Introduction

A titration is a procedure used in analytical chemistry to determine the amount or concentration

of a substance. In a titration one reagent, the titrant, is added to another slowly. As it is added a
chemical stoichiometric reaction occurs until one of the reagents is exhausted, and some process
or device signals that this has occurred. The purpose of a titration is generally to determine the
quantity or concentration of one of the reagents, that of the other being known beforehand. In
any titration there must be a rapid quantitative reaction taking place as the titrant is added, and in
acid-base titrations this is a stoichiometric neutralization. The type of titration is simply the type
of chemical reaction taking place, and so in this section we consider acid-base titrations.

Equipment

 Phenolphthalein indicator
 Burette
 Pipette
 250 ml beakers
 pH meter
 White paper towel

Methodology

A) Titration of monoprotic acid (acetic acid) with NaOH

1. 0.1 M NaOH filled in burette. 25.00 mL of CH3COOH pipetted in 250 mL beaker and 3
drops phenolphthalein indicator added. The beaker placed on a jubin.
2. Titrate the solution by added the NaOH titrant in 2 mL increments. Carefully swirl the
beaker with each addition.
3. The colored form of the phenolphthalein will begin to stay for a while and then
disappear. At this point, the dropwise NaOH added until the acetic acid is very light
color. This is the endpoint of phenolphthalein.
4. The pH of the solution in the beaker at this end point recorded and measured by pH
meter.
5. Any color change observed during the titration recorded. The pH and NaOH volume
added at that indicator’s endpoint.
6. The pH/ volume data transferred to an Excel file.
7. The data transfer to graph pH vs Volume of NaOH to observe the equivalence point and
half equivalence point.
8. Using the titration curve, the pH at this volume can be determined.
9. pKa and Ka for acetic acid calculated.
 B) Titration of polyprotic acid (phosphoric acid) with NaOH
The all steps above repeated with phosphoric acid.

Results and calculations

1. Monoprotic acid

Volume of NaOH, mL pH

2 3.18

4 3.35

6 3.82

8 4.32

10 4.53

12 4.7

14 4.86

16 5.2

18 5.5

20 5.8

22 6.7

24 7.1

26 11

28 11.4

30 11.7

32 12

34 12.3

36 12.4

38 12.5
 pH Monoprotic Acid Graph
14

12

10

8 Equivalence point

2
Volume of NaOH, mL
0
2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38

a) The first task in constructing the titration curve is to calculate the volume of NaOH
needed to reach the equivalence point, Veq.

CH3COOH(aq) + NaOH(aq) CH3COONa(aq) + H2O(l)

At equivalence point: moles of NaOH = moles of CH3COOH

Mole CH3COOH = Mole NaOH

MaVa = MbVb

where the subscript ‘a’ indicates the acid, CH3COOH, and the subscript ‘b’ indicates the base,
NaOH. The volume of NaOH needed to reach the equivalence point is
MaVa
Vb = 𝑀𝑎

0.1 M X 25.0 mL
= 0.1 𝑀

= 25 mL

b) The pH at equilibrium point is

pH = - log[𝐻+]

9.00 = - log[𝐻+]
[H+] = 1x 10-9

c) Pka of acetic acid = 4.76

So we can find the value of Ka of acetic acid

pKa = - log 𝐾𝑎

4.76 = - log 𝐾𝑎

Ka = 1.74 x 10-5

2. Polyprotic acid (phosphoric acid)

Volume of Ph of the analyte

NaOH(mL)
0 1.3
2 1.97
4 2
6 2.03
8 2.15
10 2.2
12 2.24
14 2.27
16 2.34
18 2.42
20 2.5
22 2.58
24 2.68
26 2.78
28 2.89
30 3.01
32 3.16
34 3.35
36 3.69
38 4.61
40 5.87
42 6.25
44 6.48
46 6.63
 48 6.73
50 6.84
52 6.87
54 7
56 7.1
58 7.18
60 7.29
62 7.39
64 7.49
66 7.59
68 7.7
70 7.84
72 8.01
74 8.22
76 8.66
78 9.2
80 9.93
82 10.72
84 11.04
86 11.27
88 11.44
90 11.55

pH 14
Polyprotic graph
12

10

4 Equivalent point 1

0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 72 74 76 78 80 82 84 86 88 90

Volume of NaOH
The equation of reaction between phosphoric acid and NaOH

H3PO4 + 3NaOH ---> Na3PO4 + 3H2O

If you are doing a titration, there are two end points. The reactions are:

H3PO4 + NaOH ---> NaH2PO4 + H2O

NaH2PO4 + NaOH ---> Na2HPO4 + H2O

The third H+ is not significantly neutralized by NaOH in water because the Kw of water is about
the same as the Ka3 of the H3PO4.

a) The pH at equilibrium point 1 is

pH = - log[𝐻+]

4.90 = - log[𝐻+]

[H+] = 1.25 x 10-5

b) The pH at equilibrium point 2 is

pH = - log[𝐻+]

10.0 = - log[𝐻+]

[H+] = 1.0 x 10-10

c) Pka of acetic acid = 2.16

So we can find the value of Ka of acetic acid

pKa = - log 𝐾𝑎

2.16 = - log 𝐾𝑎

Ka = 6.92 x 10-3

DISCUSSION

In our experiment, we use phenolphthalein indicator that the solution in the equivalent. The
phenolphthalein work when it added in the acid then dropped by base, the color of the solution
became light pink when the equivalent point is reached.
The main reaction in the series of acid-base titrations is neutralization. During neutralization, the
acid and base reacts to form a salt and water (i.e. H+ + OH- H2O). As the all the reactants
are colourless, an appropriate indicator must be added to indicate the colour change at the end
point.
Strong acid-weak base and weak acid-strong base titrations are employed in this experiment
instead of weak acid-weak base titrations as the hydrolysis of a salt of a weak acid-weak base is
incomplete. The hydrolysis of the conjugate base results in an acidic solution and at the same
time, hydrolysis of the conjugate acid of the salt gives rise to a basic solution. Hence, the
resulting solution at equivalence point can be neutral, acidic or basic depending on which
hydrolysis occurs at a greater extent. This means that calculations have to be done preceding the
titration in order to select the appropriate indicators. Therefore, weak acid-weak base titration is
not commonly used to determine the quantitative information of an unknown sample.
While titrating, the conical flask has to be swirled constantly throughout to ensure that the
contents are mixed evenly. Also, some titrant may drip onto the sides of the conical flask and
may not react with the solution in the conical flask. This reduces the accuracy of the results as
extra titrant would be used to achieve the equivalence point. To prevent this, deionised water can
be used to wash down the unreacted titrant when nearing the equivalence point and the conical
flask should be swirled before continuing with the titration. To achieve consistent results, one
important factor is to add in the titrant in a drop wise manner before the equivalence point.

Deionised water was used not only for diluting the sample but also for washing the apparatus,
instead of using tap water. This is because deionized water is pH neutral and will not negatively
affect the results of the acid-base titrations. This is important as acid-base titrations are pH
sensitive reactions.Multiple titrations were carried out until duplicate determinations agree to
within 0.05mL of each other. This ensures that the results are not once-off outliers. By averaging
the two most consistent and accurate results, the probability of incurring random errors was
accounted for and decreased.Other factors that would affect the accuracy of the results include
parallax error when taking the readings and making sure that no air bubbles are present within
the pipette and burette while titrating.

Conclusion

 Ka and Kb are equilibrium constants and a high value signifies a stronger acid or base.

 Acid are proton donors and bases are proton acceptors.

 Monoprotic acid/base corresponds to the donation/acceptance of only one proton.
 Polyprotic acid/base corresponds to the donation/acceptance of more than one proton.

Reference

 James Richard Fromm, Introduction to acid base titration retrieved 26 December 2017
from http://www.3rd1000.com/chem101/chem103r.htm