Lab Manual ChE-492

IITK/CHE/UO Lab/Lab Manual (CHE 492)
INDIAN INSTITUTE OF TECHNOLOGY

KANPUR
DEPARTMENT OF CHEMICAL ENGINEERING

UNIT OPERATION & PROCESS CONTROL LAB
EXPERIMENT MANUAL
CONTENTS
SR.NO.
EXPERIMENTS NAME
PAGE NO.
1.
General Instruction
I -VI
2.
Liquid Liquid Extraction
1-9
3.
Liquid Solid Adsorption In a Packed Bed
10-17
4.
Mass Transfer From a Single Drop
18-29
5.
Calendria Evaporator
30-36
6.
Batch Crystallizer
37-44
7.
Continuous Distillation
45-52
8.
Plug Flow Reactor
53-59
9.
C.S.T.R
60-65
10.
Batch Reactor
66-70
11.
Semi batch Reactor
71-74
12.
R.T.D in CSTR and packed Bed Reactor
75-83
13.
Characteristic of P.I.D Controller
84-86
14.
Characteristic of Pneumatic Control Valve
87-92
15.
Flow control Trainer
93-131
16.
Interacting And Non Interacting Tank System
132-149
17.
Time Constant of Thermocouple & Time Constant of RC
150-162
18.
Fault Finding Trainer
163-181
CHEMICAL ENGINEERING LABORATORY

The laboratory course helps the student to understand and verify by experimental work, some
of the basic laws and principals in the field of chemical engineering that is fluid flow, heat
transfer, mass transfer, thermodynamics etc. The course help the students to devise his own
experiments, and generate data when ever it is not readily available in the literature the ideas
gained in the laboratory course or long lasting and hazy notion will be dispelled by performing
the experiments further the laboratory course also helps the student in developing the
communication skills throw effective report writing clear and concise reports which
adequately describe the purpose of work ,the method adopted, the observations and conclusion.
The engineers mostly work in groups and hence it is essential to develop inter personal skill
such as communicating the ideas, planning the task, working in cooperation and in arriving at a
decision. Therefore a student is considered to have under gone a satisfactory training in
chemical engineering only when he is exposed to a good laboratory course.
General Instructions
1.
The Chemical Engineering Laboratory class will be divided in to groups of about three
students. Each group will be held responsible for the condition of the
2.
apparatus.
A schedule of experiments will be assigned which will be strictly followed .each group
will perform a total of 11 experiments in the semester.
3.
Once the experiments are assigned, the students should come prepared with sufficient
background concerning the experiments .The relevant theory the procedure and data
analysis should be known before starting the experiments. For some experiments
instruction manual have been supplied with the instruments. The should be care fully
read before starting the experiments.
4.
Before starting the experiments

a.
Study the experimental setup thoroughly
b.
Plan the experiment properly the sequence of operation to be perform and the
data to be recorded
c.
Get the required material issued from the laboratory assistance.
Page I
5.
All data recorded on the lab record sheets- (8 x11) plane sheets. At the completion
of the experiment, obtain the signature of the instructor in charge or the teaching on the
lab record sheet
6.
After the completion of the experiments

a.
Shut off the experiment.
b.
Clean the equipment and the surrounding area
c.
Close all the valve and switch off electrical connection
d.
Return the material issued to you each group will be held responsible for the loss
/breakage of any equipment clean all glassware before returning the same.
7.
The detailed lab report (one per group) should be submitted in the proper format at the
beginning of the next laboratory session.
a.
The first lab should be submit in the folder in which the subsequent
report will be placed
b.
Used thesis size bond paper (8 x11) for writing the reports .all reports must
be return in ink (blue or blue black or black only) on one side of paper only. Any
variation in the above will not be entertained.
c.
The lab record should contain the original lab record sheet (with raw data)
singed by the instructor in charge or teaching assistance.
d.
8.
Late submission of lab report is strictly not allowed .
The following format should be followed while writing the lab reports.
a.
Title of the experiment
b.
Introduction -should include the importance of the topic and the application of
the results
c.
Objective of the experiment should clearly indicate what is the purpose

of doing the experiments
d.
Theory a brief statement of the relevant theory which forms the background of
the experiment. All relevant equation should be included. Do not copy verbatim
from the laboratory manual.
Page II
e.
Experimental Apparatus and Procedure

A description of the apparatus with a neat sketch, together with the important
relevant dimensions should be included in this section. A brief outline of the
procedure indicating the sequence of operations should be given.
f.
Results and Discussion

The relevant results should be presented in either tabular or graphical form
>
The raw data should be included in the appendix.
>
Sample calculations should be shown in detail indicating clearly each of

the steps, assumptions made, source of physical properties etc.
>
Discussion should indicate the reasons for the deviations from the
expected trends, the nature and effect of the errors involved. As far as
possible, the experimental results should be compared with published
literature values or standard correlations. Any result which needs to be
emphasized should be discussed with possible explanations.
>
Any auxiliary problem which arises from the experiment and which can
be investigated with minor modifications of the existing experimental
set-up should be indicated. Recommendation for improvements in the
experimental set-up and suggestions for future work can also be
included.
g.
Conclusions
This part should briefly indicate what conclusions can be made from your
experimental data and analysis of this data.
h.
Nomenclature
All symbols used in the report should be defined, with proper units. The
symbols should be listed in alphabetical order, with Greek Letters listed at the
end. Refer to any text book or the experiments in this manual.
i.
References
Page III
The details of all references including the names of all the authors, referred to in
the text should be given here. The references are listed alphabetically in the
authors names. Refer to any standard journal such as Industrial and Engineering
Chemistry Research or AIChE Journal.
j.
h.
Answer the questions given in the write up of the experiment.
Appendix
>
Raw data should be included here.
>
Any computer listings and outputs should be given here whereas the
main results obtained from the computer are shown in the Results and
Discussion section.
>
Details of any repetitive calculations.
Some General Rules of Report Writing:

1.
As far as possible use third person, passive voice. For example, instead of writing we
took a beaker, write a beaker was taken.
2.
All equations, tables and figures should be numbered. Moreover, each table or figure
should have a caption. Any table or figure included in the report, should have been
referred to in the text.
3.
Do not use significant figures indiscriminately.
4.
References in the text should be cited using author, year convention. For articles having
one or two authors use the names of all authors followed by the year (e.g., Smith, 1975;
Anderson and Thomas, 1981). In case, the citation has more than two authors then in
the text give the surname of the first author followed by et al.(e.g. Smith et al., 1989).
However, the names of all the authors should be given in the reference list. In case of
any doubt, refer to journals such as Industrial and Engineering Chemistry Research or
AIChE Journal.
Page IV
SUGGESTED GUIDELINES FOR SAFE WORKING IN THE LABORATORY

A laboratory is built at a considerable cost to enable the students to understand and
appreciate the fundamental laws and principles of chemical engineering. It is the responsibility
of every student to use the facilities in the best possible manner for the benefit of all the
students, including the succeeding generation of students. Many of the accidents that occur in a
laboratory can be prevented by observing the safe working norms in a laboratory. Some of the
suggestions for safe working in a laboratory are listed below for your reference.
1.
Smoking is strictly prohibited in the laboratory.
2.
Do not put on loose clothing.
3.
While working in a laboratory, you should wear shoes only. No one will be allowed to
wear slippers in the laboratory.
4.
The following precautions should be observed when using electrical gadgets.

(a)
Use proper switches, sockets, adaptors and holders for electrical connections.
(b)
Do not insert naked wires in wall plugs.
(c)
Before starting the equipment, check if the equipment is properly grounded. If

the unit is not properly grounded, it may give an electric shock.
(d)
No electric cable should be left hanging in the air. All cables should be fastened
to a frame or wall.
(e)
Test a new electric gadget for leakage before use. Phase tester is available with
the laboratory assistant. If any electrical defect is noticed, report it at once to the
laboratory assistant.
5.
The laboratory is provided with a first aid kit. In case of minor injuries, have these
treated at once. In case of serious cases, notify the doctor immediately and summon the
ambulance. Dial 7666/7777, health centre for ambulance.
6.
In case of chemical burns, the affected area should be immediately cleared of the
harmful chemicals as quickly as possible.
Page V
7.
If acid gets spilled on the ground or work bench, it should be immediately neutralized
by spraying sodium bicarbonate.
8.
Do not use any tool with which you are not familiar. You may injure yourself and
damage the tool. In case of doubt consult the laboratory staff.
9.
Use the right kind of tool for specific job. Do not use a screw driver as a chisel or as a
stirrer. Do not use a hammer to drive screws.
10.
Do not use pipe wrenches on brass valves, nuts and bolts. Pipe wrenches should be used
to tighten pipes only.
11.
Never dismantle any other equipment for accessories like fittings, rotameters, pumps,
thermometers etc. which you may require. Consult the laboratory staff for your
requirement of materials.
12.
Never lean on frames, work benches or equipment.
13.
In case of fire, immediately inform the security office (Tel no. 7999) for assistance.
14.
Do not spill water on the work benches, and floor. All water connections should be
checked for leakage. Each water outlet should be connected to the drain.
EVALUATION:
The laboratory course will be evaluated based on the lab reports, weekly viva voce and
final examination which may be conducted in the lab.
Page VI
INDIAN INSTITUTE OF TECHNOLOGY KANPUR

Unit Operation Lab (ChE-492)

LIQUID-LIQUID EXTRACTION
1. Objectives
To study the extraction of acetic acid from benzene by water in an Extraction Unit and
to determine the following:
(i)
Percentage removal of solute
(ii)
The theoretical number of stages required
(iii)
The overall stage efficiency (theoretical/actual)
(iv)
The variation of stage efficiency with solvent (benzene) flow rate.
2. Introduction
Liquid extraction, sometimes called solvent extraction, is the separation of the
constituents of a liquid solution by contact with another immiscible liquid. If the solute
distributes differently between the two liquid phases, a certain degree of separation will result,
and this can be enhanced by use of multiple contacts in a manner similar to distillation. Many
types of equipment are used where there is some difference in the densities of the two phases.
Some of the common ones are perforated-plate columns and mixer-setters.In a mixer-settler,
the two liquid phases are thoroughly mixed by an impeller or mixing jet followed by separators.
The individual stages are sometimes (as in the equipment used in this experiment) grouped
vertically in a column with impellers on a common shaft separated by sections for settling.
This is called a Scheibel extraction unit and has a high efficiency due to internal baffling.
3. Theory
Since liquid-liquid extraction is an operation involving diffusion of a solute through a
stationary component, the usual equations for this type of mass transfer apply. The design of
extraction equipment depends upon acquiring performance date from laboratory equipment
operating under conditions similar to design conditions. Treybal (1981) summarizes some of
the performance data available for continuous countercurrent extraction.
Principles of Liquid Extraction

System has three liquids say A.B and C.
B denotes the solvent ( water in this
experiment), C the substance to be extracted ( acetic acid in this experiment) and A is the liquid
in which C is initially present (benzene for this experiment). Triangular coordinates are often
used to represent the phase diagram (see Figure 1). Liquid C dissolves completely in A and B
but A and B dissolve only to a limited extent in each other, to give rise to saturated liquid
solutions at L (A-rich) and at K (B-rich). The more insoluble the liquids A and B the nearer the
apexes of the triangles will points L and K be located. The curve LRPEK is the binodal
solubility curve indicating the change in solubility of the A and B rich phases upon addition of
C. Any mixture outside the curve will be a homogeneous solution of one liquid phase. Any
ternary mixture such as M will form two insoluble saturated liquid phases of equilibrium
compositions indicated by R (A-rich) and E (B-rich). The line RE is the tie line. The
equilibrium distributions of the solute can also be conveniently shown on the distribution
diagram (Figure 1b), In this case, point (E,R) lies above the diagonal y=x, but this is not always
the case. Here, y is weight fraction of C in B-rich extract liquid and x is weight fraction of C in
solvent lean (A-rich) or raffinate liquid.
The distribution coefficient is defined as equal to y*/x which is ratio of wt fraction C in
extract phase which is in equilibrium with wt. fraction C in raffinate phase.
A mixture of liquids at M will split in two phases of compositions R and E such that
R line ME x E x M
=
=
E line RM x M x R
(1)
Selectivity, b is defined as
(wt frac.Cin E) /(wt frac.A in E) y*E (wt frac.A in R)

=
=
(wt frac.Cin R) /(wt frac.A in R) x R (wt frac.A in E)
(2)
While it is not necessary that distribution coefficient is larger than 1 but larger values are
desirable since less solvent will then be required for extraction.
The coordinate scales of equilateral triangles are necessarily the same, and in order to
be able to expand one concentration scale relative to the other, rectangular coordinates can also
be used. One of these is by plotting concentration of B as absicca against concentration of C (x
and y) as ordinate, as shown in Figure 2. Unequal scales can be used in order to expand the
plot as required.
2
Single Stage Extraction

Refer to Figure 3, feed of mass F (if batch) or F mass/time if continuous contains
substance A and C at xF weight fraction C. This is contacted with mass S1 (or mass/time) of a
solvent principally B containing yS weight fraction of C to give the equilibrium extract E1 and
raffinate R1. Adding S to F produces a mixture M1 which on settling forms E1 and R1.
Total material balance: F + S1 = M1 = E1 + R1
(3)
C balance
: F xF + S1yS = MxM1
(4)
or
S1 x F x M1
=
F x M1 yS
(5)
from which xM1 can be calculated.

The quantities of extract and raffinate can be computed by the mixing rule (Eq.1) or by material
balance for C.
E1 y1 + R1x1 = M1 xM1
or
E1 =
M1 (x M1 x1 )
y1 x1
(6)
(7)
R1 can be found from an overall mass balance.
Continuous Countercurrent Multistage Extraction

A flow sheet and solubility diagram are shown on a rectangular plot in Figure 4.
A total material balance about the entire plant is
F + S = E1 + RNP = M
(8)
Point M can be located on line FS through a balance for substance C,

FxF + S ys = E1y1 + RNP xNP = MxM
or
xM =
Fx F + SyS
F+S
(9)
(10)
Eq. (8) indicates that M must lie on line RNPE1. Rearranging Eq. (8) we have
RNP S = F E1 = DR
(11)
where DR, a difference point is the net flow outward at the last stage NP. From Eq. (11) the
extended lines E1F and SRNP must intersect at DR. A material balance for stages s though NP is
or
Rs-1 + S = RNP + ES
(12)
RNP S = Rs-1 ES = DR
(13)
3
This implies that difference in flow rates at a location between any two adjacent stages is
constant, DR. Line Es Rs-1 extended must pass through DR The graphical construction is as
follows. After location of points F,S,M,E,RNP, and DR, a tie line from E1 provides R1 since
extract and raffinate from first theoretical stage are in equilibrium. A line from DR through R1
when extended provides, E2 and a tie line from E2 gives R2 etc.
As the amount of solvent is increased , point M moves towards S on Figure 4 and point
DR moves farther to the left. On the other hand, on decreasing the amount of solvent if a tie line
from DR coincides with a tile line an infinite number of stages will be required to reach this
condition. The maximum amount of solvent for which this occurs corresponds to the minimum
solvent/feed rates which can be used for specified products. Usually the tie line passing
through F will locate DRm for mimimum solvent.
When the number of stages is very large a slightly different representation shown in
Figure 5 may be more useful. A few lines are drawn at random from DR to intersect the two
branches of solubility curve. The C concentrations xs and ys+1 corresponding to these are
plotted on x, y coordinates as shown on the right to provide the operating curve. Tie line data
provide the equilibrium curve y* vs. x and the theoretical stages are stepped off as in
distillation.
4. Apparatus:
The set up consists of a glass column with baffles (Figure 6). Stirrer with variable speed DC
motor and RPM indicator is provided for mixing. Two sump tanks with individual pumps are
provided for feed solutions. The heavier phase (acetic acid and water) is fed from the top and
the lighter phase (benzene) from the bottom. The interface is maintained above the heavier
phase inlet. The samples are taken from the top and bottom for analysis.
Technical Details:
Column:
Material Borosilicate Glass, Inner Diameter 75 mm, Length

150 mm, 06 number of stages.
5. Experimental Procedure:
1. Close all the valves.
2. Ensure that ON/OFF switches given on the panel are at OFF position.
3. Connect electric supply to the set up.
4. Switch ON the pumps.
4
5. Prepare the feed solution by taking about 20 liters of benzene and adding approximately
10% by wt. of acetic acid to it. Actual concentration can be found by titration.
6. Fill the column with the heavy phase (Water) and adjust the flow rate of the heavy phase
(water) to a desired value by rotameter. Start the stirrer (flow rate 1.5 to 2 cc/sec.)
7. Start passing the lighter phase (benzene and acetic acid) and adjust its flow rate (flow rate
1.5 to2 cc/sec.) by rotameter.
8. Switch ON the stirrer and adjust the mixer speed by the dimmer stat.
9. Adjust the upper interface to a suitable height with the help of Bottom valve for water
outlet. This is the important for the success of your experiment. You should be able to see
an interface and entry of solvent and similarly another one at the bottom somewhere
between entry of the feed and exit of extract.
10. Take the first observation after the steady state has been established i.e. after 15 to 20
minutes.
11. Measure the flow rate of extract and raffinate (by the time required to collect a known
volume).
12. Take the extract and raffinate samples (3 samples for each phase after 3 minute interval.
Samples for extract and raffinate should be taken simultaneously) and analyze their solute
contents.
13. Note the stirrer speed.
14. To complete the material balance, samples of inlet and outlet phases must be titrated.
Estimation of Acetic Acid:

a. Acetic acid in extract can be estimated by titration with NaOH solution using
phenolphthalein indicator. Colour change: colourless in acidic medium; red in alkaline
medium;
b. Prepared NaOH solution will be supplied. Its strength can be found out by titration with
standard HCl solution with methyl orange as indicator. Colour change: red in acidic
medium; yellow in alkaline medium.
c. For titration of acetic acid in benzene rich phase, take a measured volume and add some
water, put 2 drops of phenolphthalein indicator, shake well put a few drops of standard
NaOH solution, shake well till the colour drops disappear. Add few more drops of NaOH
and shake well, proceed like this until water layer becomes pink.
6.0 Precautions:
1. Before titration check that the stop cock of the burette is properly greased.
2. Glassware should be cleaned thoroughly before and after the experiment. Make sure
this has been done before returning them.
3. Unused NaOH solution should be returned into the NaOH bottle.
4. As soon as you finish the experiment, drain out all the liquid from extractor and pipe
lines, pass water through the line for about 15 minutes so that pipe lines through which
acetic acid has been passed and the extractor column are washed thoroughly. This is
very very important to prevent corrosion.
5. Do not throw away the outputs which contain benzene; collect it in the proper vessel.
Equilibrium distribution of acetic acid between water and benzene at 25oC

Benzene-rich phase (wt.%)
Water-rich phase (wt.%)
Acetic Acid
Benzene
Water
Acetic Acid
Benzene
Water
0.150
99.849
0.001
4.560
0.04
95.400
1.400
98.560
0.040
17.700
0.200
82.100
3.270
96.620
0.110
29.000
0.400
70.600
13.300
86.400
0.400
56.900
3.300
39.800
15.000
84.500
0.500
59.200
4.000
36.800
19.900
79.400
0.700
63.000
6.500
29.600
22.800
76.350
0.850
64.800
7.700
27.500
31.000
67.100
1.900
65.800
18.100
16.100
35.300
62.200
2.500
64.500
21.100
14.400
37.800
59.200
3.000
63.400
23.400
13.200
44.700
50.700
4.600
59.300
30.000
10.700
52.300
40.500
7.200
52.300
40.500
7.200
References:
1. Treybal, R.H., Mass-Transfer Operations, 3rd ed., McGraw-Hill, NY, 1981.

2. W.L.McCabe& J.C.Smith, Unit Operations of Chemical Engineering, 7th ed.,
McGraw-Hill., NY, 2005.


LIQUID SOLID ADSORPTION IN PACKED BED
1.
Objective:
Study of adsorption in a packed bed for a solid liquid system.
2.
Aim:
Plotting the breakthrough curve of adsorption for a given system & calculation of
length of unused bed for the system.
3.
Introduction :
A substantial number of unit operations of chemical engineering are concerned with the
problem of changing the compositions of solutions & mixtures through methods not
necessarily involving chemical reactions. One of the well known operations for solid
liquid contacting is adsorption. The colored material which contaminates impure cane
sugar solutions can be removed by contacting the liquid solutions with activated carbon,
whereupon the colored substances are retained on the surface of the solid carbon.
In adsorption the molecules distribute themselves between two phases, one of which is a
solid whilst the other can be the liquid or gas. Adsorption suffers one drawback, that the
capacity of the adsorbent for the adsorbate in question is limited. At intervals, the
adsorbent has to be removed from the process and regenerated, that is, restored to its
original condition. For this reason, in its early applications in industry, the adsorption
unit was considered to be more difficult to integrate with a continuous process
4.Theory:
Adsorption is the selective transfer of a solute from a fluid phase to a batch of rigid
particles. The usual selectivity of a sorbent between solute and carrier fluid or between
different solutes makes it possible to separate certain solutes from the carrier or from
one another.
It occurs when molecules diffusing in the fluid phase are held for a period of time by
10
forces emanating from an adjacent surface. The surface represents a gross discontinuity
in the structure of the solid, and atoms at the surface have a residue of molecular forces
which are not satisfied by surrounding atoms like those in the body of the structure.
These residual or van der Waals forces are common to all surface and the only reason
that certain solids are designated "adsorbents" is that they can be manufactured in a
highly porous form, giving rise to a large internal surface
THE ADSORPTION WAVE

Consider
binary
solution,
containing a strongly adsorbed

solute at concentration Co.
The
fluid
is
to
be
passed
continuously downwards through

a relatively deep bed of adsorbent
initially free of adsorbate. The
uppermost
layer
of
solid,
in
contact with the strong solution

entering, at first adsorbs solute
rapidly and effectively, and what
little solute is left in the solution is
substantially all removed by the
layers of solid in the upper part of
the bed. The effluent from the top
of the bed is practically solute-free, as at Ca in the lower part of adjacent figure. The
distribution of adsorbate in the solid bed is indicated in the sketch in the upper part of
this figure at a, where the relative density of the horizontal lines in the bed is meant to
indicate the relative concentration of adsorbate. The uppermost layer of the bed is
practically saturated, and the bulk of the adsorption takes place over a relatively narrow
adsorption zone in which the concentration changes rapidly, as shown. As solution
continues to flow, the adsorption zone moves downward as a wave, at a rate ordinarily
very much slower than the linear velocity of the fluid through the bed. At a later time,
as at b in the figure, roughly half the bed is saturated with solute, but the effluent
concentration Cb is still substantially zero. At c in the figure the lower portion of the
adsorption zone has just reached the bottom of the bed, and the concentration of solute
in the effluent has suddenly risen to an appreciable value Cc for the first time. The
11
system is said to have reached the Breakpoint. The solute concentration in the effluent
now rises rapidly as the adsorption zone passes through the bottom of the bed and at d
has substantially reached the initial value Co. The portion of the effluent concentration
curve between positions c and d is termed the Breakthrough curve. If solution continues
to flow, little additional adsorption takes place since the bed is for all practical purposes
entirely in equilibrium with the feed solution.
LENGTH OF UNUSED BED CALCULATION:

Consider the adjacent figure. If
the
mass-transfer rate were infinitely

rapid, the breakthrough curve
would be the vertical line at qS,
which can be located so that the
shaded areas are equal. The
adsorption zone of the figure can
then be idealized as reduced to a
plane, with the length of bed ZS
upstream
of
the
plane
at
concentration XT and the length
Z-
ZS downstream equal to the

length of unused bed (LUB). At breakthrough, the length of the bed is taken to be the
sum of LUB and a length saturated with solute in equilibrium with the feed stream. If V
= velocity of advancement of the "adsorption plane", then at any time,
Z S = V , at time qS,
Z =V
, and
at breakthrough, Z S = V
therefore
LUB = Z Z S
=V
=V(
Z(
V=
Z
S
12
5.
Description:
The apparatus is provided for the process of Adsorption in Packed column with Solid
phase being static & fluid phase is flowing. For flow of fluid a pump & rotameter is
provided. Three borosilicate columns are provided having different diameters &
lengths. At the inlet of column, valves are provided to feed only one column at a time.
Valves are provided at the bottom of columns & liquid tanks for drain. Filters are
provided before the column drain valves to prevent the charcoal from drain.
Technical Detail:
Column 1:
Material Borosilicate Glass, Inner Diameter 25 mm,

Length 1000 mm.
Column 2:

Length 500 mm.
Column 3:

Length 300 mm.
6.
Utility required:
Electrical supply: Single Phase, 220 V AC, 50 Hz, 5-15 amp socket with earth connection.
1. Water Supply (Initial Fill)
2. Drain required.
3. Floor Area Required: 1.5 m x 1m.
4. Chemicals Required:
Activated Charcoal
2 kg
KMnO4
15 gms.
1. Prepare a curve Optical Density vs concentration for KMnO4-water system.
2. Check that all the valves are properly closed
3. Fill the colored liquid in the feed tank (upper tank) and Activated Charcoal in
columns.
4. The colored solution made; should not be too concentrated.
5. Open the valve of column to be operated.
6. Start the pump and the stop watch.
13
7. Fix a minimum flow rate using Rotameter.

8. Take the samples of the output from column after fixed time intervals.
9. Measure the Optical Density by colorimeter and hence concentration of color in the
liquid.
10. Note down flow rate, time & concentration.
11. Run the fluid till the change in color of output liquid becomes almost stable.
12. Close the pump & valve of the column.
13. Now run for second & third columns.
8.
Observation and calculations:
DATA:
Z = 1 m / 0.5 m / 0.3 m
A calibration curve between Optical Density & Concentration is plotted, as shown below
OBSERVATIONS:
F = --------- LPH
Initial I = ------------
14
OBSERVATION TABLE:
q
Iq
Plot a curve between & C,
CALCULATIONS:
Initial C
= ------------ mol/lt (Using Calibration Chart)

15
Iq
From breakthrough curve (between & C) calculate S, B
LUB =
Z(
, m = ------------ m
9.
Nomenclature:
C
Concentration of adsorbate in feed solution, mol/ltr
Flow rate, LPH
Iq
Optical density of fluid at exit at time q
Actual height of adsorbent column, m.
qB
Time when the color of product starts changing rapidly, min (take
reference from theory.)
qS
Time required for idealized breakthrough, min. (take reference from

theory.)
LUB
10.
Length of unused bed.
Precautions and Maintenance Instructions:

1. Do not run the set up if power supply is less than 180 or above 230 volts.
2. Before starting the pump ensure that bypass valve is not fully closed & Rotameter is
properly closed.
3. Check properly that only one feed valve is open at a time
4. The apparatus should be drained off as soon as possible as the color of liquid would
clot over the inner surfaces of the apparatus, making the apparatus yield incorrect
results.
11.
Troubleshooting:
1. In case of any problem regarding operation of the apparatus; the apparatus should
be quickly switched OFF and electric supply should be cut OFF.
16
12.
References:
1. Treybal, R.E, Mass-Transfer Operations, 3rd ed., McGraw-Hill, NY, 1981,
Page 623-625, 632-636, 639-640.
2. Binay K.Dutta, Principles of Mass Transfer and Separation Processes,
Prentice Hall of India Pvt Ltd., ND, 2007, Page 630-636.
17


Mass Transfer from a Single Drop
1. Objective:
1.1
To study the effect of drop size on the terminal velocity of the drops.
1.2
To study the effect of drop size on the overall and individual mass transfer
coefficients.
1.3
To study the effect of drop formation on the overall mass transfer coefficient
2. Aim:
To determine the terminal velocity, individual and overall mass transfer coefficients for a
single drop.
3. Introduction:
The motion of liquid drops in another liquid medium and the transfer of a solute from these
drops to the surrounding fluid is an important topic of interest to chemical engineers. Real
system of interest involve a large number of drops; nevertheless information obtained on
the mass transfer rated from single drops is useful in the understanding of liquid-liquid
extraction equipment, the contact between the two liquid phases is secured through the
dispersion of one of the phases as drops. Hence, a knowledge of drop phenomena should
provide the basic information needed for the design of most liquid-liquid contactors in
which the drop size is related to the mass transfer rate and the terminal velocity to the
capacity of the equipment.
4. Theory:
Motion of drops:
The study of the shapes of moving drops has been found useful in understanding the
dynamics of moving drops since the drag on the drops depends on their shapes during
movement in another medium. The shape of a liquid drop depends upon several factors
such as the viscosity of the drop fluid, viscosity of the surrounding medium and the drop
18
volume. Small drops are generally spherical. For large drops, the shape changes
periodically from ellipsoidal to prolate (Laddha and Degaleesan, 1976).
A comparison with the fall of a solid sphere in a liquid would help in understanding the
motion of drops in a fluid medium. The velocity of the fluid at the surface of a solid body is
zero (no slip condition) but this is not the case for a liquid drop due to its mobility. In the
latter case, only the normal velocity component is zero whereas the tangential velocity
component is nonzero. In the liquid drops, the interfacial area is continuously changing,
new area is being continuously created in the forward regions and equivalent area is being
destroyed in the rear portion of the drop. This is called internal circulation and mass transfer
increases due to this circulation. Very small drops at low Reynolds number settle in a
manner similar to solid spheres and the terminal velocity increases with drop size. As the
drop size is further increased, due to internal circulation, the terminal velocity attains a
maximum value. After this peak point, further increase in drop diameter does not result in
any appreciable change in the terminal velocity. Various correlations have been attempted
to relate terminal velocity, drop size, peak velocity and maximum drop size to the physical
properties of the system.
By considering the force balance on a moving spherical drop, it can be shown that
Ut =
4 gd p ( d
3
CD
(1)
where CD is the drag coefficient.

The following correlations have been suggested (Laddha and Degaleesan, 1976) for the
drag coefficient for liquid drops:
( )
C D (NWe ) S 0.5 = 5
N Re
S 0.5
1.05
N Re
< 12
S 0 .5
for
(2)
and
( )
C D (NWe ) S
0.5
2.16
N
= 0.31 0Re.5
S
for
N Re
>20
S 0 .5
(3)
where
2
N We =
Ut d p
S=
c
3
4g c (
1
c
c
19
N Re =
Utd p
The interval 12 <
N Re
< 20 represents the peak velocity region.
S 0 .5
Mass Transfer from drops:

A solute encounters three resistances as it transfers from the interior of the drop to the
surrounding fluid. These are:
(i)
The resistance encountered in the transfer from the bulk of the drop to the surface.
(ii)
The resistance encountered in transfer through the interface.
(iii)
The resistance encountered in the transfer from the interface to the bulk of the
continuous phase.
If the drops are falling in a stagnant liquid column, then the concentration of solute in the
dispersed phase will change along the column length. Let us consider the situation at a
particular level in the column. Assuming that this solute is diffusing from the dispersed
phase into the continuous phase, there must be a concentration gradient in the direction of
mass transfer within each phase. This is graphically shown in Figure 1.
Dispersed
Phase
Interface
CAci
CAd
CAdi
CAc
Continuous
Phase
Figure 1: The two resistance concept

The concentration of solute A in the main body of the drop is CAd and is assumed to be
uniform due to internal circulation. This concentration falls to CAdi at the interface. In the
continuous phase, the concentration falls from CAci at the interface to CAc in the bulk liquid.
It is generally assumed that there is no resistance to solute transfer across the interface
separating the two phase as a result, CAdi and CAci are equilibrium values, given by the
systems equilibrium distribution curve (Treybal, 1981).
The various concentrations can also be shown graphically as in Figure 2, whose coordinates
are those of the equilibrium distribution curve.
20
Concentration of solute in
dispersed phase kkl/m3)
CA
d
C
A
Equilibrium
Distribution curve
di
C*A
CA
CA
C*A
ci
c
c
Concentration
of solute
in
continuous phase kmol/m3
Figure 2: Departure of bulk-phase

from equilibrium
(kmol/m3concentration
)
Point P represents the two bulk-phase concentrations and point M those at the interface. For
spherical drops, at steady state, we can write the rate of mass transfer of A in terms of
individual or overall mass transfer coefficients as
N A = k d d p2 (C Ad
= K od d p2 (C Ad
C Adi ) = k c d p2 (C Aci
*
*
C Ad
) = K oc d p2 (C Ac
C Ac )
C Ac )
(5)
where C*Ad is the dispersed phase concentration which would be in equilibrium with CAc.
Similarly C*Ac is the concentration which would be in equilibrium with CAd.
It can be shown that
1
1 m
=
+
K od k d k c
(6)
where m is the slope of the line joining points B and M (Figure 2). If the concentration of
solute in the continuous phase is negligible, eqn (5) simplifies to
N A = k d d p2 C Ad
= K od d p2 C Ad
or
K od = k d
(7)
(8)
Since mass is transferred as the drop falls down, CAd decreases from the top to the bottom
of the column. Hence, we have to use the log mean concentration difference to evaluate the
average rate of mass transfer. In such a case
21
N av = K od d p2 Clm
(9)
Where
Clm
(C
=
Ad
)
(C
ln
(C
*
C Ad
Inlet
(C
Ad
Ad
*
Ad
Ad Outlet
*
Ad Inlet
*
Ad Outlet
)
)
(10)
The total mass transferred, M, from a single drop is then
M = N av
(11)
where is the residence time of the drop.

Correlation for kd and kc
Several correlations have been proposed for estimating the individual mass transfer
coefficients (Laddha and Degaleesan, 1976).
The following correlations have been reported from correlation of experimental data for
single file drops:
k c = 0.023U t (N Sc )c
(12)
k d = 0.023U t (N Sc )d 2 , N sc =
1
kd
d Dd
(13)
For fully developed internal circulation the following correlations have been proposed,
0.43
0.58
d pU t c
kc
c
(14)
= 0.725
Ut
D
c c
c
k d = 0.00375U t
(15)
c
c
Effect of Drop Formation and Coalescence on Mass Transfer

The mass transferred during drop formation before detachment of the drop from the
dispersing nozzle is reported to form a major fraction of the total extraction, as observed in
many investigations. This marked increase in the rate of mass transfer may be explained by
considering the extent of internal circulation in the drop.
5. Experimental Apparatus and Procedure:

Apparatus :The apparatus consists of a glass column which is filled with either pure
benzene or benzene containing some acetic acid. The dispersed phase consists of an
22
aqueous solution of acetic acid. Drops of acetic acid-water are generated using nozzles
of various diameters. The dispersed phase collected at the bottom can be withdrawn
through an opening at the bottom of the column. Besides this, burettes, pipettes, beakers
etc are required to perform the titrations.
6.1. Prepare an aqueous solution of acetic acid and determine its concentrations by
titration (refer Appendix).
6.2. Fill the column with pure benzene.
6.3. Fill the burette/syringe with the aqueous acetic acid solution. This is the dispersed
phase.
6.4. Adjust the nozzle/syringe needle approximately 2-3 cm above the level of the liquid in
the column.
6.5. Now run down the liquid from the burette/syringe and check whether drops of
approximately the same size are generated.
6.6. For approximately 2 ml of liquid running down (from burette/syringe reading). Count
the number of drops. From this information, the drop radius can be calculated.
6.7. Determine the terminal velocity of the drops by measuring the time required for the
drops to pass through a known distance (take the average for at least five drops).
Knowing the length of the benzene column and the terminal velocity, the residence
time of the drops can be calculated.
6.8. After sufficient number of drops have passed through the continuous phase, stop the
flow of the dispersed phase.
6.9. Remove the dispersed phase from the column bottom and determine its acetic acid
concentration by titration.
6.10. Change the nozzle and repeat steps 3 to 9.
6.11. Drain the benzene from the column and fill the column with benzene which contains
some acetic acid. Determine the acetic acid concentration in benzene by titration.
6.12. Repeat steps 3 to 10.
6.13. To see the effect of drop formation on the rate of mass transfer, repeat the experiment
with the nozzle/needle immersed in the column liquid. Do this for one nozzle size and
the column liquid filled with benzene-acetic acid solution.
23
7. Utilities Required:
7.1. Glass Column
7.2. Distilled Water (To Prepare Solution).
7.3. 5 Conical Flasks.
7.4. Measuring cylinder.
7.5. Stopwatch.
7.6. 3 Burettes.
7.7. CHEMICALS:
QUANTITY:
N/10 Acetic Acid
100 ml
N/10 NaOH
100 ml
Ethyl Acetate
200 ml
Indicator (phenolphthalein
and methyl orange)
Few drops
8. Observations and Calculations:

DATA:
Diffusivity of acetic acid in benzene at 20OC = 1.92 10-5 cm2/s
Density of Benzene at 20OC = 0.879 gm/ml
Viscosity of Benzene at 20OC = 0.647 cp
30OC = 0.561 cp
Viscosity of acetic acid-water solution at different concentration and temperature
(in millipoise)
Acetic acid, wt%
Temp.
O
C
10%
20%
30%
40%
25
10.65
12.50
14.50
16.55
30
9.55
11.10
12.90
14.75
35
8.55
10.00
11.50
13.15
Density of acetic acid-water solution at different concentrations and temperature
(in gm/ml)
Acetic acid, wt%
Temp.
O
C
10%
20%
30%
40%
25
1.0107
1.0235
1.0350
1.0450
30
1.0089
1.0210
1.0320
1.0446
35
1.0042
1.0153
1.0338
1.0338
24
Distribution of acetic acid between benzene and water at equilibrium at 25OC

(data in wt%)
Upper Phase
Lower Phase
Acetic Acid
Benzene
Water
Acetic Acid
Benzene
Water
0.150
99.849
0.001
4.560
0.400
95.400
1.400
98.560
0.040
17.700
0.200
82.100
3.270
96.620
0.110
29.000
0.400
70.600
13.300
86.400
0.400
56.900
3.300
39.800
15.000
84.500
0.500
59.200
4.000
36.800
19.900
79.400
0.700
63.000
6.500
29.600
22.800
76.350
0.850
64.800
7.700
27.500
31.000
67.100
1.900
65.800
18.100
16.100
35.300
62.200
2.500
64.500
21.100
14.400
37.800
59.200
3.000
63.400
23.400
13.200
44.700
50.700
4.600
59.300
30.000
10.700
52.300
40.500
7.200
52.300
40.500
7.200
Observation:
1.
Standardization of NaOH
Vol. of HCl =
Vol. of NaOH =
2.
Normality of HCl =
Initial concentration of solute

Continuous Phase
Volume taken
NaOH Required
Dispersed Phase
Volume taken
NaOH Required
*(Not necessary for pure benzene)

Temperature
=
3.
Liquid height in column

4.
Terminal Velocity
Time required to pass between two marks distance between the marks
5.
Final concentration and drop volume

No. of drops
Total volume of
Volume of dispersed
required
Dispersed phase
phase taken for
collected
titration
Volume of
NaOH
for
Neutralization
9. Results:
9.1.
Calculate the drops size of each nozzle assuming the drop to be spherical.
(volume of liquid collected = no.of drops x
dp
6
)
25
9.2. Calculate the terminal velocity and the average residence time of the drops in the
column.
9.3. Compare the calculate Ut with that calculated using equation (1) and (2) or (3).
9.4. Calculate the number of drops constituting the total amount of liquid run down.
From this and the initial and final concentration of the acetic acid in the dispersed
phase, calculate the total mass transfer (M) and the average rate of the mass
transfer for a single drop (NAv)
9.5. Calculate Kod from equation (9).Note that when the continuous phase is pure
benzene Kod is equal to kd. Knowing kd and the Kod calculated for the case of
benzene-acetic acid as the continuous phase, kc can be calculated from equation (6)
for the two drop sizes. m can be determined by plotting the equilibrium data
given in the form of Figure 2. In Figure 2, concentrations are in the units of
kmol/m3, whereas the equilibrium data in the appendix are in weight %.
9.6. Calculate kc, kd and Kod using equations (12), (13) and (6) and compare with
experimental values
9.7. Calculate kc, kd and Kod using equations (14), (15) and (6) and compare with
experimental values
9.8. Calculate the percentage change in Kod for the case when the drops are formed in
the column rather than in air.
Estimation of Acetic Acid :

a) Acetic Acid can be estimated using NaOH of known strength, with phenolphthalein as
indicator. This indicator is colorless in acidic medium and pink in alkaline medium.
b) The NaOH solution is first standardized using a standard HCl solution. For this titration,
methyle orange is used as an indicator. Methyl orange is red in acidic medium and
yellow in alkaline medium.
c) Note that only a few drops of NaOH will be required to titrate the acetic acid in benzene
rich phase.
9.
Nomenclature:
CAc
Concentration of A in the continuous phase, kmol/m3
CAci
Interface Concentration of A in the continuous phase, kmol/m3
CAd
Concentration of A in the dispersed phase, kmol/m3
CAdi
Interface Concentration of A in the continuous phase, kmol/m3

26
C*Ac
Concentration which would be in equilibrium with CAd, kmol/m3
C*Ad
Concentration which would be in equilibrium with CAc, kmol/m3
CD
Drag co-efficient, dimensionless
Clm
Log mean concentration difference, defined in eqn (10), kmol/m3
Dc
Diffusivity of solute in the continuous phase, m2/s
Dd
Diffusivity of solute in the dispersed phase, m2/s
dp
Diameter of spherical drop, m
Acceleration due to gravity, m2/s
kc
Individual continuous phase mass transfer co-efficient, m/s
kd
Individual dispersed phase mass transfer co-efficient, m/s
Koc
Overall continuous phase mass transfer co-efficient, m/s
Kod
Overall dispersed phase mass transfer co-efficient, m/s
Total amount of solute transferred, kmol
slope of the chord of the equilibrium distribution curve,

dimensionless
NA
Rate of mass transfer, kmol/s
Nav
Average rate of mass transfer, kmol/s
NRe
Reynolds Number,
(NSc)c
Schmidt Number based on continuous phase properties, (c/cDc)
(NSc)d
Schmidt Number based on dispersed phase properties, (d/dDd)
NWe
Weber number,
d pU t
=
c
3
4g c (
U t2 d p
1
c
c
, dimensionless
Ut
Terminal Velocity, m/s
Interfacial tension, N/m
Density of continuous phase, kg/m3
Density of dispersed phase, kg/m3
Viscosity of continuous phase, Pa.s
Viscosity of dispered phase, Pa.s
Average residence time of drops, s
27
10. References:
12.1
Laddha, G. S. and Degaleesan, T. E., Transport Phenomena in Liquid

Extraction, Tata McGrow-Hill, New Delhi, 1976
12.2
Treybal, R. E., Mass Transfer Operations, 3rd edition, McGrow-Hill International

Book Co., Tokyo, 1981.
11. Questions:
1. Would the overall mass transfer coefficient remain the same if water was the continuous
phase and acetic acid benzene solution was in the dispersed phase?
2. What are the implicit assumptions in equations (5) and (9)?
3. How is Koc related to kc and kd?
4. What is the Marangoni effect?
28
29

CALENDRIA EVAPORATOR
1.
Objective:
To concentrate the solution of sodium carbonate using Calendria evaporator.
2.
Aim:
To determine an overall heat transfer co-efficient for the evaporator.
To determine the steam economy and capacity of Calendria Evaporator.
To perform a mass and heat balance over the evaporator.
3.
Interdiction:
Evaporation deals with the concentration of a non-volatile solute from a solution by the
removal of required amount of volatile solvent. Usually the solvent is water. By
vaporizing a part of the solvent, useful product i.e. the concentrated solution or thick
liquor is produced and the vapour is discarded. This is usually done before crystallizing
or drying the material, or to reduce the volume for transport or storage.
4.
Theory:
For heat transfer from the condensing steam to the boiling solution, the overall heat
transfer coefficient is found from the equation:
Q = U A
----------------- (1)
The temperature difference DT is the difference between the temperature at which the
steam condenses at the shell side pressure, and the temperature at which the solution
boils at the tube side pressure (< 1 atm).
T =T s T w
------------------- (2)
30
The area could be taken as either the inside or outside surface area of the tubes. The
inside area is chosen because the greatest resistance to heat transfer is on this side. The
area of the central downcomer is included, but the area of the tube plates is excluded.
A = n( d l ) tube +( D l ) downcomer
------------------- (3)
The heat flow is expressed in Watts (W) and calculated from an energy balance on the
feed and the two outgoing streams which are:
Product stream i.e. a saturated hot liquid phase leaving the evaporator.
Condensate i.e. saturated vapour leaving the evaporator, then being condensed and
cooled.
Then the steady state energy balance (neglecting heat losses) is:
Q =w p h p + wv h v w f h f
------------------- (4)
Material Balance:
At steady state, you would expect:
w f =w p + wv
5.
------------------- (5)
Description:
Present evaporator is a vertical short tube type evaporator with copper tubes. The tubes
are surrounded by a stainless steel jacket and fitted with accumulator. Dilute solution is
feed to evaporator and heated by steam from a steam generator to concentrate the dilute
feed solution to a desired level. The jacket is fitted with a steam trap and the condensate
is collected at the end of trap. The vapors of volatile solvent are condensed in a shell
and tube type condenser.
Technical Detail:
Down comer:
Material Stainless Steel, Inner Diameter 78 mm, Length

200 mm.
Inner Tubes:
10 Nos., Material Stainless Steel, Inner Diameter

22 mm, Outer Diameter 25.5 mm, Length 200 mm.
6.
Utilities Required:
1. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 32 Amps MCB with earth
connection.
31
2. Water supply: Initial fill.

3. Drain Required.
4. Floor Area Required: 1.5 m x 1 m.
5. Sodium carbonate (Na2CO3): 2 kg.
7.
Experimental Procedure:
Starting procedure:
1. Prepare calibration curve of concentration vs. density for Na2CO3-Water solution at
room temperature (0-50 %).
2. Prepare 5 % solution of sodium carbonate in water.
4. Fill cooling water tank with water.
5. Open funnel valve & air vent valve of steam generator and fill it 3/4th with water.
6. Close both the valves.
7. Ensure that switches given on the panel are at OFF position.
8. Connect electric supply to the set up.
9. Set the desired steam temperature (110 to 120 oC) by operating the increment or
decrement and set button of DTC.
10. Switch ON the heater and wait till desired temperature achieves.
11. Fill the solution in feed tank.
12. Open feed supply valve and allow feed to enter in the evaporator by control valve
and Rotameter.
13. Open steam supply valve.
14. Open vent valve before steam trap to release air and then close the valve.
15. Stop feed supply through Rotameter after maintaining a level of solution in front
glass of evaporator and wait till observing rise in temperature of vapor.
16. Switch ON the pump and set the flow rate of cooling water by Rotameter.
17. Partially open the product outlet valve and start collecting the product in tank.
18. Open feed supply from Rotameter and adjust the flow rate of feed so that the level
of solution in the side glass remains constant.
19. Record the flow rate of steam condensed by measuring cylinder and stop watch.
20. Record the evaporated vapor condensation rate by measuring cylinder and stop
watch.
32
21. Record the temperatures & flow rate of product.

22. Record the concentration of the product from calibration curve by measuring its
density at room temperature.
Closing procedure:
1. When experiment is over switch OFF heaters.
2. Partially open vent valve of steam generator to release pressure.
3. Switch OFF the pump.
4. Switch OFF Power Supply to Panel.
5. Stop compressed air supply to the set up and release air pressure by the regulator.
6. Drain feed tank by the drain valve provided.
7. Drain the evaporator liquid by the product outlet valve.
8. Drain the condenser by the drain valve provided.
9. Drain water from steam generator.
8.
Observation and calculation:

DATA:
w
---------, kg/m3
(from data book)
OBSERVATION:
Vf
Mf
OBSERVATION TABLE:
Time
(sec)
Steam
T1
T2
T3
T4
T5
Vapour
T6
Vs
ts
Vv
tv
Product
Ff
Fc
Vp
tp
Mp
10
20
30
40
33
CALCULATIONS:
f
WS =
1000 , kg/m3
= -------------------, kg/m3
1000 , kg/m3
= -------------------, kg/m3
Vp
V s 10 6
ts
, kg/sec
= ------------------, kg/sec
, kg/sec
= ------------------, kg/sec
, kg/sec
= ------------------, kg/sec
10 3 , kg/sec
= ------------------, kg/sec
V v 10 6
Wv =
tv
Wp =
Wf =
V p 10 6
tp
F f
3600
W f =W p+WV
E=
= ------------------, kg/sec
Wv
WS
= -------------------
C = Wv 3600
9.
= -------------------, kg/hr
Nomenclature:
w
Density of water at the temperature of condensate from condenser,

kg/m3
Vf
Volume of feed, ml
Mf
Weight of Vf ml of feed sample, gms
T1
Steam Inlet Temperature, oC
T2
Temperature of condensed Steam, oC
T3
Temperature of feed at Inlet, oC
T4
Temperature of Vapour Inlet to Condenser, oC
T5
Cold Water Inlet Temperature, oC
T6
Cold Water Outlet Temperature, oC

34
10.
Vs
Volume of steam condensate collected in time ts, ml
ts
Time for S, sec
Vv
Volume condensate collected from Condenser in time tv, ml
tv
Time for V, sec
Ff
Flow rate of feed, LPH
Fc
Flow rate of cold water, LPH
Vp
Volume Product collected in time tp, ml
tp
Time for P, sec
Mp
Weight of Vp volume of product, gms
Density of feed, kg/m3
Density of product, kg/m3
Ws
Rate of steam condensation, kg/sec.
Wv
Rate of condensation of vapor from condenser, kg/sec.
Wp
Flow rate of product, kg/sec.
Wf
Flow rate of feed, kg/sec.
Steam economy.
Evaporator capacity, kg/hr
Precautions and Maintenance Procedure:

1. Never run the apparatus if power supply is less than 180 volts and above 230 volts.
2. Never switch ON mains power supply before ensuring that all the ON/OFF
switches given on the panel are at OFF position.
3. Operator selectors switch OFF temperature indicator gently.
4.
11.
Always keep the apparatus free from dust.
Troubleshooting:
1. If electric panel is not showing the input on the mains light, check the main supply.
12.
Reference:
1. Kern, D.Q., Process Heat Transfer, 16th ed., McGraw Hill, ND, 2007, Page 401403.
35
PROPERTIES & ENTHALPIES

1. Arora.Domkundwar, A Course in Heat & Mass Transfer, 6th ed., Dhanpat Rai
& CO. (P) LTD., NY, 2003, Page A.6- A.15
2. R.K Rajput, Thermal Engineering, 6th ed, Laxmi Publications (P) LTD, 2006,
Page 1653-1663.
36

BATCH CRYSTALLIZER
1.
Objective:
To study the crystallization of MgSO4. 7H2O in a batch crystallizer.
2.
Aim:
To determine the yield of MgSO4.7H2O crystals
3.
Introduction:
Crystallization is the process where by a solid separates from a solution A saturated
solution containing the solute is altered by either cooling, evaporation of solvent, or
addition of another substance so that the ability of the solvent to dissolve the solute is
lessened, and a fraction of the solute forms a solid phase, which may be removed from
the mixture. Crystallization is the formation of solid particles within a homogeneous
phase. Its wide use has a two-fold basis, a crystal formed from an impure solution is
itself pure and crystallization affords a practical method of obtaining pure chemical
substances in a satisfactory condition for packing and storing. This operation involves
both heat and mass transfer.
4.
Theory:
Crystallization is the process where by a solid separates from a solution because
conditions have been imposed on the solution so as to allow the solid phase to form and
particles of crystalline character to grow to a size sufficiently large to allow separation
by physical methods. From the solubility or phase diagram the effect of changes in the
temperature and solute and solvent concentrations can be seen.
The yield of crystals produced by a given cooling may be estimated from the
concentration of the initial solution and the solubility at the final temperature allowing
for any evaporation, by making solvent and solute balances as follows:
For the solvent, usually water, the initial solvent present is equal to the sum of the final
solvent in the mother liquor, the water of crystallization within the crystals and any
water evaporated or:
37
w1 =
w2 + y( R 1)
R + w1 E
-------------- (1)
Where w1and w2 are the initial and final masses of solvent in the liquor, y is the yield of
crystals, R is ratio (molecular mass of hydrate/molecular mass of anhydrous salt) and E
is the ratio (mass of solvent evaporated/mass of solvent in the initial solution).
For the solute:
w1c1 = w2 c2 + y / R
--------------- (2)
Where C1 and C2 are initial and final concentration of the solution expressed as (mass of
anhydrous salt/mass of solvent).Substituting for w2 from equation (1),
w1c1 = c 2 w1 (1 E ) y
R 1
y
+
R
R
----------------------- (3)
From which the yield for aqueous solution is given by,
y = Rw1
c1 c2 (1 E )
1 c2 ( R 1)
--------------- (4)
The actual yield may differ slightly from that given by the equation since, for example,
when crystal are washed with fresh solvent on the filter, losses may occur through
dissolution. On the other hand, if mother liquor is retained by the crystals, an extra
quantity of crystalline material will be deposited on drying.
Since published solubility data usually refer to pure solvent and solute that are rarely
encountered industrially, solubility should always be checked against the actual
working liquors.
Before equation (4) can be applied to vaccum or adiabatic cooling crystallization, the
quantity E must be estimated from a heat balance.
E=
qR (c1 c 2 ) + c p (T1 T2 )(1 + c1 )[1 c 2 ( R 1]
[1
c2 (R 1)] qRc2
------------------------ (5)
In this equation is talent heat of evaporation of the solvent (J/Kg),q is the heat of
crystallization of the product (J/Kg),T1 is the initial temperature of the solution (K),T2 is
the final temperature of the solution (K) and Cp is specific heat capacity of the solution
(J/KgK).
Batch crystallization is characterized by the fact that the system is always in the
unsteady state. The initial super saturation at which crystallization starts will drop
quickly from relatively high value to the saturation value. If crystal growth is to
continue, the solution must be maintained in the meta stable region. As a consequence,
cooling must continue and the batch temp. must continue to drop during the growth
38
period. In batch crystallization it is comparatively easy to penetrate the labile zone

producing a fine mass of fine crystals. By using controlled seeding the solution will not
become labile thereby aiding crystal growth.
5.
Description:
This cooling type batch crystallizer set up consists of an open jacketed vessel provided
with heating & cooling arrangement. The feed is prepared in the crystallizer itself with
water. Steam generator is provided for steam which is used to heat the solution. The hot
super saturation solution in the crystallizer is cooled by circulation of cooling water and
crystals are formed. Water tank with chilling unit is provided for cooling.
Technical Details:
6.
Evaporator
Open pan type.
Heater
4 kW (For Steam generator).
Utility required:
1. Electrical supply: Single Phase, 220 V AC, 50 Hz, 32 Amps MCB with earth
connection.
2. Water Supply
3. Drain required.
4. Chemicals Required:
MgSO4. 7H2O (approx 4 Kg)
7.
2. Open funnel valve and air vent valve provided at steam generator.
3. Fill steam generator 3/4th with water and close air vent valve and funnel valve.
4. Fill chilling vessel with water by opening the top cover and then close the cover
back to its position.
5. Ensure that ON/OFF switches of the Panel are at OFF position.
6. Connect electric supply to the apparatus.
7. Set the temperature in Digital Temperature Controller for steam in the range 105 to
115 oC.
8. Switch ON the chilling unit.
9. Switch ON the heaters and open steam supply valve.
39
10. Fill measured volume of water in the evaporator vessel (2 to 5 ltrs.).

11. Switch ON the stirrer and set the speed to maximum.
12. Prepare a saturated solution of MgSO4. 7H2O in water in the vessel at 80 C by
dissolving 66.2 gm MgSO4.7H2O in 100gms of solution (1.9586 gm MgSO4.7H2O
per gm of free water). If anhydrous MgSO4 is available then dissolve 32.5gm of
MgSO4 in 100gm of solution at 80C (0.4815gm MgSO4 per gm of free water).
13. Close steam supply valve after observing the temperature of water in the evaporator
vessel up to 80 oC.
14. Decrease the RPM in the range 2-10.
15. Open cooling water inlet and outlet valve of the evaporator vessel.
16. Switch ON the pump of chilling unit and set the flow rate by by-pass valve of
chilling unit.
17. Record Rotameter reading (flow rate may be fixed such that the rise in cooling
water temperature is maximum around 5-7C maintain).
18. Record the temperature of inlet water, outlet water and solution temperature with
the help of respective temperature sensors.
19. Put 10 gm MgSO4.7H2O in the crystallizer when the temp reaches to atmospheric
value. For seeding.
20. After two hours, stop the cooling water supply; collect the slurry in the bottom
receiving tank that is fixed with a mesh at the top. The crystals shall be collected on
the mesh and liquid in the tank.
21. Collect all the crystals from the mesh on a filter paper and weigh. Let the weight of
the product crystals be P1 (kg). (For collecting all the crystals you may flush the
crystallizer tank with 100-200ml of saturated MgSO4 solution).
22. Repeat the experiment for different stirrer speed.
8.
Observation and Calculations:
DATA:
Tsi
---------- oC
S at Tsi (80 oC) = ---------- gm/gm of solution. (from solubility data)

w
---------- kg/m3
40
OBSERVATIONS:
Wsi
---------- kg
Wsolni =
---------- kg
Vli
---------- L = ---------- 10-3 m3
Tsf
---------- oC
t, min
TwiC
P1
= ---------- kg
P2
= ---------- kg
Wml
= ---------- kg
(Wsi + Wli)
TwoC
Ts C
Calculations:
S at Tsf = ---------- gm/gm of solution.(from solubility data)
Wli =Vli
%re cov ery =
,kg = ---------- kg
P2
100
Wsi
Material Balance
Water
Solid
Total
Feed
Wli
Wsi
Wli+ Wsi
Crystal
P1 + P2
P2
P1
ML
Wml
S at Tsf
Wml+ S at Tsf
41
9.
Nomenclature:
Twi
Inlet water temperature. oC
Two
Outlet water temperature. oC
Ts
Temperature of solution. oC
Wli
Initial weight of liquid ,kg.
Wsi
Initial weight of Solid taken ,kg.
Wsolni =
Total Initial weight of Solution (Wsi + Wli) ,kg.
Wml
Weight of mother liquor recovered ,kg.
P1
Crystal recovered before drying,kg.
P2
Crystal recovered after drying ,kg.
ML
Mother liquor.
Tsi
Desired initial temperature of solution ,oC
Tsf
Final temperature of solution ,oC
S at Tsi =
Solubility at temperature Tsi ,gm/gm of solution.
S at Tsf=
Solubility at temperature Tsf ,gm/gm of solution.
Density of water, kg/m3
Vli
Initial volume of liquid taken for dissolving solid ,L
Time ,min.
10. Precautions& Maintenance Instructions:

1. Never run the apparatus if power supply is less than 180volts and above than 230
volts.
2. Seeding should be done (if required) at 4540 C.
3. Operator selector switch off temperature indicator gently.
4. Always keep the apparatus free from dust.
5. Proper cleaning with hot water is necessary after experimentation.
42
11.
Trouble Shooting:
1. If electric panel is not showing the input on the mains light, check the main supply.
12.
References:
1. McCabe, Smith Unit Operations of Chemical Engineering, 4th ed, McGrawHill, NY, 1981, Page 797-816
2. Coulson & Richardson, Chemical Engineering Vol-2, 4th ed, Asian Books
Pvt.Lt,
ND,1991,
Page
665-681
43
44

CONTINUOUS DISTILLATION
Scope:
Distillation is a practical method of separating mixtures of liquids, although competition from
other unit operations such as extraction has developed. Distillation allows relatively close
separations to be performed with the use of heat.
Several different methods of distillation are in use and are being studied extensively in the
laboratory.
-Batch distillation has been developed' where the commercial product does not have
tonnage product.
-Continuous distillation is to produce a uniform product and waste
Objective: To study continuous distillation in sieve plate column.
Theory and Formula:

In continuous distillation, feed to be continuously supply and the product removed
continuously provided that rate of feed supply is equal to the rate of distillate out. The rising
vapor comes in contact with a condensed portion of vapor previously evolved from the same
still. A transfer of material and interchange of heat result from this contact, thereby securing a
greater enrichment of the vapor in the more volatile components than could be obtained with a
single distillation operation using the same amount of heat.
Operating line for rectifying section:

F= D + B
..1
..2
The McCabe-Thiele method can be used to determine N (total number of equilibrium stages)
the minimal reflux ratio and the optimal feed stage location .
45
Besides the equilibrium curve the McCabe Thiele methods include a 45O reference line.
Operating line for the upper rectifying section and lower stripping section of the column.
....4
5
The -McCabe Thiele assumptions lead to the condition of constant molar over flow in the
rectifying section where the molar flow rate remains constant .
Since,
V= L+D
.6
7
Similarly
8
.9
46
Operating line for Stripping Section:

Stripping section extends from the feed to the bottom stage. The material balance for the light
key component in the stripping section can be expressed as
.10
11
Feed Line equation:

Value
of q
0
1
0-1
>1
<0
Slope of q-line
Condition of feed
Slope=0 ,i.e. horizontal line

Slope= infinite
Slope= -ve inclined between
saturated liquid and saturated vapor
Slope= +ve, inclined beyond
saturated q-line
Slope = +ve, inclined below
saturated q-line
Feed is saturated vapor

Feed is saturated liquid
Feed is mixture of saturated liquid and
saturated vapor
Feed is liquid below the saturated liquid line
Feed is super saturated vapor
47
12
The thermal condition of feed can be quantitatively expressed by calculating which is given by
the equation
q=
Hg
hf
Hg
hl
H g = molal enthalpy of saturated vapor

h f = molal enthalpy of feed
hl = molal enthalpy of saturated liquid.
Knowing q, the minimum reflux ratio can be calculated (no. of plates required will be infinite)
using McCabe Thiele diagram, assuming say 85 mol% purity of the distillate.
At a known reflux ratio (other than minimum) the theoretical no. of plates can be calculated
using McCabe-Thiele diagram.
Materials and Apparatus:

System used is ethanol-water. Analysis is to be made by refractive index. The actual 'no. of
plates is 12. Feed rate is measured by a rotameter. Distillation column made of glass having
perforated plates. Metering pump for feed and reflux.
1. Calibrate the rotameter with the given solution.
2. Obtain the calibration curve for refractive index vs. alcohol percent.
3. Determine the feed composition and fill reboiler with it.
4. Start heating the reboiler and circulate cooling water in the condenser.
48
5. Determine minimum reflux ratio for the feed conditions assuming 85 mol purity of
distillate.
6. Operate under a reflux ratio higher than minimum reflux, ratio, and obtain samples at
steady states.
7. Measure all flow rates (distillate, reflux, feed, cooling water) and temperature (bottom,
distillate, Condenser inlet and outlet). Measure power (kwh) point input to boiler.
8. Measure refractive indices of samples of feed, distillate and still liquid.
9. Measure the specific gravity of the distillate collected.
Results:
1. Plot refractometer and refractive index calibration curves.
2 . Report equilibrium data for the system under study.
3. Calculate theoretical plates for the reflux ratio chosen.
4. Obtain plate efficiency.
5. Set up material and energy balance equations.
6. Estimate heat loss from column.
7. Submit a McCabe-Thiele diagram for each run.
8. Include in your report the details of any instrument calibration which you have
performed. Such data should be appropriately located as an Appendix.
9. Finally, discuss in the report any difference between your proposed operation and the
actual operating conditions necessary to obtain the desired product
Questions:
1. What is the heat input per unit product at total reflux ratio
2. Discuss the limitations of McCabe Thiele method.
3. Comment on the defects in the experimental set-up .How can you improve it ?
References:
1. Treybal "Mass Transfer Operations' McGraw Hill Book Co., New York. Latest edition.
2. T.K. Sherwood, R.L. Pigford & C.R. Wilke, "Mass Transfer", McGraw Hill, New York
(1975).
3. R-H. Perry, "Chemical Engineering Hand Book", Latest Edition, "McGraw Kill, New
York.
49
Ethanol water Equilibrium Data:
Y mole %
17
38.91
43.75
47.04
50.89
54.45
55.8
X mole %
1.9
17.21
19.66
12.38
16.61
23.37
23.08
Temp.oC
100
95.5
89
86.7
85.3
84.1
82.7
82.3
58.26
61.22 65.64
65.99
68.41
73.85
78.15
89.43
32.73
39.65 50.79
51.98
57.32
67.63
74.72
89.43
T,0C
81.5
80.7
79.7
79.3
78.7
78.4
78.1
79.8
McCabe Thiele diagram:
50
Data Table :
1.1 Data table for mol fraction of ethanol Vs RI(Refractive index)
Mol
fraction of
ethanol
0.05
0.075
0.1
0.125
0.15
0.175
0.2
0.3
RI
1.331
1.339
1.3415
1.345
1.48
1.351
1.353
1.355
1.35
8
0.4
1.36
0.5
1.361
0.6
1.362
0.7
1.362
0.9
1.36
1
1.359
Fig. 7: Continuous Distillation.
51
52

Department of Chemical Engineering
Unit Operation Lab
PLUG FLOW REACTOR
1. Objective:
(a) To study the reaction between ethyl acetate and sodium hydroxide in a tubular reactor.
(b) To study the effect of axial dispersion on the conversion in tubular reactor.
2. Theory:
The reaction between ethyl acetate and sodium hydroxide is represented as (assuming
second
order, irreversible reaction)
NaOH + CH 3COOC 2 H 5
(A)
(B)
CH 3COONa + C 2 H 5 OH
(C)
[1]
(D)
Plug flow reactor design equation
V
=
FA0
xA
dx A
rA
rA = kC ACB = kC A2
= kC A2 0 (1 x A ) 2
Where
[2]
[If CA0 = CB0]
[3]
A
V
dx A
= C A0
Q
kC A2 0 (1 x A ) 2
0
[4]
The residence time is also.
V L
=
Q u
Q =
u =
V =
volumetric flow rate

linear velocity
Reactor volume
Now the flow through the reactor may be either (a) Laminar or (b) turbulent, according to
whether the Reynolds number, NRe,
N Re =
ud t
53
is less or greater than approximately 2000, where and are the density and viscosity of
the
solution (essentially water) flowing through the reactor, dt is the internal diameter of
tube and u
is the mean velocity in the tube.
dt L
u dt
(
)
1
=
kC A0
[5]
xA
dx A
2
(
1
x
)
A
0
dt L
kC A0 =
N Re
xA
A
1
=(
N Re
1 xA
Where,
dt L
N Re
A=
dt L
dx A
1
=
(
(1 x A ) 2
1 xA
0
1)
[6]
1)
[7]
kC A0
[8]
A graph between NRe and conversion of reactant can be plotted.

(a) For Laminar Flow, the velocity profile is parabolic in shape; the mean exit conversion
of NaOH is given by
a
X = 1 1 = ka0
a0
Where,
a1
a1
2 2
k 2 a0
2
ln
2 + ka0
ka0
[9]
= Mean outlet molal concentration of NaOH

= Outlet molal concentration of NaOH
(b) For Turbulent flow, the velocity profile is not too for removed from being flat in shape
(i.e. Plug flow). The Exit concentration of NaOH is given by
a1
1
=
a0 1 + a0 k (V )
Q
where,
[10]
a1 = Outlet molal concentration of NaOH
Equations (9) and (10) are based on the assumption of a second order irreversible
constant volume reaction. Provided plug flow exists and there is no radial or longitudal
diffusion of reactants in the liquid and the two reactant inlet flow rates are always in a
constant ratio to each other, it may also be shown that
54
r=
d (n1 n0 )
d (V / n0 )
[11]
Where, r = specific reaction rate at the exit of the reactor, referred to ethyl acetate
n0 = inlet molal flow rate of either reactant
n1 = exit molal flow rate of ethyl acetate
Dispersion Model
D d 2 xA
uL dz 2
dx A
dz
k C A0 (1 x A ) 2 = 0
[12]
The solution of the above equation for small deviations from plug flow is given by
C
CA
D
= 1 + 2( )kC A0 ln A0
C Ap
uL
C Ap
[13]
Where CAp is the concentration of the plug flow reactor with the same or L as the real
reactor.
Levenspiel and Bishchoff have given the graphical solution for second order reaction
having equal concentration. In this graph, conversion based on dispersion model is a
function of dispersion number.

55
3. Equipment/ Apparatus:
3.1
Coil type tubular reactor (0.5 cm ID) and o.9 meter long
3.2
Constant Temperature Bath
3.3
Rotameters for flow measurement of ethyle acetate and sodium hydroxide
solutions.
3.4
Sodium Hydroxide and ethyle acetate solutions [0.05(N)]
3.5
Standard solutions of sodium hydroxide and HCl for titration (analysis).
4. Experimental Procedure
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
Set at desired temperature the constant temperature bath.

Adjust the rotameter readings so that an equal molar flow rate of both reactants
enter the reactor.
The density of ethyl acetate is 0.898 gm/ml at 25oC and its Molecular Weight is
88. Hence 10 ml of ethyl acetate added to 2030 ml of distilled water produce a
0.05 N solution.
Collect product samples in a flask when the steady state is reached.
Analyse the samples and find the concentration of reactant by analyzing the
sample by titration.
Repeat the run at 3 different temperatures (50oC, 70oC and 80oC)
Repeat for other flow rates at a given temperature. This will generate data of
Reynolds no. vs conversion.
After the last run, pipette out the reactor contents and allow distilled water to
flow through the rotameters and reactor for a few minutes.
5. Calculation
5.1.
5.2
5.3
5.4
5.5
5.6
Calculate the conversion for different flow rates at a given temperature from the
exit concentration of sodium hydroxide.
Calculate rate constant k at different temp using plug flow reactor equation.
Calculate NRe and evaluate the rate constant for each run from equation (9) or
(10) as appropriate.
Calculate dispersion number from different conversion and flow rate.
Determine also to extent to which the specific reaction rate given by the
equation (11) is consistent with the hypothesis of an irreversible second order
reaction.
Calculate NSc (Schmidt No. /D) and N`Re ,where D is diffusion coefficient
(diffusivity of the solution ). Diffusivity of ethyl acetate into water can be taken
as diffusivity for the whole system. Diffusivity of EtOAc in water can be
calculated from
D AB =
Where
DAB
VA
MB
=
=
=
=
=
(117.3 10
18
)( M B ) 0.5 T
V A0.6
Diffusivity of ethyl acetate in water, m2/S
Solute molar volume at normal boiling point, m3/kmol
Molecular weight of the solvent, kg/kmol
Average Viscosity of reacting fluids, kg/ms
Average density of reacting fluids.
56
5.7
Calculate D/udt from following figure using value NRe and NSc
Figure-8.2
5.8
5.9
Calculate conversion x from figure 8.1 and compare with actual conversion.
Estimate the maximum possible error in measuring the rate constant at any given
temperature in the experiment.
6. Results and Discussion:

6.1
6.2
6.3
6.4
Plot NRe Vs conversion for plug flow reactor model (without dispersion) and
dispersion model for different temperature.
Plot lnk vs reciprocal of temperature (1/T) and calculate activation energy.
Plot NRe vs D/udt for given value of NSc (Similar to figure 8.2)
Discuss the experimental errors involved in the experiment and what
improvements should be made in the equipment in order to improve the
accuracy of the data.
57
7. Questions:
7.1
7.2
What are the assumptions involved in the derivation of dispersion model?

Why dispersion model is important to study the performance of the Plug Flow
Reactor?
What are the sources of error in evaluation of dispersion number and
conversion?
7.3
8. Nomenclature
=
Inlet molal concentration of NaOH
a0
=
Outlet molal concentration of NaOH
a1
=
Mean outlet molal concentration of NaOH
a1
CA
=
Molar Concentration of NaOH
CA0
=
Molar concentration of NaOH at initial conditions
CB
=
Molar Concentration of Ethyl Acetate
dt
=
Diameter of Tube
D
=
Axial dispersion coefficient for flowing fluid (m2/s)
DAB
=
Diffusivity of ethyl acetate in water, (m2/s)
FA0
=
Initial molar flow rate of A (moles/s)
k
=
Arhenious Constant
L
=
Reactor Length (m)
MB
=
Molecular weight of the solvent, kg/kmol
NRe
=
Reynolds Number
NSc
=
Schmidt Number
n0
=
Inlet molal flow rate of either reactant
n1
=
Exit molal flow rate of ethyl acetate
rA
=
Rate of reaction (moles/m3s)
T
=
Temperature, (K)
u
=
Velocity of Fluid (m/s)
Q
=
Volumetric flow rate (m3/s)
V
=
Volume of reactor (m3)
xA
=
Conversion of reactant A
=
=
=
Average Viscosity of reacting fluids, (kg/ms)

Average density of reacting fluids (Kg/m3)
Total volumetric flow rate, assumed to be equally divided at inlet between
NaOH and Ethyl Acetate.
Residence Time (s)
9. Safety measures and precautions

9.1
9.2
9.3
9.4
Never run the apparatus if power supply is less than 180 volts and more than 230
Volts
Never switch ON mains power supply before ensuring that all the ON/OFF
Operate selector switches gently
Dont operate the apparatus on uncovered feet.
58
PFR
OH Feed
Tank
NaOH (A)
Temperature
Controller cum
Indicator
Ethyl
Acetate
Mixing
Tee
Reactor Feed
Rotameter A
Reactor Feed
Rotameter B
Reactor Inlet
Reacto
Tubular Reactor
Stirrer
Temperature
Sensor
Heater
Constant Temperature bath
59

CONTINUOUS STIRRED TANK REACTOR

1. Objective:
To study a non-catalytic homogeneous second order liquid phase reaction in a
C.S.T.R at different temperatures.
2. Aim:
To determine the reaction rate constant for saponification of ethyl acetate with
NaOH at different temperatures.
3. Introduction:
The stirred- tank reactor in the form of either a single tank, or more often a series of
tanks, is particularly suitable for liquid-phase reactions, and is widely used in the
organic chemicals industry for medium and large scale production. It can form a
unit in a continuous process, giving consistent product quality, ease of automatic
control, and low manpower requirements.
4. Theory
REACTION:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH

Residence time,
VR
, min
Vo
VR
Reactor volume (volume of fluid in the reactor), ltrs.
Vo
Volumetric feed rate (Feed rate of Reactant A + Reactant B),

LPM.
The performance equation for the mixed flow reactor at steady state is:
VR
Vo
C Ao X A
rA
C Ao C A
rA
60
XA and rA are evaluated at exit stream conditions, which are the same as the
conditions within the reactor.
For a second order reaction:
A+BC+D
with CAo = CBo and negligible change in density of reaction mixture
rA = kC A2
Hence,
VR
Vo
C Ao X A
rA
Degree of conversion, X A =
and rate of reaction,
the rate constant,
(C Ao
C Ao C A
kC A2
CA )
C Ao
rA =
k=
C Ao C A
rA
C Ao * X
, g mol/l min
C Ao C A
, l/g mol. min
C A2
For nth order reaction, rA = kC An
log(
rA )= log k + n log C A
The order of the reaction, n, can be obtained from a plot of log (-rA) vs. log CA,
that yields a straight line with slope = n, and intercept (at CA= 1 or at log CA=0)
shall give the value of log (k).
Also, a plot of t vs. XA/ (1-XA)2 shall yield a straight line for an assumed second
order reaction with slope = 1/ (k CAo). From this slope, rate constant, k, can be
obtained.
5. Description:
The set up consists of two sump tanks in which reactants (ethyl acetate and NaOH)
are stored. Reactants are supplied to overhead tanks by pumps. Reactants are
supplied to the CSTR from overhead tanks at particular flow rate maintained by
rotameters. The CSTR is fitted with stirrer for proper mixing. From the top outlet of
the reactor, samples are collected for analysis. Products coming out from the reactor
are analyzed by chemical titration.
TECHNICAL DETAIL:
Reactor
:
Material SS, Volume 2.15 ltrs.
Stirrer
:
Material SS.
61
7.8. Electricity Supply: Single Phase, 220 VAC, 50 Hz, 5-15 Amp socket with
earth connection.
7.9. Distilled Water (To prepare solutions).
7.10. Drain required.
7.11. 5 Conical Flasks.
7.12. Measuring cylinder.
7.13. Stopwatch.
7.14. Burette.
7.15. CHEMICALS:
QUANTITY:
NaOH Pellets
100 gm
N/10 HCl
100 ml
Ethyl Acetate
200 ml
Indicator (phenolphthalein)
Few drops
7.1
Prepare 20 L of 0.05(N) NaOH solution by dissolving 40 gm of NaOH in 20 L

of water.
7.2
Prepare 20 L of 0.05(N) ethylacetate solution by mixing 100.12 ml of ethyl

acetate in 20 L of water.
7.3
Fill the respective tanks with these solutions.
7.4
Switch ON the pumps to fill the overhead tanks with the solutions.
7.5
Pass equal volumetric feed rates of ethyl acetate and NaOH into the CSTR.
7.6
Switch ON the stirrer after level of the reactor reaches about 3/4th its volume.
7.7
Switch on the heater provided and set the desired reaction temperature in the
temp controller.
7.8
After desired temperature is attained , about 10 min or time equal to the

residence time of the reactor (which ever is greater) i .e when steady state is
achieved, collect exact 10 ml of the sample of the liquid from the outlet of
CSTR, in a graduated cylinder that already contains 20 ml of 0.05N HCl.
7.9
Using phenolphthalein as indicator, titrate this solution (i.e excess HCl)

against 0.05N NaOH (add NaOH from burette) and note the volume of 0.05N
NaOH used ( VNaOH)
7.10 Repeat all the steps for different flow rates of feed and different reactor
temperatures.
62
8. Observation and Calculation:

DATA
VR
2.15 L
CAo
= ---------- g mole/L
VHCl
---------- ml
NHCL = ---------- g mole/L
VSAMP =
---------- ml
NNaOH = ---------- g mole/L
Observation Table:
Sl.
No.
Temperature
(degree C)
Flow Rate(LPH)
Et. Acetate
NaOH
Volume of
sample
(ml)
Burette Reading(ml)
(Vol of NaOH reqd)
Vo
--------- LPH
VNaOH =
---------- ml
CALCULATIONS:
V N
HCLO = HCL HCL , g mole
1000
HCLR = HCLO
CA =
XA =
=
k=
(VNaOH
N NaOH )
, g mole
1000
HCLR
1000 , g mole/L
VSAMP
(C Ao
CA )
C Ao
= ---------------- g mole
= ---------------- g mole
= ---------------- g mole/L
= ----------------
VR * 60
,min
Vo
= ---------------- min
C Ao C A
, l/g mol. min
C A2
= ---------------- L/g mole min
Plot t vs. XA/ [1-XA]2 on a simple graph, the slope is = 1/ (k CAo); from the slope
find k and report k at the different reaction temperatures and determine the
activation energy.
63
9. Nomenclature:
CA
Conc. of unreacted NaOH in the reactor, g mole/L
CAo
Initial concentration of NaOH in feed, g mole/L
HCLO
Amount of HCL taken as quench, g mole
HCLR
Amount of HCL reacted with NaOH, g mole
Rate constant, l/g mol. min
NHCL
Number of moles of HCL used, g mole/L
NNaOH
Number of moles of NaOH used, g mole/L
VR
Volume of the reactor, L
VSAMP
Volume of sample collected, ml
VHCL
Volume of HCL, ml
VNaOH
Volume of NaOH, ml
Vo
Volumetric flow rate, g mole/L
XA
Fractional conversion
Residence Time, min
10. Precaution and maintenance instructions:

10.1
Always use clean water and good quality chemicals and standard solution
for titration.
10.2
Use electronic balance for weighing of chemicals. Dont mix the droppers of
different chemicals.
10.3
Handle the chemicals carefully.
11. Troubleshooting:
11.1
If there is any leakage tight that part or remove that and fix that again after
wrapping Teflon tape.
11.2
If Rotameter fluctuating more than average tight control knob of that.
12. References:
12.1
Octave Levenspiel, Chemical reaction engineering,3rd ed., John Wiley &

Sons, NY, 2001, Page 90-97.
12.2
Coulson & Richardson, Chemical Engineering Vol-3 4th ed, Asian Books
Pvt.Lt, ND, 1991, Page 43-45, 61, 64-65.
64
65

BATCH REACTOR
1. Objective:
The objective of this experiment is to determine experimentally the rate equation for
the saponification of ethyl acetate using a batch reactor.
2. Theory and Formulae:

The saponification reaction between ethyl acetate and sodium hydroxide is
represented as:
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
(1)
For simplicity the reaction is represented as:
A+ B
k1
C+D
(2)
Assuming that the reaction is reversible and second order in both directions, the
specific reaction rate for the batch operation is given by
r=
dC A
1 dN
=
= (k1C A C B
V dt
dt
k 2 CC C D )
CA, CB, CC, CD represents concentrations of A, B, C and D respectively

V
Volume of the reaction mixture
Moles of ethyl acetate present in the reactor at time t
k1, k2 =
Rate constant for the forward and backward reactions.
If equal concentrations of reactant are used so that CA = CB and reverse reaction can
be neglected (k2 is very small).
dC A
= k1C A2
dt
or
Integrating (3) we get:
dC B
= k1C B2
dt
(3)
66
1/CB = 1/CB0 + kt
(4)
where t = time required to reduce the concentration of B (i.e. NaOH)

from CB0 to CB.
Thus a plot of (1/CB) vs t would yield a straight line from which k1 can be
estimated.
If differential approach is used, then plotting log
dC B
dt
and log (CB) would
yield a straight line,
log
dCB
dt
= log k1 + n log CB
(5)
where n is the reaction order

The dependency of k1 on temperature is given by the Arrhenius equation:
k1 = k10 e
RT
Thus a plot of log(k1) vs 1/T would yield a straight line, which enables evaluation of
k10 and E.
3. Description:
The apparatus consists of a stirred reaction vessel (2 liters) contained in a hot water
bath, equipped with temperature controller to control the bath temperature along
with the reactor. Measured volume of NaOH solution is to be poured in the stirred
reaction vessel. A stirred heated tank (for ethyl acetate solution) is provided to
maintain a constant temperature by another temperature controller. The outlet of this
tank is connected to reaction vessel and outlet valve is to be operated to mix the
ethyl acetate solution with NaOH solution (in reaction vessel) after reaching desired
temperature (of both solutions).
4.1
Electricity Supply: Single Phase, 220 VAC, 50 Hz, 5-15 Amp socket with
earth connection.
4.2
Distilled Water (To Prepare Solution).
4.3
Drain required.
4.4
12 Conical Flasks.
4.5
Measuring cylinder.
67
4.6
Stopwatch.
4.7
Burette.
4.8
CHEMICALS:
QUANTITY:
NaOH Solution, 0.1(N)
5 Liters
N/10 HCl
100 ml
Ethyl Acetate Solution, 0.1(N)
5 liters
Indicator (phenolphthalein)
Few drops
7.11 Standardize NaOH using given HCl.
7.12 Prepare 5 L of 0.1N NaOH solutions by dissolving 20 gm of NaOH in 5 L of
water.
7.13 Prepare 5 L of 0.1N ethyl acetate solution by mixing 49 ml of ethyl acetate in
5 L of water.
7.14 Switch ON the temperature bath and maintain a temperature of 60OC.
7.15 Add NaOH and ethyl acetate in the reactor and stir well, use appropriate
quantities to ensure that the concentrations of both equal in final 2 liter
misture.
7.16 Pipette 25 ml of the standard HCl into each of the 12 numbered 250 ml conical
flasks.
7.17 At specified times ( initially at 1 or 2 min interval and afterward at 5 min
interval), pipette out known amount (5-10 ml) of reaction mixture and add it to
the conical flasks containing known amount of HCl one after the other.
7.18 Titrate with standard NaOH using phenolphthalein as indicator.
7.19 Repeat the above procedure for 50 OC, 40 OC, 30 OC.
8. Observation, Calculation and Results:

8.1
Tabulate experimental readings as well as calculations in a format similar to

the one given below:
Time
(min), t
ml of 0.1(N) HCl 0.1(N) NaOH Unreacted NaOH NaOH

to quench 5 ml of ml
in 5 ml reaction reacted
reaction mixture
(titrate Volume) mixture (CB0- CB) CB
8.2 Plot CB vs t from this graph get smoothened CB vs t data.

68
8.3
Calculate CB and t and hence
8.4
Plot
CB
CB
t and CB avg.
t vs CB avg and calculate k1 and order of reaction from equation
(5) (on log log plot).

8.5 Plot (1/CB) vs t and estimate k1 from equation (2) compare it with results from
equations (4) and (5).
8.6
Repeat the procedure for all the 4 temperatures and plot logk1 vs 1/T.
8.7
Report the whole rate equation and the difference between results from
equations (4) and (5) as % difference.
8.8
Estimate the maximum possible error in measuring the rate constant at any
given temperature in the experiment.
8.9
Using your own experimental data calculate the rate constant, determine its
standard deviation, its 95% confidence limit and compare it with the error
calculated in 8.8. Explain whether the difference is reasonable.
9. Questions:
9.1
Set up the equations and show how you will calculate the constants if the
concentrations CA and CB are not equal.
9.2
Can you use this type of reactor for determining rate of reaction of a
(i)
Heterogeneous reaction
(ii)
Rapid reaction
(iii) Reaction yielding a number of products

(iv) Gas phase reaction
9.3
In case you can use this reactor mention additional equipments needed.
Otherwise, point out the difficulties which make it impractical to be used in a
particular case.
9.4
Write down the drawbacks of this method of finding kinetics.
9.5
Suggest improvements in the experimental set up if you come across any

drawbacks and shortcomings.
10. References:
10.1 Octave Levenspiel, Chemical Reaction Engineering,3rd ed., John Wiley &
Sons, NY, 2001, Page 90-97.
10.2 Coulson & Richardson, Chemical Engineering Vol-3 4th ed, Asian Books
Pvt.Lt, ND, 1991, Page 43-45, 61, 64-65
69
Batch Reactor
70

SEMI-BATCH REACTOR
1. Objective:
To determine the reaction rate of saponification of ethyl acetate by varying reactants
flow rate in a semi-batch reactor.
2. Theory and Formulae:

In the experimental setup, one reactant is added continuously to an initial fixed
quantity of the other reactant. No stream is taken out. The concentration changes
because of accumulation as well as reaction.
Consider a semibatch reactor, in which there is a continuous feed, no withdrawal of
product and a mass mAi of component A initially in the reactor.
The reacton taking place is:
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
A
(1)
where
B: NaOH A: Ethyl Acetate
D: EtOH
C: NaAc
The mass balance equation is:
F0W A0
(rV ) M A =
d [Va ]
MA
dt
(2)
where,
V
= volume of reactor at the particular instant in litres
F0
= mass feed rate, gm/min,
WA0
= mass fraction of A in feed
MA
= molecular weight of reactant A
= concentration of A in moles/lit.
= rate of reaction (gmol of A reacting/min.litre
The concentration will be related to conversion, x , which defined as ratio of amount

of A converted to the total amount A added up to that time and is given by:
71
a=
[ m Ai + F0W A0 t ](1
x)
(3)
M AV
Differentiating (3):
d (V .a) =
1
[ (m Ai + F0WA0 t )dx + (1 x) F0WA0 dt ]
MA
(4)
Substituting (4) in (2) and simplifying:

(5)
If there were no A initially present in the reactor, then mAi is zero and the expression
becomes
F0WA0 ( xdt + tdx) = (rVdt ) M A
(6)
where V = V0 + (F0/)t
V0
= Initial volume,
= density of the mixture,
= volume at any time t
Equation (6) can be written as:
F0WA0 [ x + t (dx / dt )] = rVM A

or
x + t (dx / dt ) =
rV
MA
F0WA0
(7)
If x vs t data are available, one can calculate the rate constant k1.
3. Materials and Apparatus:

1.1
Semibatch reactor (2 liters)
1.2
Rotameter
1.3
Standard solution of NaOH and HCl
1.4
Ethyl acetate (0.03N)
1.5
NaOH solution (0.03N)
1.6
Phenlphthalein indicator
72
4.1 Prepare standard HCl and NaOH solutions.
4.2 Fill the vessel with ethyl acetate of known concentration (1 liter)
4.3 Maintain the temperature at desired level.
4.4 Start NaOH flow rate (max 80 ml/min)
4.5 Pour 20 ml HCl solution and 1-2 drop of indicator in each of 12 numbered
conical flasks.
4.6 Fill burette with NaOH solution.
4.7 At specified times (at 5 min interval), pipette out known amount (5-10 ml) of
reaction mixture and add it to the conical flasks containing known amount of
HCl one after the other.
4.8 Titrate with standard NaOH.
4.9 Repeat the process for at least 3 different flow rates
4.10 Repeat the above procedure for at least 3 different temperatures.
5. Observation, Calculation and Results:

5.1
Tabulate experimental readings as well as calculations in a format similar to

the one given below:
Time ml of .(N) Ml of .(N)
(min), HCl to quench NaOH
t
.
ml
of (titrate Vol)
reaction mix
Unreacted
NaOH
NaOH in . ml reacted
reaction
mix CA
(CA0- CA)
Conversion
(x)
CA/ CA0
5.2
Plot change of concentration of NaOH vs time for different flow rates.
5.3
Apply equation (7) and calculate rate constant.
5.4
Discuss the experimental errors involved in the experiment and what

improvements should be made in the equipment in order to improve the
accuracy of data
5.5
Estimate the maximum possible error in measuring the rate constant at given
temperature in the laboratory experiment.
5.6
Repeat the procedure for all the 4 temperatures and plot logk1 vs 1/T.
5.7
Discuss some examples in which semi-batch operation is advantageous.
5.8
Write material balance equation for a second order irreversible reaction

A+BC+D
73
in which concentration of A is constant whereas that of B is changing.
74

RTD STUDIES IN CSTR & PACKED BED
1.
Objectives:
a).
To experimentaly measure the residence time distribution (RTD) of a

CSTR and a Packed Bed.
2.
b).
To model the non-ideality of the CSTR using the tank- in- series model .
c) .
To model the non-ideality of the packed bed using the dispersion model.
Introduction
Real reactors do not satisfy the ideal flow patterns, i.e. complete mixing (ideal
CSTR) or no mixing (plug flow reactor).Except for an ideal PFR , different
flow elements spend different times in the reactor , i.e. there is distribution of
residence times in the reactor.Deviation from
ideality may be due to the
channeling of fluid through the vessel ,recycling of fluid within a vessel or due
to the presence of stagnant regions in the vessel.
3.
Theory
The RTD of a reactor is the characteristic of the mixing that occurs in the
reactor, and can be deternind experimentally by injecting an inert tracer into the
reactor at t=0 and measuring the tracer concentration,C, in the efflunt stream as
a function of time. The two common modes of injecting the tracer are either to
give a pulse or step input .
The typical response for the pulse input for different type of reactors is shown
below:
75
Ideal CSTR
Ideal PFR
time
Non- ideal reactor
time
time
The RTD function, E(t) , is defined such that E(t)dt gives the fraction of material that
has a residence time between t and t+dt . Thus, by definition
E (t )dt = 1
(1)
It can be shown that for a pulse input

C (t )
E (t ) =
C (t )dt
(2)
where C is the tracer concentration measured at the reactor outlet.

1
For an ideal CSTR ,
E (t ) = e t / or in dimensionless coordinates E() = e-
where =t/ and E() = E.
The mean residence time , tm , can be calculated as
tm =
tE (t ) dt
E (t )dt
t E dt
(3)
It can be shown that for a closed system (i.e. fluid enters and leaves by plug flow)
V
(4)
tm = =
Q
where is the space time , V is the volume of the reactor and Q is the volumetric flow
rate.
The RTDs are usually compared by taking moments. The first moment is the mean
residence time .The second moment (taken about the mean ) is called the variance (2)
and can be calculated as
2
=
0
(t t m ) 2 E (t )dt
t 2 E (t )dt t m2
(5)
(6)
The variance measures the spread of the RTD .

76
4.
Modeling of Non-Ideal Reactors:
Different types of models have been proposed for modeling the nonideality in
chemical reactors. The most commonly used are the tank- in - series model and the
dispersion model. Both of these are one parameter models .
Tank-in-series model:
In this model, the actual reactor is taken to be equivalent to a number of equal volume
ideal CSTRs in series. The total volume of all the reactors is equal to the total volume of
the non-ideal reactor.
It can be shown that for N reactor in series
E (t ) =
t/
t N 1e
( N 1)! N
i
,
(7)
V = NV
i
N,
and
2
(8)
N
Thus, form the experimentally measured RTD, N can be calculated. It should be noted
that N has to be an integer.
Dispersion Model:
This model is usually used for the modeling tubular or packed bed reactors for which
the flow does not deviate too much from an ideal PFR . In this model , it is assumed
that all the non- idealities can be accounted for by a dispersion term superimposed on
the bulk flow . The axial dispersion coefficient, DL , is used to characterize the degree
of back mixing during the flow . DL is assumed to be independent of the axial position.
For a closed- closed system, it can be shown that.
tm =
and
2
t2
m
2
Per
(9)
2
( Per ) 2
Pe r =
(1 e
uL
DL
Per
(10)
(11)
77
where L is the length of the reactor , u is the superficial linear velocity , is the bed
voidage, and Per is the reactor Peclet number and represent the rate of transport by
convection to the rate of transport by dispersion.
The fluid Peclet number, Pef ,is defined using the characteristic length that determines
the fluids mechanical behavior. For the packed bed, the characteristics length is the
particle diameter, dp and for empty tubes it is the tube diameter, dt . For a packed bed
Pe r =
u dp
DL
where u/ is the interstitial velocity of the fluid.
( 12)
The usual values of Per and Pef for the packed bed are nearly 103 and 10 1
,respectively. From the definitions
L
for packed beds (13)
dp
L
and
for empty tubes
Per = Pe f
dt
Open open system : When a tracer is injected into a packed bed at a location
Per = Pe f
more than two or three particle diameters downstream from the entrance and measured
some distance upstream from the exit , the system is analogous to an open-open system.
For such a system
tm = 1 +
2
2
Per
(14)
2
8
(15)
+ 2
Per Per
t
We can determining Per by determining tm and 2 from the experimental data and then
and
2
m
use equation (15) to calculate Per .We can also calculate tm and then use equation (14)
as a check, but this is usually less accurate . Once Per is known DL can be estimated.
5. Description:
The setup consists of one sump tank to which water is fed. Water is supplied to the
overhead tank by pump. Two reactors (CSTR, Packed bed) are provided for RTD study
which can be used one at a time. Water is supplied from overhead tank to any of the
reactor at particular flow rate maintained by the Rotameter. A pipette is used for dozing
the tracer into the C.S.T.R. while a special arrangement is provided to inject tracer at
the lower end of reactor, using a syringe for packed bed. Samples can be taken
periodically from the top outlet of reactor.
78
Technical details :
Reactor
CSTR (Material SS, Volume 2.4 ltrs).

Packed Bed (Material Glass, Packing Rasching Rings ID
6, OD 10 length 10 mm)
6.
Utility required:
Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amps Socket with
earth connection.
1. Water Supply (Initial Fill).
2. Floor Drain Required.
3. 5 conical flask
4. Burette
5. Pipette
6. Measuring cylinder
7. CHEMICALS:
7.
QUANTITY:
N/10 NaOH
200 ml
Concentrated HCl
100 ml
Phenolphthalein indicator
Few drops
1. Fill the sump tank with water.
2. Switch ON the pump.
3. Start the supply of water to the reactor (CSTR or Packed Bed) at particular
flow rate with the help of Rotameter.
4. Input a concentrated HCl into the system (10 ml or 20 ml) with the help of
pipette (tracer signal as a pulse).
5. At regular time intervals (say 15 sec for high water rate, 30 sec for low
water rate), collect the samples at the outlet in beakers/measuring cylinder
(about 20 ml) until all tracer leaves the vessel.
6. Analyze these samples with N/10 NaOH using phenolphthalein as indicator.
79
7.
Repeat the experiment for different flow rates (before changing the flow
rate, drain the reactor first).
8.
Observations and Calculations :

Data :
V1 = -------- ml
N1 = -------- g moles/L
V2 = -------- ml
Observation Table:
S.No.
t, min
V2, ml
Q, LPH
Calculations:
Ci=
V 1N 1
98
V2
tm =
tiCi
,
Ci
= --------------- min
V R * 60
,
Q
= --------------- min
2=
Ei =
A)
ti2 Ci
Ci
= --------------- moles/L
tm2
= --------------- min2
Ci
Ci t
Plot the RTD [ E(t)] curves for both the reactors .
80
B)
For the CSTR from the experimentally determined 2, find N for the
tank-inseries model.
C)
For the packed bed reactor, from the experimentally determined tm and
2 , find Per and DL . Compare DL with those available from
correlations.
9.
Nomenclature:
Ci
10.
Concentration of H2SO4 in sample, moles/L
D/uL =
Dispersion number
Exit age distribution at time
Ei
Exit age distribution at time i
N1
Normality of N/10HaOH, g moles/L
N2
Normality of H2SO4 in solution, g moles/L
time, min
Average time difference, min
V2
Volume of H2 SO4 in sample, ml
V1
Volume of N/10 NaOH used for titration, ml
VR
Volume of reactor, L
Volumetric flow rate, LPH
Reduced time, min
tm
Mean residence time, min
Space time ,min.
s2
Variance.
Precautions and maintenance instructions:

1. Always use clean water and good quality chemicals and standard solution
for titration.
2. Flow should not be disturbed during the experiments.
3. Handle the chemicals carefully.
81
11.
Troubleshooting :
1. If there is any leakage tight that part or remove that and fix that again after
wrapping Teflon tape.
2. If Rota meter fluctuating more than average tight control knob of that.
12.
References:
12.1
Octave Levenspiel, Chemical reaction engineering,3rd ed., John

Wiley & Sons, NY, 2001, Page 260-265, 294-296.
12.2
H.Scott Fogler, Elements of Chemical Reaction Engineering,4th

edition,2006 Prentice-Hall of India, New Delhi, Chapter 13and14.
82
83


CHARACTERISTICS OF PID CONTROLLER
1.
Objective:
To study the characteristics of PID Controller.
2.
Introduction:
Most of the process industries are equipped with the advance and control systems to
improve the productivity of the plant. For design and operation of process control in the
age of rational technology change, engineers & technicians must have training of control
systems.
3. Theory:
The different types of combinations of controller actions used in industrial process are
1. Proportional Controller
2. Proportional Integral Controller
3. Proportional Derivative Controller
4. Proportional Integral - Derivative Controller
PROPORTIONAL CONTROLLER:
The proportional controller produces an output signal, which is proportional to
the error. This action is expressed as
Where
P
KC
PS
= Output signal from the controller

= proportional controller gain
= error
= a constant
The tuning parameter for proportional control are proportional band (PB) Or
proportional gain (KC) and time delay.
Proportional band or throttling range is defined as the error expressed as a
percentage of the range of the measured variable required to allow the heater
generate heat. Proportional gain is the proportional control factor, which is used
to determine the proportional band.
84
PB=100/Kc
PROPORTIONAL INTEGRAL (PI) CONTROL:

This mode of control is described by the relationship
I = Integral Time
Integral action combined with proportional control gives us a controller, which will
always act to maintain the controlled variable at its set point i.e. eliminates offset.
Integral action causes oscillation. PI controller is used widely in flow, level and pressure
control.
PROPORTIONAL DERIVATIVE (PD) CONTROL:

This mode of control may be represented by
where D = derivative time

Derivative action combined with proportional gives a controller which is good on process
containing appreciable lag. The derivative (anticipatory or rate) control gives a faster
response with less oscillations. Where process lag is short, this combination could not be
used.
PROPORTIONAL INTEGRAL DERIVATIVE (PID) CONTROL:

This mode of operation is given by
P = Kc +
Kc
t
o
dt + K c
d
+ Ps
dt
When all the three control effects are combined together, we obtain the benefits of each
control action. A three-mode controller contains the stability of proportional control, ability
to eliminate offset because of integral control and the ability to provide an immediate
correction for the magnitude of disturbance because of derivative control. The rise of the
variable is arrested more quickly and it is returned to the original value with little or no
oscillations.
4.
Description:
It consists of a stirred tank in which a heater is provided to heat the water. Water is supplied
to the tank from laboratory overhead tank by user. The flow rate can be adjusted by operating
the needle valve provided on rotameter. PID parameters can be changed for conducting
experiment on P, PI, PD and PID mode. Controller can be operated on auto tune mode in
which controller automatically fixes the value of P, I and D. Temperature is sensed by the
PID controller and the controller gives the input to the heater , accordingly. Experiment can
85
be performed on various flow rates and temperature set points.
5.
Utilities Required:
Electricity Supply: Single Phase, 220 V AC, 50 Hz, 0.5 kW with earth connection.
Water supply at 100LPH (max.)
Drain
Bench Area Required:
6.
1. Connect continuous water supply and electric supply to the apparatus.
2. Set the flow rate of water to the tank with the help of Rotameter provided.
3. Switch ON the heater and stirrer of the process tank.
4. Set the required temperature in the PID controller.
5. Set the values of P, I, D as per required mode i.e. P, PI, PD or PID.
6. Note the time taken by PV to reach the set point at that particular value of P, I, D.
7.
Observation &Calculation :
To use data logger enter the values of P, I, D and Set point (SP) in the boxes given in
interface mode at the running condition and observe the effect of changing the different
settings.
Click the LOG option to log the data by giving the file name in the appeared window.
View the saved data in Excel file to plot graphs.
8.
Precaution & Maintenance Instructions:

1. Use the stabilize A.C. Single Phase supply only.
2. Never switch on mains power supply before ensuring that all the ON/OFF
3. Never run the apparatus if power supply is less than 180 volts and above than 240
volts.
Always keep the apparatus free from dust.
9. References:
1. Donald R. Coughanowr, Process System Analysis and Control, 2
Hill, NY, 1991, Page 128-129, 130-132.
nd
ed., McGraw
86


STUDY OF A PNEUMATIC CONTROL VALVE
1.Objective:
1. To calibrate a differential pressure transducer (DPT) against a manometer for
pressure drop across the Pneumatic valve.
2. To calibrate the digital flow meter with a wet test meter for flow.
3. To calibrate the control valve.
2. Principle and Formulae:

Valve Capacity:
The Valve Coefficient CV is defined as
CV =
q
( P )1 / 2
G
where q is the volumetric flow rate through the valve in gallons per minute, P is the
pressure drop across the valve in psi ( including inlet and outlet losses) and G is the
specific gravity of the flowing fluid. Stated another way, it is the number of gallons per
minute of water at room temperature which will pass through a given flow restriction
with a pressure drop of 1 psi. For example, a control valve which in the full open
position passes 25 gpm of water with a 1 psi pressure drop has a maximum flow
coefficient of 25. The flow is similarly determined at various increments of valve lift,
and the CV at each increment is obtained. A plot of these values reveals the
characteristic curve of the valve. The curve is made by plotting the percent of
maximum travel against the percent of maximum flow. The characteristic curve thus
obtained reflects the control characteristic of that particular plug and determines
whether it or another type plug is best suited for a particular application.
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3. Equipment/ Apparatus Description:

Introduction: In process control, the final control element is most often a control valve
which is required to regulate the flow of either a process fluid or a utility stream. These
control valves are either pneumatic of motorized, the former being the most commonly
used variety. No matter how sophisticated or advanced is the control strategy, if the
final control element is not proper, the control action cannot be satisfactory. It is
therefore important to examine the performance of the final control element in some
detail. It is often said that more than 50% of the Control engineers time is spent in
calibration and one of the many equipment he has to calibrate is a control valve. We
examine a pneumatic control valve in some detail.
Valve Technology:
Capacity: Rate of flow through a valve under stated conditions.
Characteristics: Relation between flow through the valve and percent rated travel as
the latter is varied from zero to 100%.
Cv : flow coefficient the accepted unit of measurement to define the capacity of the
valve . it is defined as a number of gallons per min of water at room temperature which
will pass through a given flow restriction with a pressure drop of one Psi
Dead Band: The amount of the diaphragm pressure can be varied without limiting
valve plug motion.
Diaphragm Actuator: a fluid pressure operated spring or fluid pressure opposed
diaphragm assembly for positioning the actuator stem in relation to the operating fluid
pressure or pressure.
Equal Percentage Flow Characteristics:

An inherent flow characteristics which, for equal increment of rated travel, will ideally
give equal percentage of the existing flow. Inherent flow characteristics: flow
characteristics when constant pressure drop is mentioned across valve.
Inherent rangeability: ratio of maximum to minimum flow within which the deviation
from the specified inherent flow characteristics does not exceed some stated limits.
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Leakage: Quantity of fluid flow through an assembled valve when valve is fully closed
position under stated closer forces, with pressure differential and temperature as
specified.
Linear flow characteristic: An inherent flow characteristic which can be represented
ideally by a straight line on a rectangular plot of flow versus percent rated travel.
Normally closed: Applying to a normally closed control valve assembly, one which
closes when the actuator pressure is reduced to atmospheric.
Normally Open: Applying to a normally open control valve assembly, one which
opens when the actuator pressure is reduced to atmospheric.
P: The pressure drop across a valve. The condition must be specified. For example: P
for sizing; P at normal flow; P at valve closure etc.
Plug: A movable part which provides a variable restriction in a port.
Seat: That portion of a seat ring or valve body which a valve plug contacts for closure.
Stem: A rod extending through the bonnet assembly to permit positioning the valve
plug.
Trim: The parts (except the body) of a valve which come into contact with the flowing
fluid.
Valve Body: housing for internal valve parts having inlet and outlet flow connections.
4. Equipment and Utilities Required:
4.1
Differential Pressure Transducer (DPT)
4.2
Glass Manometer
4.3
Wet Test meter
4.4
Pneumatic control valve set up
4.5
Electricity Supply: Single Phase, 220 VAC, 50Hz, 5-15 Amp socket with
earth connection.
4.6
Dry air supply @70 psig.
4.7
Bench area required: 2 m X 1 m.
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Figure 1: Study of Pneumatic Control Valve: Pressure Regulated
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Figure 2: Study of Pneumatic Control Valve: Current regulated
Hg Manometer
5.
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5.1
To calibrate a differential pressure transducer (DPT) against a manometer

for pressure drop across the pneumatic valve.
5.2
To calibrate the digital flow meter with a wet test meter for flow
5.3
To calibrate the control valve
Start the flow of air through the test section of the pipe by adjusting the upstream
pressure to 20 psig and opening the control valve slightly by supplying 3.5 psig
pressure to the control valve. Slowly increase the valve opening in steps upto 15
psig by increasing pressure on the dial gauge and note the manometer reading, DPT
reading on a Multimeter and flow through the wet test meter as well as Digital flow
meter provided. Also note down the stem position on a millimeters scale as
accurately as you can. Then note the same readings while decreasing the valve
opening.
6. Calculate:
6.1.
The range of flow from 3 to 15 psi and the range of stem position
movement.
6.2.
Plot manometer P vs DPT output.
6.3.
Plot digital flow meter reading vs wet test meter reading.
6.4.
Plot characteristic curve for the control valve, percentage flow vs

percentage valve opening for both increasing and decreasing flow to see
hysteresis of the control valve.
7. Safety measures and precautions:

7.1
Never run the apparatus if power supply is less than 180 volts and more
than 230 volts
7.2
Never switch ON mains power supply before ensuring that all the ON/OFF
Switches given on the panel are at OFF position.
7.3
Operate selector switches gently
7.4
Dont operate the apparatus on uncovered feet.
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FLOW CONTROL TRAINER
Introduction:
Currently, the PID algorithm is the most common control algorithm used in industry.
Often, people use PID control processes that include heating and cooling systems, fluid
flow monitoring, flow control and temperature control. In PID control, you must specify
a process variable and a set point. The process variable is the system parameter you
want to control such as temperature, pressure and flow rate and the set point is the
desired value for the parameter you are controlling. A PID controller determines a
controller output value, such as the heater power or valve position. The controller
applies the controller output value to the system, which in turn drives the process
variable towards the set point value.
Control System:
The control system is that means by which any quantity of interest in a machine,
mechanism or equipment is maintained or altered in accordance with a desired manner.
Control system is of two types: -
1. Open loop control system:

It is shown in Figure1. Any physical system, which does not automatically
correct for variation in its output, is called open loop system. In these systems, the
output remains constant for a constant input signal provided the external conditions
remain unaltered. The output may be changed to any desired value by appropriately
changing the input signal but variations in external or internal parameters of the system
may cause the output to vary from the desired value in an uncontrolled fashion. The
open loop control is, therefore, satisfactory only if such fluctuations can be tolerated or
system components are designed and constructed so as to limit parameter variations and
environmental conditions as well controlled
.
It is important to note that the fundamental difference between an open and
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closed loop control system is that of a feedback action. Consider, for example, traffic
control system for regulating the flow of traffic at the crossing of two roads. The system
will be termed open loop if red and green lights are put on by a timer mechanism set for
predetermined fixe intervals of time. It is obvious that such an arrangement takes no
account of varying rates of traffic flowing to the road crossing from the two directions.
If on the other for regulating the flow of traffic at the crossing of two roads. The system
will be termed open loop if red and green lights are put on by a timer mechanism set for
predetermined fixe intervals of time. It is obvious that such an arrangement takes no
account of varying rates of traffic flowing to the road crossing from the two directions.
If on the other hand a scheme is introduced in which the rate of traffic flow along both
directions are measured and are compared and the difference is used to control the
timings of the red and green lights, a closed-loop system results. Thus, the concept of
feedback can be usefully employed to traffic control.
Unfortunately, the feedback, which is the underlying principle of most control
systems, introduces the possibility of undesirable system oscillations.
2. Close loop control system

Closed loop control system consists of a process and a controller that
automatically adjusts one of the inputs to the process in response to a signal feedback
from the process output. The performance of the system can be judged by the transient
response of the output to specific changes in the input. The change in the input may be a
change in set point or a change in any one of the several load variables. If the purpose
of the control system is to make the process follow changes in set point as closely as
possible, the operation is called servo-operation. The term regulator operation is
used when the main problem is to keep the output almost constant in spite of changes in
load. The designer must be aware of the purpose of the control system, since the system
that gives optimum servo-operation will generally not be the best for regulator
operation.
Definition:
(Referred from Modern Control Engineering By Katsuhiko Ogata, 4th edition, page no. 2 and
Control system engineering By I.J Nagrath and M.Gopal, 3rd edition, page no. 195)
Control variable & manipulated variable:

The controlled variable is the quantity or condition that is measured and controlled.
The-manipulated variable is the quantity or condition that is varied by the controller so
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as to affect the value of the controlled variable. Normally, the controlled variable is the
output of the system. Control means measuring the value of the controlled variable of
the system and applying the manipulated variable to the system to correct or limit
deviation of the measured value from a desired value.
Plants:
A plant may be a piece of equipment, perhaps just a set of machine parts
functioning together, the purpose of which is to perform a particular operation.
Procedure:
A process may be defined as natural, progressively continuing operation or
development marked by a series of gradual changes that succeed one another in
relatively fixed way and leads toward a particular result or end; or an artificial or
voluntary, progressively continuing operation that consists of a series of controlled
actions or movements systematically directed towards a particular result.
Systems:
A system is a combination of components that act together and perform a certain
objective. A system is not limited to physical ones. The concept of system can be
applied to abstract, dynamic phenomena such as those encountered in economics. The
word system should therefore, be interpreted to imply physical, biological, economic
and the like systems.
Disturbance:
A disturbance is a signal that tends to adversely affect the value of the output of
a system. If a disturbance is generated within the system, it is called internal, while the
external disturbance is generated outside the system and is an input.
Feedback Control:
Feedback control refers to an operation that, in the presence of disturbance tends
to reduce the difference between the output of a system and some reference input and
does so on the basis of this difference. Here only the unpredictable or known
disturbances can always be compensated for within the system.
Delay Time:
It is the time required for the response to reach 50% of the final value in first
attempt. It is represented by Ttd. It is shown in figure below:
95
Tr
Ts
Rise Time:
It is the time required for the response to rise from 10% to 90% of the final value for
over damped systems and 0 to 100% of the final value for under damped systems. It is
shown in figure 2.
Peak Time:
It is the time required for the response to reach the peak of time response or the peak
overshoot. It is represented by Tp. It is shown in figure 2.
Peak Overshoot MP:

It indicates the normalized difference between the time response peak and the
steady output and is defined as:
Peak percent overshoot =
Ctp C
C
x100%
The Mp is represented in figure 2.
Settling Time:
It is the time required for the response to reach and stay within a specified tolerance
band (usually 2% to 5%) of its final value. It is represented by TS in figure 2
Introduction of PID Control System:

This section will show you the characteristics of the each of proportional (P), the
integral (I), and the derivative (D) controls, and how to use them to obtain a desired
response. In this section, we will consider the following feedback system:
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Plant:
System to be controlled.
Controller:
Provides the excitation for the plant; Designed to control the overall system behavior.
THE THREE-TERM CONTROLLER

The transfer function of the PID controller looks like the following:
K c (1 +
1
+ Td s)
Ti s
Kc
Proportional gain
Ti
Integral time
Td
Derivative time
The schematic shown above. The variable (e) represents the tracking error, the
difference between the desired input value (R) and the actual output (Y). This error
signal (e) will be sent to the PID controller, and the controller computes both the
derivative and the integral of this error signal. The signal (u) just past the controller is
now equal to the proportional gain (Kc) times the magnitude of the error plus the
integral gain (Ti) times the integral of the error plus the derivative gain (Td) times the
derivative of the error
Kc
de
edt + K cTd
Ti
dt
This signal (u) will be sent to the plant, and the new output (Y) will be obtained. This
u = Kc
new output (Y) will be sent back to the sensor again to find the new error signal (e). The
controller takes this new error signal and computes its derivative and its integral again.
This process goes on until the error becomes equal to zero.
The Characteristic of P, I, And D Controllers:

A proportional controller (Kc) will have the effect of reducing the rise time and
will reduce, but never eliminate, the steady state. An integral control (Ti) will have the
effect of eliminating the steady-state error, bu t it may make the transient response
worse. A derivative control (Td) will have the effect of increasing the stability of the
system, reducing the overshoot, and improving the transient response. Effects of each of
controllers Kc, Ti, and Td on a closed-loop system are summarized in the table shown
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below.
Note that these correlations may not be exactly accurate, because Kc, Ti, and Td are
dependent of each other. In fact, changing one of these variables can change the effect
of the other two. For this reason, the table should only be used as a reference when you
are determining the values for Kc, Ti and Td.
General Tips for Designing a PID Controller:

When you are designing a PID controller for a given system, follow the
steps shown below to obtain a desired response.
Controller
Settling
Rise Time
Overshoot
Kc
Decrease
Increase
Small Change
Decrease
Ti
Decrease
Increase
Increase
Eliminate
Td
Small Change
Decrease
Decrease
Small Change
Response
Time
Steady-State Error
1. Obtain an open-loop response and determine what needs to be improved.

2. Add a proportional control to improve the rise time.
3. Add an integral control to eliminate the steady-state error.
4. Add a derivative control to improve the overshoot.
5. Adjust each of Kc, Ti, and Td until you obtain a desired overall response.
Lastly, please keep in mind that you do not need to implement all three
controllers (proportional, derivative, and integral) into a single system, if not
necessary. For example, if a PI controller gives a good enough response, then
you don't need to implement derivative controller to the system. Keep the
controller as simple as possible to obtain the system with no overshoot, fast rise
time, and no steady-state error.
Various Types of Control:

(Referred from Process control By Peter Harriott, page no. 6)
1. Proportional Controls:
The cycling inherent with the on-off control would be objectionable for most
processes. To get steady operation when the disturbances are absent, the controlled variable
must be a continuous function of error. With proportional control, the most widely used
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type; the controller output is a linear function of the error signal. The controller gain is the
fractional change in output divided by the fractional change in input.
P = Kc* e -------------------------(1)
Where:
P
= fractional change in controller output
e = fractional change in the error

Kc = controller gain.
The control action can also be expressed by the proportional band width B. The
bandwidth is the error needed to cause a 100% change in the controller output, and it is
usually expressed as a percentage of the chart width. A bandwidth of 50% means that
controller output would go from 0 to 1 for an error equal to 50% of the chart width or
from, say, 0.5 to 0.6 for an error of 5%.
B = 1/Kc * 100 ------------------(2)
Some pneumatic controllers are calibrated in sensitivity units, or pounds per square inch
per inch of the pen travel. For a standard controller with a 3 to 15 psi range and a 4-inch
chart, the gain and sensitivity are related by equation:
S = 3Kc psi/inch--------------------(3)
2. Proportional + Integral Controls:

P = Kc e +
Kc
edt + Ps .(4)
Ti
Where:
Kc = gain
TI = integral time
Ps = constant
P
output
In this case, we have added to the proportional action term, Kc * e, another term that
is proportional to the integral of the error. There is no offset with the integral control,
since the output keeps changing as long as any error persists. However, the initial
response to an error is slow and proportional control is ordinarily used with integral
control. The integral action corrects for the offset that usually occurs with proportional
control only, and the effect is similar to manual adjustment or resetting of the set point
after each load change. The terms reset action and reset rate are widely used to
characterize the integral action of a proportional integral controller.
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reset rate =
1
Ti
3.0 Proportional + Derivative Controls:

This mode of control may be represented by:
de
+ Ps
(6)
dt
In this case, we have added to the proportional term another term, Kc Td (de/dt) that is
P = K c e + K cTd
proportional to the derivative of the error. Other terms that are used to describe the
derivative action are rate control and anticipatory control.
Derivative action is often added to proportional control to improve the response
of slow systems. By increasing the output when the error is changing rapidly, derivative
action anticipates the effect of large load changes and reduces the maximum error.
Description:
For Flow Control Trainer:
The basic objective of this flow controller is to control the flow of liquid in the
pipe line. This set up consists of the following components:
Setup Assembly:
This assembly is used for supporting the various components on the front panel of the
equipment i.e. pressure gauges which is used to measure the pressure, Current to
pressure converter having a range in between 3 to 15 psi i.e. 3 psi for a current of 4mA
and 15 psi for current of 20mA which is given to the I/P converter by Digital Indicating
controller. The setup also contains a pneumatic actuator.
Schematic Diagram of Flow Control Trainer :
Differential Pressure Transmitter:

The flow of the liquid in the pipe line is sensed by the flow transmitter with the help of
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orifice given in the line and after that is transmitted by the transmitter to the computer
through interfacing unit which shows the value of the process variable. This transmitter
converts that accordingly into 4-20mA i.e. 4mA for 0% flow and 20mA for 100 % flow.
Control Valve:
A control valve basically performs the function of controlling the flow of the water in
the pipe line. It is a diaphragm type pneumatic actuator, which varies the flow of the
liquid according to the movement of the stem at a pressure range of 3 to 15 psi, which is
received from I/P converter.
Interfacing Unit:
The interfacing unit is basically a medium for communicating with the equipment from
the computer. In case of flow controller, the flow of the liquid is sensed by the flow
sensor in the pipe line, which is further transmitted into 4-20 mA which means that the
current is 4mA for 0% flow and 20mA for 100% flow and are displayed on the
interfacing unit in terms of 0 to 100%. These signals are further transmitted to the
computer through this interfacing unit by using a RS-232C where the signals are
displayed on the computer screen. The output of the interfacing unit is then transmitted
to the I/P converter, which converts it into 3 to 15 psi that means 3 psi for 4mA and 15
psi for 20mA.
Current to Pressure Converter (I/P convertor):

This converter is basically used to convert the current to pressure having a range of 3 to
15 psi, which shows 3 psi at 4 mA and maximum 15 psi at 20 mA. This I/P converter
receives the continuous input pressure of more than 15 psi and then converts this
pressure into 3 to 15 psi according to the 4 to 20 mA current received by it from the
digital indicating controller.
Installation requirement:
This section gives the necessary details regarding the installation of the equipment and
the software used for interfacing with the equipment. For the installation of the
equipment, following components are required: 8.
Table for support.
9.
Water supply.
10.
Electricity 220V, single phase, 50Hz, 5 Amps socket.
For the installation of the software, following components are required: -
Computer:
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A computer, which is the basic requirement for installing the software for interfacing
with the equipment. But the computer must fulfill the following requirements:1.
The Processor must be at least Celeron 286 MHZ, Pentium III is recommended.
2.
It must have at least 16 MB RAM.
3.
It must have 30 MB hard disk space.
4.
It must have at least Windows 98 OS or higher version of operating system.
5.
There must be an A4 size printer, which is used to get a hard copy of the stored
data required.
Software installation:
1)
Close all the programs running before inserting the CD into CD drive.
2)
Insert the provided CD for the software in the CD drive of computer.
3)
It is an AUTORUN CD. Follow the instructions appeared on the

computer screen and install the software in desired directory.
4)
After completion of installation, reboot your computer.
5)
Then, Open the software directory and double click the exe file of the
software to run the program.
6)
Follow the steps according the experimentation.
Menu and Basic Functions:

This section gives us the detailed information regarding the menus and the basic
function of the control software, which is used to control the equipment. It is shown in
figure 3.
LOGIN:
This menu enables you to start the experiment. In this option, we are given with the
User Name i.e. name of the institute and the Password, which is k.c.engineers. Here
we have also the option of the entering the Professors Name under whose supervision
test is going to be performed, Students name and the Roll Number of the student
who is performing the experiment, which can be used during the report generation. It is
compulsory to select this option first and to fill the correct user name and password to
continue the experiment. Without enabling this option and trying to continue the
process or to select any other option in the front panel shows the display box indicating
that the user must login first for selecting any other option. In this option, password is
compulsory for running the software. In case of wrong password the software will not
102
run and a dialogue box will appear with the software. All other options can be skipped
off if not desired.
View Diagram:
After LOGIN, we have to select VIEW DIAGRAM. This option, which shows us the
complete block diagram of the equipment and tells us how the equipment functions and
also helps in preparing the equipment connection. After that we have to choose the
BACK option and then decide to choose either the SIMULATION to access data from
the simulation logic in order to start the experiment or INTERFACE to access with the
real time data.
Simulation:
Selecting this option accesses data from the PID simulation logic. This option doesnt
use any real time data. In this case, the process values and set point are to be entered by
the user and then observes the change in the controller output. In this we have the
option to put some value of disturbance. Now as the value of the load or the disturbance
increases in a process, then the corresponding error between the SP and PV increases.
Hence as a result, the output response also increases and vice-versa. Also in case of
manual mode in the Simulation, when the controller output is made equal to zero, then
the value of PV decreases and finally reaches to zero.
Simuation mode :
Interfacing:
Selecting this option, accesses real time data from using interfacing unit. In order to
make the system stable, we have to change the values of P, I, D.
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Start:
By enabling this option, the equipment will be ready to perform the experiment.
Log:
On clicking the LOG button ON or selecting this option enables the data to be logged in
some particular file, which can be used later for continuing the experiment. In order to
view this saved data-logging file, click VIEW DATA FILE.
Off:
Selecting this option disables the data logging.
Function Generator :
The function generator is basically used to apply the dynamic waveform of some
particular period and amplitude to the process. The waveform is applied to the set point
in case of the close loop operation and is applied to the output in case of the open loop
function.
On:
This option enables the function generator selection and also enables the waveform to
be applied to the process.
Off:
Selecting this option disables the function generator so that it stops functioning.
Function generator parameter:

Single Type:
This function enables you to select one waveform out of the sine, triangular,
square and saw tooth waveform to be applied to the process.
Reference Point:
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This function is used to set the reference point equal to set point which helps in
making PV equal to the set point.
Period:
This function is basically used to provide some time period to a waveform so
that the waveform completes its one complete cycle in some particular interval of time.
Amplitude:
This function is used to set the amplitude of the waveform, which is selected to
be applied to the process.
Process:
This function is responsible for either increasing or decreasing the value of PV in
the SIMULATION mode.
Log (MIN):
It is also known as delay time and is measured in minutes. It is the amount of
time required for the response to reach 50% of the final value in first attempt. As the
value of the lag time increases, the change in the value of PV also increases.
Disturbance (%):
A disturbance is a signal that tends to adversely affect the value of the output of
a system. If a disturbance is generated within the system, it is called internal, while an
external disturbance is generated outside the system and is an input.
Initial:
This is the value of the PV when we continue the process without allowing the
process variable to reach its initial state i.e. equal to zero or its ambient temperature.
Ambient Temperature:
This is the initial value of PV, or due to the room temperature of the place
where the experiment is to be performed.
Output Range:
This corresponds to the maximum and the minimum range of the controller
output, which is to be set by the user.
Output High:
It corresponds to the maximum limit of the controller output means that the
output of the controller never exceeds this limit. This value is set by the user in order to
105
obtain the accurate result.
Output low:
It corresponds to the lowest limit of the controller output means that the output
of the controller can never be less than this value.
PID Gains:
This corresponds to the various values of the Kc, Ti and Td, which are to be
selected by the user in order to make the system stable. In other words, these values are
selected in order to make PV equal to SP.
Mode Status:
This option tells you that in which mode the system is operating i.e. whether the
system is operating in P, PI or PID.
P:
This option tells you that the system is operating in proportional controller
mode. P represents the proportional gain. In order to get the steady operation when the
disturbances are absent, the controlled variable must be a continuous function of error.
With proportional control, the controller output is a linear function of the error signal.
PD:
This option indicates that the system is operating in Proportional + Derivative
controller mode.
PID: This option indicates that the system is operating in proportional + Integral +
Derivative controller
BIAS: Bias is the value of the normal output of the controller at zero error. This is
added to the proportional controller.
Thus, when a process is under P only control and the SP equals the measurement (when
error equals zero), some bias value of the controller output must exist or the measured
PV will drift from the set point. This bias value of the controller output is determined
from the design flow of operation of the process to be controlled. Specifically, bias is
the value of the controller output, which in open loop causes the measured PV to
maintain steady state at the design flow of the operation when the process disturbances
are at their design.
Action: There are mainly two actions for controlling the process variable and controller
output. These actions are:
1) INC-INC
2) INC-DEC
Using INC-INC action will cause increase in output with the corresponding increase in
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process variable. Using INC-DEC action will cause decrease in controller output with
increase in process variable. This action should be observed by the user, which will
further depend on the final control element functioning.
For example: Consider a case of pneumatic actuator, which is open for air and
otherwise closed which means that the actuator valve is open for 15 psi pressure and
close for 3 psi pressure. So, the final control element sets INC-INC action or INC-DEC
action.
Switching between auto and manual:

Therere two different modes option in this software i.e. Auto and Manual. In case of
auto mode, the software automatically controls the output of the process. In this case,
user doesnt do anything to control the output of the process. So, if the output is
increasing with increase in the value of the Kc, the controller automatically decreases its
output in order to make it stable. But in case of manual control, the user controls the
output of the process. Click AUTO to select the AUTO mode and Click again to change
the system to manual mode.
Exit: This option enables you to logout of the simulation or interfacing mode.
View Data File:
This option accesses data from the data stored in the stored file using LOG
button. Results and data of the experiment conducted are observed .The user can see the
data stored in the file in the form of tables as well as graphs. After enabling this option,
user enters into a window where user has to open the file in which he has stored his/her
data while performing the experiment using the LOG button and this shows the data in
the form of table which indicates date and time i.e. which indicates when the
experiment was performed and at what time, PV, set point, output, upper and lower
range and the limit of the upper and lower hysteresis. This window also indicates the
User i.e. the name of the institute which is performing the experiment and also the
Professor name i.e. under whose supervision the experiment is going to be performed,
Student Name and Roll Number i.e. name and roll number of the student who is
performing the experiment.
Run/ Pause:
This option enables the graph to run or pauses to show the waveform according
to the data shown the table in that window.
Print Graph:
107
Use print graph option for printing graphs according to the data that is saved in
the data log file.
Enabling this option enables you to enter into the print window, which shows the
User i.e. the name of the institute, Professors Name i.e. under whose supervision test is
to be performed, Students Name and Roll number i.e. the name and the roll number of
the student who is performing the experiment and the File path i.e. the path of the file
which was saved using the LOG button. In this window the user has two options at the
top of the window i.e. one option of Print Window, which is used to take out the
printout of the window, and the second option is of Stop, which enables the user to
come out of the window.
Print Table:
Use print table option to print table from data file that are saved in the data log file. This
option opens all the data stored using the log button in the excel file where the user has
an option to set the left, right margins of the page.
Bode Plot: To view this, switch off the start button so as to return back to the front
panel and click bode plot.
Compare Data: This option enables you to compare the data between to two
experiments having different values of P, I, D. This option also enables you to compare
data between the SIMULATION mode and INTERFACING mode.
Exit : Selecting this option allows you to return back to the desktop or logout you from
the software.
Various PID Control Methods:

1. Cohen and Coon Method(C-C):
(Referred from Process systems Analysis and Control By Donald R.Coughanowr, 2nd
edition, page no.288)
COHEN-COON METHOD
108
Block diagram of control loop for measurement of process reaction curve
Figure 5: Typical process reaction curve showing graphical construction to

determine the first order with transport lag model.
The open loop method of tuning in which the control action is removed from the
controller by placing it in manual mode and an open loop transient is induced by a step
change in the signal. This method was proposed by COHEN and COON in 1953 and is
often used as an alternative to the Z-N method. Fig shows a typical control loop in
which the control action is removed and the loop opened for the purpose of introducing
a step change (M/s). The step response is recorded at the output of the measuring
element. The step change to the valve is conveniently provided by the output from the
controller, which is in manual mode. The response of the system is called the process
reaction curve; a typical process reaction curve exhibits an s-shape as shown in
Fig. 5 . It is represented by the equation:
Kce d s
Gp =
Ts + 1
The C-C method is summarized in the following steps: 10 After the process reaches steady state at the normal temperature of operation, switch
the controller to manual. In modern controller, the controller output will remain at the
same value after switching as it had before switching.
11. With the controller in manual, introduce a small step change in the controller output
and record the transient, which is the process reaction curve.
12. Draw a straight line tangent to the curve at the point of inflection, as shown in
fig..The intersection of the tangent line with the time axis is the apparent transport lag
109
(d); the apparent first order time constant (T) is obtained from
T=Bu/S ------------------------------ (8)
where Bu is the ultimate value of B at large t and S is the slope of the tangent line. The
steady state gain that relates B to M in fig is given by
Kp=Bu/M ----------------------------- (9)
13) Using the values of Kp, T and d from step 3, the controller settings are found from
the relations as given below:
Type of control
Parameter setting
Proportional (P)
Kc =
1 T
1+ d
Kp d
3T
Proportional-Integral (PI)
Kc =
1 T 9
+ d
K p d 10 12T
Ti =
Proportional Derivative (PD)
Kc =
Td =
Proportional-integral-derivative (PID)
Kc =
Ti =
Td =
20
30 +
d
9+
T
T
1 T 5
+ d
K p d 4 6T
6
d
22 +
d
d
T
T
1 T 4
+ d
K p d 3 4T
32 +
13 +
4
2
11 +
T
T
2. Zieglers Nicolas Methods :

(Referred from Modern Control Engineering By Katsuhiko Ogata)
According to Zeigler Nichol, PID controllers can be classified into two
categories: 1) A controller in which the dynamic model of the plant is not known.
110
2) A controller in which the dynamic model of the plant is known.

Zigler-nichols method
Unit step response of plant
Fig: 6
S shaped response curve
First method:
In this method, we obtain experimentally the response of the plant to a unit step
input. If the plant involves neither integrator nor dominant complex conjugate poles,
then such a unit step response curve may look S-shaped. This method applies if the
response to a step input exhibits an S-shaped curve. Such step response curves may be
generated experimentally or from a dynamic simulation of the plant.
The S-shaped curve may be characterized by two constants, delay time L and
time constant T, which is shown in fig. 6 constant are determined by drawing a tangent
line at the inflection point of the S-shaped curve and determining the intersections of
the tangent line with the time axis and line C (t)=K, as shown in the figure.
The transfer function C(s)/U(s) may then be approximated by first order system
with a transport lag as follows: -
111
Zeigler and Nichols suggested to set the values of Kp, Ti and Td according to the
formula shown in below table.
Notice that the PID controller tuned by the first order method of Zeigler- Nichols rules
gives:
1
T
1
+ Td s) = 1.2 (1 +
+ 0.5Ls )
Ti s
L
2 Ls
Thus the PID controller has the pole at the origin and double zeros at S=-1/L.
Gc ( S ) = K c (1 +
Second Method:
It is shown in fig. 7. In the second method, we first set Ti=infinity and Td=0.
Using the proportional control action only, increase Kc from 0 to critical value Kcr at
which the output first exhibits sustained oscillations, (If the output doesnt exhibit
sustained oscillations for whatever value Kp may take, then this method doesnt apply).
Thus, the critical gain Kcr and the corresponding period Pcr are experimentally
determined. Zeigler and Nichols suggested that we set the values of the parameters Kc,
Ti and Td according to the formula shown in the table
Notice that the PID controller tuned by the second method of Zeigler-Nichols
rules gives: Thus the PID controller has the pole at the origin and double zero at
s=- 4/Pcr
Gc ( S ) = K c (1 +
= 0.6 K cr (1 +
1
+ Td s )
Ti s
1
+ 0.125Pcr s )
0.5 Pcr s
112
Note that if the system has a known mathematical model (such as transfer function),
then we can use the root locus method to find the critical gain Kcr and the frequency of
the sustained oscillations Wcr, where 2*/Wcr=Pcr. These values can be found from the
crossing points of the root locus branches with the j axis. (Obviously, if the root locus
branches do not cross the j axis, this method doesnt apply).
Comments:
Zeigler-Nichols tuning rules (other tuning rules presented in the literature) have been
widely used to tune PID controllers in process control system where the plant dynamics
are not precisely known. Over many tears, such tuning rules proved to be very useful.
Zeigler Nichols tuning rules can, of course, be applied to plants whose dynamics are
known. (If the plant dynamics are known, many analytical and graphical approaches to
the design of the PID controllers are available, in addition to the Zeigler-Nichols tuning
rules).
3. Quarter Decay Ratio Method:

The following controller tuning procedures are based on the work of Zeigler and
Nichols, the developers of the Quarter Decay ratio-tuning techniques derived derived
from a combination of theory and empirical observations.
113
Close Loop (Ultimate Tuning) Tuning Procedure:

Although the closed loop tuning procedure is very accurate, you must put your
process in steady state oscillation and observe the PV on a strip chart. Complete the
following steps to perform the closed loop tuning procedure.
1) Set both the derivative time and integral time on your PID controller to zero.
2) With the controller in automatic mode, carefully increase the proportional gain
(Kc) in small increments. Make a small change in SP to disturb the loop after
each increment. As you increase Kc, the value of the PV should begin to
oscillate. Keep making changes until the oscillation is sustained, neither growing
nor decaying overtime.
3) Record the controller proportional band (PBu) as a percent, where PBu=100/Kc.
4) Record the period of oscillation (Tu) in minutes.
5) Multiply the measured values by the factors shown in the below table and enter
the new tuning parameters into your controller. This table provides the proper
values for a quarter decay ratio.
If you want less overshoot, increase the gain Kc.
Figure Output and PV step change.
Open Loop (Step Testing) Tuning Procedure:

The open loop tuning procedure assumes that you can model any process as a first order lag
and a pure dead time. This method requires more analysis than the closed loop tuning procedure, but
your process doesnt need to reach sustained oscillation. Therefore, the open loop tuning procedure
might be quicker and the PV on a strip chart that shows time on the X-axis. Complete the following
114
steps to perform the open loop tuning procedure.
1.
Put the controller in manual mode, set the output to a nominal operating value and
allow the PV to settle completely. Record the PV and output values.
2.
Make a step change in the output. Record the new output values.
3.
Wait for the PV to settle. From the chart, determine the values as derived from the
sample displayed in the given figure.
4.
Multiply the measured values by the factors shown in fig (a) and enter the new
tuning parameters into your controller. The table provides the proper values for a
quarter decay ratio. If you want less overshoot, reduce the gain, Kc.
Various Stability Methods:

1. Bode Plot:
(Referred from Process Control By Peter Harriot, Page no. 91)
A convenient method of presenting the response data at various frequencies is to
use a log log plot for the amplitude ratios, accompanied by a semi log plot for the
phase angles. Such plots are called Bode diagrams, after H.W Bode, who did basic
work on the theory of feedback amplifiers. By using wT as a parameter, a general plot
for first order system is obtained. Since the amplitude ratio approaches 1.0 at low
frequencies and 1/wT at high frequencies, the straight line portion of the response if
extended would intersect at wT = 1.0. The frequency corresponding to the wT = 1 is
called the corner frequency and the amplitude ratio is 0.707 at this point. The phase
lag is 45 degree at the corner frequency and the phase curve is symmetrical about this
point.
The system shown in fig. 6 has a gain of 1, which means that the output equals
the input as the frequency approaches zero. If the system gain K is greater than 1, the
output amplitude is greater than the input amplitude at low frequencies and a more
comprehensive definition of amplitude ratio is needed. The amplitude ratio is defined as
the ratio of output amplitude to input amplitude at a given frequency, divided by the
ratio of the amplitudes at zero frequency. This is equivalent to dividing the measured
ratio by B/A by the gain K, which makes the amplitude ratio dimensionless and makes
equation and curves applicable to the first order process.
115
Sometimes, the amplitude ratio is defined just as B/A, or output over input,
which leads to amplitude ratios, which may not be dimensionless. There is nothing
unsound about this procedure but the use of different units for each process element
makes it somewhat harder to plot the overall response of the system.
Whenever a sinusoidal input is applied to a linear system, the output has steady
state and transient terms. After a few cycles, the transient dies out and the output is a
sine wave of the same frequency. This eventual response can be characterized by the
amplitude ratio and the phase angle. Typical curves for a first order process are shown
below. At low frequency, the output is almost equal to the input, and there is only a
slight phase lag. At high frequency, the fluctuations in the input are severely damped
because of the capacity in the system and the output lags the input by almost 90
degree.
The phase angle is always negative for a first order system and the negative
angle is called phase lag. The phase lag is 360(dt/p) in fig. And approaches a limit of
90 degree at high frequencies.
2. Rouths Algorithm Method:

(Referred from Problems and Systems of control systems By A.K. Jairath, 3rd edition,
page no. 6.1)
The Routh test is a purely algebraic method for determining how many roots of
the characteristics equation have positive real parts; from this it can also be determined
whether the system is stable, for if there are no roots with positive real parts, the system
is stable. The test is limited to the systems that have polynomial characteristic
equations.
As per Rouths stability criterion the necessary conditions for a system to be stable are:
1) None of the co-efficient of the characteristics equations should be missing or
zero.
2) All co-efficient should be real and should have same sign.
The sufficient condition for a system to be stable is that each and each term of
the first column of Rouths array should be positive and should have same sign.
Rouths array for the characteristic equation
A0 s n + A1s n 1 + A2 s n 2 +
An 1s + An = 0
(11)
The Routh array for the case when n=7 is shown below:
116
If we study the array successive rows have one term fewer than the preceding
row, and hence the array is triangular. The following are the limitations of the rouths
stability criterion:
It is valid only if the characteristic equation is algebraic.
1) If any co-efficient of the characteristic equation is complex or contain power of
e, this criterion cant be applied.
2) It gives us information as to how many roots are lying in the right hand side of
the s-plane. Values of the roots are not available. Also, it cannot distinguish
between real and complex roots.
Conducting Experiments:
Description:
This section gives the functional details of the product, which is used to conduct the
experiment. Functional details and control loop description enables us to understand the
working principle of the product.
FLOW CONTROL TRAINER (SCADA):

The SCADA is basically an interfacing unit and is a medium for communicating with the
equipment from the computer. In case of flow controller, the flow of the liquid is sensed by the
sensor in the pipe line, which is further transmitted into 4-20 mA which means that the current
117
is 4mA for 0% flow and 20mA for 100% flow and are displayed on the interfacing unit in terms
of 0 to 100%. These signals are further transmitted to the computer through this interfacing unit
by using a RS-232C where the signals are displayed on the computer screen and the error
signals, which are produced by the controller, are displayed on the interfacing unit. The output
of the interfacing unit is then transmitted to the I/P converter, which converts it into 3 to 15 psi
that means 3 psi for 4mA and 15 psi for 20mA.
Start Up:
1.
Drain should be closed.
2.
Fill the sump tank with 3/4 of water and avoid the presence of foreign particles.
3.
Switch on the main supply.
4.
Switch on the pump and observe that the water is properly circulating.
5.
Check whether all the valves are properly working or not.
6.
Switch on computer and the interfacing unit.
7.
Select the Auto mode to perform the experiment automatically and in Manual mode
th
to change the values manually.

8.
Connect the equipment with compressed air supply of minimum 3 bar.
Shut down
1.
Exit from the software
2.
Switch off the inter facing unit
3.
Switch off thre pump and air supply
4.
Clean the tank.
Following experiments can be conducted with the product.

Exp 1.
To study the open loop or manual control.
Exp 2
To study the Proportional control.
Exp 3
To study the Two mode (P+I) control.
Exp 4
To study the Two mode (P+D) control.
Exp 5
To study the Three mode (PID) control.
Exp 6
To study the tuning of controller (Open loop method) using
Zeigler-Nichols method.
Exp 7
To study the stability of the system using the BODE PLOT.
118
Experiment No.1
Open Loop (Manual) Control
Objective: To study the open loop or manual control.
Theory:
In these systems, the output remains constant for a constant input signal provided
the external; conditions remain unaltered. The output may be changed to any desired
value by appropriately changing the input signal but variations in external or internal
parameters of the system may cause the output to vary from the desired value in an
uncontrolled fashion. The open loop control is, therefore, satisfactory only if such
fluctuations can be tolerated or system components are designed and constructed so as
to limit parameter variations and environmental conditions as well as controlled,
whereas in case of closed loop system, the controlled variable is measured and
compared with reference input and the difference is used to control the elements.
1.
2.
3.
4.
5.
6.
Start up the setup as mentioned in the starting.

Select the manual mode.
Set the controller output to 100%.
Apply a step change of 10% to the controller output and wait for the PV to reach
the steady state.
Repeat the above steps i.e. 2 and 3 until the output of the controller reaches to
0% temperature
Shut down the apparatus as mentioned in the starting.
Observation & Calculations:

S.No Controller output (%)
PV (%)
1.
100
2.
90
3.
80
4.
70
5.
60
6.
50
7.
40
8.
30
9.
20
10
10
Set the output of the controller to some predicted value and apply some steady state
load change and then verify the result.
119
Experiment No. 2
Proportional Control
Objective:
To study the proportional control (P control).
Theory:
In order to get steady operation when the disturbances are absent, the controlled
variable must be a continuous function of error. With proportional control, the most
widely used type; the controller output is a linear function of the error signal. The
controller gain is the fractional change in output divided by the fractional change in
input.
P = Kc * e
Where,
P= fractional change in controller output
E= SP-PV= fractional change in error.
Kc = controller gain
Whereas the equation of the proportional controller out put is given by
P = Kc (SP PV) + P0
Wher P0= bais i.e. the value of the controller output at zero error.
In this experiment, the measured process value (PV) and set point (SP) is compared And the
output of the controller is proportional to the resulting error signals
1. Start up the set up as mentioned previously.
2. Select the controller in AUTO mode.
3. Set the value of Kc as high as possible.
4. Observe the process and the output response.
5. If output response doesnt shows cycling, adjust the value of Kc to half of its
previous value.
6. Repeat steps 4 and 5 until cycling is observed.
7. Then, increase the value of Kc to twice its value and observe the Output
response.
8. Repeat step 7 until cycling is observed.
9. Record the value of Kc at which you observe the oscillations and record
120
the overshoot.
10. Now increase the value of Kc in steps and observe the corresponding overshoots.
11. Compare the relative overshoot with the value of Kc.
Observation and calculations:

1.
Observe that as the value of Kc increases, then the error or the difference
between the SP and PV increases. In other words, as the error decreases, the
proportional band decreases.
2.
In case of proportional controller, the control system is able to arrest the rise of
the controlled variable and ultimately bring it to rest at a new steady state value.
The difference between this new steady state value and the original value is
called OFFSET. There is always some offset present in case of proportional
controller.
121
Experiment No. 3
Two Mode (P+I) Control
Objective:
To study the steady state and transient response to a proportional + Integral control.
Theory:
This mode of control is described by the relationship:
P = Kce +
Kc
edt + PS
Ti
Where ;
Kc
=
gain
error = (SP-PV)
Ti
Ps
constant
output
integraltime, seconds
In this case, we have added to the proportional action term, Kc * e, another term that
is proportional to the integral of the error.
There is no offset with the integral control, since the output keeps changing as long as
any error persists. However, the initial response to an error is slow and proportional
control is ordinarily used with integral control. The integral action corrects for the offset
that usually occurs with proportional control only, and the effect is similar to manual
adjustment or resetting of the set point after each load change. The terms reset action
and reset time are widely used to characterize the integral action of a proportional
integral controller.
P = K c (e +
1
edt ) + Ps
Ti
where
Kc
gain
error = (SP-PV)
Ti
integral time.
A small reset time corresponds to an increase in the integral action. With P action the
measured value will not necessarily become equal to the set point and a deviation will
usually be present. The control algorithm that applies changes in output as long as
deviation exits, as to bring the deviation to zero is called integral action. With integral
122
action the parameters that determines how fast the output will change in corresponding
to some amount.
1. Start up the setup as mentioned previously.
2. Select auto mode option for control.
3. Select a set point.
4. Select some value of Kc as described in proportional controller and Ti as high as
possible.
5. Observe the response of the system. If over damped oscillations are occurring, then
increase or decrease the corresponding values of Kc or Ti so as to make PV equal to
SP.
6. Then, observe the output response curve. If on decreasing the value of either Ti or
Kc makes the PV equal to SP, then continue decreasing the value until PV becomes
nearly equal to SP.
7. After experimentation, switch off the apparatus as mentioned previously.
Observation & Calculations:

1.
The addition of integral action nearly eliminates the offset and the controlled
variable Ultimately returns to the original value.
2.
It is shown the fig., that the addition of integral action introduces an oscillatory
motion in the system and with the increase in the value of the integral time, the
difference between the SP and PV decreases
123
Experiments No. 4
Two Mode (P+D) Control
Objective:
To study steady state and transient response to a proportional + derivative control.
Theory:
This mode of control may be represented by:
P = Kc* e + Kc Td de/dt -------------- 16
Where Kc = gain
Td = derivative time, seconds
In this case, we have added to the proportional term another term, KcTd (de/dt) that
is proportional to the derivative of the error. Other terms that are used to describe the
derivative action are rate control and anticipatory control.
Derivative action is often added to proportional control to improve the response of slow
systems. By increasing the output when the error is changing rapidly, derivative action
anticipates the effect of large load changes and reduces the maximum error.
Larger the derivative time larger is the action. Smaller is the proportional band the larger is
the derivative action.
1. Start up the setup as mentioned previously.
2. Select auto mode option for control.
3. Select a set point.
4. Select some value of Kc as described in the proportional controller and the value of
Td to the minimum value.
5. Observe the response of the system. If over damped oscillations are occurring, then
reduce the value of Td to half of its previous value so as to make PV equal to SP.
6. Then, observe the output response curve and double the value of Td in order to make PV
equal to SP, then continue decreasing the value until PV becomes equal to SP.
7. After experimentation, switch off the apparatus as mentioned previously.
Observation &Calculations:
1. The derivative action is added to improve the response of the slow system.
2. The addition of derivative action to the PI action gives a definite improvement in the
response. The rise of controlled variable is arrested more quickly and it is returned
rapidly to the original value with little or no oscillations.
124
Experiments No. 5
Three Mode (PID) Control
Objective:
To study the steady state and transient response to a Proportional + Integral +
Derivative.
Theory:
P = Kce +
Kc
de
edt + K cTd
+ Ps
Ti
dt
Where:
e
= error
Kc
= gain = (SP-PV)
Td is derivative time, Ti is integral time and Kc=proportional gain
1.
Start up the setup as mentioned earlier.
2.
Select auto mode option for control.
3.
Select a set point.
4.
Select some value of Kc, Ti and Td.
5.
Observe the response of the system. If over damped oscillations are occurring, then
increase or decrease the corresponding values of Kc, Ti and Td so as to make PV
equal to SP.
6.
Then, observe the output response curve. If on decreasing the value of either Kc, Ti,
Td makes the PV equal to SP, then continue decreasing the value until PV becomes
equal to SP.
7.
After experimentation, switch off the apparatus
8.
Using trail and error, select the proportional gain and integral time, which gives a
satisfactory response to step change in set point.
9.
Set the derivative time to a non-zero value and carry out the above steps for different
derivative time values.
10. After experimentation shut down the setup as mentioned earlier.
The addition of derivative action to the PI action gives a definite improvement in the
response. The rise of controlled variable is arrested more quickly and it is returned rapidly
to the original value with little or no oscillations.
125
PV
Tt
PV
Tt
126
Experiment No.6
Tuning of controller (open loop method)
Objective:
To study the tuning of PID controller by open loop method, using Zeigler- Nichols
tuning rules.
Theory:
This method is basically used to calculate the value of P, I, D using the open loop
or manual control method. The values of P, I, D are selected in such a way that the error or
the difference between the SP and PV should become equal to zero.
Fig: 7
S shaped Response Curve
Since we are not given with the plant equation. So the process is assumed to be of
first order with steady state gain Kc, integral time Ti and derivative time td. The step
response i.e. process reaction curve, allows to obtain the approximate values of each
parameter. With the feedback loop open, a step response is applied to manipulated variable
and the values of P, I and D are estimated.
The delay time L and time constant T are determined by drawing a tangent line at the
inflection point of a S-shaped curve and determining the intersections of the tangent line with the
time axis and line c (t) = K as shown in the figure obtained by performing the experiment
127
1.
Start up the set up as mentioned.
2.
Select open loop option for control.
3.
Select the value of the set point to some desired value.
4.
Apply a 20-30% change to controller output. Record the step response. Wait for
the steady state.
5.
Start data logging and from the readings draw a step response curve.
6.
Calculate the value of Td and L.
7.
From this, calculate the values of PID controller settings from the table.
8.
After experimentation, shut down the set up.
Tabulate the data from stored file as follows:
Observation no.
1.
2.
3.
4.
Time in second
Process value
Calculate the value of the P, I and D from the table given in the theory part of this experiment.
128
Experiment No.7
To Study the Stability of a System
Objective:
To study the stability of the system by plotting the bode plots.
Theory:
A convenient method of presenting the response of the data at various frequencies
is to use a log-log plot for the amplitude ratios, accompanied by the semi log plot for the
phase angles. Such plots are called BODE PLOT. Plotting of BODE plot is relatively
easier as compared to other methods as the loci of (1 + sT) and K/(1 + sT) can be
represented by straight line asymptotes.
In case of Bode plot, multiplication is converted into addition,
so if G(s) = K/(1 + sT)
And putting s = jw,
Then 20 log [G (w)] = 20 log K 20 log [1 + jwt].
In case of Bode plot, study of relative stability is easier as parameters of analysis of
relative stability are gain and phase margin, which are visibly seen on the sketch.
The transfer function for a first order system is given by
ke Ls
G(S ) =
Ts + 1
The amplitude ratio of the above equation can be written as
The phase angle is always negative for a first order system and this negative angle is
called phase lag.
Stability Criteria:
1. A system is stable if the phase lag is less than 180 degree at the frequency for
which the gain is unity.
2. A system is stable if the gain is less than unity at the frequency for which the phase
lag is 180.
1. Rewrite the sinusoidal transfer function in the time constant form.
2. Identify the corner frequencies associated with each factor of the transfer function.
3. Knowing the corner frequency, draw the asymptotic magnitude plot. This plot
consists of a straight line segments with the line slope changing at each corner
129
frequency by +20 db/decade for a zero and 20 db/decade for a pole For a complex
conjugate zero or pole the slope changes by +/- 40 db/decade.
4. Draw a smooth curve through the corrected point such that it is asymptotic to the
straight-line segments. This gives the actual log-magnitude plot.
5. Draw the phase angle curve for each factor and add them algebraically to get the
phase plot.
6. The ultimate gain value i.e. Wco is that value when the phase angle curve crosses the 180
degree line and the corresponding gain value is called the ultimate gain i.e. Ku.
7. By using these two gains the other parameters that are the values of P, I, and D are
calculated from the table given in the theory part of zeiglers closed loop method.
Draw the graphs of Magnitude Vs frequency on log-log scale.
Draw the graphs of Phase angle Vs frequency on semi log co-ordinates.
Compare the values calculated from Zeigler open loop and this Bode plot.
The first order system will be stable only if the phase angle Vs frequency graph has
negative phase lag.
130
131


INTERACTING AND NON-INTERACTING TANK SYSTEM
1. Objective:
To study the dynamic response of liquid level in Single Tank, Two Tank
Interacting and Two Tank Non-Interacting System.
2. Introduction:
The principle distinction to be made in multi-capacity processes is in how the
capacities are joined. If they are said to be isolated or non-interacting, the
capacities behave exactly as they would alone. But if coupled, they interact with
one another, in which case the contribution of each is altered by the interaction. In
non-interacting system the two tanks levels do not interact because the flow from
the first tank to the second tank is independent of the level in the second tank. In
interacting system the levels in both tanks interact because any change in the down
stream level will affect the upstream level.
The following general rules are applied to the principle of interaction;
1. The degree of interaction is proportional to the ratio of the smaller to the larger
capacity (not time constant). Where this ratio is low (<0.1), the capacities may
assumed not to interact .
2. Interaction always works towards increasing the larger time constant and
decreasing the smaller one.
3. Specifically with regard to the behavior of the system with equal time constant
and of equal capacity, the effect is a combination of one large and the rest smaller
time constants.
3.
Description:
Present set-up is specially designed for studying the dynamic response of Liquid
Level in Single Tank, Two Tank Interacting and Two Tank Non-Interacting
System. Apparatus is self-contained re-circulating unit. Water from Sump Tank is
132
sucked and delivered to a Constant Level Overhead Tank by means of a

Centrifugal Pump. Flow rate of water is controlled and metered with the help of
given Rotameter. Apparatus can be operated for any of the desired modes viz.:
Single Tank System, Non-interacting System or Interacting System by operating
the valves.
Water, passing through Rotameter, can be allowed to enter first in Process Tank-1
or Process Tank-2 by fixing the valve position provided for this purpose. To run
the apparatus in Single Tank System mode, the water will be allowed to enter in
Process Tank-1.The drain of Process Tank-1 is supplied to Process Tank-2 with
provided valve and then drained back to Sump Tank. Resistance will be fixed for
the drain valve of Process Tank-1 and reading will be noted as briefed further in
the this Manual.
For conducting the experiment on Two Tank Non-Interacting System, the
apparatus will be operated in the same mode as Single Tank System, but resistance
will be produced at drain of both Process Tank-1 and Process Tank-2. Reading will
be noted down as per Manual instruction.
When the system will be operated Two Tank Interacting mode, the water will be
allowed to enter in Process Tank-2 and drain valve will be fixed in close position.
Water form Process Tank-2 will be allowed to Process Tank-3 from the bottom by
opening a valve. Resistance of this valve and drain valve of Process Tank-3 will be
fixed and reading will be noted as per the instruction of this Manual.
1. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 amp socket with earth
connection.
2. Water Supply (Initial Fill)
3. Drain Required
4. Floor Area Required: 1 m x 1 m.
5.
Precaution & Maintenance Instructions:

1. Never run the apparatus if power supply is less than 180 volts & above than
230 volts.
2. Always keep apparatus free from dust.
133
3. To prevent clogging of moving parts, Run Pump at least once in a fortnight.

4. Always use clean water.
5. It apparatus will not in use for more than one month, drain the apparatus
completely.
6.
Troubleshooting:
If pump gets jam, open the back cover of pump and rotate the shaft manually.
If pump gets heat up, switch off the main power for 15 minutes and avoid
closing the flow control valve and by pass valve simultaneously.
134
EXPERIMENT NO. 1
SINGLE TANK LIQUID LEVEL SYSTEM
1.
Aim:
To obtain the step response of a single tank liquid level system to a step change in
input flow and to compare it with the theoretical response.
To determine the time constant of the system from the step response curve in a
single tank liquid level system.
2.
Theory:
A single tank liquid level system is first order in nature. The transfer function relating
deviation of liquid level in the tank to the deviation in the inlet flow rate is:
where = AR is the time constant of the system.

For step input of the magnitude M in the inlet flow to the tank :
Taking inverse Laplace transform of equation (2)
This equation gives the theoretical variation of liquid level in the tank with
respect to time for a step input of magnitude M in the inlet flow rate.
The experimental value of is obtained from the step response curve in which
63.2% of the step response will be completed within a time equal to to one time
constant. A liquid level system is non-linear in nature.
The discharge from the vessel is proportional to the liquid level in the vessel.
where C is a constant.
135
In the linear region of the operation the above equation becomes qo = h/R
where R is the resistance of the discharge valve. The resistance R is the
reciprocal of slope of the tangent line to head (h) vs discharge (Q)curve at the
first steady state value.
3.
1. The liquid level in vessel is maintained at a steady state value around the lower
middle part of the level gauge by properly adjusting the inlet and outlet flow rates.
2. At the steady state condition note the level hs and discharge qs.
3. Now a step change in input flow is introduced by opening the cock valve at the
bypass of inlet valve.
4. Simultaneously start a stopwatch and note the rise in the level with time till the
level reaches a new steady state value.
5. At new steady state, note the level and outlet flow rate. The difference between the
initial and final flow rates gives the magnitude of step input M
To Determine the Resistance of the Valve:
1. The final steady state level and the discharge of the system in the above
experiment are noted.
2. Now the inlet flow to the vessel is decreased by a small amount and allows the
system to come to a new steady state value.
3. The experiment is repeated for different steady state value noting the level and
discharge each time.
4. A plot of discharge vs. head is drowned from which the resistance of the valve can
be obtained.
4.
D = 0.108 m
Observation Table:
t, min
h, m
h S, m
qS, LPH
qfs, LPH
Plot a graph between qS vs. hS to determine the Resistance (R) of the valve
136
Calculations:
5.
Nomenclature:
Cross-sectional area of process tank, m2
Inner diameter of tank, m
Subscript of final state
Height of liquid in process tank, m
hs
Initial Height of liquid in process tank , m
Change in height (h hS) in process tank after step Change, m
Magnitude of step change, m3/min
qfs
Final steady state feed flow rate, m3/min
qs
Initial flow rate for the process, m3/min.
Resistance given to the valve
Subscript of steady state
6.
References:
1.
Donald R. Coughanowr, Process System Analysis and Control, 2nd
Time constant, min
ed., McGraw Hill, NY, 1991, Page 64-67.
137
EXPERIMENT NO. 2
TWO TANK INTERACTING LIQUID-LEVEL SYSTEM
1.
Aim:
To obtain experimentally the step response and to compare the experimental
and theoretical responses.
2. Theory:
A dynamic system is the one in which there is some varying amount of
accumulation of conserved quantities with time. Consider a liquid level system
shown below in which two tanks are arranged in series such that the response of
first tank depends on the conditions in the second tank. Such a system is said to be
an interacting system and is a lumped parameter system.
This arrangement is such that the flow through the resistance R1 depends on both h1 and
h2. Such a system is known as interacting system. Selecting a macroscopic system
consisting of the entire tank, the total transient material balance for Tank 1 is:
138
d (h2
h2 s )
dt
h1 h1s
A2 R1
In terms of deviation variables

dH 1
A1
= Q Q1
dt
A2
dH 2
= Q1
dt
Q2
h2 h2 s
A2 R2
(5)
( 6)
139
Q1 =
Q2 =
H1
H2
(7)
R1
H2
R2
(8)
where
Q=q
H1 = h1
qs , Q1 = q1
q1s , Q2 = q2
h1s , and H 2 = h2
q2 s
h2 s
Taking the transform of equations (5) to (8)

Q( s) Q1 ( s) = A1 sH1 ( s )
(9)
Q1 ( s) Q2 ( s) = A2 sH 2 ( s)
(10)
R1Q1 ( s) = H 1 ( s) H 2 ( s)
(11)
R 2 Q2 ( s ) = H 2 ( s )
Combine these equations to eliminate Q1, Q2, H1
(12)
This equation represents the theoretical response of the system in terms of variation of
liquid level in tank 2 with respect to time for a step input of magnitude M in the inlet
flow of tank 1. There are two ways of solving Eq (15).
1. First obtain the time constant 1 & 2 of each tank (adjust the resistances R1 and R2
such that 1 = 2 = ) . The response in terms of H2 (t) can be obtained from Eq. 15
and compared with the observed response.
2. The observed response, H2 (t) vs t data can be fitted to Eq. 15 and and R2
obtained by nonlinear regression techniques. Compare the values of and R2 with
the observed values of & R2.Discrepancy in the response or in values of time
140
constant should be accounted for. One of the principal reasons for discrepancy
could be the assumption of linear resistance R1 & R2 that may not be valid.
1. Adjust valves V1& V2 (partially open).
2. Switch on the power supply and the pump; adjust the inlet flow rate, q, to the
Tank-1 at around 40 LPH by completely opening the feed valve, Vf and adjusting
the flow by the control valve of the rotameter.
3. The liquid level in the two tanks will rise. Wait till steady state is reached in each
tank.
4. Note the steady state liquid level (h1s and h2s) and the inlet steady state flow rate
(qs).
5. Now increase the inlet flow rate to tank one to say 50 LPH by suddenly opening
the rotameter needle valve in a single go and maintain the flow rate at this
level . Simultaneously start the stopwatch and record the liquid level with time in
each tank (h, h2) till next steady state is reached. Note down the final steady
state value of h1, h2 and qfs .
6. Steps (3) to (5) can be repeated for another step change in feed flow rate without
changing the valve positions V1 & V2.
7. From the steady state values of qf (s), h1(s) and h2(s) obtain the values of 1 and
2 and adjust R1 and R2 such that 1 = 2 = .
4. Observation &Calculations:
141
Plot steady state discharges qf(s) vs level h2(s).
5.
Nomenclature:
A
Cross-sectional area of process tank (1), tank (2), m2
D1
Inner diameter of Tank (1) & Tank (2), m
D2
Outer diameter of down comer, m
h1
Height of liquid in process tank (1) after step change attaining steady
142
state, m
h2
state, m
6.
H1s
Change in height (h1fs - h1S) in process tank (1) after step change
H2s
Change in height (h2fs h2s) in process tank (2) after step change
h1s
Initial height in the process tank (1)
h2s
h1fs
Final height in the process tank (1)
h2fs
qfs
Final steady state feed flow rate, LPH
qS
Initial steady state feed flow rate, LPH
QS
Initial flow rate for the process, m3/min
R1
Resistance given to the valve (1), min/m2
R2
Time constant, min
References:
Donald R. Coughanowr, Process System Analysis and Control, 2
nd
ed., McGraw Hill,
NY, 1991, Page 83-86.
143
EXPERIMENT NO. 3
TWO TANK NON- INTERACTING LIQUID-LEVEL SYSTEM
1.
Aim:
To obtain experimentally the step response and to compare the experimental &
theoretical responses.
2. Theory:
A dynamic system is the one in which there is some varying amount of accumulation of
conserved quantities with time. Consider a liquid level system shown below in which
two tanks are arranged in series such that the response of first tank does not depend on
the conditions in the second tank. Such a system is said to be a non- interacting system
and is a lumped parameter system.
Tank 1 =A1
Tank 2= A2
This arrangement is such that the flow through the resistance R1 depends only on h1.
Such a system is known as a non- interacting system.
A mass balance on Tank 1 gives :
dh1
(1)
dt
A mass balance on Tank 2 gives :
dh
q1 q2 = A2 2
(2)
dt
The flow-head relationships for linear resistances are given by
q q1 = A1
144
q1 =
h1
R1
(3)
q2 =
h2
R2
(4)
Combining eqns (1) and (3) and using deviation variables
Q1 ( s)
=
Q( s )
where Q1 = q1
1
1s + 1
q1s , Q = q q s , and
(5)
= R1 A1
Similarly combining eqs.(2) and (4)
H 2 ( s)
R2
=
(6)
Q1 ( s)
2s +1
where H2=h2-h2s and 2=A2R2
From eqns.(5) and (6)
H 2 ( s)
R2
=
(7)
Q( s) ( 1 s + 1)( 2 s + 1)
On taking the inverse Laplace transform, we obtain the theoretical response of the system as:
H 2 (t ) = MR2 1
1 2
1
t/
t/
(8)
In case 1 = 2 =, then
H 2 (t ) = MR2 1 e
t/
t/
(9)
Equation (8) represents the theoretical response of a non-interacting two tank liquid level
system to a step change of magnitude (M) in the feed rate to tank (1).
There are two ways of solving Eq (8).
1. First obtain the time constant 1 & 2 of each tank and the resistance R2 (2= A2R2), the
response in terms of H2(t) can be obtained from Eq. 8 and compared with the experimental
response.
2. The observed response, H2(t) vs t data can be fitted to Eq. 8 and 1, 2 and R2 evaluated by
non linear regression techniques. Compare the values of 1, 2 and R2 with the
observed values of 1, 2 & R2.
Discrepancy in the response or in values of time constants should be accounted for. One of the
principal reasons for discrepancy could be the assumption of linear resistance R1 & R2 that may
145
not be valid.
3.
1.
Adjust valves V1& V2 (partially open).
2.
Switch ON the power supply and the pump; adjust the inlet flow rate q, to the tank
(1) at around 40 LPH by completely opening the feed valve, Vf and adjusting the flow by
the control valve of the rotameter.
3.
The liquid level in the two tanks will rise. Wait till steady state is reached
in each tank.
4.
Note the steady state liquid level (h1s and h2s) and the inlet steady state (flow rate q(s)).
5.
Now increase the inlet flow rate to tank one to say 50 LPH by suddenly opening the
rotameter needle valve in Single go and maintain the flow rate at this level
Simultaneously start the stopwatch and record the liquid level with time in each tank (h, ,
h2) till next steady state is reached. Note down the final steady state value of h1 , h2 and q
f(s).
6.
Steps (3) to (5) can be repeated for another step change in feed flow rate without
changing the valve positions V1 & V2.
7.
From the steady state values of qf (s), h1(s) and h2(s) obtain the values of 1 and 2 and
adjust R1 and R2such that 1 = 2 = .
4.
DATA:
D1
--------
D2
---------- m
Observation:
Initial steady state value (i.e. before step change is introduced)
t
qs
=--------- LPH
h1s =
---------- m
h2s =
---------- m
Final steady state values after the step change

qfs =
--------- LPH
h1fs =
--------
h2fs =
--------
146
Observation Table:
Plot steady state discharges qf(s) vs level h2(s).
Calculations:
Theoretical response
H 2 (t )
MR2
5.
= 1
1
th
1 2
2
t/
t/
(10)
Nomenclature:
A
Cross-sectional area of process tank (1) & tank (2), m2
D1
Inner diameter of Tank (1) & Tank (2), m
D2
Outer diameter of down comer, m
h1
state, m
h2
147
state, m
H1s
Change in height (h1 - h1S) in process tank (1) after step change
H2s
Change in height (h2 h2s) in process tank (2) after step change
h1s
h2s
h1fs
h2fs
qfs
Final steady state feed flow rate, LPH
qs
Initial steady state feed flow rate, LPH
QS
Initial flow rate for the process, m3/min
R1
R2
M
S
=
=

Subscript of steady state
Time constant, min
6. Reverence:
1. Donald R. Coughanowr, Process System Analysis and Control, 2nd ed., McGraw
Hill, NY, 1991, Page 80-82.
148
149


TIME CONSTANT FOR THERMOMETER/THERMOCOUPLE
1. Objective:
To study the transient response of thermometer and to determine the time constant for
thermometer/ thermocouple.
2. Theory:
We shall develop the transfer faction of the first order system by considering the
unsteady state behavior of an ordinary mercury in-glass thermometer.
Assumptions:
1) All the resistance to heat transfer reside in the film surrounding the bulb (that is the
resistance offered by the glass and mercury )is neglected.
2) All the thermal capacity is in the mercury and at any instant the mercury assume a
uniform temperature throughout.
3) The glass wall containing the mercury does not expand or contract during the
transient response .
It is assumed that the thermometer is initially at steady state , i.e. there is no change in
the temperature with time at t =0
150
At time t=0 the thermometer will be subjected to some change in surrounding

temperature x(t)
By applying the unsteady state energy balance
Input output = Rate of Accumulation
dy
hA (x-y) 0 = mC dt .(1)
y - Thermometer temperature
x - Surrounding temperature
Equation (1) states that the rate of flow of heat through the film resistance surrounding
the bulb causes the internal energy of the mercury to increase at the same rate. The
coefficient (h) will depend on the flow rate and properties of the surrounding fluid and
the dimension of the bulb. We shall assume that h is constant.
Prior to change in x ,the thermometer is at steady state and dy/dt will be zero.
For steady state condition equation (1) can be written as
hA (xs-ys) = 0
.(2)
(t <0 )
the subscribe s indicate the steady state value.

Thermometer reads the true surrounding temperature, i.e. ys = xs
From eqns.(1) and (2) we obtain
hA [(x-xs )-(y-ys)] = mC
d(y
dt
y )
s ..(3)
If we define the deviation variable to be the difference between the variable and their
steady state values
X = (x-xs)
Y = (y-ys)
Equation (3) became
dY
hA [X-Y] = mC dt
or
[X-Y] =
dY
dt
(4)
(5)
(mC/hA= )
151
Taking a Laplace transform for the equation (5)

[X(s)-Y(s)] = sY(s) ..(6)
Rearranging above eq.
Y (s)
= 1
X ( s ) s +1
(7)
The parameter is called the time constant .

The expression on the right side of eq (7) is called the transfer function of the system .
It is the ratio of the Laplace Transform of the deviation in thermometer reading to the
Laplace Transform of deviation in the surrounding temperature.
Any physical system for which the relation between Laplace Transform of input and
output deviation variable is of the form give in equation (7) is called a first order
system . Synonym for first order system are first order lag and single exponential stage.
Step Change in first order system:

If a step change of magnitude A is introduce in the first order system the transform of
X(t) is ,
X(s)= s (8)
The transfer function which is given by the equation (7), is
Y (s)
X (s)
1
s +1
(9)
This can expanded by the partial fraction to give
A 1
y(s) = s s +1
A/ t
C1
C2
y ( s ) = ( s )( s +1/ ) = s + s +1/
Solving we get
(10)
(11)
C1= A and C2= -A
152
by taking the inverse transfer function gives the time response of Y :

Y(t) = 0
Y(t) = A(1-e-(t/))
(t <0 )
(t 0 )
Time required reaching 62.3% of steady state value is equal to the time constant.
3. Schematic Diagram :
1) Initially make sure that all the switches of the panel board is off.
2) Switch on the heater of water bath. (Make sure thermocouple is inserted in the water
bath)
3) Heat continues till water bath temperature attains 100 0C (steady state)
4) Make sure that there is ice in ice bath and measure the temp of the ice bath (O 0C
steady state)
5) Insert thermometer thermocouple in hot water bath.
6) Keep the thermometer/thermocouple till the thermometer reaches the steady state
temperatures.
7) Hold a stop watch and remove immediately thermometer from hot water bath and
insert it to ice bath.(Remember that at the time of inserting thermometer/thermocouple
in the ice bath stopwatch should be start at the same instant.)
8) Start recording time for every fall in one OC
9) Repeat the procedure from 1-8 at least three times.
153
10)
Repeat
the
procedure
from
1-8
at
least
three
times
for
the
thermometer/thermocouple initially at it lower temperature and finally insert at higher

temperature.
11) Now this record the rise in temperature with the time
For step change :

1) Make availability of the hot water bath one is at 50 oC and another is 100 oC
2) Repeat the same procedure from 1-8. (Instead of ice bathe we take water at 50 oC)
3) Repeat the procedure again initially thermometer is at it 50 oC steady steate and
insert it in 100 oC
4) Record the temperature rise with respect to time
Note:
For accurate recording of temperature change we providing computer based data recording. Which
record the temperature rise or fall with every 1 sec
5. Observation Table :
Sr. No
Time
sec
Temperature
6. Calculation:
Time required reaching 62.3% of steady state value or maximum slope of the curve
A) Heating from 12(min) OC to 100(max) OC (i.e to hot water bath)
time required to reach T= (100-34)(63/100)+34 =75.7 OC
(from graph) = 7 sec
B) Cooling from 100 to 5OC( from hot water bath)
Ti
of thermocouple = 85 OC
Tf of thermocouple = 5 OC
T = ((85-5)x63/100)+5 =53.5 OC
(from graph) = sec
154
C) Heating from 3OC to 32OC (ice to R.T.)
T= (32-3)x(63/100)+2 = 20.3 OC
= sec
D) Cooling from 32 to 15 OC( from room temp to water bath temp)
Ti
of thermocouple = 85 OC
Tf of thermocouple = 15 OC
T = ((32-15)x(63/100))+15 = 25.71OC
= sec
O
E) Heating from 32 C to 100OC (ice to R.T.)

T= (100-32)x(63/100)+32 = 78..84 OC
= sec
Thermocouple
Cooling from 50OC to 32 OC(from hot air to to RT)
Ti
of thermocouple = OC
Tf of thermocouple = OC
T=((Tf-Ti)x(63/100))+15 = 25.71OC
= sec
H > C
Time constant for cooling is lesser than the time constant of heating because of the
density differences between the fluids.
Transient response curve
155
7. Result and Discussions:

Time constant of given thermometer was:
Time constant of given thermocouple:
8. Nomenclature:
A= surface area of the bulb for heat transfer
C =heat capacity of mercury
m= mass of mercury
h= film coefficient of heat transfer
y = output temperature (thermometer reading)
ys = steady state temperature
xs = steady state temp of surrounding
x = surrounding temperature
Y(s) = y - ys
X(s) = x - xs
9. Reference:
1] Process System Analysis and Control (Second Edition) By
Donald R.Coughanowr
156
Experiment No.14 (B)

Time constant for RC circuit
1. Objective:
In this experiment we can learn about the charging and discharging process through capacitors.
Finally the time constant of RC circuits is determined.
2.Theory:
2.1. Charging a capacitor
When a battery or a DC Power supply is connected to an uncharged capacitor, the
charge on the capacitor increases exponentially from zero and when you discharge it the charge
on the capacitor decreases exponentially towered zero (1)
The circuit for charging and discharging a capacitor is shown in Fig 1. (a). Than the
battery charge the capacitor and current floe through the resistor R until the capacitor fully
charged [3]
Fig 1: RC- circuit a) the charging b) the discharging

If the Kirchoffs loop rule is applied for the first case , the following equation is obtained
iR QC = 0 .[1]
157
where
is the electromotive force (DC voltage supply) , R is the resistor Q charge of the
capacitor and C is the capacitance
when we substitute
dQ
for the current i in the equation [1]
dt
dQ
R
dt
, it becomes
Q
= 0 .[2]
C
If we rearrange the term in equation [2] , it can written as
dQ
=
dt
R
Q
C
[3]
The charge on the capacitor, the solution of equation [3] is given as a function of time t
Q = C (1 e
t
RC
[4]
Where Q = C is the maximum charge of the capacitor

The voltage across the capacitor Vc can be calculated as [1]
Vc =
Q
=
C
(1
e RC )
[5]
The product RC is called the time constant of the RC circuits denoted by
Replace
= RC
in the above equation
The voltage across the resistor and the current in the circuit also can be calculated
VR =
Vc = (e
t
RC
) .[6]
And
I =
t
RC
= I oe
t
RC
.[7]
After a time equal to RC the voltage across the resistor (or the current in the circuits)
158
Reaches (0.369) of the maximum value
VR =
(e
RC
RC
)= e
= 0.369
. [8]
Or
I = I oe
RC
RC
= I oe
Io
= 0.369 I o
e
[9]
On the other hand, voltage across the capacitor reaches 0.632 of its maximum value:
Q
Vc =
=
C
(1
RC
RC
)=
1
) = 0.632 -------------- [10]
e
(1
2.2 Discharging a capacitor:

If the switch is open fig (b) , than the battery is disconnected from the circuits and capacitor
start to discharge through the resistor. When we apply the Kirchhoffs rule we get the
following equation for the discharging,
dQ
Q
R+
=0
dt
C
.[11]
After solving the above equation we get
Q = CVc , o (e
t
RC
) = Qo (e
When we divide the equation [12] by
Vc = Vc , o (e
t
RC
C,
t
RC
[12]
we get the voltage across the capacitor
Vc
) , ..[13]
The voltage across the resistor and the current in the circuit also can be calculated
VR =
Vc =
Vc , o (e
t
RC
..[14]
And
159
I =
Vc , o
R
(e
t
RC
)=
I o (e
t
RC
) ..[15]
After a time equal to RC the voltage the across the capacitor reaches
0.369Vc , o of its maximum value:
Vc = Vc , o (e
RC
RC
) = Vc , o e
Vc , o
e
= 0.369Vc , o -------[16]
Charging Capacitor
Part-1: 1) Make sure all the switch is off.
2) Select the capacitor rating and resistant rating which you have provided.
3) Note down the value of capacitor and resistant and connect it inappropriate
socket (Take care of polarity of capacitor and resistance when connected)
4) Take any desired value of capacitor and resistance and fix it on the panel at
charging section
5) Open file RC TIMECONTANT.exe for run the experiment .
6) Choose select 5 volt from select source and than Start Charging from
charging section.
7) After full charging the time and voltage data was automatically save in
excel sheet
8) Do the same procedure from step 4-7 for every different capacitor and for
10 volt
Discharging Capacitor
Part-2 : 1) Make sure all the switch is off
2) Read the capacitor rating and resistant rating which you have provided.
3) Note down the value of capacitor and resistant and connect it in appropriate
socket (Take care of polarity of capacitor and resistance when connected)
4) Take any desired value of capacitor and resistance and fix it on the panel at
discharging section
5) Open file RC TIMECONTANT.exe for run the experiment
6) Choose select 5 volt from select source and than Start Discharging from
discharging section.
160
7) After full discharging the time and voltage data was automatically save in
excel sheet
8) Do the same procedure from step 4-7 for every different capacitor and for
10 volt
4. Calculation and Graph:

Capacitor Charging
R = 10000
C = 220 .F
theory
Vc =
= RC = 2.2 S
Q
= 0.632Vmax
C
Vc = (V )
Graph
t = (s )
= .....(s )
Capacitor discharging time constant
Vc = 0.369Vc , o
161
5. Result and Discussion:

Time constant of given R-C circuits
i) Charging
ii) Discharging
6. Nomenclature:
1)
Electromotive Fore
2)
Time Constant
3) Q
Charge on the Capacitor
4) C
Capacitor
5) R
Resistor
6) V
Voltage
7) Vc
Voltage across capacitor
8) F
Farad
9)
micro(10-6)
10)
Ohm
7. Reference:
1] Process System Analysis and Control (Second Edition) By
Donald R.Coughanowr
162


FAULT
1.
FINDING TRAINER
Introduction:
The industrial process fault finding trainer is diagnose to a provide a platform for a
student to trace a fault down to detailed level in the systematic way.
Fault can be introduce by the instructor via switches connect behind a locked
component to which the student does not access
These switches provide short circuits, and can switch in or out circuit element to
simulate a variety of fault condition.
The process cycle is controlled by the switches, which operate during the cycle and
these in turn control relay switch relay switches. The relay in their turn control the
operation of the active element of the trainer such as the pump and inlet /outlet valves
as well as the visual and audible indicators (lamp and speaker).
An interpose is provided in the form of a D type connector to allow the external
monitoring of the switches and the external control of the operation of the active
element and the indicators.
The interface effectively intercepts the circuitry between the status switches and active
control circuit elements, and allows an external user to programmed the response to
change in the state of the system switches. Typically a programmable logic controlled
would be used for this purpose.
1.1 Overview of the system:

The industrial process fault finding trainer bench mounted process rig with a mode of
operation which involves initially filling a header tank and cycling the water level
between a set of upper and lower limit , whilst simultaneously creating a demand from
the header tank via two on/off solenoid drain valves into a sump tank .
Flow is controlled by the relay operated on/off solenoid valve which control:
-the inflow of water to an header tank
-the out flow of water from the header tank
163
The level of the water in the header thank is monitored by the float switches which
open and close at the following points;
-
header than low (nearly empty)
header tank normal operation lower limit
header tank normal operation upper limit
header tank overflow
The sump tank is initially filled with water which is sufficiently fill the header tank and
provided a reserve to ensure that the system flow can be maintained in normal
operation.
If the sump is charge either with insufficient or too much water an alarm will be sound
and the system will be powered down.
Flow is maintained by the flow switches at various point in the process and the visual
direction is show on the front panel by indicator lamps. Indicator lamp is also show the
operation of the solenoid valve the alarm conditions, and whether the system is in the
initial fill system or in the normal operational cycle .
A ban of relay control the operation of the solenoid valves, the indicator lamp and the
system power on and off controls. The relay are switched on and off by the operation of
various level and flow switches in the system.
There are three independent process namely P1,P2 and Flow, controlled by a rotary
switch on the front panel . Only on of the process can be active at any instant. Each
stage processes is described in the following sections. The only difference between the
P1 and P2 process is in the rate of flow into and out of the header tank , with the P2
flow rate is greater than P1 process flow rate.
Fig 1-1 shows the schematic representation of the industrial process fault finding trainer
1.2 Initial set up of the rig.(see fig 1-1):

Ensure that the drain tap DT6 (fig1-1) is closed and that the drain pipe is copped by the
removable cap fitted .
Remove the top panel of the sump tank by ensuring the two blue fixing bolts. Fill the
sump tank 5cm of the top with clean cold water . Replace the top panel , and tighten
the bolts.
Connect the mains electricity input to single phase 13 amp fused main outlet. Ensure
that the earth leakage circuit breaker is on and press the green power on button is
164
pressed, or emergency stopped button is pressed. If the emergency stop button pressed
it must be released by turning a clockwise before power can be restored.
Check that all the lamp are lit when lamp test button are push on the front panel .
Open Tap DT1 ,DT2, DT3, DT4,DT5 and close the manual pump bypass valve in the
sump tank .
CAUTION
IN AN IMMERGENCY HIT THE RED STOP BUTTON ON THE TOP OF THE LEFT
HAND PANEL TO CUT CUICUIT TO THE RIG.
165
2. System Description:
2.1 System setup and accessories
The industrial fault finding trainer is supplied with arrange of accessories and
items with known fault
A complete industrial system consist of the following items
1X2.5 gal container
2X dummy flow indicator magnet
1X spare relay
1Xdarin tube
1Xtarainer key to control cabinet door
1X fault cabinet key
2.2 description of key component
2.2.1 Flow control valves
SV1- solenoid valve 1 header tank valve for process 1and process 2
SV2- solenoid valve 2 header tank drain valve for process 2 only
SV3- solenoid valve 3 inflow valve to the header tank for process 1
SV4- solenoid valve 4 inflow valve to the header tank for process 2
SV5- solenoid valve 5 inflow valve to the header tank for the initial fill and
the flow Process
2.2.2 Flow detectors
FD1- Flow Detector 1
detects header tank Overflow
FD2- Flow Detector 2
detects flow from the sump tank
FD3- Flow Detector 3 -
detects flow through SV3 (P1)
FD4- Flow Detector 4 -
detects flow through SV4 (P2)
2.2.3 System Operation switches
A) Sump tank:
SW1
float switch 1
Sump tank low switch
Normally open (when not

low)
SW2
float switch 2
Sump tank OK switch
Normally closed (when

not low)
SW3
float switch 3
system overcharged

overcharged)
166
B) Header tank:
SW4
- float switch 4
Header tank low

low)
SW5
float switch 5
Header tank lower limit
Normally closed (when

level lower limit)
SW6
float switch 6
Header tank full upper
limit
full)
2.3 P1 Process:
Starting the process
Operation: Set system Off button
Open the tab DT1,DT2,DT3,DT4,DT5, closed tab DT
Turn the rotary switch to flow , wait until the header tank drained and the red
header tank Indicator is illuminated .
Turn the rotary switch to P1 . The power available and header tank low lamp
should be illuminated.
Event
Action
Indicator(lamp
illuminated)
Illuminated - system on
- pump
- power
available
-initial fill
- SV5 and
FD2
-header tank
low
1. Press the green

system on button.
Water pump into header

tank and header tank fills
flow indicator switch
FD2 (the main flow
indicator is normally
open)closes
2.Float switch
SW4 (header tank
low)opens. This
switch is normally
closed.
Only the illuminated

indicator for the header
tank low is turned offNo other action
- pump
- power
available
-initial fill
- SV5 and
FD2
3.float switch
No action at initial fill
167
event of sequence then should be take -place

SW5(lowerThe following
stage.
pump
operating level or
- power
hysteresis)opens.
available
This switch is
-initial fill
normally closed.
- SV5 and
FD2
4.Float switch
SW6(header tank
full) closed. This
switch is normally
open.
Solenoid valve SV5(SV3

during cycle) closes ,
causing the flow into the
header tank to stop.
The solenoid valve SV1
open causing the header
tank to drain
- pump
- power
available
-initial fill
- SV1
-system
ready
5. Float switch
SW5(header tank
full)opens. This
switch is normally
open .
The header tank drain

down
6.float switch
SW5(Lower
Operating level or
hysteresis )closes.
This switch
normally closed.
Solenoid valve SV1

remain open so that there
is still a demand from
the header tank , which
still drains.
Solenoid valve SV3
opens to allow the water
in the header tank to be
replenished, but at a
lower rate than the initial
fill.
Flow detector FD2 and
FD3 close showing there
is a flow in the system
and through SV3.
- pump
- power
available
-initial fill
- SV1
-system
ready
- pump
- power
available
-initial fill
- SV1
-system
ready
- SV3,FD2,
FD3
7. Go to event 4 ,
and read SV3 for
SV5
The level in the header

tank will rise provide the
flow into the tank
through SV3 is greater
than the outflow through
SV1.
The system cycle
through events 4,5,6 &7
continuously
168
2.4 P2 Process:
Operation : Set system Off button
Open the tab DT1, DT2,DT3,DT4,DT5, closed tab DT6
Turn the rotary switch to flow, wait until the header tank drained and the
red header tank Indicator is illuminated.
Turn the rotary switch to P2 . The power available and header tank low
lamp should be illuminated.
The following event of sequence then should be take place
Event
Action
Indicator(lamp
illuminated)
- pump
- power
available
-initial fill
- SV5 and
FD2
-header tank
low
1. Press the green

system on button.

flow indicator switch
FD2 (the main flow
indicator is normally
open)closes
2.Float switch
SW4 (header tank
low)opens. This
switch is normally
closed.

indicator for the header
tank low is turned offNo other action
- pump
- power
available
-initial fill
- SV5 and
FD2
3.float switch
SW5(lower
operating level or
hysteresis)opens.
this switch is
normally closed.
No action at initial fill

stage.
- pump
- power
available
-initial fill
- SV5 and
FD2
4.Float switch
SW6(header tank
full) closed. This
switch is normally
Solenoid valve SV5(SV4

during cycle) closes ,
causing the flow into the
header tank to stop.
- pump
- power
available
169
open.
The solenoid volve SV1

and SV2 open causing
the header tank to drain
-initial fill
- SV1 , SV2
-system
ready
5. Float switch
SW5 (header tank
full) opens. This
switch is normally
open.
The header tank drains

down
- pump
- power
available
-initial fill
- SV1,SV2
-system
ready
6. float switch
SW5(Lower
Operating level or
hysteresis )closes.
This switch
normally closed.
Solenoid valve SV1and

SV2 remain open so that
there is still a demand
from the header tank,
which still drains.
Solenoid valve SV4
opens to allow the water
in the header tank to be
replenished, but at a
lower rate than the initial
fill.
- pump
- power
available
-initial fill
- SV1and
SV2
-system
ready
- SV4,FD2,
FD4
Flow detector FD2 and

FD3 close showing there
is a flow in the system
and through SV3.
7. Go to event 4 ,
and read SV4 for
SV5
The level in the header

tank will rise provide the
flow into the tank
through SV3 is greater
than the outflow through
SV1 and SV2.
The system cycle
through events 4,5,6 &7
continuously
2.5 Flow- Process:

Operation: Set system Off button
Open the tab DT1, DT3, DT4, DT5, closed tab DT2
Turn the rotary switch to flow, wait until the header tank drained and the
red header tank Indicator is illuminated.
170
The power available and header tank low lamp should be illuminated
Solenoid valve SV1 and SV2should open and their indicators illuminated.
The following event of sequence then should be take place
Event
Action
Indicator(lamp
illuminated)
1. Press the green

system on button.

whilst simultaneously
flowing out through
solenoid valve SV1 And
SV2.
flow indicator switch FD2
(the main flow indicator is
normally open)closes.
- pump
- power available
-initial fill
- SV5, SV1, SV2

And FD2
-header tank low
2.Float switch SW4

(header tank
low)opens. This
switch is normally
closed.

indicator for the header tank
low is turned off- No other
action
- pump
- power available
-initial fill
- SV5,SV1,
SV2 and FD2
3.float switch
SW5(lower operating
level or
hysteresis)opens.this
switch is normally
closed
No action
- pump
- power available
-initial fill
- SV5 and FD2

SV1, SV2
4.Float switch
SW6(header tank
full) closed. This
switch is normally
open
No Action water flow into

the header thank at a faster
rate than it flow out
- pump
- power available
-initial fill
- SV5,SV1,SV2,
And FD2
5.system overflows
into overflow outlet
and closes flow flow
indicator switch FD1
The system stabilizes with

water entering the header
tank through solenoid valve
SV5 and flowing out
through solenoid valve SV1
and Sv2 also through the
overflow outlet
- pump
- power available
-initial fill
- SV5,SV1,SV2,
And FD2
- system
overflow
171
System flow chart
S3 - Process P1
S7- INDICATORS,
SWITCHES AND
INTERLOCKS
The rig is control by

switches on the front
panel and relay
switches in the control
cabinet.
System operation is
shown by illuminating
indicators on the front
panel on the control
cabinet. These are
green (power and
system on) Amber
S1- INITIAL STATE

Representation the
state of the system
when external power
has been connected to
the rig. And power on
button pressed .
This representation
shows the initial state
of the control valves,
indicator lamps, flow
detector and system
switches , when no fault
are present , for all
system processes.
S2- INITIAL FILL

All process start with an
Low inflow and outflow rates into and header

tank
initial fill stage which

pumps water from sump
tank into header tank .
When the header tank is
full the process
S4 - Process P2
Medium inflow and outflow rates into and
header tank
changes into one of the

three selectable process
cycles which continue
S5 - Process Flow
indefinitely.
Fast inflow and outflow rates into and header
These three process are
tank. These foe rate it greater than the maximum
called P1, P2 and flow
outflow rate so that the header tank will normally
and operate at different
overflow.
floe rates and demands

on the header tank.
(informative). Red
S6- Proportional Process
(warning and interlock)
Provides a methods of manually regulating flow

into the header tank
172
INDICATORS
INDICATORS
Power available ON
SV1

ON
SV2

ON
SV3

ON
Power available ON
SV1

ON
SV2

ON
SV3

ON
Header tank low ON
QUNTITATIVE INDICATORS
Header tank lavel sight glass 3.0 + 0.5
Sump tank level sight glass 10+0.5
LCD flow indicator
0+1%
LCD header tank level 0+1%
RELAYS
RL5
RL7
RL9

ON
ON
ON
3 way process
Switch to flow
S1 Intermediate Level
INITIAL STATE

RELAYS
RL5
RL7
RL9
RL12
F1
System drain down
ON
ON
ON
ON
HEADER TANK LOW

Switch closes
Diagram 2
173
INDICATORS
INDICATORS
INDICATORS
System available ON
Initial fill
ON
Power available ON
Pump
ON
FD2 (closed)
ON
SV5 ON
Header tan law ON at first
than off
System on
ON
Power available ON
Pump
ON
Ready
ON
SV1(P1)
ON
SV1 And SV2(P2) ON
System on
ON
Power available ON
Pump
ON
Ready
ON
SV1(P1)
ON
SV1 And SV2
ON
S2 Intermediate
Level
INITIAL STATE
Process P1 and P2
RELAYS
RL1A
RL1B
RL5

F1 -Process
This stage is common
to P1 and P2.
Select either P1or P2
by the rotary switch

RELAYS
RELAYS
RL1A
RL1B
RL4

RL3A
RL3B
RL7(P1 and P2)
RL9(P2)

ON
ON
ON
System On
switch
F2
pump on
header
tank fills
with water
ON
ON
ON
ON
ON
ON
ON
RL1A
RL1B
RL3A
RL3B
RL7(P1 and P2)
RL9(P2)
ON
ON
ON
ON
ON
ON
Header tank full

switch open
Header tank full

switch closes
Diagram -2
Diagram -2
Diagram -1
F3 -Header
tank inflow
stops
174
INDICATORS
INDICATORS
System On ON
Power available ON
Pump
ON
Ready ON
SV1 ON
System on
ON
Power available ON
Pump
ON
Ready
ON
SV1

ON
RELAYS
RELAYS
RL1A
RL1B
RL3A
RL3B

INDICATORS
System on
ON
Power available ON
Pump
ON
Ready
ON
SV1, SV3
ON
FD2 and FD3
ON
RL1A
RL1B
RL6A
RL6B
RL3A
RL3B
RL7 and RL8

ON
ON
ON
ON
Diagram -2
F1 Stage 1
The header tank
drain drown
through SV1
ON
ON
ON
ON
ON
ON
ON
RELAYS
RL1A
RL1B
RL3A
RL3B
RL4
RL7
S3 Intermediate
Level
Process 1
Diagram -2

Header tank full
switch open
Diagram -2
The header
tank start to
refill through
SV3
Hysteresis switch
open
Indicator no change
Relay no change
ON
ON
ON
ON
ON
ON

Diagram -2
F2 stage 2
Hysteresis switch
closes
Header tank full

switch closes
F3- stage 3
The header
tank inflow
stops
175
INDICATORS
INDICATORS

System on
ON
System On ON
Power available ON
Power available ON
Pump
ON
Pump
ON
Ready
ON
Ready ON
SV1, SV2,SV4
ON
SV1, SV2 ON
FD2 and FD4
ON
ON
System on
ON
Power available ON
Pump
ON
Ready
ON
SV1,SV2
ON
RELAYS
RELAYS
RL1A
RL1B
RL3A
RL3B
RL7
RL9

INDICATORS
RL1A
ON
RL1B
ON
RL6A
ON
RL6B
ON
RL3A
ON
RL3B
ON
RL7 and RL9
ON
RL10 ON

ON
ON
ON
ON
ON
ON
Diagram -2
F1 Stage 1
The header tank
drain drown
through SV1 and
SV2
RELAYS
S4 Intermediate
Level
Process 2
Diagram -2
Diagram -2
F2 stage 2
Hysteresis switch
closes
The header
tank start to
refill through
SV4
Hysteresis switch
open
Indicator no change
Relay no change
Header tank full

switch closes
RL1A
ON
RL1B
ON
RL3A
ON
RL3B
ON
RL4

ON
RL7 AND RL9 ON

ON

F3- stage 3
The header
tank inflow
stops
Header tank full

switch opens
Diagram -2
176
S7 Intermediate Level
Interlock, switches and indicators
F1- INDICATORS

Do no permit the system to
run if either of the two
following condition are true:
-The system is overcharged or
the sump tank overflow is low.
-These conditions will power
the system process down at
any point in the process
sequence .the rig itself remain
powered up
F2- POWER AND

SWITCHES

A) System powered up by
an relay latched on which
with earth leakage
protection.
B) Three position rotary
switch to set process to
P1,P2 or Flow .
C) Process witches(system
state monitoring by float
switches in the header and
sump tanks)
F3- RELAY SWITCHES

A bank of 15 relays located in the
control cabinet on the left of the rig
and which provide the switching logic
to control the rig.
Relay are energized by the operation
of the rig process switches, warning
condition or by the action of other
relays.
Relays control the opening in shutting
of the flow control (solenoid)valves ,
shutting the system down in the event
of the warning interlock and in certain
cases the operation of the other
relays
F4- INDICATORS
A)
Audible and red visual

alarm when the overcharge
with too much water .
B)
Red visual alarm for

header tank low and
header tank overflow
C)
Informative amber visual

indicators for on/off
solenoid flow valves ,On/off
flow detectors.
D)
Digital header tank flow

rate and level display.
LOGICAL INDICATORS:
HEADER AND SUMP TANK SLIGHT
GLASSES
GLASS FLOW INDICATOR
177
F2.1
SWITCH SETTING FRONT PANNEL
Power on (Green)
Power off (Red)
Earth leakage circuit breaker
3 way rotary process switch P1, P2 and
Flow
System on (green)
System off (Red)
F2.2 HEADER TANK PROCESS SWITCHS(OPEN

/CLOSED)
Header tank low

Normally open
Header tank lower cycle limit
Normally closed
Header tank full

Normally open
Header tank overflow

Normally open
F 2.3 SUMP TANK PROCESES SWITCH(OPEN/CLOSED)
S7F2
Power and Switches
Sump tank low

Sump tank OK
System overcharge
Normally closed
Normally closed
Normally open
178
F3.1 SYSTEM ON /OFF

COTROLL RELAYS

RL1A, RL1B

A pair of relay switched on when
the system ON button is pressed
and switched on system OFF
button is pressed, or the system
is powered down by the warning
condition interlocked
F3.2 PROCESSES LOGIC

RELAYS

RL3A,RL3B

A pair of relays Powered up
when the system entered
the main P1 and P2 cycles
and the system ready
indicator is on.
They remain powered up
during the P! And P2 cyclic
Phases .
RL4
Switched on when the
header tank full switch
closed.
F3.3- FLOW VALVE

CONTROLLRELAYS
RL5
open and closes SV5
RL7
open and closes SV1
RL8
open and closes SV3
RL9
open and closes SV2 &SV3
RL10
open and closes SV4
F3.4 WARNING CONDITION

CONTROL INTER LOCK RELAYS
RL11
Powered up by the header tank
overflow switch closing.
Turns Off SV3 and SV4.
Turns on Header tank overflow
indicator
RL-12
Powered up by the header tank
switch closing .Turns Off system
Ready indicator.
RL6A, RL6B
A pair of rely used in the
control of P1 and P2 cyclic
phases. RL6A is concerned
with Process P1 and RL6B
is concerned with P2
179
S7F4
Indicator
F4.1
IITK/CHE/UO
Manual (CHE interlocks
492)
WarningLab/Lab
indicators(Red)and
F4.2 INFORMATIVE INDICATORS AMBER

Ready
Power available
Initial fill
Pump
On
SV1
ON (solenoid valve 1 open)
SV2
SV3
SV4
SV5
Header tank low

Header tank overflow
(System off interlock)
System Overcharged
(System off interlock)
F4.3 QUNTITQTIVE INDICATORS

Header tank level sight glasses(low to full )
min
3.0(+/-) 0.5
max
10(+/-)1
LCD flow indicator

(Alternative scale selected by switch)
0(+/-) 1%
4(+/-)0.1mA
100(+/-)10%
20(+/-)1 mA
LCD header tank level (low to full)

(Alternative scale selected by switch)
0(+/-)0.3 %
4(+/-)0.1mA
100(+/-)10%
20(+/-)1 mA
Flow detector 2
Flow detector 3
Flow detector 4
FD2
FD3
FD4
closed
closed
closed
180
4 Fault Diagnoses
Fault Switch No.
Fault Switch
Process Switch
Fault Symptom
Diagnostic Method
181

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IITK/CHE/UO Lab/Lab Manual (CHE 492)

INDIAN INSTITUTE OF TECHNOLOGY

DEPARTMENT OF CHEMICAL ENGINEERING

IITK/CHE/UO Lab/Lab Manual (CHE 492)

Liquid Liquid Extraction

Liquid Solid Adsorption In a Packed Bed

Mass Transfer From a Single Drop

Plug Flow Reactor

Semi batch Reactor

R.T.D in CSTR and packed Bed Reactor

Characteristic of P.I.D Controller

Characteristic of Pneumatic Control Valve

Flow control Trainer

Interacting And Non Interacting Tank System

Time Constant of Thermocouple & Time Constant of RC

Fault Finding Trainer

IITK/CHE/UO Lab/Lab Manual (CHE 492)

CHEMICAL ENGINEERING LABORATORY

Before starting the experiments

Study the experimental setup thoroughly

Get the required material issued from the laboratory assistance.

IITK/CHE/UO Lab/Lab Manual (CHE 492)

After the completion of the experiments

Shut off the experiment.

Clean the equipment and the surrounding area

Close all the valve and switch off electrical connection

Late submission of lab report is strictly not allowed .

Title of the experiment

Objective of the experiment should clearly indicate what is the purpose

IITK/CHE/UO Lab/Lab Manual (CHE 492)

Experimental Apparatus and Procedure

Results and Discussion

The raw data should be included in the appendix.

Sample calculations should be shown in detail indicating clearly each of

IITK/CHE/UO Lab/Lab Manual (CHE 492)

Answer the questions given in the write up of the experiment.

Raw data should be included here.

Details of any repetitive calculations.

Some General Rules of Report Writing:

Do not use significant figures indiscriminately.

IITK/CHE/UO Lab/Lab Manual (CHE 492)

SUGGESTED GUIDELINES FOR SAFE WORKING IN THE LABORATORY

Smoking is strictly prohibited in the laboratory.

Do not put on loose clothing.

The following precautions should be observed when using electrical gadgets.

Do not insert naked wires in wall plugs.

Before starting the equipment, check if the equipment is properly grounded. If

IITK/CHE/UO Lab/Lab Manual (CHE 492)

Never lean on frames, work benches or equipment.

IITK/CHE/UO Lab/Lab Manual (CHE 492)

INDIAN INSTITUTE OF TECHNOLOGY KANPUR

Unit Operation Lab (ChE-492)

Percentage removal of solute

The theoretical number of stages required

The overall stage efficiency (theoretical/actual)

The variation of stage efficiency with solvent (benzene) flow rate.

IITK/CHE/UO Lab/Lab Manual (CHE 492)

Principles of Liquid Extraction

B denotes the solvent ( water in this

(wt frac.Cin E) /(wt frac.A in E) y*E (wt frac.A in R)

IITK/CHE/UO Lab/Lab Manual (CHE 492)

Single Stage Extraction

from which xM1 can be calculated.

R1 can be found from an overall mass balance.