Experiment 7 The Copper Cycle

WORK INDIVIDUALLY

PURPOSE
Metallic copper, Cu(s), will be subject to a series of reactions with various reagents to produce four
different copper compounds before ultimately being restored to its original metallic form. The
chemical and physical changes of each reaction will be observed and recorded, the balanced chemical
equations for each reaction will be written and classified, and the percent recovery of the final copper
product will be determined.

OBJECTIVES
1. Perform a series of precipitation, acid-base, decomposition, and redox reactions on successive
copper-based compounds.
2. Calculate the percent recovery of the final Cu(s) product.
3. Compose five balanced chemical equations (and any necessary sub-equations) based on the
classification of each reaction in the cycle.

CONCEPTS
You should familiarize yourself with the following scientific concepts prior to attending the lab:
 Safety – working with strong acids and bases
 Proper technique of decantation of a supernatant from a precipitate
 Nomenclature of inorganic compounds
 Chemical vs physical processes
 Solubility
 Types of chemical reactions: acid-base, decomposition, precipitation, and redox reaction
 Ionic charges and periodic trends of elements

INTRODUCTION
Background & Context
Copper belongs to a group of elements called transition metals, which are also referred to as d-block
elements with regard to their placement on the periodic table. Like many other transition metals,
copper is brilliantly colored both as a pure metal and as a part of a chemical compound. It can achieve
oxidation states of –2, 0, +1, +2, +3, and +4, but the most common copper complexes contain the +2
oxidation state of the element. Copper is utilized in a wide variety of present-day applications,
including electrical wiring, plumbing, decorative architecture, and jewelry, as well as in highly
specialized materials ranging from coloring agents to antimicrobial surfaces.

During this experiment, the versatility of copper will be explored through five successive reactions
starting with elemental copper to produce four different copper-containing compounds and
ultimately recovering the elemental copper as described by the copper cycle in Figure 1.

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Figure 1: Schematic of the copper cycle.

Chemical Principles (Classification of chemical reactions)

Precipitation Reactions
In a precipitation reaction, two reactants that are dissolved in a solution react to produce an insoluble
solid. The driving force behind this type of reaction is the strong attraction between the positive and
negative ions in the solution, which can be described by the solubility rules of ionic compounds. The
overall result of a precipitation reaction is the removal of ions from the solution upon formation of
the precipitate. For example, when two aqueous solutions of K2SO4 (aq) and Pb(NO3)2 (aq) are mixed,
PbSO4 (s) will precipitate from the solution. The formula unit, total ionic, and net ionic equations for
this reaction are shown below:

Formula unit: K2SO4 (aq) + Pb(NO3)2 (aq) ⟶ PbSO4 (s) + 2 KNO3 (aq)
Total ionic: 2 K (aq) + SO4 (aq) + Pb2+(aq) + 2 NO3–(aq) ⟶ PbSO4 (s) + 2 K+(aq) + 2 NO3–(aq)
+ 2–

Net ionic: SO42–(aq) + Pb2+(aq) ⟶ PbSO4 (s)

Acid-Base Reactions
In an acid-base reaction, also referred to as a neutralization reaction, an acidic solution and a basic
solution react to produce salt and water. The driving force behind this type of reaction is the reaction
of H+(aq) from the acidic solution with OH–(aq) from the basic solution to produce H2O(l) molecules. For
example, the reaction of HCl with NaOH, a strong acid and a strong base, will produce NaCl and H2O.
The resulting formula unit, total ionic, and net ionic equations for this reaction are shown below:

Formula unit: HCl (aq) + NaOH (aq) ⟶ NaCl (aq) + H2O (l)
Total ionic: H (aq) + Cl–(aq) + Na+(aq) + OH–(aq) ⟶ Na+(aq) + Cl–(aq) + H2O (l)
+

Net ionic: H+(aq) + OH–(aq) ⟶ H2O (l)

Some acid-base reactions may not be as obvious as the strong acid-strong base example above. For
instance, the addition of an acid to a metal oxide can also be classified as an acid-base reaction due to
the nature of the resulting products – salt and water. The formula unit, total ionic, and net ionic
equations for the reaction of CaO(s) with HNO3 (aq) are shown below:

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 The Copper Cycle
Formula unit: CaO (s) + 2 HNO3 (aq) ⟶ Ca(NO3)2 (aq) + H2O (l)
Total ionic: CaO (s) + 2 H+(aq) + 2 NO3–(aq) ⟶ Ca2+(aq) + 2 NO3–(aq) + H2O (l)
Net ionic: CaO (s) + 2 H+(aq) ⟶ Ca2+(aq) + H2O (l)

Decomposition Reactions
In a decomposition reaction, a reactant is broken down into one or more smaller compounds
(products) when subjected to specific conditions. For example, a decomposition reaction occurs
during the electrolysis of water:

2 H2O (l) ⟶ 2 H2 (g) + O2 (g)

However, the most predominant method of generating a decomposition reaction involves the
application of heat (Δ) to a reactant:

Δ
2 KClO3 (s) ⟶ 2 KCl (s) + 3 O2 (g)

Oxidation-Reduction (Redox) Reactions

In a redox reaction, electrons are transferred from one reactant to another as the reactants are
converted into products, causing the oxidation states of two (or more) atoms to change. The driving
force behind this type of reaction is the transfer of electrons from an atom with a lower electron
affinity to an atom with a higher electron affinity.

The oxidation state of an atom is the charge that the atom would have if the electrons were
transferred completely (and not shared) between atoms within a compound. Most metal species are
able to achieve several different oxidation states, but the oxidation states of the s-block and p-block
elements are largely based on their location on the periodic table (Table 1).

Table 1: Typical oxidation numbers of atoms.

Chemical Species Typical Oxidation Numbers
All pure elements 0
+I (bound to a non-metal)
Hydrogen
–I (bound to a metal)
–I (in peroxides)
Oxygen
–II (in all other compounds)
Group 1A (Alkali Metals) +I
Group 2A (Alkali Earth Metals) +II
Group 3A +III
Group 5A –III
Group 6A (Chalcogens) –II
Group 7A (Halogens) –I
Other Metals Variable

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During a redox reaction, one reactant will lose electrons by transferring them to another reactant,
which in turn gains the electrons. The two processes that describe the loss and gain of electrons by
particular reactants are referred to as oxidation and reduction, respectively.

Oxidation is the process by which a reactant loses electrons, and its oxidation state therefore becomes
more positive. For example, when pure Zn(s) metal is oxidized during a 2 electron (e–) transfer, it
becomes Zn2+. Recall that all pure elements have an oxidation state of zero.

Reduction is the process by which a reactant gains electrons, and its oxidation state therefore
becomes more negative. For example, when Fe2+ is reduced during a 2 e– transfer, it becomes solid
Fe(s) with an oxidation state of zero.

A useful acronym to help describe these two processes is OIL RIG:

OIL: Oxidation Is Loss (of electrons)

RIG: Reduction Is Gain (of electrons)

When a particular reactant is oxidized, it is acted upon by an oxidizing agent. The oxidizing agent gets
reduced during the reaction by gaining the electrons lost by the oxidized reactant. Similarly, when a
particular reactant is reduced by a reducing agent, the reducing agent gets oxidized by losing the
electrons that are gained by the reduced reactant.

A redox reaction must be divided into two half-reactions in order to determine which reactant is
being oxidized (the reducing agent) and which is being reduced (the oxidizing agent). One
half-reaction represents the oxidation process, and the other represents the reduction process. The
original and final oxidation states of each atom within a reactant must be determined in order to
establish where the oxidation and reduction is occurring.

Example 1: Sodium metal reacts with chlorine gas to produce solid sodium chloride salt.
Write the balanced reaction and determine the oxidation state of each atom in the reactants
and products, then determine how many electrons are transferred during the reaction.
0 0 +I –I
2 Na (s) + Cl2 (g) ⟶ 2 NaCl (s)

The oxidation state is written above the atom (with roman numerals preceded by the +/–
sign in contrast to actual charges of ions represented by Arabic numerals which are followed
by the +/– sign) and only represents the oxidation state of a single atom, not the total number
of atoms in the element or compound.

Next, the reaction of each individual reactant is described by two balanced half-reactions:
0 +I
Oxidation: Na ⟶ Na+ + 1 e− reducing agent = Na (s)

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 The Copper Cycle

0 –I
Reduction: Cl2 + 2 e− ⟶ 2 Cl− oxidizing agent = Cl2 (g)

Electrons cannot be created nor destroyed, so the number of transferred electrons in the
reaction must be the same on both sides of the chemical equation once the two half-reactions
are re-combined:

Sum of the half-reactions: 2 Na (s) + Cl2 (g) + 2 e− ⟶ 2 NaCl (s) + 2 e−

Final balanced chemical equation: 2 Na (s) + Cl2 (g) ⟶ 2 NaCl (s)

PRE-LAB REQUIREMENTS
On the next clean page of your lab notebook, complete the following BEFORE your laboratory section
begins:
1. In your own words, state the overall purpose of the experiment and the individual objectives (DO
NOT simply copy the purpose and/or objectives from the lab manual).
2. List the chemical compounds (reactants, reagents, solvents) that you will encounter in this
experiment.
3. List the equipment required to complete this experiment.
4. What are the chemical hazards associated with this experiment?
5. What are the physical hazards associated with this experiment?
6. Write complete and properly balanced chemical equations for all the chemical reactions
that will be performed during this experiment.
7. Write an outline of the experimental procedure. You do not need to copy the entire procedure
verbatim from this lab manual.

EXPERIMENTAL
Safety
**Safety goggles, lab coats, and gloves must be worn AT ALL TIMES during the experiment**
1. Nitric acid (HNO3), hydrochloric acid (HCl), sulfuric acid (H2SO4), and sodium hydroxide (NaOH)
are CORROSIVE to flesh and can cause severe burns and/or blindness upon contact or inhalation:
In the event of skin contact, wash exposed area with soap and running water for 15
minutes and notify your TA immediately.
2. HNO3, HCl, H2SO4, and NaOH are highly EXOTHERMIC upon contact with water: Use caution
when handling these chemicals and add them SLOWLY.
3. Nitrogen dioxide (NO2) is a TOXIC brown gas that is produced during Reaction 1: Perform this
step in a FUME HOOD.
4. Ethanol is an extremely FLAMMABLE liquid: Keep away from all sources of sparks and/or
open flames.
5. Hot glass looks like cold glass and can cause painful burns. Exercise caution with steps that
involve heating with a hot plate.

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List of compounds
Cu(s) wire 6 M H2SO4
Al(s) wire 6 M HCl
16 M HNO3 ethanol
3 M NaOH deionized H2O

Materials
400 mL beaker 50 mL graduated cylinder
250 mL beaker 10 mL graduated cylinder
100 mL beaker porcelain evaporating dish
glass stirring rod hot plate/stir plate

Procedure
IMPORTANT: Remember to pour a stock solution that is in a large bottle into an appropriately sized
beaker first, then pour the solution from the beaker into a graduated cylinder for measurement.
Discard any extra solution into the appropriate waste container and/or share it with your labmates.
NEVER pour a solution back into its stock container for any reason.

Reaction 1: The Formation of Cu(NO3)2

1. Using the proper techniques described in previous experiments, use a clean watch glass to record
the mass of a single piece of pre-cut Cu(s) wire in Table 2 (located at the end of the procedure).
Record as many significant figures as possible.
2. Place the wire in a clean 250 mL beaker so that it lies flat on the bottom. It may be necessary to
bend the wire into a slightly circular configuration. Label the beaker including your name.
3. WARNING: 16 M HNO3 can cause severe eye and skin damage immediately upon contact.
Always handle wearing the proper protecting equipment (goggles, gloves, and a lab coat;
sleeves rolled completely down). Exercise extreme caution when working with this
reagent. While working inside a fume hood, use a disposable pipette to add approximately 4 mL
16 M HNO3 to the 250 mL beaker. The reaction will produce NO2, which is a toxic brown gas.
Gently swirl the beaker until the wire has completely dissolved. The evolution of NO2 will cease
once all Cu(s) has reacted.
4. Remove the 250 mL beaker from the hood and add approximately 150 mL deionized H2O.
5. Record all observations in Table 3 at the end of the procedure.

Reaction 2: The Formation of Cu(OH)2

6. Use a graduated cylinder to very slowly (dropwise) add 30 mL 3 M NaOH to the beaker while
stirring simultaneously with a glass stirring rod. Use this same glass stirring rod throughout the
entire experiment (to prevent copper mass loss between steps). Check the pH of the reaction

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 The Copper Cycle
mixture by placing a drop of the solution on the pH paper (placed on a watch glass); keep adding
more NaOH until the pH paper turns blue indicating a basic solution.
7. Record all observations in Table 3 at the end of the procedure.

Reaction 3: The Formation of CuO

8. Gently heat the 250 mL beaker containing the solution from Reaction 2 on a hot plate, and use
the glass stirring rod (or a magnetic stir bar) to stir the solution continuously and vigorously to
prevent bumping and splashing of the reaction mixture (abrupt boiling)! Do not boil the solution;
a gentle warming is sufficient. The reaction should take approximately 20-25 minutes to reach
completion. The reaction is complete when the solid is uniform in color and the solution is clear
and colorless.
9. Remove the beaker from the hot plate (use beaker tongs or a piece of folded paper towel to wrap
around the hot beaker in place of a mitten) and allow the solid to settle (be patient).
10. Once the solid has settled in the 250 mL beaker, decant the colorless solution into a clean waste
beaker, taking care not to lose any of the precipitate.
11. Add approximately 200 mL deionized H2O to a clean 400 mL beaker and heat it to just below
boiling on the hot plate.
12. To “wash” the solid, pour the near-boiling H2O into the 250 mL beaker and stir briefly with the
glass stirring rod. Allow the solid to settle, then decant the colorless solution into the waste
beaker. Turn the hot plate off. If all of the decantation steps were performed carefully and patiently,
the final volume of the liquid at this point should be below 100 mL; higher volumes will cause lower
recoveries in the final step.
13. Record all observations in Table 3 at the end of the procedure.

Reaction 4: The Formation of CuSO4

14. Use a graduated cylinder to add 15 mL 6 M H2SO4 into the beaker containing the previously
isolated CuO while stirring simultaneously with the glass stirring rod.
15. Record all observations in Table 3 at the end of the procedure.

Reaction 5: The Formation of Cu(s)

16. Place one piece of loosely-coiled Al(s) wire in the 250 mL beaker containing the newly formed
CuSO4 so that the wire is submerged entirely in the solution, add a clean stir bar and 5 drops of 6
M HCl to initiate the reaction, then cover the beaker with a watch glass. Place the beaker on the
hot plate, which should still be warm from Reaction 3, and gently stir the solution so that the stir
bar agitates the Al(s) wire. Cu(s) will begin to form on the surface of the wire, and stirring will
remove large Cu(s) solids and expose fresh Al(s) surfaces on the wire. If Cu(s) formation is slow, you
may gently heat the reaction until it is warm to touch (no higher than Level 4). You may use the
glass stirring rod to help scraping the newly formed metallic copper off the aluminum wire.
17. When the reaction has finished (indicated by loss of the color from the dissolved copper salt),
remove the beaker from the hotplate and use the glass stirring rod to remove any remaining Cu(s)
from the Al(s) wire. Remove the wire from the solution, then decant the solution into the waste
beaker.

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18. Prepare a steam bath by boiling approximately 50 mL H2O in a 100 mL beaker on a hot plate.
Proceed to Step 19 while the bath is heating.
19. Record the mass of a small evaporating dish in Table 2. Transfer the Cu(s) into the evaporating
dish using a wash bottle filled with deionized H2O. Remove excess water from the evaporating
dish as necessary. Take care not to lose or leave behind any Cu(s) in this step.
20. Wash the Cu(s) with three 5 mL portions of deionized H2O and decant the solution between
washings.
21. Wash the Cu(s) with three 5 mL portions of ethanol and decant the solution between washings.
22. Place the evaporating dish on top of the 100 mL beaker and use the steam from the boiling water
bath to heat the contents of the dish to dryness. IMPORTANT: Overheating Cu(s) during the drying
process could lead to oxidation of the product by reaction with atmospheric oxygen, so a steam
bath is used to dry the Cu(s) product rather than heating directly on the hot plate. However, take
care not to heat the reaction in excess once it has completely dried.
23. Once the Cu(s) is thoroughly dried, remove the evaporating dish from the boiling water bath, dry
the bottom of the dish, and allow to cool to room temperature.
24. Record the mass of the evaporating dish + Cu(s) in Table 2.
25. Record all observations in Table 3.
26. Dispose of all solutions in the appropriate liquid waste container(s), and dispose of all Cu(s) and
Al(s) in the appropriate solid waste beaker.

Table 2: Initial and final masses of Cu(s).

Description Mass (g)
Cu(s) wire
Evaporating dish
Evap. dish + Cu(s) product
Cu(s) product

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Table 3: Observations for Reactions 1–5.
Reaction Product Observations

1 Cu(NO3)2

2 Cu(OH)2

3 CuO

4 CuSO4

5 Cu(s)

DATA ANALYSIS
1. Determine the percent recovery for the copper product with regard to the mass of the copper
wire.
𝑓𝑖𝑛𝑎𝑙 𝑚𝑎𝑠𝑠
% 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑦 = × 100
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑚𝑎𝑠𝑠

DISCUSSION QUESTIONS
1. Describe each step of the copper cycle with regard to the five chemical reactions. Describe the
obvious physical changes that occurred and relate them to the chemical changes that copper
underwent during each step. You may want to refer to Table 3 for this part.
2. Why was it necessary to perform Reaction 1 in a fume hood?
3. Were each of the five reactions endothermic or exothermic? Explain the reasoning behind your
answer(s).
4. Classify each of the five reactions as a precipitation, acid-base, decomposition, or redox reaction,
then provide the appropriate type(s) of chemical equation(s):
a. For a precipitation or acid-base reaction, provide the balanced formula unit, total ionic,
and net ionic equations for the reaction.
b. For a decomposition reaction, provide the balanced chemical equation for the reaction.
c. For a redox reaction, provide the balanced chemical equation and the two half-reactions
that participate in the electron transfer, then name the oxidizing and reducing agents for
the reaction (refer to the Redox Reactions guide under Supplementary Information).
5. Why did some copper compounds form precipitates in this experiment while others remained in
solution?

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6. When the recovered copper product was washed repeatedly with water, what compounds were
removed during those washes?
7. Why was ethanol used during the final washes of the recovered copper product?
8. Why was a steam bath used to dry the recovered copper product?
9. What is the Law of Conservation of Mass? Taking into account the % recovery for the final copper
product, do the experimental results support this law? Was the % recovery too high or too low?
Give two plausible explanations as to why the % recovery was not (exactly) 100 %.
10. Describe the appearance of the copper wire and the recovered copper product. What might have
caused a change in appearance?

REFERENCES
Atkins, P.W.; Jones, L. L. Chemical Principles: The Quest for Insight, 3rd Edition, W. H. Freeman and
Company, 2005, pp. F58, F63-F78, 616-618.

Condike, G. F. “Near 100% Yields with the ‘Cycle of Copper Reactions’ Experiment,” J. Chem. Educ.,
1975, 52, 615.

Todd, D.; Hobey, W. D. “An Improvement in the Classical Copper Cycle Experiment,” J. Chem. Educ.,
1985, 62, 177.

Zumdahl, S. S. Chemical Principles, 5th Edition, Houghton Mifflin Company, 2005, pp. 16, 97-129, 931,
934, 942.

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