Republic of the Philippines

EASTERN VISAYAS STATE UNIVERSITY

Tacloban City

CHEMICAL ENGINEERING DEPARTMENT

COMPILATION OF EXPERIMENTS
in
ChE 512L
Chemical Engineering Laboratory 2

Submitted by:
Elias, Rachel G.
BSChE5A

Submitted to:
Engr. Juvyneil E. Cartel
Instructor, ChE 512L

In partial fulfillment of the requirements in

Bachelor of Science in Chemical Engineering
October 14, 2015
1

Table of Contents

Page No.

Rating

Preface

Experiment No. 1: Size reduction and particle size measurement by

screen analysis
Experiment No. 2: Diffusion of liquids through stagnant non-diffusing

15

Air
Experiment No. 3: Absorption of Carbon Dioxide in Water

22

Experiment No. 4: Measurement of Reaction Conversion

31

Experiment No. 5: Drying Curves

38

Experiment No. 6: Power requirement for agitation

48

Experiment No. 7: Cation Exchange

57

Experiment No. 8: Batch Distillation with packed absorption Tower

71

Experiment No. 9: Step Response of first order

83

Experiment No. 10: Motorized Control Valve

96

References
Appendices
A. Raw data
B. Calculations (contains calculations on preparations and on processing of data)
C. Documentation

Preface

The Chemical engineering students of Eastern Visayas State University Tacloban Chapter
are required to conduct 10 experiments for the subject requirement in ChE 512L (Chemical
Engineering Laboratory II). This subject serves as a continuation of the subject ChE 422L
(Chemical Engineering Laboratory I), a 4th year subject which also required the students to
perform laboratory experiments at Adamson University in Manila. These experiments are for the
students practicum specializing the principles and theories in unit operations.
The number of experiments are conducted based on the availability of the equipment and
materials that can be used for a certain unit operation experiment. The experiments was conducted
to put on action the theories and principles taught by the professors in the four corners of the
room to the students. To helped them visualize those theories and to operate equipment never
been experience to operate before. To evaluate the students performance and the ability of the
students to follow instructions correctly from the given procedures.
The students would I would like to give their wholehearted gratitude to a number of
persons, of without whom the performance of the experiments will not be a success.
To Engr. Albert Evangelista for his untiring effort in supervising the students in operating
the equipment, support and understanding our mistakes, taking in consideration that we havent
operate certain equipment before and damages and wrong handling might occur.
To Engr. Juvyneil Cartel, EVSU professor, for imparting his knowledge to the students.
And his patience in assisting us during the laboratory experiment.
To the parents, for their never ending support in permitting the travel distantly in order to
fulfill the mission in conducting this experiments. For their support in financing the travel. Thank
you so much for it is also a sacrifice not knowing what might going to happen during and after the
travel.
To the Almighty Father, for the guidance and untiring love providing us the things seen
and unseen. Thank you for never ceasing in guiding us emotionally for we had encountered a lot
of struggle on the way. Thank you so much.
3

Size Reduction & Particle Size Measurement by Screen Analysis

Experiment No.1

I.

Objectives:
1. To determine the screen analysis of the product obtained from the crusher and
pulverizer.
2. To construct fractional distribution plot, cumulative distribution plot, and
histogram presentation of the screen analysis of the given samples.
3. To determine the true arithmetic average diameter, mean surface diameter, mean
volume diameter/mean mass diameter and the specific surface (surface area per
unit mass) of the products from the crusher and pulverizer.
4. To estimate the energy requirements and the Rittingers Number for the crusher
and pulverizer.
5. To estimate the crushing efficiency of the crusher and pulverizer.

II.

Materials/Equipment Needed:

About 1 kg of small rocks practically uniform size from 1-1.5 inches in diameter

Ro-tap Sieve Shaker

Standard Tyler screen series composted of the following screens: 200, 150, 100,
80, 60, 40, 30, , mesh including cover and pan

Crusher

Pulverizer

Weighing Instrument
5

III.

Soft/Nylon Bristle Brush

Extra Pan

Equipment Set Up:

Crusher

Pulverizer

Sieve Shaker
6

IV.

Theory

Average Particle Size

Volume-Surface Mean Diameter D

s, which is related to the specific surface area
Aw. It is defined by the equation.
6
s A w p

Ds

Arithmetic Mean Diameter

n

DN =

( x i D pi )
i=1

NT

Where:
DN= arithmetic mean diameter
Ni=number of particles in each fraction
NT=number of particles in the entire sample

Mass Mean Diameter

n

Dw=

xi
i=1

D pi

Where:
7

Dw=mass mean diameter

Volume Mean Diameter

1
n

D v =[

i=1

xi
3
D pi

( )]

1/3

Specific Surface of Mixture

If the particle density p and sphericity s are known, the surface area of the
particles in each fraction may be calculated by this equation,
6m

A=Nsp= s p D p
Where:
A = total surface area
s = sphericity
p = density of the particle
Dp = diameter of the particle; m is the total mass of the sample

sp = surface area of one particle.

The results for all fractions added to give Aw, the specific surface area (the
total surface area of a unit mass of particles). If p and s are constant, Aw is given
by:
n

Aw=

6m
xi

p s i1 Dpi

Where:
8

xi = mass fraction in a given increment

n = number of increments
Dpi =average particle diameter, taken as arithmetic average of
smallest and largest particle diameters in increment

Methods of reporting screen analysis (differential and cumulative)

The information from the particle size analysis that is tabulated which showed the
mass or number fraction in each increment as a function of the average particle size (or
size range) in the increment. An analysis tabulated in this way is called differential
analysis.
A second way to present the information is through cumulative analysis obtained
by adding, consecutively, the individual increments, starting with that containing the
smallest particles, and tabulating or plotting the cumulative sum against the maximum
particle diameter in the increment.
Calculations of average particle size, specific surface area, or particle population of
mixture may be based on these two methods. In principle, methods based on the
cumulative analysis are more precise than those based on the differential analysis, since
when the cumulative analysis is used; the assumption that all particles in a single fraction
are equal in size is not needed. The accuracy of particle size measurements, however, is
greatly enough to warrant the use of the cumulative analysis, and calculations are nearly
always based on the differential analysis.

Determination of Rittingers Number experimentally

9

Determination of theoretical power requirement by a size reduction equipment

based on the new surface created (Rittingers Law)
The theories derived depend upon the assumption that the energy E required to
produce a change dX in a particle size X is a power function of X:

dE / dX =-C/Xn

V.

Procedure
A. Develop/Outline procedure followed n size reduction of small rocks using the
crusher and pulverizer.
B. Preparation of screen analysis of the products obtained from the crusher and
pulverizer.

Basic Operations of Ro-Tap Sieve Shaker

1. Assembles a stack of sieves, beginning with a top cover and then the coarsest
(largest) sieve opening on top and a pan on the bottom. Place them into the
shaker. When placing the sieves into the Ro-Taps, the hammer should be tilted
up and out of the way.
2. Place the sieve cover, with the cork installed, on the top of the stack.
3. Adjust the sieve support clamp bar with the two wing nuts, bringing the top of
the sieve cover flush with the upper carrying plate.

Hammer Drop Adjustment

10

Note: Prior to hammer adjustment; make sure cork in sieve cover is seated firmly.
Make sure sieve cover has top edge flush with upper carrying plate.

1. Remove pedestal cover

2. Jog machine until hammer rises to a maximum height, check height with
scales.
3. Set height 10 1 5/16 +- 1/16 by loosening screw on coupling and adjusting lift
rod.
4. Tighten screw on coupling.
5. Replace pedestal cover.

Starting the Shaker

1. Make sure a sieve stack is in place at this time. Set the test run in time, by
simply turning the thumb wheel + (plus) or (minus) to the desired time in the
digital window.
2. Push the start bar to start test and note countdown time. An audible tone will be
heard at the end of the test. You can stop or interrupt the test at any time, by
simply pushing the stop bar. Note that the remaining test time is frozen on the
readout. To continue, simply push the start bar. Note: the timing device also has
a clock function. To use this option, hold the clock button and adjust to the
proper time with the thumb dial.

Performing a Sieve Analysis

1. Select a set of test sieves with mesh openings that will reveal particle
distribution at critical sizes. Critical sizes are usually stated in a product
specification or are determined by material processing requirements.

11

2. Assemble a stacked of test sieves (one of top of the other) with coarsest
(largest) opening on the top of the stack. A proper sample amount should
cover the wire mesh of the top sieve, but not overload the surface.
Overloading will cause blinding or blocking of the openings, not allowing
the sample to be properly processed.
3. Place the test sieve stack into the sieve shaker, and place the cover on the
top of the stack. The sieves must be secured into place. The shaker should
be activated and set to operate for their proper length of time.
4. After completion of the agitation, weigh the material retained on each sieve
in order to record the data. Weighing should be by grams, with a balance
scale having at least a capacity of 500 grams and a sensitivity of 1/10 gram.
5. Using the extra bottom pan, empty the materials retained on the coarsest
sieve into the pan. A soft or nylon-bristle brush should be used to gently
brush the underside of the sieve, thoroughly removing all of the remaining
particles into the pan. The sieve frame can be tapped with the handle of the
brush to clean any remaining material on the sieve. Weigh the contents in
the pan to the nearest 1/10th gram immediately record the data.
6. If several extra pans are available, it is best not to discard this portion of the
sample until the entire process is completed. This same procedure should
be repeated on all sieves in the stack. The material passing through the
finest sieve into the bottom pan must also be weighed to obtain the total
weight for percentage calculations. The total weight of the material retained
on the various sieves and in the bottom pan should be extremely close to
the weight of the original sample.

VI.

Results and Discussion

Table 1.1 Crusher Experimental Screen Analysis

12

Mesh
No.
Table
1.2

Pulverizer

Seive

Wt. of

Wt. of

Wt.

Average

Opening screen

screen

of

Weight

Cumulativ

Particle

Soli
Wt.
(g)

Fractio
%
n

e wt.
%

Diameter,
Average

of

Cumulativ

Particle

95.35
e wt.

Diameter,

Mes

(mm)
Sieve
D

h No.

Openin

(g)
with
Wt. of solid
Wt. of
screen screen
(g)

30

0.600
g

390
(g)

1350
with

960
Soli

Weight
xi
95.35
Fractio

40

386

398
solid
355.8
(g)
1274
341.98
410.2
315.35

12
(g)
9.8
884
5.96
24.2
1.35

1.19
n
0.97
xi
88.75
0.59
2.43
0.13

96.54

0.51

60
8030
40
100

0.420
(mm)
0.250
Dpi
0.600
0.177
0.420
0.149

97.51
88.75
98.1
91.18
98.23

.335
.214
0.51
.163

200
60
Pan

0.074
0.250
-

354
346
388

98.8
93.58
100

.112
.335
.037

0.177

336

5
5.72
23.8
11.94
7
16.0

0.57
2.40
1.19

80

5
359.72
369.8
399.94
7
352.0

1.61

95.19

.214

314

2
317.8

2
3.85

.39

95.58

.163

354

5
371.0

17.0

1.71

97.29

.112

6
415.0

8
27.0

2.71

100

.037

pi

100

0.149

200
Pan

0.074
-

346
390
336
386
314

388

Experimental Screen Analysis

13

Screen analysis consists of the raw experimental data and the % weight faction, %
cumulative wt. and average particle diameter. Percent weight Fraction is the weight of the
solid in the mesh over the overall weight of the solid. Percent cumulative weight is the
sum of the solid in each sieve. This are the solid that did not passed through the sieve. This
are the remaining solids in the sieve. While the average particle diameter is the average
diameter of the 2 consecutive sieves.

Fractional Distribution Plot

120
100
80

% Weight Fraction

Crusher

60

Pulverizer

40
20
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

Sieve Opening,mm

Figure 1.1

14

Cumulative Distribution Plot

102
100
98
96
94

Cummulative %

Crusher

92

Pulverizer

90
88
86
84
82

0.1 0.2 0.3 0.4 0.5 0.6 0.7

Sieve Opening, mm

Figure 1.2

15

Distribution in Histogram
95.35
100
88.75
90
80
70
60
% Weight fraction 50
40
30
20
7
62.71
51.71
4 0.57
31.61
10 1.19
22.4
12.43
1.19
0.97
0.59
0.39
0.13
0
1 2 3 4 5 6 7
Screen Opening, mm
Crusher

Pulverizer

Figure 1.3
True Arithmetic Average Diameter in the Crusher and Pulverizer:
DA =

0.600+ 0.420+0.250+0.177+ 0.149+0.074

6
DA=0.2783 mm

Mean Volume Diameter:

Crusher:

Dv= 3

1
0.0119 0.00973 0.00592 0.00134 0.00568 0.0118
+
+
+
+
+
0.513
0.3353
0.214 3
0.1633
0.1123 0.037 3

Dv=1.178 mm

Pulverizer:

16

Dv= 3

1
0.0243 0.024 0.0161 0.0039 0.0171 0.0271
+
+
+
+
+
0.513 0.3353 0.2143 0.1633 0.1123 0.037 3
Dv=0.8625 mm

Mean Mass Diameter:

Crusher:

Dw=0 ( 0.9535 ) +0.0119 ( 0.051 )+ 0.00937 ( 0.335 )+ 0.00592 ( 0.214 ) +0.00134 ( 0.163 ) +0.00568 ( 0.1

Dw=0.01177 mm

Pulverizer:

Dw=0 ( 0.8825 ) +0.0243 ( 0.051 ) +0.024 ( 0.335 )+ 0.0161 ( 0.214 )+ 0.0039 ( 0.163 )+ 0.0171 ( 0.112 ) +0

Dw=0.01628 mm

VII.

Conclusion
We used a blinded sieve. There are depositions of materials used from the previous

Experiment and that is why, there is an additional amount of 6.77 g of crushed rock in the
screen analysis.

17

Screen analysis is divided into 8 columns. The sieve opening diameter was taken from the
Handbook of Perrys and Green but it can also be taken from any reliable references such as
the book of Geankoplis in Transport process and Unit Operations under Tyler Standard
Screen table.
Figure 1.1 shows the fractional distribution Plot from the screen analysis for the crushed
and pulverized rock. Figure 1.2 shows the cumulative distribution plot and Figure 1.3 for the
Histogram presentation taking %weight of the solid versus time as y and x respectively.
The true arithmetic average diameter in the crusher and pulverizer is 0.2783 mm. The
mean volume and mean mass diameter for the crusher is 1.178 mm and 0.01177 mm
respectively while 0.8625 mm and 0.01628 mm in the pulverizer, respectively.

VIII. References

Mccabe and Smith Unit operation processes

Geankoplis Transport Processes and Unit Operation

18

APPENDICES

Appendix A: Raw Data

Table 1.3. Screen Analysis (CRUSHER)

Mesh No.

Wt. of screen

wt. of screen

Wt. of solid(g)

30
40
60
80
100
200
Pan

(g)
390
386
346
336
314
354
388

with solid (g)

1350
398
355.8
341.98
315.35
359.72
399.94

960
12
9.8
5.96
1.35
5.72
11.94

Table 1.4. Screen Analysis (PULVERIZER)

Mesh No.

Wt. of screen (g)

wt. of screen with

Wt. of solid(g)

30
40
60
80
100
200
Pan

390
386
346
336
314
354
388

solid (g)
1274
410.25
369.87
352.02
317.85
371.06
415.01

884
24.25
23.87
16.02
3.85
17.08
27.01

19

Appendix B. Sample Calculation

Weight Percent
%wt=

100wt of solid on sieve

wt of sample

For Mesh 30
%wt=

100960
=95.35
1006.77

Cumulative Weight Percent Retained

%cumulative wt retained=

100wt of solid on sieve +wt of solid on sieves above

wt of sample

For Mesh 40
%cumulative wt retained=

10012+ 960
=96.55
1006.77

Average Particle Diameter

= D1+D2/2
For Mesh 40
= 0.600 + 0.420 = 0.51

20

Appendix C. Documentation

21

Diffusivity of Liquids through Stagnant, Non-diffusing Air

Experiment No.2

I. Objectives
1

To determine the mass diffusivities of volatile organic liquids in air at different

temperatures using the capillary tube method.

To compare the results with those obtained from empirical equations (Lennard-Jones
and Gilliland equations) and available data from books.

II. Materials/Equipment Needed

Water bath

5 Capillary Tubes

Small Electric fan

Barometer

Receptacles for capillary tubes

5 volatile organic liquid

Verneir caliper

Timer

Thermometer

III. Equipment Set

22

IV. Theory

Diffusion is the movement, under the influence of a physical stimulus, of an individual

component through a mixture. The most common cause of diffusion is a concentration
gradient of the diffusing component. A concentration gradient tends to move the
component in such a direction as to equalize concentrations and destroy the gradient.
When the gradient is maintained by constantly supplying the diffusing component to the
high concentration end of the gradient and removing it at the low concentration end, the
flow of the diffusing component is continuous. This movement is exploited in masstransfer operations.
Although the usual cause of diffusion is a concentration gradient, diffusion can also be
caused by an activity gradient, as in reverse osmosis, by a pressure gradient, by a
temperature gradient, or by the application of an external force fields, as in centrifuge.
Molecular diffusion induced by temperature is thermal diffusion.
Equations used to determine the diffusivity constant of the VOC.

For Experimental Data (Capillary Tube Method)

23

D=

10000 A P B ,lm RT z 2 z 1
2
t PT M A ( P A 1 P A 2 )

Where:
Z2 & Z1 Final and initial height, respectively
PA2 & PA1 Final and initial pressure of Acetone

Gilliland Empirical Equation Diffusivity constant determination

3

D=

0.0043T A 2
PT

1
3

1
+V B
A

1 2
3

1
1
+
M A MB

Where:
TA Temperature
PT Total Pressure
A Density

VB - molar volume of air (taken as STP)

MA & MB Molecular Weight of
Substance and Air, respectivel

24

V. Procedure

Prepare the water bath and fill it with tap water and set it to 50C.
Fill the capillary tube with pure volatile organic liquids and measure the

initial height of liquid.

Provide a gentle stream of air by turning on the electric fan.
Measure the height of the remaining liquid in the capillary tubes after 10

and 15 minutes.
Repeat procedure 2-4 for trial 2 (water bath temperature = 65C) and trial
3 (water bath temperatures = 80C)

VI. Results and Discussion

Table 2.1 Diffusivities Using Different Methods at Various
Temperatures (cm2/s)
Temperature Experimental
(oC)
50
65
80

Data
0.019588107
0.007824613
0.008224336

Gilliland
0.026651868
0.024165494
0.022361933

Available
Data (0oC)
0.109
0.109
0.109

Table 2.1 shows the tabulated results for diffusivities of Acetone at 50, 65 and
80oC.
Diffusivities are differentiated using 2 methods and comparing it to the
available data for the diffusivity of acetone at 273K.
VII. Conclusion
Based on the experiment, it is observed that the volatile compound submerged in
the water bath while inside the capillary tube evaporates faster when the heat is
increased while constantly being exposed to a fan.
VIII. References
GEANKOPLIS, C. J. Principles of Transport Processes and Separation
Processes, 4th Edition, Prentice Hall, New Jersey (2003). pp: 636-644

18

APPENDICES
Trail

Temperature of

Water bath (C)

Height of the Liquid

Inside Diameter

(m)

(m)

Z1
0.082
0.091
0.060

1
50
2
60
3
80
Appendix A. Experimental Data

Z2
0.069
0.085
0.050

0.0008
0.00091
0.00093

Basis: Diffusivity of volatile organic liquid at different temperature.

Table 2.2 Raw Data

Table 2.3 Properties of Acetone at a given Temperature

ti

50

(kgmol/m3)
8.3134

65
80

VA

P(Pa)

(m3/kgmol)
0.12029

83498.31

8.2272

0.12155

116649.97

8.1352

0.12292

149801.64

Properties of Air
MW = 28.951
Molar Volume, STP (m3/kgmol) = 24.463
Pressure (Pa) = 101.325

Appendix B. Sample Computation

26

For Gilliland Equation

3

0.0043T A 2

D=

PT

1
3

1
+V B
A

1 2
3

1
1
+
M A MB

Where:
TA Temperature of Acetone
PT Total Pressure
A Density of Acetone
VB - molar volume of air (taken as STP)
MA & MB Molecular Weight of Acetone and Air, respectively

Solving data for T = 50oC = 323.15K

43 (323.15) 2

D=

(101325+ 8349.31107)

1
3
+( 24.4632075)
8.313422609

1 2
3

1
1
+
58.08 28.951

D=0.026651868 cm 2 /s

For Experimental Data (Capillary Tube Method)

10000 A P B ,lm RT z 22z 12
D=
2
t PT M A ( P A 1 P A 2 )

Where:
27

T Temperature of Acetone
PT Total Pressure
A Density of Acetone
VB - molar volume of air (taken as STP)
MA Molecular Weight of Acetone and Air, respectively
Z2 & Z1 Final and initial height, respectively
PA2 & PA1 Final and initial pressure of Acetone
P A 2= g Z 1
t Time
PB,lm Log mean pressure of Air
PB , lm=

( P T P A 1 )( PT P A 2 )
( PT P A 1)
ln
( PT P A 2 )

Solving data for T = 50oC = 323.15K

D=

10000 ( 8.313422609 )( 48050.78652 )( 8313.72 ) (323.15)

0.06920.0822
( 600 ) ( 101325+ 8349.31107 ) (58.08) ( 8349.311076.680508486 )
2

D=0.019588107 cm / s

28

Appendix C. Documentaion
Taking an amount of volatile liquid (acetate) using capillary tubes

Measuring the remaining liquid after submerged of the capillary tube with VL
inside in the water bath at a certain temperature

29

Absorption of Carbon Dioxide into Water

Experiment No.3

I.

Objective:
To measure the absorption of carbon dioxide into water flowing down the
tower, using the gas analysis equipment provided.

II.

Materials/Equipment Needed:

Gas absorption column

Carbon dioxide cylinder with integral pressure regulator, connected to

regulator R on the gas inlet on the apparatus.

Approximately 300 mL of 1.0 M caustic soda solution.

Small funnel and tubing for filling analysis equipment.

Standard 0.0277M sodium hydroxide solution prepared by diluting 27.70

mL of 1M caustic soda standard solution to 1 L with carbon dioxide free
distilled water. Prepare daily and protect from carbon dioxide in the
atmosphere by keeping in a stoppered Pyrex bottle.

Standard 0.1M sodium bicarbonate solution prepared by dissolving

approximately 0.1 gram of anhydrous sodium bicarbonate in carbon
dioxide free distilled water to 100 ml.

Phenolphthalein indicator prepared from carbon dioxide free distilled

water.

III.

Hempl Apparatus for gas analysis

Fresh tap water.

Thermometer and barometer.

Equipment Set Up

30

IV.

Theory

Nomenclature:
G = molar flow rate of Gas
G = Molar flow rate of dry Gas (solute free gas)
y = mole fraction of solute in gas
Y = mole ratio of solute in gas (mole of solute per mole of solute free gas)
L = molar flow rate of Liquid
L = molar flow rate of pure solvent (solute free Liquid)
x = mole fraction of solute in liquid
X = mole ratio of solute in liquid (mole of solute per mole of solute free liquid)
Z = height of the tower or column

31

Basic Assumptions:
1. Evaporation of solvent is negligible. Therefore, flow rate of pure solvent is
constant.
2. The solute free gas is relatively insoluble in solvent used. Therefore, solute free
gas flow rate is constant.
Using data on gas analysis, the amount of solute absorbed, N, can be computed.
N= G1y1 G2y2
= G1Y1 G2Y2
= G (Y1 Y2)
V.

Procedure
Absorption of carbon dioxide into water flowing down the tower, using the
gas analysis equipment provided.
1. First fill the two gloves of the absorption analysis equipment on the left of
the panel with 1.0 M caustic soda. Wear gloves and goggles while doing
this. Adjust the level in the gloves to the 0 mark on the sight tube, using
drain valve C into the flask to do this.
2. Fill the liquid reservoir tank to three-quarters full with fresh tap water.
3. With gas flow control valves C2 and C3 closed, start the liquid pump and
adjust the water flow through the column to approximately 6 L/min on
flow meter F1 by adjusting flow control valve C1.
4. Start the compressor and adjust control valve C 2 to give airflow of
approximately 10% of full scale on flow meter F2.
5. Carefully open the pressure- regulating valve on the carbon dioxide
cylinder, and adjust valve to give a value C 3 on the flow meter F3
approximately of the airflow F2. Ensure the liquid seal at the base of the
absorption column is maintained by, if necessary, adjustment of control
valve C4.
6. After 15 minutes or so of steady operation, take sample of gas
simultaneously from sample points S1 and S2. Analyze this consecutively
32

for carbon dioxide content in these gas samples as shown in the

accompanying sketch and following notes.
7. Flush the sample lines by repeated sucking from the line, using the gas
piston and expelling the contents of the cylinder to the atmosphere. Note
that the volume of the cylinder is about 100 ml. Estimate the volume of
the tube leading to the device. Then decide how many times you need to
suck and expel. (Step B and C).
8. With the absorption glove isolated and vent to the atmosphere closed, fill
the cylinder from the selected line by drawing the piston out slowly (Step
B). Note volume taken into cylinder V1, which should be approximately
20 ml for this particular experiment. Note: Wait at least 2 minutes to allow
the gas to come to the temperature of the cylinder.
9. Isolate the cylinder form the column and the absorption glove and vent the
cylinder to atmospheric pressure. Close after 10 seconds (Step D).
10. Connect cylinder to absorption glove. The liquid level should not change.
If it does not change, briefly open to atmosphere again.
11. Wait until the level in the indicator tube is zero showing that the pressure
in the cylinder is atmospheric.
12. Slowly close the piston to empty the cylinder into the absorption glove.
Slowly draw the piston out again (Step E and Step F). Note the level in the
indicator tube. Repeat steps E and F until no significant change in level
occurs. Read the indicator tube marking V. This represents the volume of
the gas sampled.
13. Repeat the experiment for trials 2 and 3.

Warning: If the concentration of carbon dioxide in the gas sampled is

greater than 8%, it is possible to suck liquid into the cylinder. This will
ruin your experiment and takes time to correct. Under these
circumstances, do not pull the piston out to the end of its travel. Stop it
at a particular mark, e.g. V1 = 20 on the coarse scale, and read the final
scale.
33

VI.

Results and Discussion

Table 3.1 Absorption of carbon dioxide into water flowing down the tower,
using the gas analysis equipment provided
Trial
No.
1
2
3

Mole Fraction of CO2

Inlet (Bottom)
Outlet (Top)
0.24
0.14
0.095

0.22
0.11
0.06

CO2 Absorbed
(gmole/min)
5.6 * 10^-4
1.104*10^-3
1.414*10^-3

Table 3.1 shows the calculated mole fractions of CO 2 taken from the inlet
and outlet and the carbon dioxide absorbed in gmole/min in each trial.

VII.

Conclusions
Based on the table above, CO2 absorbed molar rate increases as the trials
go on. Therefore, if the trials goes on, there is a decrease in the mole fraction
of CO2 in the inlet and outlet but an increase in the mole rate of CO2 absorbed.
As the mole fraction decreases, CO2 absorption increases.

VIII. References
GEANKOPLIS, C. J. Principles of Transport Processes and Separation
Processes

34

APPENDICES
Appendix A. Experimental data
Absorption of carbon dioxide into water flowing down the tower, using the gas
analysis equipment provided

Column pressure drop:

Column Temperature:82 F = 27.77C

Atmospheric pressure: 1 atm

14

Table 3.2 Raw Data

Readings at inlet
From Hempl
From Flow meters
Apparatus & Sample

Readings at outlet
From Hempl
Apparatus & Sample

point S1

point S2

Trial No.

F3

F2

V1

V2

V1

V2

1
2
3

(L/min)
9
11
11

(L/min)
18
18
18

(ml)
20
30
40

(ml)
3.7
2.6
1.1

(ml)
20
30
40

(ml)
1.8
1.3
0.55

Nomenclature:
F3 = flow rate of carbon dioxide
F2 = flow rate of air
V1 = volume of gas sample taken in Hempl apparatus (ml)
V2 = corresponds to amount of gas absorbed in Hempl apparatus (ml)
Appendix B. Sample Computation
35

Calculating for the mole fractions:

Y i=

V2
i
V1

( )

Y o=

V2
o
V1

( )

Trial #1.
Y 1=

( 4.820 ) i

Y 1=

= 0.24

( 4.320 ) o=

0.22

Calculating for the Volume Flow Rate (Fa):

Fa =

Y iY o
( F 2 + F 3)
1Y o

Trial #1.
F 1=

( 18+9 )
( 0.240.22
10.22 )

F1 = 0.6923 L/min
Calculating for the molar rate (G):
G=

P
(F )
RT a

Trial #1:
G=

1 atm
( 0.06923 L/min )
Latm
(0.08205
)(301.48 K )
molK

G = 0.0280 mol/min
Calculating for the Gas Absorbed (N):
N = G (Yi-Yo)
Trial #1.
36

N = 0.0280 mol/min (0.24 0.22)

N = 5.6 10^-4 mol/min

Measurement of Conversion Reaction

Experiment No.4
I. Objective
To determine the degree of conversion of the reactants mixed in a flask at
certain time.
II. Materials/Equipment Needed

0.1 M NaOH 250 ml

0.1 M EtOAc 250 ml

0.1 M HCl

Phenolphthalein

Iron Stand and Clamp

Pipette

Beaker

Timer

dropper

10 units 125 ml Erlenmeyer Flask

Reagent Bottles

III. Equipment Set Up

Figure 4.1 Titration Set-up
37

IV. Theory

The amount of NaOH (component A) reacted can be determined by

conducting NaOH balance over the reactor at steady state:
Moles of A in = Moles reacted + Moles of A out
FACAT = (FA + FB) CAi = Moles reacted + (FA + FB) CAO
Moles Reacted = (FA + FB) CAi - (FA + FB) CAO
Moles Reacted = (FA + FB) (CAi - CAO)
Moles Reacted (A or B) is a measure of conversion X%.
moles of A
moles od Amoles of A out
X=

X=

100( F A + F B)(C AiC AO)

( F A+ F B)C Ai
X=

(C AiC AO )
100
C Ai

Where:
C Ai=

FA
C AT
F A+ F B

38

V. Procedure
Reaction in a Flask
1. Mix 250 mL of standardized 0.1 M NaOH and 250 mL of standardized
of 0.1 M EtOAc in 1 L flask and secure stopper.
2. After say 1 hour of mixing, take 10 mL sample and place in the
filtration flask.
3. Quench this sample with 10 mL of 0.1 M HCl then add
phenolphthalein indicator.
4. Titrate this mixture with 0.1 M NaOH until end point is reach. Note
volume used.
VI. Results and Discussion
Table 4.1 Concentration and percent conversion of NaOH with respect to
time.
Sample

Time (min)

Conc. of NaOH

% conversion

1
2
3
4
5
6
7

10
20
30
40
50
60
70

(M)
0.0880
0.0860
0.0840
0.0840
0.0840
0.0830
0.0640

0.12
0.14
0.16
0.16
0.16
0.17
0.36

It is observed from Table 4.1 that in the 3rd Trial from samples 3-5, refer to table
4.2, % conversions are the same. Thus, it is closer to steady state. The data
collected from that trial is used for the computation for the percent conversion as
presented in Table 4.2.
From regression analysis, the reaction is in second order, and the linear equation
is presented as

39

1
1
=
kt
C Ao C Ai
Where k is the slope of the linear equation. From the regression analysis, k =
-0.05193850812 L/mol-min. And the complete reaction equation is given by
10=

1
+0.05193850812t
C Ai

VII. Conclusions
Based on the tabulated results in Table 4.1, it is concluded that as the time
increases, the concentration of NaOH increases resulting to an increase of the
conversion.
Time, concentration and the percent conversion is proportional to each other.
All are increasing dramatically.
VIII. References
Unit Operations of Chemical Engineering, 4th Edition (McCabe, W.L., et.al,)
Principles of Transport Processes and Separation Processes (Geankoplis, C.J.)

40

APPENDICES
Appendix A. Experimental Data
Table 4.2 Mixing in a Flask Raw Data

Sample

Time

Trial

(min)

No.

10

20

30

40

50

60

70

1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3

Sample
Volume
(ml)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10

Standard

Volume

Volume

Solution
EtOAc NaOH

HCl

NaOH

Quench

Back-

(ml)

(ml)

0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1

0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1

(ml)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10

titer (ml)
7.5
3.2
1.2
4.3
1.8
1.4
1.7
2.3
1.6
9.0
2.5
1.0
2.7
2.8
1.6
1.1
0.9
1.7
0.3
2.7
3.6

Appendix B. Sample Computations

Initial concentration of NaOH in the flask

250 mL

1L
0.1 moles NaOH
=0.25 L NaOH
=0.025 moles NaOH
1000 mL
1L
41

M=

moles of solute
ave . volume of solution sample

0.025 mole NaOH

=9.562841531 M
0.002614285714 L

Volume of HCI used and not used in quenching the sample

VHCL used =

concentrationof NaOH
concentrationof HCl

VHCL used =

0.1 M
0.1 M x 2.614285714 mL = 2.614285714 mL

x ave. volume of titrated NaOH

Vnot used = VHCl - Vused

V3 = 10 mL 2.614285714 mL = 7.385714286 mL

Amount of reacted and unreacted NaOH in the sample

NaOH
reacted NaOH:
n1 = concentration NaOH x volume of NaOH titrated
n1 = 0.1 M x 0.002614287514L
n1 = 0.0002614287514 mole
42

moles of HCI reacted with NaOH in sample(n1)

concentrationof HCI x volume of HCI reacted with NaOH sample

1000

0.1 M x 7.385714286 mL
1000

moles of HCl reacted with NaOH in sample = 0.0007385714286 mole

n2 = n1
n2 = 0.0007385714286 mole

Concentration of reacted NaOH in the sample

CNaOH =

n2
X 1000 =
v

0.0007385714286mole
10 mL

x 1000 = 0.07385714286

Percentage conversion of NaOH

X=

(CNAoH )
(1 CNAoH
,0)

x 100% =

x 100=99.23
(1 0.07385714286
9.562841531 )

Appendix C. Documentation

43

Drying Curves
Experiment No.5

44

I.

Objectives:
1. To produce drying and drying rate curves for a wet solid being dried with
air of fixed temperature and humidity.
2. To determine the critical and equilibrium moisture contents, bound and
unbound moisture of the wet solid being dried.

II.

Material/Equipment Needed

Tray Drier

Sieve Shaker

Sand (+20 mesh)

2-sling psychrometers

8-thermometers

Weighing instrument

Oven (if necessary)

Stop Watch

Water

Container

III.

Equipment Set Up

IV.

Theory

Humidity of an air-water vapor mixture (H):

45

H = Mass of Water (kg) Mass of Dry Air (kg)

Moisture content of a solid (X):

X = Mass of Water (kg) Mass of Dry Solid (kg)

Equilibrium Moisture Content of a Solid (Xe): Is the final moisture content

of a solid after being brought into contact with a stream of air (having
humidity H and temperature T) long enough, for equilibrium to be
reached. Is expressed in the same way as X.

Free Moisture Content of a solid: Is the moisture above the equilibrium

moisture content. Is the only moisture that can be removed by drying
under the given drying conditions.

Critical Moisture Content of a solid (Xc): Is the solid moisture content

attained, during the drying process, when the entire surface of the solid is
no longer wetted.

Experimental Determination of the Rate of Drying Curve

The rate of drying R is defined as the mass of liquid evaporated by unit time
and by unit of exposed surface area for drying. It can be mathematically expressed
by
S
R=
A

dX

(1)
dt

Where:
R = drying rate (kg H2O/sm2)
S = weight of dry solid (kg)
A = exposed surface area for drying (m2)
46

X = solid moisture content (kg H2O/kg dry solid)

t = time (s)

To experimentally determine the rate of drying for a given material (case study
sand), a sample is placed in a dryer and under constant drying conditions, the loss
in weight of moisture during the drying process is determined at constant time
intervals.

With the data obtained from the batch experiment, a plot of the solid moisture
content X versus time can be made (Figure 1). From this plot, the rate of drying
curve can be obtained by measuring the slopes of the tangents drawn to the curve,
which give the values of dX/dt at given values of t. The drying rate R is
calculated for each point using equation (1). The drying rate curve is obtained by
plotting R versus the solid moisture content X as in figure 2.
The plot of the rate of drying curve can presents several shapes but generally the
two major points constant and falling rate period are present. At time zero the
initial moisture content of the solid is shown at point A or A depending on the
solid temperature. At point B the surface temperature as attained its equilibrium
value and the constant rate period starts. This period continues as long as the
water is supplied to the surface as fast as it evaporates. At point C, the solid
critical moisture content Xc is attained. At this point there is no insufficient
water on the surface to maintain a continuous film of water and the first falling
rate period starts. The wetted area of the solid continually decreases until the
surface is totally dry at point D. At this point begins the second falling rate period,
that continues until the equilibrium moisture content of the solid is reached, at
point E.
Figure1: solid moisture content X versus time for constant drying conditions

47

Figure2:

drying

Rversus

solid

rate
moisture

content X for constant drying conditions

V.

Procedure

Design a detailed procedure that will attain the experimental

objectives.

Partial Procedure:

Screen sufficient dry sand (bone dry) to approximately 500 mesh using
sieve shaker to fill the four drying trays to a depth of about 10 mm
each.

Weigh accurately the dry sand that will be loaded to four drying trays.
Also, weigh accurately each empty tray.

Place the sand on a suitable container and saturate it with water.

Remove the sand from the container and drain the excess free water.

Load the sand evenly and smoothly into the drying trays, taking care
to avoid any spillage. The total weight of the wet sand should be noted
before drying commences.
48

VI. Result and Discussion

Table 5.1 Moisture Content
Time

10

15

20

25

30

35

40

45

50

55

(min)
Moist

0.45

0.43

0.40

0.36

0.32

0.28

0.23

0.23

0.18

0.16

0.16

0.16

ure

96

45

67

49

31

13

96

96

38

99

85

85

Cont
ent

Table 5.2 Free Moisture Content

Time

10

15

20

25

30

35

40

45

50

55

(min)
Moist

0.2911

0.26

0.23

0.19

0.15

0.11

0.07

0.07

0.0153

0.00

60

81

64

46

28

10

10

ure

14

Conte
nt

Figure 5.1 Drying Curve

VII.

Figure 5.2 Drying Rate Curve

Conclusions
After performing the experiment, conclusions attained from processing the data.

The major conclusion drawn from this experiment with regards in constructing drying
49

curves for wet solids is the fact that the humidity and conditions of the air surrounding
plays key role in the drying process. As theory dictates, drying is the extraction of water
from solids. The transfer of this water content will now be dependent of the water content
present surrounding the wet solid.

VIII. References

GEANKOPLIS, C. J. Principles of Transport Processes and Separation

Processes, 4th Edition, Prentice Hall, New Jersey (2003).

50

APPENDICES

Appendix A Raw Data

Mass of Bone Dry Sand: 718 g

% relative humidity was taken from the psychometric chart found in Perrys and Green
8/ed Handbook

Table 5.3 Weight of Sand

Time (min)
Wt of Wet
Sand & Tray

10

15

20

1048 1030 1010 980

(g)

95
0

25
920

30
89
0

35

40

45

890

850 840

50

55

83

839

Time (min)

10 15

25

30

40 45

55

Dry Bulb Temp (oC)

30 30

0
3

30

30.5

5
3

30 30

0
3

30.5

28 28

0
2

28.5 28.5

0
2

27 28

0
2

29

0
2

Wet Bulb Temp ( C)

8
9
0

%RH

90 90

8
9
0

91

89

8
9
0

80 90

8
9
0

94

Table 5.4 Entering Air Condition

Time (min)
Dry Bulb Temp (oC)

10

20

25

30

35

40 45 50

55

42 40

5
4

42

40

42

40

40 42 40

42

0
51

Wet Bulb Temp (oC)

34 29

31

28

29

30.

30 33 30

33

%RH

60 45

0
5
0

47

40

39

1
50

50 56 50

56

Table 5.5 Outgoing Air Condition

Table 5.6 Preheated Air Condition
Time (min)

10

15

20

25

30

35

40

50

55

63

63

Point 1

56

46

57

61

62

62

62

5
6

Point 2

2
2

34

32.

32.5

34

34

34

34

2
3

34

34

Point 3

4
3

32.5

5
32.

32

33

34

34

33.

4
3

33.9

34

Point 4

2
4

42

1
42.

42

8
44

4
4

43

44

Point 5

1
5

62.5

5
63.

58

62

55

55

45

4
5

63

54

Point 6

1
4

44

5
46

48

48.

49

50

48

6
5

51

51

Point 7

1
4

54

43

50

5
54

54

55

52

1
5

55

55

41

42

44

Appendix B Sample Computation

Moisture content at t = 0

Xt=

W W s 1048718
gTotalWater
=
=0.45961003
Ws
718
gSolid

Equilibrium Moisture Content at from t = 50min and t = 55min

X =

W W s 839718
gTotalWater
=
=0.1685327
Ws
718
gSolid

Computing for the free moisture content at t = 0

52

X =X t X =0.459610030.1685327=0.2910864

gTotalWater
gSolid

Table B.1 Data For Determining Drying Rate Curve

Point
A-B
B-C
C-D
D-E

X1
0.29
0.235
0.07
0.025

X2
0.235
0.07
0.025
0

t1
0
11
35
41

X
0.055
0.165
0.045
0.025

t2
11
30.5
41
55

t
11
19.5
6
14

Xave
0.2625
0.1525
0.0475
0.0125

R
269.92481
456.79584
404.88722
96.401719

Drying rate R was solved by using the formula

R=

W Solid dX
A dt

We get the value for A by using the properties and date of sand, since sand is the
dominating sample.
Sand =1.33

A=

g
0.00133 g
=
3
3
cm
mm

V sand
W Sand
718 g
=
=
h sand Sand hsand
0.00133 g
10 mm
mm3

A=53984.9624 mm

dX/dt was taken as the averages X/t of the tangents within the curve between
two points. Plotting the curve in Figure 5.2 was done by plotting R with the arithmetic
mean of the values of X between two points.
Between Point A and B
718 gSand
R=
2
53984.9624 mm

gTotalWater
gSand
(110 ) min

( 0.290.235 )

53

R=269.9841

gTotalWater
2
minmm

Appendix C. Documentations

Power Requirement for Agitation

Experiment No.6

54

I. Objectives:
1. To be able to determine the effect of impeller speed on the power requirement for
agitation with and without baffles.
2. To be able to determine the effect of impeller dimensions (straight blade turbine)
on the power requirement for agitation with and without baffles.
II. Materials/Equipment Needed:

20 L distilled water

Agitator (with three types of straight blade impeller)

Wrench

1 pc 2-L plastic Graduated Cylinder

1 pc 5-L plastic Beaker

1 pc Vernier Caliper

1 pc Ruler

1 pc 100-ml glass beaker

III. Equipment Set-Up

Figure 6.1 Agitator (with three types of straight blade impeller)

IV. Theory

55

Agitation refers to the induced motion of a material in a specified way,

usually in a circulatory pattern inside some sort of container. Liquids are agitated
for a number of purposes, depending on the objectives of the processing step.
These purposes include suspending solid particles, blending miscible liquids,
dispersing a gas through the liquid in the form of small bubbles, dispersing a
second liquid, immiscible with the first, to form an emulsion or suspension of fine
drops and promoting heat transfer between the liquid and a coil or jacket.
The power requirement is an important factor to consider especially in
designing an agitated tank. The power requirement is important to estimate the
power needed to rotate or drive the impeller. To estimate the required power at a
given speed, empirical correlations of power with the other variables of the
system are needed given the important measures of the tank and impeller, the
distance of the impeller from the tank floor, the liquid depth, and the dimensions
of the baffles, the number and arrangement of the baffles and the number of
blades in the impeller. The variables that enter the analysis are the important
measurements of tank and impeller, the viscosity
the liquid, the speed

and the density

of

and because Newtons law applies, the dimensional

gravity constant gc .

Power requirement formula involving speed and force:

P = (T) (Ni) = (F) (l) (Ni)

(Eq. 1)

Or
P = (F) (l) [Ni (2pi/60)]

(Eq. 2)

Where:
2pi/60 = conversion factor to convert impeller speed rpm to rad/s
l = equal to 0.098 m as measured
Using Equation 2, Power Requirement in Agitation is generated.

56

V. Procedure
Preliminary Steps:
1. Disconnect the cord between the torque arm and the balance before removing the
motor or baffles.
2. Measure the dimensions of the impeller and attach the shaft assembly. Record the
relevant dimension of the baffles and the tank, i.e. width, height, and diameter.
3. Place baffles in the tank, tighten the screw by hand, and attach the cord of the
balance back to the torque arm. Check the dynamometer balance for correct
setting.
4. Close the discharge valve before filling the tank with water. The liquid height
should not exceed 350 mm.
5. Record the water temperature and determine the density and absolute viscosity
from appropriate tables in available literature.
6. Ensure that the speed control knob (next to the on/off switch) is set at zero.
7. Release the support screw and let the balance come to rest. Tighten the support
screw when the balance is in its rest position and record the initial value.
Experiment Proper in Determining Power Requirements:
1. Switch on the agitator and ensure that the red indicator is lit.
Shutdown operations:
1. Set the speed to zero before turning off the power.
2. Remove the impeller and baffles from the tank, clean them, and place the cleaned
baffles back.
3. Position the outer sleeve of the force balance at its up-most position and lock it so
that there is no tension on the cord or balance.
57

VI. Results and Discussions

Table 6.1 Power requirement in different impeller dimensions without baffles.
Without baffles
Impeller A
(W = 0.0209 m)

Impeller B
(W = 0.0428 m)

Impeller C
(W = 0.0652 m)

Speed,

Force,

Power,

Speed,

Force,

Power

Speed,

Force,

Power,

in rpm
0
50
100
150
200
250
300

in N
0
0
0
0.03
0.08
0.13
0.16

in J/s
0
0
0
0.0462
0.1642
0.3335
0.4926

in rpm
0
50
100
150
200
250
270

in N
0
0
0.1
0.12
0.2
0.32
0.35

, in J/s
0
0
0.1026
0.1847
0.4105
0.8210
0.9698

in rpm
0
50
100
150
200
250

in N
0
0.01
0.01
0.09
0.15
0.39

in J/s
0
0.0051
0.0103
0.1385
0.3079
1.0006

Impeller speed vs Power requirement without baffles

1.2
1

Power Requirement in J/s

0.8

at 0.0209

0.6

at 0.0428

0.4

at 0.0652

0.2
0

50 100 150 200 250 300 350

Speed in rpm

58

Figure 6.1
Table 6.1 shows the tabulated results after the power requirement computation
given the impeller speed and force exerted in different impeller dimensions without
baffles.
Figure 6.1 shows the relationship between speed and power requirement given the
three impeller dimensions corresponding to the three different colors in the curve with
baffles. The relationship between power and speed is shown in a figure to visually
differentiate the effect of the speed in the power requirement in impeller without baffles.
Table 6.2 Power requirement in different impeller dimensions with baffles
Impeller A
(W = 0.0209 m)
Speed, Force, Power,
in rpm
0
50
70
100
130
150
170
200
230
250

in N
0
0
0
0
0.01
0.02
0.1
0.2
0.65
0.7

in J/s
0
0
0
0
0.0133
0.0308
0.1745
0.4105
1.5343
1.7959

With baffles
Impeller B
(W = 0.0428 m)
Speed,
Force, Power,
in rpm
0
50
70
100
110
120
130

in N
0
0
0.01
0.1
0.3
0.5
0.75

in J/s
0
0
0.0072
0.1026
0.3387
0.6158
1.0006

Impeller C
(W = 0.0652 m)
Speed, Force, Power,
in rpm
0
50
60
70
80
90
100
110
120

in N
0
0
0
0.02
0.08
0.12
0.31
0.5
0.52

in J/s
0
0
0
0.0144
0.0657
0.1108
0.3181
0.5644
0.6404

Impeller speed vs Power requirement with baffles

2
1.5
1
Blade A in
at J/s
0.0209
Power requirement

Blade B

Blade C

0.5
0

50

100

150

200

250

300

Speed in rpm

Figure 6.2
59

Table 6.2 shows the tabulated results after the power requirement computation
given the impeller speed and force exerted in different impeller dimensions with baffles.
Figure 6.2 shows the relationship between speed and power requirement given the
three impeller dimensions condition corresponding to the three different colors in the
curve with baffles. The relationship between power and speed is shown in a figure to
visually differentiate the effect of the speed in the power requirement in different impeller
dimension with baffles.

VII. Conclusion
The power requirement increases either the agitation has baffles or without as the
impeller speed is increased. Hence, impeller speed showed significant effect on the power
requirement either when agitation is with or without baffles.
It is also observed that as the dimension of the impeller is increased, power
requirement is also increased. Therefore, the dimension of the impeller also showed
significant effect on the power requirement when agitation with or without baffles.
In addition, it also concluded that using baffles decreases the power requirement
for agitation at constant impeller speed.
VIII. Reference
Geankoplis CJ. 2003. Principles of Transport Processes and Separation Processes

60

APPENDICES
Appendix A. Data
Raw Data
A. Preliminary Data:
Table 6.3 Physical Properties of the material and equipment used
Physical Properties
Density of water at T =
28 oC (g/ml)
Viscosity of Water at T =

0.9965 g/ml
0.858 Pa.s

28 oC (Pa.s)
Tank Dimensions

61

Diameter of the Tank, Dt

0.2860 m

(m)
Water Level or height

0.306 m

(m), H
Length of Lever arm (m)

Impeller Width, W
Impeller Diameter, Da
Baffle Diameter, J

0.098 m
Impeller Dimensions
Blade A
Blade B
0.0209
0.0428 m
m
0.176 m
0.176 m
Baffle Dimension
0.0249 m

Blade C
0.0652 m
0.176 m

Experimental Data
Table 6.4 Impeller Speed and Force exerted by agitator using different dimensions of
impellers.
Without baffles
With baffles
Impeller A
Impeller B
Impeller C
Impeller A
Impeller B
Impeller C
(W = 0.0209 (W = 0.0428 (W = 0.0652 (W = 0.0209 (W = 0.0428 (W = 0.0652
m)
Spee Forc

m)
Spee Forc

m)
Spee Forc

m)
Spee Forc

m)
Spee Forc

m)
Spee Forc

d, in

e, in

d, in

e, in

d, in

e, in

d, in

e, in

d, in

e, in

d, in

e, in

rpm
0
50
100
150
200
250
300

N
0
0
0
0.03
0.08
0.13
0.16

rpm
0
50
100
150
200
250
270

N
0
0
0.1
0.12
0.2
0.32
0.35

rpm
0
50
100
150
200
250

N
0
0.01
0.01
0.09
0.15
0.39

rpm
0
50
70
100
130
150
170
200
230
250

N
0
0
0
0
0.01
0.02
0.1
0.2
0.65
0.7

rpm
0
50
70
100
110
120
130

N
0
0
0.01
0.1
0.3
0.5
0.75

rpm
0
50
60
70
80
90
100

N
0
0
0
0.02
0.08
0.12
0.31
0.5
0.52

62

Appendix B. Sample Computation

Introducing one computation as a basis for the others. Since, power is the only required,
we can acquire it by directly substituting the values in the equation given as:
P = (F) (l) [Ni (2pi/60)]

eq.2

Sample:
Given: (Taken from Table 6.4)
Ni =150 rpm
F = 0.03 N
Solution:
Direct substitutions of the given to equation 2 yield:
P = (0.03 N) (0.098 m) [150 rpm (2pi/60)]
P = 0.0462 J/s

63

Cation Exchange
Experiment No.7

I.

Objective of the Experiment

1.
2.
3.
4.

II.

Characterize Dowex Monosphere 650C (H) cation- exchanger;

Establish Na+- H+ exchange isotherm at 30 C;
Estimate adsorption parameters;
Derive mathematical equation for uptake.

Materials/Apparatus/Equipment:

III.

Dowex Monosphere 650C (H)

Solutions of different concentration of sodium chloride (NaCl)
Hydrochloric acid (0.1 N) and sodium chloride (0.1 N) solutions
Erlenmeyer flask of 125 ml capacity
A rotary shaker (New Brunswick Scientific rotary shaker model G25)
A pH meter (ORION 210-A)

Theory
Ion-exchange processes are basically chemical reactions between ions in solution
and ions in an insoluble solid phase. The techniques used in ion exchange so closely
resemble those used in adsorption that for the majority of engineering purposes ion
exchange can be considered as a special case of adsorption.
In ion exchange certain ions are removed by the ion-exchange solid. Since electro
neutrality must be maintained, the solid releases replacement ions to the solution. The
first ion-exchange materials were natural-occurring porous sands called zeolites and
are cation exchangers. Positively charged ions in solution such as Ca 2+ diffuse into the
pores of the solid and exchange with the Na+ ions in the mineral.
where

the

solid. This is the

represents

the

basisfor

softening of water. To regenerate a solution of NaCl is added which drives the

64

reversible to reaction above of the left. Almost all of these inorganic ion-exchange
solids only exchange cations.
Most present-day ion-exchange solids are synthetic resins or polymers. Certain
synthetic polymeric resins contain sulfonic, carboxylic, or phenolic groups. These
anionic groups can exchange cations.
here the R represents

the solid resin. The

Na+ in the solid resin

can be exchanged

with H+ or other cations.

Similar synthetic resins containing amine groups can be used to exchange anions
and OH- in solution

IV.

Procedures
Resin Preparation
The Dowex Monosphere 650C (H) cation exchanger is supplied in H+-form.
Prior to use in the experiments, about 50 g of wet resin was placed in a 125-ml
Erlenmeyer flask.
The resin was conditioned by 5 cycles of rinsing with de-ionized water,
bringing to H+ form using 0.1 N HCl, rinsing, and then back again to Na +-form
using 0.1 N NaCl. Per cycle, 500 ml of NaCl and HCl was used to condition 50 g
of resin.
Each rinsing cycle lasted for one hour. A rotary shaker was used in agitating for
better contacting of resin and conditioning solution. Then, the conditioned resin in
H+-form was rid of adhering moisture by suction filtration. Finally, resin was
placed in a media bottle, covered with a paraffin film, and stored in the
refrigerator at 4C to prevent dehydration.
Resin Characterization

65

Water content. The water content of the hydrated resin in H +-form is

determined by noting the decrease of the weight of the resin placed in an
evaporating dish upon oven-drying (Memmert Um 500F Nr Oven) at 105C for
24 hours.
Resin Density. The density of Dowex Monosphere 650C (H) resin is given by the
manufacturer as approximately equal to 1.2 g / ml. However, experimental
determination of the density of Dowex Monosphere 650C (H) was still conducted
in order to countercheck the quoted value. First, 2 grams of resin was equilibrated
with 50 ml of 0.1 N HCl solution for 24 hours and then the swollen resin was
weighed. BOD bottle of known volume (determined experimentally) was filled
with 50 ml solution and the resin was allowed to settle into the bottom of the
bottle. After that, the bottle was weighed at thermal equilibrium. The volume, V
of the ion exchanger resin was computed using the following equation:

V =V b

(W b W )

(5)

where Vb is the volume of the bottle, Wb is the weight of the bottle content, W is
the dry weight of the Dowex Monosphere 650C (H) resin, and is the density of
the solution.
Density of the solution was determined experimentally at room temperature
using electronic balance (KERN EW150-3M) and densitometer (SARTORIUS
YDK O1).
The volume of the bottle was determined using the following procedure:
First, BOD bottle was dried with the cover in the oven for two hours at
105 oC. After that, the empty bottle was weighed with the cover and filled with
distilled water of known temperature. The volume of the bottle was then
determined using Equation 7.
Finally, the density of the resin,

was computed using the following

equation:

66

W /V

(6)

where W as defined previously, is the dry weight of the Dowex Monosphere 650C
(H) resin while V is the corresponding volume of it.
Resin Capacity. The total exchange capacity of the resin was given by the
manufacturer as equal to 1.9 equivalents / liter or approximately 1.56
milliequivalents / gram. However, the value was still verified using the procedure
given by Helfferich (1962): 2 grams of hydrated resin was placed in a 125 ml
Erlenmeyer flask and then equilibrated with 1.0 N NaCl solution. Effluent was
collected and the pH was determined using the pH meter. Resin capacity or Na+
+

uptake of the resin,

Na
q

was computed through the mass balance equation,

,i
,f
C
C
mw W

V
Na+ =
q

where V is the volume of solution in ml,

(7)

mw

is the mass of hydrated ion

exchange resin, W is the gram dry resin per gram hydrated resin,

,i
C

,f
and C

are the initial and final Na+ concentrations in the solution in meq/ml. By mass

67

balance,

,i
f
C
C

which is the amount of Na+ taken up by the cation exchanger is

equal to

,f
,i
C
C

or the amount of H+ released.

Equilibrium Experiment
For the determination of ion-exchange equilibrium, a batch method was
employed and carried out in a single set of eight NaCl concentrations with the set
having a duplicate. This was made by placing 2.0 g of conditioned resin in
individual 125- ml Erlenmeyer flasks containing 20 ml NaCl solution with varied
concentrations.
The concentrations of NaCl used in the experiment were 0.2 N, 0.3 N, 0.4 N,
0.5 N, 0.6 N, 0.7 N, 0.9 N and 1.0 N where N is the normality of the solution also
expressed as

milli-equivalents per liter (meq/L). Actual concentrations were

determined using a conductivity meter, which are shown in Appendix 7.2.

Twenty milliliters of NaCl solutions with varying concentrations were
obtained by diluting with the stock solution with de-ionized water.
The initial pH of the sample was measured. The flasks were then placed in the
incubator-shaker moving at 200 rpm and 30C. The solution was allowed to reach
equilibrium in 6 hours. The equilibrium pH in each flask was measured again.
Initial and equilibrium pH were converted to H+ concentration using Equation 6 to
determine the amount of H+ released to the liquid which by mass balance is equal

68

to the Na taken up by the cation exchanger. The Na uptake of the resin,

Na
q

was computed through the mass balance equation in Equation 7.

IV. Results and discussion

Resin Characteristics
It was found out through experimental investigation that the resin
has a density of 1.1866 grams per milliliter, water content of 0.5560 grams water
per hydrated resin, and resin capacity of1.0820 milli-equivalents (Na+) per gram
dry resin.

Cation-Exchange Equilibrium
The figure shows the sodium ion uptake of the cation-exchanger at different Na+

concentration at equilibrium here using the raw data in the Appendix.

Comparison of Equilibrium Uptakes

1.2
1
0.8
q (meqNa+/g solid)

Freundlich Isotherm

0.6

Langmuir Isotherm

0.4

Experimental Data

0.2
0
0

0.5

1.5

C (meq/mL)

Figu
re 10.1 Equilibrium uptake of Dowex Monosphere 650C (H) at different equilibrium
concentrations of sodium ion in comparison with the Langmuir and Freundlich
model.
69

Adsorption Parameters
As a result of regression analysis, it was determined that the
experimental data followed close to the ideal isotherm of the Freundlich Model
with

r =0.8471572829
The linear equation for the Freundlich Isotherm is given by
ln q=ln k + n ln C

Also from regression analysis, it was found that

n=0.2471361427

k =0.9814370797

mL 0.2471361427 m eq0.7528638573
g

Deriving the Mathematical Equation

By using the parameters achieved from the previous part, the mathematical
equation for the experimental data achieved is

q=0.9814370797 C

0.2471361427

V. Conclusion
Based on the experiment, the density of the resin is 1.1866 g/ml which is so close
to the commercially made resin which has a density of 1.2 g/ml. Water content is
0.5560 grams per hydrated resin and the resin capacity is 1.0820 meq. per gram of dry
resin.

The

adsorption

parameter,

k,

is

0.9814371^ml^0.2471361427meq^0.7528638573/g and the equation for the uptake is

q = 0.9814371c^0.2471361427, Freundlich equation.
VI. References
70

Dorfner K. 1991. Ion Exchangers, Walter de Gruyter and Co., Berlin.

Geankoplis CJ. 2003. Principles of Transport Processes and Separation Processes, 4 th
ed., Pearson Education, Inc., New Jersey.
Helfferich F. 1962. Ion Exchange, McGraw Hill, New York.
Muraviev D, Gorshkov V, Warshawsky A, Deker M. 2000. Ion exchange, New York.
Zagorodni A. 2006. Ion Exchange Materials: Properties and Applications, Elsevier
Publications, Amsterdam.

APPENDICES

Appendix A: Experimental Data

Table 7.1 Moisture Content Determination of Swollen Resin
Crucible
#
4
5
6

Wc (g)

, Wro
(g)

Wc +
Wr (g)

21.7618
16.7084
18.4129

2.006
2.0038
2.0026

22.6563
17.6061
19.2904

Notes:

Wr (g)

%Moisture
Content

0.8945
0.8977
0.8775
Ave.:

55.40877368
55.20011977
56.18196345
55.5969523

Wt.
water
(g)
1.1115
1.1061
1.1251

Wt. water/wt.
hydrated
resin (g/g)
0.554087737
0.552001198
0.561819634
0.555969523

wt. dry
resin/hydrated
resin (g/g), W
0.445912263
0.447998802
0.438180366
0.444030477

Wc weight condition resin

Wro initial weight of resin
Wr final weight of resin after swelling
71

Ave. average
W - the gram dry resin per gram hydrated resin
Table 7.2 Resin Density Determination
BOD
Wbc + Ww
#
Wb (g)
(g)
1
81.8508
137.5315
2
76.0435
131.6881
9
79.1582
134.2641
Notes: Wb- weight bottle
Wbc weight bottle with cover
Ww weight water

W(a), g
0
0
0

Ww, (g)
Vapp (ml)
55.6807
55.8
55.6446
56.1
55.1059
55.5
Vapp apparent volume
Vtrue true volume

Vtrue@
27.5 oC
55.8833
55.8471
55.3064

% rel.
error
0.1491
0.4528
0.3500

Table A.3 Density of 0.1 N HCl solution using densitometer at

27oC
Bouyancy,
W(fl), g
G (g)
HCl (g/ml)
-10.006
10.006
1.0006
-10.008
10.008
1.0008
-10.004
10.004
1.0004
Average
1.0006

Notes: W(a) weight of the solid plummet

W(a) W(fl)
W(fl) weight of the fluid
0.1 N HCl solution = G/Vtrue

G buoyancy =
HCl - density of

Table A.4 Volume and density of resin at 27oC

Wb + Wha
Wb + Wha + Wr
Wha + Wr
BOD#
Wb (g) Wro (g) (g)
(g)
(g)
Wr (g)
Vr (ml)
1 81.8508
2.0038
131.8808
138.6728
56.822
6.792
5.8833
2 76.0435
2.0049
126.0735
132.7755
56.732
6.702
5.8471
9 79.1582
2.0045
129.1882
135.8702
56.712
6.682
5.3064
Average:
Notes:

Wc weight condition resin

Wr final weight of resin after

swelling
Wro initial weight of resin
Ave. average

72

Table A.5 Resin Capacity

f (g)

Wcr (g)

3091
1312
0139

2.0048
2.0045
2.0043

Volume,
V of 1.0 N
NaCl
used (ml)
100
100
100

Initial
Conductivity

Initial Na+ Conc.

(meq/ml)

Initial pH

39.0
39.1
39.1

0.9412
0.9438
0.9438

7.16
7.17
7.12

Initial H+
conc.
(meq/ml)
6.9183E-08
6.7608E-08
7.5858E-08

Final pH
2.00
2.01
2.04

Final H+ conc.
(meq/ml)

Amount Na+
taken up (meq)

1.0000E-02
9.7724E-03
9.1201E-03

1.0000
0.9772
0.9120
Average:

Notes: Wf weight flask

Wcr weight conditioned resin
Amount Na+ taken up = Amount of H+ released = V x (Final H+ - Initial H+)

EF
#

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16

Table A.6 Raw Data (Na+ - H+ Exchange)

Wf +
Wf +
Wcr (g)
Wdcr
V
Wsoln. (g)
Wsoln. +
(g)
(ml
Wcr (g)
)
99.7637
105.3300
92.7512
108.6454
97.0368
108.3589
104.9354
106.7184
106.7550
104.4584
110.2461
99.4693
112.6516
104.6796
105.8744
110.8050

101.8184
107.4065
94.8133
110.6725
99.0703
110.3610
106.9934
108.9196
108.8720
106.6402
112.2808
101.5774
114.7009
106.7254
107.9297
112.8461

2.0547
2.0765
2.0621
2.0271
2.0335
2.0021
2.0580
2.2012
2.1170
2.1818
2.0347
2.1081
2.0493
2.0458
2.0553
2.0411

0.9123
0.9220
0.9156
0.9001
0.9029
0.8890
0.9138
0.9774
0.9400
0.9688
0.9035
0.9361
0.9100
0.9084
0.9126
0.9063

20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20

CNa+, i,
(meq/ml
)

Initial
Na+
(meq)

Initial
pH

0.2
0.2
0.3
0.3
0.4
0.4
0.5
0.5
0.6
0.6
0.7
0.7
0.9
0.9
1
1

4
4
6
6
8
8
10
10
12
12
14
14
18
18
20
20

7.28
7.29
7.3
7.28
7.53
7.53
7.39
7.39
7.24
7.25
7.26
7.27
7.20
7.19
7.16
7.17

Initial H+
Conc.
(meq/ml)

Initial
Amount H+
(meq)

Final
pH

5.248E-08
5.129E-08
5.012E-08
5.248E-08
2.951E-08
2.951E-08
4.074E-08
4.074E-08
5.754E-08
5.623E-08
5.495E-08
5.37E-08
6.31E-08
6.457E-08
6.918E-08
6.761E-08

1.05E-06
1.026E-06
1.002E-06
1.05E-06
5.902E-07
5.902E-07
8.148E-07
8.148E-07
1.151E-06
1.125E-06
1.099E-06
1.074E-06
1.262E-06
1.291E-06
1.384E-06
1.352E-06

1.49
1.55
1.5
1.52
1.45
1.46
1.44
1.43
1.41
1.39
1.38
1.38
1.41
1.38
1.33
1.31

Final H+
Conc.
(meq/ml)
0.0324
0.0282
0.0316
0.0302
0.0355
0.0347
0.0363
0.0372
0.0389
0.0407
0.0417
0.0417
0.0389
0.0417
0.0468
0.0490

Notes: Wf weight of flask

CNa+, i initial sodium ion concentration of the solution in the aqueous solution
Wsoln weight of the solution
Wcr weight
conditioned resin
V volume of the solution
Wdr weight dry resin
Appendix B. Sample Computation CNa+, f - final or equilibrium sodium ion concentration in the aqueous solution;
Linear Regression/Regression Analysisalso expressed as C
Table A.7 shows the valuses used for regression analysis in determining the isotherm to
be used for the acquired data.

68

Table A.7 Table for Regression

Analysis
Freundlich
ln C
1.7861
8
1.7614
2
1.3152
8
1.3100
7
1.0092
3
1.0070
4
0.7685
2
0.7704
6
0.5778
6
0.5810
7
0.4180
9
0.4180
9
0.1495
4
0.1528
0.0479

Langmuir

ln q

1/C

1/q

0.34334

5.96658
7

1.40964
2

0.49217

5.82072
2

1.63585
8

0.37005

3.72578
2

1.44780
7

0.39899

3.70644
9

1.49031
3

0.24093

2.74348
4

1.27242
7

0.24833

2.73747
6

1.28188
7

0.22992

2.15656
7

1.25849
5

0.27404

2.16076
1

1.31527

-0.1891

1.78221
4

1.20816
7

0.17316

1.78794
9

1.18906
1

0.08034

1.51906
4

1.08365
8

0.11575

1.51906
4

1.12271
2

0.15654
0.08578
0.02469
3

1.16130
5
1.16509
4
1.04909
8

1.16945
4
1.08956
2
0.97561

71

3
0.0502
4

0.07770
2

1.05152
5

0.92524
1

For Freundlich, r2 = 0.8470832766. While for Langmuir, r2 = 0.7649011693.

As a result of the analysis, Freundlich Isotherm is used.

q=k C n

Solving for the parameters

Using the linearized form of the Freundlich Model

ln q=ln k + n ln C
And getting the values for the linear parameters

yintercept =ln k =0.01873737359

m ( slope )=n=0.2471361427
Getting the value of k

k =e0.01873737359=0.9814370797

72

Batch Distillation with Packed Absorption Tower

Experiment No.8

I.

Objectives:
1. To be able to determine the average concentration of a specified volume
of the distillate that is obtained from a feed mixture of known
composition by operating the distillation unit at constant reflux.
2. To be able to predict the time required to obtain a particular concentration
of the distillate using experimental data.

II.

Materials/Apparatus:

Reboiler System
Special Vessel
Heat Exchanger
fractionating column
Overhead Condenser
Product Cooler
Product Receiving Vessels
Refractometer
Thermometer
Beaker
Timer/Stopwatch
Culture tubes
Graduated Cylinder
Pipette
73

Aspirator

III. Experimental Set-up:

74

IV.

Theory
Distillation is the core operation in oil refineries and is most widely used to
separate liquid mixtures into their several constituents. It is based on the difference
in composition between a liquid mixture and its vapor caused by dissimilar
effective vapor pressure, or volatilities, of the components. When such
dissimilarity does not exist, as at an azeotropic point, it is not possible for
separation to occur effectively by simple distillation and more complicated
methods have to be employed.
Distillation is the most widely used method of separating liquid mixtures
into their various components (Coulson et al., 1996). In this method, the
separation of the various components in the liquid mixture depends on the
volatility of the components. During distillation, the components are distributed
between a vapor phase and a liquid phase where the vapor phase is created from
the liquid phase by vaporization at the boiling point (Geankoplis, 2003). In the
process, the vapor phase is in contact with the liquid phase and mass is transferred
from the liquid to the vapor and from the vapor to the liquid. The liquid and vapor
generally contain the same components but in different relative quantities. The
liquid is in equilibrium with vapor where the liquid is at its bubble point and the
75

vapor is at its dew point. The more volatile component is progressively transferred
to the vapor phase and the less volatile condenses out in the liquid resulting to an
increase in concentration of the more volatile component in the vapor and a
decrease in concentration of the less volatile component in the liquid (Foust,
1980).
There are two main methods in distillation. The first method involves the
production of a vapor by boiling the liquid mixture to be separated in a single
stage and recovering and condensing the vapors. The second method involves the
returning of a portion of condensate to the still or rectification. Moreover, there
are three main types of distillation that occur in a single stage that do not involve
rectification namely, flash distillation, simple batch distillation or differential
distillation, and simple steam distillation.

In simple batch distillation, the more volatile component is evaporated

from the still which therefore becomes progressively richer in the less volatile
constituent. Distillation is continued, either until the residue of the still contains a
material with an acceptably low content of the volatile material, or until the
distillate is no longer sufficiently pure with respect to the more volatile
component (Coulson et al., 1996).
The batch distillation experiment involves the use of reflux. Since batch
distillation does not give good separation unless the relative volatility is very
high, a rectifying column with reflux is used in many cases to improve the
performance of the batch still (McCabe et al. 2001). Reflux ratio (R) is defined as
the ratio of the quantity of liquid reflux per (L 0) unit quantity of product removed
from the process unit (D) as given in equation 1 below.
Lo
R=Lo / D R= D

(1)

76

In batch distillation, the mixture is

constantly being depleted of its more
volatile

components,

hence,

the

composition in the still pot and vapor

changes continuously with time.
Figure 1 shows a simple still of a
batch distillation column. Originally,
a charge
Figureof1.L1Simple
moles of
batch
components
distillation

A and B with a composition of x 1 mole fraction of A is placed in the still. At any

given time, there are L2 moles of liquid left in the still with composition x 2, and the
composition of the vapor leaving in equilibrium is y. A differential amount dL is
vaporized. To relate the total moles of feed at the beginning and at the end, the
equation below is obtained from the material balance over the component in a
batch distillation column. Equation 2 is commonly known as the Rayleigh
equation.
x1

L1
dx
ln =
L2 x yx
2

The integration of equation (2) can be done graphically by plotting

1
y x

against x. The total area under the curve is calculated from x 1 to x2 and

consequently the L2 moles of liquid left in the still is obtained. The equation for
(3)

average composition of a specified volume of the distillate can be obtained

through material balance as shown in equation 3.
y_ave = (L_1 x_1-L_2 x_2) / (L1- L2 )
V. Procedure:
A. Preparation of Standard Calibration Curve
1. Mix specific amounts of ethanol (analytical grade) with distilled water to make
solutions which correspond to 20, 40, 60, and 80 percent by weight ethanol. By
using a refractometer, measure the refractive index of each solution.
77

(2)

2. Also determine the refractive indices of pure distilled water and pure ethanol.
These correspond to 0 and 100 percent by weight ethanol, respectively. Check the
measured data with those given in a handbook.
3. Make a graph of percent by weight ethanol (y-axis) vs. refractive index (x-axis) at
ambient temperature.
B. Preparation of Feed
Prepare 27 liters of by approximately 30% by weight ethanol (technical grade) in
water. Stir well. Take a 2-ml sample and determine its refractive index.
C. Pre-startup Operation
1. Open all vents.
2. Close all drain valves, steam supply valve, and steam regulating valve. Also check
that the reboiler steam inlet valve is closed.
3. Close the reflux control valve, recycle valve, the valve which connects the two
product receivers, and the soft water inlet valve.
4. Open the seal of the cylindrical still and charge the feed into it by means of a
siphon until it is about 2/3 full.
5. Allow soft water to flow through the pipeline. As soon as a steady flow is
obtained, open trapped in the lines.
6. Provide each thermometer pocket with a 0-1000C thermometer.
D. Start-up Operation
1. Open the by-pass valve. Allow steam to surge through the drain and release
unconsensable gases.
2. Close the by-pass valve and slowly open the steam supply valve. Ensure that the
steam supply pressure gauge indicates a value greater than 20 psig.
3. Slowly adjust the regulating valve until the regulated steam pressure gauge
registers 10 psig. Then open the steam inlet valve. Ensure that the pressure is
maintained at 10 psig.
E. Experiment Proper
1. Once the liquid mixture in the still starts to boil, operate at total reflux for about
20 minutes.
78

2. Open the reflux control valve to give total offtake of products. Note the time to
fill the upper product receiver from lower to the upper on it.
3. Open the recycle valve to drain the product back to the reboiler and then close it
again.
4. Once again operate at total reflux for a few minutes. Then adjust the reflux control
valve so that it is approximately 1/6th open. Note the time to fill the product
receiver to the same marks as in step E2. Withdraw the distillate into a 2-liter
graduated cylinder.
5. At regular intervals (i.e. 5-minute periods), simultaneously take samples of the
distillate and the liquid mixture in the still. Shake each sample well and determine
the refractive index of each. Record the temperature during each sampling
operation. Continue the distillation and sampling operation until about 3 liters of
the distillate are collected.
F. Shutdown Operation
1. Set the reflux control valve to total reflux.
2. Close the steam regulating valve. Carefully vent the residual steam in the reboiler
through the by-pass valve.
3. Close the reboiler steam inlet valve, steam regulating valve, and the steam supply
valve.
4. Turn off the condenser cooling water when boiling has stopped.
5. Close the soft water supply valve.
6. Allow the bottoms to cool and then drain to a suitable receiver.
VI. Results and Discussions:
Table 8.1 Process Data in determining the Concentration of the Distillate and
Bottoms using the calibration curve.
Refractive Indices

Concentration from Calibration Curve

Bottoms

Distillate

Bottoms

Distillate

1.3501
1.3498
1.3493
1.3491
1.3489
1.3485
1.3483
1.3476

1.3630
1.3632
1.3629
1.3629
1.3631
1.3628
1.3629
1.3627
1.3629

32.1
31.8
30.5
30.2
29.9
29
28.8
27.5

74.5
78
74
74
77.9
73.9
74
72

79

Plotting the Concentration from the calibration curve of the Bottoms and
Distillate vs. Time

Concentration vs. Time

90
74.5

80

78

74

77.9

77.9

73.9

70
60
50

Concentration

Bottom

40

32.1

31.8

30.5

30.2

29.9

29

10

15

20

25

30

30

Distillate

20
10
0

35

Time

Figure 8.1 Concentration by % weight vs. Time of the solution of water and
ethanol from the calibration curve

SHOW DATA ON average concentration of a specified volume of the distillate that is

obtained from a feed mixture of known composition at constant reflux

VII. Conclusion
80

Based on the table 7.1, the concentration of the distillate is higher than the
concentration of the bottom. Using the calibration cure by plotting the relationship
between the refractive index of the solution versus time interval, we did able to
predict the values for the concentration of the bottom and distillate using the
formed curved known as the calibration curve for this experiment. Using this
calibration curve, we will be able to predict the concentration of the bottom and
distillate at any time.
VIII. Reference
Chemical Engineering Laboratory Instructional Manual No. 51B-6 of the
University of San Carlos

APPENDICES
Appendix A. Raw Data

81

Table 8.2 Refractive Indices of Ethanol Water Solution

Ethanol Concentration (Wt. %)
0
20
40
60
80
99.5

Refractive Index
1.3325
1.3434
1.3539
1.3602
1.3631
1.3599

Time to fill the receiver at total reflux

6 mins. and 12 secs.

Time to fill the receiver at 1/6th opening of reflux valve

11 mins. and 17.15

secs.
Gathered distillate before the start of the time

1200 mL

Table 8.3 Raw Data from Distillation of Ethanol-Water Solution

Sample
No.

Time
(min)

1
2
3
4
5
6
7
8

5
10
15
20
25
30
35
40

Refractive Index
Bottom
1.3501
1.3498
1.3493
1.3491
1.3489
1.3485
1.3483
1.3476

Distillate
1.3630
1.3632
1.3629
1.3629
1.3631
1.3628
1.3629
1.3627

Distillate
Volume
(mL)
300
210
250
250
255
225
225
240

T1
85
81
85
87
87
87
86
86

Temperature (0C)
T2
T3
79
30
77
30
77
30
79
30
80
30.5
80
30.5
80
30.5
80
30.1

T4
30
30.5
30
29.5
31.5
32
32.1
33

Nomenclature:
T1 = temperature of the reboiler
T2 = temperature of the vapor as it enters the top condenser
T3 = temperature of distillate during measurement of refractive index
T4 = temperature of bottoms during measurement of refractive index

82

1.

Refractive Index

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
3 2 .3 2 .3 2 .3 2 .3 3 .3 3 .3 3 .3 3 .3 3 .3 4 .3 4 .3 4 .3 4 .3 4 .3 5 .3 5 .3 5 .3 5 .3 5 .3 6 .3 6 .3 6 .3 6 .3 6 .3 7

Graph II. Calibration Curve of Refractive Index vs. Methanol Concentra

5
0

15
10

25
20

35
30

45
40

55
50

65
60

75
70

85
80

95
90

105
100

Methanol Concentration

Calibration Curve
Figure 8.2 Calibration Curve

83

Step response of First Order System

Experiment No.9
I.

Objective
To plot the response of first order liquid level system as a function of time
and to evaluate the flow resistance R of a first order liquid level system.

II.

Materials/Apparatus/Equipment
Water
PCT 9 Process Module
PCT 10 Electric Module

III.

Theory
The step response of a system in a given initial state consists of the time
evolution of its outputs when its control inputs are Heaviside step functions. In
electronic engineering and control theory, step response is the time behavior of
the outputs of a general system when its inputs change from zero to one in a very
short time. The concept can be extended to the abstract mathematical notion of a
dynamical system using an evolution parameter.
Time behavior of a system is important. In designing a system, the time
behavior may well be the most important aspect of its behavior. How long it takes
the temperature to reach a new steady state is important in a control system thats
controlling a temperature.
The parameters you find in a first order system determine aspects of
various kinds of responses. Whether we are talking about impulse response, step
response or response to other inputs, we will still have the following quantities
and system parameters:
x(t) = Response of the System,
u(t) = Input to the System,
= The System Time Constant,
Gdc = The DC Gain of the System.
84

Every system will have an input which we can call u (t), and a response
we will denote by x (t). Each system will also have a time constant and a DC
gain.
, the time constant, will determine how quickly the system moves toward
steady state. Gdc, the DC gain of the system, will determine the size of steady state
response when the input settles out to a constant value.
Step Response of a First Order System:
A standard first order linear system will satisfy this differential equation.
dx( t) x (t)
=
+ Gdc U (t)
dt

A first order linear system will almost always have this form - or can be
put into this form.
When the step is applied, the derivative of the output changes immediately
(http://www.facstaff.bucknell.edu)

Unit-Step Response of First-Order Systems

1
s ( Ts+1 )

R(s) = 1/s, and therefore the unit-step response is: Y(s) =

Expanding Y(s) into partial fractions: Y(s) =

1
T

s Ts+1

Take the inverse Laplace transform: y(t) = 1 e t/T , t 0

The solution has two parts: a steady-state response: y(t) = 1, and a transient

1
1

s
1
s+
T

response: yt (t) = e
,, which decays to zero as t

The steady-state error is the error after the transient response has decayed leaving
only the continuous response. The error signal: e(t) = r(t) - y(t) = 1 - 1 + e-t/T = et/T

85

86

87

88

89

IV.

Procedure
Set up the PCT 9 with motorized valve fully open, solenoid valve 3, open,
V3 and V4 closed. Adjust the flow meter to 0.50 L/min and record steady state
height. This will take few minutes. When the height of the liquid is steady, adjust
the flow meter to 0.70 L/min manually in the PCT 10 simultaneous with the timer.
Record the time for every 5 mm of increase in liquid level.
V.

Results and Discussion

Processing the experimental data tabulated in Table A.1, it appears that the
results for the Response of the liquid height to a disturbance in flow rate is
presented in Table B.1 and is shown in Figure 9.1. From the figure provided, it
can be seen that the curve is linear, and at t = 3.0833333 min the system
approaches steady state.

90

Plot of Experimental Data

120
100
80
Response Heigt, (mm)

60
40
20
0
0

0.5

1.5

2.5

Time (min)

Figure 9.1 Curve for Liquid Level Response from Experimental Data

91

But according to theory, the response of the liquid level of the system with a
disturbance to the inlet flow rate is presented in Figure 9.2, where steady state

condition is met at t = 12 min.

Figure 9.2 Curve for liquid level step response

The Response Equation for the curve in figure 9.2 is now

H (t )=120.10 1e 1.927047532

Solution for the Response equation is shown in Appendix B of this laboratory

report.
As for the resistance of the system, using the method of the ideal response
equation, following approximations of actual liquid level responses and using the
equation
q os =C h s1/ 2
2 hs1 /2
R 1=
C
the resistance R1 is found to be 60.05 mm/L-min. Sample computations provided
in Appendix B.

92

VI.

Conclusion and Recommendation

Figure 9.2 shows the curve for the unit step response. It can be seen that it
increases exponentially. At 0.50 L/min, the resistance is at 60.05 mm/L/min.

VII.

Reference
COUGHANOWR, D. R., LEBLANC S. E., Process Systems Analysis
and Control, 3rd Edition, The McGraw-Hill Companies, Inc. (2009)

93

APPENDICES
Appendix A. Raw Data
Table 9.1 Liquid Level (q1 = 0.5 L/min; q2 = 0.7 L/min)
Liquid Level, (mm)
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
105
110
115
120
125
130
135

Time, (s)
7
14
21
28
36
43
50
58
66
73
80
88
95
103
110
118
127
134
142
150
159
167
176
185
192

Appendix B Sample Computation

Solving for the Resistance R1
q os =C h s1/ 2
0.5 L/min=C [( 15 mm ) ]
C=0.129 L/minmm

1
2

1/ 2

94

1 /2

2h
R 1= s =
C

2 15 mm
L
0.129
1 /2
minmm

R1=60.05

mm
L
min

Deriving the Step Response Equation

R1
H (s)
=
Q(s) ( s+1)
Q ( s )=

A
s
w/r A refers to the unit step input of the system
H ( s )=

A R1
s (s+1)

H (t )= A R1 1e

A=qos 2q os 1=( 0.70.5 ) L/min

A=0.2 L/min

The step Response Equation is

t

H (t )=120.10 (1e )
Getting the Average Time Constant Ave for the Step Response Equation

Table 9.2 Data Achieved By Using the Response Equation

Liquid Response
H(t), (mm)

Time, (min)

Time Constant ,
(min)

0
95

5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
105
110
115
120

0.11667
0.23333
0.35
0.48333
0.6
0.71667
0.85
0.98333
1.1
1.21667
1.35
1.46667
1.6
1.71667
1.85
2
2.11667
2.25
2.38333
2.53333
2.66667
2.81667
2.96667
3.08333

2.743587
2.683976
2.623443
2.653417
2.570741
2.493581
2.46736
2.427691
2.342897
2.259774
2.204441
2.118497
2.053454
1.963467
1.88883
1.82324
1.720694
1.625958
1.522452
1.417166
1.28599
1.137684
0.939091
0.434829

H2

( H ) dH
Ave =

H1

H 2H 1

By regression analysis, (H) was found to be

( H )=1.856281378+0.02594514156 H3.095713207 x 104 H 2
Then substituting to the above equation and integrating with limits H 1 = 0 mm and
H2 = 120 mm. The result being
Ave =1.927047532min
The response equation is now
96

H (t )=120.10 (1e

t
1.927047532

Motorized Control Valve

Experiment No.10
I.

OBJECTIVE
1. To demonstrate a manual operation of a motorized control valve
2. Determine the characteristics of flow rate versus valve position; and
3. Determine the relationship between the current input to the positioned
and mechanical position of the valve (linearity of the positioner).
II.

MATERIALS/ APPARATUS/ EQUIPMENT

Water

PCT 9 Process Module

PCT 10 Electrical Console

97

III.

THEORY
Motorized Control valves are valves used to control conditions such
as flow, pressure, temperature, and liquid level by fully or partially opening or
closing in response to signals received from controllers that compare a "setpoint"
to a "process variable" whose value is provided by sensors that monitor changes
in such conditions. The opening or closing of control valves is usually done
automatically by electrical, hydraulic or pneumatic actuators. Positioners are used
to control the opening or closing of the actuator based on electric or pneumatic
signals. These control signals, traditionally based on 3-15psi (0.2-1.0bar), more
common now are 4-20mA signals for industry, 0-10V for HVAC systems, and the
introduction of "Smart" systems, HART, Fieldbus Foundation, and Profibus being
the more common protocols.
Process plants consist of hundreds, or even thousands, of control loops all
networked together to produce a product to be offered for sale. Each of these
control loops is designed to keep some important process variable such as
pressure, flow, level, temperature, etc. within a required operating range to ensure
the quality of the end product. Each of these loops receives and internally creates
disturbances that detrimentally affect the process variable, and interaction from
other loops in the network provides disturbances that influence the process
variable. To reduce the effect of these load disturbances, sensors and transmitters
collect information about the process variable and its relationship to some desired
set point.
A controller then processes this information and decides what must be
done to get the process variable back to where it should be after a load
disturbance occurs. When all the measuring, comparing, and calculating are done,
some type of final control element must implement the strategy selected by the
controller. The most common final control element in the process control
industries is the control valve. The control valve manipulates a flowing fluid, such
as gas, steam, water, or chemical compounds, to compensate for the load
98

disturbance and keep the regulated process variable as close as possible to the
desired set point. Many people who talk about control valves or valves are really
referring to a control valve assembly.
The control valve assembly typically consists of the valve body, the
internal trim parts, an actuator to provide the motive power to operate the valve,
and a variety of additional valve accessories, which can include positioners,
transducers, supply pressure regulators, manual operators, snubbers, or limit
switches. Other chapters of this handbook supply more detail about each of these
control valve assembly components. Whether it is called a valve, control valve or
a control valve assembly is not as important as recognizing that the control valve
is a critical part of the control loop. It is not accurate to say that the control valve
is the most important part of the loop. It is useful to think of a control loop as an
instrumentation chain. Like any other chain, the whole chain is only as good as its
weakest link. It is important to ensure that the control valve is not the weakest link
(http://www.documentation.emersonprocess.com/groups/public/documents/book/
cvh99.pdf, 10/21/12).

IV.

Procedure
Characteristics of Flow Rate versus Valve Position:
Connect the equipment as shown in the equipment set up. Open the
motorized valve fully by rotating the knob on the more positioned fully clockwise
and check that the maximum flow rate is 3000 cm3/min on F1. If not adjust V2.
Closed the motorized valve. Adjust the position of the valve in steps of 10% from
0% to 100%. This may be achieved by adjusting the current flow to give steps of
0.8 volts on the voltmeter. At each position of the valve, record the corresponding

99

flow rate on F1. Repeat the procedure for the valve closing in steps of 10% to
determine any hysteresis.
Relationship between the current input to the positioned and Mechanical position
of the valve:
Rotate the knob on 4-20mA Manual Output anticlockwise to close the
valve. Rotate the valve drive system gradually by adjusting 4-20mA input to the
motor positioned until the valve coupling has rotated turn. Note the current
supplied to the positioned. Repeat procedure, noting position and current until
valve is fully closed.

V.

Results and Discussions

A relationship between valve opening and flow rate can be observed from the

experimental data achieved. Figure 10.1 shows the said relationship. The figure shows
this relationship at valve opening and valve closing. Both curves show an approximately
linear relation. But it appears that the curve for closing is closer in linearity compared to
that of the valve at opening.

Relationship of Valve Position and Flow Rate

100
90
80
70
60
Valve Position (%Opening)

Valve Opening

50

Valve Closing

40
30
20
10
0
0

1000

2000

3000

Flow Rate (cm3/min)

Figure 10.1 Plot Valve Position vs Flow Rate

100

Relationship of Current and Valve Position

1
0.9
0.8
0.7
0.6
Current (V)

0.5
0.4
0.3
0.2
0.1
0
0

10

20

30

40

50

60

70

80

90

100

Valve Position (%Opening)

Upon operating the equipment, a certain amount of current is required to operate

the motorized valve. The relationship between current and valve opening position is
presented in Figure 10.2.
VI.

Conclusion

Figure 10.2 Plot of Current vs Valve Position

From Figure 10.1, it can be seen that the curve for the closing is much
more linear. Which can be concluded that the closing valve offers much more
steady flow rate in comparison to that when the valve is at opening.
Figure 10.2 clearly shows a very linear direct linear relationship between
the valve position and current. It appears that a linear relationship having a slope
of 0.008. As stated in the procedure, by increasing the current by 0.8 volts, the
valve opening increases by 10%.

VIII. Reference
(http://www.documentation.emersonprocess.com/groups/public/documents/bo
ok/cvh99.p df, 10/21/12).

101

APPENDICES

Appendix A Raw Data

Table 10.1 Characteristics of Flow Rates versus Valves Position
Position
V on Meter
0.2
0.28
0.36
0.44
0.52
0.60
0.68
0.76
0.84
0.92
1.00

Flow Rate

% of Opening
0

Valve Closing (cm3/min)

0

10
20
30
40
50
60
70
80
90
100

Valve Opening (cm3/min)

0

580
970
1395
1710
2110
2420
2620
2800
2900
3000

580
910
1290
1810
2050
2370
2600
2780
2900
3000

Appendix B. Sample Computation

Solving for the slope of the curve for the Current vs. %Opneing
slope=

Current
10.2
=
=0.008
%Opening 1000

102