Cal Poly Humboldt General Chemistry – CHEM 110 Laboratory

B UFFERS : A CETIC A CID –A CETATE

Objective

The objective of this laboratory experiment is to determine the composition, preparation, and
properties of buffer solutions, specifically the acetic acid–acetate system.

Background and Introduction

A buffer or buffered solution (the terms are used synonymously) is a solution that resists large
changes in pH when a strong acid or a strong base is added. The key word here is “resists”. A
buffer does not maintain a constant pH upon the addition of an acid or base, but the pH of a
properly prepared buffer changes much less than the pH of an unbuffered solution treated
similarly.

A solution containing an appreciable quantity of a weak acid (HA) and its anion (A–) or a weak
base (B) and its cation (BH+) will have the properties of a buffer. An example of a weak acid (HA)
and an anion (A-) would be acetic acid (CH3COOH) and acetate ion (CH3COO–), respectively.
An example of a weak base (B) and the cation (BH+) would be ammonia (NH3) and the
ammonium ion (NH4+), respectively.

The following outline shows three different approaches for the preparation of optimal buffer
solutions for either a weak acid or weak base system. Examples assume that all solutions are of
the same concentration.

1. A buffer can be prepared by mixing:

a. equal parts of a weak acid (HA) solution with a solution containing its anion (A-)

b. equal parts of a weak base (B) solution with a solution containing its cation (BH+)

2. A buffer can be prepared by adding a strong base to a weak acid solution:

a. two parts of a weak acid (HA) solution with one part of a strong base solution

HA + OH– H2O + A– (1)

b. two parts of a solution containing the cation (BH+) with one part of a strong base solution

BH+ + OH- H2O + B (2)

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3. A buffer can be prepared by adding a strong acid to a solution containing a weak base:

a. two parts of a weak base (B) solution with one part of a strong acid solution

B + H+ BH+ (3)

b. two parts of a solution containing the anion (A-) with one part of a strong acid solution

A– + H+ HA (4)

The ability of a buffer to resist the change in pH can be shown by equations (1) and (4) for
systems containing a weak acid and anion. Remember that the buffer contains both chemical
species in appreciable amounts. Equation (1) shows how the buffer resists changes in pH upon
the addition of a strong base. Note that the added OH– is converted to H2O. Similarly, Equation
(4) shows how the buffer resists changes in pH upon the addition of a strong acid and the added
H+ is converted to HA. Thus, a buffer resists change in pH because one of its principal chemical
species reacts with added base and the other reacts with added acid. In the absence of an
appreciable quantity of either species, buffering action cannot occur.

A titration curve is a graphical

representation of the data
available during a titration. It is a
graph of pH vs the volume of
titrant added. Remember, pH has
been defined as –log [H+] for our
purposes. Figure 1 shows a
titration curve for the titration of
25 mL of a 0.10 M acetic acid
solution with a 0.10 M sodium
hydroxide solution. The region
between points A and B is one
where the pH changes only
slightly as the strong base is
added, which is referred to as the buffer region. The solution present in this region has the
properties of a buffer and the larger this region is the larger the buffering capacity of the
solution. Point C is the equivalence point, where equal amounts of acid and base are present
in the solution. Recall for a weak acid titrated with a strong base the equivalence point will have
a basic, or alkaline, pH as the conjugate base of a weak acid is a fairly good base. The
equivalence point for a strong acid titrated with a strong base will have a pH of 7.0 as the
conjugate base of a strong acid and conjugate acid of a strong base have little, if none, effect
on pH aside from the auto-ionization of water already present in the solution.

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In this lab exercise, we will prepare acetic acid-acetate buffer solutions using three different
approaches. Four titration curves will be produced by measuring pH upon added increments
of titrant (HCl and NaOH) and the buffering capacity of the prepared buffer solutions will be
determined. The definition of buffering capacity will not be as precise as those methods that
determine the equivalence point on a titration curve because the increments of added titrant
used in the four titrations are too large. Here, the buffering capacity will be taken as the quantity
of acid or base that must be added to a buffer to break out of the buffer region of an acid-base
titration curve. In other words, for our purposes, buffering capacity is the largest amount of
added acid or base for which the buffer solution retains its ability to resist large changes in pH.

Procedure

Chemicals: Acetic Acid, CH3COOH (0.10 M)

Hydrochloric Acid, HCl (0.10 M)
Sodium Acetate, NaCH3COOH, (0.10 M)
Sodium Hydroxide, NaOH (0.10 M)

Equipment and Supplies: 50 mL Buret (stock room)

Magnetic stir bar (stock room)
pH Meter (stock room)
10 and 25 mL graduate cylinder
Various sizes of beakers
Wash bottle

Safety and Waste Disposal:

Many chemicals are considered toxic. Hazard information is printed on the chemical label.

Combine all your solutions in one common beaker. If the pH of your titrated solutions is 5–
12 the solution may be disposed of by pouring them down the drain followed by plenty of
tap water.

If your combined solution or any residual solution is not within the allowable range, place
the pH probe in the solution and slowly add sodium carbonate until the pH of the solution
is between 5 and 12. The solution may be disposed of down the drain as directed above.

DO NOT PUT ANY SOLUTIONS DOWN THE DRAIN IF THE pH IS LESS THAN 5 OR
GREATER THAN 12.

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Part A: Pre-Lab Exercise for the Preparation of Buffers.

1. Write the net ionic equations for the reactions, if any, for solutions a through f. Enter your
net ionic equations, if any, in the Pre-Lab Exercise portion of the laboratory report.

2. Using the net ionic equations in Part A.1 as a starting point, devise two other ways you could
prepare 50 mL of a solution that contains the same concentrations of acetic acid and acetate
as in buffer 1A. These two buffers will be known as 2a and 2b. Review the introduction of this
lab in which three approaches on how to prepare a buffer are described. In each case, use only
two of the mixed solutions mentioned in Part A.1. Do not use water. Make calculations that
verify that the concentrations of acetic acid and acetate ions in buffer 2a and 2b are the same
as the concentrations in the original buffer of 1a. Note: Mixing 25 mL of 0.20 M acetic acid and
0.20 M sodium acetate is not satisfactory as the concentrations of acetic acid and acetate ion
in the final mixture will be twice those in the original buffer of Part B.1. Verify with the instructor
before continuing.

Part B: Preparation of Three Identical Acetic Acid-Acetate Buffers by Different Routes and
the Measurement of the pH of these Buffers.

Work in pairs. Each group should obtain one 50 mL buret and one magnetic stir bar from the
stockroom. Make all pH measurements with a pH meter.

0. Standardize the pH meter following the instructions in Appendix (Part 5).

1. Preparation of Buffer 1a: Using a graduated cylinder, obtain a 25 mL portion of 0.10 M

acetic acid and place it in a beaker. Measure the pH of the solution. Obtain a 25 mL
portion of 0.10 M sodium acetate and measure and record its pH. Now pour the solutions
together and measure and record the pH of the mixture. Calculate (from solution
stoichiometry, ignoring equilibrium effects) the concentration of acetic acid and acetate
ion in the buffer (mixture). Enter your values in Part B.1 (a-c) of the laboratory report.
Label this mixture buffer “1a”.

2. Preparation of Buffer 2a and 2b: Prepare two additional buffers, designated “2a” and
“2b”, and measure the pH of each. If you have designed your buffers correctly, there
might still be some small deviation in pH from your expected value. The stock solutions
are only approximate in concentration, and, in addition, the solutions are too concentrated
to behave ideally. Enter the requested information in Part B.2 (a-b).

3. Preparation of Buffer 3a and 3b: Measure 10 mL of buffer 2b and add it to 90 mL of

deionized water, mix well, and measure the pH of this diluted buffer. This buffer will be
designated “3”. Enter the requested information in Part B.3. Finally, divide buffer 3 into
two 50 mL portions and label these buffers “3a” and “3b”.
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Part C: Titration of the Buffers and the Effect of Dilution on pH and Buffer Capacity.

One way to save time when titrating is to perform the two titrations using HCl as the titrant for
buffers 1a and 3a and those using NaOH as the titrant for buffers 2a and 3b back-to-back. It
does not matter which titrant you use first. This way the buret will only have to be rinsed three
times during the laboratory exercise. The buret will be rinsed before the first two titrations,
before the last two titrations, and before you return the buret to the stockroom.

1. Buffer 1a: Titrate with 0.10 M hydrochloric acid and measure the pH after each addition
of 3.0 mL of titrant until a total of 33.0 mL of HCl has been added. You should have 11
data points in total.

2. Buffer 2a: Titrate with 0.10 M sodium hydroxide and measure the pH after each addition
of 3.0 mL of titrant until a total of 33.0 mL of NaOH has been added. You should have
11 data points in total.

3. Buffer 3a: Titrate with 0.10 M hydrochloric acid and measure the pH after each addition
of 0.5 mL until you have added a total of 5.0 mL of HCl has been added. You should
have 10 data points in total.

4. Buffer 3b: Titrate with 0.10 M sodium hydroxide and measure the pH after each
addition of 0.5 mL until you have added a total of 5.0 mL of NaOH has been added.
You should have 10 data points in total.

Because the term buffer capacity has been defined for this laboratory so crudely, there
is no need for precise volume measurements. Buret readings to the nearest 0.1 mL will
be adequate for your needs. Adjust the increments of titrant addition appropriately if
time does not allow for a large number of data points to be collected. Plot the “titration”
curve for each data set. Estimate the buffer capacity as mL of the appropriate titrant.
See the notes on graphing and plotting in Part D for hints on how to plot the data that
you have recorded.

Part D: Some Notes on Graphing Your Data.

For this laboratory experiment, you are asked to plot your data recorded from Part C. You
are to do this by using a spreadsheet program such as Microsoft Excel or Google Sheets.
The following are a few suggestions for your graphs.

1. Your graphs are two-dimensional and are often called x-y plots, in which the x-axis
represents the independent variable, and the y-axis represents the dependent variable.
In this experiment, the independent variable is the number of mL of titrant added, while
the dependent variable is the pH of the solution resulting from the addition.
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2. Arrange the scales such that the data “fills” the entire graph. Make sure the graduations
in your graph are legible and have a regular interval, such as every 1 or 0.5 mL
depending on your data set.

3. The labels for each axis should be clear and concise and must include the units of your data.
For example, the x-axis of one of your plots might be labeled “Volume 0.10 M NaOH
added (mL)”

4. Plot your points clearly and do not include lines between those points (i.e., markers
only). For this laboratory experiment, you might try sketching a light curve through your
points, similar to the shape of the curve in Figure 1, to help you identify the portions of
the graph described in the problems and questions. The curve should be generated by
hand drawing a best-fit line (curve) rather than a point-to-point line.

5. The title of your plot should be descriptive of the experiment so that one graph is not
mistaken for another set of data plotted.

6. Print and attach your graphs to the end of this document for a complete grade. Consult
your lab instructor on the size and scale of each graph, (i.e., one per page, two per
page, or all four on one page).

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Data Sheet: BUFFERS: ACETIC ACID-ACETATE Name: _____________________

Lab Day:________ Time:______

Part A: Pre-Lab Exercise for the Preparation of Buffers

1. Write the net ionic equations for the following reactions. Note, if you do not expect a
reaction to occur indicate this by saying “no reaction”.

a. acetic acid (0.20 M) and sodium acetate (0.20 M)

b. acetic acid (0.20 M) and hydrochloric acid (0.10 M)

c. acetic acid (0.20 M) and sodium hydroxide (0.10 M)

d. sodium acetate (0.20 M) and hydrochloric acid (0.10 M)

e. sodium acetate (0.20 M) and sodium hyroxide (0.10 M)

f. hydrochloric acid (0.10 M) and sodium hydroxide (0.10 M)

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2. Calculations for the Preparation of Buffers in Part B: Part B.1 in the procedure describes
one way to make a buffer by mixing 25 mL each of 0.10 M acetic acid and 0.10 M acetate
ion to produce a 50 mL buffer. Calculate the concentrations of acetic acid and acetate
ion in Buffer 1a. Show your work to receive full credit.

a. [CH3COOH] in buffer 1a _______________________ M

b. [CH3COO–] in buffer 1a _______________________ M

Refer to reactions 1-4 of the introduction and devise two other ways to prepare the acetic
acid buffer solution with the same volume and species concentrations as Buffer 1a.

c. Which two reactions, b-f on the previous page, yield solutions containing the
same two species that are present in the buffer of Part B.1?

d. Describe the preparation of the two “new” buffers. Specify the volume,
concentration and name of each solution used in the preparations. The solutions
needed to make the buffer two other ways are located in the back of the
laboratory. These two “new” buffers should have the same final volume and
concentrations of acetic acid and acetate ion as Buffer 1a.

Solution Names Concentration (M) Volume (mL)

Buffer 2a

Buffer 2b

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e. Use the table below to calculate the final concentration of acetic acid and acetate
ion in Buffer 2a and Buffer 2b. Show calculations that verify that the final
concentation of acetic acid and acetate ion are identical to the concentration of
these species in Buffer 1a. Both dilution and the reaction between species affect
these concentrations. Show your work in calculating the initial concentrations.

Buffer 2a

Reaction:

Initial
Concentration
(after dilution):

Change:

Final
Concentation:

Buffer 2b

Reaction:

Initial
Concentration
(after dilution):

Change:

Final
Concentation:

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Part B: Measurement of the pH of Acetic Acid-Acetate Buffers

1. Buffer 1a

a. measured pH of 0.10 M acetic acid: ______________________________

b. measured pH of 0.10 M sodium acetate ______________________________

c. measured pH of Buffer 1a ______________________________

2. Buffer 2a & 2b

a. measured pH of Buffer 2a ______________________________

b. measured pH of Buffer 2b ______________________________

3. Buffer 3 (dilute)

a. measured pH of Buffer 3 ______________________________

Part C: Titration of Buffers and Plotting Titration Curves: Determining the Effect of
Dilution on pH and Buffering Capacity.

1. Record the titration data for each of the four titrations on one or more separate sheets
of paper. Use Microsoft Excel or Google Sheets to generate your graphs. Consult your
laboratory instructor on the size and scale of your graphs (i.e., one per page, two per
page, or all four on one page). Label the axes with names, units, and numbers. Title each
curve. See Part D in the procedure section for guidance.

2. Estimate the buffer capacity of each buffer with respect to the addition of the 0.10 M
HCl and 0.10 M NaOH from your titration curves.

a. Buffering Capacity of Buffer 1a __________________ mL

b. Buffering Capacity of Buffer 2a __________________ mL

c. Buffering Capacity of Buffer 3a __________________ mL

d. Buffering Capacity of Buffer 3b __________________ mL

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Questions

1. Refer to your results in Part B and answer the following questions.

a. Use the measured pH value of the 0.10 M acetic acid solution to calculate Ka of
acetic acid. Show your work for full credit.

b. Use the accepted value of Ka (1.78 x 10–5) to calculate the pH of 0.10 M acetic
acid. Show your work for full credit.

c. Calculate the % error of the experimental Ka. Show your work for full credit.

d. Calculate the % error of the experimental pH. Show your work for full credit.

e. A small “error” in pH measurements leads to a ___________ “error” in Ka

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2. Refer to your results in Part C and answer the following questions.

a. Does dilution significantly change the pH of a buffer? Explain briefly.

b. Does dilution significantly change the buffering capacity of a buffer? Does it

decrease, increase, or remain the same? Explain briefly.

3. Would a buffer containing HF and F– in appreciable quantities be expected to have a

pH of around 3, 5, 7, or 9? It may help to look up the Ka value of HF in the literature.
Justify your answer briefly.

4. Consider a buffer containing a weak acid and an anion of that weak acid. If you needed
to prepare such a buffer having a pH of around 8, would you select an acid having a Ka
of around 4x10–4, 8x10–9, or 2x10–11? Justify your answer briefly.

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