MT 304 – Gas Liquid Absorption

CL 333 Chemical Engineering Lab-III [2021]

Group B4a
Members:
Jyotirmoy Roy 180020044

Saksham Gautam 180020088

Yukti Yashogupta 180020125

Raghav Ghanshyamdass 180020071

Guide: Prof. Bharat Kumar Sunthar

Department of Chemical Engineering, Indian Institute of Technology, Bombay

October 04, 2021
 Experiment Number MT 304

Title Gas Liquid Absorption

Sub-group Code A4a

Date of Experiment 1st October 2021

Date of Report Submission 4th October 2021

Roll Number Name Responsibility owned

(data, analysis, plots, report,
none)

180020044 Jyotirmoy Roy Observation,Hypothesis,

and Conclusions

180020088 Saksham Gautam Calculations and Error

Analysis

180020125 Yukti Yashogupta Introduction and

Procedure

180020071 Raghav Ghanshyamdass Data Analysis

(For use by examiners only)

Criterion TA Grade Faculty assigned grade

Data analysis

Graphical plots

Inference

Report quality

Bonus marks (Y/N)

Initials with date

R&P TA initials with date

 Contents

1. Objective _________________________________________________4

2. Theory____________________________________________________4

3. Procedure_________________________________________________5

4. Experimental Setup_________________________________________6

5. Results from Experimental Data ______________________________7

6. Sample Calculations_________________________________________9

7. Observations_______________________________________________12

8. Hypothesis_________________________________________________13

9. Conclusion_________________________________________________13

10. Special Question____________________________________________13

Objectives:

To study and compare the yield of reaction between carbon dioxide (CO2) and hydroxide
(NaOH) solution in an absorption column and a bubble column.

Apparatus:

Gas Liquid Absorption set up

Theory:
Gas-Liquid absorption is a separation process where particles from a gaseous mixture
are dissolved into a liquid solvent. Here, the gaseous mixture contains air and carbon
dioxide (CO2) whereas the liquid is sodium hydroxide (NaOH).

There are two kinds of absorption:

1. Physical Absorption- No chemical reaction occurs in this case. The gaseous
component is more soluble in the liquid and hence, is absorbed.
2. Chemical Absorption- A chemical reaction occurs between the gaseous
component being absorbed and the liquid absorbent.

In the absorption column, the liquid (NaOH in excess) enters from the top of the column
and the CO2+air mixture enters the column from the bottom. The absorption column is
packed with Raschig rings. These help in increasing the surface area and ensuring
efficient absorption.

This is a case of Chemical Absorption. The following reaction occurs:

2NaOH + CO2 → Na2CO3 +H2O

First equivalence occurs when H+ ions react with the OH- ions in excess and with the
CO3 -- ions as follows:
CO3 -- → + H- HCO3-
OH- + H+ → H2O
From the above reaction, we can say that the moles of bicarbonates formed = moles of
carbonate ions present. That means n (HCO3- formed) = n (CO3-- present)
Also, n (H+ ) = n (OH- ) + n (CO3--)
The second equivalence occurs when the bicarbonate HCO3 - ion reacts with the H+
ions as follows: H+ + HCO3- → H2CO3
The phenolphthalein indicator used in this reaction has only one H+ ion. Hence, we
achieve only one equivalence. Whereas the methyl orange indicator has two H+ ions
and we achieve both the equivalences.

Procedure:

1. Switch on the apparatus.

2. Prepare 20 liters of 1.5 N NaOH and check the concentration of the feed solution
by titration against 0.1N HCl.
3. Fill the bubbling pot with 3 liters of NaOH solution and check the concentration
similarly.
4. Set the flow rates of NaOH, CO2, and air as 10 L/H, 70 L/H, and 720 L/H
respectively.
5. Take out samples at 10, 20, and 30 minutes from both columns.
6. Titrate the collected sample against 0.1 N HCl using the phenolphthalein
indicator.
7. Repeat the same with the methyl orange indicator.
8. Calculate balance on NaOH and CO2.

Experimental Setup:

Figures 1 & 2: Diagrammatic Actualand Experimental Setp

Raw Data

Absorption Column

Flow Rate of CO2 (Litre/hr) Time (min) v1(ml) v2(ml)

70 10 14 17
70 20 12.6 15.7
70 30 14.2 17.4
90 10 10 12.8
90 20 11.2 14.3
90 30 13.1 15.8

Bubble Column

Flow Rate of CO2 (Litre/hr) Time (min) v1(ml) v2(ml)

70 10 17 17.5
70 20 15.5 16.2
70 30 16.5 17.2
90 10 12.5 13.2
90 20 17.5 18
90 30 12.5 13.8
 Results from Experimental Data:

Table 1 : Yield for Absorption Column

Absorption Column
Conc of NaOH
NaOH CO2
Flow rate of Time at outlet CO2 fed
v1 (ml) v2 (ml) reacted reacted Yield (%)
CO2 (L/h) (min) (10^-3 (mol/hr)
(mol/hr) (mol/hr)
mol/m3)
70 10 14 17 1.10 4.00 3.125 2.00 64.00
70 20 12.6 15.7 0.95 5.50 3.125 2.75 88.00
70 30 14.2 17.4 1.10 4.00 3.125 2.00 64.00
90 10 10 12.8 0.72 7.80 4.018 3.90 97.07
90 20 11.2 14.3 0.81 6.90 4.018 3.45 85.87
90 30 13.1 15.8 1.04 4.60 4.018 2.30 57.24

Table 2: Yield for Bubble Column

Bubble Column
Conc of
NaOH CO2
Flow rate of Time NaOH at CO2 fed
v1 (ml) v2 (ml) reacted reacted Yield (%)
CO2 (L/h) (min) outlet (10^-3 (mol/hr)
(mol/hr) (mol/s)
mol/m3)
70 10 17 17.5 1.65 -0.45 3.125 -0.23 -7.20
70 20 15.5 16.2 1.48 0.06 3.125 0.03 0.96
70 30 16.5 17.2 1.58 -0.24 3.125 -0.12 -3.84
90 10 12.5 13.2 1.18 0.96 4.018 0.48 11.95
90 20 17.5 18 1.7 -0.60 4.018 -0.30 -7.47
90 30 12.5 13.8 1.12 1.14 4.018 0.57 14.19
Table 3: Outlets values

Average reacted in
CO2 fed (10^-3 Absorbed in
Time (min) bubble column Outlet (mol/s)
mol/sec) column (10^-3
(10^-3mol/s)
mol/s)
10 0.8681 0.5556 -0.0625 0.3750
20 0.8681 1.5278 0.0167 -0.6764
30 0.8681 1.6667 -0.1000 -0.6986
10 1.1161 1.0833 0.1333 -0.1006
20 1.1161 1.9167 -0.1667 -0.6339
30 1.1161 1.9167 0.4750 -1.2756

Error Analysis:

Least count of burette (ml) 0.1

Δ V1 (mL) 0.1
Δ V2 (mL) 0.1
Δ V3 (mL) 0.141
Δ V4 (mL) 0.173
Δ V5 (mL) 0

Absorption Column

Error in moles of NaOH

Error in moles of CO2 reacted Error in % yield
reacted
0.063 0.0315 0.6442
0.100 0.0501 1.4102
0.063 0.0315 0.6442
0.187 0.0937 2.2639
0.147 0.0737 1.5747
0.077 0.0383 0.5451
 Bubble Column

Error in moles of NaOH

Error in moles of CO2 reacted Error in % yield
reacted
0.0047 0.0024 0.0054
0.0007 0.0004 0.0001
0.0026 0.0013 0.0016
0.0141 0.0070 0.0209
0.0061 0.0031 0.0057
0.0176 0.0088 0.0311

Sample Calculations:
Initial concentration of NaOH = 1.5N
NaOH flow rate in absorption column = 10 lph
Air flow rate = 720 lph
CO2 flow rate in absorption column = 70/22.4 mol/hr = 3.125 mol/hr
= 90/22.4 mol/hr = 4.018 mol/hr

Calculation for absorption column

For CO2 flow rate = 70 lph, time = 20 minutes

● Titre reading for NaOH + Na2CO3 in terms of amount of HCl reacted (V1) -
Phenolphthalein indicator = 12.6 ml
● Titre reading for the above compounds + NaHCO3 (formed by reaction of HCl +
Na2CO3) (V2) - Methyl orange indicator = 15.7 ml
● Titre reading for HCO3- formed (V3) = 15.7-12.6 = 3.1 ml
● Titre reading only for Na2CO3 = 3.1 ml
● Effective reading for NaOH = V4 = V1 - V3 = 9.5 ml
● Concentration of NaOH used in titration = (Normality) X (volume of HCl)/ Vol.
NaOH
Here, Normality of HCl = 0.1 N, volume of NaOH = 10 ML,
Concentration = 0.1 x 9.5/10 = 0.095
As the NaOH solution at column outlet was diluted 10 times before titration, the
concentration of NaOH solution at outlet = 10 x (conc. Of NaOH titrated)
= 10 x 0.095 = 0.95
● Balance on hydroxide solution :
 nNaOH reacted = (nNaOH inlet - nNaOH outlet) x flow rate
= (1.5 - 0.95) mol/l x 10 l/hr = 5.5 mol/hr
● According to the reaction, 1 mol CO2 reacts with 2 moles NaOH, therefore,
Rate of CO2 consumption = 5.5/ 2 moles/hr = 2.75 mol/hr

● Yield of reaction:
Yield = moles of CO2 absorbed / moles of CO2 fed *100
= 2.75/3.125 *100 = 88%
Exit CO2 flow rate = (3.125-2.7) moles/hr = 0.425 mol/hr = 0.0071 moles/min

● Moles of CO2 fed in the bubble reactor at t=20 min = 0.0071 x 20 = 0.1417 moles.

Calculation for Bubble Column:

For CO2 flow rate = 70 lph, time = 20 minutes

● Titre reading for NaOH + NaCO3 in terms of amount of HCl reacted(v1) -
Phenolphthalein indicator = 15.5 ml
● Titre reading for the above compounds + NaHCO3 (formed by reaction of HCl +
Na2CO3) (v2 ml) - Methyl orange indicator = 16.2 ml
● Titre reading for HCO3- formed(v3 ml) = 16.2-15.5 = 0.7 ml
● Titre reading only for Na2CO3 = 0.7 ml
● Effective reading for NaOH = v4 = v1-v3 = 15.5 - 0.7 = 14.8 ml
We make an assumption here that all CO2 will first react with OH- to form CO32- rather
than react with CO32- to form HCO3- in column
● Concentration of NaOH used in titration = (Normality) X (volume of HCl)/ Vol.
NaOH
Here, Normality of HCl = 0.1 N, volume of NaOH = 14.8 ML,
Concentration = 0.1 x 14.8/10 = 0.148
As the NaOH solution at column outlet was diluted 10 times before titration, the
concentration of NaOH solution at outlet = 10 x (conc. Of NaOH titrated)
= 10 x 0.148 = 1.48
● Balance on hydroxide solution :
nNaOH reacted = (nNaOH inlet - nNaOH outlet) x flow rate
= (1.5 - 1.48) mol/l x 3 l = 0.06 moles
● According to the reaction, 1 mol CO2 reacts with 2 moles NaOH, therefore,
Rate of CO2 consumption = 0.06 / 2 moles/hr = 0.03 moles
● Yield of reaction:
Yield = moles of CO2 absorbed / moles of CO2 fed *100
= 0.03/3.125 *100 = 0.96%
Exit CO2 flow rate = (3.125-2.7) moles/hr = 0.425 mol/hr = 0.0071 moles/min
Final Balance on CO2 :

For CO2 flow rate = 70 lph, time = 20 minutes

● Total moles of CO2 fed in time t = 20, into the absorption column
= molar flow rate of CO2 x time = 2.6x20/60 = 0.8681 moles
● Total moles of CO2 absorbed in time t into absorption
= (molar rate of absorption at end of time t) x time = 2.75 x 20/60
= 0.7693moles
● Total Moles of CO2 reacting in bubble column = 0.0083
● Therefore, molar flow rate of CO2 at the exit = (0.8681-0.7963-0.0083) /
=0.0958mol/s
This is the average molar flow rate as CO2 consumption in the bubble reactor has been
averaged out.
Error analysis calculations:

Least count of burette = 0.1 ml

ΔV1 = ΔV 2 = 0.1 ml

V3 = V2 - V1
So, ΔV3 = √( ΔV 12 + ΔV 22) = √0.02 = 0.1414 ml
Similarly, V4 = V1,- V3 and ΔV4 = 0.173 ml

Absorption column:

For CO2 flow rate = 70lph and at t = 20 min,

Error in moles of NaOH reacted = nNaOH x √(( ΔV4/V4)2 + (ΔV5/V5)2)
= 0.1 mol/h

Error in moles of CO2 reacted = 0.5 * Error in moles of NaOH reacted = 0.05 mol/h

Error in yield% = yield * (error in CO2 reacted/ moles of CO2 fed)

= 88 * (0.05/3.125)
= 1.41 %

Bubble column:

For CO2 flow rate = 70lph and at t = 20 min,

Error in moles of NaOH reacted = nNaOH x √(( ΔV4/V4)2 + (ΔV5/V5)2)
= 0.0007 moles

Error in moles of CO2 reacted = 0.5 * Error in moles of NaOH reacted = 0.0035 moles
Error in yield % = yield * (error in CO2 reacted/ moles of CO2 fed)
= 0.96 * (0.0035/3.125)
= 0.0001%

Observations:
● There is large deviation of theoretical yield from experimental for NaOH
● The yield increases and then decreases with time for both 70lph and 90lph
● There must be some error in the data reported. This is because some of the
yields are coming negative which has no physical relevance. There is an error in
the data since the calculations give a negative value of flow rate which is not
physically possible.
● The yield is much higher in the absorption column than in the bubble column
● No specific increasing or decreasing pattern in yield is observed with increase in
flow rate.

Hypothesis:
The reported data is erroneous as can be seen from the negative values of yield.

This can also be justified from the titration data:

1) In absorption column,

Vol. of HCl Vol. of HCl (Methyl

CO2 flow rate (L/h) Time (min) (Phenolphthalein) (ml) Orange) (ml)
90 10 10 13.2
90 20 11.2 18

The sample at 20 min is much more than that at 10min which is against theoretical
explanation. Ideally NaOH concentration should decrease with time as it gets used up in
the reaction and thus less HCl should be required.
 2) Similarly error has been observed for the bubble column, we can observe the
discrepancies in the below data points

Vol. of HCl
(Phenolphthalein) Vol. of HCl (Methyl
CO2 flow rate (L/h) Time (min) (ml) Orange) (ml)
90 10 12.5 13.2
90 20 17.5 18

These large errors can only be attributed to wrong titration values being reported .

Conclusion:

● There is no specific pattern in results, mostly due to errors in given data, we do

not see the trends as expected.
● High error percentages in absorption columns indicates there must be error in the
reported data due to which expected trends are not observed

Special Question:
o Suggest an improvement in existing setup which will improve the reliability of the
experimental setup and quality of measured variables.

Since the major errors in the experimental values is due to wrong titration values being
reported , the following steps can be taken for improving the accuracy of titration:
● We need to re-check if the primary standard 0.1N HCl we are using is properly
standardized. This can be cross checked by carrying out titration with a stnadard
0.1N NaOH solution.
● The glass wares used for titration should have should have higher precision.
● The titration experiment should be repeated for 3 times at least and the average
value should be taken as it is often seen values can go off in a particular reading
due to human error