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Evan Pfeifer
24 July 2016
Acid-Base Equilibria: Identification of an Unknown Diprotic Acid
Introduction
The purpose of this experiment is to identify the point(s) of equilibrium in an acid-base
solution. In an acid-base solution, the reactants exchange protons to create an acid and base. The
acid donates a proton to the solvent to create a base. Strong acids completely dissolve, which
more effectively produces a base, while weak acids dissolve only partially. The example equation
used in this experiment is:

+ + A
HA + H 2 O H 3 O
The first reactant (HA) is a monoprotic acid in this example. In this lab, students will use both
monoprotic and diprotic, which produce graphs with one and two equilibrium points,
respectively. This lab allows students to practice with titration techniques and increases their
understanding of acids, bases, equilibrium points, and their properties.

Procedure
Week 1
The melting point of the solution must be determined. A small sample of the solution is
put in a capillary tube. The capillary tube is then inserted into a MelTemp machine and the
melting point is recorded during a rough (fast) test, and a precise (slow) test.
The second step is titration. A 200 mg sample of crotonic acid is weighed (220 mg) and
put in a 100 mL beaker. 10 mL water is then added. When the acid dissolves in the solution, the

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titration can begin. When setting up the station, the pH monitor was first calibrated with the
room temperature (21.8 C) and pH buffers 4 and 7. The drop counter was aligned underneath the
buret and tested with a waste beaker to ensure that the drops would be counted. The pH monitor
was then submerged in the solution so that the tip was just below the surface. The stir rod was
added and the stir plate was activated. The mL of NaOH in the buret was recorded, and data
collection was begun, with the buret set to drip about one drop per second. When the data
collection was finished, the experiment was repeated to ensure accuracy in the results.
Week 2
The second week was similar in both melting point and titration steps. Students were
given an unknown diprotic acid, out of five, and were instructed to determine which one they
had. Station setup and the experiment was the same for titration, and the melting point
measurement was the same as well. The amount of unknown acid used per titration was reduced
to 100 mg to account for the diprotic acids second reaction.

Results
Week 1
Melting Point
Moles NaOH used
Ka

Trial 1
64-68 C (rough)
0.00244 mol NaOH
3.31x10-5

Trial 2
66-68 C (precise)
0.00245 mol NaOH
3.24x10-5

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pH vs Volume for Crotonic Acid (Trial 1)

14

0.45

12

0.4
0.35

10

pH

0.3

0.25

0.2
0.15

0.1

2
0

pH/V (derivative)

0.05
0

100

200

300

400

500

0
600

Volume (drops)

pH vs Volume for Crotonic Acid (Trial 2)

14

0.35

12

0.3

10

0.25
0.2

pH

0.15

6
4

0.05

pH/ V (derivative)

0.1

10

15

20

25

30

35

-0.05

Volume (mL)

Week 2

Unknown Number: 9

Melting Point
Moles NaOH used
Moles Unknown Acid
Ka1
Ka2
Molar Mass

Trial 1
92-94C (rough)
0.00206 mol NaOH
0.00103 mol
2.57x10-2
1.38x10-4
111 g/mol

Trial 2
92-94C (precise)
0.00256 mol NaOH
0.00128 mol
2.34x10-2
2.24x10-5
89.8 g/mol

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Diprotic Acid Unknown 9 Trial 1

pH

14

0.6

12

0.5

10

0.4

0.3

0.2

0.1

10

15

20

25

30

pH/ V (derivative)

-0.1

Volume (mL)

Diprotic Acid Unknown 9 Trial 2

14

0.7

12

0.6

10

0.5
0.4

pH

0.3

0.2

0.1

10

15

20

Volume (mL)

Calculations and Error Analysis

Example: week 2 trial 1

25

30

-0.1

pH/ Volume (derivative)

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I am confident that my unknown acid from week 2 is oxalic acid. The recorded melting
points were 92-94C for both trials, which was closest to the actual melting point of oxalic acid,
which is 102-103C. The melting points of the other acids were too high for the results to be
considered accurate. The first trial for Ka1 was 2.57x10-2, and the second trial was 2.34x10-2. The
actual Ka1 of oxalic acid is 5.4 x 10-2. The Ka1 of maleic acid is 1.5x10-2, which is much closer to
the achieved Ka1, but the melting point and molar mass more closely resemble oxalic acid, and
the Ka2 is much lower at 8.50x10-7. The value for Ka2 was 1.35 x 10-4 in trial 1 and 2.24 x 10-5 in
trial 2. The actual Ka2 value of oxalic acid is 5.4x10 -5, which would give a percent error of 150%.
The calculated molar mass is 90 g/mol in trial 2. The actual molar mass of oxalic acid is 89.8
g/mol, which is very accurate.

Discussion
The equilibrium constants were the focus of this experiment. When the acid dissolved
into the solution, the H+ protons bonded with H2O to form H3O+, which is a base. The shift in
equilibrium was done by adding more NaOH to the solution. As more OH - ions were added, the
solution became increasingly basic. The equivalence point was reached as the solution became
more basic: once for the first reaction, and then again for the second reaction (in part 2 only). In

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terms of the equation, the diprotic acid turned into a monoprotic acid during the first reaction,
and then the acid was fully dissolved during the second reaction.
I was uncertain what results the experiment would return because I did not know which
acid I had, but I expected the graphs to appear similar to the example, with two equivalence
points. While I attained two equivalence points, the K a1 and Ka2 of the acid were off by quite a
bit. The percent error was 54.6% for K a1 and 150% for Ka2, for trial 1. While this portion of data
is unreliable, the calculated molar mass and melting point were very close to the actual values of
oxalic acid. No other acid has similar values to what was found in lab, which leads me to believe
that my unknown acid is oxalic acid.
It is worth noting that the recommended weights of acid used was 100. mg, while I used
120. and 115 mg for my two trials. The increased concentration of the acid could have affected
the Ka values that were achieved in lab. Other possible errors include the ineffectiveness of the
chemicals used. The accuracy of melting point and molar mass but the incorrectness of the Ka
values leads me to believe that the acid sample I used could have lost some of its effectiveness,
due to the acid sample being expired or otherwise. That being said, I believe a different sample
of oxalic acid would have produced a more accurate Ka1 and Ka2 value.

Conclusion
The goal was to find the point(s) of equilibrium for an unknown solution to discover tbe
unknown acids identity. My unknown acid is believed to be oxalic acid through comparison of
its properties, so the goal was accomplished.