NSCI/NENG 115: Chemical Principles of NANO I

Experiment 4: Acid-Base Titration

Lab Designers: Susan Sharfstein and Sarah Nicoletti
Zumdahl: Chapters 7 and 8
Edited 10-15-14 by Thomas Begley

I. Safety Instructions:
Follow all standard safety rules as demonstrated in class. Safety glasses, lab-coats, and
gloves must be worn when working with chemicals. Special caution should be exercised when
working with chemicals and glass products which are easily broken. Do not allow chemicals to
come into contact with your skin. In particular, hydrochloric acid, sodium hydroxide, and acetic
acid solutions are corrosive. Solid sodium hydroxide is also corrosive and much heat evolves
when sodium hydroxide is added to water. Contact can cause severe burns to skin and eyes. If
skin contact should occur, rinse the affected area with plenty of water. All of the acids are also
volatile and irritating or toxic by inhalation. Concentrated acid solutions should be handled
within a fume hood. Hands should be washed at the end of the laboratory activity. Dispose of
acid-base reactions in the appropriate waste container. Dispose of sharps in the sharp container.

II. Objectives:

1. Prepare an aqueous solution of sodium hydroxide to a target molar concentration.

2. Determine the concentration of your NaOH solution by titrating it with a solution of
potassium hydrogen phthalate, abbreviated KHP, with an exact molar concentration.
3. Use the NaOH solution prepared to accurately conduct acid-base titrations.
4. Determine the equivalence point of a strong acid-strong base titration.
5. Determine the equivalence point of a weak acid-strong base titration.
6. Calculate the molar concentrations of two acid solutions.

III. Procedure Outline:

This will be a two-week laboratory. In the first week, you will prepare and standardize a solution
of sodium hydroxide. In the second week, you will use that sodium hydroxide solution to
calculate the concentrations of unknown solutions of hydrochloric acid and acetic acid. You will
also explore the use of various indicator dyes for the determination of pH optically.

1. The instructor will demonstrate the use of the Vernier pH electrodes and Labquest
devices (Part A)
2. Prepare a solution of 250 ml of 0.1 M NaOH (Part A)
3. Determine the exact concentration of your sodium hydroxide solution, by titrating your
solution with sufficient KPH to neutralize 15 mL of 0.10 M NaOH (Part A)
4. Use your standardized NaOH solution to titrate solutions of unknown concentrations of
hydrochloric acid and acetic acid (Part B)
5. Determine the equivalence points of the strong and weak acid titrations and the molar
concentrations of the solutions (Part B)
6. Use your equation to determine the pH of an unknown solution (Part B)
IV. Background:

Part A. Standardization of sodium hydroxide solution concentration1: It is often necessary to

test a solution of unknown concentration with a solution of a known, precise concentration. The
process of determining the unknown’s concentration is called standardization.

Solutions of sodium hydroxide are virtually impossible to prepare to a precise molar

concentration because the substance is hygroscopic. In fact, solid NaOH absorbs so much
moisture from the air that a measured sample of the compound is never 100% NaOH. On the
other hand, the acid salt potassium hydrogen phthalate, KHC8H4O4, can be measured out in
precise mass amounts. When dissolved in water, KHP is a weak acid that reacts with NaOH in a
simple 1:1 stoichiometric ratio, thus making it an ideal substance to use to standardize a solution
of NaOH. In addition to being hygroscopic, sodium hydroxide will react with the carbon dioxide
in air, so it is very important to keep your sodium hydroxide solution in a sealed container except
when using it to perform a titration reaction.
Before coming to lab you will need to calculate the mass of sodium hydroxide needed to
prepare 250 mL of a 0.10 M solution and the mass of KHP needed to react completely with
15 mL of a 0.10 M NaOH solution. These numbers should be clearly indicted in your
notebook and Dr. Begley must initial your numbers before you weigh out the amount.
Consider the reaction equation to be as shown below.

HP– (aq) + OH– (aq) → H2O(l) + P2– (aq)

The equivalence point is the point at which you have added enough
base to neutralize all of the acid as shown in the figure to the right.
You will titrate to find the equivalence point using two approaches,
first the addition of phenolphthalein (which will turn pink once you
have reached the equivalence point) and second, by measuring the
pH and calculating the first and second derivatives of a pH vs.
volume added curve.

Part B. Calculation of the concentrations of two unknown acids,

a strong acid (HCl) and a weak acid (acetic acid)2: A titration is a
process used to determine the volume of a solution that is needed to
react with a given amount of another substance. In this experiment,
your goal is to determine the molar concentration of two acid solutions by conducting titrations
with a base of known concentration. You will be testing a strong acid, HCl, solution and a weak
acid, HC2H3O2, solution. You will use the sodium hydroxide, NaOH, solution that you
standardized above as your base of known concentration. The reaction equations are shown
below in net ionic form.
H+ (aq) + OH– (aq) → H2O(l)
HC2H3O2(aq) + OH– (aq) → H2O(l) + C2H3O2– (aq)
The stoichiometry of the two reactions is identical; thus, your calculations will be
straightforward. However, you will observe a significant difference in how the two acid solutions
react with NaOH.
In this experiment, you will monitor pH as you titrate. The region of most rapid pH change will
then be used to determine the equivalence point. The volume of NaOH titrant used at the
equivalence point will be used to determine the molarity of the acid solutions.

V. Detailed Procedure (Work in groups of two or three)

Part A:
1. Measure out ~150 mL of distilled water into a 200 mL beaker.
2. Measure out the mass of NaOH that is needed to prepare 250 mL of a 0.10 M solution and
add it to the flask of distilled water. Remember that Dr. Begley should have seen this
number in your notebook and initialed it. Stir the contents of the beaker to dissolve the
solid. CAUTION: Sodium hydroxide solution is caustic. Avoid spilling it on your skin or
clothing.
3. Transfer the solution completely to a 500 ml volumetric cylinder and add water to the fill line
to make exactly 250 ml of solution.
4. Measure out the mass of KHP that will completely neutralize 15 mL of 0.10 M NaOH
solution. Remember that Dr. Begley should have seen this number in your notebook and
initialed it. Dissolve the KHP in about 50 mL of distilled water in a 250 mL beaker. Place
the beaker of KHP solution on a magnetic stirrer and add a stirring bar. Add 1-2 drops of
phenolphthalein solution.
5. Connect the pH Sensor to LabQuest and choose New from the File
menu.
6. Set up a ring stand, buret clamp, and buret to conduct a titration (see
Figure 3). Rinse and fill the buret with the NaOH solution.
7. Use a utility clamp to suspend the pH Sensor on a ring stand as
shown in Figure 3. Position the pH Sensor in the KHP solution and
adjust its position so that it is not struck by the stirring bar. Gently
stir the beaker of solution.

8. On the Meter screen, tap Mode. Change the data-collection mode to

Events with Entry. Enter the Name (Volume) and Unit (mL). Figure 3

9. Collect titration data. Conduct the titration carefully, as described

below.
a. Start data collection.
b. Before you have added any of the NaOH solution, tap Keep and enter 0 as the buret
volume in mL. Select OK to store the first data pair.
c. Add the next increment of NaOH titrant (enough to raise the pH about 0.3 units). When
the pH stabilizes, tap Keep, and enter the current buret reading as precisely as possible.
Select OK to store the second data pair.
d. When a pH value of approximately 6.5 is reached, change to 1–3 drop increments. Enter a
new buret reading after each increment. At about pH 6.7, add NaOH one drop at a time.
Note also the volume at which the pink color appears and remains constant
e. After a pH value of approximately 10 is reached, again add larger increments that raise the
pH by about 0.3 pH units, and enter the buret reading after each increment.
f. Continue adding NaOH solution until the pH value remains constant.
10. Stop data collection to view a graph of pH vs. volume. Dispose of the reaction mixture as
directed. Rinse the pH Sensor with distilled water in preparation for a second titration.

11. Examine your titration data to identify the region where the pH made the greatest increase.
The equivalence point is in this region.
a. To examine the data pairs on the displayed graph, select any data point.
b. As you move the examine line, the pH and volume values of each data point are displayed
to the right of the graph.
c. Identify the equivalence point (i.e., volume of NaOH that puts pH at 7.0) as precisely as
possible and record this information.
d. Store the data from the first run by tapping the File Cabinet icon.
12. An alternate way of determining the precise equivalence point of the titration is to take the
first and second derivatives of the pH-volume data.
Determine the peak value on the first derivative vs. volume plot.
a. Tap the Table tab and choose New Calculated Column from the Table menu.
b. Enter d1 as the Calculated Column Name. Select the equation 1st Derivative (Y,X). Use
Volume as the Column for X and pH as the Column for Y. Select OK.
c. On the displayed plot of d1 vs. volume, examine the graph to determine the volume at the
peak value of the first derivative.

Determine the zero value on the second derivative vs. volume plot.
d. Tap Table and choose New Calculated Column from the Table menu.
e. Enter d2 as the Calculated Column Name. Select the equation 2nd Derivative (Y,X). Use
Volume as the Column for X and pH as the Column for Y. Select OK.
f. On the displayed plot of d2 vs. volume, examine the graph to determine the volume when
the 2nd derivative equals approximately zero.
13. Repeat the titration with a second KHP solution. Analyze the titration results in a manner
similar to your first trial and record the equivalence point.

14. Transfer the data to a computer, using Logger Pro software. Print a copy of the graph of each
titration.

15. Store your NaOH solution for next week as directed.

 Part B:
1. Obtain about 65 mL of a hydrochloric acid solution of unknown concentration. Add to a 250
mL beaker. CAUTION: Handle the hydrochloric acid with care. It can cause painful burns
if it comes in contact with the skin.

2. Place 1-2 drops of of phenolphthalein solution into the HCl solution.

3. Place the beaker on a magnetic stirrer and add a stirring bar.

4. Connect the pH Sensor to LabQuest and choose New from the File menu.

5. Set up a ring stand, buret clamp, and 25 mL buret to conduct the titration (see Figure 3).
Rinse and fill the buret with your standardized 0.1 M NaOH solution. CAUTION: Sodium
hydroxide solution is caustic. Avoid spilling it on your skin or clothing.

6. Use a utility clamp to suspend the pH Sensor on the ring stand, as shown in Figure 3.
Position the pH Sensor so that its tip is immersed in the HCl solution but is not struck by the
stirring bar. Gently stir the beaker of acid solution.

7. On the Meter screen, tap Mode. Change the data-collection mode to Events with Entry. Enter
the Name (Volume) and Unit (mL) and select OK.

8. Conduct the titration carefully, as described below.

a. Start data collection.
b. Before you have added any NaOH solution, tap Keep and enter 0 as the buret volume in
mL. Select OK to store the first data pair.
c. Add the next increment of NaOH titrant (enough to raise the pH about 0.3 units). When
the pH stabilizes, tap Keep, and enter the current buret reading as precisely as possible.
Select OK to save the second data pair.
d. Continue adding NaOH solution in increments that raise the pH by about 0.3 units and
enter the buret reading after each increment. When a pH value of approximately 3.5 is
reached, change to a one-drop increment. Enter a new buret reading after each increment.
e. After a pH value of approximately 10 is reached, again add larger increments that raise the
pH by about 0.3 pH units, and enter the buret level after each increment.
f. Continue adding NaOH solution until the pH value remains constant.
9. Stop data collection to view a graph of pH vs. volume.

10. Dispose of the reaction mixture as directed. Rinse the pH Sensor with distilled water in
preparation for the second titration.

11. Examine your titration data to identify the region where the pH made the greatest increase.
The equivalence point is in this region.
a. To examine the data pairs on the displayed graph, select any data point.
b. As you move the examine line, the pH and volume values of each data point are displayed
to the right of the graph.
c. Identify the equivalence point as precisely as possible and record this information.
d. Store the data from the first run by tapping the File Cabinet icon.
12. An alternate way of determining the precise equivalence point of the titration is to take the
first and second derivatives of the pH-volume data.
 Determine the peak value on the first derivative vs. volume plot.
a. Tap the Table tab and choose New Calculated Column from the Table menu.
b. Enter d1 as the Calculated Column Name. Select the equation 1st Derivative (Y,X). Use
Volume as the Column for X and pH as the Column for Y. Select OK.
c. On the displayed plot of d1 vs. volume, examine the graph to determine the volume at the
peak value of the first derivative.
Determine the zero value on the second derivative vs. volume plot.
d. Tap Table and choose New Calculated Column from the Table menu.
e. Enter d2 as the Calculated Column Name. Select the equation 2nd Derivative (Y,X). Use
Volume as the Column for X and pH as the Column for Y. Select OK.
f. On the displayed plot of d2 vs. volume, examine the graph to determine the volume when
the 2nd derivative equals approximately zero.
13. Conduct one titration trial with the HC2H3O2 solution in the same manner as you did the HCl.
Note that the equivalence point of this titration will not be identical to the HCl titration.
Analyze the titration results and record the equivalence point in your data table.
15. Print a copy of the graph of each titration by transferring the data to a computer, using
Logger Pro software.

VI. Lab Report Outline

1. Purpose. Describe the purpose of the experiment.
2. Materials. List the chemicals and supplies used in the experiment.
3. Experimental Procedure. Describe what was done. Specifically, mention any
changes in procedure or unexpected observations. State who did what in the lab and
in the analysis and write up.
4. Results-Remember these are guidelines for what information should be in your
report. This is not a problem set. You should have complete sentences to answer
these questions and refer to figures and tables you have made.
Part A:
a. Calculate the molar amount of KHP used to neutralize the NaOH solution.

b. Calculate the molar concentration of the NaOH solution that you prepared
(note that this should be calculated from your titration curves, not from the
weight of sodium hydroxide you added-consider why this is).

c. Compare the actual molarity of your NaOH solution with your goal of 0.10 M
and the “molarity” you calculate based on the weight of sodium hydroxide
added to the solution.

d. Show all of your plots for equivalence point

Part B:

a. Calculate the molar amounts of NaOH used in the reaction with the HCl
solution and with the CH3COOH solution.

b. Calculate the molar concentration (molarity) of the HCl solution and the
CH3COOH solution.
 c. Compare the actual molar concentrations of your two acid solutions with your
calculated molarities. Were the calculated molarities of your acid solutions
within a reasonable range (about 5%) of the actual values? If not, suggest
reasons for the inaccuracy.

d. The equivalence points of the two titration curves were not in the same pH
range. Explain and discuss the relationships between concentration and acid
strength, equivalence point and equivalence point pH.

1
Adapted from Advanced Chemistry with Vernier, Experiment 6, Vernier Software and Technology, 2007
2
Adapted from Advanced Chemistry with Vernier, Experiment 7, Vernier Software and Technology, 2007