ANALYSIS OF AN

UNKNOWN VINEGAR
SAMPLE
EXPERIMENT 2
NAME: ANAS BIN MOHD KAMAL (2016655836)

LECTURERS NAME : DR. SUHAILA MOHAMAD HANAPI

PROGRAMME CODE : AS246

COURSE CODE : CHM421

DATE : /03/2017
 ABSTRACT

Vinegar is a common household item containing acetic acid as well as some

other chemicals. This experiment is designed to determine the molar concentration
of acetic acid in a sample of vinegar by titrating it with a standard solution of
NaOH.

CH3COOH(aq) + NaOH(aq) -> CH3COONa(aq) + H2O(l)

By adding the sodium hydroxide, which is a basic solution, to the acetic acid,
which is an acidic solution, a neutralization reaction occurs. An indicator known as
phenolphthalein, is also added to the vinegar. This indicator turns the solution to a
dark pink when excess NaOH is added to make the solution more basic. Thus,
when the solution turns light pink, this indicates that it has successfully been
neutralized. The amount of NaOH used to standardize the vinegar can then be used
to determine the amount of acetic acid in the vinegar as they are both at a 1:1 ratio
as seen in the above equation. Thus, the moles of NaOH used to neutralize the acid
must equal the number of the moles of acetic acid present in the vinegar.

INTRODUCTION

In this experiment, primary standard, standardisation and standard solution is

studied. 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 , in 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 ca 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, KHC 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.
METHOD
A)Preparation of the sodium hydroxide solution.

1. 300 ml of distilled water was measured using measuring cylinder and placed
into the plastic bottle.

2. 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.

3. Next , 100ml of distilled water was added into the plastic bottle , so that the
contents was mixed throughly each time.

4. 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. 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
110c for 2 hours and stored in a desiccator prior to use.

2. 1 g sample above was used as appearance as a guide accurately to weigh two

more sample by difference.

3. 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.

4. 35mLof 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.
 5. 50 mL burette was rinsed using distilled water and was filled with
NaOH stock solution the we had been prepared . Add three drops
phenolpthalein into the conical flask.

6. The conical flask was place under the burette and lower the tip well into it.
Start the titration. The stopcock was control gentlely so the NaOH slowly
flow into the conical flask. The solution was gently swirled and the first
permanent pink colour appear red close the stopcock and the reading was
taken.

7. Repeat all the step three times and the result was recorded.

C) Analysis of the unknwon vinegar sample.

1. 10.0mL vinegar was pipetted into dry pre-weigh 50mL beaker and the beaker
was reweigh back.

2. More vinegar was added into the beaker.10.0mL of vinegar sample

was pipetted from the beaker into the conical flask.

3. Three more same solution was also prepares and the side of each conical
flask was washed using 25mL of distilled water.

4. The pipette was filled with the NaOH stock solution. Three drops of
phenolpthalein was added into each conical flask and the solution was
titrated until it achieve the end point.

5.The titration was repeated for other three solution in the other conical flask.
RESULTS AND CALCULATION
A. Preparation of the sodium hydroxide solution
Volume of NaOH taken from the 50% stock solution = 14.6378 mL

B. Standardisation of the base against potassiumm

hydrogen phthalate

Rough 1

Weight of KHP 1.0036 g 1.0059g

Final reading of NaOH 26.4 mL 26.6 mL

Initial reading of NaOH 0.0 mL 0.0 mL

Volume of NaOH (mL) 26.4 mL 26.6 mL

used

Ratio volume of
NaOH/weight of KHP

C. Analysis of the unknown vinegar sample

Density of vinegar sample = 0.95126 g/mL

Rough 1 2

Volume of
unknown vinegar
(mL)
Final reading of 37.0 mL 32.1 mL 37.2 mL
standard NaOH

Initial reading of 0.0 mL 0.0 mL 0.0 mL

standard NaOH

Volume of 37.0 mL 32.1 mL 37.2 mL

standard NaOH
(mL) used

CALCULATION

The chemical equation is :

KHC8H4O4 (aq)+ NaOH(aq) KNaC8H4O4 (aq) + H2O(l)

The net ionic equation is:

HC8H4O4-1(aq)+ OH-(aq)C8H4O4-2 (aq) + H2O(l)

Molar mass KHP = 204.23 g/mol

There is formula on calculating of KHP :

B. Standardisation of the base against potassium hydrogen phthalate

1)ROUGH

Calculating molarity of KHP

=1.0036 g( 1 mol KHP / 204.23 g)

= 0.005 mol KHP

=(0.005 mol KHP / 35 ml H2O)

=0.000143M(mol/L) KHP
Calculating molarity NaOH

=0.005 mol KHP ( 1 mol NaOH / 1 mol KHP) = 0.005 mol NaOH

=(0.005 mol NaOH / 26.4 mL) = 0.0002 M(mol/L) NaOH

2) Titration 1

Calculating molarity of KHP

=1.0059 g( 1 mol KHP / 204.23 g)

= 0.005 mol KHP

=(0.005 mol KHP / 35 ml H2O)

=0.000143M(mol/L) KHP

Calculating molarity NaOH

=0.005 mol KHP ( 1 mol NaOH / 1 mol KHP) = 0.005 mol NaOH

=(0.005 mol NaOH / 26.6 mL) = 0.0002 M(mol/L) NaOH

C. Analysis of the unknown vinegar sample

DISCUSSION

Vinegar is a solution of acetic acid in water. Acetic acid, CH3COOH, is a

weak monoprotic acid with a molar mass of 60.05 g/mole. The percent by mass of
acetic acid in vinegar can be determined by titrating a known amount of vinegar
with a standardized solution of sodium hydroxide, i.e., a sodium hydroxide
solution of accurately known concentration. Acetic acid and sodium hydroxide
react as shown below:

CH3COOH (aq) + NaOH (aq) CH3COONa (aq) + H2O (l)

60.05 g/mole
 Sodium hydroxide is a hygroscopic solid which means it absorbs water from
the air. A weighed quantity of sodium hydroxide therefore contains an unknown
mass of water. Therefore, a solution of known molarity cannot be made by
dissolving a known mass of solid sodium hydroxide in water. The concentration of
a sodium hydroxide solution must be determined experimentally. This is done by
titrating the sodium hydroxide solution against a primary standard. A primary
standard is a substance from which a solution of known concentration can be
prepared. The primary standard used in this experiment is potassium hydrogen
phthalate, C6H4(COOH)COOK, which is referred to by the shorthand notation of
"KHPh". KHPh has several advantages: it does not absorb moisture readily (i.e., is
not hygroscopic); it is easily dried; it can be accurately weighed; it can be obtained
in very pure form; it has a high molar mass of 204.22 g/mole; and it is very soluble
in water.

KHPh is an acid, which reacts in aqueous solution to neutralize the base, sodium
hydroxide, as shown below:

C6H4(COOH)COOK (aq) + NaOH (aq) C6H4(COONa)COOK (aq) + H2O (l)

204.22 g/mole

One possible error would be 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 buret. 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.

CONCLUSION
The standard solution of sodium hydroxide has been prepared. From the second
experiment the molarity of sodium hydroxide has been determine that is 0.0002
M(mol/L) NaOH. The percentage of acetic acid in the vinegar solution is %.

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

A systematic error means that a constant error is applied to the true weigh of the
object. Mass is determined by the difference between two readings, a systematic
error in the absolute mass on the balance will be removed 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 the titration?

We had been weigh the mass of KHP , which contain the number of moles KHP.
We dissolve the KHP in water in order to do the titration. But water does
not increase or decrease the mass of KHP present. The water also does not play any
role in the reaction.Therefore adding much or less water into the KHP does not
affect the experiment.

REFFERENCES

1. Spencer L.Seager and Michael R.Slabaugh , Safety-Scale Laboratory

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

2. Vickie Williamson and Larry Peck , Experiment in General Chemistry

(Inquiry Skillsand Building), published in 2009 by Cole Cengage
Learning,page:89-90