Experiment 4

Determination of a Chemical Formula

hen atoms of one element combine with those of another, the combining ratio is typically an integer or
W a simple fraction; 1:2, 1:1, 2:1, and 2:3 are ratios one might encounter. The simplest formula of a com-
pound expresses that atom ratio. Some substances with the ratios we listed include CaCl2, KBr, Ag2O, and
Fe2O3. When more than two elements are present in a compound, the formula still indicates the atom ratio.
Thus the substance with the formula Na2SO4 indicates that the sodium, sulfur, and oxygen atoms occur in that
compound in the ratio 2:1:4. Many compounds have more complex formulas than those we have noted, but
the same principles apply.
To find the formula of a compound we need to find the mass of each of the elements in a weighed sample
of that compound. For example, if we resolved a sample of the compound NaOH weighing 40 grams into its
elements, we would find that we obtained just about 23 grams of sodium, 16 grams of oxygen, and 1 gram of
hydrogen. Since the atomic mass scale tells us that sodium atoms have a relative mass of 23, oxygen atoms a
relative mass of 16, and hydrogen atoms a relative mass of just about 1, we would conclude that the sample
of NaOH contained equal numbers of Na, O, and H atoms. Since that is the case, the atom ratio Na:O:H is 1:1:1,
and so the simplest formula is NaOH. In terms of moles, we can say that that one mole of NaOH, 40 grams,
contains one mole of Na, 23 grams, one mole of O, 16 grams, and one mole of H, 1 gram, where we define
the molar mass to be that mass in grams equal numerically to the sum of the atomic masses in an element or a
compound. From this kind of argument we can conclude that the atom ratio in a compound is equal to the mole
ratio. We get the mole ratio from chemical analysis, and from that the formula of the compound.
In this experiment we will use these principles to find the formula of the compound with the general for-
mula CuxCly ⋅ zH2O, where the x, y, and z are integers which, when known, establish the formula of the com-
pound. (In expressing the formula of a compound like this one, where water molecules remain intact within
the compound, we retain the formula of H2O in the formula of the compound.)
The compound we will study, which is called copper chloride hydrate, turns out to be ideal for one’s first
venture into formula determination. It is stable, can be obtained in pure form, has a characteristic blue-green
color which changes as the compound is changed chemically, and is relatively easy to decompose into the ele-
ments and water. In the experiment we will first drive out the water, which is called the water of hydration,
from an accurately weighed sample of the compound. This occurs if we gently heat the sample to a little over
100°C. As the water is driven out, the color of the sample changes from blue-green to a tan-brown color sim-
ilar to that of tobacco. The compound formed is anhydrous (“no water”) copper chloride. If we subtract its
mass from that of the hydrate, we can determine the mass of the water that was driven off, and, using the molar
mass of water, find the number of moles of H2O that were in the sample.
In the next step we need to find either the mass of copper or the mass of chlorine in the anhydrous sample
we have prepared. It turns out to be much easier to determine the mass of the copper, and find the mass of
chlorine by difference. We do this by dissolving the anhydrous sample in water, which gives us a green solu-
tion containing copper and chloride ions. To that solution we add some aluminum metal wire. Aluminum is
what we call an active metal; in contact with a solution containing copper ions, the aluminum metal will react
chemically with those ions, converting them to copper metal. The aluminum is said to reduce the copper ions
to the metal, and is itself oxidized. The copper metal appears on the wire as the reaction proceeds, and has its
typical red-orange color. When the reaction is complete, we remove the excess Al, separate the copper from
the solution, and weigh the dried metal. From its mass we can calculate the number of moles of copper in the
sample. We find the mass of chlorine by subtracting the mass of copper from that of the anhydrous copper
chloride, and from that value determine the number of moles of chlorine. The mole ratio for Cu:Cl:H2O gives
us the formula of the compound.

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 24 Experiment 4 Determination of a Chemical Formula

Experimental Procedure
Weigh a clean, dry crucible, without a cover, accurately on an analytical balance. Place about 1 gram of the
unknown hydrated copper chloride in the crucible. With your spatula, break up any sizeable crystal particles
by pressing them against the wall of the crucible. Then weigh the crucible and its contents accurately. Enter
your results on the Data page.
Place the uncovered crucible on a clay triangle supported by an iron ring. Light your Bunsen burner away
from the crucible, and adjust the burner so that you have a small flame. Holding the burner in your hand, gently
heat the crucible as you move the burner back and forth. Do not overheat the sample. As the sample warms,
you will see that the green crystals begin to change to brown around the edges. Continue gentle heating, slowly
converting all of the hydrated crystals to the anhydrous brown form. After all of the crystals appear to be
brown, continue heating gently, moving the burner back and forth judiciously, for an additional two minutes.
Remove the burner, cover the crucible to minimize rehydration, and let it cool for about 15 minutes. Remove
the cover, and slowly roll the brown crystals around the crucible. If some green crystals remain, repeat the
heating process. Finally, weigh the cool uncovered crucible and its contents accurately.
Transfer the brown crystals in the crucible to an empty 50-mL beaker. Rinse out the crucible with two 5- to
7-mL portions of distilled water, and add the rinsings to the beaker. Swirl the beaker gently to dissolve the
brown solid. The color will change to green as the copper ions are rehydrated. Measure out about 20 cm of
20-gauge aluminum wire (∼0.25 g) and form the wire into a loose spiral coil. Put the coil into the solution so
that it is completely immersed. Within a few moments you will observe some evolution of H2, hydrogen gas,
and the formation of copper metal on the Al wire. As the copper ions are reduced, the color of the solution
will fade. The Al metal wire will be slowly oxidized and enter the solution as aluminum ions. (The hydrogen
gas is formed as the aluminum reduces water in the slightly acidic copper solution.)
When the reaction is complete, which will take about 30 minutes, the solution will be colorless, and most
of the copper metal that was produced will be on the Al wire. Add 5 drops of 6 M HCl to dissolve any insol-
uble aluminum salts and clear up the solution. Use your glass stirring rod to remove the copper from the wire
as completely as you can. Slide the unreacted aluminum wire up the wall of the beaker with your stirring rod,
and, while the wire is hanging from the rod, rinse off any remaining Cu particles with water from your wash
bottle. If necessary, complete the removal of the Cu with a drop or two of 6 M HCl added directly to the wire.
Put the wire aside; it has done its duty.
In the beaker you now have the metallic copper produced in the reaction, in a solution containing an alu-
minum salt. In the next step we will use a Buchner funnel to separate the copper from the solution. Weigh
accurately a dry piece of filter paper that will fit in the Buchner funnel, and record its mass. Put the paper in
the funnel, and apply light suction as you add a few mL of water to ensure a good seal. With suction on, decant
the solution into the funnel. Wash the copper metal thoroughly with distilled water, breaking up any copper
particles with your stirring rod. Transfer the wash and the copper to the filter funnel. Wash any remaining
copper into the funnel with water from your wash bottle. All of the copper must be transferred to the funnel.
Rinse the copper on the paper once again with water. Turn off the suction. Add 10 mL of 95% ethanol to
the funnel, and after a minute or so turn on the suction. Draw air through the funnel for about 5 minutes. With
your spatula, lift the edge of the paper, and carefully lift the paper and the copper from the funnel. Dry the
paper and copper under a heat lamp for 5 minutes. Allow it to cool to room temperature and then weigh it
accurately.

DISPOSAL OF REACTION PRODUCTS. Dispose of the liquid waste and copper produced in the
experiment as directed by your instructor.

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 Name _____________________________________ Section ________________________________

Experiment 4

Data and Calculations: Determination of a Chemical Formula

Atomic masses: Copper ______________ Cl ______________ H ______________ O ______________

Mass of crucible ______________ g

Mass of crucible and hydrated sample ______________ g

Mass of hydrated sample ______________ g

Mass of crucible and dehydrated sample ______________ g

Mass of dehydrated sample ______________ g

Mass of filter paper ______________ g

Mass of filter paper and copper ______________ g

Mass of copper ______________ g

No. moles of copper ______________ moles

Mass of water evolved ______________ g

No. moles of water ______________ moles

Mass of chlorine in sample (by difference) ______________ g

No. moles of chlorine ______________ moles

Mole ratio, chlorine:copper in sample ______________ :1

Mole ratio, water:copper in hydrated sample ______________ :1

Formula of dehydrated sample (round to nearest integer) ______________

Formula of hydrated sample ______________

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 Name _____________________________________ Section ________________________________

Experiment 4

Advance Study Assignment: Determination of a Chemical Formula

1. To find the mass of a mole of an element, one looks up the atomic mass of the element in a table of atomic
masses (see Appendix III or the Periodic Table). The molar mass of an element is simply the mass in
grams of that element that is numerically equal to its atomic mass. For a compound substance, the molar
mass is equal to the mass in grams that is numerically equal to the sum of the atomic masses in the formula
of the substance. Find the molar mass of

Cu ___________ g Cl ___________ g H ___________ g O ___________ g H2O ___________ g

2. If one can find the ratio of the number of moles of the elements in a compound to one another, one can
find the formula of the compound. In a certain compound of copper and oxygen, CuxOy, we find that a
sample weighing 0.6349 g contains 0.5639 g Cu.

a. How many moles of Cu are there in the sample?

⎛ No. moles = mass Cu ⎞

______________ moles

b. How many grams of O are there in the sample? (The mass of the sample equals the mass of Cu plus
the mass of O.)

______________ g

c. How many moles of O are there in the sample?

______________ moles

d. What is the mole ratio (no. moles Cu/no. moles O) in the sample?

______________ : 1

e. What is the formula of the oxide? (The atom ratio equals the mole ratio, and is expressed using the
smallest integers possible.)

______________

f. What is the molar mass of the copper oxide?

______________ g/mol

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Editorial review has deemed that any suppressed content does not materially affect the overall learning experience. Cengage Learning reserves the right to remove additional content at any time if subsequent rights restrictions require it.
 Copyright 2011 Cengage Learning. All Rights Reserved. May not be copied, scanned, or duplicated, in whole or in part. Due to electronic rights, some third party content may be suppressed from the eBook and/or eChapter(s).
Editorial review has deemed that any suppressed content does not materially affect the overall learning experience. Cengage Learning reserves the right to remove additional content at any time if subsequent rights restrictions require it.