Introductory Chemistry

SCHOOL OF SCIENCE AND HEALTH

Introductory Chemistry
Laboratory 6
Buffers and Redox
Competition for protons and competition for electrons

Student Number

Family Name

First Name

Campus

Prac Start time

session
(Day) (AM or PM, or evening)
Introductory Chemistry - Buffers and Redox

Aims
In this lab session, you and your lab partner will:

 Prepare and test a buffer solution to maintain the pH at an approximate value if

a small amount of strong acid or base is added.
 Gain practical experience in various concepts of
electrochemistry
 Investigate the relative strength of several oxidising agents by examining the
products of various reactions.
 Construct a series of electrochemical cells and examine the properties of
these cells.

INTRODUCTION PART A.

Involves making a buffer solution to keep the pH reasonably constant (the value will
be assigned to you). A buffer requires two components:
 an acid component to neutralise any added base, and
 a base component to neutralise any added acid.

Ideally the acid and base components are conjugates of each other:

If hydroxide ions are added to your buffer, the following neutralisation needs to happen:

For example:
Acid component + OH-  Base component +H2O

CH3COOH(aq) + OH-  CH3COOH(aq) +H2O

If hydronium ions are added to your buffer, the following neutralisation needs to happen:

Base component + OH-  Acid component +H2O

Write the equation for what happens when a small amount of acid (write as H+) is
added to an acetic acid/acetate buffer.

+ +

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Introductory Chemistry - Buffers and Redox

For your assigned pH, you will need to work out which combination of acid and
base components to use in your buffer, and the relative amounts of these
components. Your choices are:

Conjugate Base
Acid Component pKa
Component

CH3COOH CH3COO- 4.76

2
H2PO4- HPO4 - 7.18

EXPERIMENTAL WORK

Part A: Preparation and Evaluation of a Buffer Solution

You and your partner will be given the challenge of preparing a buffer for a given pH
value. The buffer should be able to keep the pH reasonable constant if small amounts of
strong acid or base are added. The acid component of your buffer has to be selected
from two of the three acids whose titration curves are drawn in the graph below.

Here is a summary of the steps that follow:

 select the appropriate buffer system for the pH your require

 calculate the appropriate solution volumes of the acid and base components of
the buffer
 produce the buffer solution by combining the appropriate solution volumes
of the acid and base components of the buffer, and adjust its pH by adding
concentrated HCl or NaOH
 test your buffer for its capacity to keep the pH constant when small amounts of
concentrated acid or base are added
 compare these pH changes with what happens when you add the same small
amounts of concentrated acid or base to 0.100 M sodium chloride

The following solutions are available for you to produce your buffer:

 0.200 M acetic acid, CH3COOH(aq)

 0.200 M sodium acetate, Na+ (aq) + CH3COO- (aq)
 0.200 M potassium dihydrogen phosphate, K+ (aq) + H2PO4- (aq)
2
 0.200 M potassium monohydrogen phosphate, 2K+ (aq) + HPO -(aq) 4

 0.100 M sodium chloride, Na+ (aq) + Cl- (aq)

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Introductory Chemistry - Buffers and Redox

Answer the following questions in your notebook and in these prac notes

Designated pH

1. Select the appropriate combination of acid and base solutions above for your pH
buffer on the basis of pKa values. (The best buffer system is the one that has the
largest buffer region around your pH ii.e. the system whose pKa is closest to your
pH)

Chosen Buffer Acid Conjugate base

2. Use the Henderson‐Hasselbalch equation

to calculate an approximate ratio of volumes of appropriate acid and conjugate

base solutions to produce your pH buffer

Ratio ([A-]/]HA])

3. From this ratio, calculate the volumes of appropriate acid and conjugate base
solutions to produce 50 mL of your pH buffer.
(The equation for doing this is on the board)

Once you have checked your calculations with your demonstrator or supervisor,

Prepare 50 mL of your buffer as follows:

1. Use 25‐mL measuring cylinders to mix the appropriate volumes you

calculated to prepare 50.0 mL of the required buffer solution in a 100‐mL
beaker.

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Introductory Chemistry - Buffers and Redox

2. Measure the pH of your buffer, and adjust it to the value you have been
allocated by carefully adding 1.0 M HCl or 1.0 M NaOH dropwise to the
solution. (This is common practice when making up a buffer solution because
the calculations are only approximate since ignore ion activity effects).

3. Divide your prepared buffer solution into approximately two equal

volumes in separate 100‐mL beakers.

4. Measure the initial pH of your buffer solution and record the pH in the first
box in the table below:

pH values of your buffer solution with:

1.0 M HCl added 1.0 M NaOH added

Initial 2 10 20 2 10 20
pH drops drops drops drops drops drops

5. Then add 1.0 M HCl drop‐wise to one solution, first 2 drops, then 10,
then 20 (as per the table) recording the pH after adding each of the
specified volumes of acid in the table.

6. Repeat this procedure with the other half of the buffer solution, but adding
1.0 M NaOH instead.

7. Repeat Steps 5 to 8 again, but this time use 0.1 M NaCl solution
instead of your buffer solution.

pH values of 0.1 M NaCl solution with:

1.0 M HCl added 1.0 M NaOH added

Initial 2 10 20 2 10 20
pH drops drops drops drops drops drops

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Introductory Chemistry - Buffers and Redox

Write a clear concise statement regarding the changes in pH when NaOH and HCl
are added to solutions containing
1) the buffer and
2) the salt NaCl.

Does NaCl function as a buffer?

Why?

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Introductory Chemistry - Buffers and Redox

PART B REDOX REACTIONS (A COMPETITION FOR ELECTRONS)

Background

Chemical reactions, which involve the transfer of electrons, or electron density, are
referred to as reduction-oxidation (“redox”) reactions. For example, when chlorine gas
is bubbled through a potassium iodide (KI) solution, iodine is produced:

Cl2(g) + 2I-(aq)  Cl-(aq) + I2(s)

This reaction can be broken down into two half-reactions which describe the
individual oxidation and reduction reactions:

Cl2(g) +2e-  2Cl-(aq) (reduction)

2I-(aq)  I2(s) + 2e- (oxidation)

Note that reduction involves gain of electrons, and oxidation involves loss of
electrons. In the above reaction, chlorine is reduced during the course
of the reaction; conversely, iodide ion is oxidised.

The terms, ‘reducing agent’ and ‘oxidising agent’, are also used to
describe the species within a redox reaction. A reducing agent
reduces the other species in the reaction. For example in the reaction
above, iodide is the reducing agent in the reaction because it reduces
the chlorine.

Note also that the reducing agent itself is oxidised as it transfers (loses) its
electrons to the reduced species.

Similarly, an oxidising agent oxidises the other species. In this

example, chlorine is the oxidising agent as it takes electrons from
iodide. Chlorine, as the oxidising agent, is reduced (gains electrons).
Electron transfer in the reaction occurs from the reducing agent to the
oxidising agent.

In any redox reaction, the oxidation and reduction reactions occur simultaneously and
with exactly the same rate of electron transfer, i.e., the reactions are dependent on
each other - you can’t have one without the other. Thus, in a redox reaction, there is
only one reactant which acts as an oxidising agent and one reactant that acts as a
reducing agent. Also, these species form products, which are themselves oxidising and
reducing agents. The reacting oxidising agent forms a product, which is a reducing
agent and similarly, a new oxidising agent is formed as a product from reducing agent.
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Introductory Chemistry - Buffers and Redox

In the reaction of chlorine and iodide discussed above, the new reducing agent is the
product chloride, Cl-, whereas the new oxidising agent is the product I2.

Whether a reaction that we write on paper can occur spontaneously is always an

important chemical question. For redox reactions, the competition for electrons
between the species governs the reaction and determines whether it happens.
Whether a redox reaction occurs can be predicted by comparing the strength of the
two oxidising agents within the reaction i.e. the strength of the oxidising agent on the
reactant side vs. the strength of the oxidising agent on the product side of the
reaction.

This is a thermodynamic consideration and only predicts whether a redox reaction can
occur. It does not indicate how fast the reaction will proceed.

In the above reaction:

Cl2(g) + 2I-(aq)  Cl-(aq) + I2(s)

there is an oxidising agent on the left hand side, Cl2, and another oxidising agent on
the product side, I2. Because this reaction proceeds as written, Cl2 must be the
stronger oxidising agent of these. Thus, Cl2 pulls the electrons in the reaction, away
from the other redox couple

In this part of this experiment, you will compare several oxidising agents and evaluate
their strengths as oxidizing agents by observing whether reactions occur between
particular species.

Remember: if a reaction proceeds as written, the oxidising agent on the reactant

side is the stronger than the oxidizing agent on the product side in the reaction.

Electron transfer from reducing agent to oxidising agent can occur in two ways. The
reducing and oxidising agents can both be contained in the same vessel and react by
collision, like the reagents in a normal reaction.

The other way, is called an electrochemical cell, which has the reducing agent in one
container and the oxidising agent in another. The two solutions are connected by a wire
and a salt bridge. The wire allows the transfer of electrons between the cells. The wire
is connected to each cell through an electrode. Each electrode is made of material that
conducts electrons and the individual half-reactions occur at the surfaces of the
electrodes. Each electrode is made of metal or an inert conducting material like
graphite.

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Introductory Chemistry - Buffers and Redox

The component that is oxidised is placed in the cell conventionally connected to the +ve
terminal of the voltmeter and the released electrons are transferred to the cathode
through the wire connecting the cells and onto the electrode in the cell where reduction
occurs. The cells are also connected by a salt bridge, which allows the transfer of ions
between the cells. Without a salt bridge, no electron transfer occurs because there
would be a build-up of electrons in one container, and a deficiency in the other. An
electrochemical cell is illustrated below for the redox reaction between Zn(s) and Cu(II)
ions.

Figure 1. Electrochemical cell involving half-reactions with Zn and Cu

Zn2+ + Cu  n + Cu2+

Zn2+ + 2e-
Zn 
Cu2+ + 2e- 
Cu

In this experiment, you will construct electrochemical cells, using metal electrodes.
Then you will measure the voltage difference between cells created using different
strength of redox pairs in the cells and determine which metal ion is the stronger
oxidising agent.

EXPERIMENTAL

In this part, you will construct a series of electrochemical cells with metal electrodes.

Remember: when the measured potential is positive, electrons flow from the cell
connected to the negative terminal of the voltmeter to the cell connected to the
positive terminal.

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Remember: electrons always flow to the cell containing the substance that is
being reduced (conventionally the right hand cell). When the measured potential
is positive, the RHS cell contains the metal ion which is the stronger oxidising
agent i.e. the one that is reduced.

Prepare four beakers in the following manner, one for each metal, Cu, Fe, Ni and Zn.

 Place 20 mL of the metal ion in separate 100-mL beakers. Insert the metal
electrode into the beaker containing the SAME metal ions in solution.

 Construct the electrochemical cells between all of the possible combinations of

metal pairs. There are therefore 6 experiments for the 4 metals, Cu, Fe, Ni and
Zn to be tested.

 Use a piece of paper hand-towel soaked with 0.1 M Na2SO4 solution to create
a salt bridge. Connect the positive terminal of the voltmeter to one metal
electrode and the other metal of the pair to the negative terminal.

Do NOT complete the external circuit between the electrodes as this will cause
the voltage to drop as current (electrons) flow. Instead you should only measure
the voltage via the voltmeter. This will measure the EMF or voltage when no
current flows

 When finished, return the metal electrodes, washed and cleaned to their
containers. Dispose of the metal ion solutions appropriately as directed

Complete the table below

Voltage Direction of Which

(including electron flow metal ion is
positive negative
sign) (outside being
circuit) reduced

Cu Fe
Cu Ni
Cu Zn
Fe Zn
Ni Zn
Ni Fe

Input the results of your experiments into this table and in your laboratory
book.

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Introductory Chemistry - Buffers and Redox

In your laboratory book draw one example of the electrochemical cells you
constructed, labelling the sign of each electrode, together with the anode and the
cathode and writing the half reactions below each cell.

From your results list the metal ions as oxidising agents, in decreasing order of
oxidising agent strength in your laboratory notebook:

Strongest Oxidising

agent

Strongest Reducing

agent

End of the Experimental Section

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TOTAL MARKS FOR LABORATORY PRACTICAL (25 MARKS)

PREWORK (0-1 marks)

No preparation of lab book Correct preparation of Lab book

0 1

TECHNIQUE (0-6 marks)

Did not complete Errors in technique No errors in technique

experiment (includes late arrival in practical)
0 1-5 6

LABORATORY BOOK (0-3 marks)

Correct legible
Little data or
Not all data recorded record of all
No Laboratory experimental
or incorrectly data including
Book observations and
recorded procedure and
illegible records
observations
0 1 2 3

Quality of experimental data

No results Average quality Good results

0 1-5 6

Buffer calculation
Calculation error Arithmetic errors Calculation correct
0 1-2 3

All parts of redox section completed

Error or not Completed with

Data correct
completed errors
0 1-5 6

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