ENGR 265

Chemical Engineering Laboratory

Projects
Lancaster University
15/03/2019

Emily Smith
Maximilian Smith

Table of Contents

1
Experiment Page
Number
General Summary 3
Practical 1 (P1) : Determination of Distribution Coefficient 4
Practical 2 (P2) : Measurement of the liquid diffusion 8
coefficient
Practical 3 (P3): Measurement of the pressure differential 14
and flooding in a gas-liquid extraction column

Practical 4 (P4): Mass balance and determination of the 19

mass transfer coefficient for liquid-liquid extraction
process

Practical 5 (P5): Distillation 24

Practical 6 (P6): Modelling of Unit Operations 29
Practical 7 (P7) : Chemical Reactors 31
Practical 8 (P8) : Particle Formation 36
Practical 9 (P9) : Filtration 40
References 46

2
General Summary

The main aim of practical 1 was to determine the distribution coefficient

between 2 phases. The expectation was that the concentration in the
extract phase is greater than the raffinate phase, which the results agreed
with because K was greater than 1, with a value of 5.27.

Practical 2’s main aim was to determine the diffusion coefficient of

Sodium Hydroxide at various temperatures. The expectation was that the
higher the diffusivity and temperature, the higher the mass transfer would
be, however the results showed that as temperature increases this isn’t
always the case, as the optimum diffusivity of 0.459m2/s occurred at
30˚C.

The main aim of practical 3 was to analyse the pressure differential as air
and water flow rate varied and observe when the column flooded.

In Practical 4 , the aim was to measure the mass transfer co efficient.

Using the results from the experiment, only an equilibrium line could be
constructed, which contradicted the original hypothesis that both an
equilibrium and operating line could be drawn.

The aim of practical 5 was to calculate the efficiency of the distillation

column. This required equilibrium data obtained in practical 6 to work out
the number of trays needed in the column. To create the operating line,
refractive indexes were used to find the compositions of the top and
bottom of the column, which gave 8 trays and an efficiency of 43.5%.

Practical 6 required ASPEN plus to be used to run a model of ethanol and

water under two different equations of state, ideal and UNIFAC.

The objective of practical 7 was to find the reaction rate constant between
sodium hydroxide and ethyl acetate at different temperatures. To find
this, initial and final concentrations were found using a calibration curve,
which gave results that matched the theory.

Practical 8 was conducted as a Full factorial, to find out which conditions

gave the smallest particle size. Conductivity and PSD results enabled this
to be calculated.

The aim of practical 9 was to work out the experimental specific cake
resistance and compare it to the theoretical value. The theoretical value
from the PSD gave r =1.557∗10 14 and the experimental value was
r =1.095∗1014 . These results were larger than expected, but like each other
which was the desired outcome.

3
 Practical 1 (P1) : Determination of Distribution Coefficient

Aim
To find out the distribution co-efficient for the system, which is made up of
an organic solvent (leksol), water and propionic acid.

Introduction
It is a liquid-liquid extraction with two immiscible liquids. The solvent in
this experiment is water and the solution is propionic acid and the two are
mixed together and then separated into an extract phase and a raffinate
phase. The extract phase will be made up of water and the propionic acid
and the raffinate phase will be comprised of organic solvent with traces of
the propionic acid. This is shown more clearly below in figure Figure 1.1.
The reaction for the experiment is shown below between propionic acid
and sodium hydroxide.

CH 3 CH 2 COOH + NaOH →CH 3 CH 2 COONa+ H 2 O

The stoichiometric ratio is 1:1 so the moles

of the propionic acid in the water phase will
be the same as the moles of NaOH.

Liquid-liquid extraction is a mass transfer

operation in which the two liquids are in
contact in order to achieve the transfer of the solute from the feed to the
solvent.

Liquid-liquid equilibrium and the distribution coefficients calculated from

them are crucial to the design of all extraction processes.

Figure 1.1/ the separation

of the 2 phases K can be found using equation 1.1 shown below, where
K is the distribution coefficient.

(Equation 1.1)

The concentration of the solute in the extract phase, Cy, in this

experiment can be found by titrating the propionic acid in water against
Sodium Hydroxide. The concentration of a solute in the raffinate phase,
Cx, can be calculated as a difference as the assumption is that the two
phases are immiscible.

4
 Experimental Section

i) Materials and Equipment

- 250ml Measuring cylinder
- 250ml Separating funnel
- Pipettes with rubber bulb
- Sodium Hydroxide Solution (0.1M)
- Phenolphthalein
- Propionic acid
- Leksol
- De-mineralised water

ii) Experimental Procedure

In a separating funnel, mix 50ml of organic solvent (Leksol) and 50ml of
water together. Then to measure the propionic acid, measure the syringe
before putting the acid in and after as well, to ensure that the actual
volume and weight are achieved. When this is done add 0.1ml of propionic
acid to the mixing funnel.
Shake the funnel and then leave it for 5 minutes to separate. After this
remove the lower organic phase layer and dispose of it in the waste
bucket. Take 10ml from the remaining water layer and titrate it against
0.1M NaOH solution. To ensure there are no anomalies two titres are
taken.
When this is done, repeat the same procedure 4 more times, with
different masses of propionic acid, 0.2ml, 0.3ml, 0.4ml and 0.5ml.

Results and Discussion

Obtained results are presented below in Table 2.1, showing how the
volume of the NaOH titre increases with an increase in mass of propionic
acid.

Initial Mass of propionic acid added (g) Volume of NaOH spent for neutralization Vol of
propionic acid (mL) organic
added (mL) phase (mL)
Measurement Measurement Change in Measurement Measurement Average
1 2 mass 1 2 Titre
0.1 2.209 2.337 0.128 2.7 2.5 2.6 10
0.2 2.212 2.438 0.226 4.6 4.9 4.75 10
0.3 2.228 2.565 0.337 7.3 7.5 7.4 10
0.4 2.233 2.647 0.414 9.1 8.8 8.95 10
0.5 2.25 2.769 0.519 11.8 12.1 11.95 10

In order to find the concentrations, the moles need to be found, as

Moles
concentration can be given as . The molar mass of NaOH is 40g/mol
Volume
and the molar mass of propionic acid is 74g/mol. In order to find out the

5
 mass
moles, use the formula moles= . The results for these calculations
molar mass
using the change in mass are given in the table below.

Table 2.2 below shows the results of calculations to find the moles and
therefore the concentration of the two phases

Moles of acid Moles of Moles of acid Concentration Concentration

added NaOH in organic in aqueous in organic
(moles) (moles) phase (moles) phase (mol/L) phase (mol/L)
0.00172973 0.00026 0.00146973 0.0052 0.029394595
0.003054054 0.000475 0.002579054 0.0095 0.051581081
0.004554054 0.00074 0.003814054 0.0148 0.076281081
0.005594595 0.000895 0.004699595 0.0179 0.093991892
0.007013514 0.001195 0.005818514 0.0239 0.11637027

Plot of Cx vs Cy
Concentration in organic phase (mol/L)

0.14

0.12
f(x) = 4.7 x + 0.01
0.1

0.08

0.06

0.04

0.02

0
0 0.01 0.01 0.02 0.02 0.03 0.03
Concentration in aqueous phase (mol/L)

Graph 1.1 below which shows Cx plotted against Cy

Cy
From equation 1.1, K= the values of K can be found out as:
Cx

Initial propionic acid added (mL) Value of K

0.1 5.652806731
0.2 5.429587474
0.3 5.154127095

6
 0.4 5.250943687
0.5 4.869048954

This gives an average value of 5.271302788 for K. This is similar to the

gradient of the line in graph 1.1 shown above, which makes sense as the
trendline dips slightly below the actual line, so the gradient worked out is
slightly lower than the real value.

1. C Y =K C X can be valid for this experiment because earlier on it’s

stated that “at low concentrations, the distribution coefficient is
dependent on the concentration and thus C Y =K C X ”. The
concentrations obtained are low and therefore it’s valid for this
experiment. This means that the K value obtained is positive which
means there are more particles in the organic phase than in the
aqueous phase, meaning that it’s attracted to the organic phase, as
it’s polar.

2. The values obtained in this experiment are higher than those

obtained by (Braz. J. Chem. Eng. 21 (2004) 647) and a lot more
uniform. Their results however are for three different materials,
whereas in this experiment the K value for only one is being tested,
which may explain why they’re more uniform.

Conclusion
The aim of the experiment was to find out the distribution coefficient for
the system, the average value of which was 5.27.
The values of K obtained in this experiment are very similar, at
approximately 5 for each one, and from the graph the relationship
between Cx and Cy is linear, as it’s a straight line through the origin.
Ensuring that the correct amount of the organic phase was used during
the experiment was difficult and could be a limitation, as it was initially
difficult to distinguish between the two phases. However, after 10-15, they
were immiscible and were easier to tell apart when discarding of the
aqueous phase.

7
 Practical 2 (P2) : Measurement of the liquid diffusion coefficient

Aim
To work out the diffusion coefficient of a 1M NaCl solution in different
temperatures in distilled water and find the diffusion coefficient
dependency from the temperature.

Introduction
Mass transfer occurs when there is a concentration gradient of the
component that is diffusing. Therefore, mass transfer partially depends on
the diffusivity of the fluids involved in the experiment. Fluid flow also
depends partially on the diffusivity, making it a very important aspect of
experiments and design of plants. The reason that the experiment is
being conducted at several different temperatures is because
temperature is one of the main things that affects the diffusion coefficient.
The rate of diffusion of salt correlates to the accumulation rate in the
vessel, which is shown in the equation below.

V dk πd 2 M
=D AB N
C M dt 4 x

Considering the flux between the bottom and top of the capillaries:

C A 2−C A 1
N A ¿−D AB
x

Combining these 2 equations:

(Utar.edu.my,
2019)

8
 Figure 2.1/ The schematic for the liquid diffusion
equipment

Experimental
Section
i) Materials and Equipment
- Liquid diffusion coefficient apparatus
- 1M NaCl Solution
- 1L Deionised Water
- Conductivity Probe

ii) Experimental Procedure

Fill the diffusion cell with 1M NaCl and the vessel with room
temperature water, then turn on the conductivity meter and click
record. Straight after the recording has begun, put the diffusion cell
into the vessel and start the recording on the Armfield software.
Then turn on the stirrer gently and keep recording until the values for
conductivity begin to stabilise. Once they have stabilised, stop the
recording and then save and clear the data.
Change the temperature to 30˚C, which is done by warming up the
distilled water in a water bath and repeat the previous paragraph for
this new temperature. After this do the same thing for 35˚C, which is
again done using the water bath.
While these experiments are running, create a calibration curve for the
three temperatures using NaCl at 0.025, 0.05, 0.075 and 0.1M and
noting down the conductivities for each of them.

Results and Discussion

Obtained results are presented below in Table 2.1, showing how the
conductivity of the NaCl increases with an increase in concentration and
temperature.
Concentration (M) Temperature (˚C) Conductivity (mS)
22.30 2.59
0.025 30 3.25
35 3.63
22.30 5.02
0.05 30 6.27
35 7.10

9
 22.30 7.56
0.075 30 9.42
35 10.6
22.30 9.41
0.1 30 11.53
35 13.17

Calibration Curve
0.12

0.1
f(x) =f(x)
10.27
f(x) x= 7.32
= 8.3 x x
0.08
Concentration (M)

0.06

0.04

0.02

0
0 0 0.01 0.01 0.01 0.01 0.01

Conductivity (mS)
22.3 degrees celcius Linear (22.3 degrees celcius)
30 degrees celcius Linear (30 degrees celcius)
35 degrees celcius Linear (35 degrees celcius)
The calibration curve from the conductivity values in the table above are
shown below in graph 2.1

The graph shows that the higher the temperature, the higher the
conductivity will be for a given concentration.

10
 f(x) = NaN ln(x) NaN
Room Temperature
12
10
conductivity (mS/cm)

8
6
4
2
0
00:00 02:52 05:45 08:38 11:31 14:24 17:16 20:09
time (s)

Graph 2.2 below shows the effects of conductivity against time at room
temperature, showing that the conductivity clearly increases with time in
this experiment.

30 Degrees
0.25
conductivity (mS/cm)

0.2

0.15

0.1

0.05

0
00:00 00:43 01:26 02:09 02:52 03:36 04:19 05:02 05:45
time (s)

Graph 2.3 below shows the effects of conductivity against time at 30˚C,
with the conductivity increasing with time

35 Degrees
0.25
conductivity (mS/cm)

0.2

0.15

0.1

0.05

0
00:00 01:26 02:52 04:19 05:45 07:12 08:38
time (s)

Graph 2.4 showing the effects of conductivity against time at 35˚C, with
conductivity increasing with time

11
dk
is the gradient of each of the conductivity curves above, the gradient
dt
for each temperature will be calculated below, in order to find 3 different
values for D AB.

0.199−0.1048
For room temperature the gradient = = 9.24∗10−5
17∗60
To find C A 1, graph 2.1 was used to find the concentration from the
conductivity measured in the experiment. Using the trendline of
y=10.268x and the conductivity of gives

C A 1=9.4828∗10−4
C A 2=0

Using equation 2.3 and substituting in known values:

0−(9.482∗10−4 ) 2
−2
∗π ( 1∗10−3 )
0.45∗10
∗1
1 ( −5 4
9.24∗10 )= (−D AB )
0.112 0.45∗10−2

D AB=0.211 m2 / s

dk 0.1994−0.0263
For 30˚C the gradient, = =5.41∗10−4
dt 320

C A 1=0.0375, found using y=8.3013x from the trendline.

C A 2=0

Using equation 2.3 and substituting in the new values for 30˚C:
π (1∗10¿¿−3)2
∗1
1 ( −4 0−0.0375 4
5.41∗10 )=(−D¿¿ AB) ∗ ¿¿
0.112 0.45 ¿ 10−2 0.45∗10−2

D AB=0.459 m2 / s

dk 0.1998−0.1305
For 35˚C the gradient, = =1.67∗10−4
dt 415
C A 1=¿ 1.223∗10−3, found using y=7.3205x
C A 2=0

Using equation 2.3 and substituting in the new values for 35˚C:

12
 π (1∗10¿¿−3)2
∗1 −3
1 ( −4 0−(1.223∗10 ) 4
1.67∗10 ) =(−D¿¿ AB) ∗ ¿¿
0.112 0.45∗10−2 0.45∗10−2

D AB=0.240 m2 / s

Taking these 3 calculated values for the diffusion coefficient and plotting
them against temperature gives the graph below which shows the
relationship between them.

Relationship between the diffusion constant and temperature

0.5

0.45

0.4
Diffusion constant (m2/s)

0.35

0.3

0.25

0.2

0.15

0.1

0.05

0
20 22 24 26 28 30 32 34 36

Temperature (˚C)

The 3 values for D AB plotted against their corresponding temperatures are

shown below in graph 2.5
As this makes a curve, the diffusion of the specific reaction is best at the
peak of the curve, which is at 30˚C. This is therefore the optimum
temperature to be operated at.

Conclusion
The aim of the experiment was to find the optimum diffusion constant.
From graph 2.5, the maximum value for the diffusion constant is 0.459,
operating at a temperature of 30˚C.

When measuring the conductivity at different concentrations for the

calibration curve at various temperatures, it was difficult to obtain the

13
values for 30˚C and 35˚C exactly using the water bath. This limited the
precision of the results because as soon as they were removed from the
water bath the temperature would constantly drop from the beginning to
the end of the experiment. The values for the conductivity are therefore
slightly inaccurate because of the slight variations in the temperature for
the different concentrations.

Practical 3 (P3): Measurement of the pressure differential and

flooding in the gas-liquid extraction column

Aim
To examine the air pressure differential across the column as a function of
air flow for different water flow rates and to determine the flooding
pressures.

Introduction
The purpose of this experiment is to study the pressure differential across
a packed column as air flows counter currently to liquid at different flow
rates. If we consider just one stream of gas flowing through a packed
colum, it can be assumed that as the flowrate of the air increases, as will
the pressure drop. It can also be assumed that since we are dealing with
air, the flow is be turbulent. From line A in Figure1.1 this relationship can
be observed, where pressure drop is approximately the gas velocity to the
power of 1.8 (Coulson and Richardson’s Chemical Engineering Volume 2).

The gas isn’t the only stream since the purpose of this experiment is to
find the fastest air flow rate to ensure maximum efficiency in extraction.
As a liquid flow down the column (with the aid of gravity) and the air flows
up the column; increasing the air flow rate increases the pressure drop in
the column. This pressure increases at a faster rate once it hits the
loading point (labelled ‘x’ on the diagram). The loading point is the point
at which the upward flowing gas is starting to hold up the flow of liquid
flowing down the column since free space is being filled. As the air flow
rate continues to increase, there is more interaction between the gas and
liquid meaning the resistance to flow increases exponentially as shown in
Figure 1.

When the air flow rate is large enough to fully prevent the liquid flowing
down the column this is known as the flooding point which is highlighted

14
with point ‘y’ on the figure. Beyond this flow rate, there is no further
increase in pressure drop.

The most optimal gas flow rate is to operate at the loading point since at
this point, contact between the 2 components is high but not too violent in
order to cause the process to flood.

Figure 1.1 – General relationship between velocity and pressure,

emphasising loading and flooding points.

Experimental Section

i) Experimental Procedure
There are primarily 3 main features in this experiment. The column itself,
liquid flow flowing in from the top of the column and gas entering from the
base of the column. In addition to this, there were 3 main valves labelled
v1,v2 and v3 in Figure 1.2. These valves allowed the pressure within the
column to be monitored using water manometers.

Before starting the experiment, the column must be completely dry. Once
the column is dry, the air flow rate can be set at variable flowrates and
the pressure can be found by recording the change in the height of the
water level in the manometer. The total pressure difference is the total
change in water height between the top and bottom halves of the column.

The pump pulls water back to the top of the column for recirculation and
the compressor is used to set the required flow rate, as shown in Figure
1.2

The recordings were taken initially with an air flow rate at 30 l/min up to
150 l/min.
Once all data had been recorded for the air flowrate with no water flowing
into the column, the experiment was repeated using the same procedure
but with varying liquid flow rates ranging from 0-7 l/min.

15
The pressure differential was calculated using equation 1.1 which
illustrates that the pressure change in the system is a function of height of
the manometer reading in the top and bottom of the column.

ΔPcolumn = (PMiddle – PBottom) + (PTop – PMiddle) (Equation 1.1)

Figure 1.2 - schematic diagram

of the experiment.

Results and Discussion

16
 Table 3.1/raw data showing pressure drop at various liquid and air flow

rates
Table 1.2/raw data showing pressure drop at various liquid and air flow
rates

From a general observation at the results obtained from this experiment,

it can be stated that generally as the flow rate of liquid in the column
increased, the flowrate required to cause flooding in the column
decreased.

This general hypothesis makes sense when referring to the theory of mass
transfer and interaction in a column. This is because as more liquid flows
through a column less air is needed to fill free space and cause interaction
between the two phases and in turn the loading point is found at much
lower air flow rates, as is the flooding point.
However, in industrial processes, it can potentially be very expensive to
increase the liquid flow rate compared to the air flow rate and vice versa
for other processes. As a result, a compromise needs to be found to
ensure optimal flow rate of both the liquid and gas in order to increase the
efficiency of the extraction at loading point.

The pressure drop at each air flow rate was calculated using equation 1.1
with each individual reading referring to the pressure at each point in the
column as expressed using the four colours.

17
 Pressure drop in the colum as a function of air flow rate (l/min)
10
Pressure Drop in the column

1
1 10

Air flow rate (l/min)

Figure 1.3-processed data showing pressure drop as a function of air flow

rate.

Pressure drop in the colum as a function of air flow rate (l/min)

10
Pressure Drop in the column

1
1 10

Air flow rate (l/min)

Figure 1.4-processed data showing pressure drop as a function of air flow

rate.
As it can be seen with the raw data, the experiment didn’t flood at 7l/min
liquid flow rate which is very confusing and deviates from the trend that

18
was observed. This is most likely because the column was not fully wet
when the data was being recorded for this high flow rate since as the
experiment was run, we started at this flow rate and gradually worked
down to 1l/min of liquid flowing through the column. Therefore, is can be
concluded that this data is an anomaly as the column wasn’t wetted fully.

Conclusion
Overall, it can be concluded from this experiment that as liquid flow rate
increases in a gas-liquid extraction process, the flowrate of gas required
to achieve both flooding and loading point decreases. This is shown in the
results tables-table 1.1 and table 1.2.

There were also limitations to this experiment especially when recording

the raw data at flooding point since it was hard to accurately record the
height of the manometer at this point as it happened rather fast in
particularly at height liquid flow rates such as 5 and 6 l/min. This
experiment could have been repeated in order to increase the reliability of
obtained results and aloud to spot and discard any anomalies such as
7l/min since the column wasn’t fully wetted.

Further research may be necessary to study the effect of loading point

with varying flow rates and how interactions at the interface occur to
increase efficiency.

19
 Practical 4 (P4): Mass balance and determination of the mass
transfer coefficient for liquid-liquid extraction process

Aim
To perform a mass balance on the extraction column and to measure the
mass transfer co-efficient with the aqueous phase as the continuous
medium.

Introduction
The purpose of this experiment is to find the mass transfer coefficient
between propanoic acid and water (leskol) as the continuous medium and
the packing within the extraction column. Whilst this experiment is
operating, a mass balance around the system is also performed.

The main principle behind this technique is to transfer a solute from one
liquid phase to a different liquid phase, usually organic and aqueous
phases since these are immiscible. In general, if the flow rate of each
stream was to increase, the Reynolds number of each flow would also
increase meaning that the flow would become more turbulent and hence,
more efficient mixing between the two phases. This suggests that the
mass transfer rate would increase. However, if the process is reversed and
the packing within the column is wetted by the organic phase, emulsions
my form and in turn reduce the rate of mass transfer.

Further to this, it is unrealistic to say that increasing the flow rate

increases the mass transfer continuously since the 2 phases will hit a
point at which flooding occurs. At this point one of the phases in the
column is rejected. This specific flow rate for flooding differs between
different phases.

The equilibrium point in this extraction technique is achieved when the

concentration of the extract solute is constant in both phases.

Experimental Section

i) Materials and Equipment

- Burette
- Erlenmeyer 100mL
- Sodium Hydroxide Solution (0.1M)
- Sample flasks
- Phenolphthalein

ii) Experimental Procedure

For this process to run effectively, the packing within the column must be
fully wetted and so initially, the column needs to be filled with water by
using switch s in the schematic as shown below. The water flow rate
should be set to 100 ml/min once the column is fully wetted. At this point,

20
the pump for the organic phase can be turned on (switch 4) and set to 50
ml/min.

As this extraction technique progresses, water flows into a collection tank

from the top over the column due to water overflow. This tank has probes
fit into it and once the interface between the phases is at the top of the
middle probe, the level control can be set. This means a solenoid valve
will open to prevent accumulation in this tank.

In order to work out when equilibrium is achieved, samples from this tank
need to be taken and titrated against 0.1M NaOH with phenolphthalein
solution as an indicator. In this experiment, samples were taken every 10
minutes with 3 at each interval in order to increase reliability of the
results. From these titres, a mass balance equation can be generated as
shown in equation 2.1.

Nacid = Vo (X2 - X1) = Vw(Y2 - Y1) (equation 4.1)

In equation2.1, X2 is a known concentration of 9.8g/L and since there is no

extract in the pure aqueous feed, it can be assumed that Y1 is 0 g/L. From
this mass balance, an equilibrium line can be populated since:

Y = 3.27X (equation 4.2)

Once this is generated, along with the mass

balance, the aim of the experiment can then
be achieved by calculating the mass
transfer coefficient, expressed in equation
2.3.

(equation 4.3)

21
 Figure 4.1/ the schematic for the
experiment

Results and Discussion

Table 4.1/ the results obtained from the titration of Leksol against NaOH

Time the sample was Sample Volume (ml) Volume of 0.1M NaOH
taken (min) (ml)
10 10 4
3 2.5
20 10 3.5
10 3.8
6 2.5
30 10 3.7
10 3.6
9 3.2
40 10 3.2
10 3.3
10 3.3
50 10 3.2
10 3.2
10 3.2

Flow rate of aqueous phase (Vw) = 100ml/min

Flow rate of organic phase (Vo) = 54ml/min
Average Titre of 0.1M NaOH = 3.45ml

Equation:

CH 3 CH 2 COOH + NaOH →CH 3 CH 2 CO O−¿ Na+H 2 O¿

C = 0.1M = 0.1mol/L
n = cv = (0.1x(3.45∗10−3)) = 3.45∗10−4
This gives the moles of NaOH, and based on the above equation for the
reaction it appears to be a 1:1, which means that the moles of
CH 3 CH 2 COOH will also be 3.45∗10−4 .

Equation 2.1 can be used to work out the values of X 1 and Y 2, as the
values for X 2 and Y 1 are given as 9.8g/L and 0g/L respectively.
0.054 (9.8- X 1 ) = 0.1 (Y 2 -0)
0.5292 – 0.054 X 1 = 0.1Y 2 (Equation 2.4)

22
m = nM = 3.45∗10−4 x 74 = 0.02553 = 2.553g/L
Therefore Y 2 = 2.553g/L

Subbing this value into equation 2.4:

0.5292 – 0.054 X 1 = 0.1(2.553)
X 1 = 5.072222g/L

Nacid = 0.1 x 2.553 = 0.2553 g/min (Using

As shown in the booklet:

Δ X 1 = Driving force at the bottom of the column (Δ
X 1 =( X 1−0)) = 5.072222g/L
Δ X 2 = Driving force at the top of the column (Δ
2.553
X 2 =( X 2−X ¿2 )) = 9.8 - = 9.019266055g/L
3.27

Figure 4.2/ the extraction column

with the results of the calculations

equation 2.1)

From equation 2.3:

0.2553
K X=
( 9.019..−5.0722.. )
0.575∗( )
9.019..
(
ln
5.0722.. )
K X = 0.06474700609 min−1

To construct the equilibrium line, equation 4.2 is used to plot out various
values of X and Y. To find out the points for the operating line the
Vw
equation: Y = ( X− X 1 ) +Y 1 is used. Subbing in the values, the line obtained
Vo
becomes:
54
Y= ( X−5.072222 ) +0
100
Y = 0.54X – 2.738999888

Table 4.2 below shows the points required to plot the equilibrium and
operation lines. The values for the equilibrium line are shown in blue and
the operation line is shown in orange.

X Y X Y
0 0 0 -2.739
0.1 0.37 0.1 -2.685

23
 0.2 0.74 0.2 -2.631
0.3 1.11 0.3 -2.577
0.4 1.48 0.4 -2.523
0.5 1.85 0.5 -2.469
0.6 2.22 0.6 -2.415
0.7 2.59 0.7 -2.361
0.8 2.96 0.8 -2.307
0.9 3.33 0.9 -2.253
1 3.7 1 -2.199

Graph 4.1 which shows the equilibrium and operation line that correspond
to the obtained values

Equilibrium and Operating Lines

5

2
Mole Ratio Y

0
0 0.2 0.4 0.6 0.8 1 1.2
-1

-2

-3

-4
Mole Ratio X

The equilibrium curve is a straight line from the point (0,0) which is
expected. The operation line however is negative which isn’t correct. For a
counter-current process it’s expected that there’s a positive slop and that
it’s below the equilibrium curve because it’s a desorption process.
However, with the negative values obtained, it’s assumed that the
operation line can’t be plotted, this may be because the mole ratios are
being used instead of the mole fractions, which would give different
values.

Conclusion
The aim of this experiment is to measure the mass transfer coefficient
with the aqueous phase as the continuous medium. This value was found
to be 0.0647/min.
As a result of this lab, it’s been shown that a correct equilibrium line can
be plotted but an operating line can’t, because there isn’t enough

24
information to work out the mole fractions for a liquid-liquid extraction
process.
Some limitations of the experiment were that it was difficult to obtain the
exact amount of Leksol, which is why some of the readings weren’t
exactly 10ml as they should have been. The valve would also be slow to
open, and therefore not all the readings were taken exactly on the
minute.
The flow rate should have been calibrated at 50ml/min however when it
was tested it showed to actually be 54ml/min, so this value was used in
the calculations instead.

Practical 5 (P5): Distillation

Aim
To determine the distillation column’s overall efficiency and to reduce the
rate of mass transfer.

Introduction
In distillation a feed mixture of two components, or more, is separated
into products, bottoms and distillate which all have different compositions
to the feed. The composition of the feed in this experiment is binary
because there are two components that are being separated.
The inside of the distillation column is made up of column internals, which
are trays or packing. The greater the number of trays, means the greater
the degree of separation, as their design maximises the contact between
the two distributions in the column. This increased contact gives a better
separation at each tray and therefore a reduced mass transfer resistance.
(263, lecture 2).

Figure 5.1 The project schematic

for the distillation. The image is
from the lab manual.

25
Experimental Section

i) Materials and Equipment

- 11 litres of a 1L ethanol and 10L water mixture
- 250ml measuring cylinder
- Stopwatch
- Refractometer

ii) Experimental Procedure

To obtain results for the calibration curve use a digital refractometer
for 11 different mole fraction compositions. The weight of water and
ethanol needed to make these up are individually calculated, using the
equation:

moles of ETOH
X E +OH = (Equation 5.1)
(moles of ETOH +moles of water )

To measure the boil-up rate, collect condensate into a measuring cylinder

every 120s. Collect 5 samples from V 3 and 5 samples from V 2 . When
collecting, try to ensure that the flow rate is the same as V 0 .
Store these samples in individually marked vials and wait for them to cool.
This is when their refractive index can be measured using the digital
refractometer.

To work out the number of theoretical plates from the data collected in
the experiment, equation 5.2 below must be used. Here ‘n’ denotes the
number of theoretical plates, ‘ x A’ is the mole fraction of the more volatile
component, ‘ x B’ is the mole fraction of the least volatile component and ‘
α AV ’ is the average relative volatility.

(Equation 5.2)

To work out the average relative volatility equation 5.3 below must be
used, where the subscripts D and B indicate the distillate and the bottom
respectively.

26
 (Equation 5.3)

Once the number of actual and theoretical plates are calculated, the
efficiency can be found using the equation 5.4 shown below.

(Equation
5.4)

Results

Table 5.1 showing the values obtained for the refractive index of the
various mixtures of ethanol and water. This will be used to make the
calibration curve.
Ethanol mole Mass of Water Mass of Refractive
fraction (g) Ethanol (g) Index (~)
Composition
(~)
1 0 1.000 13627
0.9 0.087 2.000 13641
0.8 0.0978 1.000 13662
0.7 0.168 1.000 13660
0.6 0.261 1.000 13658
0.5 0.391 1.000 13648
0.4 0.587 1.000 13638
0.3 0.913 1.000 13590
0.2 1.56 1.000 13573
0.1 3.52 1.000 13485
0 1.000 0 13332

Table 5.2 with volumes taken from the Distillation Column (at a
temperature of 79.6˚C)
Column Time(s) Volume (ml) Refractive
Index (~)
V3 120 30 13640
240 34 13637
360 28 13639
480 23 13640
600 25 13638
V2 120 29 13364

27
 240 29 13352
360 26 13351
480 27 13358
600 26 13357

T 1=78.3˚C and T 8=83.4˚C

Level of liquid in the reboiler = 20cm

Diameter of the reboiler = 30cm
Length of the reboiler = 50cm

Results obtained for the rate are shown below in table 5.3
Sample Rate (ml/min)
1 8.73
2 8.22
3 8.84

Average Boil up rate = 8.6ml/min or 0.483L/hour

Graph 5.1 showing the calibration curve obtained by plotting the ethanol
mole fraction composition against the refractive index

Calibration Curve
13700

13600
Refractive Index

13500

13400

13300

13200

13100
0 0.2 0.4 0.6 0.8 1 1.2
Ethanol Mole Fraction Composition

An
equilibrium curve and operation line are required to find the number of
trays needed for this distillation column. In order to plot the equilibrium
curve, results from ASPEN in practical 6 are used, using the UNIFAC graph
for ethanol in the vapour/liquid phase. Ethanol is used because it’s the
more volatile component in the mixture.
To plot the operation line, the calibration curve above, plotted using data
recorded during the experiment, must be used. In the top of the
distillation column the average refractive index was 13639. This value
gives a corresponding Ethanol mole fraction composition of 0.88 from the
graph. In the bottom of the distillation column the average refractive
index was 13346, which gives an ethanol mole fraction composition that’s
approximately equal to 0.
These values make up the operation line in graph 5.2 below.

28
 Graph 5.2- showing the
number of trays to be 8

The
number of
triangles that would fit in between the equilibrium and operating lines
show the number of actual trays that would be in the distillation column,
which is 8.

Using equation 5.4, the efficiency of the column can be calculated. In the
265 manual the value of theoretical trays is worked out using Fenske’s
equation (equation 5.2) to be 3.48.

3.48
E= ∗100=43.5 %
8

The efficiency of the column in this experiment is 43.5%.

Discussion

Is a full separation of ethanol from water possible? Explain the effect of

the equation of state (UNIFAC and Ideal) on the vapour-liquid equilibrium
data.

Practically no it wouldn’t be. Would only be possible with an infinite

number of trays which wouldn’t be possible realistically in terms of cost
and space. This is shown on the equilibrium curve where the operating
line meets it, with such a small space you could fit an infinite number of
trays in between.

Is there any obvious relationship between boil-up rate and column

efficiency?

29
The graph on the right (Che.utah.edu, 2019) shows the
relationship between efficiency (y axis) and boil-up rate (x
axis). This shows that as the boil up rate increases, the
efficiency will stay constant up until a certain point, where
efficiency will fall, before beginning to increase again.

How does the efficiency of the column compare to full-

scale columns in use in industry?

A typical value for column efficiency is between 50-70% (Tham and

Costello, 2018). Considering the size of the industrial distillation columns
compared to the much smaller one in the laboratory, a lower column
efficiency is expected. 43.5% is lower than the typical efficiency but is
near the lower end of the expected values.

Conclusion
The aim of this experiment was to determine the column’s overall
efficiency, which was found to be 43.5%, below the expected industrial
efficiency but acceptable.
When operating the flow rate at valves V2 and V3, it wasn’t very accurate
which may have limited the accuracy of the results. The results were also
done manually, so there’s the possibility of human error in the results.

Practical 6 (P6): Modelling of Unit Operations

Aim
To run a model of ethanol and water under two equations of state;
‘UNIFAC’ and ‘Ideal’.

Introduction
Aspen Plus is the program that’s used to simulate this. Aspen Plus allows 3
working environments to be used; Properties, Simulation and Energy
analysis.
ASPEN is widely used in industry because it simulates different processes
and predicts the outcome of those processes and how they will perform
(Chems.msu.edu, 2019).

Experimental Procedure
Open Aspen plus and create a new simulation with the “Chemicals with
English Units” title. Enter water and ethanol into the components list and
go into “Base method” to choose UNIFAC to run the simulation using the
UNIFAC equation of state. Run the values in order to make the TXY
diagrams shown below.

30
Save this and repeat the same steps but using the ideal equation of state
instead of the UNIFAC. This will give two different TXY diagrams to
compare.

Results and Discussion

Graph 6.1/ the UNIFAC TXY Graph obtained from Aspen plus

T-xy diagram for WATER/ETHANOL

212.5

x 14.696 psia
210.0
y 14.696 psia

207.5

205.0

202.5

200.0

197.5

195.0
Temperature, F

192.5

190.0

187.5

185.0

182.5

180.0

177.5

175.0

172.5

170.0
0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00
Liquid/vapor mole fraction, WATER

Graph 6.2/ the ideal TXY Graph obtained from Aspen plus

31
 T-xy diagram for WATER/ETHANOL
212.5

x 14.696 psia
210.0 y 14.696 psia

207.5

205.0

202.5

200.0

197.5

195.0
Temperature, F

192.5

190.0

187.5

185.0

182.5

180.0

177.5

175.0

172.5
0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00
Liquid/vapor mole fraction, WATER

Both graphs show Temperature plotted against the Liquid/vapour mole

fraction of water.

Conclusion
Both graphs follow a generally similar pattern, starting from the bottom
left corner and moving up to the top right. As the temperature increases
the mole fraction in the vapour phase increases and in the liquid phase
decreases.
The activity coefficient is used in thermodynamics to account for
deviations from ideal behaviour to actual behaviour, and this explains why
the UNIFAC graph is different, because it represents real, rather than ideal
conditions and behaviour. The concept of fugacity and how this interacts
with the general equation of state explains these graphs. (O'Connel and
Haile, n.d.).

32
 Practical 7 (P7) : Chemical Reactors

Aim
To determine the reaction rate constant and the temperature dependence
of the reaction between sodium hydroxide and ethyl acetate to produce
sodium acetate and ethyl alcohol.

Introduction
The reaction will be carried out at 3 temperatures, room temperature
(approximately 21.5˚C), 30˚C and 40˚C in order to find out the effect
temperature has on the specific reaction rate, K. Equal amounts of sodium
hydroxide and ethyl acetate will be used (0.5L). The reaction is:

NaOH +CH 3 COOC 2 H 5 → CH 3 COONa +C2 H 5 OH

Sodium hydroxide + Ethyl Acetate → Sodium Acetate + Ethyl Alcohol

Both reactants contribute to the conductivity of the reaction, but the

products do not, so they will be left out of the calculations for the reaction
rate k in this experiment.
To work out the reaction rate constant, k, the following equation 7.1 needs
to be used. It’s a derivation from the original second-order batch reactor
molar balance equation. It’s been integrated for Ca = Cao and when t=0.

(Equation 7.1)

The Arrhenius equation will then be used to plot a graph that will make it
easy to calculate the different values for activation energy and A. The
Arrhenius equation is shown below.

−Ea
lnk= + lnA (equation 7.2)
RT

(Figure 7.1/ the batch reactor controlled

by the Armfield software. It includes
more detailed schematics of the tubular
reactor, batch reactor and tank reactor
that make up the main reactor.
(Eleceng.dit.ie, 2019))

33
Experimental Section

i) Materials and Equipment

- Armfield Software
- 1L measuring cylinders
- Conductivity probe
- Thermometer
- Batch reactor

ii) Experimental Procedure

Ensure that the Armfield Software is open and the correct settings for the
batch reactor are met (making sure it’s in isothermal operation).
Measure 0.5L of NaOH and transfer it to the reactor and then set the
reactor agitator to 50 and turn the power on until the desired temperature
is met (initially this will be room temperature, followed by 30˚C and 40˚C).
When the temperature is achieved add 0.5L of ethyl acetate to the batch
reactor and start the data collection.
Collect the date for 30 minutes, or until the conductivity becomes stable.
Save the data in excel, clear the data on Armfield, stop the agitator and
empty the batch reactor into its blue base.
After this, change the temperature in isothermal operation to 30˚C and
repeat the process, doing the same afterwards for 40˚C.

Results and Discussion

Conductivity of NaOH at varying temperatures and Concentrations for the

Calibration Curve in table 7.4
Concentration (M) Temperature (˚C) Conductivity (mS)
20.9 4.87
0.025 30 5.67
40 6.64
20.8 9.62
0.05 30 11.34
40 13.12
20.8 14.33
0.075 30 17.07
40 20.00
20.9 19.21
0.1 30 /
40 /

34
The conductivity probe wouldn’t show value above 20mS, so for the 0.1M
concentration we were only able to collect one reading at room
temperature.

Graph 7.1 - the calibration curve for each temperature, showing that the
conductivity steadily increases with temperature
f(x) = 0
Calibration Curve
25
f(x) = 267.2 x − 0.11
f(x) = 228 x − 0.04
20 Room
Temp
eratu
Conductivity (mS)

15 re
Linea
r
10 (Roo
m
Temp
eratu
5 re)

0
0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.1 0.11
Concentraion (M)

Table 7.1 - for the results at room temperature, the temperature is

included because it fluctuated slightly
Measured Concentr Kt K ln(K) T 1/T(K)
Conductivity ation (˚C)
lamba1 0-20 (mol/dm3
[mS] )
7.89 0.0409366 4.427988 0.049199 - 21.3 0.00339616
5 8 88 3.011864
2
7.53 0.0390440 5.612073 0.046767 - 21.4 0.00339501
9 57 28 3.062571
5
7.20 0.0373049 6.806076 0.045373 - 21.5 0.00339386
7 89 85 3.092819
4
6.91 0.0358216 7.916106 0.043978 - 21.5 0.00339386
1 92 37 3.124057
3

Table 7.2 - the obtained results for 30˚C. The temperature is omitted
because it was maintained at 30˚C throughout the experiment

35
 Measured Concentr Kt K ln(K) 1/T
Conductivity ation
lamba1 0-20 (mol/dm3
[mS] )
8.18 0.0360683 9.253623 0.102818 -2.2747945 0.0032987
9 62 04
7.75 0.0341838 10.67576 0.088964 -2.4195158 0.0032987
23 69
7.39 0.0325990 12.02212 0.080147 -2.523887 0.0032987
3 05 47
7.08 0.0312284 13.20627 0.073368 -2.6122647 0.0032987
1 62 2

Table 7.3 - the results for 40˚C, the temperature isn’t included as it’s
constant
Measured Concentra Kt K ln(K) 1/T
Conductivity tion
lamba1 0-20 (mol/dm3)
[mS]
7.19 0.027299 18.00567 0.1000315 -2.3022696 0.00319336
97 5
6.92 0.026312 19.14760 0.0911790 -2.39493 0.00319336
2 6
6.72 0.025544 20.18245 0.0840935 -2.4758254 0.00319336
27 5
6.54 0.024886 21.08756 0.0781020 -2.5497385 0.00319336
34 9

The values for kt increase with temperature, as shown below in graph 7.2

36
For the final graph plotting the Arrhenius equation using equation 7.2 1/T
is the x axis and ln(k) is the y axis. The gradient is -Ea/R and the y
intercept is equal to lnA.
The initial results as shown in tables 7.1-7.3 are used to plot this graph.
The average of the first four results are used, for stability.

A graph following the Arrhenius equation, graph 7.3

Linear Interpolation of Ln(k) against 1/T

0
0 0 0 0 0 0 0

-0.5

-1

-1.5
ln(k)/s

-2
f(x) = − 3863.32 x + 10.2
-2.5

-3

-3.5

1/T (K)

From the equation shown on the graph’s trendline, the y intercept =

10.203. This means that the value of A is:
A=e 10.203=26984.016818 s−1

The value for the activation energy can be found by multiplying the
gradient by -R. The activation energy is:

Ea =−8.314∗(−3863.3 ) =32119.4762 J

Conclusion

The values obtained in this experiment for activation energy and A are
quite high which show that it’s a high energy process. The results for the
table are recorded on the Armfield software, so there shouldn’t be any

37
limitations or errors in those values. The trendline on the graph however
isn’t particularly accurate and could mean that the results aren’t very
precise.

Practical 8 (P8) : Particle Formation

Aim
The aim is to work out how to achieve the smallest particle size, by
varying parameters such as temperature, stirring rate, addition rate and
concentration.

Introduction
The method used in this experiment is a precipitation from Ce(III) nitrate
and potassium hydroxide to make Ce(III) hydroxide. The reaction is
detailed below.

Ce(NO ¿¿ 3)3 (aq) +3 KOH (aq ) → Ce(OH )3 (s )+ 3 KNO 3(aq) ¿

The optimal ceria powder will be the one with the smallest particle size, at
the fastest rate. The particle diameters will be tested using the Malvern
Master-sizer 3000. In order to see which conditions are optimum, a ‘full
factorial’ will be conducted with the other groups, in order to compare the
different conditions.

Experimental Section

i) Materials and Equipment

- Malvern Master sizer 3000
- Armfield computer-controlled reactor unit with CSTR

ii) Experimental Procedure

Load the reactor with 500mL of 0.2M KOH and set the reactor stirring rate
to 50rpm, with the log set to record results every 30 seconds. Add 400mL
of 0.1M cerium nitrate solution from pump 2 for 5 minutes for the correct
rate. After 5 minutes has passed, continue stirring with no addition for 3
minutes.
Take a sample of this to the Master-sizer to measure the particle size
distribution. Add 100ml of Polyethyleneimine solution and add it to the
main container, stir at 50rpm and then leave it to rest for 5 minutes. Take
a sample of this and take it to the Master-sizer to measure its PSD.

38
 Finally, put the contents of the container into a big beaker and rinse the
reactor out with deionised water. Then using a Buchner funnel filter the
contents of the beaker and give them away to be sintered at 700˚C.

Results

In order to determine the fastest rate for the particle size to reduce, a
conductivity graph against time was plotted for various parameters.

The results for our experiment which measured conductivity (mS) had
conditions where the stirrer rate was 50 rpm, 80ml/min additional flow
rate and 0.1M concentration, are shown in Figure 8.1. Figure 8.2 shows
the response of all systems at various parameters.

A graph showing the relationship between conductivity and time with a stirrer rate at
50rpm and additional rate (pump) at 80 ml/min
20.00
18.00
Measured Conductivity (mS)

16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
0 2 4 6 8 10 12 14 16 18
Time (mins)

Graph 8.1

39
A graph showing the relationship between conductivity and time
at various stirrer rates, additional rates (pump) and concentration.
25.00

20.00 100 80
0.1
10 80
0.2
Conductivity (mS)

15.00 50 40
0.1
50 40
0.2
10.00 10.29
50 80
0.2
50 80
0.1
5.00

0.00
0 5 10 15 20 25 30

Time (s)

Graph 8.2

From graph 8.2, at 100rpm, 80ml/min additional rate and 0.2M the
gradient is at its greatest, which shows that the conductivity reaches
stability fastest at these parameters. Along with this, when referring to
table 8.1, which shows the particle size distribution at all parameters,
these operating conditions give a D(50) value of 14.5 um after 100ml of
Polyethyleneimine solution (10% w/w), which is the smallest value in the
collected data.

Hence, together with the fact that the particle size diameter is the
smallest and reaches stability in conductivity the fastest, these can be
concluded to be the optimum parameters for this process.

Table 8.1 – the PSD results at various parameters from the Malvern
Master-sizer 3000, from the full factorial experimental matrix.
Stirring rate (rpm) Additional rate (ml/min) cerium nitrate concentration (M) Dx(50) (um) Dx(90) (um) Dx(10) (um) Dx(50) (um) Dx(90) (um) Dx(10) (um)
50 40 0.1 38.7 144 6.51 21.9 117 7.48
50 40 0.2 28 80.2 8.74 30.6 92.9 10.5
50 80 0.1 79.3 182 21.9 23.2 52.6 9.53
50 80 0.2 425 844 132 1260 2370 382
100 40 0.1 79.3 182 21.9 23.2 52.6 9.53
100 40 0.2 209 630 25.1 48.3 197 9.51
100 80 0.1
100 80 0.2 223 878 5.32 14.5 398 1.99

The individual PSD graphs obtained in this experiment for a stirring rate of
50rpm, additional flow rate of 80ml/min and 0.1M concentration.

40
 Graph
8.3 – PSD before adding the 100ml of Polyethyleneimine

Graph 8.4 – PSD after adding 100ml of Polyethyleneimine

Conclusion
The aim of this experiment was to find out the optimum conditions and
parameters to obtain the smallest particle size possible. This was found to
be at a stirring rate of 100rpm, additional flow rate of 80ml/min and a
concentration of 0.2M.
There was supposed to be an additional component of this experiment,
where Buchner funnel filtration was used on the mixture and then taken
away to be sintered, however the results of this were never shared, so it
wasn’t possible to do any further analysis and include the results in the
final report.
In table 8.1, there is missing data in the row for 100rpm, 80ml/min and
0.1M because the group carrying this experiment out didn’t share results
and they were therefore omitted from the final graph.

41
 Practical 9 (P9) : Filtration

Aim
To use a vacuum filtration set up to determine the cake specific
resistance and compare the value measure in this experiment with the
theoretical value based on the particle size.

Introduction
The main piece of equipment being used in this experiment is the
Armfield filter press, which is a batch filtration unit with a continuous flow.
(Discoverarmfield.com, 2019). It’s used for solid/liquid filtration, for
calcium carbonate in the case of this experiment. Cake filtration is also
used in this press, with positive pressure, which is clearly shown in the
figure below. For large scale processes with high specific surface area,
positive pressure has many advantages, such as building thicker cakes
under good conditions, which can be transferred into the small-scale
process in this experiment.

42
 Figure 9.1 is a schematic of the
cake filtration process, obtained
from the lab manual

From the particle size from the Master sizer the theoretical cake specific
resistance can be calculated, but under the assumption that all the
particles are spherical and aren’t compressible.
The basic equation for cake filtration is equation 9.1:
2
dV A (−ΔP)
=
dt rμvV

Carmen-Kozney equation can be used to estimate specific resistance, r,

for hard spheres and is equation 9.2:

1 1
= }} {{e} ^ {3}} over {{{S} ^ {2} (1-e)} ^ {2} ¿
r K ¿
To calculate an experimental r however, the pressure drop across the
cake needs to be taken into account because it increases with the amount
of filtrate that’s passed through. This is assuming that the pump was
working at a constant flow in the experiment, which was the case.
This means that rμvV is proportional to A2 (− ΔP).

Experimental Section
i) Materials and Equipment
- Armfield filter press
- Malvern Master sizer 3000
- 7L Calcium Carbonate

ii) Experimental procedure

Pour the suspension of 7L of calcium carbonate into the main vessel of
the Armfield filter press. Turn on the agitator and the pump, with the
pump set to run at 20Hz. Wait for the initial 50ml of filtrate to pass

43
through before beginning to record. Once it had, start a timer and
record the time and pressure every 50ml for the first 1000ml and after
that, record every 100ml. Keep the filtrate and separate it into 1L
samples, making sure that they’re labelled in the correct order.
Once the samples have been collected, turn off the agitator and pump
and take the samples to the master sizer 3000 to measure their
particle size distribution.

Results and Discussion

The results obtained from the filter press at pump speed 20Hz are
shown below in table
9.1

Volume (ml) Time (s) Pressure (bar)

0 0 0.36
50 42 0.40
100 56 0.43
150 74 0.46
200 90 0.50
250 107 0.62
300 121 0.59
350 140 0.69
400 152 0.73
450 165 0.76
500 180 0.76
550 195 0.76
600 210 0.79
650 225 0.80
700 240 0.81
750 250 0.82
800 265 0.78
850 280 0.78
900 295 0.78
950 310 0.80
1000 328 0.81
1100 355 0.83
1200 386 0.84
1300 415 0.85
1400 445 0.84
1500 472 0.86
1600 502 0.87
1700 536 0.86
1800 564 0.85
1900 592 0.86
2000 622 0.87
2100 656 0.89
2200 688 0.88

44
 2300 717 0.89
2400 744 0.90
2500 778 0.92
2600 805 0.93
2700 834 0.95
2800 864 0.97
2900 894 0.96
3000 924 0.65
3100 954 0.71
3200 985 0.74
3300 1015 0.77
3400 1046 0.67
3500 1076 0.74
3600 1107 0.76
3700 1136 0.74
3800 1168 0.78
3900 1194 0.81
4000 1226 0.83

There’s an error in the readings above, at 3000ml the pressure suddenly

drops before continuing to steadily increase, which shouldn’t happen. This
anomaly can be clearly seen on graph 9.1 where the pressure suddenly
drops.

The results obtained from the pressure drop and volume are shown below
in graph 9.1.

Pressure Drop vs Volume Filtered

1.2

0.8 f(x) = 0 x + 0.68

Pressure (Bar)

0.6

0.4

0.2

0
0 500 1000 1500 2000 2500 3000 3500 4000 4500
Volume (ml)
45
According to the lab manual, this should yield a straight line, the gradient
of which can be used to determine the value of r. However, this is clearly
not the case, and although a trendline has been fitted on the graph it’s
not very accurate at all. The graph of volume vs time however does give a
linear line, and therefore a much better trendline. This will be used to
calculate the value of r.

The graph, 9.2, of time vs volume which gives a straight line, showing a
linear relationship between the two.

The results from the Malvern Master-sizer 3000 for particle size
distribution

Graph 9.3 – Initial results for the particle size distribution of Calcium
Carbonate before any filtration had occurred.

46
Graph 9.4 – the PSD for the 1st litre of filtrate

Graph 9.5 – the PSD for the 2nd litre of filtrate

Graph 9.6 – The PSD for the 3rd litre of filtrate

Graph 9.7 – The PSD for the 4th litre of filtrate

Using equation 9.1 and graph 9.2, a value for r can be calculated.

dV
The gradient, of the graph is shown to be 0.0002m 3 /min = 0.000003m 3 /s
dt

c 0.01 1
v= = =
1−e 1−0.4 60

0.000003=¿ ¿

r =1.095∗1014

47
Theoretically, from the Master sizer 3000 at 4L and δ(μ10) = 2.55μm,
using equation 9.2 (Carmen-Kozney) the following value for r was
obtained:

1
∗0.4 3
1 5
=
r ¿¿

r =1.557∗10 14

Conclusion
The aim of this experiment was to determine the cake specific resistance
and compare the value measured with the theoretical value based on
particle size. The experimental value for the specific resistance of the
cake is 1.095∗1014 and the theoretical value, based on the particle size
distribution is 1.557∗1014. This theoretical value is reasonably similar to the
value for r calculated from the experimental data, with a percentage
difference of 29.6%.
One of the major limitations in the results of the experiment was the
pressure after the 3000ml sample dropping significantly and going against
the trend of the previous values.

References

Chems.msu.edu. (2019). ASPEN Tutorial | Chemical Engineering and

Materials Science. [online] Available at:
https://www.chems.msu.edu/resources/tutorials/ASPEN [Accessed 12 Feb.
2019].

Utar.edu.my. (2019). Liquid Diffusion Coefficient. [online] Available at:

http://www.utar.edu.my/fes/file/UEMK2411%20ChemEng%20Lab%20I
%20Manual-200905-2.pdf [Accessed 25 Feb. 2019].

Eleceng.dit.ie. (2019). [online] Available at:

http://eleceng.dit.ie/gavin/DT275/CEM%20MKII%20manual%20issue
%2014.pdf [Accessed 1 Mar. 2019].

Tham, M. and Costello, R. (2018). Distillation Column Design. [online]

Rccostello.com. Available at: http://www.rccostello.com/distil/distildes.htm
[Accessed 13 Feb. 2019].

Sinnott, R. and Coulson, J. (2005). Coulson & Richardson's chemical

engineering. Boston: Butterworth-Heinemann.

48
Che.utah.edu. (2019). [online] Available at: https://www.che.utah.edu/site-
specific-resources/chemical-
engineering/department_equipment/Projects_Lab/S_Distillation_Column/MI
S_Description.pdf [Accessed 14 Feb. 2019].

O'Connel, J. and Haile, J. (n.d.). Thermodynamics, Fundamentals of

Application. John.P.O'Connel, p.208.

49