UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

ENGINEERING CHEMISTRY LABORATORY I
(CHE485)






Remarks:

Checked by: Rechecked by:


--------------------------- ---------------------------
Date : Date :
No. Title Allocated Marks (%) Marks
1 Abstract/Summary 5
2 Introduction 5
3 Objective/Aims 5
4 Theory 5
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Recommendations 5
11 Conclusion 5
12 Reference / Appendix 5
13 Supervisors grading 10
TOTAL MARKS 100
NAME : MOHAMMAD AMIR HAKIM BIN RUSLI
STUDENT NO. : 2014294432
GROUP : GROUP 4
EXPERIMENT : DETERMINATION OF THE CONCENTRATION OF ACETIC ACID IN
VINEGAR SOLUTION
DATES PERFORM : 3 OCTOBER 2014
SEMESTER : 3
PROGRAMME/ CODE : EH22O
SUBMITT TO : PN. RAFEQAH BINTI RASLAN
TABLE OF CONTENT









i. abstract
ii. Introduction
iii. Aims/ objectives
iv. Theory
v. Apparatus
vi. Procedure
vii. Result & calculation
viii. Sample error calculation
ix. Discussion
x. Conclusion
xi. Recommendation
xii. References
xiii. Appendices
ABSTRACT
The objective of this experiment is to determine the molarity of a solution and the percent by
mass of acetic acid in vinegar by titration with a standardized sodium hydroxide solution. The
first experiment, 250 mL of approximately 0.6M sodium hydroxide was perepared from 3.6
grams NaOH solid in a beaker. Then, measured 1.5 grams of KHP was added into another
beaker and 30 mL of distilled water then was added into the beaker and the solution was stirred
until KHP dissolved completely. The solution then titrated with NaOH solution and pH with
every 1 mL of NaOH solution added was recorded until we reach equivalence point. The steps
were repeated with another two solutions for NaOH standardization. Then, the graph of pH
versus NaOH was plotted to get volume of NaOH required to neutralize KHP solution for each
titration. Molarity of sodium hydroxide for titrations 1, 2 and 3 was calculated. Then, the average
molarity of sodium hydroxidewas calculated. For the second experiment which is determination
of molarity of acetic acid and mass percent in vinegar, firstly, 10.00 mL of vinegar was
transferred into a clean and dry 250 mL beaker by using a 10 mL volumetric pipette. Then, 80
mL of sufficient water was added to cover the pH electrode tip during the titration. Then, 2 mL
of NaOH was added into the vinegar solution and the pH of the solution was recorded. pH
reading was recorded for every NaOH solution added into the solution until we reach the
equivalence point. The steps was repeated twice more. Graph of pH versus NaOH volume added
was plotted to get volume of NaOH required to neutralize the vinegar in each titration. The data
was recorded. Molarity of acetic acid in vinegar, average molarity of acetic acid and percent by
mass of acetic acid in vinegar for titrations 1, 2 and 3 was calculated. The percent by mass also
was calculated. For the first experiment, volume of NaOH solution required to neutralize KHP
solution in titration 1 is 11.9mL while the titration 2 need 11.8mL . For the second experiment,
volume of NaOH solution required to neutralize vinegar solution in titration 1 is 28.5mL while
the other titrations need 29.9mL.The conclusion for this experiment is the objective was
achieved. From the experiment, we get the average molarity of sodium hydroxide is 0.620 M, the
average molarity of acetic acid is 1.8104 M and the average percent by mass of acetic acid is
10.87 % .


INTRODUCTION
Concentration of solution is an amount of solute in a given amount of solvent. In a solution,
the solvent is the major component while the solute is the minor component. A concentrated
solution contains large quantity of solute in a given amount of solvent and vice versa for dilute
solution. There are two specific terms to express concentration, molarity and percent by mass.
Molarity is the number of moles of solute per volume of solution (in L)


( )

Percent by mass is the mass of solute (in g) per 100 grams of solution

( )
( )

Vinegar is dilute solution of acetic acid. The molecular formula for acetic acid is CH
3
COOH.
The molarity and percent by mass of acetic acid in vinegar can be determine by titration. A
titration is a process in which small increments of a solution of known concentration are added to
a specific volume of a solution of unknown concentration until the reaction is attained. Knowing
the quantity of the known solution required to complete a titration enables calculation of the
unknown solution concentration. The purpose of titration is to determine the equivalence point of
the reaction. The equivalence point is reach when the added quantity of one.








OBJECTIVE
To determine the molarity of the solution and percent by mass of acetic acid in vinegar by
titration with a standardized sodium hydroxide solution.

THEORY
A titration mixes two solutions which contain reactants for a known chemical reaction under
conditions such that:
a) the point at which both reactants have been completely consumed by the known
reaction can be detected (end point)
b) the amount of one reactant can be calculated from the known concentration of reactant
in a standard solution, the volume of standard solution used, and the balanced known
chemical equation.

In this experiment, the equivalence point occurs when the moles of acid in the solution equals the
mole of base added in the titration. For example, the stoichiometry amount of 1 mole of the
strong base, sodium hydroxide (NaOH), is necessary to neutralize 1 mole of the weak acid, acetic
acid (CH
3
CO
2
H), as indicated in the Equation 1 :
NaOH
(aq)
+ CH
3
CO
2
H
(aq)
NaCH
3
CO
2(aq)
+ H
2
O
(l)
(Equation 1)
The sudden change in the solution pH shows that the titration has reached the equivalence point.
pH in an aqueous solution is related to its hydrogen ion concentration. Symbolically, the
hydrogen ion concentration is written as [H
3
O
+
]. pH is defined as the negative of the logarithm
of the hydrogen ion concentration.
pH = -log
10
[H
3
O
+
] (Equation 2)
pH scale is a method of expressing the acidity or basicity of a solution. Solution with pH < 7 are
acidic, pH = 7 are neutral, pH > 7 are basic. pH electrode will be use in this experiment. The
titration is initiated by inserting the pH electrode into a beaker containing the acid solution (pH
within 3-5). As sodium hydroxide, NaOH, is incrementally added to the acid solution, some of
the hydrogen ions will be neutralized. As the hydrogen ion concentration decreases, the pH of
the solution will gradually increase. When sufficient NaOH is added to a completely neutralize
the acid (most of the H
3
O
+
ions are removed from the solution), the next drop of NaOH added
will cause a sudden sharp increase in pH. The volume of based required to completely
neutralized the acid is determined at the equivalence point of titration.



In this experiment, titration of the vinegar sample with a standardize sodium hydroxide solution
will be performed. To standardize the sodium hydroxide solution, a primary standard acid
solution is initially prepared. In general, primary standard solutions are produce by dissolving a
weighed quantity of pure acid or base in a known volume of solution. Primary standard acid or
bases have several common characteristics :

Must be available in at least 99.9 purity
Must have a high molar mass to minimize error in weighing
Must be stable upon heating
Must be soluble in the solvent of interest
Most acids and bases are available in primary standard form. To standardize it, titration of
the solution with a primary standard should be performed. In this experiment, NaOH solution
will be titrated with potassium hydrogen phthalate. The reaction equation for this is
:KHC
8
H
4
O
4(aq)
+ NaOH
(aq)
KNaC
8
H
4
O
4(aq)
+ H
2
O
(l)
(Equation 3)
Once the sodium hydroxide solution has been standardized it will be titrated with 10.00mL
aliquots of vinegar. The reaction equation for vinegar with NaOH is :
CH
3
COOH
(aq)
+ NaOH
(aq)
NaCH
3
COO
(aq)
+ H
2
O
(l)
(Equation 4)
Knowing the standardize NaOH concentration and using equation 4, we can determine the
molarity and percent by mass of acetic acid in the vinegar solution.




Equivalence
point
Apparatus & Materials
Beaker , 50-ml burette, magnetic rod, pH meter, conical flask, stirrer, electronic balance, spatula,
retort stand, NaOH solution, vinegar, droppers , stirrer, stir bar, buret clamp, pipet 10mL, Funnel,
analytical balance, potassium hydrogen phthalate (KHP)

PROCEDURE
PART A
1. 250 mL of 0.6 M sodium hydroxide solution was prepared from NaOH solid. The
solution was prepared in a beaker; the calculation was checked by the laboratory
instructor prior to preparing the solution. The calculation was recorded.
2. The beaker was placed on the balance and was tare. 1.5 grams of KHP was added to the
beaker. The mass of KHP was recorded to nearest 0.001 g. 30mL of distilled water was
added to the beaker. The solution was stir until the KHP completely dissolved.
3. The solution was titrated with NaOH and the pH was recorded with 1 mL addition of
NaOH solution.
4. Steps 1 to 3 were repeated and to more solutions was prepared for NaOH
standardization.
5. The graph of pH versus NaOH was plotted. The volume of NaOH required to neutralize
the KHP solution in each titration was determined from the plots.
6. The molarity of NaOH for titrations 1, 2 and 3 was calculated.
7. The average molarity of the sodium hydroxide solution was calculated. The resulting
sodium hydroxide concentration was used in part B of the experiment.
PART B
1. 10.00mL of a vinegar was transferred to a clean, dry 250mL beaker using a 10mL
volumetric pipette. 75 to 100 mL of water was added to cover the pH electrode tip during
the titration.
2. 2 mL of NaOH was added to the vinegar solution and the pH was recorded.
3. The above steps was repeated twice more.
4. The graph of pH versus NaOH volume added was plotted and the volume of NaOH
required to neutralize the vinegar in each titration was determined from the plots. The
data was recorded.
5. The molarity of acetic acid in vinegar for titration 1, 2 and 3 was calculated.
6. The average molarity of acetic acid for each solution was calculated.
7. The percent by mass of acetic acid in vinegar for titrations 1, 2 and 3 was calculated.
8. The percent by mass of acetic acid in vinegar was calculated.
RESULT AND CALCULATION

Titration 1 Titration 2
Mass of beaker (g) 100.69 100.72
Mass of beaker + KHP (g) 102.19 102.22
Mass of KHP 1.5 1.5


a) Volume of NaOH to neutralize KHP
Titration 1
st
2
nd




Volume of NaOH
to neutralize KHP
(ml)
0 4.74 0 4.88
1 4.96 1 5.06
2 5.15 2 5.24
3 5.35 3 5.36
4 5.47 4 5.51
5 5.61 5 5.62
6 5.75 6 5.75
7 5.86 7 5.87
8 6.01 8 6.02
9 6.16 9 6.18
10 6.37 10 6.34
11 6.55 11 6.60
12 7.01 12 7.05
13 12.36 13 12.50
14 12.81 14 12.88
15 12.95 15 13.03
16 13.04 16 13.13








b) Volume of NaOH to Neutralize vinegar








Volume of NaOH
to neutralize
vinegar (ml)
1
st
2
nd

V(ml) pH V(ml) pH
0 3.17 0 3.29
2 3.88 2 4.02
4 4.25 4 4.34
6 4.47 6 4.57
8 4.67 8 4.75
10 4.84 10 4.90
12 4.97 12 5.05
14 5.09 14 5.18
16 5.21 16 5.30
18 5.35 18 5.43
20 5.46 20 5.55
22 5.61 22 5.70
24 5.77 24 5.86
26 5.99 26 6.06
28 6.31 28 6.32
30 7.45 30 7.03
32 12.11 32 12.03
34 12.43 34 12.49
36
12.55
36 12.65












a) Standardization of sodium hydroxide solution
Titration 1
Volume of NaOH (ml) pH
0 4.74
1 4.96
2 5.15
3 5.35
4 5.47
5 5.61
6 5.75
7 5.86
8 6.01
9 6.16
10 6.37
11 6.55
12 7.01
13 12.36
14 12.81
15 12.95
16 13.04


When pH is 7, the volume NaOH is 11.9mL
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
0 2 4 6 8 10 12 14 16 18
p
H

Volume of NaOH (mL)
Titration of KHP with NaOH
Titration 1
Titration 2
Volume of NaOH (ml) pH
0 4.88
1 5.06
2 5.24
3 5.36
4 5.51
5 5.62
6 5.75
7 5.87
8 6.02
9 6.18
10 6.34
11 6.60
12 7.05
13 12.50
14 12.88
15 13.03
16 13.13


When pH is 7, the volume NaOH is 11.8mL

0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
0 2 4 6 8 10 12 14 16 18
p
H

Volume of NaOH (mL)
Titration of KHP with NaOH
Column1
Titration 2
Calculation
1
st
titration
a) Mole KHP :
=



= 7.35x103 mole

b) Mole NaOH required
=



=7.35x103 mole

c) Molarity
=


=



=0.6176 M NaOH
2
nd
titration
a) Mole KHP :
=



= 0.007345 mole KHP

b) Mole NaOH required
=



=0.007345 mole NaOH

c) Molarity
=


=



=0.6224 M NaOH

Average molarity

( )

( )

= 0.620 M



b) Molarity of acetic acid and mass percent in vinegar
Titration 1
Volume of NaOH
(ml)
pH
0 3.17
2 3.88
4 4.25
6 4.47
8 4.67
10 4.84
12 4.97
14 5.09
16 5.21
18 5.35
20 5.46
22 5.61
24 5.77
26 5.99
28 6.31
30 7.45
32 12.11
34 12.45
36 12.55


When pH is 7, the volume of NaOH is 28.5mL
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
0 5 10 15 20 25 30 35 40
p
H

Volume of NaOH (mL)
Titration of Vinegar with NaOH
Titration 1
Titration 2
Volume of NaOH
(ml)
pH
0 3.29
2 4.02
4 4.34
6 4.57
8 4.75
10 4.90
12 5.05
14 5.18
16 5.30
18 5.43
20 5.55
22 5.70
24 5.86
26 6.06
28 6.32
30 7.03
32 12.03
34 12.49
36 12.65


When the pH is 7, the NaOH is 29.9mL

0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
0 5 10 15 20 25 30 35 40
p
H

Volume of NaOH (mL)
Titration of Vinegar with NaOH
Titration 2
Calculation
1
st
titration
a) Moles of NaOH that reacted :



= 0.01767 mol NaOH
b) Molarity of the CHCOOH :

1 mole of NaOH 1 moles of CHCOOH
0.01767 mole of NaOH 0.01767 moles of CHCOOH







CHCOOH

c) Calculate the mass of acetic acid in the solution

d) Percentage by mass of acetic acid in the solution

2
nd
titration
a) Moles of NaOH that reacted :



= 0.018538 mol NaOH
b) Molarity of the CHCOOH :

1 mole of NaOH 1 moles of CHCOOH
0.018538 mole of NaOH 0.018538 moles of CHCOOH







CHCOOH

c) Calculate the mass of acetic acid in the solution

d) Percentage by mass of acetic acid in the solution

Average molarity of acetic acid

( )

= 1.8104 M
Average percentage

( )

( )

= 10.87%












Sample calculation for standardization a base with NaOH
Let, equivalence point =
Mass of KHP = Y grams (g)
moles of KHP (KCH
3
H
4
O
4
) used in the titration
= Y g KHP



= V mol of KHP
Number of sodium hydroxide (NaOH) used
= V

mol KHP





= Z

mol
Volume of solution
= Y mL



=Y L

Molarity of NaOH solution
Molarity ( M ) =
( )
( )

=



= A Molal (M)
Sample calculation for determine the acetic acid concentration in vinegar by titration with
standardized base.
A 40.00 mL aliquot of vinegar requires U mL of A M standardized NaOH solution to reach the
equivalence point of the titration. Calculate the molarity and the percent by mass of acetic acid in
the vinegar solution. Assume the density of the vinegar solution is 1.00 g/mL.


Equivalence point: U mL
Number of moles of NaOH that reacted
= y mL



= y L NaOH
=y L NaOH



= Z mol NaOH
Z mol NaOH react with T mol of CH
3
COOH

Volume of solution
= 10.0 mL



= 0.01 L
Molarity of acetic acid (CH
3
COOH)
Molarity ( M ) =
( )
( )

=



= C Molal (M)
Mass of acetic acid
Number of moles =
( )
(

)

T mol of CH
3
COOH =
( )
(

)

mass = H g
Mass of solution
= 1 mL



= 10 g

Mass percent of acetic acid
Percent solute =
( )
( )

=



= D % of CH
3
COOH


DISCUSSION
This experiment was constructed to determine the molarity of a solution and the percent by mass
of acetic acid in vinegar by titration with a standardized sodium hydroxide solution. The
experiment perform by a titration of the sodium hydroxide into the KHP and vinegar. From the
titration, the volume of the sodium hydroxide titrate was recorded to plot the graph. From the
graph, we can determine the accurate volume to neutralize the KHP and vinegar solution. From
the volume, we can determine the molarity and percent by mass of acetic acid in vinegar by do
the several calculation.
In this experiment, we get the molarity and the percent by mass of acetic acid in vinegar. Even
though we get the molarity and percent by mass of acetic acid, it might be not the accurate one.
This is because of the several errors that might be happened during the experiment. One of the
error that might be happen during the experiment is parallax error. The reading of the sodium
hydroxide solution in the burette may be not accurate. This is because it might have air bubble at
the end of the burette. This will give the effect to the volume of sodium hydroxide solution used
to neutralize the KHP and the vinegar.
Besides that, it might be an error happen during the measurement of pH value. The pH reading
taken may not the actual reading because the solution might be not mixed well. This happen
because we take the pH reading after the titration without wait it until it really mixed. It will give
effect on the volume of sodium hydroxide solution required to neutralize the KHP and the
vinegar.
Furthermore, it might be an error happen that cause by the surrounding. For example when we
want to measure the mass of KHP in the balance. We might not get the accurate 1.5 grams of
KHP. This is because of the balance is too sensitive. It can detect the small change in mass. The
air molecule might influence the mass of KHP because we not close the surrounding of the
beaker while taking the mass of the KHP.
An error also might be happen during we measure the volume of vinegar for titration. We use the
volumetric pipette to measure the volume of vinegar. The pipette that we use is not function well.
We just take the approximate reading of the pipette.All this error will influence the result that we
get.
RECOMMANDATIONS
In a way to get more accurate results, several steps can be done to give us more accurate results.
The steps that can be do during the experiment to get more accurate results is make sure the eye
is parallel to the reading of burette during we do the titration. Also make sure there is no air
bubble at the end of the burette. The air bubble must be removed to get the accurate volume of
sodium hydroxide. Furthermore, during we measure the mass of KHP, make sure we close the
balance. Therefore, the air molecule will not effected the reading of balance. Another way to get
the more accurate result, make sure we mixed the solution well before we take the pH reading of
the solution. If the solution not mixed well, it will give the different reading of pH. Moreover, we
have to make sure that the apparatus that we use during the experiment must be in good in a way
to get more accurate reading.

CONCLUSION
The objective of the experiment was achieved. The molarity and percent by mass of acetic acid
in vinegar was determine from the calculation of the results. From the experiment, we get the
average molarity of sodium hydroxide is 0.620 M, the average molarity of acetic acid is 1.8104
M and the average percent by mass of acetic acid is 10.87 % .

REFERENCES

ChemCollective (2014) Determine the concentration of Acetic Acid in Vinegar .
Retrieved at 10 October 2014 : http://chemcollective.org/activities/autograded/131
TitrationInfo(n.d) Determination of acetic acid in vinegar by titration
Retrieved at 10 October 2014 :http://www.titrations.info/acid-base-titration-acetic-acid-
in-vinegar
Eileen Y.L and Cham (2009) Determination of Ethanoic Acid in Vinegar
Retrieved at 10 October 2014: http://www.slideshare.net/wkkok1957/determination-of-
concentration-of-ethanoic-acid-in-vinegar-by-titration

Lab Manual (UiTM Shah Alam, 2014) Determination of Acetic Acid in Vineger.
APPENDIXES