Beruflich Dokumente
Kultur Dokumente
2013-14
SIMPLE DISTILLATION
Aim:
Apparatus required:
Simple distillation setup, measuring jar, specific gravity bottle and beaker.
Theory:
In simple distillation, a batch of liquid is charged to a kettle or flask fitted with some
sort of heating device. the charge is boiled slowly and the vapors are withdrawn as rapidly
as they form in a condenser where they are liquefied and the distillate collected in the
receiver the vapor leaving the flask at any time is in equilibrium with the liquid in the flask,
but since the vapor is richer in the more volatile component , the composition of liquid and
vapor are not constant .the first portion of the distillate will be the richest in the more
volatile component and as distillation proceeds ,the vaporized product become leaner, the
distillate can therefore be collected in several separate batches to give a series of distilled
product of various purity.
Rayleighs equation is:
ln F / W
xF
xW
dX
Y X
*
Procedure:
1) Take 200 ml of component A (Acetone) and 100ml of component B (Water) in the
distillation flask and heat over a heating matter.
2) Carry out the distillation until 2/3rd of the mixture get distilled.
3) Collect the distillate in conical flask.
4) Find out the volume of distillate.
5) Cool the residue to room temperature.
6) Find out the volume of the residue.
7) Find out the density of residue using specific gravity bottles.
Observation:
Volume of Acetone taken
ml
ml
Density of Acetone
g/cc
Density of Water
g/cc
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Tabulation: 1
Calibration Chart:
S.
No.
Volume in ml
Aceton
e
Water
Weight in g
Sp. gr. Bottle
+ Sample
Mole fraction of
Sampl
e
Acetone
Refractive
Index/Specific
gravity of Acetone
Water
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
Calculation:
Weight of Acetone
Weight of Water
Total Moles
ml
ml
Density of Residue
g/cc
From the graph Specific Gravity (Y-axis) vs. Mole Fraction of Acetone (X-axis),
Mole fraction of Acetone in Residue, Xw =
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Tabulation: 2
VLE data for Acetone-Water system:
(Refer Chemical Engineering Handbook by Robert. H Perry & Don Green, 6th edition, Page
Nos: 13.11-13.12 & 13.21)
S.
No.
Y*
Y* - X
1/(Y* - X)
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
Verification:
Rayleighs equation is
ln F / W
xF
xW
dX
X
From graph X (y-axis) vs. 1/(Y* - X) (x-axis), find the area under the curve between
XF and XW. That is,
xF
xW
dx
Y* X
RHS =
Check LHS=RHS
=
LHS = ln (F/W) =
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Analytical Method :
ln (F/W) = ln [(xD xR)/(xD xF)]
Result:
Thus Rayleighs equation is verified.
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DIFFUSIVITY MEASUREMENT
AIM
To determine the diffusion coefficient of organic vapor in air at various temperatures.
APPARATUS
Diffusivity cell, stop watch.
THEORY
Some liquid 'A' is taken in a diffusivity cell. The concentration of liquid vapour just
above liquid surface is the vapour pressure of the liquid. If a stream of air is being drawn
along the top edge of the cell, the concentration of liquid vapours there is determined by the
amount of liquid vapour present in atmospheric air. The diffusion that occurs in this case is
diffusion of acetone (A) through stagnant air (B). Since the height of the liquid in the cell is
not maintained constant, a Pseudo Steady State diffusion model may be used.
According to this model ,
D AB=
R T 0 a PBM (X X )
2
2
0
2 P M A t (P A 1P A 2)
Where
D AB = Diffusivity of A in stagnant B, m2/sec.
T0
= Operating temperature, oK
P BM
P
MA
PA1
PA2
t
X & X0
DESCRIPTION:
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Water bath is
controller. Stirrer is given to maintain the constant temperature bath. Air pump is provided
to supply the air, passed through the tube. Change in the liquid level is observed by the
travelling microscope with sliding vernier scale.
PROCEDURE
o
o
o
o
o
o
o
the bath
Fill the T-tube with acetone solution up to two centimeters of the capillary leg.
Note down the initial height of liquid in the capillary
Make the connection with air pump and allow a gentle current of air to flow
o
o
o
DATA:
OBSERVATIONS
T = ______________
X0 = ______________
OBSERVATION TABLE
Sl.No.
t (min)
X (cm)
Calculation:
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A =
kg/m3
x= X0/100 (m) (initial height of liquid at t1 = 0)
x = X/100 (m)
t1 = t 60 (sec)
T0 = 273 + T (K)
PA1 =
( A
D AB=
B
)
C +T
(mm Hg)
R T 0 PBM ( X X )
2
2
0
2 P M A t ( P A 1P A 2 )
Calculation Table:
S.No
t1 (sec)
x (cm)
RESULTS
Diffusivity of the given organic liquid in air is calculated.
(2)
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(4)
(5)
(6)
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Utilities required:
Forced draft tray dryer, Drying solids: sand/asbestos/silica.
THEORY
In many cases, drying of materials is the final operation in the manufacturing
process, carried out immediately prior to packaging or dispatch. Drying refers to the final
removal of water, and the operation often follows evaporation, filtration or crystallization.
Drying is carried out for one or more of the following reason:
1. To reduce the cost of transport
2. To make a material more suitable for handling
3. To provide definite properties
4. To remove moisture this may otherwise lead to corrosion.
Drying of solids is considered to occur in two stages, a constant rate period followed
by a falling rate period. In the constant rate period, the rate of drying corresponds to the
removal of water from the surface of the solid. The falling rate period corresponds to the
removal of water from the interior of the solid. The rate in either case in dependent on:
Flow rate of air, The solid characteristics and Tray material.
The drying rate of a solid is a function of temperature, humidity, flow rate and
transport properties of drying gas. The rate of drying can be determined for a sample of a
substance by suspending it over an electronic balance in the duct. The weight of the drying
sample can then be measured as a function of time.
Let Ws is mass of solid A is drying area, x is moisture content at any time t. The rate of
drying is given as:
N = - (Ws x)/ (A t)
Where x is moisture content difference and t is time difference.
PROCEDURE:
o
o
o
o
o
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Using stop watch check the balance reading at every 3-5 minutes interval.
Continue the experiment till three consecutive reading are unchanged.
Repeat the experiment for different solid material and different air flow rate.
OBSERVATIONS:
Data:
TABULAR COLUMN:
S.No
t (sec)
w (kg)
R (m)
Calculations:
Xt = Ww W/W
W=
kg (Final value of w)
X* = Ww W* / W
X* = Xt X*
X = Xn Xn+1
t = tn+1 tn (n=1,2,3.)
Calculation Table:
S.No
t (min)
t (min)
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a0 = /4
do
m2
ap = /4
d 2p
m2
H = R (w/a-1) m
Qa = Cd
G = Qa
S.No
ao a p
2
p
ao
2 g H
m3/sec
a kg/sec
N (kg/sec m2)
G (kg/sec)
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t (sec)
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RESULT
SIMPLE LEACHING
AIM
To plot the theoretical and actual recovery Vs solvent feed ratio.
APPARATUS
Measuring jar, conical flask, burette, pipette, beaker and stirrer
THEORY
Leaching is the process of removal of a solute or solutes form a solid by the use of a
liquid solvent. It originally refers to the percolation of liquid through a fixed bed, but it is
also used to mean solid liquid extraction generally.
distinguishes it from liquid extraction. Two steps involved in solid liquid extraction are :
1. Contact of solid and solvent to effect transfer of solute to the solvent and
2. Separation of the resulting solution from the residual solid.
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FORMULA
Y1 = Volume of extract = volume of NaOH* normality of NaOH
Volume of extract
Theoretical recovery =
50/50 = 1
X1 = (Y1 * 53 * 50 )/1000
2. 100/50 =2
X2 = (Y2 * 53 * 50 )/1000
3. 150/50 =3
X3 = (Y3 * 53 * 50 )/1000
4. 200/50 =4
X4 = (Y4 * 53 * 50 )/1000
5. 250/50 =5
X5 = (Y5 * 53 * 50 )/1000
% Actual recovery = (X / 5) * 100.
PROCEDURE
About 45 gm of sand and 5 gms of oxalic acid and 100 ml of distilled water are taken
as feed in each of the five beakers.
stirred well, allowed to settle. From the supernatant solution 10 ml is pipetted out and is
made upto 100 ml. 10 ml of this solution is used for titrating against 0.2 N NaOH. Sodium
hydroxide is standardised using 0.1N oxalic acid. Then 100 ml of water is added to the
second beaker and the same procedure is repeated. Likewise 150 ml, 200 ml of distilled
water is added respectively to third, fourth and fifth beakers and the same procedure are
repeated.
From this, actual recovery, theoretical recovery and solvent feed ratio are calculated.
A graph of percentage actual recovery and percentage theoretical recovery Vs solvent feed
ratio was plotted.
STANDARDISATION OF SODIUM HYDROXIDE:
Volume of
sodium
hydroxide, ml
Burette reading in ml
Initial
Final
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Volume of Oxalic
acid, ml
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Normality of
Sodium Hydroxide
Bottle
Volume of
number
extract
20
20
20
20
20
2013-14
Burette readings in ml
Initial
Final
Volume of
Normality of
NaOH (ml)
extract N
RESULT
The theoretical, actual recovery Vs solvent feed ratio was calculated and a graph was
also drawn.
Y
X
%
Recovery
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Burette reading
Initial
Final
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Volume of oxalic
acid used
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Strength of NaOH
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Volume of NaOH
Stage Number
RESULT
The result obtained were compared by leaching a given feed
1. Number of stages used
= ___________
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To the first beaker 300 ml of distilled water was added. The contents are stirred well and
allowed to settle. Similarly 150 ml of water added to second beaker and 100 ml of water to
the third beaker respectively.
After the sand particles have settled the clear supernatant liquid was decant into the
corresponding beaker.
The procedure is repeated again with 150 ml of water in second beaker and 100 ml of water
in third beaker.
Finally again 100 ml of distilled water is added to the third beaker.
20 ml of makeup solution from each beaker was titrated against standard HCl.
The amount of Sodium carbonate was calculated in each stage.
Calculation Procedure:
Volume of leached solution V2 = 20 ml
Normality of HCl N1 = 1 N
Stage I:
Volume of HCl added V1 =
ml
Volume of leached
Volume of
Burette reading ml
Volume of HCl
solution in ml
extract in ml
Initial
in ml
Final
Result:
Stagewise leaching experiment was performed and percentage extraction was calculated.
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LIQUID-LIQUID EXTRACTION
Aim:
To carryout liquid-liquid extraction for extracting acetic acid from water using solvent and to
find the distribution coefficient and percentage of extraction.
Apparatus Required:
Conical flask, Separating funnel, Burette, Pipette, Measuring Jar
Formulae Used:
Distribution coefficient: Kd = Cd / Cn
Cd Concentration of extractable in organic phase
Cn - Concentration of extractable in water phase
Procedure:
Prepare 1N acetic acid solution and 0.1N NaOH solution. 40 ml of acetic acid and 20 ml
of solvent is taken in a separate flask and stirred using rotary shaker for 15 minutes. Then
the mixture is allowed to separate as layers and pour it into a separating funnel.
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bottom layer raffinate was measured and 20 ml of it is pipette and titrated against NaOH
solution. From the titration value distribution coefficient and % extraction were calculated.
Calculation procedure:
Before extraction:
1. Amount of acetic acid in 40 ml solution of 1N = (Volume of acetic acid Equivalent
weight of acetic acid Normality of acetic acid / 1000)
After extraction:
2. Normality of acetic acid V1 N1 = V2 N2
3. Amount of acetic acid in 40 ml = (Volume of acetic acid Equivalent weight of acetic acid
Normality of acetic acid / 1000)
6. Distribution coefficient =
Result:
The distribution coefficient and % extraction of various solvents were calculated.
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ROATARY DRYER
OBJECTIVE
To study the operation of rotary dryer.
AIM
To calculate the rate of drying for different air flow rates and different air inlet temperatures.
To plot the rate of drying curve.
Theory:
In many cases, the drying of materials is the final operation in the manufacturing process,
carried out immediately prior to packaging or dispatch.
Drying is
stuffs, fertilizers.
To provide definite properties, such as maintaining free flowing nature of salt.
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To remove moisture; which may otherwise lead to corrosion, for example, the drying
of coal gas or benzene prior to chlorination.
Almost all drying processes involve the removal of water by vaporization, & thus require the
addition of heat.
The rotary dryer is a type of industrial dryer employed to reduce or minimize the liquid
moisture content of the material by bringing it direct contact with a heated gas. The dryer
is made up of large rotating cylinder which slopes slightly so that the discharge end is lower
than the material feed end is order to cover the material under gravity. Material to be dried
enters the dryer as the dryer rotates, the material is lifted up by a series of internal fins
lining the inner wall of the dryer. Heating option include steam, gas, oil, thermal oil, and
auxillary biomass burner system.
Consider a rotary continuous direct heat counter current dryer fed with a nonporous
material having all moisture as unbound moisture. As this material enters the dryer, it is
first heated to the drying temperature.
nearly the wet-bulb temperature and theoretically at the end of the dryer, the material shall
be discharged as dry material nearly at the wet bulb temperature.
Assumptions:
shell.
All the moisture present is free moisture.
There is no evaporation of moisture in the preliminary heating period.
Drying proceeds at a constant wet bulb temperature until desired amount of water has been
removed. The entering air is assumed to be 100% saturated, so its temperature needs to
be raised so as to decrease the relative saturation.
moisture from the wet solid feed. In turn the exiting air is more saturated than the entering
one.
For continuous dryer at steady state operating conditions,
F(X1 X2) = G (Y1 Y2)
This assume that the dry gas flow G and dry solids flow F do not change between dryer inlet
and outlet. Mass balances can also be performed on the overall gas and solids entrainment
in the exhaust gas stream.
The required solids flow rate, inlet moisture content X1 and outlet moisture X0 are normally
specified, and the evaporation rate and outlet gas flow are calculated.
For batch dryer with dry mass m of solids, a mass balance only gives a snapshot at one
point during the drying cycle and an instantaneous drying rate given by:
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m2
0.026 m
0.052 m
0.64
9.81 m/sec2
1000 & 1.21 kg/m3
29 & 18 g/mole
Observations:
Z0 =
kg
Z=
W=
kg
kg
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T=
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sec
S.No
T1 (C)
T2 (C)
T3(C)
T4 (C)
h1 (cm)
Calculations:
H=
h1 h2 w
1 m
100 a
a1= d 2P ( m2)
4
a2= d 2o ( m2 )
4
Q a=
G=
a1 a2
a a
2
1
2
2
C d 2 g H
a Q a
( kg/m2 sec )
A
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S.No
t (sec)
N ( kg of moisture / m2 sec)
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