FACULTY OF APPLIED SCIENCE

BACHELOR OF APPLIED CHEMISTRY (Hons.)

CMT 450 (UNIT OPERATION)
EXPERIMENT 1: SIMPLE EQUILIBRIUM DISTILLATION

BIL STUDENT NAME MATRC NUMBER

01. ANNAMIRAH ULON AZMI 2019294994

02. ANIS AMIRA BINTI BADROL HISHAM 2019685518

03. OMMY MADINA BINTI ABDUL HALIM 2019295426

LECTURE’S NAME : MOHD FAUZI BIN ABDULLAH

OBJECTIVE:
To illustrate the use of distillation for separating a mixture of two volatile liquid with
different boiling point.

PROCEDURE:
1. The apparatus has been arranged according to the diagram drawn.
2. The unknown mixture [mixture A] has been put into the round bottom flask until it
reaches about half of the flask.
3. The mixture has been heated until boil by turning on the heating mantle until the first
drop of distillate produce.
4. The temperature has been recorded for the first drop of the distillate.
5. The heating mantle has been controlled in order to maintain the temperature of the
first distillate.
6. Step 5 has been continued until there was no more drop of distillate produce.
7. The temperature has been increased until another drop of distillate produced.
8. The second temperature of distillate has been recorded.
9. All reading has been recorded in table.

CHEMICALS/PROCEDURE:
1. Round bottom
2. Distilling head
3. Heating mantle
4. Thermometer with adapter
5. Receiving flask
6. Retort stand with clamp
7. Condenser
8. Vacuum adapter
9. CHEMICAL: Unknown mixture [mixture A]
DATA AND RESULT :

Distillate Temperature (0C) Expected Compound

First 80 Benzene
Second 129 Toluene

DISCUSSION:

Distillation is common method which used for separating mixture based on difference
in boiling point. To separate a mixture of liquids, the liquids can be heated to force the
component to turn into vapor phase. As the mixture is heated, the temperature rises until it
reaches the temperature of the lowest boiling substance in the mixture, while the other
components of the mixture remain in their original phase in the mixture. Vapor rich with
volatile component. The resultant hot vapor passes into a condenser and is converted to the
liquid, which is then collected in a receiver flask which known as distillate. The other
components of the mixture remain in their original phase until the distillate has boiled off is
known as residue. Residue is less volatile compound compare to the distillate which more
volatile components.

In this experiment, the first drop of distillate at the temperature, 80 °C and the second
drop of distillate at the temperature, 129 °C. The expected compound of the first drop of
distillate is benzene and toluene is the second drop of distillate. The compound was identified
due the temperature has been obtained with their respective boiling point.

During the distillation process, the vapors produced from the mixture with move into
water-cooled condenser and condensed into liquid and then the distillate collected in the
receiver will contain more volatile than the residue. In this experiment benzene are more
volatile because have low boiling point which higher vapor pressure compare to toluene is less
volatile component due the higher boiling point.

There are several precaution steps that will take to avoid any accident and the result
more reliable. Most organic liquids are flammable and sometime toxic so avoid to use the
compound near flames or heat source. Next, avoid inhaling the vapors or ingesting these
compounds which handle the material and apparatus during conducting the experiment in the
fume hood. Besides that, make sure thermometer that insert in the thermometer adaptor should
hold the thermometer close to the adaptor and twist gently away from you.
CONCLUSION:

In conclusion, this experiment we can illustrate the use of distillation for separating a mixture
of two volatile with different boiling point. The lower boiling point is more volatile
component which is benzene while the higher boiling is less volatile which is toluene.

REFERRENCE:

Fazsroul (n.d), [Lab Report Operation Unit] Experiment 4: INTRODUCTION TO A BATCH

……PROCESS: SIMPLE BATCH DISTILLATION. Retrieved May 10, 2020 from
……https://www.scribd.com/document/265494964/Lab-Report-Operation-Unit-
………Experiment-4-INTRODUCTION-TO-A-BATCH-PROCESS-SIMPLE-BATCH DISTILLATION

Naim, I, (October, 2017) Experiment 2 Simple Distillation. Retrieved May 10, 2020 from
…….https://www.academia.edu/37645606/EXPERIMENT_2_SIMPLE_BATCH_DISTILL
ATI …….ON

Roslan, N, ( March, 2015) EXPERIMENT 2 - LAB REPORT UNIT OPERATION CMT 463
No of ……the... Retrieved May 10, 2020 from
……https://www.coursehero.com/file/13758996/EXPERIMENT-2/
QUESTION

1. Why we need to control the temperature of the first distillate?

The head temperature rises as the vapors of lower-boiling compound fill the distillation head.
The temperatures drops because the lower-boiling compound finishes distilling before vapors
of the higher-boiling compound can fill the distillation head, which then cause the head
temperature to rise.

2. Suggest what type of unknown mixture [Mixture A]? Homogenous mixture or

heterogeneous mixture? Why?

The type of unknown mixture is homogenous because the components in the mixture dissolved to each
other and is in one continuous phase.

3. Suggest the expected compound for first distillate and second distillate and why you
choose that respective compound?

The expected compound for first distillate and second distillate is ethanol and water respectively. This
respective compounds are chosen due to the comparison of recorded temperature of the first drop of
distillate with the theory boiling point of components

4. Discuss in atomic level, what happen during distillation process? How do you relate the
volatility of the first distillate and second distillate with their boiling point?

During distillation, the molecules of the liquid are held close by intermolecular forces and slowly pulled
away resulting a much weaker bond, thus the molecule separated from each other and become a vapour.
Then the vapour condensed into a liquid which it is called distillate. The more volatile the components,
the lower the boiling point of the components. Thus, the component that distillate first is more volatile
than the component that distillate after that.

5. Explain the precaution steps in conducting this experiment.

There are some precaution steps in conducting this experiment. Firstly, make sure that the apparatus is
set up correctly in order to prevent the apparatus from being broken. Next, make sure to alert the first
drop of distillate as the temperature of the first drop distillate need to be recorded and maintained until
there is no any distillate produce. Moreover, make sure to control the temperature of the first distillate
as the intermolecular bond of the liquid can be break.
 FACULTY OF APPLIED SCIENCE
BACHELOR OF APPLIED CHEMISTRY (Hons.)
CMT 450 (UNIT OPERATION)
EXPERIMENT 2 :SIMPLE BATCH DISTILLATION

BIL STUDENT NAME MATRC NUMBER

01. ANNAMIRAH ULON AZMI 2019294994

02. ANIS AMIRA BINTI BADROL HISHAM 2019685518

03. OMMY MADINA BINTI ABDUL HALIM 2019295426

LECTURE’S NAME : MOHD FAUZI BIN ABDULLAH

Theory :
An ordinary binary mixture is a mixture which contains only two components ( A and B )
that
mixes at all proportion to form a homogeneous solution. ‘A’ denotes much volatile
component
that has lower boiling point or higher vapor pressure while component B is less volatile. By
utilizing their difference in volatility, we can separate these components by heating the
mixture.
The vapor generated by the heating generally has a higher content of component A while
component B is normally concentrated in the residual liquid. Hence separation has taken
effect. This separation is called distillation.
In this particular experiment, we will distill a mixture of acetic acid-water using a simple
batch
technique whereby the generated vapor is condensed as fast as it forms so that the vapor will
not reach an equilibrium with the liquid. The mathematical treatment of this type of
distillation
is given in the form of Raleigh equation.

INTRODUCTION :
Simple distillation is a procedure by which two liquids with different boiling points can
be separated. Simple distillation (the procedure outlined below) can be used effectively to
separate liquids that have at least fifty degrees difference in their boiling points. As the liquid
being distilled is heated, the vapors that form will be richest in the component of the mixture
that boils at the lowest temperature. Purified compounds will boil, and thus turn into vapors,
over a relatively small temperature range (2 or 3°C); by carefully watching the temperature in
the distillation flask, it is possible to affect a reasonably good separation. As distillation
progresses, the concentration of the lowest boiling component will steadily decrease.
Eventually the temperature within the apparatus will begin to change; a pure compound is no
longer being distilled. The temperature will continue to increase until the boiling point of the
next-lowest-boiling compound is approached. When the temperature again stabilizes, another
pure fraction of the distillate can be collected. This fraction of distillate will be primarily the
compound that boils at the second lowest temperature. This process can be repeated until all
the fractions of the original mixture have been separated

Continuous distillation is a thermodynamically efficient method of producing large

amounts of material of constant composition. When small amounts of material or varying
product compositions are required, batch distillation has several advantages. In batch
distillation a charge of feed is loaded into the reboiler, the steam is turned on, and after a short
startup period, product can be withdrawn from the top of the column. When the distillation is
finished, the heat is shut off, and the material left in the reboiler is removed. Then a new batch
can be started. Usually the distillate is the desired product.
Batch distillation is a much older process than continuous distillation. Mesopotamian clay
distillation pots have been dated to around 3500 B.C.E. (RT, 2007), and alchemists in
Alexandria used simple batch retorts in the first century A.D. (Davies, 1980). Batch distillation
was developed to concentrate alcohol by Arab alchemists around 700 A.D. (Vallee, 1998). It
was adopted in Western Europe, and the first known book on the subject was Hieronymus
Brunschwig’s Liber de arte distillandi, published in Latin in the early 1500s. This book
remained a standard pharmaceutical and medical text for more than a century. The first
distillation book written for a literate but not the scholarly community was Walter Ryff’s Das
New gross Distillier Buch, published in German in 1545 (Stanwood, 2005). This book included
a “listing of distilling apparatus, techniques, and the plants, animals, and minerals able to be
distilled for human pharmaceutical use.” Kockmann (2014) thoroughly reviews the history of
batch distillation. Advances in batch distillation have been associated with its use to distil
alcohol, pharmaceuticals, coal oil, petroleum oil, and fine chemicals.

Batch distillation is versatile. A run may last from a few hours to several days. Batch
distillation is used when the plant does not run continuously and batches must be completed in
one or two shifts (8 to 16 h). It is often used when the same equipment distills several different
product at different times. If distillation is required only occasionally, batch distillation is the
usual choice.

Objective :
The purpose of this experiment is to separate an ordinary binary mixture consisting of acetic
acid and water using a simple batch distillation technique.

Apparatus :
Beaker, conical flask, measuring cylinder, Erlenmeyer flask, distillation kit, hot plate, burette,
and volumetric flask.

Procedure :
A. Distillation
1. An acetic acid-water solution was prepared by adding 40 ml acetic acid (sg = 1.048) to 20
ml
distilled water in an Erlenmeyer flask (a conical flask from your distillation kit).
2. The flask was put on a heating mantel. Using apparatus supplied in the distillation kit, the
solution was set up for distillation as demonstrated by your instructor. Work gently since the
glassware is quite fragile and rather expensive to replace.
3. The tap gently turned on to let cooling water into the condenser. The hose
for outlet water was made sure is inside the sink. The inlet water was adjusted so that the
cooling water enters at a rate sufficiently high enough to cool and condense the vapor
completely but not too high as to render the equipment set-up unstable.
4. A clean and dry 150 ml beaker was weighed and was positioned in beneath the distillate
outlet spout to collect the distillate.
5. All connections was checked they were fit snugly before the distillation process begin. The
distillation was started by turning on the hot plate. The heating control switch should be
positioned at 6 or 7.
6. When the solution inside the flask is approximately one-third vaporized, the hot
plate was turned off.
7. The plate was waited until it cools down and all the vapors was let to condense before
disassemble the distillation equipment. While disassembling the glassware, we should be
careful not to spill any distillate that might be trapped in between the connections. We should
collect this trapped distillate and add up to our collecting beaker.

B. Titration of distillate
1. The collecting beaker was reweighed including its content.
2. All distillate from the beaker was poured into a 250-ml volumetric flask. The remaining
distillate left on the beaker-wall was washed onto the flask with distillated water.
3. Half of the flask was filled with distilled water. Its cap was put and the flask was shaked
gently a few times. Then the flask was filled up to the mark with distilled water. The cap was
put on again and the flask was turned upside down a few times so that the solution is well-
mixed.
4. About 100 ml of the diluted solution was poured into a clean beaker. Using a pipette, 20
ml or 25 ml of the solution each was took into 3 separate clean conical flasks. Then, 2
drops of phenolphthalein indicator was squeezed into each flask.
5. A burette was filled with 2.0M NaOH solution and the content of each flask was titrated
with NaOH.

C. Titration of liquid residue

1. Steps B1 to B5 was repeated for the liquid residue.
RESULT AND DATA :
A.DISTILLATION

RESIDUE DISTILLATE

Mass of Mass of Mass of Mass of Mass of Mass of

empty empty residue empty beaker + distillate (g)
Erlenmeyer Erlenmeyer beaker (g) distillate (g)
flask (g) flask + (g)
residue (g)

180.04 195.59 15.05 97.86 139.66 41.80

Table 1 : Distillation

B.TITRATION OF DISTILLATE

Conical flask 1 2 3

Initial reading of 0.0 0.0 0.0

NaOH (mL)

Final reading of 22.0 21.0 21.5

NaOH (mL)

Volume of NaOH 22.0 21.0 21.5

used (mL)

Table 2 : Titration of Distillate

C. TITRATION OF LIQUID RESIDUE

Conical flask 1 2 3

Initial reading of 0.0 0.0 0.0

NaOH (mL)

Final reading of 12.5 12.0 11.5

NaOH (mL)

Volume of NaOH 12.5 12.0 11.5

used (mL)

Table 3 : Titration of Liquid Residue

CALCULATION:

A. DISTILLATION

Residue: 195.59 – 180.54 = 15.05 g

Distillate: 139.66 – 97.86 = 41.80 g

B. TITRATION OF DISTILLATE
22+21+21.5
Average Volume of NaOH used =
3

= 21.5

C. TITRATION OF LIQUID RESIDUE

12.5+12.0+11.5
Average Volume of NaOH used =
3

= 12.0
QUESTION:

1. Calculate the molar composition of feed solution (Given ρCH3COOH = 1.048 g/mL and
ρH2O= 1.000g/mL)

Molar composition of feed solution :

𝑀𝑎𝑠𝑠
Density = 𝑉𝑜𝑙𝑢𝑚𝑒

Mass = Density x Volume

Density of acetic acid = 1.048 g/cm3

Mass = (1.048 )(20)

= 20.96 g

Composition Mass (g) Mole (gmol) Mole fraction Mole percent

Water (A) 10.00 10.00 0.5556 0.6139 x 100 %

18 0.9046
= 61.39 %
= 0.5556 mol = 0.6139

Acetic acid (B) 20.96 20.96 0.3493 0.3860 x 100 %

18 0.9046
= 38.60 %
= 0.3493 = 0.3860

Total 30.96 0.9049 1.000 100%

 2. From titration data, determine the composition of the distillate.

Acid-Base titration Equation :

CH3COOH + NaOH → CH3COONa + H2 O

Molarity of NaOH = 2.0 M ; Volume of NaOH = 21.5 mL

Molarity of CH3COOH = ? ; Volume of CH3COOH = 25 mL

No of moles CH3COOH = ( 2.0 )( 0.0215)

= 0.043 moles

Therefore 0.043 mole of CH3COOH are present in the 25 mL . So the number of moles of
CH3COOH in 250 mL solution can be calculate which the composition of distillate :

M1V1=M2V2

250
𝑋 0.043 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑 𝑖𝑛 25 𝑚𝐿
25

= 0.4300 moles of acetic acid in 250 mL

Composition Mass (g) Mass Mole (gmol) Mole Mole percent

fraction fraction (%)

Water ( A ) 41.80 – 16.00 16.00 0.8889

25.80 41.80 18.00 1.3189
0.6740 x 100
= 0.3828 = 0.8889 = 0.6740
= 16.00
= 67.40

Acetic Acid 0.43 x 60 25.80 0.4300

(B) 41.80 1.3189
= 25.80 = 0.4300 0.3260 x 100
= 0.6172 = 0.3260
= 32.60

Total 41.80 1.0000 1.3189 1.0000 100

 3. From titration data, determine the composition of the residual liquid.

Acid-Base titration Equation :

CH3COOH + NaOH → CH3COONa + H2 O

Molarity of NaOH = 2.0 M ; Volume of NaOH = 12.0 mL

Molarity of CH3COOH = ? ; Volume of CH3COOH = 25 mL

No of moles CH3COOH = ( 2.0 )( 0.0120)

= 0.0240 moles

Therefore 0.0240 mole of CH3COOH are present in the 25 mL . So the number of moles
of CH3COOH in 250 mL solution can be calculate which the composition of distillate :

M1V1=M2V2

250
𝑋 0.0240 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑 𝑖𝑛 25 𝑚𝐿
25

= 0.2400 moles of acetic acid in 250 mL

Composition Mass (g) Mass Mole (gmol) Mole Mole percent

fraction fraction (%)

Water ( A ) 15.55 – 1.15 1.15 0.0640

14.40 15.55 18.00 0.3040
0.2110 x 100
= 0.0740 = 0.0640 = 0.2110
= 1.15
= 21.10

Acetic Acid 0.24 x 60 14.40 0.2400

(B) 15.55 0.3040
= 14.40 = 0.2400 0.7890 x 100
= 0.9260 = 0.7890
= 78.90

Total 15.55 1.0000 0.3040 1.0000 100

4. Using Raleigh equation, calculate the theoretical composition of distillate and residual
liquid. Compare the theoretical values with experimental values. (Equilibrium data
for water-acidic system at 1 atm is provided in Appendix 1)

Raleigh equation =

𝑥1
𝐿1 1
𝑙𝑛 = ∫ 𝑑𝑥
𝐿2 𝑦−𝑥
𝑥2

L1 = Number of moles of liquid at t1 = 0.9049

2
L2 = Number of moles of liquid residue at t2 = 0.9049 x 3

= 0.6033

𝟏
= 𝑻𝒉𝒆 𝒉𝒐𝒕 𝒑𝒍𝒂𝒕𝒆 𝒘𝒂𝒔 𝒕𝒖𝒓𝒏𝒆𝒅 𝒐𝒇𝒇 𝒘𝒉𝒆𝒏 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏 𝒊𝒏𝒔𝒊𝒅𝒆 𝒕𝒉𝒆 𝒇𝒍𝒂𝒔𝒌
𝟑

x1 = Mole fraction of A in liquid residue

x2 = Mole fraction of A in liquid distillate

MATERIAL MASS BALANCE :

L1 = V + L2

0.9049 = V + 0.6033

V = 0.3016
V = 0.3016

Y2 = ?

L1 = 0.9049

DISTILLATION
X1 = 0.6139

L2 = 0.6013

X2 = ?
 COMPONENT MOLE FRACTION A IN

A B LIQUID VAPOR

0.0000 0.0000

0.1881 0.0063

0.3084 0.4467

0.4498 0.5973

0.5195 0.6580

0.5824 0.7112

ACETIC 0.6750 0.7797

WATER
ACID 0.7261 0.8239

0.7951 0.8671

0.8556 0.9042

0.8787 0.9186

0.9134 0.9409

0.9578 0.9708

1.0000 1.0000

Appendix 1 : Equilibrium data for water-acidic system at 1 atm

 1
x
Y y-x 𝑦−𝑥
(x-axis)
(y-axis)

0.0000 0.0000 0.000 0.00

0.1881 0.3063 0.1182 8.46

0.3084 0.4467 0.1383 7.23

0.4498 0.5973 0.1475 6.78

0.5195 0.6580 0.1385 7.22

0.5824 0.7112 0.1288 7.64

0.6750 0.7797 0.1047 9.55

0.7261 0.8239 0.0978 10.22

0.7951 0.8671 0.0720 13.89

0.8556 0.9042 0.0486 20.58

0.8787 0.9186 0.0399 25.06

0.9134 0.9409 0.0275 36.36

0.9578 0.9708 0.0130 76.92

1.0000 1.0000 1.0000 1.0000

 1/Y-X vs X
12

9.55
10
8.46
7.64
8 7.23 7.22
6.78
1/Y-X

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
X AXIS

Graph 1 : Equilibrium for water-acidic system at 1 atm

0.6139
𝑂. 9049 1
𝑙𝑛 = ∫ 𝑑𝑥
0.6033 𝑦−𝑥
𝑥2

0.6139 1
0.4054 = ∫𝑥 𝑑𝑥
2 𝑦−𝑥

AREA UNDER GRAPH :

0.4054 = P + Q

1
= 2 ( 8.1 − 7.3)( 0.6139 − 𝑥2 ) + (0.6139 − 𝑥2 )(6.8)

0.4054 = 0.4 ( 0.6139 – 𝑥2 ) + ( 0.6139 – 𝑥2 )(6.8)

0.4054 = 4.4201 – 7.2 𝑥2

4.0147
𝑥2 =
7.2

= 0.5576
Therefore : X1L1=VY2+X2L2

(0.6139)(0.9049) = (0.3016) Y2 + (0.5576)(0.6033)

0.5556 = 0.3016Y2 + 0.3364

0.5556−0.3364
Y2 = 0.3016

= 0.7268

THEORETICAL VALUE EXPERIMENTAL VALUE

COMPOSITION MOLAR COMPOSITION MOLAR

COMPOSITION COMPOSITION
(%) (%)

DISTILLATE 72.68 DISTILLATE 67.40

RESIDUE 55.76 RESIDUE 21.11

5. What is the advantage of batch distillation compare with simple equilibrium

distillation?
The advantage of batch distillation is the feed quantity small which the quantities of
material are to be handled at regularly scheduled periods. It is often more economical
for small volume productions. Batch distillation also flexible which the little change is
required when switching from one mixture to another. It flexible in accommodating
change in product formulation, changes in production rate, changes in feed
composition.
DISCUSSION:

For this experiment, we need to separate an ordinary binary mixture which is

consisting of acetic acid and water. We will use two steps which are a simple batch
distillation technique (main steps) and titration of distillate and liquid residue to get the final
result. Ordinary binary mixture is a mixture that contains two components that mixes at all
proportion to form a homogeneous solution. Batch distillation refers to the use of distillation
in batches, meaning that a mixture is distilled to separate it into its component fractions
before the distillation still is again charged with more mixture and the process is repeated. We
will use acetic acid-water as solution for distillation.

In this experiment, we need to calculate molar composition of feed solution. We will

use this formula to find it;

Density = 𝑀𝑎𝑠𝑠 /𝑉𝑜𝑙𝑢𝑚𝑒

So, the feed solution are water and acetic acid. The value of molar composition for
both feeds are 38.6% and 61.39%. Then, from this experiment we also can determine the
composition of the distillate and residual liquid. For distillate, the value of compositions are
67.70% for water and 32.60% for acetic acid while for residue, the value of composition are
21.10% for water and 78.90% for acetic acid.

Based on the result, there might be an error to the reading of acid and water. After the
distillation process, there is still water in the condenser that was left. This may affect the
reading of mass of water in the receiving flask. Apart from that, some of evaporated water
may be escaped from the process due to the error in setting the apparatus. This can affect the
results.
CONCLUSION:

As a conclusion, the separation of ordinary binary mixture consisting of acetic acid and
water can be done by using a simple batch distillation technique.

REFERENCES:

1.https://en.wikipedia.org/wiki/Batch_distillation

2. https://onlinelibrary.wiley.com/doi/pdf/10.1002/cae.21556

3. http://library.wolfram.com/infocenter/mathsource/8304/binous_al_harthi.pdf
 FACULTY OF APPLIED SCIENCE
BACHELOR OF APPLIED CHEMISTRY (Hons.)
CMT 450 (UNIT OPERATION)
EXPERIMENT 3 : TERNARY PHASE DIAGRAM
(LIQUID-LIQUID EXTRACTION)
BIL STUDENT NAME MATRC NUMBER

01. ANNAMIRAH ULON AZMI 2019294994

02. ANIS AMIRA BINTI BADROL HISHAM 2019685518

03. OMMY MADINA BINTI ABDUL HALIM 2019295426

LECTURE’S NAME : MOHD FAUZI BIN ABDULLAH

INTRODUCTION:
The aim of this experiment was to determine a bimodal solubility curve and to
determine the line and plait point for a system of acetic acid, chloroform and water at room
temperature and atmospheric pressure. The tie line is drawn using the mass fraction of
chloroform, water and acetic acid of mixture. This experiment will used separation technique
or process which the solute in feed stream are extracted by contacting the feed with a solvent
which known as solvent extraction. Mostly the solvent and the feed are partially in one another.
Ternary system are consists of the solvent, solute and the feed. The composition the system are
conveniently represented on an equilateral triangle plot with each corner of the triangle
representing one of the three components. Lastly , in this experiment show that the feed are in
the formed of water, chloroform are the solvent while acetic acid are the solvent .

OBJECTIVES :

i)To determine a bimodal solubility curve .

ii)To determine the line and plait point for a system of acetic acid, chloroform and water at
room temperature and atmospheric pressure.

APPARATUS AND MATERIAL :

Conical flask, burette , flask , separating funnel , dry conical flask , chloroform, acetic acid ,
1.0M NaOH , phenolphthalein .
PROCEDURE :

A. To obtain a bimodal solubility curve .

Table 1 in the result section was completed by calculating volume of acetic acid and
chloroform needed to form 10 g of two component solutions with the indicated
compositions.(Complete the calculations before laboratory start ). In a conical flask ,10 g of
two components solution that is made of acetic acid and chloroform using the volumes that
have pre-calculated in step 1.Distilled water was put inside a burette ,the initial burette reading
was took and slowly the mixture was titrated that have been prepared in step 2 with water until
the solution become turbid (cloudy). While titrating, do not forget to gently shake the mixture
in order to mix them well. The titration was stopped when resulting solution in the flask turns
turbid. The final burette reading was took. While was waited and allowed sufficient time for
equilibrium to establish, it should notice the intermediate mixture will separate into two distinct
heavy and light phases. The flask was held against the light and was tried to look for the phases
from the bottom of flask if cannot see the phases clearly. It is possible that might not be able
to see the phases especially at very low concentration.

B. To obtain a tie lines and plait point.

Using the combination in Table 2, a three-component mixture was placed in a separating

funnel. Shaked it well and gently for a while.Then point the tip of the funnel away from yourself
and friends and the vent stopcock was opened to release any build-up vapor pressure.Continue
shaked and vented for about 5 minute,make sure the stopcock was closed before shaking. The
separating funnel on its o-ring support was placed and was left it for 3 minute to allow heavy
and light phases to separate.2 dry conical flask was weighted and each phase was drained into
it.Then each flask was reweighted.Each phase was titrated with 1.0M NaOH solution using
phenolphthalein as indicator .The end point was when the solution changes color.The
procedure above was repeated for the other combination in Table 2.
RESULT AND DATA:
A: Data for bimodal solubility curve
Table 1: Result for titration of 10g acetic acid-hloroform mixture with water
MASS % MASS OF VOLUME MASS OF VOLUME OF VOLUME MASS TOTAL
OF ACETIC OF CHLOROFORM ACETIC ACID OF OF MASS
ACETIC ACID (g) ACETIC (g) (ml) WATER WATER (g)
ACID ACID (ml) (ml) (g)

90 9 8.58 1 0.67 18.2 18.2 28.2

80 8 7.63 2 1.35 7.4 7.4 17.4

70 7 6.67 3 2.02 5.4 5.4 14

60 6 5.72 4 2.70 3.5 3.5 13.5

50 5 4.77 5 3.37 1.2 1.2 11.2

40 4 3.81 6 4.05 1.0 1.0 11.0

30 3 2.86 7 4.72 0.6 0.6 10.6

20 2 1.91 8 5.39 0.4 0.4 10.4

10 1 0.95 9 6.07 0.2 0.2 10.2

*Densities of chloroform, acetic acid and water are 1.483, 1.049 and 1.000 g/ml respectively.

B: Data for tie lines and plait point

Table 2 : Result for titration of phases with 1 M NaOH.
Mass (g) Volume (mL) of 1.0 M
NaOH to titrate

Chloroform Acetic Water Heavy Light Heavy Light

acid Phase Phase Phase Phase

10 6 6 10.99 9.66 30.10 56.7

8 6 6 6.41 11.56 15.40 79.2

6 4 10 4.31 14.23 4.70 60.6

CALCULATION:

A: Data for bimodal solubility curve

1) Volume of acetic acid:

𝑚𝑎𝑠𝑠, 𝑔
𝑑𝑒𝑛𝑠𝑖𝑡𝑦 =
𝑣𝑜𝑙𝑢𝑚𝑒, 𝑚𝑙

𝑚𝑎𝑠𝑠, 𝑔
𝑣𝑜𝑙𝑢𝑚𝑒, 𝑚𝑙 =
𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑔𝑚𝑙 −

9.00 𝑔
= 1.049𝑔𝑚𝑙−

= 8.58 mL

2) Weight Fraction of chloroform, acetic acid and water

i) Weight Fraction of acetic acid:

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑

𝑠𝑎𝑚𝑝𝑙𝑒 1 =
𝑡𝑜𝑡𝑎𝑙 𝑚𝑎𝑠𝑠(𝑔)

9𝑔
= 28.2 𝑔

= 0.3191

ii) Weight Fraction of chloroform

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑐ℎ𝑙𝑜𝑟𝑜𝑓𝑜𝑚 (𝑔)

𝑠𝑎𝑚𝑝𝑙𝑒 1 =
𝑡𝑜𝑡𝑎𝑙 𝑚𝑎𝑠𝑠(𝑔)

1
=
28.2

= 0.0355

iii) Weight Fraction of water

 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑔)
𝑠𝑎𝑚𝑝𝑙𝑒 1 =
𝑡𝑜𝑡𝑎𝑙 𝑚𝑎𝑠𝑠(𝑔)

18.2
=
28.2

= 0.6454

SAMPLE WEIGHT FRACTION WEIGHT FRACTION OF WEIGHT FRACTION OF

OF ACETIC ACID CHLOROFORM WATER

1 0.3191 0.0355 0.6454

2 0.4598 0.1149 0.4253

3 0.4895 0.2098 0.3007

4 0.4444 0.2963 0.2593

5 0.4464 0.4464 0.1071

6 0.3636 0.5454 0.0909

7 0.2830 0.6604 0.0566

8 0.1923 0.7692 0.0385

9 0.0980 0.8824 0.0385

B: Data for tie lines and plait point

i) Chemical equation:

𝐶𝐻3 𝐶𝑂𝑂𝐻 + 𝑁𝑎𝑂𝐻 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐻2 𝑂

ii) Mass of acetic acid in heavy phase:

Sample 1

1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻 60 𝑔 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 30.10 × 10−3 𝐿 𝑁𝑎𝑂𝐻 × × ×
1𝐿 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 1.806 𝑔

Sample 2

1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻 60 𝑔 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 15.40 × 10−3 𝐿 𝑁𝑎𝑂𝐻 × × ×
1𝐿 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 0.924 𝑔

Sample 3

1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻 60 𝑔 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 4.7 × 10−3 𝐿 𝑁𝑎𝑂𝐻 × × ×
1𝐿 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 0.282 𝑔

iii) Mass of acetic acid in light phase:

Sample 1

1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻 60 𝑔 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 56.7 × 10−3 𝐿 𝑁𝑎𝑂𝐻 × × ×
1𝐿 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 3.402 𝑔

Sample 2

1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻 60 𝑔 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 65.2 × 10−3 𝐿 𝑁𝑎𝑂𝐻 × × ×
1𝐿 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 3.912 𝑔

Sample 3

1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻 60 𝑔 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 60.6 × 10−3 𝐿 𝑁𝑎𝑂𝐻 × × ×
1𝐿 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐶𝐻3 𝐶𝑂𝑂𝐻

= 3.636𝑔

Phase 1 2 3

Heavy 1.806 g 0.924 g 0.282 g

Light 3.402 g 3.912 g 3.636 g

iv) Mass percent of acetic acid:

Heavy Phase:

Sample 1

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑

=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑖𝑛 𝑓𝑙𝑎𝑠𝑘

1.806 𝑔
= × 100%
10.99 𝑔
 = 16.43%

Sample 2

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑

=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑖𝑛 𝑓𝑙𝑎𝑠𝑘

0.924 𝑔
= × 100%
6.41 𝑔

= 14.41%

Sample 3

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑

=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑖𝑛 𝑓𝑙𝑎𝑠𝑘

0.282 𝑔
= × 100%
4.31 𝑔

= 6.54%

Light Phase:

Sample 1

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑

=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑖𝑛 𝑓𝑙𝑎𝑠𝑘

3.402 𝑔
= × 100%
9.66 𝑔

= 35.22%

Sample 2

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑

=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑖𝑛 𝑓𝑙𝑎𝑠𝑘

3.912 𝑔
= × 100%
11.56 𝑔

= 33.84%

Sample 3
 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑
=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑖𝑛 𝑓𝑙𝑎𝑠𝑘

3.636 𝑔
= × 100%
14.32 𝑔

= 25.39%

Mass percent (%) 1 2 3

Heavy phase 16.43% 14.41% 6.54%

Light phase 35.22% 33.84% 25.39%

DISCUSSION

The aim of this experiment was to determine a bimodal solubility curve and to
determine the line and plait point for a system of acetic acid, chloroform and water at room
temperature and atmospheric pressure. We have two main procedure which is Part A and Part
B to achieve our objectives in this experiment.

Plait Point is the point where the raffinate phase and extract phase both have same
composition. Analogous to azeotropic mixture of distillation where the composition is same in
both liquid and vapour phase hence separation is not possible unless the azeotrope is broken
by external effects, at plait Point the composition of solute is same in both raffinate and extract
phase. It's the maxima of the curve ( in ternary phase diagram) where tie line becomes a dot
and separation is not possible. Phase diagram is graphical representations of the liquid, vapor,
and solid phases that co-exist at various ranges of temperature and pressure within a reservoir.
Ternary phase diagrams represent the phase behavior of mixtures containing three components
in a triangular diagram.

In part A, for the data for bomidal solubility curve, the volume of acetic acid is 8.58
mL. The weight fraction of acetic acid, chloroform and water are 0.3191, 0.0355, and 0.6454
respectively.

In part B, the data for tie lines and plait point, we got the chemical equation which is :

𝐶𝐻3 𝐶𝑂𝑂𝐻 + 𝑁𝑎𝑂𝐻 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐻2 𝑂

Mass of acetic acid in heavy phase is 1.806 g in sample 1, 0.924 in sample 2 and 0.282
g in sample 3. However, mass of acetic acid in light phase is 3.402 g in sample 1, 3.912 g in
sample 2 and 3.636 g in sample 3. The mass percent of acetic acid for heavy phase is 16.43%
, 14.41% and 6.54% for sample 1, sample 2 and sample 3 respectively. While for light phase
the mass percent of acetic acid is 35.22%, 33.84% and 25.39 % for sample 1, sample 2 and
sample 3 respectively.
CONCLUSION

In conclusion we successfully determine a bimodal solubility curve. We also got to determine

the line and plait point for a system of acetic acid, chloroform and water at room temperature
and atmospheric pressure.

REFERENCES

Madeira. A.A (2019). Ecletica Quimica Journal. Application of a ternary phase diagram to the
liquid-

liquid extraction of ethanoic acid using ethyl ethanoate. Retrieved June 20 ,2020 from
https://revista.iq.unesp.br/ojs/index.php/ecletica/article/view/1025

Course Hero (2020). Experiment 3 UO- Lab report CM 463 experiment 3 ternary phase
diagram

(liquid-liquid extraction). Retrieved June 20, 2020 from

https://www.coursehero.com/file/17224334/exp-3-uo/
QUESTION

1. From table 1, obtain the bimodal solubility curve and calculate the mass fraction
for each component in the turbid mixture.

Answer based on calculation.

2. Using the mass fractions, construct the bimodal solubility curve (ternary phase
diagram) for the three components mixture by means of right angle triangular
diagram.

Acetic-chloroform-water ternary diagram

1.2

0.8
Acetic Acid

0.6

0.4

0.2

0
0 0.6454 0.4253 0.3007 0.2593 0.1071 0.0909 0.0566 0.0385 0.0196 0
Water

3. Write a chemical equation for the titration. The equation enables you to calculate
the mass of acetic acid present in each sample.

CH3 COOH + NaOH → CH3 COONa + H2 O

4. Calculate the mass percent of acetic acid in each heavy phase and light phase at a
particular combination in Table 2 which will give you a tie line for your ternary
system. You should have 3 tie lines. From the tie lines, determine the plait point.
Answer based on calculation.

Acetic-chloroform-water ternary diagram

1.2

0.8
Acetic Acid

0.6 P
0.4

0.2

0
0 0.6454 0.4253 0.3007 0.2593 0.1071 0.0909 0.0566 0.0385 0.0196 1
Water
 FACULTY OF APPLIED SCIENCE
BACHELOR OF APPLIED CHEMISTRY (Hons.)
CMT 450 (UNIT OPERATION)
EXPERIMENT 4 : SINGLE STAGE EXTRACTION
(LIQUID-LIQUID EXTRACTION)
BIL STUDENT NAME MATRC NUMBER

01. ANNAMIRAH ULON AZMI 2019294994

02. ANIS AMIRA BINTI BADROL HISHAM 2019685518

03. OMMY MADINA BINTI ABDUL HALIM 2019295426

LECTURE’S NAME : MOHD FAUZI BIN ABDULLAH

OBJECTIVE:

In this experiment, students will perform a single-single extraction to separate acetic acid
from its solution in chloroform using water as an extraction solvent. This acid contents in the
raffinate and extract phases will be determined by titration and its results are compared to the
theoretical result.

PROCEDURE:

1. A binary acetic acid-chloroform solution has been prepared by adding 4 ml acetic acid
to 5 ml chloroform in separating funnel.
2. With the funnel mouth still open, the mixture has been swirled to mix it well into a
homogenous binary solution. This will be our fed solution.
3. The acid has been extracted from the binary solution using equal mass of an
extraction solvent, water. 10 mL of distilled water has been measured and has been
pour it into the funnel.
4. Hand glove has been put on. With the stopper on, the funnel has been gently shook
and then open its stopcock to release any pressure build-up.
5. The funnel has been put on the o-ring support and lets its content settle into phases.
Need to wait for about 5-10 minutes to allow the heavy and the light phases reach
their equilibrium.
6. Two clean empty conical flasks have been weighed and each phase has been
transferred into each flask. The beaker has been reweighed.
7. About two drops of phenolphthalein has been put into each flask and has been titrated
them by using 2.0 m NaOH (aq). The endpoint is when the solution turns color.
RESULT AND DATA :

Extracted phase ( Heavy)

Mass of empty conical Mass of empty conical flask Mass of solution (g)
flask (g) + solution (g)

115.0333 120.963 5.5297

Raffinate phase ( light)

Mass of empty conical Mass of empty conical flask Mass of solution (g)
flask (g) + solution (g)

111.7857 125.3748 13.5891

Conical flask Extracted phase (A)) Raffinate phase (B)

Initial reading of NaOH 0 0

(mL)

Final reading of NaOH (mL) 31.5 2.3

Volume of NaOH (mL) 31.5 2.3

CALCULATION :

Feed Solution Extracting Solvent

Acetic Acid Chloroform Water

Component
(A) (B) (C)

Volume Used
4.00 5.00 10.00
(mL)

Density 1.05 1.48 1.00

4 X 1.05 5 X 1.48 10 X 1.00

Mass (g)

= 4.20 = 7.40 = 10.00

4.2 + 7.4

Total Mass (g) 10.00

= 11.60

Mass fraction of component A = 4.20

11.60

= 0.3621

Basis known: 11.60 g Feed solution

Total mass balance:

F + S = M

11.6 + 10.0 = 21.6

M = 21.6
A mass balance:

xF (F) + yS (S) = xM(M)

0.3621 (11.6) + 0 = xM (21.6)

xM = 0.1945

Based on the graph:

From point E, extract phase contains 0.265 mass fraction of component A (acetic acid)
From point R, raffinate phase contains 0.065 mass fraction of component A (acetic acid)

11.6 g, Feed (F)

0.3621 A E, Extract phase

SINGLE – STAGE 0.265 A

LIQUID – LIQUID M, intermediate

EXTRACTION 0.1945 A

10 g, Extract (S) R, Raffinate phase

0.0000 A 0.065 A

Total mass balance:

F + S = E + R

11.6 + 10.0 = E + R

21.6 = E + R

E = 21.6 - R ________________ A

A mass balance:

xF (F) + yS (S) = x*(R) + y*(E)

0.3621 (11.6) + 0 = 0.065R + 0.265E

4.2004 = 0.065R + 0.265E __________________ B

Substitute A into B:

4.2004 = 0.065R + 0.265 (21.6 – R)

4.2004 = 0.065R + 5.724- 0.265 R

R = 7.618 g

Substitute R = 7.618 g into A:

E = 21.6 - R

E = 21.6 - 7.618

E = 13.982 g

Mass of extract phase: 13.982 g

Mass of acetic acid in extract phase :

0.265 X 13.982

= 3.705 g

Mass of raffinate phase: 7.618 g

Mass of acetic acid in raffinate phase:

0.65 X 7.618

= 4.952 g

From the experiment

Molecular formula of acetic acid : CH3COOH

Element Atomic mass

C 12.0107

H 1.0079

O 15.9994

Molecular weight CH3COOH

2(12.0107) + 4(1.0079) + 2(15.9994)

 = 60.0518

For raffinate phase :

(a) (b) (c) (d)

CH3COOH + NaOH → NaCH3COO + H2O

M: ? M : 2.0 M
2.4
V :? V : (𝟏𝟎𝟎𝟎) L

𝑴𝒂 𝑽𝒂 𝟏
=
𝑴𝒃 𝑽𝒃 𝟏

Mass of CH3COOH in raffinate phase

mol 2.4 1 mole of CH3 COOH g

2.0 M of NaOH X ( )L X X 60 of CH3 COOH
L 1000 1 mole of NaOH mol

= 0.288 g of CH3COOH in raffinate phase

For extract phase

a b c d
CH3COOH + NaOH → NaCH3COO + H2O

M:? M : 2.0 M
𝟐𝟖.𝟒
V :? V : (𝟏𝟎𝟎𝟎) L

𝑴𝒂 𝑽𝒂 𝟏
=
𝑴𝒃 𝑽𝒃 𝟏

Mass of CH3COOH in extract phase

mol 28.4 1 mole of CH3 COOH g

2.0 M of NaOH X ( )L X X 60 of CH3 COOH
L 1000 1 mole of NaOH mol

= 3.408g of CH3COOH in extract phase

 Mass of Acetic Mass of Acetic
Mass of Mass of Acid(A) Acid (A)
Extract Raffinate
in extract phase in raffinate phase
(g) (g)
(g) (g)

Theoritical Value

(from mass balance and 13.9820 7.618 3.705 0.492

graph)

Actual Value 13.616 5.356 3.408 0.288

DISCUSSION:
In this experiment which involve acetic acid that considered as solute A, water is solvent C
while chloroform as diluent B. So this experiment to determine a bimodal solubility curve, the lines and
the plait point for a system of acetic acid-chloroform-water component at room temperature and
atmospheric pressure. Next, it also can separate acetic acid from its solution in chloroform using water
as an extraction solvent.

In addition, this process will formed two layers which are heavy phase which mixture solid that
is feed solution and light phase that is solvent t. Heavy phase can be seen formed at the below of the
separating funnel and the light phase on the top of separating funnel because heavy phase at the most
concentrated and higher density compared to light phase. In this experiment, acetic acid, chloroform
and water will involve. Even though 3 components are added which is acetic acid + chloroform + water
but there are only 2 visible phases, which are extract and raffinate. This is because acetic acid and water
only reacts with each other, but not with chloroform.

A feed liquid (heavy phase) containing desirable compound that is to be separate together with
other compounds. Then extraction liquid (light phase) is added and mixed with the feed liquid through
agitation. The species redistribute themselves between two liquid phase. Agitation of two phase is
continued until equilibrium and then agitation will stop and the liquid are allowed to settle until both
phase are clear. The two phase can then be separated. Therefore, the light phase known as extract phase
and heavy phase act as raffinate phase. Extract phase containing extracted acetic acid and dissolved
water and raffinate phase containing water, leftover acetic acid and dissolved chloroform.

The presence of bubbles in the separating funnel indicated the movement of water
through chloroform, forming intermediate phase momentarily. The bubbles produced provide large
surface are between the chloroform and water solvent. After a period of 5 minutes, the intermediate
settles to raffinate liquid phase and extract liquid phase, showing equilibrium. During titration of each
phase with sodium hydroxide solution (base), the solution produced is hot (energy released: exothermic)
due to the breaking of C-H and C-Cl bonds found is acetic acid and chloroform solution. The end-point
of the titration was indicated by the colour change from colourless to pink by phenolphthalein indicator.
The mass of acetic acid in extract phase in lower than the theoretical value (3.408< 3.705) due to the
evaporation of acetic acid into atmosphere. Contributing error was from titration error and the presence
of random error.
There are some precaution steps were taken while conducting this experiment to avoid any
unnecessary accident and the result are more reliable . Acetic acid vapour is known to be very corrosive,
so be careful not to exhale any of this vapour. Chloroform however is suspected cancer causing agent.
Quickly wash it with a lot of water when you accidently spill it on your skin. Besides that, vent the
separating funnel frequently during the extraction in order to avoid the building up of vapour pressure
which will blow out the stopcock and perhaps also the dangerous content. Make sure the tip of the
separating funnel away from yourself and others when releasing the pressure.

CONCLUSION:
As a conclusion, a bimodal solubility curve, the lines and plait point for a system of three

components consisting of acetic acid, chloroform and water at room temperature and atmospheric

pressure can be determined .Single-stage extraction to separate acetic acid from its solution in

chloroform using water as an extraction solvent also can perform and the acid contents in the raffinate

and extract phases will be determined by titration and its results are compared to the theoretical result.

REFERRENCES:
Fathinizyan (n.d), Experiment4: single-singleextraction(liquid-liquidextraction). Retrieved
June 8, 2020 from https://www.coursehero.com/file/22941874/EXPERIMENT-4-UNIT-
OPERATION-NEW/

Syahiirah (n.d), CHE504 - Lab Report on Liquid - liquid Extraction (L7) (2018), Retrieved
June 8,2020 from https://www.academia.edu/36855639/CHE504_-_Lab_Report_on_Liquid_-
_liquid_Extraction_L7_2018_.
QUESTIONS :
1. Briefly explain what you do to your data in order to obtain your results?
To obtain the result, firstly we need to get the mass of heavy phase and light phase. The, calculate
volume of 2M NaOH used to titrate heavy phase and light phase. Next, calculate masss of feed and
solvent solution. We have to use total material balance equation to find the value of Xm. I mol of
CH3COOH is equal to 1 mol of NaOH. We take the mass of CH3COOH divide with the mass of
heavy phase liquid to get the mass fraction of CH3COOH, x in raffiate heavy phase. The mass of
CH3COOH can be obtained by mol of CH3COOH multiplied by RRM of CH3COOH. Lastly, to get
mass fraction of CH3COOH, y in extract light phase, we divide mass of CH3COOH with mass of
light phase liquid.

2. Discuss your experimental result by comparing to your theoretical result. If they

differ,
how much?

Mass of Acetic
Mass of Acetic
Mass of Mass of Acid (A)
Acid(A)
Extract Raffinate in raffinate
in extract phase
(g) (g) phase
(g)
(g)

Theoretical Value

(from mass balance 13.9820 7.618 3.705 0.492

and graph)

Actual Value 13.616 5.356 3.408 0.288

Mass of extract from the experiment ( 13.616 g ) is lower than the theoretical value (13.9820
g). Its different is 0.366 g. Mass of raffinate from the experiment is 5.356 g and the theoretical
value is 7.618 g. This means mass of raffinate from the experiment is lower than the theoretical
value. So, the different between these two value is 2.262 g. Mass of Acetic acid (A) in extract
phase in the experiment is 3.408 g while for the theoretical value is 3.705. Mass of Acetic acid
(A) in extract phase in the experiment is lower than the theoretical value. Its different is 0.297
g. Mass of acetic acid (A) in raffinate phase in the experiment ( 0.288 g ) is lower than the
theoretical value (0.492 g). The different between these two value is 0.204 g.

3. Why do you think they differ? Include all contributing errors and how these
errors effect
your result.

There’s still a small difference because of some errors that might happen during conducting
experiment such as random error when conducting the venting process, the gas pressure might
not be removed properly. Ext is human error occurred when conducting titration, the eyes
might not parallel to meniscus f the burette. All of these could affect the result of the
experiment.

4. Compare a standard binodal solubility curve for chloroform-acetic acid-water

system
with your binodal solubility curve you obtain from this experiment. Discuss if
exist any
differences

There is difference in formation of new E line at the curve.

5. Explain when liquid-liquid extraction method is suitable to apply compare

with
distillation method.

Extraction can be done for liquid phase and solid phase mixtures and use the different
solubilities of some component in two phases while distillation can be done only for liquid
phase mixtures and use the differences between boiling points of chemical components in a
mixture.
 FACULTY OF APPLIED SCIENCE
BACHELOR OF APPLIED CHEMISTRY (Hons.)
CMT 450 (UNIT OPERATION)
EXPERIMENT 5 : AIR PRESSURE DIFFERENTIAL ACROSS DRY
AND WET COLUMN (GAS ABSORPTION PACKED COLUMN)
BIL STUDENT NAME MATRIC NUMBER

01. ANNAMIRAH ULON AZMI 2019294994

02. ANIS AMIRA BINTI BADROL HISHAM 2019685518

03. OMMY MADINA BINTI ABDUL HALIM 2019295426

LECTURE’S NAME : MOHD FAUZI BIN ABDULLAH

INTRODUCTION:
Gas Absorption was conducted to determine the loading and flooding points in the
column and to determine the air pressure drop across the column as a function of airflow for
different water flow rates through the column. Loading point of a column is when the gas
velocity is high enough to restrict the flow of liquid. When all the liquid carried away by the
gas ,the pressure drops at much faster rate till the another point which known as flooding point.
Higher tray pressure drop due to excessive vapor flow rates holds up the liquid. The column
flooding conditions sets the upper limit of vapor velocity. The flooding point reading cannot
be recorded due the pressure and bubble the column.

Absorption is mass transfer process that is vapour solute A which in the gas mixture
absorbed .This means a liquid which less soluble than the vapour solute A. This occurs because
the gas mixture consists of inert gas and the soluble .The liquid primaly in the gas phase and
its vaporization slight into gas phase. As example absorption of the solute ammonia from air-
ammonia mixture by water which the solute recovered by the distillation from the solution.

Gas absorption which one or more soluble components of gas mixture that dissolved in
a liquid. The gas phase is inert gas while liquid immiscible in the gas phase which that why
liquid phase will vaporize very slightly in gas phase. Chemical reaction between solute and
solvent depends on the types of absorption process which are physical absorption and chemical
absorption.

OBJECTIVE :

i) To determine the air pressure differential across the column as function of air flow
rate.
EQUIPMENT SET UP :

Diagram 1 : Air Pressure Differential Across Dry And Wet Column (Gas Absorption Packed
Column)
METHOD :

PROCEDURE A (Dry Column ) :

The column must be dried by passing the maximum air flow until all evidence of
moisture in the packing has disappeared. Valve of V1,V2 and V3 as shown in the diagram was
set so that the differential pressure in the top and bottom sections of the column are indicated
on the two water manometers. Manometer readings of pressure differential across the column
was took for a range of air flow rates by formula which the total pressure differential is sum of
the differential across the top and bottom halves of column.

PROCEDURE B (Wet Column ) :

The sump to three quarters full was filled with tap water. Valves V1, V2,V3 as shown
on the diagram was set so that differential pressure in top and bottom sections of the column
are indicated on the two water manometer. The water pump was switch on and C1 was set to
give a flow rate of say 3 liters/minute down the column .After about 30 seconds C1 was closed
and the pump was switch off while the column was allowed to drain for 5 minutes. The air
pressure differential across the wet column was measured as a function of the air flow rate for
different water flow rates up to say 5 liters/minute ,noting the apperearance of the column at
each setting.
RESULT and DATA:

PART A: DRY COLUMN

Air Flow rate (1/min) 160 140 120 100 80 60 40 20

Total Pressure Differential 0 3 4 5 9 12 14 15

(mmH20)

PART B: WET COLUMN

AIR FLOW (l/mm) 20 40 60 80 100 120 140 160 180

WATER FLOW
(l/mm)

1.0 7 6 7 7 12 18 22 28 34

2.0 15 15 16 12 16 24 32 42 88

3.0 20 23 21 19 26 35 48 71 -

4.0 5 4 7 15 31 45 80 111 -

5.0 14 12 15 70 70 97 163 - -

6.0 17 14 31 82 - - - - -

7.0 36 28 63 103 - - - - -

8.0 28 54 133 - - - - - -

9.0 78 109 231 - - - - - -

10.0 114 139 - - - - - - -

CALCULATION

DRY COLUMN

LOG AIR 2.20 2.15 2.68 2.00 1.90 1.78 1.60 1.30
FLOW RATE
(1/min)

LOG 0 0.47 0.60 0.69 0.95 1.08 1.15 1.18

PRESSURE
DIFFERENTIAL
(mmH2O)

WET COLUMN

AIR FLOW 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0
(l/mm)

WATER
FLOW(l/mm)

1.301 0.845 1.176 1.301 0.699 1.146 1.230 1.556 1.892 2.057

1.602 0.778 1.176 1.362 0.602 1.079 1.146 1.447 2.037 2.143

1.778 0.845 1.204 1.322 0.845 1.176 1.491 1.799 2.364 F

1.903 0.845 1.079 1.279 1.176 1.845 1.914 2.013 F F

2.00 1.079 1.204 1.415 1.491 1.845 F F F F

2.079 1.255 1.079 1.544 1.653 1.987 F F F F

2.146 1.342 1.380 1.681 1.903 2.212 F F F F

2.204 1.447 1.623 1.851 2.045 F F F F F

2.255 1.531 1.944 F F F F F F F

DISCUSSION

The objective of this experiment is to determine the air pressure differential across the column
as function of air flow rate. This has been visualize in the log-log graph. The air flow rate is adjusted
from 20 L/min until 160 L/min with 20 L/min increment within 2 minutes as the allocated time for each
flow rate to collect the pressure drop for the particular gas flow rate at 1 L/min of water flow rate. The
data is collected until flooding occurs before proceeding to the next water flow rate up to 3 L/min with
increment 1 L/min. The log pressure drop increases as the log air flow rate increases. This also indicates
that as the air flow rate increases, the pressure drop also increases.

From the graph, we can say that the higher the water flow rate the lower the log air flow rate.
This is due to the water flow downwards hinder the air flow upwards, resulting in high pressure drop.
Thus, at high water flow rate, flooding happen rather faster than at the lower one since the resistance
that the water flow give to the air flow is greater. The
same case happens for the theoretical data. Proving that the experimental data shows the same pattern
as theoretical one.

Although for both theory and experimental data, the relationship between pressure drop
and air flow rate is proportional to each other, the experimental pressure drop is larger compared
to the theoretical pressure drop at water flow rate of 1 L/min and 2 L/min. Vary at 3 L/min, the
experimental pressure drop is smaller compared to the theoretical pressure drop. This could be
due to error in controlling the water flowrate from hindering the gas flowrate downwards at the
bottom of the gas absorption column.

The flooding occurrence at water flow rate of 1 L/min according to the theory should
have been at 160 L/min air flow rate, however during the experiment the flooding occurs at 180L/min.
As for water flow rate of 2 L/min and 3L/min, theoretical flooding occurs at120 L/min
and 100 L/min however the experimental flooding happens at 160 L/min and 120 L/min,
respectively. This resulting in error for the experiment. The reason of the error could be due to
human error. During the experiment, the students need to control the water from
exceeding the entrance of the gas flow rate at the bottom of the column. However, at any time
the water level at the bottom could be too high which hinder the gas flow thus resulting in the late
flooding flow rate.

The error could also happen due to the parallax error during the adjustment of the next flow
rate as if we did not read the marking scale at eye level where the eyes should be perpendicular to the
marking scale. Maybe we mistakenly adjusted from 1L/min to 2L/min be the 1.9L/min. this will
affecting the flooding flow rate. Next, maybe the equipment used is not maintain which is resulted in
different value at the marking scale of the flow rate.
Besides, the theoretical data and the experimental data vary could also due to the
differences in packing tower such as the packings within the tower.

Although error occurs, the experiment is still considered

success since the errors is not too big and the distance of the respective graph at the theory and
experimental data is not far.Based on the experiment, we could also observe the fact that the packed to
wer used inthe experiment is working efficiently at lower liquid flow rate since flooding occurs at ver
y highgas flow rate. This allow the contacting time between the gas and liquid to be lengthen and thus
maximize the absorption rate. However, at high liquid flow rate, flooding is quick to happenedeven at
low gas flow rate. This shorten the contact time between gas and liquid which thenminimize the absor
ption rate.

CONCLUSION

In conclusion, we already achieve our objective for this experiment which is to determine the air
pressure differential across the column as function of air flow rate. We also could see the flooding
happen. The pressure drop increase as the air flow rate increases. So, the experiment is successfully
done.

REFERENCES

Fazsroul (n.d). CPE533 gas absorption full lab report. Process engineering laboratory 2.

Retrieved June 19, 2020 from https://www.scribd.com/document/344601846/CPE533-Gas-

Absorption-Full-Lab-Report

Tarhizi. I. ( 2015). Gas absorption. Retrieved June 19, 2020 from

https://www.academia.edu/18917634/Gas_absorption
QUESTION

DRY COLUMN

1. Plot the total pressure differential as a function of air flow rate on log-log graph
paper and establish the relationship between these variables.

Total Pressure Differential vs Air Flow Rate

16
Total Pressure Differential (mmH2O)

14

12

10

0
20 40 60 80 100 120 140 160
Air Flow Rate (l/mm)

2. Compare standard diagram for total pressure differential vs log air flow rate
with the experimental one. Discuss any difference between them.

LOG PRESSURE DIFFERENTIAL vs LOG AIR FLOWRATE

1.4
LOG PRESSURE DIFFERENTIAL

1.2
1
(mmH20)

0.8
0.6
0.4
0.2
0
1.3 1.6 1.78 1.9 2 2.08 2.15 2.2
LOG AIR FLOWRATE (l/mm)

3. Is there any loading and flooding point exist in dry packed column? Give reason
why.
 No. Loading and flooding point does not exist as the gas pressure drop is very low.
The entire column is not filled with liquid and gas. So the gas now has no bubble
through the liquid in the packing voids.

WET COLUMN

1. Plot the total pressure differential should be plotted as a function of air flow rate
on log-log graph paper for each water flow rate.

PRESSURE DROP vs AIR FLOW RATE

250
PRESSURE DIFFERENT (mmH2O)

200

150

100

50

0
1 2 3 4 5 6 7 8 9 10
AIR FLOW RATE (l/mm)

20 40 60 80 100 120 140 160 180

2. Compare standard diagram for total pressure differential vs log air flow rate
with the experimental one. Discuss any difference between them.

Log total pressure vs Log total air flow rate

2.5
LOG TOTAL PRESSURE (mmH2O)

1.5

0.5

0
1.301 1.602 1.778 1.903 2 2.079 2.146 2.204 2.255
LOG TOTAL AIR FLOW (l/mm)

1 2 3 4 5 6 7 8 9 10

3. Is there any loading and flooding point exist in wet packed column? Give reason
why.
Yes, loading and flooding point will exist in wet packed column. The gas pressure
drop is now very high. At this point the entire column is filled liquid and the gas now
has to bubble through the liquid in the packing voids. At higher liquid rate, the
loading and flooding points occur at lower gas pressure drop.
 FACULTY OF APPLIED SCIENCE
BACHELOR OF APPLIED CHEMISTRY (Hons.)
CMT 450 (UNIT OPERATION)
EXPERIMENT 6 : INTRODUCTION TO HAMMER MILL

BIL STUDENT NAME MATRC NUMBER

01. ANNAMIRAH ULON AZMI 2019294994

02. ANIS AMIRA BINTI BADROL HISHAM 2019685518

03. OMMY MADINA BINTI ABDUL HALIM 2019295426

LECTURE’S NAME : MOHD FAUZI BIN ABDULLAH

INTRODUCTION

Hammer mill is a machine used to shred material into fine particles (size reduction).
They have many sorts of applications in many industries, including milling grain, ethanol
plants (corn), grinding used shipping pallets for mulch, sawmills, size reduction of trim scrap
and planer shavings into boiler fuel or mulch, a farm machine (which mills grain into coarse
flour to be fed to livestock).

The principle of hammer mill is straightforward. A hammer mill is a steel drum

containing a vertical or horizontal rotating shaft or drum on which hammers are mounted.
The hammers are free to swing on the ends of the cross, or fixed to the central rotor. The
rotor is spun at a high speed inside the drum while material is fed into a feed hopper. The
material is impacted by the hammer bars and is thereby shredded and expelled through
screens in the drum of a selected size.

Hammer mills reduce the particle size of materials by impacting a slow moving target,
such as a cereal grain, with a rapidly moving hammer. The target has low kinetic energy,
whereas the hammer has high kinetic energy. The transfer of energy resulting from the
collision fractures the grain into many pieces.

Since impact is the primary force used in a Hammer mill to reduce the size of the
particles, so, whatever increases the chance of a collision between a hammer and a target,
increases the magnitude of the collision, would be an enhancer to particle size reduction.

Particles produced using a hammer mill are spherical in shape with a polished surface.
A wide variation in the particle size distribution would occur where there will be some large-
sized and many small-sized particles.

In the feed processing process there may be a number of ingredients that require some
form of processing. These include coarse cereal grains, corn that requires particle size
reduction which will improve the ingredient performance & increase the nutritive value. One
of the methods to achieve this particle size reduction is using hammer-mills.

There are some advantages of using hammer mill which are being to produce a wide
range of particle sizes, suitable for friable material and fiber, easy to use, lower cost when
compared with a roller mill and easy to maintain.
OBJECTIVES

1. To observe the effect of screen size on the finishing product after grinding process.
2. To determine the percentage of size reduction before and after grinding process.

APPARATUS AND MATERIALS

Hammer mills, beaker, ground nuts

PROCEDURE

1. The Hammer Mill machine was checked in the right condition..

2. Hammer Mill was made sure already equipped with mesh screen (starting with coarse
size first).
3. The switch was turned ‘ON’.
4. Material (groundnuts) is fed into mill’s chamber typically by gravity. All the
groundnuts was grinded for 5 minutes.
5. All the grinded groundnuts was collected using beaker 500 ml at the end of discharge
chute.
6. Any grinded groundnuts which stick on the surface of the equipment was made sure
are not left. Please collect all of them was collected and it was weighed using weigh
b7alance.
7. All the parts was cleaned with air blower before starting new experiment.
8. Step 1 -7 was repeated for other screen size (continue with medium and fine.
9. Do not throw all the groundnuts. These groundnuts will be used in experiment 9
(Filter
Press Machine)
RESULT AND DATA :

Weight of grind product

Percent of size reduction = X 100
Weight of raw material

Size of screen Mass of beaker (g) Mass of beaker + Percent size

groundnuts (g) reduction (%)

Coarse 211.59 297.27 85.48

Medium 211.59 285.80 74.04

Fine 211.59 276.91 65.17

Table 1 : Hammer Mill

Mass of raw material = 100.23 g

CALCULATION :
Size of Screen : Coarse

Percent of size reduction (%) = 297.27 - 211.59

X 100
100.23

= 85.48 %

Size of Screen : Medium

Percent of size reduction (%) = 285.80 - 211.59

X 100
100.23

= 74.04 %

Size of Screen : Fine

Percent of size reduction (%) = 276.91 - 211.59

X 100
100.23

= 65.17 %
DISCUSSION:
For this experiment, we need to observe the effect of screen size on the finishing
product after grinding process. An also to determine the percentage of size reduction before
and after grinding process. We will use groundnuts to be grind into Hammer Mill machine.
For Hammer Mill machine, we will use different coarse size as we want the perfect screen
size at the finishing part. For the first step, we will start with large mesh screen. After that, we
will follow with intermediate and smaller size of mesh screen.

The small mesh screen has the least mass production while the large mesh screen has
the highest mass production between the three of the mesh screens. This may be due to the
size of the nuts after being grinded by the hammer mills. The bigger the size of particles, the
higher the mass of particles. When coarse mesh screen was used, it reduced the size of the
nuts but not into fine powder. When the smaller mesh screen was used, it reduced the size of
the nuts into powder.

After we done grinded the nuts, we need to weight them because we need to find the
percent of reduction. It will take all value of weight nuts from each size of screen. We will
use this formula as we need to find the percentage of it ;

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑔𝑟𝑖𝑛𝑑 𝑝𝑟𝑜𝑑𝑢𝑐𝑡

𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑓 𝑠𝑖𝑧𝑒 𝑟𝑒𝑑𝑢𝑐𝑡𝑖𝑜𝑛 (%) = 𝑥 100%
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑟𝑎𝑤 𝑚𝑎𝑡𝑒𝑟𝑖𝑎𝑙

From the calculation, the percentage of production by using small mesh screen is the
lowest but the product is the fine product. The percentage of production by using coarse mesh
screen is the highest but the product is not really fine or not in powder form compared to the
product by using small mesh screen. So, the percentage for coarse screen is 85.48%. For
medium screen, the percentage of size reduction is 74.04%. While for fine screen, the percent
of size reduction is 65.17%.

For this experiment, there have a few steps that need to be alert. First, make sure do
not left any grinded nuts which stick on the surface of the Hammer Mill. It must be collected
and weight together as the final mass. Second, clean all part of Hammer Mill before starts the
next step. Lastly, make sure grind the nut for 5 minutes.
CONCLUSION:
The operation of hammer mills was studied and the percentage production of crushing
by using different types of metal screens was obtained. It is recommended that by using
different types screen size, shaft speed or hammer configuration can alter the size of the
product that we wanted. As we do this experiment, we can find the percentage of size
reduction which is from nuts that we grinded it before. So, the value are 85.48%, 74.04% and
65.17%.

REFERENCES:

1. https://www.ukessays.com/essays/engineering/introduction-to-what-is-a-hammer-
mill-engineering-essay.php
2. https://www.coursehero.com/file/22656728/265496810-Lab-Report-Operation-Unit-
Experiment-7/
QUESTION :
1.Discuss the importance of size reduction in unit operation application ?

Size reduction is a process of reducing large solid unit masses into small unit masses which
coarse particle or fine particle. The important of size reduction in unit operation application are
easy to handling ,increase in surface area per unit volume and separation entrapped
components. Hammer mills produce a fairly inhomogeneous product, with brittle materials
making up a higher portion of the fines than ductile materials.

2.What type of common solid broken in Hammer Mill equipment and discuss the application
of Hammer Mill in our life?

The purpose of hammer mill is to shred or crush aggregate material into smaller pieces by
the repeated blows of little hammers. The common application of Hammer Mills in our life
are grinding grain into flour for the livestock, creating fruit juice production ,recycling of
paper (shredding).

3. From you opinion (support with the studies ) is fine product is the best one ? Give your
reason?

Yes the fine product is the best one because the sized pieces pass through the bottom while
any large particles remain until they are broken down small enough to pass through the
screen. Hammer mills are ideal for most situations and can have narrow particle size
distributions along with relatively fine grinds (down to ~1.5mm).