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CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 1 of 13

1 What is Refractive index?
2 Where in a distillation column is the
temperature the lowest?
a) At the bottom of the column, because the heat rises
to the top due to natural convection of the hot gas
flow.
b) At the feed position, because the stream has to be
cooled down before entering the column.
There are no temperature differences over the whole
column.
At the top of the column. In fact the more volatile
components (lower boiling point) are withdrawn at
the top of the column.
3  What is the effect of the pressure inside the
distillation column?
The pressure affects the internal flow-rates of
the column. Therefore in order to simplify the
calculation, with the CMO assumption (i.e.
constant internal flow-rates) we assume also
that the pressure is constant all over the column.
The pressure affects the vapour pressure of the
feed mixture. Therefore the higher the pressure,
the purer the distillate.
Pressure affects the vapor-liquid equilibrium,
therefore also the degree of separation obtained
in the distillation process depend on the
pressure set.
CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency
1 If you assume CMO and do all the calculations, but CMO is
not true, what happens?
a)The efficiency of the column will be reduced
b) The L and V flow-rates in the column are different at
every stage. The McCabe-Thiele method cannot be applied
anymore. A punctual design considering every single stage
of the column must be done in order to calculate the
distillation products.
c) No effect. The CMO is only an assumption to simplify
the calculations during the process design and has no
influence on the functionality of the column.
d) Raoult's law is also not valid anymore.
2 Which are the products of a distillation column
which has an infinite reflux ratio?
a) There is no Distillate production: everything is
withdrawn at the bottom.
b) There are no products and, at steady state, also feed
rate is zero. The number of stages is the minimum
possible.
c) The column runs normally since the products are only
feed dependent.
d) The infinite reflux ratio is only a "trick" for calculation
purposes. It has no physical meaning therefore it cannot
be used with a real column.
3) What happens in a distillation column if the reflux
ratio is zero?
a. If no liquid is recycled back to the column,
the internal liquid and vapour flow-rates
can not be controlled and the design of the
column gets more difficult.
b. In this case a partial condenser should be
used since we don't need any liquid for the
recycle.
c. The entire product is withdrawn as Distillate
and moreover we save the investment costs
for recycle piping and pump. This is the best
configuration possible for a distillation
column.
d. No liquid is recycled back to the column.
Step by step the only vapour phase will be
present in the rectification section and no
mass transfer is possible anymore.
Total Marks
Page 2 of 13
 Determine the Overall Column Efficiency on a Continuous Plate
Distillation Column operation at total reflux

1. Objective:
To calculate the number of theoretical plates for the given separation at total reflux

2. Theory: Formula: FENSKE’s Method

x D ( 1−x B )

N min =
ln
( x B ( 1−x D ) )
ln α AB
OR
log ❑[ XA ∈top product . XB ∈bottoms product ]
( )
XB XA ( )
n+1 = ________________________________________________________

α
Log av

Where Nmin = Minimum number of theoretical plates

XD = mole fraction of more volatile component in the distillate (Top Product)

XB = mole fraction of the more volatile component in the Bottom product.

α
AB =average relative volatility

Subscripts DB indicate the distillate and bottoms respectively

α
av = √ αD . αB
The efficiency is given by
Number of Theoretical plates
E= x 100
Number of Actual plates

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 3 of 13

 Mass ofMethanol
Mass Fraction =
Mass of Methanol + Mass of water

Mass of Methanol
MW of Methanol
Mole Fraction =
Mass of Methanol Mass of water
+
MW of Methanol MW of water

Methanol = CH3OH
Water = H2O

3. Equipment:
1. Continuous Plate Distillation Column (you need a sketch for this)
2. 250 ml measuring cylinder
3. Stop watch
4. Refractometer.
See the attached notes for equipment details and operation

ATAGO ABBE Recfractometer - DR-A1

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 4 of 13

 Eye piece

Display

View finder

Sample compartment

What is "refractometer"?
When a chopstick is dipped in water in a glass, it looks bent. If the chopstick is dipped in thick sugar
water, it looks bent much more. This phenomenon arises from "refraction of light beam". Applying this
principle (with increase of solution in concentration, the refractive index becomes high in proportion
to it) to practical use, Dr. Ernst Abbe (German) first devised the refractometer at the beginning of the
20th century.

What is "refractive index

The refractive index n of an optical medium is defined as the ratio of the speed of light in vacuum,

c = 299792458 m/s, and the phase velocity v of light in the medium, [1]n=c /v

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 5 of 13

4. Safety:
Students must wear goggles, laboratory coats and hand gloves during practical classes.

5-a. Procedure (Refractometer):

1) Switch on the refractometer

2) Open the lid of the sample compartment, clean the quartz surface with fibreless tissue socked in

acetone. Leave it to dry

3) Add a few drops of pure known component over the Quartz surface.(never use glass dropping

pipettes!)

4) Adjust the view finder to match the boundary line appearing in the refraction field of

vision with the intersection point of the cross line.

5) As this knob is turned, the refractive index (nD) appearing in the display continuously changes

and the measurement value is displayed when the boundary line and the intersection point of

the cross line match with each other.

6) Record the nD of the pure component and refer it with nD of standard component.

7) Open the lid, clean the surface with fibreless clean tissue soaked in acetone. Leave it to dry

8) Add a few drops of the sample to be tested over the quartz surface, adjust the view finder to

match, record the refractive index (nD) of the sample.

9) Open the lid, wipe the surface with fibreless tissue followed by acetone socked tissue.

10) Close the lid switch off the power.

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 6 of 13

5-b. Procedure:

a) Make calibration curve of Methanol/water mixture at different composition.

b) Plot the Calibration Curve for Methanol – Water Mixture

c) The equipment will be set up to operate at total reflux so the charge of feed mixture can be loaded
directly into the re boiler through the filler cap provided without first charging the feed tank. At total
reflux there will be no feed or top product or bottom product.

d) Make up 10 liters of mixture of 50 mole percent Methanol and 50 mol percent water.

e) Prepare a calibration graph for ethanol water mixture for reference using refractometer

f) Note: Three way distillate receiver (C1) can be used to take the boil up rates. While total reflex not in
operation, the condensate will be collected in top product receiver.

g) Fill the boiler with 10 liter Methanol/Water mixture.

h) Set the heater controller high at first and then reduce heat as reflux is introduced to give steady
bubbling on all trays and total reflux.

i) Leave the apparatus for 30 minutes so that the system can reach equilibrium condition.

j) Using valve C1, record three different boil up rates and take the average.

k) Take the sample of the overhead through valve C1 and record the refractive index

l) Record the temperature T5 and T6 to calculate the average column temperature

m) Repeat this procedure for several different boil up rates to cover the operating range of the column.

n) The calibration graph can be used to determine the concentrations of the components

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 7 of 13

6. Readings and Calculations:

Temperature Location Temperature ° C

Top Tray Temperature T1

Bottom Tray Temperature T8

Select the heating value in the Reboiler:

Bottom Tray Top tray Bottom
Heat input Boil up rate Overhead
Temperature Temperature °C composition R2
KW Liters / hour composition RI
°C @ T8 @ T1

0.65

0.75

0.85

0.95

0.105

Composition of Methanol in Water by Mole fraction

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 8 of 13

 Volume Of Volume Of Total Volume(g) Refractive Index
Methanol(g) Water(g)
0 30.0019 30.0019 1.334
4.9612 25.1371 30.0983 1.3379
10.4179 20.0961 30.514 1.3419
14.9032 15.1198 30.023 1.3433
19.9421 10.0031 29.9452 1.3418
25.0047 5.0154 30.0201 1.3317
26.1635 4.1856 30.3491 1.3358
27.227 2.776 30.003 1.3348
28.226 2.1671 30.3931 1.3341
29.1643 1.1125 30.2768 1.3331
30.1018 0 30.1018 1.3296

Mole fraction of Methanol in water

32 18
total moles of Methanol
Mass of Moles of water and Mole
Mass of methanol moles of methanol water water methanol fraction nD
0 0 30.0019 1.666772222 1.666772222 0 1.334
4.9612 0.1550375 25.1371 1.396505556 1.551543056 0.099924717 1.3379
10.4179 0.325559375 20.0961 1.11645 1.442009375 0.225767863 1.3419
14.9032 0.465725 15.1198 0.839988889 1.305713889 0.356682275 1.3433
19.9421 0.623190625 10.0031 0.555727778 1.178918403 0.528612178 1.3418
25.0047 0.781396875 5.0154 0.278633333 1.178918403 0.662808277 1.3382
26.1635 0.817609375 4.1856 0.232533333 1.050142708 0.778569778 1.3358
27.227 0.85084375 2.776 0.154222222 1.005065972 0.848758398 1.3348
28.226 0.8820625 2.1671 0.120394444 1.002456944 0.879900633 1.3341
29.1643 0.911384375 1.1125 0.061805556 0.973189931 0.906362132 1.3331
30 0.9375 0 0 0.9375 1 1.3296

             

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 9 of 13

 Mole Fraction of Methanol in Water
1.35

1.34

1.34

Refractive Index

1.33

1.33

1.32
0 0.2 0.4 0.6 0.8 1 1.2

Methaol Mole Fraction

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 10 of 13

 a) Using the formulae given in page3, calculate the number of theoretical plates

b) Column efficiency

Lab report Format and Marking Scheme

1. Objectives 5%
 Purpose of experiment
 Possible outcomes results of experiment

2. Introduction & Theory 10 %

 Introduction to the topic and purpose of the experiment
 Explanation of the relevant theory in detail, including relevant laws, equations or theorems
CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 11 of 13
  Indication of the methods that will be used for analysis

3. Apparatus and Resources 5%

 List no. of chemicals , Equipment’s

4. Procedure 10%
 Write step by step procedure in detail

5. Experimental Data/ Readings 10%

 Data table
 Formulas , calculations

6. Results and Calculations 20%

 Use Formula in lab report to calculate number of theoretical plates
 Calculate column efficiency

7. Discussions 25%
 Discuss the results you obtained;
1. Determining the effect of power and temperature in column efficiency
2. What will be effect if number of plates increase or decrease?
 Compare the expected and experimental results
 Explain any unexpected results

8. Conclusions 10%

This section will summarize the key results and discussion points.

 Indicate to what extent the aims of the experiment were achieved.

 Summarize the main points of the findings including key values.
 Summarize important limitations and the cause of unexpected results.
 Recommend improvements to overcome experimental limitations.

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 12 of 13

9. References 5%

CHE 3323_Mass Transfer_Lab04_Determination of Column Efficiency Page 13 of 13