FACULTY OF APPLIED SCIENCE

CHM421 – ANALYTICAL CHEMSITRY

LABORATORY REPORT

NO OF EXPERIMENT: 2
TITLE OF EXPERIMENT: ANALYSIS OF UNKNOWN VINEGAR
SAMPLE
STUDENT’S NAME: NUR HANNAN NAJIHAH BINTI HAMDHAN
MATRIC NO: 2022478318
CLASS GROUP: AS2352A2

DATE OF EXPERIMENT: 12 APRIL 2023

DATE OF SUBMISSION: 24 MAY 2023
LECTURER’S NAME: DR NURULFAZLINA EDAYAH BINTI
RASOL
OBJECTIVES
1. To prepare the Sodium Hydroxide Solution
2. To standardise the base against Potassium Hydrogen Phthalate
3. To analyse the unknown vinegar sample

INTRODUCTION
From this experiment, we will learn about primary standard, standardisation and standard solution.
Standard solution is a solution whose solute concentration is accurately known. A primary standard
is a solute that can be obtained in a very pure, stable, weighable form. An accurately weighed
primary standard is dissolved in the desired solvent and diluted to an accurately known final
volume in a volumetric flask.
Sodium Hydroxide solution is not a primary solution because it is hygroscopic where it absorb
moisture rapidly when exposed to air. The accurate concentration can only be determined by
standardising the solution against a very pure potassium hydrogen phthalate in a series of replicate
titration. This process is called as standardisation. The standardised sodium hydroxide then used to
determine the acetic acid content of a vinegar sample.
The secondary standard form can be used if the primary standard cannot be obtained. An
approximate concentration of the solution of the reagent is fist prepared and then its true
concentration is determined by standardisation process. Standardisation can be achieved by titrating
the prepared solution against (a) a measures mass of a suitable primary standard substances; (b)
another reliably known secondary solution; or (c) by direct analysis for the reagent of interest by
some suitable non-volumetric method such as spectroscopic analysis. For this experiment. We used
method (a) using potassium hydrogen phthalate as the primary standard to prepare the secondary
standard solution of sodium hydroxide .

PROCEDURE
A. Preparation of the Sodium Hydroxide Solution

1. Firstly, the density of the prepared 50% NaOH was determined by measuring the
mass of 10 ml solution. A dry and empty 50 ml beaker was weighed. 10 ml of the
NaOH solution was measured in a cylinder and transferred to the pre-weighed
beaker. The beaker was reweighed and the difference of the weight gives the weight
of 10 ml 50% NaOH prepared in the laboratory. The volume of the stock solution
required to prepare 600 ml of approximately 0.25 M sodium hydroxide solution was
calculated using the density of the prepared 50% NaOH.
2. About 300 ml of distilled water was placed into a clean plastic bottle. The calculated
volume of the stock NaOH solution required was measure into a graduated cylinder
using a dropper and the content was carefully poured into the partially filled plastic
bottle. The plastic bottle was rinsed. The plastic bottle was swirling to mix the
solution inside it. The remaining volume of water in 3 time 100 ml was added and
the content was mixed each time. The bottle was shaken about 20 times after the last
addition of water.
B. Standardisation of the base against Potassium Hydrogen Phthalate

1. About 1 g sample of dry primary-standard grade potassium hydrogen phthalate

(KHP) was weighed accurately. The KHP has been dried earlier in an oven at 110℃
for 2 hours and stored in a desiccator prior to use.
2. Two more sample of KHP was weighed using the first sample as the guide. Each
sample than transferred into a 250 ml conical flask. The weighing boat then rinsed
with a small amount or water to make sure all the sample has been transferred. 35 ml
of water was then added to each flask and the flask was swirled until the solid was
fully dissolve. The side walls of the conical was rinsed with the distilled water.
3. N A 50 ml burette was rinsed and filled with the NaOH solution that was prepared
in part A. make sure there are no air bubbles trapped in the burette. The initial
volume was recorded.
4. 3 drops of phenolphthalein was dropped into the conical flask and the flask was
placed under the burette. A white tile was placed under the flask. Start the titration
process while swirling the flask until pale pink colour formed.
5. The same steps repeated for the next 2 sample and record its final volume of acid
used.

C. Analysis of the Unknown Vinegar Sample

1. The density of the vinegar sample was determined. 10.0 ml vinegar was pipetted in
to a dry pre-weighed 50 ml beaker. The beaker was reweighed. The difference will
give the weight for 10 ml vinegar sample. More vinegar sample was taken into the
50 ml beaker for titration.
2. 10.0 ml of vinegar sample was pipetted from beaker into a clean 250 ml conical
flask. 2 more same sample was prepared. The sides of each flask was washed with
water from the wash bottle.
3. 3 drops of phenolphthalein indicator was added into each conical flask. The titration
was started using the NaOH solution from part B. The titration was continued until
the permanent pale pink colour solution formed. The steps were repeated for the
next 2 sample. The initial and final volume of NaOH was recorded for every
titration.
RESULT AND CALCULATION
A. PREPARATION OF THE SODIUM HYDROXIDE SOLUTION

50 g 1.525 g 1 mol 1000 ml

Molarity = × × ×
100 g ml 39.99 g 1L
= 19.06 mol/ L
M 1 V 1= M 2 V 2

(19.06)( V 1) = (0.25)(600)
V 1 = 7.9 ml

Volume of NaOH taken from the 50% stock solution = 7.9 ml

B. STANDARDISATION OF THE BASE AGAINST POTASSIUM HYDROGEN

PHTHALATE

Rough 1 2 3
Weight of KHP 1.607 1.0212 1.0932 1.0065

Final reading of NaOH 36.2 35.7 37.3 34.2

Initial reading of NaOH 0.0 0.0 0.0 0.0

Volume of NaOH (ml) used 36.2 35.7 37.3 34.2

Ratio volume of NaOH/ weight of KHP 33.93 34.96 34.12 33.98

KHC 8 H 4 O4 + NaOH → KNaC 8 H 4 O4 + H 2 O

mass ( g)
Mol of KHP=
g
molar mass ( )
mol

1.067
¿
204.1

¿ 0.0052 mol
mol
Molarity of KHP=
volume ( L)
0.0052 mol
¿
0.035 L
= 0.15 M
From equation
1 mol KHP react with 1 mol NaOH
0.0052 mol KHP react with 0.0052 mol NaOH

For sample 1 :
0.0052 mol
Molarity of NaOH =
0.0357
= 0.15 M
For sample 2 :
0.0052
Molarity of NaOH =
0.0373
= 0.14 M
For sample 3 :
0.0052
Molarity of NaOH =
0.0342
= 0.15 M

0.15+0.14+ 0.15
Average molarity =
3
= 0.15 M

C. ANALYSIS OF THE UNKNOWN VINEGAR SAMPLE

Rough 1 2 3
Volume of unknown vinegar ( ml ) 10 10 10 10
Final reading of standard NaOH ( ml) 63.5 51.7 66.5 51.4
Initial reading of standard NaOH (ml) 0.0 0.0 13.5 0.0
Volume of standard NaOH used (ml) 63.5 51.7 53.0 51.4

Weight of beaker + 10 ml vinegar = 42.4147 g

Weight of beaker = 30.0008 g
Weight of 10 ml vinegar = 42.4147 – 30.0008
 = 12.4139 g

mass of vinegar
Density of 1ml vinegar = volume of vinegar
¿
¿
12.4139 g
=
10 ml
= 1.24139 g/ml

Mol of acetic acid = molarity x volume

Sample 1:
Mol acetic acid = 0.15 x 0.0517 L
= 0.00776 mol
Sample 2:
Mol acetic acid = 0.15 x 0.053
= 0.00795 mol
Sample 3:
Mol acetic acid = 0.15 x 0.0514
= 0.00751 mol

0.00776+0.00795+ 0.00751
Average mol of acetic acid =
3
= 0.00774 mol

Mass of acetic acid = mol acetic acid x molar mass acetic acid
= 0.00774 mol x 60.053 g/ml
=0.4648 g

mass solute
% (w/w) acetic acid = × 100
mass sample
0.4648 g
= ×100
12.4139 g
= 3.74 %
DISSCUSSION
The first experiment was to prepare a sodium hydroxide solution. The volume taken from 50%
stock solution that was calculated using the density of NaOH 1.525 g/ml was 7.90 ml. 600 ml
distilled water was added to empty plastic bottle and mixed with the stock solution. Then the
sodium hydroxide solution was prepared.
The second part of the experiment was the standardisation of the base against potassium hydrogen
phthalate. A titration process between diluted NaOH solution from part A and KHP was carried out
as the titrant will be the standard NaOH solution and the analyte is Potassium Hydrogen Phthalate.
The equation of the reaction was KHC 8 H 4 O4 + NaOH → NaKC 8 H 4 O4 . The indicator used in this
experiment was phenolphthalein. The reaction considered as completed if the solution of KHP with
3 drops of indicators turns into permanent pale pink. The result obtained for the first titration is
1.0212 g of KHP and the volume of NaOH used was 35.70 ml. the second titration with 1.0932 g oh
KHP use about 37.30 ml of standard NaOH solution. The last titration resulted that 1.0065 g of
KHP used 34.20 ml of NaOH solution. The ratio volume of NaOH and weight of KHP was 34.96,
34.12 and 33.98 respectively. The average value of molarity calculated using the stoichiometry was
0.15 M
The last part of the experiment was to determine the density of the vinegar sample. Using the same
method as in part B, titration method was used. the density of the vinegar sample calculated is
1.24139 g/ml.

CONCLUSION
The sodium hydroxide solution was prepared by mixing 7.9 ml of NaOH solution with 600 ml of
distilled water. The average molarity of NaOH obtained from the calculation was 0.15 M. the
density of the vinegar sample is 1.24139 g/ml and from this 2 value, the %(w/w) obtained was
3.74 %.

QUESTIONS
1. Explain how weighing by difference eliminates systematics balance error.
= systematic error is an error which in the course of a number of measurement carried out
under the same conditions of a given value and quantity either remains constant in absolute
value and sign. Weighing by difference can eliminate the systematics error by subtracting
the final weight from the initial weight.

2. Why does it not matter how much water you add when dissolving the acid (KHP) or when
carrying out titration ?
 = Because in this experiment, water are used to dissolve the KHP and distilled water does
not affect the outcome of the titration because water is a solvent. Solvent does not react with
other chemical species in the solution.

REFERENCES
1. Behera, B. R. (2012). Modelling the structure of woven fabrics. In Elsevier eBooks (pp.
229–263). https://doi.org/10.1533/9780857095589.2.229

2. Libretexts. (2021). d. Solid Acid Titration. Chemistry LibreTexts.

https://chem.libretexts.org/Courses/University_of_Arkansas_Little_Rock/
Chem_1403%3A_General_Chemistry_2_Lab_(Spring_2021_Hybrid)/6%3A_Acid-
Base_Equilibria_Part_2/d._Solid_Acid_Titration

3. Admin. (2023b). Sodium Hydroxide - Properties, Structure of Sodium Hydroxide,

Reactions, Uses. BYJUS. https://byjus.com/jee/sodium-hydroxide/