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Chemical Experiment of ammonia absorption

Technical Report · February 2013

DOI: 10.13140/2.1.3167.2323

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1.2 [Ammonia absorption]
Experiment conducted on [13 February 2013]

Module title: EUB_5_968 Principles of reaction and separation

Occurrence Number: [9]
Course: [BEng (Hons) Petroleum Engineering]
Prepared for: Dr Rim Saada

Prepared by: [Arcanjo Malo Wacunzo]

Student Number: [3021399]

[February/2013]

London South Bank University

Department of Urban Engineering
Faculty of Engineering, Science and the Built Environment
103 Borough Road, London, SE1 0AA
www.lsbu.ac.uk
 February 27, 2012 [AMMONIA ABSORPTION]

CONTENTS

Contents ........................................................................................................................... 2
List of Appendices……………………………………………………………………….2
Summary ......................................................................................................................... 3
CHAPTER 1 INTRODUCTION............................................................................ 4
BACKGROUND ............................................................................................................... 5
CHAPTER 2 EXPERIMENTAL EQUIPMENT ................................................. 5
INSTRUMENTS ............................................................................................................. 6
EXPERIMENTAL PROCEDURE ................................................................................. 7
CHAPTER 3 PROCEDURE AND OBSERVATIONS ................................... 8-14
CHAPTER 4 RESULTS AMD CALCULATIONS............................................ 15
CHAPTER 5 DISCUSSION ................................................................................ 16
CONCLUSION ……………………………………………………………………………17
REFERENCES ........................................................................................................... 18

LIST OF TABLES

TABLE 1.1 RESULTS OBTAINED ................................................................................................. 8,9,10

LIST OF FIGURES

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SUMMARY

The experiment undertaken was the ammonia absorption using counter current system. This is
a process used in the chemical industry and also within the petroleum industry whenever the
engineers obtain impurities from the down hole. These impurities can be diverse undesired
fluids or gas like H2S, CO2 and others.

By and large, the main objective of the experiment was to calculate the Kga which is known
as the overall mass-transfer coefficient. This coefficient would have been calculated based on
the data acquired from a system constituted of ammonia, air and water. This system had a
packed column, in addition to it the air flow rate was been changed whenever the system was
been restated.

In general, to proceed with the experiment in order to achieve the goals mentioned, a range of
instruments composed a system such as rasching rings, pipette, and volumetric glass.
Moreover, Air passing from a rotameter bubbles through a concentrated solution of ammonia
to pick up ammonia gas, also a stop watch to control the time. Safety was not forgotten,
equipment such as gloves and glasses were used due to the highly dangerous and volatile
substances used.

In general, a range of data were obtained and the flow rate of the air was been reduced from
14 to 4 overall. This resulted in a reduction of the volume of water absorbed and the duration
of the test was also longer as the air flow rate was been decreased. This fact was noticed by
the last test which nearly 30 minutes until the change of the parameter acid/basic.

Overall, the data required to make the calculation of the mass-transfer coefficient were
obtained in normal conditions, and it can be affirmed that the decrease of the air flow rate in a
absorption system can result in a longer time to determine whether the based was totally
transformed. These facts were relevant for our knowledge baggage, it was possible for the
group to understand a process used in real life and be able to observe the colour that indicated
an acid and an alkaline.

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CHAPTER 1 -- INTRODUCTION

I.I Background
The counter current System consists of two or more High Rate fluidized bed
reactor vessels connected in series raw water flows from vessel to vessel being
contacted with resin of a higher capacity in each subsequent reactor vessel.
Fresh regenerated resin is fed to the final reactor vessel while loaded resin is
removed from this vessel at the same rate and sent to the preceding vessel. (10)
The counter current contacting of raw water with Resin Allows more selective
competing anions to be removed with partially loaded resin in the first reactor
vessel so that fresh resin added to the final reactor vessel will remove less
selective target anions such as nitrate and bromide. This configuration can also
be used to remove high levels of more selective anions. The more efficient
sequential loading of Resin reduces the regeneration system size that would
otherwise be required for challenging contaminant removal using a standard
High Rate System, allowing significant reductions in waste volumes, salt
consumption and operating costs. (10)
Gas absorption is a mass transfer process in which a gas mixture is contacted
with a liquid to specially absorb the components of the gas stream. This action is
found in the chemical industry for the recovery of valuable products and
cleaning of exhaust or vent streams. (4)
In the oil and gas industry the ammonia is neutralizing the acid constituents of
crude oil and for protection of equipment from corrosion. In addition to
it, Ammonia is recycled in the mining industry for mining of metals. (3)
Ammonia is a very valuable source of nitrogen that is essential for plant growth
Agricultural industries are the major users of ammonia. (2)
The NH3 is a usual factor that is used in the production of fertilisers such as the
Urea. This has a great impact on various products which adds to its significance
and importance in the chemical and petroleum industries. (1)
Ammonia Absorption is a process in which a gas mixture of ammonia contacted
with a solvent commonly water to dissolve on or more components of the gas
and to provide a solution of them in the liquid. (1)

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Image 1: A counter current process system by MIEX. (Source Ref.10)

Falling film Theory statuses that the mass transfer process happens alongside an
interface, in which each phase is in the form of a stagnant layer of fluid of
specified thickness. This layer of fluid is called film and it is adjacent to the
interface. In the film, mass transfer takes place by steady-state one-dimensional
molecular diffusion in the direction normal to the interface. (3)
The penetration theory proposes that the time of contact of a fluid to mass
transfer is little. Consequently the concentration of the dissolved gas might be
considered to be equal to the bulk liquid concentration when the element is
reaches the surface. The residence time at the phase interface is the same for all
elements. Mass transfer takes place by unsteady molecular diffusion in the
various elements of the liquid surface. (3)

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The procedure taking place in the absorption column can also be visualised on the basis
of Two-Film theory. This happens in a way that an imaginary interface exists at the
border between the gas and water. With this the Gas and liquid films similarly exist at
either side of the interface and they are respectively bounded at the other end by the bulk
gas and bulk liquid. The concept clarifies that mass transfer will only occur at the
interface when there is a driving force on the gas film.
The aims of this experiment are to define the overall Mass Transfer coefficient of the
(ammonia, air, water) mixture at different air flow rates. This is a combined coefficient
of the fluid in the turbulent section, the transition section and the laminar film as well as
the coefficient of the mass transfer in the liquid.
A further objective of the experiment was to demonstrate why the gradient obtained
from the experimental curve did not match the literature value. This was verified by
calculating the Reynolds’s number as explained above.
Based on the theory investigated the formula used to calculate the mass transfer was:

K g a  B.FA
0.83

Mass Transfer
Coefficient vs Air
Flow Rate
5.0E-01
4.0E-01 Mass
3.0E-01 Transfer
Coefficie
2.0E-01
nt vs Air
1.0E-01 Flow
0.0E+00 Rate
0 0.2 0.4

This information investigated shows that as the air flow rate increased the mass transfer
coefficient increased which shows a direct proportionality between them.

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CHAPTER 2 - EXPERIMENTAL EQUIPMENT

2 - Diagram of the ammonia absorption system – Counter Current

Water
rotamete
r

Air
rotameter
Packed
rings

20ml 5ml H2SO4

H2SO4

H2O Air

Acid

H2O + NH3

Excess NH3 + H2H

H2O NH3

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Figure 2 – Photograph taken from the logbook sketch illustrating the system

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2.2 -- EXPERIMENTAL PROCEDURE

 Firstly, The water flow rate was set at 1L/min, and the water was allowed to
flow for 10 minutes to allow the packing to be fully wetted

 Then bottle one and two were filled up with 5ml and 20ml of sulphuric acid
respectively before being diluted with distilled water up to an equal mark on
both bottles

 6 drops of Phenolphthalein indicator was then added to the two solutions,

 Air flow was set to 14L/min and the air was allowed to bubble through the
Ammonia supply bottle. The air then went up through the column into the safety
bottle of sulphuric acid.

 The stop watch was initiated as the three-way valve was turned on allowing the
air to go through the absorption train (Bottle one & two).

 When the contents of bottle one changed colour to pink, the test was stopped by
closing the three-way valve and recording the time taken using the stop watch.

 Then the water containing the NH 3 was collected over the same period.

 the two bottles of acid were mixed together and were them used in back titration
using 0.01M solution of sodium Hydroxide (NaOH)

 After that, 25ml sample of the water collected was also titrated using 0.01M
solution of Sulphuric acid ( H 2 SO4 )

 The experiment was repeated for different air flow typically (14,10, 8, 4 L/min)

 The results were tabulated in the tables shown in results & calculations section.

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CHAPTER 2.1 – OBSERVATIONS

 The Colum with the packed rasching rings was showing vapour.

 The indicator showed the purple colour whenever the parameter changed

 As soon as the three way valve is opened the ammonia/air mixture bubbles
through the acid bottles

 The raching rings are randomly positioned to give maximum contact area

 The air rotameter was fluctuating at higher flow rates

 As the Air flow rate increased errors started occurring and less liable results
were obtained.

 The volume of NaOH used for the back titration in the first test was unusually
very high and the test was rerun and found to be normal.

 The air rotameter and water flow meter were not steady throughout the
experiment. This could lead possibilities of minor errors in the readings obtained

 The Three-way valve was controlled manually. There are possibilities of

discrepancies in the time recorded to shut the valve.

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CHAPTER 4 – CALCULATIONS

Graph 1 – Results obtained in the experiment to use for the

calculations.

Duration of Water Air H2SO4 Initial Back Volume of

test flow flow concentration H2SO4 titre water in
(L/min) (L/min) used in Volume absorption
absorption used

(s) FW FA N ml ml ml
135 1 14 0.01 25 19.3 4.8

298.8 1 10 0.01 25 22.5 3.4

384.6 1 8 0.01 25 31.2 2.5

1800 1 4 0.01 25 25 1.5

Sample Calculations
Sample calculation for the following tests tests in minute at air flow rate = 14, 10, 8, 4
L/m

First the values are converted to SI units the flow rate from L/m to L/s as shown below:
FA = 14 L / m → 14/60 = 0.23 L/s

FW = 10 L / m → 10/60 = 0.16 L/s

FW = 8 L / m → 8/60 = 0.13 L/s

FW = 4 L / m → 4/60 = 0.06 L/s

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 Calculations of the volume

The volume of H 2 SO4 used in absorption = 25 ml and the volume of back titration =
19.3 ml

Volume of H 2 SO4 neutralized by NH 3 = 25 – 22.5 = 2.5 ml

2.5 ml of 0.01 N solution contain ( 2.5*0.01) mol = 0.025 mol

 Calculating moles of NH 3 absorbed:

Moles of NH 3 0..025
Moles of NH 3 absorbed =  = 0.001 mol / s
Duration 22.5

 Calculating
NH 3 in air leaving ( yo ):

Moles of NH 3 absorbed 0.001

yo=  l  0.0043 mol NH 3 /L
Air flow rate in L/s 0.23

 Calculating moles of NH 3 in 10 gm sample:

2.9  10 3  0.01  2.9  10 5 mol

Calculating NH 3 in water leaving ( x o ):

2.9  10 5
xo =  0.0029 mol/L
10  10 3

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 Calculating y i by mass balance as shown below:

FA  yi  FA  yo  FW  xo

FW  x0  FA  y 0 (0.016  0.0029)  (0.23  0.0043)

yi    0.00045 mol / L
FA 0.23

 Now calculating the mass transfer coefficient k g a using this

equation:

N  k g a  ( y) mean

Where:

N  FA ( yi  yo )  0.23(0.00045  0.0043)  0.000046 Mol NH 3 / s

And:

1
( y ) mean   (ytop  ybottom)
2

to find ytop and ybottom

ytop  ( y0  yi* )  yo  2.4  10 -4

since Yi=0 when Xi =0

Change of concentration of ammonia (NH3) in air at the bottom of column is given by;

ybottom  ( yi  yo* )

Y*= 0.0012x y*= equilibrium value for ammonia concentration in the liquid
phase

yo*  0.0012  xo  0.0012  0.0026  3.12  10 6

ybottom  0.00045  3.48 10 6  4.49x1 03

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And now calculating ( y)mean :

( y) mean  0.5(3.12  10 -6  4.49x1 0 3 )  2.246  10 -3

So now calculating K g a :

N 0.000046
kg a    0.186
( y ) mean 0.000246 mol.s-1.m-2

 Determination of the slope n from the Log – Log graph of kga against FA

Using the equation Kg.a= B*FAn

After log both side of the equations

Log(Kg.a) = logB + n logFA

using the points on figure 2.

Slope (n) =

NH3 in NH3 in NH3 in Mass

Duration Water Air Air Air Water Transfer
of test Flowrate flowrate absorption Leaving Leaving Coefficient
S L/s L/s Yi (mol/L) Yo(mol/L) X0(mol/L) Kga log FA logKg.a

-
135 60 0.23 0.00045 2.46E-07 0.0029 0.455 0.57403 -0.2672

- -
298.8 60 0.16 0.00043 6.14E-08 0.0015 0.184 0.69897 0.55351

- -
384.6 60 0.13 0.000120029 2.88E-08 0.0012 0.15 0.77814 0.65042

-
1800 60 0.06 0.000125004 4.17E-09 0.001 0.144 0.87506 -0.7296

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0.0000003

2.5E-07

0.0000002
flowrate

1.5E-07
Series1
0.0000001
Linear (Series1)
5E-08

0
0 0.001 0.002 0.003 0.004
-5E-08
kag

Chart Title
0
-1 -0.8 -0.6 -0.4 -0.2 0
-0.1

-0.2

-0.3
slop 2

-0.4
Series1

-0.5

-0.6

-0.7

-0.8
slop 1

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CAPTER 6 – ANALISYS AND DISCUSSION

 The increase of air flow rate (8, 10, 12, 16 L/min) as shown in figure 2 in this
experiment with constant water flow rate of (1 L/min) has resulted an increase of
mass transfer coefficient, this indicates that the mass transfer coefficient is
directly proportional to the air flow rates, as the air flow rates increases the mass
transfer increases, this is means the air molecules entering the column increase
there will be a better mixing of air and water. Which in return results increases
mass transfer coefficient.
 The results obtained from the experiments indicates an increase in air flow rate
leads to more transfer of ammonia which in turn leads to an increase in mass
transfer coefficient.

 To accomplish the aims of experiment, which was to determine the overall

mass-transfer coefficient (Kga), in a small packed column for the air/ammonia/
water system at several different air flow rates? In experiment Four different air
flow rates of 14, 10, 8 and 4 L/min) were carried out with constant water flow
rate of 1 L/min and 25 ml of 0.01N sulphuric acid.

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 The packed Rasching rings were in the absorption column of up to 12 cm height

to provide greater contact area between the air and water. Which in turn provides
increased contact area between the air, which contains ammonia, and other side
which contains no ammonia just water only, therefore increased mass transfer
coefficient

 The 25ml volume of Sulphuric acid with of concentration of 0.01 N was

recycled during the experiment for the ammonia absorption, the volume of
H2SO4 used in absorption increases with the increases of air flow rate start with
(1.5 and 2.9 ml) at air flow rate of 10 L/min and 14L/min respectively, during
this experiment the volume of H2SO4 absorber was not part of parameter
intended to determine, therefore will require other parameter to take account
into. Adding 6 drops droplets of phenolthalein as an indicator, the time taken to
change colour in the bottle containing diluted sulphuric acid decreases with the
increase of air flow rate. This indicates that the higher the air flow rate the
shorter the time taken for the acid to exhaust.

 The investigations undertaken during the research shows that the reduce of the
air would definitely affect the results of the mass transfer coefficient. The
counter-current is a very different process used in the industry compared to the
rest of the currents used in the absorp[tion.

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CHAPTER 5-- CONCLUSION

In conclusion, the experiment allowed the group to consider the key points. These
points are:

 The counter current system is the most effective in this type of process were the
air enters from the bottom and the water from the top

 The parameter change takes longer as the airflow rate decreases.

 Considering the results it can be affirmed that the mass transfer coefficient is proportional to
the flow rate.

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References
1- Unit Operations of Chemical Engineering, 5th ed., W.L. McCabe & J.C. Smith,
McGraw-Hill, 1993. ( accessed on 15.02.13 )

2- Chemical Engineering, Vol. 2. 4th ed., J.M. Coulson & J. F. Richardson, Pergamon,
1991. . ( accessed on 15.02.13 )

3- Mass Transfer in Engineering Practice, A. L. Lydersen, Wiley 1985 . ( accessed on

19.02.13 )

4- Separation Process Principles, 2nd ed., J.D. Seader & Ernest J. Henley, John Wiley &
Sons 2006 . ( accessed on 21.02.13 )

5- Physical chemistry: Chemical principles: the quest for insight; P.Atkins, L.Jones. 3rd
edition 2005; Freeman. (Or earlier works by Atkins & Jones) . ( accessed on 22.02.13 )

6- Chemical reactors: Introduction to chemical reaction engineering and kinetics;

R.Missen, C.Mims, B.Saville; 1999; Wiley . ( accessed on 25.02.13 )

7- Catalysis: Catalytic chemistry; B.C.Gates; 1992; Wiley . ( accessed on 25.02.13 )

8- Concepts of modern catalysis and kinetics; I.Chorkendorff, W.Niemantsverdriet;

2003, Wiley . ( accessed on 26.02.13 )

9- http://www.miexresin.com/files/partnerSite/TechNote_CounterCurrent_V0608.pdf (
accessed 27.02.2013)

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Nomenclature

Symbols Description Units

T test Seconds
N mass transfer mol∙NH3∙s-1

FA Flow rate of the air L∙s-1

FW Flow rate of water L∙s-1

yi concentration of ammonia in inlet mol∙NH3∙L-1 of air

air
yo concentration of ammonia in outlet mol∙NH3∙L-1 of air
air
y* concentration of ammonia in air in
equilibrium with the solution of
ammonia

xo Concentration of ammonia in water mol∙NH3∙L-1 of water

out

xi Concentration of ammonia in inlet mol∙NH3∙L-1 of water

water
kga mass transfer coefficient, mol∙s-1∙bar-

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