EXPERIMENT NUMBER : 2

TITLE : ANALYSIS OF AN UNKNOWN VINEGAR SAMPLE

NAME : MUHAMAD ARFAN ADIB BIN MOHD AZRAN

ID NUMBER : 2022470852

CLASS : AS2451M3

SUBJECT : CHM 421

LECTURER NAME : DR. MOHD AZRI BIN AB RANI

OBJECTIVE:
1.To prepare the sodium hydroxide solution.
2.To standardise the base against potassium hydrogen phthalate.
3.To analyse the unknown vinegar sample.

INTRODUCTION:
Standard solution is a solution whose solute concentration is accurately known. A solute
which can be obtained in a very pure, stable, weighable form is called a primary standard.
An accurately weighed primary standard is dissolved in desired solvent and diluted to an
accurately known final volume in volumetric flask.
Sodium hydroxide is not a primary standard because it is hygroscopic; meaning that it
absorbs moisture rapidly when exposed to air. Thus, its accurate concentration can only be
determined by standardising the solution agains a very pure potassium hydrogen phthalate
in a series of replicate titrations. This process is called standardisation.
Standardisation can be achieved by titrating the prepared solution against a measured mass
of a suitable primary standard substance or another reliably known secondary standard
solution or by direct analysis for the reagent of interest by some suitable non-volumetric
method such as spectroscopic analysis.

PROCEDURE:
A. Preparation of the sodium hydroxide solution
1. The rough density of the prepared 50% NaOH has been determined by measuring
the mass of 10 mL solution.
A dry and empty 50mL beaker was weighed.
10mL of NaOH solution was measured in a cylinder and has been transferred to the
pre-weighed beaker. Reweighed the beaker.
The difference in weight of 10 mL 50% NaOH prepared in this laboratory.
The density of prepared 50% NaOH, has been used to calculate the volume of stock
solution required to prepare 600 ml of approximately 0.25 M sodium hydroxide
solution.
2. About 300 ml of distilled water was placed into a clean plastic bottle.
A dropper has been used to measure into a graduated cylinder, the calculated
volume of the stock NaOH solution required. The contents of the cylinder has bees
pour carefully into the partially filled plastic bottle.
Cylinder has been rinsed out a few times with fresh distilled water and add all rinsed
into the contents of the plastic bottle.
The cap has been screwed on the plastic bottle and the contents was mixed
thoroughly by carefully and vigorously inverting the bottle and swirling it repeatedly.
 Finally, the remaining volume of water was added in three 100 ml batches, mixing
the contents in the bottle thoroughly each time.
The bottle should be shaken at least 20 times after the last addition.

B. Standardisation of the base against potassium hydrogen phthalate.

1. 1g sample of dry primary-standard grade potassium hydrogen phthalate (KHP) was
weighed accurately on to a weighing boat.
The KHP has been dried earlier, in an oven at 110°C for 2 hours and stored in a
desiccator prior to use.
2. The appearance of the above 1g sample has been used as a guide to weighed
accurately two more such samples by difference.
Each sample has been transferred quantitatively from the weighing boat into a 250
ml conical flask.
Make sure all the sample has been transferred by rinsing the boat with a small
amount of water from wash bottle. Then 35 ml of water has been added to each
flask and swirl the flask gently until all the solids dissolve.
Any drops of sample solution has been rinsed on the side walls of the flask with
distilled water.

3. A 50 ml burette has been rinsed and filled with NaOH solution that to standardise.
Be very careful with air bubbles especially at the tip of the burette.
The stopcock has been turned quickly 360° a few times until all bubbles are
removed.
Then, the initial volume has been adjusted.
The actual starting volume has been read and recorded to the nearest 0.02 ml. Any
adhering solution has been wiped at the sides and the tip of the burette with the
laboratory tissue before beginning the titration.
4. Three drops of phenolphthalein indicator were put into the first conical flask. The
flask was placed under the burette and lower the burette tip well into it. A piece of a
white tile was placed under the flask, control the stopcock of the burette with left
hand and start the titration by carefully turning the stopcock to let a gentle and
steady stream of titrant flow into the acid solution.
The solution in the flask was swirl gently.
The base can be added rapidly at first but concentrate on the colour change.
Initially the pink colour disappears as soon as it is formed but with time, this
colour begins to linger as swirl the flask.
The first permanent faint pink colour that persist for at least 20 second is the end
point.
RESULT AND CALCULATION:
A. Preparation of the sodium hydroxide solution

Mass beaker = 29.9586g

Mass cylinder = 36.1157 g

Mass cylinder + NaOH = 50.1614 g

Mass NaOH = 50.1614 – 36.1157

= 14.0457g
Density NaOH = 14.0457/10
= 1.4046g/ml
Volume, NaOH = 100/1.4046
= 71.2 ml = 0.07 L

Mole NaOH =
= 1.25 mol
Molarity = 1.25/0.0712
= 17.56 mol/L
M1V1 = M2V2

17.56(V1) =0.25 (500)

V1 = 7.192mL

Volume of NaOH taken from the 50% stock solution = 7.192 mL

 B. Standardisation of the base against potassium hydrogen phthalate

1 2 3
Weight of KHP (g) 1.003 1.005 1.003

Final reading of NaOH 25.5 27.0 24.7

(ml)

Initial reading of NaOH 0 0 0

(ml)

Volume of NaOH (ml) 25.5 27.0 24.7

used

Ratio volume of 25.42 26.87 24.63

NaOH/weight of KHP
(ml/g)
DISCUSSION:

In this experiment, the sodium hydroxide solution has been prepared by diluting a
laboratory prepared stock solution of approximately 50% (w/w) NaOH. The density of the
commercially prepared stock solution is 1.525 g/ml. From this information, the volume of
NaOH taken from the 50% stock solution can be calculated for prepare 500 ml of
approximately 0.25 M sodium hydroxide solution. For prepared 500ml of approximately
0.25 M sodium hydroxide we used about 7.192 ml of volume of NaOH taken from the 50%
stock solution.
In next part, the standardisation of base against potassium hydrogen phthalate has been
done in this experiment. The prepared sodium hydroxide solution was standardized against
the primary standard, potassium hydrogen phthalate (KHP). We also adopt a weighing
technique called weighing by difference. This technique is a very important technique to
learn and used because it eliminates systematic errors from the balance. Titration technique
has been done by titrate NaOH solution into three conical flasks containing 1g sample KHP
that has been dissolved in 35ml water and 3 drops of phenolphthalein indicator. The
titration was carried out until get permanent faint pink colour. All the result has been
recorded.
Before the titration, removed the air bubbles before adjusting the initial volume. We also
make sure that eyes must be perpendicular to the reading scale of burette to avoid parallax
error.

CONCLUSION:
In conclusion, the preparation of sodium hydroxide solution has been prepared by using 7ml
of volume of NaOH taken from the 50% stock solution. The standardisation of the base
against potassium hydrogen phthalate has been done by titrate KHP solution with prepared
NaOH solution.

REFERENCE:
https://www.coursehero.com/file/23076915/CHM421-2
QUESTION:

1. Explain how weighing by difference eliminates systematic balance errors.

Weighing by difference is the most accurate method to measure quantitatively the

mass of a solid sample. This procedure involves repetitive weighing of a weighing
bottle containing a quantity of solid reagent

2. Why does it not matter how much water you add when dissolving the acid (KHP) or
when carrying out the titration?

Adding water does not affect the results, since we are measuring the amount of acid
in solution, not the amount of water present.