the changes of reaction rate on concentration differences, the concentration
of solution A was to be altered. This was done so by transferring 8.0mL of solution A into the
graduated cylinder and the graduated cylinder was then filled up to the 10.0mL mark using tap
water. The 10.0 mL of diluted solution A was then transferred to a test tube and the trial proceeded
as before. Note that only the concentration of A changed, while 10.0 mL of solution B was always
used. Trials of 6.0mL, 4.0mL and 2.0mL of solution A were then performed, always filled up to
the 10.0mL mark on the graduated cylinder using water. The times for the black-blue colour to
appear was then recorded in Table 1. The results from Table 1 were then copied onto the
blackboard in the front of the laboratory to produce a class data set.

Table 1. Summary of the data obtained for reaction times of the iodine clock reaction while
varying concentration of solution A. The reaction rates are calculated using the average
of the class data in calculations. The complete class data set is included in the back of the
report, on the handwritten observations sheet. These reactions occurred at 25 degrees Celsius.

Volume of Solution A 10mL 9mL 8mL 7mL 6mL 5mL 4mL 3mL 2mL

[IO3-] (M) 0.010 0.0090 0.0080 0.0070 0.0060 0.0050 0.0040 0.0030 0.0020

Reaction Time (s) 11 n/a 13 n/a 18 n/a 30 n/a 57

Average of class 11 13 14 15 18 21 29 35 57
reaction times (s)

Reaction Rate 0.091 0.077 0.071 0.067 0.056 0.048 0.034 0.029 0.018
(s-1)

2
 October 1st, 2010

Part II:
In this portion of the laboratory, both concentrations were remained constant. Five millilitres of
solution A combined with 5.0 mL of water was to be reacted with 10.0 mL of solution B in the
other. The concentration of IO3- in part II would be the same, at 0.0050 M. A water bath of 5.0oC
was produced in a beaker obtained from the laboratory. Using a thermometer, the temperature was
maintained constant at 5oC by adding ice cubes as necessary. This was to ensure the most accurate
measurement possible was obtained. Again, the volumetric pipettes were utilised to measure out
exact amounts of solutions, and pouring them into the test tube using different graduated cylinders.
Both test tubes, the diluted solution A and solution B, were placed in the water bath and left for
approximately 2 minutes, until the temperature of both solutions reached 5oC.
When that occurred, the diluted solution A was poured into the test tube containing test tube B.
The timer was started as soon as the solutions came in contact. The test tube was then swirled a
couple times to mix the solution and was placed back into the water bath after. After 41 seconds,
the clear solution started turning black-blue, very similar to the observations taken in Part I, this
time measurement was then recorded in Table 2. The only difference was that this reaction was
slightly more gradual, occurring over the course of approximately 5 seconds before the colour
remained a constant black-blue. The contents of the test tube were then poured down the sink, and
the test tubes washed thoroughly.
The steps described above in Part II were repeated three more times, using water baths of 15,
25, and 35 degrees Celsius. Less ice cubes were added to make a water bath of 15oC and the
temperature did not need to change for a water bath at 25oC. Finally, a small amount of boiling
water was added to tap water to produce a water bath at 35oC. It was noticed that the reaction
occurred faster with a higher temperature, and the colour change more abrupt and sudden. The
times for each reaction are recorded in Table 2.

3
 October 1st, 2010

Table 2. Summary of data obtained for the iodine clock reaction while temperature was being
altered. The average of the class data is used for calculations and further analysis. The
results obtained in our laboratory are bolded for ease of identification.

Temperature 5°C 10°C 15°C 20°C 25°C 30°C 35°C 40°C

Reaction Times 36,42, 32, 36, 26, 31, 23, 29, 25, 25, 22, 23, 23, 22, 21, 18,
(seconds) 44,42, 30, 42, 30, 28, 31.3, 27, 22, 26.5, 20.7, 12, 19,
41 38.1 29 24, 31 24 18, 28 20, 21 23.2

Average reaction 41 36 29 28 25 24 21 18
time (seconds)

Average Reaction 0.024 0.028 0.034 0.036 0.040 0.042 0.048 0.056
Rate (s-1)

Results:

The reactions performed in this laboratory consists of two main parts. The third reaction is
simply one that would help identify the completion of the previous two reactions by having a
colour change. The first reaction includes IO3- reacting with HSO3- ions to produce I- ions and
SO42- ions. The IO3- is from KIO3 of solution A and the HSO3- ion is from NaHSO3 of solution B;
both the K+ and Na+ are spectator ions and not involved in the reaction. The equation for the first
reaction in this laboratory is the following:
IO3-(aq) + 3HSO3-(aq)  I-(aq) + 3SO42-(aq) + 3H+(aq)
This is the slowest step in the reaction and is therefore the rate determining step. The reason for
this is because this reaction must occur five times to produce 5 I- ions in order for the second
reaction to proceed:
IO3-(aq) + 5I-(aq) + 6H+ (aq)  3I2 (aq) + 3H2O (l)

The third reaction was simply one indicating the completion of the reaction. The starch in
solution B would make the solution turn the black-blue in the presence of I2, as observed. The
reaction would be written as:
I2 + starch  Black-blue color
When the concentration of A is lowered, by increasing volume in this case, the time for the
reaction to occur increased, and subsequently a lower reaction rate. This is because there are less

4
 October 1st, 2010

ions in the same amount of space, successful collisions are less likely to occur. To be more
specific, decreasing the [IO3-] slows down the first step of the reaction, which is the rate
determining step. If the second reaction was slowed down slightly, there would be little to no
effect on the overall reaction rate, since the first reaction would still be the rate determining step.
The rate determining is essentially the slowest step in the reaction chain, and it limits the speed of
the overall reaction.
Shown in Table 1 is the average reaction time with each different concentration of IO3-
(solution A). This relationship between these two figures can be graphed as shown in Figure 1.

Figure 1. Graph of the concentration of IO3- ions in M versus the average reaction rate of the
class, in s-1. Expressed clearly in this graph, as the concentration increases, the reaction
rate also increases.

Concentration vs. Reaction Rate

0.100

0.075

Reaction
0.050
Rate s-1

0.025

0
0 0.003 0.005 0.008 0.010
[IO3-] Moles/L

The same reaction was performed in Part II, but this time the controlled variable was the
temperature. The temperature of a substance is basically the kinetic energy of its molecules.
Therefore, increasing temperature would accelerate the movement of molecules in solution and
therefore create more chances for successful collisions with enough energy to overcome the
activation energy barrier. Faster-moving molecules also mean there will be more collisions,

5
 October 1st, 2010

providing a greater chance for a collision with favorable geometry. All these suggest that reaction
rate will be significantly higher as the temperature goes up. Similarly, if the temperature goes
down, kinetic energy is decreased and therefore there is less chance of having a collision with
correct geometry and also sufficient kinetic energy. As that is essentially what a reaction is, the
reaction rate ultimately goes down. Table 2 proves this fact and the temperature is graphed
against the reaction rate, shown in Figure 2.

Figure 2. Graph of reaction rate of iodine clock reaction vs. temperature of solutions during
reaction. The average reaction rate of the class is used in this graph.

Temperature vs. Reaction Rate

0.060

0.045

Reaction
0.030
Rate s-1

0.015

0
0 10 20 30 40
Temperature (Celsius)

Conclusion:
In this laboratory experiment, it was concluded that the rate of reaction of the iodine clock
increased as the concentration of the reactants go up. This is also true when temperature is
increased. At a lower temperature, when the reaction occurred slower, it was noticed that the color
change was gradual, indicating the reaction wasn’t “sudden” as observed with faster reactions.

6
 October 1st, 2010

Questions:
1. One of the variations of the iodine clock reaction performed in our laboratory is a combination
of hydrogen peroxide, potassium iodide, glacial ethanoic acid, anhydrous sodium ethanoate,
sodium thiosulfate-5-water, and soluble starch. With the exception of the corrosive glacial
ethanoic acid, and the hydrogen peroxide, which is an irritant, these chemicals are relatively non
dangerous. The equation for the first step of this reaction is:
H2O2(aq) + 2I– (aq) + 2H+ (aq) → I2(aq) + 2H2O(l).
Hydrogen peroxide reacts with iodide ions and hydrogen ions in order to form I2 and water.
Following this, thiosulfate combines with the I2 to recycle the iodide ions by the equation
2S2O32–(aq) + I2(aq) → S4O62–(aq) + 2 I– (aq).
Once the limited amount of sodium thiosulfate-5-water is used up, I2 combine with starch to form
the black-blue colour.

The above reaction was found at the following site:

http://www.practicalchemistry.org/experiments/iodine-clock-reaction,55,EX.html: