Name of Experiment: Preparation of Buffer Solution
Date of the experiment was performed: 20 April 2023
Module Code: PHC62104
Aim
To learn to prepare buffers of specific pH by both the direct and indirect methods
Introduction
Weak acids are slightly dissociated in dilute aqueous solutions. Following dissociation, it
produces a small concentration of hydronium ion (H3O+ ) and an equal concentration of the
conjugate base of the acid. This dissociation reaction will always be in equilibria, which can
be utilized to calculate concentrations of the ions present in solution.
𝐻𝐶𝑂𝑂𝐻 + 𝐻2𝑂 ↔ 𝐻3𝑂 + 𝐻𝐶𝑂𝑂− (𝑖𝑛 𝑎𝑞𝑢𝑒𝑜𝑢𝑠 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛) ……Eq 1
Although a weak acid dissociates slightly in water, the soluble salt of a weak acid or base (for
example, sodium formate) is a strong electrolyte and dissociates completely.
𝐻𝐶𝑂𝑂𝑁𝑎 + 𝐻2𝑂 ↔ 𝑁𝑎+ + 𝐻𝐶𝑂𝑂− (𝑖𝑛 𝑎𝑞𝑢𝑒𝑜𝑢𝑠 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛) ……Eq 2
If a salt is added to the solution of weak acid, produces a large amount of formate ion in
comparison to that produced by the acid dissociation. Adding formate ion to the equilibrium of
Eq 1 stresses the system by adding a product. According to Le Châtelier's principle,the
equilibrium will shift to the left (toward reactants) and the concentration of H3O+ will decrease
(and the pH will increase). The suppressed dissociation caused by adding an ion already present
in the solution is called the common ion effect.
One can prepare a solution using a weak acid and its conjugate base (the common ion). The
resulting solution will resist major changes in pH when an acid or base is added to that solution,
which will be called as buffer solution.
Addition of acid stresses the system by adding a product. The equilibrium of Eq 1 shifts toward
the reactants, consuming formate ion and some of the added H3O+ . Result of which will be
reflected by a small decrease in the pH. At the same time, addition of base can cause the
hydronium ion to neutralize the base. This stresses the system by removing a product. Some
formic acid dissociates to replace the H3O+ and the equilibrium of Eq 1 shifts toward the
products. Result of which will be reflected by a small increase in the pH.
It is important to mention that the quantity of additional base or acid can be added to the buffer
to exhaust its buffering capacity depends on the concentration of acid and its conjugated base
in the buffer. This capacity of the buffer is known as buffer capacity, and is defined as the
moles of acid or base necessary to change the pH of one liter of solution by one unit.
Conventionally, the buffer capacity is expressed as the amount of strong acid or base, in gram
equivalents, that must be added to 1 liter of the solution to change its pH by one unit.
𝐵𝑢𝑓𝑓𝑒𝑟 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = (𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑂𝐻− 𝑜𝑟 𝐻3𝑂 + 𝑎𝑑𝑑𝑒𝑑) /(𝑝𝐻 𝑐ℎ𝑎𝑛𝑔𝑒)(𝑣𝑜𝑙𝑢𝑚𝑒
𝑜𝑓 𝑏𝑢𝑓𝑓𝑒𝑟 𝑖𝑛 𝐿) ……Eq 3
The preceding discussion will also apply if a buffer is prepared using a weak base and its
conjugate acid. However, buffers cannot be made with strong acids or strong bases and their
conjugates. No buffer capacity exists in such solutions because there is no equilibrium;
everything has completely dissociated into ions.
The pH of a buffer solution may be calculated with the Henderson-Hasselbalch equation:
𝑝𝐻 = 𝑝𝐾 + 𝑙𝑜𝑔 [𝑏𝑎𝑠𝑒]/ [𝑎𝑐𝑖𝑑] Or 𝑝𝐻 = 𝑝𝐾 + 𝑙𝑜𝑔 [𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑏𝑎𝑠𝑒]/ [𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑎𝑐𝑖𝑑] ……Eq
4
It is clear that the concentration of either acid or base or the number of moles of each could be
determined from the Eq 4 if we know the alternate. The Henderson-Hasselbalch equation also
depicts that the pH of a buffer is closed to the pKa of the weak acid from which it is made.
Buffer of a specific pH should be selected based on the pKa value.
In this practical, buffer solutions need to be prepared by the direct method, measure and adjust
the pH of the solution. In this process, desired base to acid ratio will be obtained by addition
of the conjugate acid and base in solution. Preparation of buffer using indirect method should
also be used for the second experiment, and finally pH of the solution will be measured and
adjusted the pH of each solution. In this process, a strong base will be added to the weak acid
OR strong acid will be added to the conjugate weak base.
Procedure:
Experiment part A: Preparation of 100.0 mL 0.1 M sodium phosphate buffer (pH 7.4)
using the direct method.
1. Sodium phosphate monobasic and dibasic salts were weighed accurately using an
electronic balance.
The weight of Sodium phosphate monobasic and dibasic salts obtained from:
The molar mass of sodium phosphate monobasic, NaH2PO4=120gmol-1
0.1M x 0.1L=0.01mol
Mass=0.01 x 120gmol-1
The mass of sodium phosphate monobasic, NaH2PO4 required 1.2g
The molar mass of sodium phosphate dibasic, Na2HPO4=142gmol-1
0.1M x 0.1L=0.01mol
Mass=0.01 x 142gmol-1
The mass of sodium phosphate monobasic, Na2HPO4 required 1.42g
2. Sodium phosphate monobasic and dibasic salts are separately dissolved in the breaker
and the volume was made in volumetric flasks.
3. The pH of this solution was measured and recorded. It was ensured that the electrode
bulb of the pH metre was fully immersed before measuring the pH of the solution.
4. The required proportion of the solutions prepared with two sodium phosphate salts was
mixed to obtain pH 7.4.
5. By using a stirring rod, the solution was stirred. The pH of the solution was measured
and recorded.
6. If the pH differed from the target pH, it was adjusted by adding 1.0 M HCl or 1.0 M
NaOH dropwise until the desired pH was achieved. In the notebook, the action to adjust
the pH of the buffer was described.
a. Experiment A
Table 1: To represent observed pH change during preparation of 100.0 mL 0.1 M sodium
phosphate buffer
Observed Ph
Initial pH of sodium Initial pH of sodium pH after addition of Final pH
phosphate phosphate dibasic required proportion
monobasic solution solution
4.62 9.53 7.59 7.4
b. Experiment B: Preparation of 100.0 mL 0.6 M acetate buffer using indirect method
1. A clean 100 mL beaker was used to prepare 100.0 mL of 0.60 M acetic acid. The pH
of the solution was measured and recorded.
Volume of acetic acid required:
Density of acetic acid= 1.049gml-1
Density= Mass/Volume
Volume= Mass/Density
Volume= 3.603/1.049
Volume of acetic acid required= 3.43mL
3.43mL of acetic acid is required to add distilled water to get 100mL of acetic acid.
2. 30 mL of the 0.60 M acetic acid was taken in another clean 100 mL beaker.
3. The solution was thoroughly mixed after 1 mL of 1.0 M NaOH was added. The pH of
the solution was measured and recorded.
4. In succession, 1.0 M NaOH was added and thoroughly mixed using a glass rod. The
pH was then adjusted to 5.5.
5. The cumulative number of moles of NaOH added was entered.
Table 2: To represent observed pH change during the preparation of 100.0 ml 0.6M acetate
buffer
Solutions Observed pH
Initial 0.60M acetic acid solution 2.50
Addition of 1 ml of 1.0M NaOH 2.98
Addition of 2 ml of 1.0M NaOH 5.26
Addition of 0.5 ml of 1.0M NaOH 5.36
Addition of 0.5 ml of 1.0M NaOH 5.41
Addition of 0.5 ml of 1.0M NaOH 5.50
Final pH 5.50
Experiment B (Calculation of moles of NaOH added)
Total volume of NaOH added
Total volume of 1.0M NaOH added= 1ml + 2 ml + 0.5ml + 0.5ml + 0.5 ml
Total volume of 1.0M NaOH added= 4.5ml
As the experiment NaOH solution provided is 1.0M
Number of mol of NaOH required = Molarity x volume
= 1.0M x (4.5/1000)l
=4.5 x 10-3mol
Experiment C
1. Fill a burette with 1M NaOH for the buffer solution get from experiment A.
2. Drop by drop and stir the buffer solution into the NaOH solution.
3. Verify the pH change.
4. Determine the volume where the pH deviated by one (1) unit from the starting pH.
5. Determine the capacity of the buffer.
6. In a similar manner, fill a burette with 1M HCl for the experiment B buffer solution.
7. Drop by drop, and add the HCl to the buffer solution.
8. Examine the pH change.
9. Determine the volume where the pH deviated by one (1) unit from the starting pH.
10. Determine the capacity of the buffer
Table 3: Determination of buffer capacity
Buffer solution Initial pH Volume of 1M HCl Volume of 1M of
required to change 1 NaOH required to
unit of original pH change 1 unit of
original pH
Phosphate buffer 7.4 1.2 1.2
Acetate buffer 5.5 7.5 10.8
Discussion
A buffer solution is one which resists changes in pH when small quantities of an acid
or an alkali are added to it. In experiment A, we prepared an acidic buffer solution since it is
made from a weak acid which is acetic acid (CH3COOH) with its salt sodium Acetate
(CH3COONa). Acetic acid is a weak acid, and the position of this equilibrium will be well to
the left: CH3CO2H + H2O ↔CH3CO2- + H2O. Adding sodium acetate to this adds lots of extra
acetate ions. The solution consists of lots of un-ionized acetate acid, lots of ethanoate ions from
the sodium acetate, and enough hydrogen ions to make the solution acidic.
An acid-base reaction is what gives a solution a buffered quality. The conjugate base
of the acid is created when the acid transfers a proton, H+, to the base as well as the base's
conjugate acid (Khan Academy, 2016). Common terminology for the process is a neutralization
reaction. The equilibrium between an acid and its corresponding conjugate base determines the
pH of a buffer solution. In a buffer solution, the concentration of the conjugate base of the acid
is about similar. As a result, the reaction happens when an acid or base is added to the buffer,
but the buffer shows resistance to a significant pH change.
The conjugate acid is created when an acid is added to a buffer solution through a
reaction with the base already present in the buffer. A modest increase in the concentration of
H+ ions in the buffer solution will result from this reaction. The pH level of the buffer solution
will slightly decrease as a result of the increase in H+ ion concentration. When a base is added
to a buffer solution, the base reacts with the acid to create a conjugate base. The concentration
of OH ions in the buffer solution slightly increases as a result of this reaction. The buffer
solution's pH will only slightly rise as a result of the addition of OH ions.
From this practical, we can get buffer capacity from experiment C
Buffer capacity of phosphate buffer exposed Buffer capacity of acetic buffer exposed to
to 1.0ml OF NaOH 1.0ml of NaOH
Number of moles of NaOH used: Number of moles of NaOH used:
Number of mol = molarity x volume Number of mol=molarity x volume
= 1.0M x (1.2/1000) = 1.0M x (10.8/1000)
= 0.0012mol = 0.0108mol
Buffer capacity of phosphate buffer exposed Buffer capacity of phosphate buffer exposed
to 1.0M of NaOH to 1.0M of NaOH
Buffer capacity = 0.0012mol/1 Buffer capacity = 0.0108mol/1
= 0.0012 = 0.0108
Buffer capacity of phosphate buffer exposed Buffer capacity of acetic buffer exposed to
to 1.0ml of HCl 1.0ml OF HCl,
Number of moles of HCl used: Number of moles of HCl used:
Number of mol = molarity x volume Number of mol = molarity x volume
= 1.0M x (1.2/1000) = 1.0M x (7.5/1000)
= 0.0012mol = 0.0075mol
Buffer capacity of phosphate buffer exposed Buffer capacity of phosphate buffer exposed
to 1.0M of HCl to 1.0M of HCl
Buffer capacity = 0.0012mol/1 Buffer capacity = 0.0075mol/1
= 0.0012 = 0.0075
Conclusion
A buffer solution's pH is maintained by the acid and base reacting when an acid or base is
added. Although the buffer solution's pH does slightly change when an acid or base is added,
the system is resistant to significant pH changes because the acid and its conjugate base are in
equilibrium.
References
1. Clugston, Michael & Rosalind Flemming. Advanced Chemistry. OUP Oxford, 2000.
Print.
2. Farrell, Shawn & Lynn Taylor. Experiments in Biochemistry: A Hands on Approach.
Boston, MA: Cengage Learning. 2005. Print.
3. Sawhney, S. K. &Randir Singh. Introductory Practical Chemistry. New Delhi:
Nairosa Publishing House, 2000. Print.