CHEM 121L

General Chemistry Laboratory

Revision 3.0

The Synthesis of Magnesium Oxide

 Learn how the elemental composition of a chemical compound is determined.

 Learn about the Fundamental Laws of chemistry.
 Learn how to determine the empirical formula of a chemical compound from mass data.
 Learn about the oxides of the metallic elements.

In this laboratory exercise, we will determine the elemental composition of the compound
Magnesium Oxide. We will do this by roasting metallic Magnesium in Air to determine its
Oxygen uptake and therefore the percentages Magnesium and Oxygen in the compound. This
information, used in conjunction with the Atomic Theory of matter, will allow us to then
determine the Empirical Formula of this compound. Comparison will then be made with the
accepted chemical formulas of this and the Oxides of the other Alkaline Earth metals.

To illustrate how the elemental composition of a compound can be determined consider the
combination of elemental Titanium and elemental Oxygen. If powdered Titanium is heated with
a Red Heat in an Oxygen rich atmosphere, the compound Unitrane, or Titanium Oxide, is
produced:

Titanium + Oxygen Unitrane (Titanium Oxide)

Titanium Oxide
https://en.wikipedia.org/wiki
/Titanium_dioxide#/media
/File:Titanium(IV)_oxide.jpg
Titanium
http://images-of-elements.com/titanium-crystal.jpg
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If we start with, 1.576g of Titanium, once the combustion is complete, 2.629g of Unitrane will be
formed. By the Law of Conservation of Mass:

Mass Oxygen Consumed = 2.629g - 1.576g = 1.053g

This gives us the elemental composition of Unitrane:

% Titanium = ( 1.576g / 2.629g ) x 100 = 59.95 %

% Oxygen = ( 1.053g / 2.629g ) x 100 = 40.05 %

By the Law of Definite Proportions, every sample of Unitrane, no matter its source or method of
production, will have this composition. Further, it should be noted only simple mass
measurements are required for this compositional determination; measurements which can be
made with high precision using even a simple pan balance.

According to the Atomic Theory, a sample of elemental Titanium is composed of distinct

Titanium atoms. Also, the Oxygen gas consumed during the combustion is composed of distinct
Oxygen atoms; in this case, in the form of diatomic Oxygen molecules. The Atomic Theory
requires that atoms of Titanium and Oxygen combine in a fixed whole number ratio when
forming the compound. Thus Unitrane has a fixed number of Titanium atoms relative to a fixed
number of Oxygen atoms. In other words, Unitrane can be represented by a Chemical Formula
of the form TixOy; where x and y are simple whole numbers representing the numbers of atoms of
each element in the compound. The ratio of Oxygen to Titanium atoms (y/x) must be consistent
with the composition determined by application of the Law of Definite Proportions. Thus, there
is a distinct relationship between the mass percentage data determined in the laboratory and the
chemical formula of the compound.

In order to relate the chemical formula of a compound to measured mass data, we must be able to
count the atoms in a sample of the compound. This counting is problematic, however; atoms are
too small to be seen, let alone counted, and are too numerous to be counted individually. The
trick is to count them collectively, just like we might count eggs by the dozen. In the case of
atoms, we count them by the mole. The mass per mole of atoms is typically reported as a part of
each element's entry in the Periodic Table.

For Titanium and Oxygen, we have:

1 mole Ti atoms = 47.87 g

1 mole O atoms = 16.00 g
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This mass-per-mole data allows us to convert mass data to numbers of moles, which in turn
allows us to determine the ratios of atoms of each element in the compound. For the Titatnium
combustion data above, we found the elemental composition of Unitrane to be:

% Titanium = 59.95 %
% Oxygen = 40.05 %

Thus, a 100g sample of Unitrane contains 59.95g Titanium and 40.05g Oxygen. In order to
convert this to the empirical formula for Unitrane, we:

1. Convert the mass of each element to numbers of moles of atoms:

# mole Ti atoms = 59.95g / (47.87g / mole) = 1.25 mole Ti atoms

# mole O atoms = 40.05g / (16.00g / mole) = 2.50 mole O atoms

2. Form an appropriate mole ratio:

# mole O / # mole Ti = (2.50 mole O) / (1.25 mole Ti) = 2

3. Interpret the result as an empirical formula for the compound:

2 = 2 / 1 = 2 Oxy. Atoms / 1 Ti Atom

or

TiO2

Note, we have merely determined the ratio of Oxygen atoms to Titanium atoms in Unitrane. This
ratio could equally well be consistent with any of the following chemical formulas; Ti2O4, Ti3O6,
Ti4O8, etc. The smallest of these whole number ratios is the Empirical Formula for the
compound. The chemical formula will be one in this long list of formulas. The chemical
formula represents not just the ratio of atoms within the compound, but the number of atoms that
are bound together to form a Formula Unit of the compound. The Molecular Weight of the
compound is needed in order to resolve the question of which formula is the correct chemical
formula. We will discuss methods of measuring the molecular weight, and how it is used to
resolve the chemical formula question, at a later time. As it turns out, the chemical formula for
Unitrane is in fact TiO2.

Titanium is typical of the elements in that it readily reacts with Oxygen. Oxygen is a non-
metallic element with fairly high reactivity toward the other elements. With the exception of the
lighter Noble Gases (He, Ne, Ar), Oxygen forms compounds with all other elements. With
metals it forms ionic compounds and with non-metals, covalent compounds. Among the ionic
oxides, we speak of normal oxides, peroxides, and superoxides. Normal oxides, such as Li2O,
involve the simple Oxide Ion, O2-. Examples of peroxides and superoxides are Na2O2 and KO2,
respectively. Reactivity towards Oxygen varies significantly; metallic Sodium and white
Phosphorus both immediately react with atmospheric oxygen, but gaseous Nitrogen only
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combines with atmospheric Oxygen under high pressure and temperature conditions. Finally,
oxides of the elements vary in their reactivity toward water. For the Main Group (Group A)
elements, metal oxides are basic in water; for example, Barium Oxide (BaO) forms basic Barium
Hydroxide (Ba(OH)2):

BaO(s) + H2O Ba(OH)2(aq)

Non-metal oxides, on the other hand, are acidic upon reaction in water; for example, Sulfur
Dixodie (SO2) forms acidic Sulfurous Acid (H2SO3):

SO2(g) + H2O H2SO3(aq)

Oxides of elements which are intermediate in their metallic characteristics are amphoteric; both
acidic and basic.

In this laboratory, we will carry out a slow roasting of elemental Magnesium metal to form
Magnesium Oxide. Employing a process similar to that described above for Titanium Oxide, we
will determine the Empirical Formula of this compound.

Magnesium is a moderately reactive Alkaline Earth Metal. (The Alkaline Earth’s comprise
Group 2A of the Periodic Table of the Elements. They are referred to as Alkaline because their
Oxides are basic in Water. The term “Earth” was used by early alchemists to describe non-
metals, the Oxides in this case, that did not melt in their furnaces.) At room temperature,
Magnesium reacts only very slowly with Oxygen and can be kept for long periods of time
without appreciable oxide build-up. At elevated temperatures, however, Magnesium will ignite
in an excess of Oxygen gas, burning with an intensely white flame and producing Magnesium
Oxide. Because of the brightness of its flame, Magnesium is used in flares and in photographic
flashbulbs.

http://simple-science.weebly.com/explaining-what-happens-when-
we-burn-magnesium-metal-8e-task-sheet-l5-7.html

For our purposes, the Magnesium will be heated in a closed crucible, exposing it only gradually
to the Oxygen of the air. Under these conditions, the Magnesium will undergo a more controlled
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oxidation, gradually turning from the shiny metal to grayish-white powdered oxide. The reaction
of interest is:

Magnesium + Oxygen Magnesium Oxide

Elemental Magnesium
http://www.cwmdiecast.com/alloys/magnesium-die-casting.html

Because Air also contains a great deal of Nitrogen gas, a portion of the Magnesium being heated
may be converted to Magnesium Nitride. This will then react, on careful heating, with water to
form Magnesium Oxide and Ammonia. The Ammonia produced by this reaction can be detected
by its characteristic odor.

Magnesium + Nitrogen Magnesium Nitride

Magnesium Nitride + Water Magnesium Oxide + Ammonia

The upshot is that if we are careful, all the Magnesium can be converted into Magnesium Oxide.
Thus, we can determine the percentage by mass Magnesium in Magnesium Oxide. The
remainder, by the Law of Conservation of Mass, will be Oxygen. We will use this measured
mass data to determine the empirical formula of Magnesium Oxide.
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Pre-Lab Safety Questions

1. Should you use a CO2 Fire Extinguisher to put out a piece of burning Magnesium?
Explain.

2. Do a short internet search for a Safety Data Sheet (SDS) for Barium Oxide. What are the
First Aid measures required for Skin and Eye contact with this substance? With ingestion?

3. How will stockroom personnel treat your burns if you get your fingers in the hot Bunsen
Burner flame?
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Procedure
Uncontrolled Combustion of Magnesium

1. Set-up a Bunsen Burner.

2. Obtain a small strip of Magnesium; no more than 1 inch in length. Using tongs to hold the
strip, ignite the Magnesium in the burner's flame. Do not look directly at the resulting
bright light.

Controlled Combustion of Magnesium in Crucible

1. Thoroughly clean a crucible by moistening it and rubbing with a paper towel. If this does
not remove all foreign debris, and after consulting with your instructor, add 5-10 mL 6M
HCl to the crucible and allow it to stand for 5 minutes. Then discard the HCl and rinse the
crucible with water. After the crucible has been cleaned, use tongs to handle the crucible
and cover.

2. Set up a clay triangle on a ring stand. Transfer the crucible and cover to the triangle.

3. Light your Bunsen burner. Adjust the flame so that it is ~3-4 inches high with a bright blue
center indicating the flame is very hot. (Consult with your instructor to make sure the
flame is adjusted correctly. Failure to heat your sample sufficiently will result in
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incorrect results. Further details concerning Bunsen burner flames can be found in
the Appendix below.)

4. Begin heating the crucible and cover in the cooler upper region of your burner’s flame to
dry them. When the crucible and cover show no visible droplets of moisture, lower the
crucible into the hotter region of the burner’s flame, and heat the crucible for 5 minutes.
Your instructor will demonstrate how to raise and lower the Ring with a pair of tongs
without removing the burner flame. Remove the flame, and allow the crucible to cool to
room temperature. This takes about 10 minutes. Weigh the crucible and cover on the
indicated balance.

5. Repeat the intense heating procedure, allow the crucible to cool and re-weigh the crucible
and cover. Check with your instructor to make sure the weight is sufficiently constant, and
all the water has been driven out of the crucible.

6. Add approximately 1 teaspoon of magnesium turnings to the crucible. Weigh the crucible
again. (Smaller amounts are better. You want enough magnesium so that the uptake of
oxygen can be accurately measured. However, if you use too much, oxygen will have
difficulty infusing into the sample.)

6. Set up the crucible on the clay triangle with the crucible at a slight angle and with the cover
slightly ajar. Begin heating the crucible gently in the cooler upper region of your flame. If
the sample begins to smoke when heated, close the crucible until only a crack between the
jar and lid exists and heat for 2-3 minutes. If the sample continues to smoke, close the lid
entirely and heat gently for 2-3 minutes; then move the lid until only a crack exists and heat
for another 2-3 minutes. If you are still having trouble with the sample smoking, consult
your instructor. The smoke consists of the magnesium oxide product and must not be lost
from the crucible. Continue to heat gently for 5-10 minutes with cover of the crucible
slightly ajar. Remove the heat and allow the crucible to cool 1-2 minutes.

7. Remove the cover and examine the contents of the crucible. If portions of the magnesium
still demonstrate the shiny appearance of the free metal, return the cover and heat with a
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cool flame for an additional 5 minutes; then re-examine the metal. Continue heating with a
cool flame until no shiny metallic pieces are visible and the sample no longer “flares”.

8. When the shiny magnesium metal appears to have been fully converted to the dull gray
oxide, return the cover to its slightly ajar position, and heat the crucible with the full heat of
the burner flame (hottest part of the flame) for 10 minutes. Then slide the cover to about
the half-open position and heat the crucible in the full heat of the burner flame for an
additional 10 minutes.

9. Remove the heat and allow the crucible and contents to cool on a ceramic-centered wire
gauze pad. With a dropper, add about 10 drops of distilled water to the crucible, spreading
the water evenly throughout the solid.

10. Return the crucible to the clay triangle, and set the cover in the slightly ajar position. With
a cool flame, begin heating the crucible. When it is certain that all the water has been
driven off, slide the cover so that it is in the half-open position, and lower the sample into
the hotter portion of the burner’s flame. Heat the crucible and contents in the full heat of
the burner for 5 minutes. Allow the crucible to cool completely to room temperature.
When completely cool, weigh the crucible and contents.

11. Obtain a 3 dram vial and submit a sample of your product. Label the vial with the
following information:
Name(s)
Name of Compound
Formula of Compound
Date
Weight of Product
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Data Analysis
1. Determine the Mass Oxygen consumed during the combustion reaction for Magnesium.

2. Determine the elemental composition, mass percentage Magnesium and Oxygen, of

Magnesium Oxide.

3. Use a Reference source such as The Merck Index to determine the accepted elemental
composition of Magnesium Oxide. Calculate the Percentage Error in your results.

4. Use your composition data to determine the Empirical Formula of Magnesium Oxide.

5. Analyze the steps in your procedure to determine the likely source of error in your
determination of the elemental composition of the compound.
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Post Lab Questions

1. Which reactant limits the production of magnesium oxide?

2. In analyzing the mass data in order to determine the elemental composition of the
Magnesium Oxide, we have assumed the reaction is 100% complete. How is the
percentage Magnesium affected if this assumption is not correct?

3. Use the Merck Index, the CRC Handbook of Chemistry and Physics, or other source such as
Wikipedia to determine the chemical formulas of the Oxides of the other Alkaline Earth
Metals.

4. Do the same, to determine the chemical formulas of the oxides of the Alkali Metals.
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Appendix - The Bunsen Burner

The standard laboratory gas burner was developed by Robert Bunsen and George Desaga in 1854
when Bunsen's new laboratory was being supplied with Natural Gas. The design is intended to
maximize the mixing of the Gas and Oxygen, supplied via the Air, before combustion begins.
This will produce hot flames with a minimum of luminosity.

Robert Bunsen
(http://www.communicatescience.eu/
2011/03/robert-bunsen-200-years-of-
science.html)

The style of burner used in our laboratories is pictured above.

Note the position of the Gas and Air controls. The burner
should always be operated such that the main gas valve is in
the fully open position. Control of the gas supply to the
burner's flame should be accomplished with the gas control of
the burner itself. This will allow for a more fine-tuned
control of the flame height. Control of the quality of the
flame, hot or cold, is achieved by rotating the burner's barrel
so as to allow more or less Oxygen to mix with the Gas. A
cold flame will appear yellowish due to the incomplete combustion of the Gas. A hot flame will
have a bright blue cone at its center, the hottest part of the flame, with a colder light blue cone
about it.

You should practice using both burner controls to produce a flame with the desired properties.
http://en.wikipedia.org/wiki/File:Bunsen_burner_flame_types_.jpg
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Addendum

Acid-Base Properties of the Group A Oxides

In this short exercise we will examine the Acid-Base properties of the Oxides of several of the
Group A elements. As was noted above, the Group A metal Oxides form basic solutions in
Water, as exemplified by Barium Oxide (BaO) which reacts with Water to form Barium
Hydroxide (Ba(OH)2):

BaO(s) + H2O Ba(OH)2(aq)

And, non-metal oxides, are acidic upon reaction in Water. For example, Sulfur Dixodie (SO2)
forms acidic Sulfurous Acid (H2SO3):

SO2(g) + H2O H2SO3(aq)

Elements that are metalloids will form Oxides which are both acidic and basic. Compounds that
can behave as both an acid and a base are referred to as amphoteric.

The Acid-Base properties of a solution can be easily examined by using Acid-Base Indicators.
These Indicators are compounds that change color, depending on whether or not they are in an
Acidic or Basic environment. For instance, the compound Phenolphthalein is colorless in an
acidic environment and pink in a basic environment.

So adding an Acid-Base Indicator to an aqueous solution containing the Oxide will allow us to
determine if the Oxide is acidic or basic. We will do this for the following Oxides:

Magnesium Oxide
Calcium Oxide
Barium Oxide
Sulfur Dioxide (SO2)
Phosphorus Pentoxide (P4O10)

Procedure
1. Test your Magnesium Oxide product against reaction with water: Place ~50mL of water in
a 100mL beaker. Add a few drops of the Acid-Base indicator Phenolphthalein. This
indicator is clear in Acidic-Neutral solutions. It is bright pink in Basic solutions. Add a
spatula tip of your product to the water and stir with a stirring rod. Observe the results over
the period of a few minutes.

2. Do the same with a sample of Calcium Oxide.

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3. For Barium Oxide, do the same. Except wear gloves and carry the reaction out in a fume
hood on a metal pan. (Barium compounds tend to be toxic, so always was your hands
after using them. And, avoid getting them on your clothes or breathing the dust.)

4. Make sure your laboratory instructor is nearby to supervise the next exercise.

To test the oxide of Sulfur, obtain a Combustion Spoon, Stopper and 500mL Round
Bottomed Flask. Run the Combustion Spoon through the stopper. Place about 50mL water
in the flask. Add 7 drops Congo Red indicator. (This indicator is Red in Neutral solutions
and Blue in Acidic solutions.) Place a small amount of Sulfur in the Combustion Spoon.
In a Fume Hood, ignite the Sulfur in a Bunsen burner flame. Once the Sulfur has been
ignited and begins producing Sulfur Dioxide (SO2) vapors:

S8(s) + 8 O2(g) 8 SO2(g)

put the spoon in the flask and stopper the flask. Do not place the spoon in the water.
Allow the combustion to continue for a minute or two. Once the fumes fill the flask, swirl
the water so that it can absorb the fumes. Note the results. Clean the combustion spoon
by burning off the excess Sulfur. Leave the flask in the fume hood.

5. White Phosphorus can ignite spontaneously in Air to form Phosphorus Pentoxide (P4O10).

Your laboratory instructor will perform the following exercise.

If White Phosphorus touches the skin, the area should be immersed in water immediately. As soon
as possible, substitute a solution of Copper Sulfate for the water. When the burning subsides, was
well with soap and water.

Observe a small piece of White Phosphorus (~1/4” square). Your instructor will obtain a
small piece on the tip of spatula. The White Phosphorus may ignite spontaneously; if not,
your instructor willignite it with a burner.

P4(s) + 5 O2(g) P4O10(g)

They will then collect the fumes in a small Erlenmeyer Flask to which a few milliliters (no
more than 25 mL) Water (containing the indicator Congo Red) has been added by tilting the
flask and placing the burning sample above the Water. What reaction is occuring?

Data Analysis
1. Write chemical reactions for what happens when Magnesium and Calcium Oxides are
added to Water.

2. Write a chemical reaction for what happens when the Phosphorus combustion product
reacts with Water.