Gas Absorption Colum-Mass Transfer Experiment A

A Research Study Presented to the

Faculty of the Department of Chemical Engineering
School of Engineering and Architecture
Saint Louis University

In Partial Fulfillment of the Requirements for the Degree

Bachelor of Science in Chemical Engineering

By
Liis, Nemuel Cyzar F.
Sario, Glen G.
Alindayo, Aimee C.
Felipe, Leica Jane G.
Juganas, Jasmin – Clary C.
Ramos, Kathrynne L.

September 2019

i
 TABLE OF CONTENTS

Gas Absorption Column-Mass Transfer Experiment A.....Error! Bookmark not defined.

TABLE OF CONTENTS .................................................................................................... ii

LIST OF TABLES ............................................................................................................. iii

LIST OF FIGURES ........................................................................................................... iv

ABSTRACT ........................................................................................................................ v

Chapter 1: Introduction ....................................................................................................... 1

Chapter 2: Design and Methodology .................................................................................. 3

Chapter 3: Results and Discussion ...................................................................................... 6

Chapter 4: Conclusion and Recommendation..................................................................... 8

REFERENCES ............................................................................................................... 100

APPENDICES ................................................................................................................ 111

APPENDIX A: List and Uses of Apparatus ............................................................... 111

APPENDIX B: Definition of Terms ........................................................................... 122

APPENDIX C: Computations ..................................................................................... 133

APPENDIX D: Documentation .................................................................................... 15

APPENDIX E: Answer to Questions ............................................................................ 17

ii
 LIST OF TABLES

Table 3.1 Rate of CO2 Absorption ...................................................................................... 6

Table 3.2 CO2 absorbed over a time period ........................................................................ 7

iii
 LIST OF FIGURES

Figure 1.1 Schematic of CO2 /water absorption system (Retrieved from:

http://ww2.che.ufl.edu/unit-ops-lab/experiments/GA/GA-Overview.pdf) ................ Error!

Bookmark not defined.

Figure 2.1 Schematic Diagram for Standardization of NaOH ......... Error! Bookmark not

defined.

Figure 2.2 Schematic Diagram for Standardization of Gas Absorption . Error! Bookmark

not defined.

Figure 2.3 Schematic Diagram for analysis of CO2 absorbed by water ............................. 5

Figure D.1 The Gas Absorption Column with CO2 Cylinder .......................................... 15

Figure D.2 The Student regulates the valve on the CO2 cylinder .................................... 15

Figure D.3 The Student adjusts and controls the flowmeter. ............................................ 15

Figure D.4 The students measure 100 ml of the samples taken into separate Erlenmeyer

flasks. ................................................................................................................................ 16

Figure D.5 The students add phenolphthalein indicator solution and it remained colorless.

The students titrate with standard NaOH solution.. .......................................................... 16

iv
 ABSTRACT

THIS EXPERIMENTAL STUDY IS ALL ABOUT GAS ABSORPTION

COLUMN-MASS TRANSFER. THE OBJECTIVES OF THIS STUDY IS TO
CALCULATE THE RATE OF ABSORPTION OF CARBON DIOXIDE INTO
WATER FROM ANALYSIS OF LIQUID SOLUTIONS FLOWING DOWN THE
ABSORPTION COLUMN. A POSITIVE AND NEGATIVE VALUES COULD BE
OBSERVED AT EVERY 10 SECONDS INTERVAL FROM THE CALCULATED
VALUES OF RATES. THE EXPERIMENT WAS CONDUCTED AT CONSTANT
FLOWRATES OF AIR, WATER AND CARBON DIOXIDE. RESULTING TO A
CONSTANT RATE OF ABSORPTION FOR EVERY GIVEN TIME PERIOD,
THE AMOUNT OF CARBON DIOXIDE DEPENDS ON THE VOLUME OF
NAOH. THE INLET CONCENTRATION INCREASES TOGETHER WITH THE
OUTLET CONCENTRATION. MEANWHILE, THE NEGATIVE RATE OF
ABSORPTION OBTAINED BY GROUPS 2, 4, AND 6 ARE BELIEVED TO BE
CAUSED BY THE HUMAN ERRORS DURING TITRATION.

KEYWORDS: Absorption, Mass Transfer, Carbon Dioxide

v
 Chapter 1

INTRODUCTION

Diffusion is the process by which molecules, ions, or other small particles

spontaneously mix, moving from the regions of relatively high concentration into regions

of lower concentration. This process can be analyzed in two ways. First, it can be described

with Fick’s law and a diffusion coefficient, a fundamental and scientific description used

in the first two parts of this book. Second, it can be explained in terms of a mass transfer

coefficient, an approximate engineering idea that often gives a simpler description.

Analyzing diffusion with mass transfer coefficient requires assuming that changes in

concentration are limited to that small part of the system’s volume near its boundaries. For

example, in the absorption of one gas into a liquid, it is assumed that gases and liquids are

well mixed, except near the gas-liquid interface. (Alo, n.d.)

The definition of mass transfer is based on empirical arguments like those used in

developing Fick’s law. Imagine we are interested in the transfer of mass from some

interface into a well-mixed solution. The mass transfer flux is proportional to the

concentration difference,

N1 = 𝑘(𝐶1𝑖 − 𝐶1 )

where k is called the mass transfer coefficient, A is the area of the interface, N1 is the flux

at the interface, C1i and Ci are the concentration at the interface and the bulk solution,

respectively.

Gas absorption is a unit operation in which soluble components of a gas mixture

are dissolved in a liquid (Perry, et al, 2008). Most gas absorption aims at separation of

acidic impurities from mixed gas streams. These acidic impurities include carbon dioxide

1
(CO2), hydrogen sulfide (H2S), sulfur dioxide (SO2), and organic sulfur compounds. The

most important of these are CO2 and H2S, which occur at concentration of five to fifty

percent. Gas absorption at an industrial scale is most commonly practiced in packed towers

(Alo, n.d.).

Figure 1.1 Schematic of CO2 /water absorption system (Retrieved from:

http://ww2.che.ufl.edu/unit-ops-lab/experiments/GA/GA-Overview.pdf)

2
 Chapter 2

DESIGN AND METHODOLOGY

This experiment aims to air pressure differential across the dry column as function

of the air flow rate, and to calculate the rate of absorption carbon dioxide into water form

analysis of liquid solutions flowing down the absorption tower. The approach applied in

this experiment was an experimental and qualitative design. To conduct this experiment, it

was aided with Gas absorption column with CO2 Cylinder, analytical balance, 1-L

Volumetric flask, Pipette and pipetol, Base buret and iron stand, Erlenmeyer flask, 1 – L

Reagent Bottle, stirring rod, watch glass, weighing bottles, Deionized water, 1 – L 0.02 M

NaOH Solution, KHP, Phenolpthalein indicator, CO2 – free distilled water.

For the procedure of this experiment, a schematic diagram is shown below:

A. Preparation and Standardization of Solutions

Prepare a 1 - L 0.02 M NaOH using a

CO2 - free distilled water

Standardize the NaOH Solution with

KHP standard then dissolve the KHP in
CO2 - free distilled water and dilute to
100 ml/.

Titrate the NaOh until the endpoint is

reached. Record the volume and
calculate the true molarity

Figure 2.1: Schematic Diagram for Standardization for NaOH

3
B. Gas Absorption

Fill the reservoir tank with 3/4 full of deionized

water.

Making sure that the valves C2 and C3 are closed.

Start the liquid pump having the water flow to 6
L/min.

Start the compressor by adjusting the valve C2 to

give an air flowrate of 20 L/min.

Adjust the C3 valve in order to regulate the flow of

Carbon dioxide to 10 L/min.

After 15 - minutes steady operation, take 150 ml

sample in every 10 minute intervals.

Figure 2.2: Schematic Diagram for Gas Absorption

4
C. Analysis of CO2 absorbed by Water

Place 100 mL of each samples in a separate erlenmeyer flask.

Titrate each sample with NaOH solution using

phenoplthalein as indicator.

Calculate the amount of free CO2 in water samples using :

𝑔𝑚𝑜𝑙𝑒 𝑉𝑁𝑎𝑂𝐻 𝑁𝑁𝑎𝑂𝐻
𝑓𝑟𝑒𝑒 − 𝐶𝑂2 = = 𝐶𝐶𝑂2
𝐿 𝑉𝑚𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒

Figure 2.3: Schematic Diagram for analysis of CO2 absorbed by water

5
 Chapter 3

RESULTS AND DISCUSSION

In this experiment, the efficiency of a packed gas-liquid absorption tower was

evaluated by determining the rate of absorption of carbon dioxide in water at different time

periods. Each group were assigned two trials for each time. The water used in the

experiment was subjected to be CO2-free to ensure that the readings for the absorption is

purely from the air. Also, deionized water was used because distilled water could dissolve

the CO2 until it is in dynamic equilibrium with the atmosphere which means that the

amount being dissolved balances the amount coming out of solution.

Table 3.1 Rate of CO2 Absorption

Time Sump tank Sample, S5 Liquid Outlet Sample, S4 Rate of CO2

from
Trial VNaOH, CCO2 in tank, VNaOH, CCO2 in tank, absorption,
start,
mL Ci, gmole/L mL Ci, gmole/L gmole/sec
mins.
1 22.2 2.5863 x10-3 19.8 2.3067 x10-3 2.7960 x10-5
10 2 24.2 2.1893 x10-3 20.2 2.3533 x10-3 4.6600 x10-5

1 18.1 2.1087 x10-3 23.1 2.6912 x10-3 -5.8250 x10-5

20 2 16.9 1.9689 x10-3 25.2 2.9358 x10-3 -9.6690 x10-5

1 24.6 2.8659 x10-3 15.9 1.8524 x10-3 1.0135 x10-4

30 2 25.3 2.9475 x10-3 22.2 2.5864 x10-3 3.6120 x10-5

1 22.8 2.6562 x10-3 30.6 3.5649 x10-3 -9.0870 x10-5

40 2 25.2 2.9358 x10-3 31.3 3.6465 x10-3 -7.1070 x10-5

1 27.9 3.2504 x10-3 25.8 3.0057 x10-3 2.4470 x10-5

50 2 28.8 3.3552 x10-3 24.7 2.8776 x10-3 4.7760 x10-5

1 23.0 2.6795 x10-3 24.0 2.7960 x10-3 -1.1650 x10-5

60 2 23.5 2.7378 x10-3 26.0 3.0290 x10-3 -2.9120 x10-5

1 22.5 2.2613 x10-3 12.2 1.4213 x10-3 1.2000 x10-4

70 2 - - - - -

6
 Table 3.1 shows the data used in order to solve for the rate of carbon dioxide

absorption in mole/second. From the calculated values of rates, a positive and negative

values could be observed at every 10 seconds interval. The experiment was conducted at

constant flowrates of air, water and carbon dioxide. The amount of carbon dioxide is

dependent on the volume of NaOH. The inlet concentration increases together with the

outlet concentration, resulting to a constant rate of absorption for every given time period.

The negative rate of absorption obtained by groups 2, 4, and 6 are believed to be caused by

the human errors during titration.

Table 3.2 CO2 absorbed over a time period

Time Period CO2 absorbed, gmole/sec
10-20 -3.9840 x10-5
10-30 6.1170 x10-6
10-40 1.8640 x10-6
10-50 9.0000 x10-6
10-60 7.0200 x10-8
10-70 -8.1500 x10-7

Table 3.2 shows the amount of carbon dioxide absorbed at different time period.

As the duration of absorption increases, it could be observed that the carbon dioxide

absorbed decreases. This is because at longer contact time between the carbon dioxide and

water, the carbon dioxide to be absorbed decreases.

7
 Chapter 4

CONCLUSION AND RECOMMENDATIONS

Gas absorption is a unit operation in which a soluble component is absorbed

by contact with a liquid phase in which the component is soluble. In this experiment, water

is used to remove carbon dioxide from air. The performance of packed gas-liquid

absorption tower is evaluated to determine how the mass transfer rate is affected by gas

flow rate, especially as the column approaches its loading and flooding points. The flow

rate for water, carbon dioxide and air were maintained constant, 6 L/min, 10 L/min and 20

L/min respectively, while having 10 minutes interval to get the concentration of the liquid

outflow in the tank. Titration was performed using a sodium hydroxide titrant up to the end

point.

From the data, it can be observed that if the volume of the standardized sodium

hydroxide solution increases, the concentration increases, and also the rate of absorption

increases. The negative rate of absorption values indicates that there is no occurrence of

absorption was found. It is concluded that at constant gas flow rate, the gas pressure drop

is higher at larger liquid rate. Thus, flooding is accompanied by a dramatic increase in

pressure, resulting in inefficient operation. It has been reported in literature that CO2

absorbs better at near flooding.

In this experiment, it is recommended to follow the procedure carefully in order to

avoid errors in the data needed. Parallax error must be avoided to maintain accurate data.

The students must read the marking scale in the burette perpendicular to the meniscus of

the titrant. Titration of the solutions must be carefully done to avoid over titration.

8
Accuracy must be established in measuring the volume of every solution that will be used.

Make sure to clean the apparatus before and after the experiment to avoid contamination

in the solution. Conducting the experiment accurately and precisely can lead to none or

less erroneous data.

9
 REFERENCES

Alo, J. (n.d.). Academia. Retrieved December 12, 2019, from

https://www.academia.edu/3997197/62986961_Lab_Report?auto=download
Green, D. W., & Perry, R. H. (2008). Perry's Chemical Engineers' Handbook, Eighth
Edition. The McGraw-Hill Companies, Inc.
(n.d.). Unit Operations. doi:http://ww2.che.ufl.edu/unit-ops-lab/experiments/GA/GA-
Overview.pdf

10
 APPENDICES

APPENDIX A

List and Uses of Apparatus

A. Gas Absorption column with CO2 Cylinder- The gas absorption column is a scale

unit designed to study hydrodynamic and absorption processes in packed columns. This

system absorbs ammonia or CO2 from a mixture with air in a watery solution that

descends along the column.

B. Analytical balance- It was used to measure the weight of the NaOH pellets.

C. Volumetric flask- It was used to contain the diluted the NaOH pellets for the desired

concentration.

D. Pipette and pipetol- It was used to measure and transport the solution to the

Erlenmeyer flask

E. Base burette- It was used to deliver the standard NaOH for titration.

F. Erlenmeyer flask- It was used to contain the solution for titration.

G. Reagent bottle- It was used to mix and contain the solution.

11
 APPENDIX B

Definition of Terms
A. Absorption- Absorption is a condition in which something takes in another substance.

It is a physical or chemical phenomenon or process, in which atoms, molecules, or ions

enter in the inner part of a gas, liquid, or solid material.

B. Mass Transfer- Mass transfer is the net movement of mass from one location to

another. It occurs in many processes, such as absorption, evaporation, drying, etc.

C. Carbon Dioxide- Carbon dioxide is a chemical compound composed of once carbon

and two oxygen atoms. It acts as a greenhouse gas. It is a major component of the

carbon cycle.

12
 APPENDIX C

Computations

mNaOH = 4 g Cconc. EtOAc = 10.2068 M

Vconc. HCl = 10 mL VHCl for quenching = 10 Ml
CNaOH = 0.0968 M CHCl = 0.1019 M

PREPARATION OF SOLUTIONS
 0.1M NaOH
𝒎𝑵𝒂𝑶𝑯 = 𝑪𝑵𝒂𝑶𝑯 × 𝑴𝑾 × 𝑽𝑻
𝑚𝑜𝑙 𝑔
𝑚𝑁𝑎𝑂𝐻 = (0.1 ) (40 ) (1𝐿) = 4 𝑔
𝐿 𝑚𝑜𝑙
For standardization:
𝒎𝑲𝑯𝑷
𝑪𝑵𝒂𝑶𝑯 =
𝑴𝑾𝑲𝑯𝑷 𝑽𝑵𝒂𝑶𝑯
0.408 𝑔
𝐶𝑁𝑎𝑂𝐻 = = 0.0975 𝑀
𝑔 1𝐿
(204.22 )(20.5 𝑚𝐿)( )
𝑚𝑜𝑙 1000 𝑚𝐿
 0.1M HCl
𝑪𝑯𝑪𝒍 𝑽𝑯𝑪𝒍
𝑽𝒄𝒐𝒏𝒄. 𝑯𝑪𝒍 =
𝑪𝒄𝒐𝒏𝒄. 𝑯𝑪𝒍
𝑚𝑜𝑙
(0.1 𝐿 )(1000 𝑚𝐿)
𝑉𝑐𝑜𝑛𝑐. 𝐻𝐶𝑙 = = 10 𝑚𝐿
𝑚𝑜𝑙
10 𝐿

For standardization:
𝑪𝑵𝒂𝑶𝑯 𝑽𝑵𝒂𝑶𝑯
𝑪𝑯𝑪𝒍 =
𝑽𝑯𝑪𝒍
(0.0968 𝑀)(10.55 𝑚𝐿)
𝐶𝐻𝐶𝑙 = = 0.1021 𝑀
10 𝑚𝐿
 0.1M EtOAc
𝑪𝑬𝒕𝑶𝑨𝒄 𝑽𝑬𝒕𝑶𝑨𝒄
𝑽𝒄𝒐𝒏𝒄. 𝑬𝒕𝑶𝑨𝒄 =
𝑪𝒄𝒐𝒏𝒄. 𝑬𝒕𝑶𝑨𝒄

13
 (0.1 𝑀)(1000 𝑚𝐿)
𝑉𝑐𝑜𝑛𝑐. 𝐸𝑡𝑂𝐴𝑐 = = 9.7944 𝑚𝐿
(10.2068 𝑀)

UNREACTED NaOH
𝑽𝑯𝑪𝒍 𝒇𝒐𝒓 𝒒𝒖𝒆𝒏𝒄𝒉𝒊𝒏𝒈 𝑪𝑯𝑪𝒍 − 𝑽𝑵𝒂𝑶𝑯 𝒇𝒐𝒓 𝒕𝒊𝒕𝒓𝒂𝒕𝒊𝒐𝒏 𝑪𝑵𝒂𝑶𝑯
𝒖𝒏𝒓𝒆𝒂𝒄𝒕𝒆𝒅 𝑵𝒂𝑶𝑯 =
𝑽𝑵𝒂𝑶𝑯
For 1:1
𝑚𝑜𝑙 𝑚𝑜𝑙
(10 𝑚𝐿)(0.1019 𝐿 ) − (10.1 𝑚𝐿)(0.0968 𝐿 )
𝑢𝑛𝑟𝑒𝑎𝑐𝑡𝑒𝑑 𝑁𝑎𝑂𝐻 = = 4.132 × 10−3 𝑚𝑜𝑙⁄𝐿
10 𝑚𝐿

RATE CONSTANT, 𝒌
𝟏 𝟏
−
𝒖𝒏𝒓𝒆𝒂𝒄𝒕𝒆𝒅 𝑵𝒂𝑶𝑯 𝑪𝑵𝒂𝑶𝑯
𝒌=
𝑽𝒕𝒊𝒕𝒓𝒂𝒕𝒆𝒅

For 1:1
1 1
𝑚𝑜𝑙 − 𝑚𝑜𝑙
4.132 × 10−3 0.0986 𝐿
𝐿
𝑘= = 11.5841
20 𝑚𝐿

RATE CONSTANT, 𝑲𝒆
𝟐(𝑪𝑵𝒂𝑶𝑯 )
𝑲𝒆 =
(𝑪𝑵𝒂𝑶𝑯 )(𝑪𝑬𝒕𝑶𝑨𝒄 )
For 1:1
2(0.0968)
𝐾𝑒 = = 20
(0.0968)(0.1)

14
 APPENDIX D

Documentation

Figure D. 1: The Gas Absorption Column with CO2 Cylinder

Figure D. 3: The Student

Figure D. 2: The Student regulates adjusts and control the
the valve on the CO2 cylinder flowmeter

15
 Figure D. 4: The students measure 100 ml of the
samples taken into separate Erlenmeyer flasks.

Figure D. 5: The students add phenolphthalein indicator

solution and it remained colorless. The students titrate with
standard NaOH solution.

16
 APPENDIX E

Answer to Questions

1. In the above experiment, why do you have to use CO2-free water in all your
solution preparations?
Solid sodium hydroxide is hygroscopic, which means that it absorbs
moisture from the atmosphere. Once it has a little moisture it also absorbs carbon
dioxide which is always present in air. The reaction is:
NaOH (s) + CO (g) → Na CO (aq) + H O (l)
2 2 3 2

This means that solid reagent grade sodium hydroxide is not pure enough
to weigh and use directly. Furthermore, the carbonate ion interferes in acid-base
titrations because 1) it is a weak base, and 2) it tends to make the color change at
the end point less sharp. This reaction also takes place in the aqueous phase,
where sodium hydroxide in solution reacts with CO2 from the air to form sodium
carbonate. This can change the concentration of standard solutions if steps are
not taken to minimize the carbon dioxide uptake.

2. Why is it preferred to use deionized water in the absorption column?

Deionized water is generally carbonate-free therefore it is preferred in the
absorption column.

3. What is the effect of temperature on the solubility of CO2?

As the temperature increases, the solubility of a gas decreases. That is why
more gas is present in a solution with a lower temperature compared to a solution
with a higher temperature.

17