FACULTY OF RESOURCE SCIENCE AND TECHNOLOGY

DEPARTMENT OF CHEMISTRY

STK1211 - PRACTICAL ANALYTICAL CHEMISTRY

EXPERIMENT NO: 1

TITLE OF EXPERIMENT: ACID AND BASE TITRATION

DATE OF EXPERIMENT : MARCH 7 2017

GROUP MEMBERS & MATRIC NUMBER : 1. DARVINDRAN A/L THEIVINDRAN 55786

2. SUSAN SANI ANAK USIT 59210
3. MARYLIN ANAK MIGA 58698
4. ALEXANDER ADAM SU 59518
5. SHAHIDATUL AMIRAH BINTI
MHD SAID 59165

LAB FACILITATOR :

REPORT DUE DATE : MARCH 14 2017

1. SUMMARY
This report represent the titration experiment of weak acid and strong base. Titration is a common
technique used in many laboratory experiment. The experiment require two main chemical solution
called the titrant, and the analyte. The titrant usually has a known volume and concentration, whereas,
analyte has known volume but unknown concentration. Besides that, the titrant is placed inside the burette
and analyte is placed inside Elenmeyer flask. During the experiment, the titrant is titrated slowly towards
analyte and clamps on the retort stand until their reaction have reached end point. Titration involves the
principle of high equilibrium and rapid reaction. This means by each addition of the titrant must be
consumed completely and rapidly by analyte until analyte is used up. This is also called the end point.
The equivalent point however, means that the amount of titrants are the same as the analyte, which is the
main result of the experiment.
The experiment is carried out using sodium hydroxide (NaOH) solution as a stock solution and a
titrant. Whereas, potassium hydrogen phtalate (KHP) and vinegar are used as analytes for separated
experiments. Besides that, each solution is diluted with distilled water and the analytes is added with an
indicator. The indicator use must be specific to determine the end point of the reaction accurately since
the transition range of different indicators have different. As for the experiment, phenolphthalein is the
most suitable. Phenolphthalein has a transition range from pH 8.0 to 10.0, where it is colourless when in
acidic solution and red in basic solution. The equivalent point of the titrant and the analytes fall upon the
transition range.
The main objectives of the experiment is to demonstrate the basic laboratory techniques of
titration. Besides that, to calculate the molarity based on each titration. Finally, to study the equivalent
point of the titration.
2. OBJECTIVES
A. To demonstrate the basic laboratory techniques of titration
B. To learn to calculate molarity based on titrations
C. To study the equivalent point between the titrant and analyte
D. To demonstrate the technique of preparing the stock solution
E.

3. PROCEDURES

PART A: Preparation of the sodium hydroxide solution

1. A 1L volumetric flask and stopper were cleaned and rinsed. The flash was labelled Approx.
0.1M NaOH. About 500mL of distilled water was put into the flask.
2. Approximately 2.0 g of sodium hydroxide pellets were weighed out and transferred to the 1L
flask. The flask was stoppered and shaken to dissolve the sodium hydroxide.
3. Additional distilled water was added until the mark on the neck of the flask when all the sodium
hydroxide pellets have dissolved. The flask was stoppered and shaken thoroughly to mix.

PART B: Standardization of the sodium hydroxide solution

 1. The burette was set up in the burette clamp. The burette was rinsed and filled with the sodium
hydroxide solution that was prepared.
2. Three 250 mL Erlenmeyer flasks were cleaned with water and the rinsed with distilled water. The
flasks were labelled as 1,2 and 3.
3. The bottle of dried KHP was removed from the oven. When the KHP was completely cooled,
three samples of KHP between 0.6 and 0.8g were weighed, one for each the Erlenmeyer flasks.
The exact weight of each KHP sample was recorded to the nearest mg.
4. 100 mL of distilled water was added to the KHP sample. 1-2 drops of phenolphthalein indicator
solution was added. The KHP sample was swirled to dissolve completely.
5. The initial reading of the NaOH solution in the burette was recorded to the nearest 0.02mL.
6. NaOH solution was added from the burette to the the sample in the Erlenmeyer flask and swirled
constantly during the addition.
7. NaOH was added one drop at a time when the titration approaches the endpoint with constant
swirling until one drop of NaOH caused a permanent pale pink colour that does not fade on
swirling. The reading of the burette to the nearest 0.02 mL was recorded.
8. Steps 4-7 was repeated with other 2 KHP samples.
9. The molecular mass of KHP is 204.2, the number of moles of KHP in samples 1,2 and 3 was
calculated.
10. The molar concentration (M) of NaOH in the titrant solution was calculated from the number of
moles of KHP present in each sample and the volume of NaOH solution used to titrate the
sample. The reaction between NaOH and KHP was of 1:1 stoichiometry.

PART C: Analysis of vinegar solution

Vinegar is a dilute solution of acetic acid and can be effectively titrated with NaOH using the the
phenolphthalein endpoint.

1. Three Erlenmeyer flasks were cleaned and labelled as sample 1,2 and 3.
2. The 5 mL pipette was rinsed with small portions of the vinegar solution and the rinsings were
discarded.
3. 5 mL of the vinegar solution was pipetted into each of the Erlenmeyer flasks. About 100 mL of
distilled water and 2-3 drops of phenolphthalein indicator solution were added to each flask.
4. The burette was refilled with NaOH solution and the initial reading of the burette was recorded to
the nearest 0.02 mL. Sample 1 of vinegar was titrated in the same manner as in the
standardization until one drop of NaOH causes the appearance of the pink colour.
5. The final reading of the burette was recorded to the nearest 0.02 mL.
6. The titration for the other two vinegar samples were repeated.
7. The molar concentration of the vinegar solution was calculated based on the volume of vinegar
sample taken and on the volume and average concentration of NaOH titrant used.
8. The percent by mass of acetic acid in the vinegar solution was calculated given the formula mass
of acetic acid is 60.0 and the density of the vinegar solution is 1.01 g/mL.
4. RESULTS

PART A

Particulars Trial 1 Trial 2 Trial 3

Mass of KHP taken (g) 0.615 0.645 0.676

Final burette reading (mL) 34.5 36.9 39.3

Initial burette reading (mL) 50.00 50.00 50.00

Volume of NaOH used (mL) 15.5 13.1 10.7

Molarity of NaOH solution

Average molarity of NaOH solution

PART B

Particulars Trial 1 Trial 2 Trial 3

Volume of vinegar solution used

Final burette reading

Initial burette reading

Volume of NaOH used

Molarity of NaOH solution

Molarity of vinegar solution

% mass of acetic acid in vinegar

Average molarity of vinegar solution

Average % mass of acetic acid in vinegar

5. CALCULATION
6. DISCUSSION

Molar concentration, also known as molarity, is one of the fundamental ways of expressing
solution concentration. The molar concentration of a solution is the number of species that is contained in
1 litre of the solution. A commonly used unit for molar concentration in chemistry is the molar (unit
symbol: M), which is defined as the number of moles per litre (unit symbol: mol/L).

The concentration of a basic solution is determined, one way, by titrating it with a known volume
of a standard acid solution of known concentration required to neutralize it. The equivalence point in a
titration is a theoretical point reached when the amount of added titrant is chemically equivalent to the
amount of analyte in the sample. In other words, it is the point in a titration when the amount of added
standard reagent is equivalent to the amount of analyte (Skoog et al). The amount of reactants mixed at
the equivalence point depends on the stoichiometry of the reaction.

Standardization is the process of determining the exact concentration (molarity) of a solution.

Titration is one type of analytical procedure often used in standardization. Titration methods, often called
titrimetric methods, include a large and powerful group of quantitative procedures based on measuring the
amount of a reagent of known concentration that is consumed by an analyte in a chemical reaction. These
can determine either the concentration of a solution of unknown molarity or the number of moles of a
substance in a given sample. These are used for this purpose, and the reactions must be fast, complete,
and have a determinable end point. Reactions of strong acids and bases meet these criteria generally, and
acid-base titrations are among the most important examples of this method.

In most titrations, there are no obvious indication that the equivalence point has been reached.
Instead, titrant is stopped being added when an end point is reached. Often this end point is indicated by
an observable physical change, for example, in the color of a substance, added to the solution containing
the analyte. Such substances are known as indicators.

In part A, the sodium hydroxide, NaOH solution was added with distilled water. To ensure that
the NaOH pellets dissolved completely, the flask was shaken thoroughly. Some chemicals can be
purchased in a pure form and remain pure over a long period of time. However, NaOH is a deliquescent
solid, where it possesses a strong affinity for moisture and will absorb relatively large amounts of water
from the atmosphere if exposed to it, forming an aqueous solution, thus it is easily contaminated. If NaOH
solution is prepared by weighing NaOH, the concentration of the solution may not be precisely the
intended concentration.

On the other hand, KHP has a lesser tendency to absorb water from the air and when dried will
remain dry for a reasonable period of time. KHP may be purchased in pure form at reasonable cost, which
means it is a primary standard. Hence, carefully prepared solutions of known concentration of KHP may
be used to determine, by titration, the concentration of another solution such as NaOH. KHP, a large
compound (KHC8H4O4) having a molecular mass of 204.2 g/mol, served as the primary standard. It is a
monoprotic acid and reacts with NaOH in a simple 1 to 1 relationship according to the following
equation:
 NaOH(aq) + KHC8H4O4(aq) ---> KNaC8H4O4(aq) + H2O(l)

In part B, the standardization of the NaOH solution was conducted by using titration. KHP
solution was prepared by adding distilled water to KHP. Since KHP needs to dissolve completely, so the
Erlenmeyer flask was swirled thoroughly. The mass of KHP that we weighed for three of the trials are
0.615 g for the first trial, 0.645 g for the second trial, and 0.676 g for the third trial, respectively. For the
first trial, the volume of NaOH used is 34.50 mL, for the second trial is 36.90 mL and for the third trial is
39.30 mL. The molalities of NaOH solution are 0.087M in the first trial, 0.087M in the second trial and
0.083M in the third trial. So, the molality of NaOH is 0.086M. The reaction between NaOH and KHP is
of 1:1 stoichiometry. NaOH is a strong base while KHP is a weak acid. NaOH will dissociate completely
in water to form a Na+ ion and OH- ion. Meanwhile, KHP will dissociate partially in water to form a low
concentration of H+ ion. The equation for the reaction of potassium hydrogen phthalate with sodium
hydroxide is:

KCO2C6H4CO2H + NaOH KCO2C6H4CO2Na + H2O

Using an indicator, such as phenolphthalein, determines when neutralization occurs.

Phenolphthalein (C20H14O4) is an indicator which undergoes a distinct color change at or near the
equivalence point. It changes its color to light pink at pH range 8.2-10.0. The point at which the indicator
changes color and the titration is stopped is called the endpoint. Ideally, the endpoint should match with
the equivalence point. Phenolphthalein is colorless in acidic solution and reddish violet in basic solution.

In part C, a vinegar solution was analysed. Vinegar solution is a weak acid and it contains acetic
acid. Hence, when reacted with NaOH which is a strong base, it will produce a basic solution. NaOH will
ionise completely in the water to form high concentration of OH- ion. Meanwhile, acetic acid is a weak
acid. It will dissociate partially in the water to form low concentration of H+ ions. 1 mole of NaOH
supplies 1 mol of OH- ion while 1 mole of CH3COOH supplies 1 mol of H3O+ ion. The overall reaction
shows that 1 mole of NaOH reacts with 1 mole of CH3COOH to form 1 mole of CH3COONa and 1 mole
of H2O. This experiment involves the reaction between strong base and weak acid.

a+ + OH-
Half equation: NaOH N
3O+ + CH3COO-
CH3COOH + H2O H

Overall equation: NaOH (aq) + CH3COOH (aq) CH3COONa (aq) + H2O (l)

The volume of vinegar solution that we used in this experiment is 5.00 mL for the three trials.
The volume of NaOH used are 37.00 mL for the first trial, 37.60 mL for the second trial and 38.00 mL for
the third trial. Since the molarity of the NaOH solution is 0.1 M, the molarity of vinegar are 0.64 M, 0.64
M and 0.68M respectively. The average molarity of acetic acid and the density of the vinegar solution
were then used to calculate the mass percent concentration of acetic acid in the vinegar. The percentage
mass of acetic acid in vinegar are 4.40% in the first trial, 4.47% in the second trial and 4.51% in the third
trial. So, the average percentage mass of the acetic acid in vinegar is 4.46%.

Impractically, sometimes a very small difference occurs, this shows the titrations error. The
indicator and the experimental conditions should be selected so that the difference between the visible
point and the theoretical point is so small as possible. Accuracy will indicates the closeness of the
measurement to its true or accepted value and expressed by the error. The term error refers to the absolute
value of the numerical difference between the known value and the experimental value. The closer the
percent error is to zero, then the more accurate your experimental value, which means the more closely
the experimental value agrees with the known value. Precision is obtained through measurement of
replicate samples. In the experiments, three trials were done each for both experiment B and experiment C
titration.

However, naturally, in every experiment, there might be a small error done. This might be either
due to systemic error or random error. In the experiment, some error such as difference in the rate of
swirling between each trial, and error while weighing the KHP on electronic balance will affect the
expected result. Another error is when recording an incorrect initial volume of NaOH solution, such as
recording the initial volume as 0.00 mL if the level of solution was actually higher than the 0.00 mL on
the burret. The excess NaOH solution above the 0.00 mL mark would result in more NaOH solution
delivered than is actually recorded based on the endpoint. Because an incorrectly low volume of NaOH
delivered will be recorded, the resulting calculated molar concentration of acetic acid will be incorrectly
low as well. Thus, correct technique is essential for obtaining good data and accurate and precise results
in this experiment.
7. CONCLUSION

8. POST LAB
9. REFERENCES

A.