FACULTY OF ENGINEERING AND BUILD ENVIRONMENT

DEPARTMENT OF CHEMICAL, METALLURGICAL AND

MATERIALS ENGINEERING

PRACTICAL REPORT: DETERMINATION OF THE CONCENTRATION OF

SODIUM HYDROXIDE USING POTASSIUM HYDROGEN PHTHALATE

COURSE: METALLURGY
SUBJECT:CHEMISTRY
CODE: CHE115B
PRESENTED BY: CE LUKWICHI
STUDENT NUMBER: 222441560

ACADEMIC YEAR 2021

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EXPERIMENT 05: DETERMINATION OF THE CONCENTRATION OF SODIUM
HYDROXIDE USING POTASSIUM HYDROGEN PHTHALATE

1. OBJECTIVES

After completing this experiment you should:

1. Know how to calculate required mass for titration process
2. Know how to perform quantitative analysis by titration
3. Know how to use the titration data to determine the concentration of the analyte.

2. INTRODUCTION

Chemical analyses fall into two categories, qualitative and quantitative. Qualitative analysis
which reveals the identity of the different species present in a sample of matter and
quantitative analysis which determines the relative amounts of one or more species in the
sample.
Volumetric analyses are amongst the most useful and accurate quantitative methods of
analysis. In volumetric analysis a reactant of exactly known concentration is reacted with a
measured volume of the sample containing the component to be determined by the
analysis (the analyte). Using the volume of reactant solution required to react completely
with the analyte, the concentration of the analyte in the sample can be determined.
Volumetric analyses are usually performed by a laboratory procedure called a titration.
Titrations are often used for quantitative analyses using acid-base neutralization reactions to
determine the exact concentration of either an acid or a base.
A measured volume of acid (or base) is placed in a receiving flask called an erlenmeyer
flask. A drop or two of indicator is added to the flask before the titration starts. An indicator
is a dye that has one colour in acid solution and another colour in basic solution. A solution of
base (or acid) is then slowly added to the solution in the erlenmeyer flask using a calibrated
glass instrument called a burette. A burette looks like a long glass tube and is marked with

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volumes usually in 0.10 ml increments. A tap called a stopcock at the lower end of the
burette allows small drops to be released into the erlenmeyer flask at a controlled rate.
During an acid-base titration, the analyst adds the solution slowly, watching for any change in
the colour of the indicator which would indicate that the solution has changed from acidic to
basic (or from basic to acidic). Usually this change happens suddenly. When the colour
change is observed, the end-point has been reached. At this time, the addition of solution
from the burette is stopped and the total volume that has been added to the erlenmeyer
(removed from the burette) is recorded and used to calculate the concentration of the analyte
(acid or base).An acid-base neutralisation reaction is a reaction in which an acid and a
base react completely to form water and a salt? An example of such is a reaction is the
reaction between nitric acid and potassium hydroxide:

HNO3(aq) + KOH(aq) ────➢ KNO3(aq) + H2O

Acid + Base ────➢ Salt + Water

According to the Brønsted theory of acids and bases, acids are proton donors while
bases are defined as proton acceptors.

Potassium hydrogen phthalate (also known as KHP) is a stable substance with high
molecular mass. It has the molar mass of 204.22 g mol-1.

The titration of KHP with sodium hydroxide is a neutralization reaction of a weak acid with
strong base. The concentration of an unknown sodium hydroxide solution can be determined
by titrating it against the potassium hydrogen phthalate solution.

C6H4(CO2K)COOH + NaOH → C6H4(CO2K)COONa + H2O

3. REAGENTS

Potassium Hydrogen Phthalate (KHP), Unknown concentration of NaOH solution,

Phenolphthalein indicator

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 4. APPARATUS:

50.00 ml burette, Burette stand, 25.00 ml pipette, Weighing boat, Funnel, Spatula
3 x Erlenmeyer flasks, Pro-pipette

5. PROCEDURE

Determination of the exact concentration of sodium hydroxide solution by titration

using KHP solution.
6.1 PART A: Preparation of KHP standard.

6.1.1 Make sure that the analytical balance is level by checking that the
bubble is in the centre of the level indicator.
6.1.2 Use a brush to clean the pan.
6.1.3 Tare the balance so that a 0.0000 g reading is displayed.
6.1.4 Place your weighing boat on the centre of the pan and close the doors.
Tare the balance the container on the pan again to display 0.0000
reading. This allows the mass of your sample to be read directly.
6.1.5 Remove the weighing boat and add approximate calculated amount of
solute, return the weighing boat to the balance, and record the reading.
Repeat this until the desired mass is attained. Make sure the windows
are closed when taking the reading. Record the mass of the solute to
four decimal places.

Mass of KHP weighed =

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 ……………………………………………………………………

6.1.6 Transfer the solute into the volumetric flask with an aid of funnel. The
use of funnel minimizes the possibility of losing solid during the trans-
fer.
6.1.7 Add distilled water to the volumetric enough to dissolve the solute.
Rinse the funnel thoroughly to collect solute into the flask. Swirl to dis-
solve the solute, and then add water until the solution just reaches the
calibration mark on neck of flask.
6.1.8 Pipette 25.00 cm3 aliquots of the KHP solution into 3 Erlenmeyer
flasks. Add 3-5 drops of indicator and rinse the sides of the flask with
water from the wash bottle.

6.2 PART B: Preparation of a titration burette with NaOH solution.

25.00 mL
standard KHP
solution
Unknown

4 drops
indicator 25.00 mL

6.2.1 Ensure that the burette is clean. Fix the burette into the burette holder,
taking care that it is vertical and stable. Place a beaker underneath the
burette

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 6.2.2 Close the tap, and run some de-ionised water into the top of the bur-
ette. Open the tap, and allow the water to drain out.
6.2.3 Close the tap, and (using the funnel) run some of the sodium hydrox-
ide solution. Open the tap, and allow the reagent to drain through into
the beaker. Repeat three times.
6.2.4 Close the tap, and fill the burette to just above the 0.00 cm 3 mark with
the sodium hydroxide solution. Remove the funnel. Make sure that
there are no air bubbles inside the burette. Slowly open the tap, and al-
low the solution to run down to (or just past) the 0.00 cm 3 mark. Close
the tap.
6.2.5 Close the tap, and fill the burette to just above the 0.00 cm 3 mark with
the sodium hydroxide solution. Remove the funnel. Make sure that
there are no air bubbles inside the burette. Slowly open the tap, and al-
low the solution to run down to (or just past) the 0.00 cm 3 mark. Close
the tap.
6.2.6 Dry the external surface of the tip with the lab paper towel.
6.2.7 Record the initial volume in Table 1 below.

6.3 PART C: Titration of KHP against NaOH to determine the concentration of NaOH.

6.3.1 Open the stopcock of the burette and add some titrant (NaOH) to the
contents of the flask. Swirl the flask gently to mix the solution.
6.3.2 Continue to add titrant to the flask with swirling. As the addition pro-
ceeds, you will see a faint pink colour appear and quickly fade.
6.3.3 When the colour begins to disappear more slowly, slow the addition of
titrant to a dropwise rate.
6.3.4 Rinse the walls of the flask and the tip of the burette with deionized
water from a wash bottle as you approach the endpoint. This ensures
that all of the NaOH delivered from the burette ends up in the reaction
mixture.

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 6.3.5 The endpoint has been reached when the solution turns faint pink. Re-
cord the final reading on the burette to the nearest 0.01 mL in the data
Table 1. To take the reading use paper backing.
6.3.6 Calculate the Endpoint volume = Final volume - Initial volume.

Initial volume = the upper meniscus reading on the burette at the start of the
titration.
Final volume = the lower meniscus reading at the end of the titration.

6.3.7 Fill the burette again with enough solvent and complete titration 2 and
3.

RESULTS

Mass of KHP weighed:

V= 250mL=0.25L M=0.10mol/L
C8H5KO4 Mm=204.1g/mol n=V.M = 0.25L *0.10 mol/L = 0.025mol

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 m = n*Mm = 0.025 mol * 204.1 g/mol = 5.1025

Table 1: Titration of KHP solution with 0.10 M NaOH solution.

Burette reading Titration 1 Titration 2 Titration 3

Initial reading (ml) 0.00 0.12 0.39

Final reading (ml) 24.89 25.27 26.10

End point volume (ml) 24.89 25.15 25.71

VEP=VF-VI

Questions

7.1 Use the mass weighed to calculate the exact concentration of KHP in the
prepared solution.

m = 5.10g Mm = 204.1g/mol n =
M=

7.2 Calculate the average endpoint volume.

24 . 89 + 25 . 15 + 25 . 71

AVERAGE VOLUME =
3
¿
25
.
25
m
L

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7.3 Use the titration data to calculate the EXACT concentration of the NaOH
solution. Show calculations.

C6H4(CO2K)COOH + NaOH → C6H4(CO2K)COONa + H2O

n =c *v
n NaOH = n C6H4(CO2K)COONa
0.1 ¿ 24.85
25
¿
c ¿ 25.4
25

0.994=c*1.0096 C=

7.4 Why is the titration carried out in triplicate?

It is a good idea to carry out titration in triplicate in order to

make sure that the results would not vary that much. This is
done to minimize any errors done when titrating a sample.
When the value of the triplicate are of close values, then we
can get the average of the three and report the average value.

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 7.5 What are the colour intervals for phenolphthalein in an acidic, basic and
neutral solution?

The interval couleur of phenolphthalein in acidic solution in colourless , in basic

solution is light pink and in neutral solution is colourless.

6. REFERENCES

Brown, Le May and Bursten. Chemistry: The Central Science, 12th ed. Page 145 – 148.

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