Jawaharlal Nehru Engineering College

Laboratory Manual

Process Instrumentation & Analytical Chemistry

For

Third Year Students Chemical Engineering

16, Dec 2003 Rev 00 Chemical Engg. ISO 9000 Tech Document

Author JNEC, Aurangabad

FORWARD

It is my great pleasure to present this laboratory manual for Third year

engineering students for the subject of Mass Transfer Operation keeping in
view the vast coverage required for visualization of concepts of Mass Transfer
Operation with simple language.
As a student, many of you may be wondering with some of the questions in
your mind regarding the subject and exactly what has been tried is to answer
through this manual. As you may be aware that MGM has already been
awarded with ISO 9000 certification and it is our endure to technically equip
our students taking the advantage of the procedural aspects of ISO 9000
Certification. Faculty members are also advised that covering these aspects in
initial stage itself, will greatly relived them in future as much of the load will be
taken care by the enthusiasm energies of the students once they are
conceptually clear.

Principal

LABORATORY MANNUAL CONTENTS

This manual is intended for the Third year students of Chemical Engineering
branch in the subject of Mass Transfer Operation. This manual typically
contains practical/Lab Sessions related Mass Transfer Operation covering
various aspects related the subject to enhanced understanding.
We have made the efforts to cover various aspects of the subject covering Various
Mass transfer operations used in chemical industry will be complete in itself to make
it meaningful, elaborative understandable concepts and conceptual visualization.
Students are advised to thoroughly go though this manual rather than only topics
mentioned in the syllabus as practical aspects are the key to understanding and
conceptual visualization of theoretical aspects covered in the books.

Good Luck for your Enjoyable Laboratory Sessions

S D YADAV of Chemical Engineering Department

SUBJECT INDEX

1.

To determine time constant& study step response for first order

system (Mercury bulb Thermometer).

2.

To determine time constant & study step response for Single level
liquid tank.

3.

To determine time constant & study step response for second order
system (Mercury Manometer).

4.

To illustrate characteristics of Thermocouple.

5.

To illustrate characteristics of Thermister.

6.

To illustrate characteristics of Resistance Temperature Detector.

7.

To determine Normality of Acid by Conduct metric Titration.

8.

To determine Normality of NaoH by Conduct metric Titration

9.

To determine PH of given solution by pH Meter.

10.

To determine the relative fraction value (Rf) for given compound by

Chromatography.

11.

Quiz on the subject

12.

Conduction of Viva-Voce Examinations:

13.

Submission

14.

Evaluation and Marking Systems

DOs and DONT DOs in Laboratory:

1.

Do not enter the laboratory without wearing apron, preferably use shoes.

2. Safety should be given topmost priority.

3. Follow the instructions given by the teacher.

4. Do not touch any Equipment/Chemicals without prior permission.

5. Check the glassware before getting issued.

6. Handle the chemicals carefully as per instructions.

7. Do not pipette any solution/chemical with mouth.

8. During performance of the practical if any glassware is broken inform immediately.

9. Return the borrowed apparatus after the expt. is over.

10. Observe safety precautions while performing the expts.

Instruction for Laboratory Teachers::

1.

Submission related to whatever lab work has been completed should be done during the
next lab session.

2. The promptness of submission should be encouraged by way of marking and evaluation

patterns
that will benefit the sincere students.

Exercise No10: (2 Hours) 1 Practical

A] Aim: To determine the relative fraction value (R f) for given compound by Chromatography.

Chemicals: Benzene
Apparatus: Silica

+ Ethanol (Solvent), Acetophenon, Aniline & Iodine crystals.

gel plate, flask, oven

Theory:

Procedure: 1) Prepare a std. solvent in 100ml of Benzene by adding two three drops of alcohol.
2) Prepare Silica gel plate and dried in oven for 1 hr at 106 c.
3) Mark spot of Acetophenon & mixture on the plate. Then take plate and then place plate in
Iodine crystal in flask, wait for some time.
4) The some spots are observed mark those spots. & measure difference from solvent line
5) Measure distance travelled by each individual molecule measured.

Result:

Conclusion:

Exercise No11: (2 Hours) 1 Practical

A] Aim: To study ferric salicylic Acid complex absorption potentially by Jobs method of continued titration.

Chemicals: N/500

Apparatus:

Hcl, 10-3 m3 Salicylic Acid in N/500 Hcl &10-3 m3 ferrous ammonium in N/500 Hcl.

stopper glass bottles, beakar

Theory:

Procedure: 1) The optimum Ph for the stability of complex is about 2.6 to 2.8. This is obtain using
solution of reactant in N/500 Hcl.
2) Mix the salicylic Acid solution in different proportions in properly stopperd glass bottles.
3) Measure the transmission or optical density for particular mixture using different filter.
4) Measure the transmission or optical density for each bottles.

Sr. No.

Volume of Salicylic Acid (ml)

1
2
3
4

Result:

Conclusion:

Volume of Ferrous Ammonium (ml)

Transmission (%)

Exercise No7: (2 Hours) 1 Practical

A] Aim: To determine Normality of Acid by Conduct metric Titration.

Chemicals: Acetic

Acid, Hcl & NaoH.

Apparatus: Conduct

meter, Beaker, microburtte

Theory:

Procedure: 1) Prepare pipette out 5ml of Hcl solution & 5ml of Acetic Acid in beaker.
2) Add 40 ml distilled water to it. & dip conducting bridge fill the microburtte with steel NaoH
solution.
3) Titrate the Acid mixture solution conduct metrically and note down conductance value

Sr. No.

Volume of NaoH added

Observed conductance

Calculations: plot the graph of Volume of NaoH Vs Conductance

Result: 1) Normality of Hcl is =

2) Normality of CH3COOH is =
3) Normality of H2Ol is =

Conclusion:

Exercise No8: (2 Hours) 1 Practical

A] Aim: To determine Normality of NaoH by Conduct metric Titration.

Chemicals: Acetic

Acid, Hcl & NaoH.

Apparatus: Conduct

meter, Beaker, microburtte

Theory:

Procedure: 1) Prepare pipette out 5ml of NaoH l solution & 5ml of Acetic Acid in beaker.
2) Add 40 ml distilled water to it. & dip conducting bridge fill the microburtte with steel NaoH
Solution.
3) Titrate the Acid mixture solution conduct metrically and note down conductance value

Sr. No.

Volume of NaoH added

Observed conductance

Calculations: plot the graph of Volume of NaoH Vs Conductance

Result: 1) Normality of Hcl is =

2) Normality of CH3COOH is =
3) Normality of H2Ol is =

Conclusion:

Exercise No6: (2 Hours) 1 Practical

A] Aim: To determine the temperature using RTD (Resistance Temperature Detector).

Chemicals:
Apparatus: Resistance

Temperature Detector, LCR meter, Water heater etc.

Theory:

Procedure: 1) Make the connections as shown in the figure.

2) Change the temperature of water by using heater change in the corresponding resistance
should be noted.
3) Plot the graph of R/R0 vs. temperature and resistance vs. temperature.

Observation Table:

Sr. No.

Result:

Conclusion:

Temperature in ()

Resistance R in ()

R/R0

Exercise No5: (2 Hours) 1 Practical

A] Aim: To determine the temperature using Thermister.

Chemicals:
Apparatus: Thermister,

Water heater, Water pot, Stand, Milivoltmeter, Digital millimeter

Theory:

Procedure: 1) Make the connections as shown in the figure.

2) Measure the resistance of Thermister at room temperature step by step providing heat and
note down the change in resistance at different temperatures.
3) Plot the graph temperature vs. Resistance.
Resistance at given temperature.
R1 = R2 e (1/ T1 1/T2)
R1 = Resistance of Thermister at T1.
R2 = Resistance of Thermister at T2.
= Constant depending upon material of Thermister.

Observation Table:

Sr. No.

Temperature in ()

Result: The average value of

Thermal Resistance

Conclusion:

Exercise No4: (2 Hours) 1 Practical

A] Aim: To determine the temperature using Thermocouple.

Chemicals:
Apparatus: Thermocouple,

Water heater, Water pot, Stand, Milivoltmeter, Digital millimeter.

Theory:

Procedure: 1) Make the connections as shown in the figure.

2) Change the temperature of water by using heater change in the corresponding resistance
should be noted.
3) Plot the graph of R/R0 vs. temperature and resistance vs. temperature.

Observation Table:

Sr. No.

Result:

Conclusion:

Temperature in ()

Resistance R in ()

R/R0

Exercise No3: (2 Hours) 1 Practical

A] Aim: To determine the time constant of a second order system (Mercury manometer).

Chemicals:
Apparatus: U

tube Mercury Manometer.

Theory:

Procedure: 1) Check the U-tube manometer for atmospheric pressure acts on both limbs or nor.
2) observe the steady state height of U-tube manometer where no atmospheric pressure acts
On both either limbs.
3) Apply the pressure inputs to one of the limbs for a certain amount of time.
4) Note the displacement of manometric fluid from the steady state height and time of
oscillation.
Observations:

1) steady state height H(s) =

2) Initial Height, H (i) =

cm.

cm.

Observation Table:

Sr. No.

Calculations: plot

Height H(t) (cm)

a graph of Y(s) Vs Time (t)

Results: 1) Time constant =

Conclusion:

Time t in (sec)

Y(t) = ( H(t) H(i)/ H(s)- H(i)

Exercise No2: (2 Hours) 1 Practical

A] Aim: Experiment to determine time constant and study the step response for a single tank liquid system.

Theory:

Procedure:

1. Admit water into the tank at a known flow rate and wait for steady to be
achieved.
2. When the outlet flow rate will be such that height of liquid does not change.
3. Measure the steady state flow rate Q(s) and height H(s) of the tank.
4. Repeat the about step for different inlet flow rates.

Observations:

1. Cross Sectional Area of tank=

m2

Observation table:

Sr.No.

Time (sec.)

H(t) Experimental (cm.)

1.
2.
3.
4.
5.

Calculations:

Area of tank = / 4 d2
For step change input, H (t) = A x R (1-e-t/)

Q(s) m3/sec

H(t) Theoretical(cm.)

Resistance R = 1/ slope.
= A.R

Graph:

Plot a graph of Q(s) Vs H (t).

Results:

The time constant for first order system of Single tank liquid level system is. sec

Conclusion:

Exercise No1: (2 Hours) 1 Practical

A] Aim: To determine the time constant for mercury bulb thermometer..

Chemicals:
Apparatus:

Water heater, Water pot, Stand, thermometer.

Theory:

Procedure: 1) Fill the water bath completely and heat it till it boils.
2) Note down the thermometer reading Y(s) and insert it in to water bath.
3) Record the thermometer reading Y (t) after every 5 second for either positive.
Or negative step change.
Observation table:

1) Y(s) = Room temperature =

Sr. No.

Calculations: Time

Time t in (sec)

Y(t)

Y(t)/A

constant, = m c / h A

Where m = Mass of thermometer bulb in Kg.

C = Specific heat of mercury in KJ/kg K
H = Heat transfer Co. in W / m2 K
A = Area of thermometer bulb in m2
Plot a graph of Y (t)/A Vs Time (t) and time constant.
Results: 1) Time constant for first order system of mercury bulb thermometer is = sec.

Conclusion:

Exercise No1: (2 Hours) 1 Practical

A] Aim: To determine the pH of given solution by pH Meter.

Chemicals: Std.
Apparatus:

solution having pH of 4, 7, 9.

Water heater, Water pot, Stand, thermometer.

Theory:

Procedure: 1) Deep Electrode into std. solution of 2M KCl & AgCl.

2)