CHM130

Determination of Mass Percentage of Oxygen in KClO3

Introduction

In this experiment, we will determine experimentally the mass percent of oxygen in potassium chlorate, KClO3, and
compare our experimental value with the value calculated from the chemical formula. Several of the skills we learn
and practice, including proper safe heating techniques, heating to constant mass, and percent error calculations
using correct significant figures, will be useful in your subsequent science labs and courses.

When heated strongly, KClO3 decomposes according to the unbalanced equation

KClO3(s) → KCl(s) + O2(g) (1)

We will aid the decomposition reaction by mixing KClO3 with a solid catalyst, MnO2. A catalyst is a substance that
speeds up a reaction, by providing an alternate reaction pathway with lower activation energy, but is not consumed
itself.

In Equation 1, notice oxygen is a gaseous product. As such, when we carry out the reaction in a heated test tube,
oxygen gas will escape and will account for the only mass loss in the reaction mixture. If we know our initial mass
of KClO3 and the final mass of the reaction mixture after heating, we can easily calculate by difference the mass of
oxygen liberated by the reaction. According to Equation 1, all of the liberated oxygen comes from KClO3, and
since the other product (KCl) contains no oxygen, the mass of the oxygen produced must be the mass oxygen
contained in our initial sample of KClO3. If we know the mass of oxygen liberated and the initial mass of KClO3,
we can calculate the experimental mass percent of oxygen in our KClO3 sample, Equation 2.

(2)

You will also compare your experimental mass percent oxygen to the actual or “true” value based on the chemical
formula using a percent error calculation, Equation 3.

| |
(3)

Heating to Constant Mass

How do you know when you have heated the KClO3 long enough and the reaction is complete? This is an
important skill in chemistry lab. As long as there are no side reactions or phase transitions, the easiest and most
reliable way to ascertain if a heated reaction is complete is to heat to constant mass: when your recorded mass does
not change between one heating and the next, the reaction is complete. For CHM130 lab, we may consider the
reaction is complete if the mass changes by ≤ 0.005 g between heatings. You will need to go through the cycle of
heating your sample, allowing it to cool completely, and weighing it, several times until you achieve constant mass.

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Procedure
* The first thing to note is the extreme importance of wearing your safety goggles at all times during this lab *

1) Weigh ~0.5g of the catalyst MnO2 and place it into a test tube.

a. The easiest method to weigh and deliver the MnO2 is as follows: crease a piece of weighing paper,
tare it on the balance pan, use a spatula to add ~ 0.5 g MnO2 to the paper, then pour the MnO2
along the crease into the test tube.
b. The exact mass of MnO2 is not important, you will weigh it again in a little bit.
c. Please be careful: MnO2 is a fine black powder that gets everywhere if you spill it.

2) Using an asbestos clamp, clamp the test tube containing the MnO2 to a ring stand, as shown in Figure 1a.
Be sure the opening of the test tube is pointed AWAY from your neighbors.

3) Heat the entire tube using a Bunsen burner with a blue flame (not a blue cone) for about 3 minutes, as
shown in Figure 1b.

a. Your purpose here is to dry the test tube and its contents thoroughly. If you are unsure of how to
use the Bunsen burner, please ask your instructor to demonstrate. Note it is completely safe to
handle the Bunsen burner from the base. The base will not get hot and you will have control of
where you heat.

Figure 1a: Proper clamping of the test tube showing asbestos

4) After heating in Step 3, allow the test tube containing the MnO2 to cool completely.

a. You should never weigh an object when it is hot: not only can you burn yourself, but convection
currents can affect your mass.

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5) When the tube is cool, place it in an appropriate support beaker or flask, as shown in Figure 2. Weigh
everything together, record the exact mass as “Mass of Container” on your data table.

a. As always, please read and record all digits from the balance. We use the support beaker or flask as
part of the container as a convenient way to hold the test tube upright for subsequent weighings.
b. A note on handling: our balances are precise enough that oils from your skin can add mass, so try
to handle glassware with a paper towel or gloves as an interface between your skin and the glass.
This level of care is probably not necessary in CHM130, but you may want to be aware of it if you
will be continuing your science education.

Figure 2: The container comprising the test tube, MnO2, and the support beaker or flask

6) Add about 1.5 g of KClO3 to the test tube, using the “creased weighing paper method” as described in Step
1.
a. When using the spatula to remove the KClO3 from its bottle, try to get fine powder and avoid big
chunks. Fine powdered KClO3 will mix better with the catalyst and react faster.
b. When pouring your KClO3 into the test tube, try to make sure most of it goes to the bottom (with
the MnO2) and very little is stuck to the sides.

7) When you have delivered the KClO3 to the test tube and the tube is placed back into its support beaker,
weigh the container and test tube together. Record this mass as “Mass of Container + KClO3” on your
data table.

8) Back at your lab bench, roll the test tube in your fingertips a few times to mix the KClO3 and MnO2.

9) Spread out the KClO3/MnO2 mixture by gently rolling until it is about 1/3 of the way up the test tube, as
shown in Figure 3.

a. If your mixture is spread out, and not all in the bottom, the reaction will go more quickly.

10) Clamp the test tube as shown in Figure 3. As you prepare to heat, aim the opening of the test tube AWAY
from your neighbors.

Figure 3: Reaction mixture of KClO3 and catalyst MnO2 spread ~1/3 to 1/2 the length of the test tube
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11) Hold the Bunsen burner by the base and start moving a blue flame (not a blue cone) over the portion of the
test tube containing the reaction mixture.

a. When the reaction starts, it will look like the solid mixture is boiling as molecular oxygen is
formed and escapes. If the “boiling” gets too vigorous, move the flame away from the test tube.
You are in control of the reaction.

12) Once the “boiling” has stopped, adjust your Bunsen burner flame to a blue cone and heat the entire test tube
strongly for about 5 minutes.

a. Make sure you move the flame all over the test tube. If it looks like there are unreacted bits of
material, you may hold the flame under the bits and watch them react.

13) After the test tube has cooled completely, place it in the support beaker and record its weight carefully in
the “1st heating” block of your data table.

14) Return to your lab bench, clamp the test tube as you did in Figure 3, and heat strongly with a blue cone
flame for 5 more minutes. Allow the tube to cool completely and then record its weight carefully in the
“2nd heating” block of your data table.

a. Notice your data table contains columns for up to 5 heating cycles, though if you heat strongly and
carefully it may only require 3, or even 2, heating cycles. You will repeat Step 14 until you record
a ≤ 0.005 g mass change between subsequent heatings.

15) Once your heating is complete (i.e. you have “heated to constant mass”), record your final heating mass as
“Mass of Container + KCl” on your data table.

16) Complete the rest of the data table and finish your calculations.

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Name_____________________ Section____________________ Lab Partner____________________________

Mass Percent of O in KClO3 Report Sheet

Experimental Data

a) Initial Mass Data:

Mass of Container (grams)

Mass of Container + KClO3 (grams)

Mass of KClO3 (grams)

b) Heating Data:

1st heating 2nd heating 3rd heating 4th heating 5th heating

c) Final Mass Data:

Mass of Container + KCl (g)

Mass of Oxygen released (g)

Calculations

a) Mass Percent Oxygen from Experimental Data

b) Mass Percent Oxygen from the Chemical Formula for KClO3

c) Calculate the percent error of your experimental percentage oxygen value

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Advance Study Assignment

1) Balance the chemical reaction for the thermal decomposition of potassium chlorate

2) Is the reaction in this lab exothermic or endothermic? How do you know?

3) Read the procedure section and list 3 main safety considerations for this lab experiment

4) a) A lab student decomposed 1.241 g of AlCl3 and was left with 0.263 g of Al. From the experimental data,
what mass of Cl was in the original sample?

b) According to the student’s data, what is the experimental weight percent of Cl in AlCl3?

c) According to the chemical formula for AlCl3, what is the actual (true) weight percent of Cl in AlCl3?

d) To the correct significant figures, what is the percent error of the student’s weight percent of Cl?

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