Acid-Base Equilibrium

Lab: Determination of the Identity of an Unknown Weak Acid

Introduction:
A common question chemists have to answer is how much of something is present in a sample or a
product. If the product contains an acid or base, this question is usually answered by a titration. Acidbase titrations can be used to measure the concentration of an acid or base in solution, to calculate the
molar mass of an unknown acid or base, and to determine the equilibrium constant of a weak acid (Ka) or
weak base (Kb).
Concepts:
Weak Acid
Equivalence Point

Equilibrium Constant, Ka
End Point

Titration Curve
Indicator

Background:
Titration is a method of volumetric analysisthe use of volume measurements to analyze an
unknown. In acid-base chemistry, titration is most often used to analyze the amount of acid or base in a
sample or solution. Consider a solution containing an unknown amount of hydrochloric acid. In a
titration experiment, a known volume of the hydrochloric acid solution would be titrated by slowly
adding drop wise a standard solution of a strong base such as sodium hydroxide. (A standard solution is
one whose concentration is accurately known.) The titrant, sodium hydroxide in this case, reacts with
and consumes the acid via a neutralization reaction (Equation 1). The exact volume of base needed to
react completely with the acid is measured. This is called the equivalence point of the titrationthe point
at which stoichiometric amounts of the acid and base have combined.
HCl(aq) + NaOH(aq)

NaCl(aq) + H2O(l)

Equation 1

Knowing the exact concentration and volume added of the titrant gives the number of moles of
sodium hydroxide. The latter, in turn, is related by stoichiometry to the number of moles of hydrochloric
acid initially present in the unknown.
Indicators are usually added to acid-base titrations to detect the equivalence point. The endpoint
of the titration is the point at which the indicator changes color and signals that the equivalence point has
indeed been reached. For example, in the case of the neutralization reaction shown in Equation 1, the pH
of the solution would be acidic (< 7) before the equivalence point and basic (> 7) after the equivalence
point. The pH at the equivalence point should be exactly 7, corresponding to the neutral products
(sodium chloride and water). An indicator that changes color around pH 7 is therefore a suitable
indicator for the titration of a strong acid with a strong base.
The progress of an acid-base titration can also be followed by measuring the pH of the solution
being analyzed as a function of the volume of titrant added. A plot of the resulting data is called a pH
curve or titration curve. Titration curves allow a precise determination of the equivalence point of the
titration without the use of an indicator.
In this experiment, the pH of the titration solution will be monitored using a pH meter; the
obtained titration plot will then be used to determine the molar mass and equilibrium constant (Ka) of
the unknown. These values will then let you decide the identity of the weak acid.

The molar mass is determined by titrating an acid with a standard solution of NaOH. Since one
mole of NaOH reacts with one mole of hydrogen ion, at the equivalence point the following relation holds:
Vb

Mb = moles base = moles H+

Equation 2
Equation 3

where Vb is the volume of the base added at the endpoint, Mb is the molarity of the base, grams acid is the
mass of acid used, and MMa is the molar mass of the acid.
A graph of pH versus volume of NaOH added (See Figure 1) for the titration of a weak acid with
NaOH is obtained by carefully following the titration with a pH meter. There is a significant change in pH
in the vicinity of the equivalence point. Note that when a weak acid is titrated with a strong base, the
equivalence point is NOT at pH 7, but is on the basic side. The value of the equilibrium constant for the
dissociation of the acid is determined from a titration curve by considering the pH when the acid is halfneutralized.
If the dissociation of the acid is represented as:
Equation 4
the equilibrium constant expression is:
[

][
[

Equation 5

When the acid is half neutralized, [HA] = [ ], these terms cancel in Equation 5 above, and
Ka = [H3O+]. Therefore, when the acid is half-neutralized, the pH = pKa. The point where pH is equal to
pKa can be determined from the graph. (See Figure 1)

1.
2.
3.
4.

Initial pH is in acidic range, though not as low as strong acid.

pH stays relatively constant through this buffer region.
There is a jump in pH from pH 7 to pH 11. pH at equivalence is > 7.
After equivalence, pH flattens out at high value (pH of a strong base).

Materials:
Chemicals
Phenolphthalein indicator solution, 1.0%, 1mL
Sodium hydroxide solution, NaOH, 0.1M
Unknown weak acid
Distilled Water

Equipment
Balance
Beaker, 250mL
Buret, 50mL
Erlenmeyer Flask, 125mL or 250mL
Funnel
Magnetic Stirrer and Stir Bar
pH Probe
Data Collection Device
Wash Bottle

Safety Precautions:
Dilute sodium hydroxide solutions are irritating to skin and eyes. Phenolphthalein is an alcoholbased solution and is flammable. It is moderately toxid by ingestion. Keep away from flames and other
ignition sources. Avoid contact of all chemicals with eyes and skin and wash hands thoroughly with soap
and water before leaving the laboratory. Wear chemical splash goggles and chemical resistant gloves and
apron.
Procedure:
IT IS IMPORTANT THAT YOU ARE CAREFUL WITH THE TIP OF THE pH PROBE! THEY EASILY BREAK!!
Carefully unscrew the container of storage solution at the tip of the pH probe and set the container in a
safe place where it will not tip over. When you are not using the pH probe, gently rest it in a beaker of tap
water.
Be sure to rinse the pH probe with distilled water EACH TIME before using!
Part 1-Prepare for Data Collection
1. Connect the Chemistry sensor with pH probe attached to the SPARKlink Air.
a. Turn on and connect the SPARKlink Air to your device.
b. Connect the Temperature Probe to the SPARKlink Air interface.
c. Turn on the SPARKlink Air using the black power button on the back of the SPARKlink Air.
d. Under the Settings on your iPad select Bluetooth.
e. Ensure that the Bluetooth is in the ON position on your iPad. Select the SPARKlink Air
device that matches the number on the back of the SPARKlink Air that your group is using.
WAIT. You will see the device as Connected when you have successful linked the
SPARKlink Air to your iPad.
2. Open the SPARKvue App on your iPad and prepare for data collection.
a. WAIT UNTIL until the SPARKvue APP picks up the Chemistry sensor with pH probe that is
connected to your SPARKlink Air device. If it does not pick up your desired probe, close the
app, return to settings, return to Bluetooth, disconnect the SPARKlink, and then reconnect
the SPARKlink.
b. Select Build.
c. Choose a Background Image that has two boxes.
d. One box should depict a graph. The second box should depict a data table.
3. Touch the
icon at the bottom the screen and change the settings for data collection from
periodic to manual.

4. Set up your graph to show volume (on the x-axis) and pH (on the y-axis).
a. Touch one of the axis labels.
b. Horizontal Axis (x)
i. Measurement > Time > User-entered > Create Data Set (User-entered Number Data)
1. Measurement Name: Volume
2. Unit Name: mL
3. Touch OK
c. Vertical Axis (y)
i. Measurement > Sensors > pH
ii. Touch OK
5. Set up your data table to show volume (in the first column) and pH (in the second column).
a. Touch the label for the first column.
i. Column: 1
1. Measurement > Time > User-entered > Volume
ii. Column: 2
1. Measurement > Sensors > pH
6. You are now ready to collect data.

SIMULTANEOUSLY
Group Members 3-4
Group Members 1-2

Part 2-Determination of the Molar Mass of an Unknown Acid

1. Based on the assignment provided by your instructor, weigh about
Group A
Group B
0.1-0.2g
0.2-0.3g
of a sample of the unknown acid in a weighing dish using an analytical balance. Record the precise
mass in the appropriate Data Table.
2. Transfer the unknown acid into an Erlenmeyer flaskuse a funnel to facilitate the transfer. Use
distilled water from a wash bottle to rinse all of the remaining solid from the weighing dish or
funnel into the flask as well.
3. Add about 50mL of distilled water to the Erlenmeyer flask and swirl until all of the unknown acid
is dissolved.
4. Clean your buret, then rinse it with three small portions (about 7mL each) of the NaOH solution
and discard as directed.
5. Fill the buret to above the zero mark with the NaOH solution.
6. Open the buret stopcock to allow any air bubbles to
escape from the tip. Close the stopcock when the liquid
level is between the 0 and 10 mL marks.
7. Measure the precise volume in the buret and record this
value in the appropriate Data Table as initial volume.
Note: volumes are read from the top down in a buret.
Always read from the bottom of the meniscus
remembering to include the appropriate number of
significant figures.

8. You will be provided with various indicators. Add three drops of the indicator that your group
determines to be the appropriate indicator for the titration to the unknown acid solution in the
flask.
9. Carefully add a magnetic stir bar to the flask and thoroughly stir your acid solution before
continuing.
10. Touch the

button.

11. Place the pH probe in the Erlenmeyer flask containing the unknown acid solution. Touch the
button ONCE to record the initial pH of your unknown acid solution. Touch the Volume column in
your data table next to the pH value that you just recorded. Enter a volume of 0.00mL.
12. Begin the titration by adding 1mL of the NaOH solution to the Erlenmeyer flask. Close the buret
stopcock and place the flask on the stir plate to mix the contents.
13. Remove the flask from the stir plate and carefully place the pH probe in the Erlenmeyer flask
containing the unknown acid solution. Touch the
button ONCE to record the pH of the
solution after this addition. Touch the Volume column in your data table next to the pH value that
you just recorded. Record the exact volume added to the hundredths place. There is also a place
to record this value in your data table.
14. Add another 1 mL increment of sodium hydroxide solution. Close the buret stopcock and place
the flask on the stir plate to mix the contents.
15. Remove the flask from the stir plate and carefully place the pH probe in the Erlenmeyer flask
containing the unknown acid solution. Touch the
button ONCE to record the pH of the
solution after this addition. Touch the Volume column in your data table next to the pH value that
you just recorded. Record the exact volume added to the hundredths place. There is also a place
to record this value in your data table.
16. Continue adding NaOH in 1 mL increments. Be sure to stir the solution thoroughly and record the
exact volume of NaOH added after EACH addition.
17. When the pH begins to increase by more than 0.3 pH units after 1 mL of NaOH is added, decrease
the amount of sodium hydroxide added to about 0.2 mL.
18. Continue adding NaOH in about 0.2 mL increments. Be sure to stir the solution thoroughly and
record the exact volume of NaOH added after EACH addition.
19. When the pH change is again about 0.3 pH units, resume adding the sodium hydroxide in 1 mL
increments. Be sure to stir the solution thoroughly and record the exact volume of NaOH added
after EACH addition.

20. Stop the titration by touching the

button when the pH of the solution is greater than 12.
Record the final volume of solution in the buret in your Data Table.
21. Screen shot your graph and upload to your Drive account. Share with group members.
22. Clean up and dispose of chemicals as directed by your instructor.

Data:

Data Table 1
Trial 1

Mass of Unknown Acid, g

Final Volume, mL
Initial Volume, mL
Volume of NaOH added, mL
Concentration of Standardized NaOH, M
Moles of NaOH added, mol
Moles of H+ ion reacted, mol
Molar Mass of Unknown Acid, g/mol

Data Table 2
Group 2 Molar Mass
Group 3 Molar Mass

Group 1 Molar Mass

Volume NaOH
Added
(mL)

.101 g
8.00 mL
0 mL
8.00 mL
0.1 M
.0008 mol
.0008 mol
126.25 g/mol

pH

Data Table 3
Volume NaOH
Added
pH
Continued
(mL)

Average Molar Mass

Volume NaOH
Added
Continued
(mL)

pH

Calculations:
1. From the information collected in Data Table 1, show the calculations for the molar mass of the
unknown acid for your individual trial.

2. From the information collected in Data Table 2, show the calculations for determining the average
molar mass for the unknown acid for the trials from three separate groups.

3. From the titration curve of pH versus volume of NaOH added, determine the pKa of the unknown
acid. Show the calculations for determining the value of Ka for the unknown acid.

4. Use the molar mass and pKa values that you calculated above and the information provided below
to determine the identity of your unknown acid.
Name
glycolic
acid
potassium dihydrogen
phosphate
potassium hydrogen
sulfate
potassium hydrogen
sulfite
sodium dihydrogen
phosphate
sodium hydrogen
sulfate
sodium hydrogen
sulfite
sodium hydrogen
tartrate

Formula of Most
Common Form

Molar Mass
(g/mol)

Ka

pKa

HC2H3O3

76.05

1.6x10-4

3.80

KH2PO4

136.09

Ka2 of H3PO4 = 6.2x10-8

7.21

KHSO4

136.17

Ka2 of H2SO4 = 1.2x10-2

1.92

KHSO3

120.16

Ka2 of H2SO3 = 6.4x10-8

7.19

NaH2PO4H2O

138.01

Ka2 of H3PO4 = 6.2x10-8

7.21

NaHSO4H2O

138.08

Ka2 of H2SO4 = 1.2x10-2

1.92

NaHSO3

104.07

Ka2 of H2SO3 = 6.4x10-8

7.19

NaHC4H4O6H2O

190.09

Ka2 of H2C4H4O6 = 4.6x10-5

4.34

Identity of Unknown Acid

potassium hydrogen sulfite