SARDAR VALLABHBHAI PATEL EDUCATION SOCIETY MANAGED

N. G. PATEL POLYTECHNIC
Chemical Engineering Department
Bardoli – Navsari Road, At: Isroli, Po: Afwa, Tal: Bardoli, Dist: Surat – 394620
Website: www.ngpatelpoly.ac.in, Phone No.: 9512900459

LABORATORY MANUAL
4350501 – Mass Transfer - II
Fifth Semester

Rules & Regulations for Students:

 Do’s

 Observe good housekeeping practices. Replace the materials in proper place after work to
keep the lab area tidy.
 Conduct yourself in a responsible manner at all times in the laboratory.
 Before starting Laboratory work follow all written and verbal instructions carefully. If you
do not understand a direction or part of a procedure, ask your concern faculty before
proceeding with the activity.

Don’t

 Do not eat food, drink beverages or chew gum in the laboratory

 Do not wander around the room, distract other students, startle other students or interfere
with the laboratory experiments of others.
 Students are not allowed to work in Laboratory alone or without presence of the teacher.

Safety Precautions in Lab:

1. Ensure appropriate attires: no slippers, sandals or open-toe footwear allowed.

2. Long hair should be properly tied.
3. Make sure hands are dry when conducting experiment.
4. Before using any chemicals or glassware one must get acquainted with its operation
manual, paying particular attention to advices and warnings related to chemicals and
user safety.
5. Laboratory equipments, glassware and chemicals should be used for purposes they are
intended for, in the way described in their operation manuals and only within the scope
of the work being carried out.
6. The Equipments should be operated in a careful, delicate and thoughtful manner,
students can use the three-phase mains only upon explicit consent of their teacher or
supervisor.
7. Exercises should be carried on strictly according to guidelines contained in the exercise
manual, strictly observing safety guidelines given in bold type.
8. Never leave experiments while in progress. Immediately report any spills, accidents, or
injuries to your instructor.
9. Make sure no flammable solvents are in the surrounding area when lighting a flame.
Turn off all heating apparatus, gas valves, and water faucets when not in use.
10. Properly dispose of broken glassware and other sharp objects immediately in
designated containers.

DETAILS OF COURSE COORDINATORS AND BATCH COORDINATORS

Course Batch Co-ordinators

Coordinator 1 2 3 4 5 6
 N. G. Patel Polytechnic
Chemical Engineering Department

CERTIFICATE
This is to certify that Mr. / Miss. __________________________________ bearing

enrolment number _____________ of Class _____________ has satisfactorily

completed his / her laboratory work in the subject

__________________________________________________________________

_ in the institution premises and submitted a complete laboratory record during the

academic year ___________.

Date : _________
Place : Isroli, Bardoli

Subject Teacher Head of Department

Lecturer in Chemical Engg. Chemical Engg. Dept.

Principal
N. G. Patel Polytechnic
 INDEX
Name of Student :
Enrolment No. :
Class & Batch :

Sr. Marks Obtained

Date Name of Practical Sign
No. Manual Que. Viva Total

10

11

12

Total Marks
Average Marks
Average of Total Marks
EXPERIMENT NO: DATE:
CRYSTALLIZATION
AIM:- To find out Crystal Yield with& Without seeding.
APPARATUS:- Weight box , Beaker, Thermometer, etc.,
CHEMICALS:- Water, Benzoic acid.
THEORY:-
Crystallization is a unit operation that involves the separation of a solute form its
solution in the form of crystals. In this solid – liquid separation process solid
particles are formed within a homogeneous phase. It can occur as
1)Formation of solid particles in a vapor,
2)Formation of solid particles from a liquid material and
3)Formation of solid crystals from a solution
Crystallization is normally carried out in process industry either from solution
or from melts, the former being very common because it gives almost pure
product from relatively impure solution. Crystallization requires much low
energy for separation compared to other purification method like distillation, etc.
It is more convenient to use any material in the crystalline form because it is
facilitates packing and storing. Crystallization process usually involves two
steps:-
Concentration of solution and cooling of solution until the solute concentration
becomes greater than its solubility at that temperature. Then the solute comes
out of the solution in the form of pure crystals.
In case of crystallization from solution, the tow phase mixture of mother liquor
and the crystals occupies the crystallizer and in the Withdrawn as a product is
called as Magma
Crystallization is generally followed by filtration for separation of crystals form
mother liquor.In majority of industrial crystallization process, the mother liquor
and the solid crystals are allowed to make contact with each other for a log time
to reach equilibrium, so that mother liquor is saturated at the final temperature.
The final concentration of the solute in the solution can be obtained from the
solubility curve.
 Formation of structure
Preparation of crystal matter from a solution is a two step process. The first is
“nucleation” and the second is the “growth of crystals” to macroscopic size the
generation of new solid phase either on an inert material in solution or in the
solution it self is called “nucleation” while “growth” is the increase in size of this
nucleus with layer by layer addition of solute. Super saturation is the common
driving force for nucleation & crystal growth. Unless the solution is super
saturated neither nucleation nor crystal growth occurs means there is no
crystallization.
Super saturation
It is the quantity of the solute present in which crystal are growing compared
with the quantity of the solute that is in equilibrium with the solution.

PROCEDURE:- 1. Take 100 ml water in beaker & heat up to 70 0 C.

2. Then add 32 gm of benzoic acid as a solute & stir it still it
becomes completely soluble.
3. Then cool it up to 20 c. & weight the crystals.
4. Repeat the procedure in another beaker in this case adds 5 gm
of acid crystals at the rest temperature & cool it at 5°C & weigh
the Crystals.
OBSERVATION:-
1. Test temperature =
2. Room temperature=
3. Weight of crystals obtained theoretically=
4. Weight of crystals without seeding=

CALCULATIONS:-
Crystals without seeding

Wt. of crystals Obtained

= -----------------------------------------------------------------
Solubility at 70°C – Solubility at room temperature
 = ------------------- %

Crystals with seeding

Wt. of crystals Obtained
= -----------------------------------------------------------------
Solubility at T0C – Solubility at room temperature

= ------------------ %
RESULT: - Yield without seeding = ------------- %
Yield with seeding = ------------- %

CONCLUSION:_____________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________

QUESTION:-
1. Define : Crystallization
2. Explain the term super saturation which is the techniques to
bring super saturation?
3. In our experiment which technique of super saturation we
adopt?
4. What do you mean by fractional crystallization, zone
refining & adductive crystallization?
5. In our crystallization operation crystals are generated from
homogeneous phase: Justify the statement in our case.
EXPERIMENT NO: DATE:
STEAM DISTILLATION

AIM:- To verify Henry’s law for steam distillation.

APPARATUS:- Distillation flasks ,Steam generator ,Measuring cylinder, Beakers,

Thermometer, Stop watch

CHEMICALS:- Nitrobenzene, water

THEORY:-

Steam distillation relies on the unique vapor pressure relations of immiscible

liquids, predominately hydrocarbons. In steam distillation, the open steam is
used to reduce the operating temperature. If the components of binary mixtures
are completely insoluble, both components will exert their true vapor pressure
at prevailing temperature. When sum of the separate vapor pressure equals the
total pressure, the vapor composition is readily computed by (pA + pB = pt). So as
two liquid phases are present, the mixture will boil at the same temperature, and
the high organic liquid can be made to vaporize at the temperature much lower
than its normal boiling point at atmospheric pressure

Steam distillation is a convenient technique for distilling certain difficult to

handle materials. It offers a simple solution to some knotty separation or
purification problems involving.

1. Chemicals having relatively high boiling point at atmospheric pressure.

2. Chemicals that are likely to decompose even at their atmospheric boiling point
e. g. fatty acid.

3. Chemicals that pose hazards when distilled by direct heating e.g. turpentine.
PROCEDURE:- 1. Take 100 ml of nitrobenzene in distillation flask.

2. Fill up the water in steam generator.

3. Arrange the assembly as shown in figure.

4. Start the assembly as shown in figure.

5. Start the condenser water flow as shown in figure.

6. After sometime steam will generator and will enter into the
distillation flask.

7. The distillation operation will start.

8. The distillate water vapor of nitrobenzene and steam will go to

the condenser and finally the vapor mixture is condensed.

9. Record the distillation temperature.

OBSERVATION:-

Density of water= 1gm/cc

Density of nitrobenzene = 1.27 gm/cc

Vapor pressure of water at distillation =

Vapor pressure of nitrobenzene at distillation=

Volume of water collected=

Volume of nitrobenzene collected=

Boiling point of nitrobenzene=

Temperature of distillation =

CALCULATIONS:-
 1. WA = ρA * VA
where, WA = weight of Nitrobenzene
ρA = Density of Nitrobenzene
VA = Volume of Nitrobenzene
2. WB = ρB * VB
where, WB = weight of Water
ρB = Density of Water
VB = Volume of Water
3. WA / WB

4. As par Henry’s law,

WA / WB = PA * MA / PB * MB
where, PA = vapor pressure of nitrobenzene
PB = vapor pressure weight of steam
MA = molecular weight of nitrobenzene
MB = molecular weight of water

5. L.H.S. = WA / WB

6. R.H.S. = PA * MA / PB * MB

RESULT:- (1) Experimental ratio of distillate =

(2) As per Henry’s law,
Theoretical ratio of distillate =

CONCLUSION:_____________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________

QUESTION:-
1. Instead of ordinary methods of distillation why do you go for
 Steam Distillation or What is the principle of steam distillation?
2. What kind of steam are you used for steam distillation?
3. What are advantage & disadvantage of steam distillation?

EXPERIMENT NO: DATE:

HUMIDIFICATION

AIM:- To study the humidification operation and calculation all the

terminology’s used for air – water contact operation.
THEORY:-
Psychometric refers to the systemized knowledge of the properties of air
and water but it also includes the principles which govern the properties
and behavior of mixtures of the so called “fixed gas” with condensable vapors.

Knowledge of the water vapor content of air under various conditions of

temperatures and pressure and the properties of these mixtures is very
important in many unit operations and transport processes. When this air –
water vapor mixtures comes in contact with water or wet solids many changes
occur, with simultaneous mass and heat transfer between the phases.

Humidification operations refers to an operations in which transfer of water

occurs form a liquid phase to a gaseous mixture of air and water vapor, while in
dehumidification the reverse process occurs, i.e. water vapor is transferred from
the vapor to the liquid state.
Air –conditioning units used in home and business houses are the most
examples of these two operations.
The most convenient method of handing psychometric relationships is
application of humidity chart or psychometric chart with is simply plot of the
properties of the mixtures under considerations at a specified total pressure.
Usually at one atmosphere.
The common terminologies used for air –water contact operations are listed
below.
Absolute humidity:-
The ratio of mass of vapor to mass of gas is termed as “absolute humidity (Y’)”.
Saturated Mole Absolute Humidity :-
If an insoluble dry gas B is brought into contact With sufficient liquid B, the
liquid will evaporate into the gas unit ultimately. At equilibrium The partial
pressure of a in the vapor – gas mixture reaches its saturation value, the vapor
part the prevailing temperature.

Dry bull temperature:-

Temperature of a vapor – gas mixture as ordinarily determined by immersion of
a thermometer in the mixture is called as “Dry bulb temperature.”
Relative saturation:-
It is defined as the ratio of partial pressure of water vapor in the air to the
saturation vapor pressure of water at the dry bulb temperature of the mixture.
% saturation:-
It is defined as the as the ratio of absolute Humidity ( or molal absolute
humidity ) to saturated absolute humidity ( or molal saturated absolute
humidity).
Dew point:-
It is the temperature at which a vapor gas mixture becomes saturated when
cooled at constant total pressure out of contact with a liquid.
Humid volume:-
The humid volume (VH) of a vapor gas mixture is the volume of unit mass of dry
gas and it accompanying vapor at the prevailing temperature and pressure.
Humid Heat :-
humid heat (CS) is the heat required to raise the temperature of unit mass of gas
and its accompanying vapor by one degree at constant pressure. Fox a mixture of
absolute humidity
Wet bulb temperature:-
Wet bulb temperature reached by a small amount o liquid evaporating in a large
amount of a large amount of unsaturated vapor gas mixture.
To measure it, the surface of a thermometer bulb is kept wet by a wick or cloth
thoroughly saturated with water. The thermometer with wetted bulb gives the
equilibrium temperature which is note as wet bulb temperature.
Wet bulb temperature is always less then or equal to dry bulb temperature.
Adiabatic saturation temperature :-
 Adiabatic process is one in which there is no transfer of heat between the system
and the surround but during it thermal changes usually occur within the system.
When a define quantity of water is allowed to evaporate in a stream of gas
adiabatically, the dry bulb temperature of the gas drops While humidity will

increase. The final temperature of the intimately mixed stream is called “adiabatic
saturation temperature
Enthalpy:-
The enthalpy (H’)of a vapor gas mixture is the sum of the enthalpies of the gas
and the vapor content.

PROCEDURE:- Note the DBT and WBT and calculate the properties defined
above.
OBSERVATION:-
Dry bulb temperature = --------------0C.
Wet bulb temperature = --------------0C.
CALCULATIONS:-

 Absolute Humidity=

 Dew point =

 Molal absolute Humidity (Y) =

 Partial pressure of water vapor in the sample (P A) =

 % relative Humidity =

 Humid Volume (VH) =

 Humid Heat (CS) =

 Enthalpy (H’) =
RESULT:-

 Absolute Humidity (Y’) =

 Dew Point =
 Molal Absolute Humidity (Y) =
 Partial pressure of Water Vapor in the sample (PA) =
 % relative Humidity =
 Humid Volume (VH) =
 Humid Heat (CS) =
 Enthalpy (H’) =

CONCLUSION:_____________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________

QUESTION:-
1. Differentiate vapor & gas.
2. Define following terms:
a) Dry bulb thermometer.
b) Wet bulb thermometer.
c) Dew point..
3. Why the wet bulb temp is lower than dry bulb temp in our
experiment. Explain the phenomena in detail.
EXPERIMENT NO: DATE:

DIFFERENTIAL DISTILLATION
AIM:- To verify Rayleigh’s equation for differential distillation
CHEMICALS:- Benzene, Toluene
THEORY:-

Infinite number of flash vaporization of the liquid gives small portion of the
liquid infinite times during overall flashing and the net result would be
equivalent to a differential, or simple distillation.

Simple or different distillation is used to get high at the expense if a lowered

distillate concentration. If a relatively small amount of a highly volatile
component is to be recovered from the bulk of a component of low volatitility, it
performs very well.

PROCEDURE:-
1. Arrange the assembly as shown in the figure.
2. Charge 50 mol % benzene & toluene mixture in round
bottom flask.
3. Start heating at lower rate.
4. Note down the temperature at which distillate collected from
condenser.
5. Collect approximately 50 ml distillate and note down the
temperature on 50 ml collection of distillate.
6. Take the sample from distillate for analysis on refractometer or
by specific gravity bottle.
CALCULATION:-
Therefore,
Y*dL = Ldx + xdL

F=D+W

In F/W = dx / (y* - x)

FxF = Dy d,av + W xw

XF = Xw =

For 100ml, V = Volume of a + volume of B

 L.H.S.= ln F/W =
R.H.S = dx / (y* - x) =

PLOT:- Area under curve 1/(y* - x) v/s x

RESULT:-

CONCLUSION:_____________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________

QUESTION:-
1. What is destination
2. Explain dictation is varietal process
3. Industrial application differntaion application

EXPERIMENT NO: DATE:

VAPOR-LIQUID EQUILIBRIUM
AIM:- To generate Vapor-Liquid Equilibrium Data by specific Gravity
method.

APPARATUS:- VLE Apparatus, Measuring cylinder, Specific gravity bottle, Beakers,

MATERIAL:- Benzene & Toluene.
THEORY:-
The more the difference between the diagonal line and
the equilibrium curve, the separation will be easier by distillation.
Property detecting this difference is termed as (α).

If y* = x [except at = 0 or 1], then α will be unity and in this case

separation is not possible. The larger the value of α the degree of
separation will be more.

PROCEDURE:-
 Prepare about 200 ml sample by taking two miscible components
(Benzene + Toluene) in 50:50 composition (Vol % ) & pour into RBF
using feed neck.
 Replace the feed neck topper & switch on the heating mantle.
 Start the cooling water supply in both the condenser.
 After sometime condensed vapor will be colleted in the collection bulb
below the second condenser.
 Keep the recycle valve of the collection bulb open. Then allow the
material to flow back into the RBF via a deeped line.
 Empty out the collected bulb after half an hour of recycling & pour
it back to the RBF immediately.
 Take out the sample of liquid & condensed vapor by opening the
valve provided at the bottom of the RBF & collection bulb
respectively after an hour.
 Steady state in the system can be judge by constant temp. values T1 &
T2.
 Find out the density of sample with the help of the specific gravity
bottle.
 Repeat the procedure for (benzene + toluene) in 70:30 composition.
 Compare theoretical and graphical points.
Data:-
Sr. no. Composition (Vol %) Sp. Gravity
 Benzene Toluene
1 10% 90% 0.975
2 20% 80% 0.962
3 30% 70% 0.946
4 40% 60% 0.935
5 50% 50% 0.928
6 60% 40% 0.918
7 70% 30% 0.912
8 80% 20% 0.895
9 90% 10% 0.883
10 100% 0% 0.869

OBSERVATION:- Weight of Specific Gravity bottle =

Weight of Benzene + Sp. Gravity bottle=

Volume of Benzene =

Weight of Toluene + Sp. Gravity bottle=

Volume of Toluene =

Weight of Benzene + Toluene(50%) mixture =

Weight of distillate – Sp. Gravity bottle =

Density of distillate of mixture=

Density of residue (bottom product)=

CALCULATIONS:-

Composition of distillate =

Composition of residue (bottom product) =

GRAPH:- Plot a graph of mole fraction of distillate v/s temperature and

fraction of residue (bottom product) v/s temperature.
RESULT:-

Composition of distillate=

Composition of residue (bottom product)=

CONCLUSION:_____________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________

QUESTION:-
1. What is relative volatility? Give its significance?
2. What is significance of VLE and boiling point diagram in
distillation?

4. Calculate the equilibrium data of a system where

relative volatility is 2.5 and constant?
5. State and Explain Raoult’s law with application?