LAB MANUAL

CMT450
(UNIT OPERATION)

FACULTY OF APPLIED SCIENCES

BACHELOR OF APPLIED CHEMISTRY (HONS)

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 EXPERIMENT 1 : SIMPLE EQUILIBRIUM DISTILLATION

Objective :

To illustrate the use of distillation for separating a mixture of two volatile

liquid with different
boiling point.

Chemicals / Apparatus :

Round bottom flask

Distilling head
Heating mantle
Thermometer with adapter
Receiving flask
Retort stand with clamp
Condenser
Vacuum adapter
Chemical : Unknown mixture [ Mixture A]

Procedure :

1. Arrange the apparatus according to the diagram drawn below.

2. Put the unknown mixture [Mixture A] into the round bottom flask until it
reaches about
half of the flask.
3. Heat the mixture to boil by turning on the heating mantle until the first
drop of distillate
produce.
4. Record the temperature of the first drop of the distillate.
5. Control the heating mantle in order to maintain the temperature of the first
distillate.
6. Continue step 5 until there was no more drop of distillate produce.
7. Increase the temperature until another drop of distillate produce.
8. Record the second temperature of distillate.
9. Record all reading into a table.

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Results :

Distillate Temperature (0C) Expected

Compound
First
Second

QUESTION

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

2. Suggest what type of unknown mixture [Mixture A]? Homogenous mixture or
heterogeneous mixture? Why?
3. Suggest the expected compound for first distillate and second distillate and
why you
choose that respective compound?
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?
5. Explain the precaution steps in conducting this experiment.

Figure 1 : Distillation Column Setup In Laboratory

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 EXPERIMENT 2 : SIMPLE BATCH DISTILLATION

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.

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.

Procedure :

A. Distillation

1. Prepare an acetic acid-water solution 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. Put the flask on a heating mantel. Using apparatus supplied in the
distillation kit, set the
solution up for distillation as demonstrated by your instructor. Work gently
since the
glassware is quite fragile and rather expensive to replace.
3. Gently turn on the tap to let cooling water into the condenser. Make sure
that the hose
for outlet water is inside the sink. Adjust the inlet water so that the
cooling water enters

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 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. Weigh a clean and dry 150 ml beaker and position in beneath the distillate
outlet spout
to collect the distillate.
5. Check and make sure all connections fit snugly before the distillation process
begin.
Start the distillation 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, turn
off the hot
plate.
7. Wait until the plate cools down and let all the vapors condense before
disassemble the
distillation equipment. While disassembling the glassware, you should be
careful not to
spill any distillate that might be trapped in between the connections. You
should collect
this trapped distillate and add up to your collecting beaker.

B. Titration of distillate

1. Reweigh the collecting beaker including its content.

2. Pour all distillate from the beaker into a 250-ml volumetric flask. Wash onto
the flask
the remaining distillate left on the beaker-wall with distillated water.
3. Fill half of the flask with distilled water. Put its cap and shake the flask
gently a few
times. Then fill up flask up to the mark with distilled water. Put the cap on
again and
turn the flask upside down a few times so that the solution is well-mixed.
4. Pour about 100 ml of the diluted solution into a clean beaker. Using a pipette,
take 20
ml or 25 ml of the solution each into 3 separate clean conical flasks. Then
squeeze 2
drops of phenolphthalein indicator into each flask.
5. Fill a burette with 2.0M NaOH solution and titrate the content of each flask
with NaOH

C. Titration of liquid residue

1. Repeat steps B1 to B5 for the liquid residue.

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RESULTS

A. Distillation
RESIDUE DISTILLATE
Mass of empty Mass of Mass of Mass of
Mass of
Mass of
Erlenmeyer Erlenmeyer flask residue beaker +
distillate
empty beaker
flask + residue distillate
(g)
(g) (g) (g) (g)
(g)

B. Titration of Distillate
Conical flask 1 2
3
Initial reading of NaOH (mL)

Final reading of NaOH (mL)

Volume of NaOH used (mL)

C. Titration of Liquid Residue

Conical flask 1 2
3
Initial reading of NaOH (mL)

Final reading of NaOH (mL)

Volume of NaOH used (mL)

QUESTION

1. Calculate the molar composition of feed solution (Given ρCH3COOH = 1.048

g/mL and ρH2O =
1.000 g/mL)
2. From titration data, determine the composition of the distillate
3. From titration data, determine the composition of the residual liquid
4. Using Raleigh equation, calculate the theoretical composition of
distillate and residual
liquid. Compare the theoretical values with the experimental values.
(Equilibrium data
for water-acetic acid system at 1 atm is provided in Appendix 1)
5. What is the advantages of batch distillation compare with simple
equilibrium
distillation?

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Appendix 1: Equilibrium data for water-acetic acid system at 1 atm

x y
0 0
0.1881 0.3063
0.3084 0.4487
0.4498 0.5973
0.5195 0.658
0.5824 0.7112
0.675 0.7797
0.7951 0.8671
0.8556 0.9042
0.8787 0.9185
0.9134 0.9409
0.9578 0.9708
1 1

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 EXPERIMENT 3 : TERNARY PHASE DIAGRAM (LIQUID – LIQUID EXTRACTION)

Objective :

The main objectives of this experiment are to determine 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. Acetic acid is the solute.

Procedure :

A. To obtain a binodal solubility curve

1. Complete Table 1 in the result section by calculating volumes of acetic acid

and
chloroform needed to form 10 g of two-component solutions with the indicated
compositions. You should complete the calculations before you to come to the
laboratory.
2. In a conical flask, prepare 10 g of two-component solution that is made of
acetic acid
and chloroform using the volumes that you have pre-calculated in step 1.
3. Put distilled water inside a burette, take the initial burette reading and
slowly titrate the
mixture that you have prepared in step 2 with water until the solution
becomes turbid
(cloudy). While titrating, do not forget to gently shake the mixture in order
to mix them
well.
4. Stop the titration when the resulting solution in the flask turns turbid.
Take the final
burette reading. If you wait and allow sufficient time for equilibrium to
establish, you
should notice the intermediate mixture will separate into two distinct heavy
and light
phases. Hold the flask against the light and try to look for the phases from
the bottom of
flask if you cannot see the phases clearly. It is possible that you might not
be able to see
the phases especially at very low concentrations.

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Result and Data :

A: Data for a bimodal solubility curve

Table 1 : Result for titration of 10g acetic acid-chloroform mixture with water.

Mass % of Mass of Volume of Mass of Volume of Volume of

Mass of
acetic acid acetic acid acetic acid chloroform chloroform water
water
(g) (ml) (g) (ml) (ml)
(g)
90 9
80 8
70 7
60 6
50 5
40 4
30 3
20 2
10 1

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 1M NaOH.

Mass (g) Volume

(ml) of 1.0M
NaOH to
titrate
Chloroform Acetic acid Water Heavy Light Heavy
Light
phase phase phase
phase
10 6 6
8 6 6
6 4 10

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B. To obtain a tie lines and plait point

1. Using a combination in Table 2, place a three-component mixture in a

separating funnel.
2. Shake it well (gently) for a while. Then point the tip of the funnel away
from yourself
and your friends, and open the vent stopcock to release any build-up vapor
pressure. Do
not inhale the vapor.
3. Continue shaking and venting for about 5 minutes. Make sure the stopcock is
closed
before shaking.
4. Place the separating funnel on its o-ring support and leave it for 3 minutes
to allow
heavy and light phases to separate.
5. Weight 2 dry conical flasks and drain each phase into it. Then reweigh each
flask.
6. Titrate each phase with 1.0 M NaOH solution using phenolphthalein as
indicator. The
end point is when the solution changes color.
7. Repeat the procedures above for other combination in Table 2.

Precaution :

1. Be careful not to inhale corrosive acetic acid vapor.

2. Be extra careful not to let your skin come in contact with chloroform since
chloroform is
suspected cancer causing agent. If you accidentally spill chloroform on your
skin, quickly
wash it with a lot of amount running water.
3. Vent the separating funnel frequently during the extraction in order to avoid
the
building up of vapor pressure which will blow out the stopcock and perhaps
also the
dangerous content. Point the tip of the separating funnel away from yourself
and others
when releasing the pressure.

QUESTION
 From table 1, obtain the bimodal solubility curve and calculate the mass fraction
for each
component in the turbid mixture.
 Using the mass fractions, construct the bimodal solubility curve (ternary phase
diagram) for
the three component mixture by means of right angle triangular diagram.
 Write a chemical equation for the titration. The equation enables you to
calculate the mass
of acetic acid present in each phase.
 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.

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 EXPERIMENT 4 : SINGLE STAGE EXTRACTION (LIQUID-LIQUID EXTRACTION)

Objective :

In this experiment students will perform a single-stage extraction to separate

acetic acid from
its solution in chloroform using water as an extraction solvent. The acid contents
in the
raffinate and extract phases will be determined by titration and its results are
compared to the
theoretical result.

Precautions:

1. Be careful not to inhale corrosive acetic acid vapor.

2. Be extra careful not to let your skin come in contact with chloroform since
chloroform is
suspected cancer causing agent. If you accidentally spill chloroform on your
skin, quickly
wash it copious amount of running water.
3. Vent the separating funnel frequently during the extraction in order to avoid
the
building up of vapor pressure which will blow out the stopcock and perhaps
also the
dangerous content. Point the tip of the separating funnel away from yourself
and others
when releasing the pressure.

Procedure :

1. Prepare a binary acetic acid-chloroform solution by adding 4 ml acetic acid

to 5 ml
chloroform in separating funnel. CAUTION: This might generate a lot of vapor.
To avoid
sudden pressure burst, do not stopper the funnel.
2. With the funnel mouth still open, gently swirl the mixture to mix it well
into a
homogenous binary solution. This is your feed solution.
3. Now extract the acid from binary solution using equal mass of an extraction
solvent,
water. Measure 10 ml distilled water and pour it into the funnel. CAUTION:
This mixture
might generate a lot of vapor.
4. Put on your hand glove. With the stopper on, gently shake the funnel and then
open its
stopcock to release any pressure build-up. Continue shaking and venting for
about 5
minutes.
5. Put the funnel on the o-ring support and let its content settle into phases.
You should
wait about 5 – 10 minutes to allow the heavy and light phases reach their
equilibrium.
6. Weigh two clean empty conical flasks and then transfer each phases into each
flask.
Reweigh the beaker.

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 7. Put about two drops of phenolphthalein into each flask and titrate them using
2.0 M
NaOH (aq). The endpoint is when the solution turns color.

Results and data :

Using the ternary phase equilibrium curve obtained in the previous experiment
provided in
Appendix 2, determine the theoretical mass fractions of acid in the raffinate and
extract phases
and compare to those obtained by this experiment.

QUESTION
1. Briefly explain what you do to your data in order to obtain your results?
2. Discuss your experimental result by comparing to your theoretical result. If
they differ,
how much?
3. Why do you think they differ? Include all contributing errors and how these
errors effect
your result.
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
5. Explain when liquid-liquid extraction method is suitable to apply compare with
distillation method.

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Appendix 2: Ternary Diagram of Acetic Acid-Chloroform-Water at 1atm

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 EXPERIMENT 5 : AIR PRESSURE DIFFERENTIAL ACROSS DRY AND WET COLUMN
(GAS ABSORPTION PACKED COLUMN)

Objective :

To determine the air pressure differential across the column as a function of air
flow rate.

Equipment Set-up:

No additional equipment is required for this exercise.

Procedure A (Dry Column):

1. The column must be dried by passing the maximum air flow until all evidence
of moisture in the
packing has disappeared.
2. Set valves V1, V2 and V3 as shown in the diagram so that differential
pressures in the top and
bottom sections of the column are indicated on the two water manometers.
3. Take manometer readings of pressure differential across the column for a
range of air flow rates.
The total pressure differential is the sum of the differential across the
top and bottom halves of
the column, i.e. add the reading from the two water manometers.
*Total pressure different = manometer top + manometer bottom

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Results and data :

AIR FLOW RATE (1/min) 160 140 120 100 80 60

40 20

TOTAL PRESSURE DIFFERENTIAL

(mmH20)

QUESTION

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.
2. Compare standard diagram for total pressure differential vs log air flow rate
with the
experimental one. Discuss any difference between them.
3. Is there any loading and flooding point exist in dry packed column? Give
reason why.

Procedure B (Wet Column):

1. Fill the sump to three-quarters full with tap water. Set valves V1, V2 and V3
as shown on
the diagram so that differential pressures in the top and bottom sections of
the column
are indicated on the two water manometer.
2. Switch on the water pump and set C1 to give a flow rate of say 3
liters/minute down the
column.
3. After about 30 seconds close C1, switch off the pump and allow the column to
drain for
5 minutes.
4. Measure the air pressure differential across the wet column as a function of
the air flow
rate.
5. Measure the air pressure differential across the column as a function of the
air flow rate
for different water flow rates up to say 5 liters/minute, noting the
appearance of the
column at each setting.

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 Result and data:

Pressure differential (mm water)

Air flow
(l/min)
Water 20 40 60 80 100 120 140
160 180
flow (l/min)

1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0

The range of possible air flow rates will decrease with increasing water flow
rate due to onset
of ‘flooding’ of the column, which should be noted.

QUESTION

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.
2. Compare standard diagram for total pressure differential vs log air flow
rate with the
experimental one. Discuss any difference between them.
3. Is there any loading and flooding point exist in dry packed column? Give
reason why.

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 EXPERIMENT 6 : INTRODUCTION TO HAMMER MILL

Objective :

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

Procedure :

1. Please check the Hammer Mill machine is in right condition.

2. Make sure Hammer Mill already equipped with mesh screen (starting with coarse
size
first).
3. Turn the switch ‘ON’.
4. Material (groundnuts) is fed into mill’s chamber typically by gravity. Grind
all the
groundnuts for 5 minutes.
5. Collect all the grinded groundnuts using beaker 500 ml at the end of
discharge chute.
6. Make sure do not left any grinded groundnuts which stick on the surface of
the
equipment. Please collect all of them and weight using weigh balance.
7. Clean all the parts with air blower before starting new experiment.
8. Repeat step 1 -7 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 :

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

Size of screen Mass of beaker Mass of beaker + Percent

size reduction
(g) groundnuts (g)
(%)
Coarse
Medium
Fine

QUESTION

1. Discuss the importance of size reduction in unit operation application.

2. What type of common solid broken in Hammer Mill equipment and discuss
application
of Hammer Mill equipment in our life.
3. From your opinion (support with other studies), is fine product is the best
one? Give
your reason.

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