Chemistry 209 – Laboratory Manual - Fall 2021 Experiment #1 - Page 1 of 6

Experiment 1: Kinetics of the Iodine-Clock Reaction

What lab skills will you practice? What chemical concepts will you
• Collecting data in a timed experiment apply?
• Preparing solutions in volumetric • Using the method of initial rates to
glassware determine rate laws (Essential Skill 5)
• Examine experimental kinetic data
What report writing skills will you use? Reminders:
• Recording data and observations • Complete the pre-lab quiz with a minimum
• Presenting data and results in tables grade of 60% and flowchart at least one
• Answering introduction and discussion hour before lab
questions • Print & bring all of Experiment 1 to the lab

Objective
In this experiment, you will use the method of initial rates to determine the rate law for an iodine clock reaction.

Introduction
Kinetics and Pseudo-Order Conditions
As you have seen in class and in your textbook (Silberberg sections 14-2 & 14.3), the rate of reaction can be
related to the reactant concentrations through an expression called the rate law for a particular reaction. For the
iodine clock reaction studied in this experiment the general form of the rate is:

𝑅𝑎𝑡𝑒 = 𝑘[𝐻 + ]𝑥 [𝐼 − ]𝑦 [𝐻2 𝑂2 ] 𝑧 [1]

Where: k is the rate constant for the reaction (temperature dependent)

x is the order with respect to H+
y is the order with respect to iodide
z is the order with respect to hydrogen peroxide
We assume that p and n are whole numbers (most commonly 0, 1, or 2).

In this experiment you will determine the values for k, y and z.

Solving a system with four unknown variables is possible but is much easier if the experiments are designed so
that only one variable changes at a time. Since k is already a constant value, we will control the reactant
concentrations in order to manipulate the variables in the equation. You will approximate a constant [H+] by
using a large excess of this reagent. Since the [H+] is so much larger than the [I-] and the [H2O2] it remains
effectively constant, while the relative changes in [I-] and the [H2O2] are very large.

If we make the (reasonable) assumption that [H+] is constant under the conditions described above, we can
rewrite Equation [4] as:

𝑅𝑎𝑡𝑒 = 𝑘′[𝐼 − ]𝑦 [𝐻2 𝑂2 ]𝑧 [2]

Where: 𝑘 ′ = 𝑘[𝐻 + ]𝑥

The constant k’ is a pseudo-order constant – it behaves and can be treated as if it were a rate constant for a
reaction of orders of y and z, but it is not a true rate constant because its value depends on the concentration of a
reactant (in this case, [H+]).
Reactions
+
2𝐻(𝑎𝑞) −
+ 2𝐼𝑎𝑞 + 𝐻2 𝑂2(𝑎𝑞) → 𝐼2(𝑎𝑞) + 2𝐻2 𝑂(𝑙) [3]

𝐼2(𝑎𝑞) + 2𝑆2 𝑂32−(𝑎𝑞) → 2𝐼(𝑎𝑞)

−
+ 𝑆4 𝑂62− (𝑎𝑞) [4]

Iodine clock reactions typically consist of two reactions occurring at the same time in a cyclic manner1. The first
reaction [3] is slow oxidation reaction1, which is the rate determining step. The second reaction [4], a reduction,
occurs quickly1. Once the thiosulfate – our limiting reagent – is consumed, Reaction [4] can no longer proceed,
and the I2 produced by Reaction [3] begins to accumulate in the system, showing a characteristic yellow-brown
colour.

In the “demonstration” version of the Iodine Clock reaction, an indicator such as starch or thiodene is often added
to make this colour change more visible: I2 binds to the indicator, producing a deep black-blue colour. Since this
happens very quickly once the thiosulphate is consumed, the colour change is quite dramatic.

Method of Initial Rates

In order to determine the rate law for the iodine clock studied, the rate of the reaction with respect to the
appearance of I2 will first be determined. This will be done by relating the time required for the appearance of I2
(yellow colour) to be visible to concentration of I2.

1 𝑚𝑜𝑙 𝑟𝑥′𝑛 ∆[𝐼2 ]

𝑅𝑎𝑡𝑒 = ×
1 𝑚𝑜𝑙 𝐼2 ∆𝑡

Using a modification of the method of initial rates you will have seen in class, you will determine the order of both
I- and H2O2 in the pseudo-rate law. Rather than measuring the true initial rate, in this experiment we assume that
the average rate for the reaction will follow the same trends in rate (e.g. for a first order reaction doubling the
concentration doubles the rate). The ‘end’ of the reaction is taken as the moment the thiosulphate is completely
consumed and excess iodine begins to build up (see Reaction section below). In this method:
• While [I—] is constant, if [H2O2] is doubled:
o If the rate does not change, the reaction is 0th order with respect to H2O2.
o If the rate doubles (half the time to completion), the reaction is 1st order with respect to H2O2.
o If the rate quadruples (1/4 the time to completion), the reaction is 2nd order with respect to H2O2.
By extension, you can make the same determination for the order with respect to [I—] (found while H2O2 is
constant), or if the concentration is not exactly doubled (if it is increased by 1.5 times or 3 times, for instance).

References
1. Sattsagi, P.D. A Microscale Approach to Chemical Kinetics in the General Chemistry Laboratory: The
Potassium Hydrogen Peroxide Iodine-Clock Reaction. J. Chem. Educ. 2011, 88(2), 184-188.
2. Barrera, L.A., Escobosa, A.C., Alsaihati, L.S. and Noveron, J.C. Conducting a Low-Waste Iodine Clock
Experiment on Filter Paper to Discern the Rate Law, J. Chem. Educ. 2019, 96(1), 165-168.
3. Rennie, S., Experimenting in Kinetics. Chemistry 402 Final Report 2019, 20 pp
Chemistry 209 – Laboratory Manual - Fall 2021 Experiment #1 - Page 3 of 6

Experimental Procedure
For this experiment you will work in pairs.
Each partner must submit an individually written lab report.

Before beginning, sign out a Supplementary Equipment Tray (SET) from your
TA, containing:
• 1 digital stopwatch
• 2 – 25.00 mL volumetric flasks with stoppers
• 3 medicine droppers
By ‘signing out’ this equipment, you are responsible for it until you and your
TA sign it back in at the end of lab.

Part 1: Getting Ready

Label all beakers and
flasks with the 1. Obtain 5 pieces of filter paper from your TA.
solution and 2. Record the exact stock concentrations of the reactants into Table 2.
concentration they
contain. Everything is 3. Obtain one pump (12.5 mL) of Na2S2O3 in a 50 mL beaker.
a clear liquid. 4. In a 50 mL beaker, obtain 10 mL of 0.2 M KI.
5. Obtain one pump (12.5 mL) of 0.1 M H2O2 in a 50 mL beaker.
Note: Do not tamper
6. Divide the filter paper into quarters.
with the pumps!

Part 2: Preparation of Solutions

1. In a 25.00 mL volumetric flask add one pump (12.5 mL) of 0.1M H2O2 and
dilute to the mark with RO water.
2. In a 25.00 mL volumetric flask add one pump (12.5 mL) of 0.2M KI and dilute
to the mark with RO water.

6M HCl is 3. To the 0.05M and 0.1M hydrogen peroxide solutions add 10 drops of 6M
corrosive! HCl. Mix well.

Part 3: Run 1
1. Place your watch glass on top of your white tile.
2. Place a piece of filter paper on top of a watch glass. Label the filter paper
with an ‘x’ to mark the center or target area for your reagents (see Figure 1
on next page).
3. Add the reagents as shown in Table 1 on the target you marked on the filter
paper. Your medicine dropper should be no more than an inch from the
filter paper.
4. Start the timer as soon as you add the first drop H2O2.
5. Record the time when you see the first sight of brown on the filter paper.
6. Repeat steps 1-5 for this run four more times, cleaning the watch glass and
using a new filter paper for each trial.
Chemistry 209 – Laboratory Manual - Fall 2021 Experiment #1 - Page 4 of 6

Figure 1: Appearance of filter paper over time.

From left to right: Before reaction has started; first hint of brown appears; too much brown (after the point time
should be recorded); an extreme example of brown.

Table 1: Reagents for Runs 1-4

Na2S2O3 KI KI H2O2 H2O2 For the eyedroppers

0.005M 0.1M 0.2M 0.05M 0.1M given, 1 drop ≈ 10 μL
Run 1 1 drop 2 drops ----------- ----------- 2 drops
Run 2 1 drop ----------- 2 drops ----------- 2 drops Be sure to add the
reagents in order as
Run 3 1 drop ----------- 2 drops 1 drop -----------
listed from left to
Run 4 1 drop ----------- 2 drops ----------- 1 drop right.

Part 4: Runs 2-4

1. Repeat the steps in Part 3 for runs 2-4. You should have 5 trials per run.

Part 5: Clean up
1. Put your used filter paper into the filter paper waste container in the fumehood.
2. All solutions can be disposed of in the inorganic waste (white jug with the CHEM 209 sign).
3. Clean your glassware and medicine droppers and return your SET to your TA.
Chemistry 209 – Laboratory Manual - Fall 2021 Experiment #1 - Page 5 of 6
TA Initials:
Procedure Flow Chart – Pre-Lab Assignment
Fill in the flowchart below with all relevant experimental details:
Chemistry 209 – Laboratory Manual - Fall 2021 Experiment #1 - Page 6 of 6

Data Tables

Table 1: Reference Values Given in Lab

Quantity Value

[Na2S2O3] stock

[KI] stock

[H2O2] stock

k’

Table 2: Reaction Times - Time taken from first addition of H2O2

to first show of brown colour

Run # Trial 1 (s) Trial 2 (s) Trial 3 (s) Trial 4 (s) Trial 5 (s)