EXPERIMENT 2 : ANALYSIS OF AN UNKNOWN VINEGAR SAMPLE

Name : NUR HANIS FIRZANAH BINTI RIDZUAN

Student number : 2019295448
Lecturer’s name : SIR MOHD HAFIZ YAAKOB

ABSTRACT
This experiment was carried out to analyze the unknown acetic acid solution in order to further
the experiment. It was important to prepare the sodium hydroxide, NaOH solution. In this
experiment, we had to prepare 1L of approximately 0.25M NaOH by diluting a prepared stock
solution of approximately 50%(w/w) NaOH by mass. This experiment also required to
standardize the NaOH as a base against potassium hydrogen phthalate, KHP. This part of the
experiment exposed us about weighing technique called weighing by difference. It was
important to get accurate weight of KHP. The main part of this experiment was to analyze the
unknown acetic acid solution. This part of the experiment required us to find the density of
vinegar sample first as phenolphthalein indicator was used for titration with standardized NaOH
solution.

OBJECTIVES

1. To prepare the sodium hydroxide solution.

2. To standardise the base against Potassium Hydrogen Phthalate(KHP)
3. To analyse the unknown the vinegar sample.

INTRODUCTION

In this experiment we will learn about primary standard, standardisation and

standard solution. Primary standard is a reagent which are very pure , representative
of the number of moles the substance contains and easily weighed , for example
sodium chloride.Next , the definition standardisation is the condition in which a
standard has been succesfully established.While standard solution is solution of
accurately known concentration prepared from a primary standard that is weighed
accurately and made up to a fixed volume.

Next process is standardization,sodium hydroxide is not primary standard because it is

hydgroscopic.The definition of hygroscopic is material which attract so much water that they will
form solutions.Thus accurate solution can be determined by standardising the solution against a
very pure potassium hydrogen phthalate(KPH). Sodium hydroxide is deliquescent so it is not
possible to prepare a standard solution of sodium hydroxide by weighing NaOH. Its
concentration is then determined by titrating it against a solution of the primary standard, KHP.
Standardization of sodium hydroxide is important to determine the acetic content acid of a
vinegar sample.

Potassium hydrogen phthalate, KHC8H4O4 is a non-hygroscopic, crystalline, solid that

behaves as a monoprotic acid. It is water soluble and available in high purity. Because of its
high purity, we can determine the number of moles of KHP directly from its mass and it is
referred to as a primary standard. We use the primary standard to determine the concentration
of a sodium hydroxide solution.

The acetic acid content of a vinegar may be determined by titrating a vinegar

sample with a solution of sodium hydroxide of known molar concentration .
Phenolphthalein will be used as an indicator because it will be colorless before the
completion of the reaction but pink after the completion. Phenolphthalein, an organic
dye, is colorless in an acid solution and pink in a basic solution. We need to be
prepared to search carefully for a point in the titration at which one drop of the NaOH
solution will cause the solution being titrated to turn from colorless to a barely
discernible pink color. This point is called the end point and indicates the reaction is
complete.

PROCEDURE

A)Preparation of the sodium hydroxide solution.

First, the rough density of the prepared 50% NaOH determined by measuring the mass of 10
mL solution. A dry and empty 50 mL beaker weighed. 10 mL of NaOH solution measured in a
cylinder and transferred to pre-weighed beaker. The beaker reweighed. The difference in weight
gives the weight of 10 mL 50% NaOH prepared in this laboratory. By using density of the
prepared 50% NaOH, the volume of stock solution required to prepare 800 mL of approximately
0.25 M NaOH solution.

500 ml of distilled water was measured using measuring cylinder and placed into the clean
plastic bottle.Placed 10 ml of NaOH stock solution into the plastic bottle.The measuring cylinder
was rinsed using distilled water.Then the solution was added into the plastic bottle.The cap was
screwed and vigorously swirling the plastic bottle repeatedly.Next ,100ml of distilled water was
added into the plastic bottle , so that the contents was mixed throughly each time.Another 100
ml was added into the same bottle and mix. Lastly 100 ml of distilled water also added into the
same plastic bottle.The bottle was shaked more than 20 times after the last addition distilled
water.

B)Standardisation of the base against Potassium Hydrogen Phthalate.

1 g sample of dry primary – standard grade potassium hydrogen phthalate(KPH) was weighed
using analytical balances.KHP had been dried earlier in an oven at 110˚c for 2 hours and stored
in a desiccator prior to use.1 g sample above was used as appearance as a guide accurately to
weigh two more sample by difference.The sample was transferred into weighing boat into 250
mL conical flask .The weighing boat was rinsed and solution was poured into the conical
flask.35mL of water was measured using measuring cylinder and was placed into the conical
flask and the flask was swirled until the solid was dissolved in the liquid.The side wall of conical
flask was rinsed using the distilled water. 50 mL burette was rinsed using distilled water and
was filled with NaOH stock solution the we had been prepared . Add three drops
phenolphthalein into the conical flask.The conical flask was placed under the burette and lower
the tip well into it.Start the titration.The stopcock was control with gentle so the NaOH slowly
flow into the conical flask.The solution was gently swirled and the first permanent pink colour
appeared to stopcock and the reading was taken. All steps repeated three times and the result
was recorded.
C) Analysis of the unknown vinegar sample

10.0mL vinegar was pipetted into dry pre-weigh 50mL beaker and the beaker was reweigh
back.More vinegar was added into the beaker.10.0mL of vinegar sample was pipetted from the
beaker into the conical flask.Three more same solution was also prepares and the side of each
conical flask was washed using 25 mL of distilled water.The pipette was filled with the NaOH
stock solution. Three drops of phenolphthalein was added into each conical flask and the
solution was titrated until it achieve the end point.The titration was repeated for other three
solution into other conical flask.

RESULTS AND CALCULATION

ANALYSIS OF AN UNKNOWN VINEGAR SAMPLE

A)Preparation of the Sodium Hydroxide Solution

Dry empty beaker = 38.8156 g

Beaker with 50% NaOH(10mL) = 52.0337 g
Weight of 10 mL NaOH = 52.0037-38.8156
= 13.2181 g

Rough density = 13.2181/10

= 1.32181 g/mL

Amount of NaOH to fill in bottle;

Conc. 50% = 50 x 1.32181 x 1mol x 1000

100 1L 40 1
= 16.52 M

M1V1 = M2V2
16.52 X V1 = 0.25(800)
V1 = 12.11 mL

Volume of NaOH taken from the 50% stock solution = 12.11 mL

B)Standardisation of the base against Potassium Hydrogen Phthalate

Mol of KHP = 1.00311

 204.23
= 4.912 x 10^-3 mol
≈ 0.005 mol

ROUGH :
From equation :

1 mol KHP : 1 mol NaOH

Molarity of KHP = 0.005 x 1000
35ml H2O 1
= 0.14 M

Molarity of NaOH = 0.005 x 1000

16.6 1
= 0.30 M

TITRATION 1 :

Molarity of KHP = 0.005 x 1000

35ml H2O 1
= 0.14 M

Molarity of NaOH = 0.005 x 1000

18.0 1
= 0.28 M

TITRATION 2 :
Molarity of KHP = 0.005 x 1000
35ml H2O 1
= 0.14 M
Molarity of NaOH = 0.005 x 1000
17.8 1
= 0.28 M

c)Analysis of the Unknown Vinegar Sample

CH3COOH(aq) + NaOH(aq) → CH3COO- Na+(aq) + H2O(l)

Mass of empty beaker = 39.8972 g

Mass of beaker+vinegar = 49.9355 g
Mass of vinegar = 49.9355-39.8972
= 10.0383 g

Density of vinegar = 10.0383/10

=1.00383g/mL

Moles NaOH = 0.005 mol

Molar mass acetic acid=60.02

From chemical equation;

1 mole of NaOH ≡ 1 mol of CH3COOH

0.005 mole of NaOH ≡ 0.005 mole CH3COOH

Mass of acetic acid = mol x molar mass

= 0.005 x (60.02) = 0.3001 g

% w/w = mass of acetic acid(g) x 100

Mass of vinegar(g)

= 0.3001 x100
10.0383
= 2.99%

DISCUSSION
 From the first experiment the preparation sodium hydroxide solution.As we know sodium
hydroxide cannot be used as a primary standard as it really absorbs water and carbon dioxide
from the air.So in order to determine the concentration of the sodium hydroxide solution through
titration we use KHP because it is non hygroscopic which is not react with any of the
components. KHP is an organic acid that is solid thus, easily weighed. In a titration the volume
of a solution added to a reaction is measured using a burette. A burette is a long tube with a
stopcock at one end that can be used to control the flow. Burettes are typically calibrated in
milliliters.

The KHP and NaOH are reacted together until one of the two is completely reacted. That
point is called the endpoint that is neutral. If additional base is added, the solution will then
become basicidic depending on which was added in excess.We cannot visually determine end
point without using the indicator. To determine the endpoint, an indicator is added to the
reaction. An indicator is a chemical that changes colors at a particular pH. When just a tiny
excess of the acid or base is added beyond the completion of the reaction, the indicator
changes color. The amount added from the buret at this point is called the endpoint.In this
experiment we are using phenolpthalein indicator , which the colour change to pink when the
solution is basidic.

The first pink colour appear is the end point.There is the chemical equation for the
experiment :
KHC8H4O4 (aq) + NaOH(aq) KNaC8H4O4 (aq) + H2O(l)

From above chemical equation we know that ; 1 mol of KHC8H4O4 need 1 mol of NaOH
to produce 1 mol KNaC8H4O4 and H2O 0.005 mol of KHC8H4O4 need 0.005 mol of NaOH to
produce 0.005 mol KNaC8H4O4 and H2O

Next the analysis of the vinegar sample. Vinegar is a solution of acetic acid in water.
Acetic acid, CH3COOH, is a weak monoprotic acid. There is the chemical equation : CH3COOH
+ NaOH produced CH3COO- Na+ + H2O

From the above equation we can determine that number of mol of acetic acid by using
stoichiometry . We had been calculated the number of mol of sodium hydroxide from the part b
experiment. 1 mol of CH3COOH need 1 mole of NaOH to produce 1 mole CH3COO- Na+ and
H2O 0.005 mol of CH3COOH need 0.005 mol of NaOH to produce 0.005 mol CH3COONa +
and H2O So by using the number of mol we can get the mass of acetic acid ,that is 0.3001g

There is some precaution in handling experiment.First wear lab coat in all times while
working in the laboratory.Both acids and bases can be corrosive to human tissue.When it
concentrated it can break down the human tissue.As we know sodium hydroxide are very
corrosive and cannot contact directly to our hand, so we can use spatula to handle the
substance.The lab coat can protect our body when handling the chemical. If the acid or bases
get into our eyes , flush it out immediately with lots of water until it the chemical was removed.It
ts the same , when other place part of our body was spilled with chemical , flush the area with
water and the sink or use the safety shower in the lab

CONCLUSION

The standard solution of sodium hydroxide has been prepared. From the experiment the
molarity of sodium hydroxide has been determined that is 0.28M(mol/L) NaOH.The percentage
of acetic acid in the vinegar solution is 2.99%.

REFERENCES

1. Vickie Williamson and Larry Peck , Experiment in General Chemistry (Inquiry Skills and
Building), published in 2009 by Cole Cengage Learning,page:89-90

2. Spencer L.Seager and Michael R.Slabaugh , Safety-Scale Laboratory Experiments for

Chemistry for today,seventh edition, published in 2008 by Cole Cengage
Learning,page:183-188