Experiment 7

The Empirical Formula of Magnesium Oxide

Reference
Experiments in General Chemistry, R.A.D. Wentworth, 2nd Edition, 1990, Houghton
Mifflin Company, pp. 69-79, Chemistry 101 Laboratory Manual, Providence College

Objective
To determine the empirical formula for magnesium oxide.

Materials Needed

1. 0.1 gram of magnesium ribbon (about 4 inches long)

2. Balance
3. Desiccator
4. Bunsen burner
5. Tongs
6. Crucible
7. Lid
8. Wire gauze

Background
What happens when an element is heated in air?

Molecular oxygen, alone or in air, is a very reactive substance when it is heated. Many
elements will react with it. When an element reacts, it combines chemically with
molecular oxygen, an oxide (a compound of the element with oxygen) is formed. This
process is called combustion.
heat
Magnesium + oxygen  Magnesium oxide

Molecular nitrogen, the chief component of air, is a rather unreactive substance, even at a
high temperature. Only the more reactive metals will react and combine chemically with
molecular nitrogen during heating. When nitrogen does react with an active metal, a
nitride (a compound of the element with nitrogen is formed.

heat
Magnesium + nitrogen  Magnesium nitride

Although the amount of molecular nitrogen in air is approximately four times the amount
of molecular oxygen, more oxide than nitride will be formed when an active metal is
burned in air. The reason for this is the superior reactivity of molecular oxygen.

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Concept of this experiment
In this experiment, after a known mass of magnesium is combusted, the product
will consist of magnesium oxide and smaller amounts of magnesium nitride. Water will
convert the nitride to magnesium hydroxide with the liberation of ammonia. Heat will
cause the conversion of hydroxide with the loss of gaseous water.

heat
magnesium nitride + water  magnesium hydroxide + ammonia

heat
magnesium hydroxide  magnesium oxide + water

Since the product will consist solely of magnesium oxide after this treatment, you
can determine the mass of oxygen that is present in the magnesium oxide from its mass
and the original mass of the magnesium. The law of definite proportions and the concept
of the mole will lead you to the method by which you can determine the empirical
formula of the magnesium oxide.

Procedure
Part I: Getting started

1. Obtain a crucible and lid. Wash, rinse, and dry them.

2. Place the covered crucible in a clay triangle on an iron ring attached to an

aluminum rod. Adjust the height of the ring so that the bottom of the crucible will
be the hottest part of the burner flame.

Part II: Heating the Crucible to Constant Mass

3. Heat the covered crucible strongly for about 10 minutes. The bottom of the
crucible should glow red-hot during this time. The heating should be sufficient to
thoroughly dry the crucible. Shut off the burner, and allow the crucible to cool
for a few minutes, but do not let it cool to room temperature. Using crucible
tongs, transfer the warm crucible to a desiccator and allow the crucible to cool to
room temperature in the closed desiccator. This will prevent the reabsorbtion of
water.

Caution: Avoid burning your fingers. Do not touch the crucible or iron ring during
the experiment. Use the tongs to handle the crucible. Do not place hot objects on the
bench top.

4. When the covered crucible is cool, transfer it to the balance using the crucible
tongs while holding a wire gauze under the crucible. If you must wait to use the
balance, do not place the crucible directly on the bench. Put it on the wire gauze
or leave it in the clay triangle.

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5. Obtain and record the mass of the covered crucible. (NOTE: It is a good idea to
record the mass of the lid alone at this point in case the lid breaks and a
replacement is needed.)

Part III: Synthesis of the magnesium oxide compound.

6. Obtain about 0.1 g (about 4 inches long) of magnesium ribbon. Clean the surface
with sandpaper until the magnesium is shiny.

7. Fold the magnesium ribbon into a loose ball, and place the magnesium ribbon in
the crucible. Do not fold the ribbon too tightly. The best results will be obtained
when the surface of the ribbon is as exposed as possible.

8. Cover the crucible, and record the mass.

9. Return the crucible to the clay triangle, using the crucible tongs and the wire
gauze. The lid should be in place. Brush the bottom of the crucible with the
flame for about 2 – 3 minutes. Next, place the burner on the lab bench and heat
the crucible in the hottest part of the flame for another 3 minutes.

10. Use crucible tongs to lift the lid carefully by a slight amount to allow more air to
enter the crucible. This procedure allows a small amount of fresh air to enter the
crucible. Do not open the lid too far, as this will allow the metal to enflame. The
metal shall glow brightly without bursting into flame. Otherwise, flames from the
metal will carry part of the solid oxide out of the crucible and into the air as white
smoke, which will affect your results.

11. Continue to introduce small amounts of air into the crucible by repeating step 11
every few minutes until no metal is evident and no glow is observed when the lid
is lifted. The accuracy of your experiment depends on the care with which you
carry out the combustion process, and this cannot be hurried.

12. Next, introduce larger amounts of air by placing the lid on the crucible so that the
lid is covering less than half of the crucible contents. Heat the crucible contents
strongly for 15 to 20 minutes.

13. Allow the covered crucible and its contents to cool on the clay triangle.

14. Remove the lid and set it on the wire gauze. Add deionized water (about 5 mL)
from a pipet directly to the crucible contents. Be sure that water contacts the
entire sample in the crucible.

15. Replace the crucible lid so that it is slightly ajar. Heat the crucible by brushing it
with the flame until the contents are dry. Next, heat the crucible strongly for 8 to
10 minutes to convert the magnesium hydroxide to magnesium oxide.

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 16. Allow the completely covered crucible and its contents to cool as described in
step 3.

17. Obtain and record the mass after the crucible has cooled.

18. Heat the covered crucible again strongly for about 3 minutes. Obtain and record
the mass after the crucible has cooled.

19. You will have obtained “constant” mass if the two measurements agree to 0.01 g.
If not, repeat step 19 until the two successive measurements differ by no more
than this amount.

Part IV: Disposal

20. Dispose of your product by first dissolving it in 10 ml of 2 M HCl (the black

precipitate probably won’t come out of the crucible).

21. Place the solution in the waste container.

22. Clean the crucible and the lid.

Results
Mass of empty crucible and lid

Mass of lid alone

Mass of crucible, lid, and magnesium

Mass of crucible, lid, and magnesium oxide

Average mass of empty crucible and lid

Mass of magnesium oxide

*To be used only if lid is broken during the course of the experiment and a replacement
lid is needed.

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Calculations and interpretations
1. Using your results, determine the empirical formula of magnesium oxide. Show
all of your reasonings and calculations.
2. Write correctly balanced chemical equations for the following reactions. Do not
forget to include physical states.
a. magnesium with molecular oxygen
b. magnesium with molecular nitrogen
c. magnesium nitride with water
d. heating magnesium hydroxide

Questions

1. What is the law of definite proportions, and how does it apply to this experiment?
Identify the assumption of Dalton’s atomic theory that explains the law of
constant composition. Cite any references used.
2. What is the limiting reagent in this reaction: magnesium or oxygen? Explain your
answer.
3. How would your determination for the empirical formula be affected by the
following sources of error? Be specific – would you have a larger or smaller ratio
of magnesium to oxygen? Explain your answer completely.
a. The magnesium was not allowed to react in sufficient air.
b. The magnesium nitride was not converted to magnesium oxide.
c. During the reaction, the magnesium metal burst into white flame and
white smoke escaped from the crucible.
4. Only the empirical formula can be calculated from the percentage composition
data. For molecular substances, what additional information is needed to convert
the empirical formula to molecular formula, and how is this conversion carried
out? Explain.
5. A sample of iron oxide weighing 1.60 grams is heated in a stream of hydrogen gas
until it is completely converted to 1.12 grams of metallic iron. What is the
empirical formula of the iron oxide. Show your calculations and reasoning.

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Part 2 – Calculation (while you are waiting)
Reference
Chemistry 101 Laboratory Manual, Providence College

Objective
To determine the cost of a single atom in a roll of aluminum foil. Your answer
should be correct to three significant figures and be expressed in scientific notation.

Given:
The teacher will give you a 8” x 8” square of aluminum foil and will tell you the
cost and the amount of square feet of aluminum foil in the box.

Report:
Each group should have a report showing measurements and calculations as
appropriate and as described above.